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THE CONTENTS OF THIS DOCUMENT ARE THE HIGHEST QUALITY AVAILABLE.

INITIAL DATE ,/.30/9 CPP-621 Chemical Storge Area Acid Spills

SUBUNIT #4

SLUDGE PIT

•Sludge. Pit

SUBUNIT #3

NITRIC ACID SPILL

Approximate Uhit Soundry

VES-CS.100 -4,54zeillitoi (12)

VES-05 152 French Drain

WS-C.S.151 VES-CS-102 French Drain

VES-CS-101

SUBUNIT #2

ALUMINUM NITRATE AREA

CPP 727 CPP 757 SUBUNIT #1

ACID STORAGE VAULTS

CPP-45 CHEMICAL STORAGE AREA SUBUNITS c,I 91 vi

N 694,750 [ 296,407 719-A (VES -CS- 100) 719-B ( VES-CS 15 ) 1 1 757 w /7/ 16,7)3- x X > I I 607 621 617 -CS-152)72C-A -CS 102)72 727 (VES -CS ECA—CPP-45 o 25. so. ma' 7ONE C-5 isar""""%somr • /2() C (VI 1 kau ILYSPOOKO

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111 1111 weirt-IIWOr SUM1-11115 nt011-44PaSti cr— Q Val EZZ)- 0- add 9-23-- Si'LS-28

Draft: 8/2/90: GS

Cateqorical Exclusion for Sampling SWMU CPP-45: CPP-621 Chemical Storaqe Area Spills. r. L. L- V

Unit Description/HistorY

Various acids (HC1, HNO3, HF, and H2SO4) and aluminum nitrate are stored in large metal and fiberglass tanks encircled by earth berms south of CPP-621. The storage area consists of 8 tanks, 2 open bottom limestone pits and six French drains (see Figure 1). During the history of operations in the CPP-621 area, five releases are known, or are suspected to have occurred. A summary of the pertinent areas and known or suspected releases within the CPP-621 area is given below.

1. Hydrofluoric Acid (HF) tank (VES-CS-169) was surrounded by an open bottom pit (CPP-727) which contained limestone to neutralize the contents of the HF tank if the acid and limestone were contained in a completely mixed tank. VES-CS-169 has a capacity of 9,700 gallons. In the past, a steam condensate drain from building CPP-621 discharged to a small (approximately 11 x 1') collection pit on the north wall of CPP-727.

Prior to 1986, any leakage in this pit would have gone directly to the soil. In 1986, a floor was constructed in CPP-727 to contain releases, and the overflow from VES-CS-169 was rerouted to an overflow collection container.

CPP-727 received HF and potentially HC1 and H2SO4, from past releases from the tank overflow and vent lines. One HF spill is known

C.Y\

REF .4 5 _y_1149-0-rGS to have occurred (approximately 15 L in 1988), and numerous small spills are suspected. In addition, steam condensate from building CPP-621 drained into a small pit located at the foot of the north wall.

2. The HCL (VES-CS-167) and H2SO4 (VES-CS-164) tanks were surrounded by an open bottom pit (CPP-757). Each of the tanks has a 4,000 capacity. The vent and overflow lines from VES-CS-167 and -164 drained to CPP-727, however, accidental spills could have drained directly to the soil in CPP-757. These acid tanks have been taken out of service and removed from the unit.

CPP-757 received a release of approximately 1,136 L of H2SO4 during a pipe flushing operation in 1988. In addition, CPP-757 may have received small releases of HCL and H2SO4 prior to the decontamination and decommissioning of VES-CS-164 and -167.

3. Three aluminum nitrate tanks (VES-CS-101, -102 and -152) are located south of building CPP-621 and west of the the chemical trench. VES-CS-101 and -102 have a 8,000 gallon capacity and VES-CS-152 has a 18,400 gallon capacity. Two nitric acid tanks (VES-CS-100 and -151) are located south of building CPP-621 and east of the chemical trench. VES-CS-100 has a 34,100 gallon capacity and VES-CS-151 has a 18,400 gallon capacity. Prior to the construction of the chemical trench in 1986, the tanks were surrounded by earthen berms and each tank had a French drain used for collecting overflow discharges. In 1986, secondary containment was constructed around the tanks.

In March 1982, HNO3 was delivered to tank VES-CS-100. Approximately 1,200 gallons of acid overflowed to the French drain and eventually over the ground. The soil in the spill area was sampled at the time of the spill and was found to have a pH of approximately 10. The acid was not contained since the berm had been removed for construction of c c Draft: 8/2/90: GS the chemical trench. The overflowed acid pooled along side the concrete wall being installed for the pipe trench, south of VES-CS-151. Several thousand pounds of soda ash was applied to neutralize the acid and the contaminated soil was excavated for disposal.

4. A sludge pit is located adjacent to the northeast corner of building CPP-621. The sludge pit was installed when the aluminum nitrate tanks were installed. Prior to approximately 1986, deliveries of aluminum nitrate were filtered to remove impurities. The impurities were then sent to the pit. After 1986, all aluminum nitrate ordered has been filtered prior to delivery and the use of the pit was discontinued.

No releases of hazardous waste have been documented to the sludge pit, however, sampling conducted by the University of Utah Research Institute (UURI) indicate elevated levels of Hg.

5. Building CPP-1614 is a corrugated metal building located adjacent to VES-CS-151 and pit CPP-757. The building houses pumps used for transferring H2SO4 from VES-CS-164 to the FAST facility (CPP-666).

A release of approximately 86 L of H2SO4 is known to have occurred in building CPP-1614. The release was due to a pipe leak which occurred in 1986.

Preliminary Sampling

Preliminary sampling was conducted by the University of Utah Research Institute, Murry, UT in 198_i"The areas sampled are shown in Figure 2. The preliminary analysis indicate that the hazardous wastes/constituents were found above background levels in the following areas: o mercury was above background in the three aluminum nitrate French S/2 3,41/90: GS drains. The aluminum nitrate French drains were remediated in 198_. o fluorides were above background in CPP-727; o lead is above background in the chemical trench.

No hazardous wastes/constituents were found above background levels in CPP-757.

Since the UURI sampling program was preliminary in nature, additional sampling will be required to verify that no contaminated soils are present.

Environmental Concerns

Progosed Actions

Sampling will be conducted in containments CPP-727 and CPP-757. Initially, 3 boreholes will be drilled in each containment to a depth of six feet. Each hole will be sampled at 0-2, 2-4 and 6-6 feet. At the completion of sampling, each borehole will be backfilled with clean soil taken from the clean construction soil pile located south of the ICPP fence.

A11 sample analyses will be conducted in accordance with the methods outlined in EPA's "Test Methods for Evaluating Solid Wastes" (SW-846). Soil samples collected from CPP-727 will be analyzed for fluorides, TCLP metals and pH. Soil samples collected from CPP-757 will be analyzed for sulfides, chlorides, TCLP metals and pH. One sample from each containment will be analyzed for 40 CFR 261, Appendix VIII constituents. Draft: 8/2/90: GS If analyses indicate that contamination is present at the six foot level in either containment, a decision will be made to either drill additional FV boreholes to collect samples at greater depths, or to defer further sampling until required by the COCA or Interagency Agreement schedule.

Contractor Environmental Organization Review

A categorical Exclusion is appropriate for the described activity. A categorical exclusion should be granted on the basis that the proposed activity is a Site Characterization and Environmental Monitorinq activity as outlined in the list of categorical exclusion in the Federal Register, Volume 55, number 67, page 13066, April 6, 1990. Sludge Pit

232 -4E- Approximate Unit Boundry CPP 621

*200 202 230 201 203* VES-CS-100 *231

VES-CS-152

215 * 204 216 North Pit 205 229 217 226* French Drain 227

VES-CS-102 C• VES-CS-151 218,219* —J. South Pit French Drain 220. 221* / Nitric Al C.) VES- CS-101 *222 223 CPP 1614

224* 225 Chemical Trench 209 710

VES-CS-I69 VES-CS-167 VES-CS-164 • 211, 213 4, HE *208 *

212* 214 CPP 727 CPP 757 Condensate Dry Well •206. 207

CPP 607

SCALE

0 10 20 Ft - Sample Location Sample Locations At The CPP-621 Chemical Storage Area MOMI59 winfiv Draft: 7/31/90: GS .9 CLOSURE PLAN FOR ACID CONTAINMENTS AND FRENCH DRAINS IN THE CPP-621 AREA

EPA Facility ID No.: ID 4890008952 Owner's Name: Department of Energy, Idaho Operations Office Address & Phone No.: 785 DOE Place Idaho Falls, Idaho 83402 (208) 526-1505 Facility Address: Scoville, Idaho

I. UNIT CONDITIONS

A. General Information

The Idaho Chemical Processing Plant (ICPP) acid storage area, located at CPP-621, is shown in Figure 1. The acid storage area has six french drains and two open-bottomed containment areas which are filled with limestone (constructed to be used in the event of an overflow or spill). This closure plan will address the method- ology used to eliminate the french drains and open-bottomed con- tainment areas, in addition to the proposed plans for controlling overflows and/or spills once the drains are closed.

The acid storage area (CPP-621) consists of eight tanks. There are two nitric-acid tanks - CS300 capacity of 34,100 gallons and has one french drain;--a6d 013451 has a capacity of 18,400 gallons and has one french drain. The sulfuric acid tanks, CS-164 and CS-167, each have a capacity of 4000 gallons, giving a total capacity of 8000 gallons. The two tanks share a limestone-pit containment area where there are no french drains. The hydrofluoric acid tank, CS-169, has a capacity of 9700 gallons and has one french drain with an open- bottom limestone pit containment area. This tank was recently con- structed as part of the FAST facility and is surrounded by a limestone pit which is approximately 20 feet by 15 feet by 6 feet. Each of the aluminum-nitrate tanks, CS-101 and CS-102, has a capacity of 8000 gallons and(eactOlas a separate french drain. Another aluminum- nitrate tank(IlaS a capacity of 18,400 gallons and has one french drain. Thus, a total of six french drains and two open-bottom limestone-pit containment areas must be closed.

The actual quantity of acid which has overflowed or spilled into the h CiL drains is unknown; however, the quantity is believed to be smell. c-0 c Sampling of the soil has not previously been accomplished. The average pH of soil at the ICPP has,,19egft_found to be approximately 10. This fact, in conjunction with thettreatment of the.acid in limestone pits, leads us to believe thatvehtsoil will ribt\ be found to be contaminated with hazardous wastes

n•A ' ?,t Qer o

B. Schedule of Partial Closure

To reduce the likelihood of acid flowing into the soil through any of these french drains or limestone pits, WINCE) has initiated a policy whereby no tank is filled to more than 80 percent capacity. This administrative control has eliminated any acid disposals that might occur as a normal mode of operation.

C. Maximum Amount of Waste in the Unit

It is believed that the waste soil derived from the closure of the acid storage area will consist of hazardous waste. Soils will be analyzed for pH, sulfates, and fluorides. There are no indications that radioactively-contaminated soils will be found. However, due to the nature of operations at the ICPP, soils will be analyzed for radionuclides. In the unlikely event that mixed waste is found, the waste will be packaged and sent to a permitted storage facility at the INEL. However, if the soil is acidic and has no other hazardous characteristics or constituents, it will be neutralized and disposed of as backfill. The maximum amount of hazardous waste is believed to be relatively small due to the use of limestone, the pH of the soil, and the rarity of overflows or spills from the storage tanks.

D. Inventory of Auxiliary Equipment

Auxiliary equipment which may need to be decontaminated and/or disposed of will include old piping, french drains, and miscellaneous equipment. All equipment will be analyzed for hazardous material and radionuclides. If the equipment is found to be contaminated with hazardous wastes, then the equipment will either be treated with a caustic solution to neutralize it, or it will be transported to an off-site TSD facility. If the equipment is found to be radio- actively contaminated, then it will either be decontaminated on site or sent to the Radioactive Waste Management Complex (RWMC). In either event, all procedures and guidelines will be adhered to throughout the process of decontamination and disposal or storage.

E. Schedule of Closure

Figure 2 provides a milestone chart for the closure of the acid storage area french drains and open-bottom limestone-pit containment areas. A project scheduled for ICPP involves the construction of containment vaults. The new containment vaults will be constructed to meet the specifications of the regulations under RCRA (40 CFR 260-265).

F. Estimated Cost of Closure for Unit

This estimate assumes the worst case to include a possible mixed and/or radioactive waste in addition to hazardous waste. $K

Sample collection: 50 Sample analysis: 30 Engineering remedial design: 30 Closure completion: 60

Total: 170

II. DECONTAMINATING THE UNIT

A. Area of Unit with Potential Soil Contamination

The potential contamination should be limited to the soil beneath each tank to include the french drains.

EPA-approved field procedures will be used to collect representative samples by qualified and trained personnel. Also, vadose-zone- monitoring may be conducted to determine the extent of releases. WINCO or other laboratory facilities, with appropriate quality control and quality assurance programs, will use EPA-approved laboratory pro- cedures to quantify the presence or absence of hazardous materials. These samples will be analyzed for: pH, fluoride, sulfate, EPA EP- toxic materials, and radionuclides. If significant levels of contam- ination exist in any sample, then additional sampling and analysis will be performed to determine the degree and extent of contamination. This information will be used to estimate the volume of contaminated soil. All contaminated material will be removed and sent to an off- site TSD facility. Contaminated soil will not be disposed of on site. If mixed radioactive waste is identified, it will be removed and sent to a permitted storage facility at the INEL.

B. Equipment Requiring Decontamination

If the soil is found to be hazardous and/or mixed waste, then removal will be performed. All equipment used to perform this task will require decontamination. A11 contaminated equipment will be placed in a stainless-steel pan and decontaminated. A11 wash water and/or solvents will be disposed of as required according to RCRA require- ments. A11 solid waste generated during decontamination operations will also be disposed of according to RCRA requirements.

III. GROUNDWATER MONITORING

Since all soils found to be contaminated will be removed and/or treated in place, long-term groundwater monitoring will not be required. How- ever, short-term vadose-zone-monitoring may be performed as part of the unit characterization to evaluate the extent of the release from this unit. O C: IV. CLOSURE CERTIFICATION -a An independent, professional engineer will verify that every major step of the closure process is completed in accordance with the approved plan and will certify that closure is complete. Closure certification will not be necessary if all waste is transported off site to an EPA- approved TSD facility. Figure 2 Closure Schedule for ICPP Acid Storage Area (CPP-621)

Number of days from start

Strt 60 120 180 240 300 360 420 480 540 600 660 720 780 840 900 960 Activity

Final date unit was used (April 23,1985)

EPA Approval of Closure Plan

Complete Charcterizatfort

If soll Is non-ftazardous, administratively close or if soll Is hazardous or mixed waste, begln removal

Complete unft decontamination

Obtain closure certification SM. CPP 666 MAH-FE F ^ ST FACILITY C 84 304 tJE UNDER CONS T ) o .-__,Weertfrressittlisitensthitite- CA w CP P 767 cLj MAPLE S VES-CS-164 ;41 0 CP 759- Pc VES-CS-100 LE HING VES CS- 1 67-\ VES-CS-151 T-1 T-5 CE POOL CPP 719 734 A o SLAB MING STATION CD PP-72C LIQUID QXYGEN CPP 617 VES-SAA-121,2y CPP 621 A A CS-152 CS-101 4".1 CS-102 BIRCH STREET

_L x—x VE3-CS-169 CPP 613 CPP-727 CPP x CPP 718 x 653 O I GREASE PIT nn ano x rurnigi ‘-/14-PP 7S8 MONITORING VMF OFFICE CESSPOOL

SPATROL ROAD C PP 661

LOCOV E R LIESYT 200' 300'

Figure 1 r-- MEMO OF CONVERSATION

Date: February 11, 1992 Time: 15:00 Commitment Made [ ] Yes [ ] No

Person Calling: Bruce Culp Person Called: Keith Farmer

Representing: WINCO ER Representing: WINCO Production

Purpose of Conversation: Confirm physical features at CPP-621

Text of Conversation: I asked Keith several questions to confirm physical features and processes at the CPP-621 Acid Storage Area.

Question #1: What lines have run through the chemical trench south of CPP- 621. Answer #1: Only Nitric Acid and Aluminum Nitrate.

Question #2: What lines have run through the chemical trench running next the Acid Storage Vault CPP-727.

Answer #2: Hydrochloric, Hydroflouric, Sulfuric, Nitric and Aluminum Nitrate all run through this pipe trench.

Question #3: What is the history and how did the sludge pit operate east of CPP-621 Chemical Storage Pumphouse.

Answer #3 Aluminum Nitrate was filtered in the CPP-621 building and the filters were backwashed through a pipe to the sludge pit. The Sludgepit has not been operated since 1986 and the pipe has been removed. As far as he knows, no other chemicals have gone to the sludgepit.

Signed: Date: ,./tc(ct

REF *7 00 MEMO OF CONVERSATION

Date: February 11, 1992 Time: 15:45 Commitment Made [ ] Yes [ ] No

Person Calling: Bruce Culp Person Called: Larry Chigbrow

Representing: WINCO ER Representing: WINCO Production

Purpose of Conversation: Inquire about secondary containment project at Nitric Acid tanks.

Text of Conversation: (Larry was the project engineer working for Ruffner during the secondary containment project in 1987/88.)

Question #1: What was done to french drains and soils under the nitric acid tanks at CPP-621 before the stainless containment vaults were placed? Answer #1: The French drain tiles were removed, however no soils were removed and the holes were filled in. The entire area was leveled and a layer of sand several inches deep was laid down before the secondary containment vaults were constructed.

Signed: Date: /1/14 1q3

REF A 0-- c c National Engineering Laboratory -,J ECN-01-86 CD N' GO From E. C. Newsome Phone 6-3188/CPP-602 Date March 11, 1986 SAKI Requirement for Filtering Aluminum Nitrate

m J. A. Rindfleisch, Manager Technical Process Analysis LuDGE 12(1- cc: B. R. Dickey J. E. Johnson C. E. Jones J. L. Lee D. J. Poland mj L. L. Weidert E. C. Newsome (2)

You are probably aware of the environmental concerns with discharge of chemicals to "French drains" at the ICPP. Management is committed to eliminating all of this type of drain as soon as possible.

One of these French drains, specifically a sludge pit, receives solution from aluminum nitrate filtering operations at CPP-621. Currently, a maintenance package is being formulated to isolate the filtering vessels and piping from the sludge pit. As a result, no method is available for filtering aluminum nitrate during the second and third cycle operation.

I propose to eliminate the requirement for filtering aluminum nitrate at the ICPP and I request your concurrence based upon the fact that the aluminum nitrate furnished by the supplier is pure enough for use as is.

The aluminum nitrate that is received is filtered by the manufacturer before it is loaded for shipment. The filter media used is diatomaceous earth, and for all purposes, is the same that is used in the CPP-621 filtering operation. Samples of the bulk receiving tank solutions (unfiltered) show that the undissolved solids (UDS) are in the order of 3.08 micro grams per milliliter of solution. Samples of the solutions in the filtered tanks show the undissolved solids to be approximately 3.16 micro grams per milliliter. The sample results indicate that filtering of the bulk aluminum nitrate solution at the ICPP is not needed.

(VV) Westinghouse Idaho Nuclear Company. Inc. Mr. J. A. Rindfleisch Page 2 ECN-01-86 March 13, 1986

Furthermore, all of the feed tanks where aluminum nitrate solutions are fed into the process have in-line filters installed.

I request that you evaluate this information and my proposal to eliminate any future filtering of aluminum nitrate at the ICPP. I need your response by March 18, 1986 so as not to adversely affect the second and third cycle operation.

e)" . .g..“--e-rntee---- E. C. Newsome Fuel Processing Facilities

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REMEDIATION O CONTAMINATED SOILS CHEMICAL SI PAGE-AREA IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

Earth Science Laboratory

University of Utah Research Institute 391 Chipeta Way, Suite C Salt Lake City, Utah 84108 (801) 524-3422

September, 1987 Rer o o CI: A) FINAL REPORT O C, REMEDIATION OF HG CONTAMINATED SOILS

CHEMICAL STORAGE AREA

IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

TABLE OF CONTENTS

1.0 Introduction 1

2.0 Remediation Procedures 1

3.0 Sample Procedures 4

4.0 Analytical Procedures and Results 4

5.0 Data Quality 5

6.0 Evaluation of Results 6

References 7 LIST OF FIGURES

Figure 1 Map of CPP facility showing location of project area 8

Figure 2 Location of excavations 9

LIST OF TABLES

Table 1 Sample locations, pH, percent moisture, nitrate, and Hg contents of samples 10

Table 2 Precision and accuracy data for analyses 11 o o CO

o cn 1.0 Introduction

This report documents the removal and verification sampling of mercury contaminated soils from french drains located at the

Chemical Storage Area (CPP 621) of the Chemical Processing Plant

(CPP). The complex is managed by the Westinghouse Idaho Nuclear

Company Inc. (WINCO). Mercury contaminated soils had previously been identified as a result of an initial site characterization

(reference 1) conducted by the University of Utah Research

Institute (UURI).

2.0 Remediation Procedures

Two excavations were required to remove the contaminated soils. The bulk of the soil was removed with a backhoe fitted with a flat plate welded across the teeth of the bucket to prevent cross contamination of adjacent soil. The locations of the excavations are shown in Figures 1 and 2. Their size and depth was limited by the presence of aluminum nitrate tanks adjacent to the drains. During the excavation, shoring requirements for tank stability and for workmen's safety were closely monitored by site engineers and safety personnel.

The excavation of the soil was conducted in four steps.

1. Non-contaminated soil was excavated to a depth of 2'6".

This depth was within one foot of the bottom of the drains. The

1 o o CO NI excavated material was stockpiled for future use as backfill. o Cr, The clay pipes that were used for the french drains were broken up and placed into drums. A plywood sheet wrapped in visqueen was placed over the area where the drain was located in order to cover the potentially contaminated exposed surfaces. After these areas were covered, the surrounding area was excavated to remove loose soil and to widen the excavation prior to removing the potentially contaminated material.

2. Potentially contaminated material between 2'6" and 6'6" directly under the drains, and to 5'6" peripheral to the drains, was excavated with the backhoe and placed directly in drums.

Excavation of the soil below 2'6" proceeded in increments of 4 to

The drums were placed on visqueen and a large plastic funnel was used to preclude the spreading of potentially contaminated soil. The visqueen was removed and drummed after each set of drums were filled. The drums were moved by crane onto pallets for further processing and labeling.

3. After both holes were excavated, the backhoe bucket was again decontaminated to insure that potentially clean material remaining in the pits was not contaminated with soils from the bucket. The excavations were deepened an additional 1'6" to 2' and the removed material was placed onto clean visqueen and stockpiled. In order to insure the safety of the workers, the backhoe was used to remove the final layer of potentially contaminated soil from the north pit which was excavated to

6'10". The south pit was deepened to a depth of 7' with

2 decontaminated shovels. The maximum depths of the excavations

were dictated by the need to insure the stability of the storage

tanks.

3.0 Verification Sampling Procedures

Soil samples were taken from the excavated material, the

walls and bottom of the excavation, and from a depth of 2' below

the excavations to verify that the contaminated soil had been

removed. A11 samples were collected by qualified personnel. The

sampling, sample handling, and decontamination procedures

followed during the collection of the soils are described in the

Quality Assurance Sampling Plan prepared for this project

(reference 2). Soil sample locations are given in Table 1.

4.0 Analytical Procedures and Results

The soil samples were analyzed for percent moisture, pH,

nitrate-nitrogen (NO3-N), and mercury (Hg) by the University of

Utah Research Institute (UURI) located in Research Park at 391

Chipeta Way, Suite A, Salt Lake City, Utah. This laboratory is

certified by the State Health Laboratory, Bureau of Laboratory

Improvement, for the required analyses. Utah is a "Primacy"

state in which EPA RCRA programs are managed at the state level

by authorized state agencies.

The analytical results are presented in Table 1. Nitrogen

values are given in parts per million (ppm), Hg values in parts

per billion (ppb).

3 CD o Cr) 00 Background concentrations of Hg and NO3-N were determined on O Cr) samples taken from the area around the CPP complex. (reference

1). A summary of the background data (mean, standard deviation and mean + 2 standard deviations) is given in Table 1. For comparison the Hg contents of soils developed over volcanic rocks typically ranges from 10 - 180 ppb and averages 50 ppb (reference

3).

5.0 Data Quality

The accuracy and precision of the analyses were determined from a statistical evaluation of the quality control samples.

Accuracy data were obtained from the analysis of standard reference materials, spiked field samples and standards analyzed along with the project samples. Precision data were obtained from duplicate analyses of field samples and standards analyzed with project samples. Control limits for accuracy and precision are nominally established by the EPA to be equal to the mean + 3 standard deviations. Quality control data for the analyses are contained in Appendix 1. These data indicate that the analyses fall within acceptable limits. A summary of the precision and accuracy data for the analyses is presented in Table 2.

Soil samples are heterogeneous and thus present inherent analytical problems. Often very small particles of a particular contaminant may not be present uniformly throughout the sample causing anomalies in data which must be verified through addi-

4 o o CD tional analysis. The UURI Laboratory performed multiple analyses I\D o in order to confirm the accuracy of its reported data. m

6.0 Evaluation of Results

The following conclusions can be drawn from a comparison of the analytical data with the background analyses:

1. Soil excavated from the northern pit has Hg contents greater than the background values.

2. The average Hg concentration of unexcavated soil is

<58.3 ppb. This value is approximately equal to the background mean + 2 standard deviations and is within the range of Hg contents of soils developed over volcanic rocks.

3. Repeat analyses of the samples indicate that the Hg is heterogeneously distributed in the soil.

4. No systematic variation in the Hg content of the unexcavated soil is apparent.

5. The NO3-N contents of the soils are slightly elevated above the background values, suggesting some contamination of the soil by either nitric acid or aluminum nitrate. SAMPLE AREA

FIGURE-1 9(2900 0 0 FD = French Drain Ci: Sludge ND P it * 0 CPP 621 0 Sample Location cn 232 r ,Excavations

230

..; 215 204 216 205 ...... 217 o North pit

209 210 Chemical Trench

Condensate Dry Well •206, 207

CPP 607

SCALE

0 10 20 Ft I 1 1

Sample locations at the Chemical Storage Area FIGURE 2 o o

TABLE 1 11.D cr) LOCATION AND ANALYTICAL RESULTS OF SAMPLES COLLECTED DURING EXCAVATION OF THE FRENCH DRAINS

SAMPLE MOISTURE pH NO3-N Hg NUMBER (%) (ppm) (ppb) SAMPLE LOCATIONB

860400 4.06 8.48 4.24 53 Excavated from NP 860401 3.59 8.37 1.40 75 Excavated from NP 860402 8.56 8.31 2.75 260 Excavated from NP 860403 7.38 8.32 4.02 <82A Excavated from NP 860404 5.20 8.40 2.74 <50 Excavated from NP 860405 5.23 7.93 8.58 50 Excavated from SP 860406 4.33 8.30 6.30 <50 Excavated from SP 860407 5.28 8.27 7.12 <50 Excavated from SP 860408 2.63 8.66 0.77 <50 Unexcavated soil, SP 860409 3.86 7.30 4.64 <50 Unexcavated soil, SP 860410 4.02 8.02 0.79 <55A Unexcavated soil below drain SP 860411 3.86 8.30 5.15 <50 Unexcavated soil, SP 860412 5.28 7.94 8.57 <50 Unexcavated soil, SPy 860413 3.48 8.25 3.13 <50 Unexcavated soil, SP 860414 5.73 8.13 0.95 <50 Unexcavated soil, SP 860415 4.18 7.74 2.30 <50 Unexcavated soil, SP 360416 5.32 7.65 1.19 <50 Unexcavated soil (duplicate), SP 860417 8.98 7.09 1.90 <75A 2' below pit bottom, SP 860418 3.58 7.80 1.98 <50 2' below pit bottom, SP 860419 4.43 8.11 4.43 <50 Unexcavated soil, NP 860420 7.81 6.83 1.66 93 Unexcavated soil below drain NP 860421 3.85 8.57 0.77 <50 Unexcavated soil, NP 860422 8.57 7.49 1.87 58 Unexcavated soil below drain NP 860423 7.72 7.42 1.96 <50 Unexcavated soil, NP 860424 6.87 7.20 3.16 <59A 2' below pit bottom, NP 860425 6.08 7.75 0.70 126A 2' below pit bottom, NPAc- 71 600i 860426 11.60 8.37 1.72 <50 Ledge, SP 860427 2.77 8.63 16.90 <50 Ledge, NP Pa 2 . Lai Average Background .49 32 Standard Deviation .25 12.5 Mean + 2 Standard Deviations .98 57 C ot.)ccavv. A = Average of duplicate analyses USt_Th B: NP = North Pit; SP = South Pit C(1.:51t1A. N.)k:;.1,..31- /-3 t\-s,carr,

10 o o Cr.: ND o TABLE 2 C!)

Precision and accuracy data for analyses.

PRECISION DATA ACCURACY DATA

% MEAN RELATIVE 95% % MEAN RELATIVE 95% RECOVERY ST.DEV.(%) CONFID. RECOVERY ST.DEV.(%) CONFID.

Hg 100.5 9.0 27.0 100 7.2 21.6 NO3-N 100.1 2.9 8.7 100 3.3 9.9

11 o o cn REFERENCES n.) o CI 1. Final Report, Chemical Storage and Zirconium Feed Tank Storage Areas, Idaho Chemical Processing Plant: University of Utah Research Institute, July, 1986.

2. Quality Assurance Sampling Plan, Chemical Storage and Zirconium Feed Tank Storage Areas, Idaho Chemical Processing Plant: University of Utah Research Institute, July, 1986.

3. Kabata-Pendias, A., and Pendias, H., 1984, Trace elements in soils and plants: CRC Press, Inc., Boca Raton, Florida, 315 p.

6 - bcc: A. J. Matule P. I. Nelson D. J. Poland IdahoWEL National Engineering Laboratory W. L. Random GP&CE Document Control (1.0) J. W. Ruffner

JWR-48-86

NoveMber 25, 1986

S. Silverman Project Engineer Departnent of Energy Idaho Operations Office 785 DOE Place Idaho Falls, Idaho 83402

noAr mr. Silverman:

Subject: Environmental Sampling for the Secondary Containment Vaults Project

Attached plaage find the chronology of events that you requested concerning the Secondary Containment Vaults Project Environmental Sampling. It is felt that the Sampling Plan that we have outlined is the hest possible to ensure a Sampling and Closure Plan which would be acceptable to the Environmental Protection Agency (EPA). This plan is based on WINCO's interpretation of the regulations and discussions with groups who have surressfully completed Sampling and Closure Plans for similar areas. Unless guidance is received from EPA as to what the minimum requirenents will be for the closure plan, we feel that we must continue to piupose a detailed sampling plan.

It has been proposed that the sampling be conducted concurrently with construction. Sampling concurrent with construction would be a very dangerous option for both the project schedule and budget. Unless the extent of amtamination is known, if any, the bid package cannot be adequately prepared to cover all excavation required for clPan-up. The time for sampling, analysis, and clean-up would be very difficult to bid and more than likely result in delay charges. This would dramatically impact both the project budget and schedule. Impacts on the project schedule could be quite garious becauPP of the limited window available for this construction area and the fact that it will not occur again within the next few years. There are also safety concerns for the construction personnel working with soil in which the condition is unknown. I feel it is very unwise to conduct all sampling concurrently with construction because we will open ourselves up to a great many problems.

Westinghouse Idaho Nuclear Company. Inc. Box 4000 Idaho Falls, ID 83403 Mr. S. Silverman Page 2 JWR-48-86 NoveMber 25, 1986

If you have any questions, please feel free to contact me at 6-4471.

Very truly yours,

J. W. Ruffner, Project Engineer GP&CE Projects

/big

Attachments CYY ACTIVITIES ON c P-621 EVALUATION TO DATE

08/13/86 Discussed characterization of CPP-621 Area with Montana Tech and University of Utah Researdh Institute (UURI).

08/18/86 Montana Tech called to discuss their capabilities for the characterization then indicated that they did not have the QA documentation or required sampling equipment.

08/22/86 Further discussions with UURI on sampling plan.

08/26/86 UURI visits CPP to inspect project area and requests underground line drawings.

08/28/86 Mailed out underground line drawings to UURI.

09/08/86 Meeting conducted with Wendell Random, Jeff Ruffner, George Buker, Tony Matule and Joan Poland to discuss Secondary Containment Project impacts and characterization.

09/08/86 Preliminary Scope of Work received from UURI who estimated that $138K would be required to complete a comprehensive characterization of the area.

09/09/86 M-K Boise Engineering visited CPP to discuss modeling of CPP-621 area and also grease pit S. of CPP-608 area. (Bob Secondo, DOE-ID, indicated that M-K in Boise had done some computer modeling and work at CPP which would be helpful in determining extent of migration of materials from spills nPar the CPP-621 area.) M-K could offer no information but rade a sales pitch for a contract to assist in studies or work in the area.

09/19/86 Meeting conducted with Ken Hein, Wendell Random, Jeff Ruffner, Tony Matule, George Buker and Joan Poland to discuss characterization cost and time to characterize area to be used for Secondary Containment Project. Conference call placed to Jerry Lyle DOE-ID to discuss the characterization. See attached for alternatives to the $138K sanpling plan as suggestPd by Jerry Lyle. DOE-ID indicated they would contact WINCO when they have decided on the option WINCO should use. DOE asked that we explore a fla1ed down sampling program which would give indications of the ragnitude of cleanup which would be required or be used to determine if more characterization would be required.

09/22/86 UURI was requested to submit a cost estimate for a scaled down sampling activity.

10/08/86 UURI sutmittPd a cost estimate of $18K for small scale sampling (grab samples). o o Page 2 - I CD 1\.) 10/86 Jerry Lyle (DOE) indicated WTNCO should take some grab samples for acid analysis since the soil may have had a neutralizing effect. Jerry recommended a review of the history of bulk Chemical receipts for indications of hazardous constituents in the Chemicals.

10/86 Bulk chemical specifications were reviewed on a preliminary baqis. Indications are that heavy metals are not present.

11/86 Samples which are available from a previous grab sample program are being analyzed. This will not give conclusive results for characterization but will give preliminary indication to plan future work. Until more information is available it is thought that the project excavation could proceed with concurrent sampling. This mode could place the project in jeopardy if the samples indicate hazardous materials which cannot be cleaned up concurrent with construction. Construction personnel concerns with excavating of hazardous materials or in low PH soil are possible and could cause project delays. this situation exists whernever any excavation is undertaken but is more likely at a known spill site. NI SECTION® 17.7!±:e SCALE 4e-rIt0-

. SECTION .CS)

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"74S7 7,O, Z Co\ec-cc)0,,_ or l0 o(\ F-4\kr\r(31ez ',,i'!/.N4aLCi‘m123(11.1x MATERIAL AND SERVICE =u J./‘ Page 01 ;TAM W PVC1 1,1 j) REQUISITION FOR , ,Prir.- ,. mr-P-IAr il . . .. '-' 1 AA tii*. '-:A. :A . :ir 191 ."' r;tr. 1.1)CATI0N MAME YE is- 13•BANCA OR •APANY OBIIVER TO _ ' ' 1 uN''''' NE,IS/R&ES - N/A _ ) r RHO DIRG OS EL OAR PATE NEEDED . . /7-O r , imc i. . . • 'IL...400 T530 , 6/30/86 '' 7h/86 • j',. 4.11ASER, r N-•. ••-i. zR BCCAOCIA PHONE PROPERTY ClIgOOLAN r 4 L. J t D.J. POland CDP-631 50 /A - ' (7 ---' .. ,'" ER B.GNATNRE ~is,ybA , ,.4,,c , ...„ , fidrillis - 7. • ,,f) RE Pt AO SAFETY PIP ENV 0 A LfVEL : OA.'BAN NO,. / REC PSI U)C4ION WINC0-5730 _ q . N/A N/A iEnEniDNO - gm------"Thi/A ,0 r4 23 PROBITY poo€ t ,, • 'lliBEIR3• TY 'EM usa INOIJNI (AO. MODEL ')Er! '''. - 03 --$ IIRRIP` O MMEE ? Pall _....___ PART NUMBER •' ,.. . Provide services to include: coordinating the collection - e.., 4:-. of a total of 50 soil samples (actual qollection I( ,i by others); QA services for all samplelhandling, , ,.,,. -B..14 analysis, and renorting activities inc)uding EPA -- .* • ,, chain-of -custody; handlina transnortatdon and refrigerat)on w 1 of samples from collection point to laratory r "21.0%,i:= per EPA reauirements; laboratory analylis of the „,,s-' ..^11,NT ,-a-17 ; , e ...,13, 50 samples for toluene, benzene, xylend, Ba, Cr, ,-.... A C r- As, Aq, Pb. Hg.. Se and Cd; and renortilia analysis . , , resuits. Services shall Spc]ude providing sample ,to Ls. - 404R1!• .., con---ers and pregarafion of cortaine4s .fro re9erve 7„:„,sw--;s . _ >ABS POR ESLMA:E NUR NO — A DiTML ATTACsED _ C Rt.B•SBEO PRICES 7 A AAs- otpcj•ANES a- 0 EXPER,ENCE&KWNLEDGE • N/A ..omSESTED SuPPLBPS CEBING PRICE EST University of Utah PRICE TORL .:iIa (Existing URI Contract University Outreach Program) s $16,500 ., . ,

RAC s fat , ... - ,..".... NEMO 0 .. SHP ym .._ a SHIP 113 CONES:14NC ID , 10 Y 0 mg..- ,j"” ,,---,,- coula 0.It '•.'n- , ,1_,...• is?.,...,:"-i , CPP-654 p .,,, ,. •-p,., ..:-. , • ,, - - - a oric, --- - -iv- rwitr a ADO D fit 4 - •- ....x., - - 1 '7.--i- _ ?p- r: . PACCJRE MEW CCOOPIG' "‘.4 0;,•:. "4 CZ e - --r. EMLMSY.4..'", MML DEGEREW - CWE ?KIMMEL' ,L --t• ElNEM uv.,,,,:r r..0- cue .... _mfrs. . /1C:7LCL ONP - ,...,115. SIZ , OM - RE/A. Irdi M!;'.-.7 "....-i., €471.44.- -F '1-"4.1... ,•41, Sr!, "- , .,471 7•Yt47tVat.r:C1 t i. 1 -' 11-711:- --..ti -.. „nr_st- g,---- ,-•,•;-c. tr ,_ - --, ARfillaEs --,--` 7., te .4,„ CONT GS-WS-. , --r k 4.3 .- .1.1-, Si•-••fi,t'- —) .4-"V- - •

HAVE1011 CHECKED:THE STORES CATALOG FOR THIS MATERIAL? CltE THE FORM,WINO0-6160

Requester Do Not Write in Shaded Areas A .te, ,s- e Idah0 omaanY. Inc- d.r . restatits 'lwsb (Rory. 3-64) REQUISITION FOR MATERIAL. AND SERVICES (Continuation Sheet) etarlaCiLtH 22. 28337

P(iODUCT SVC. CODE EST. PRICE 0() " • (U/117)

HAVE YOU CHECKED THE STORES CATALOG FOR THIS MATERIAL? USE THE FORM WINCO-6160 FOR STORES.

Requester Do Not Write in Shaded Areas

1 0110CLIPEMFMT c ldaho Narwhal Engtneenng Laboratory c

July 1, 1986

Mr. Richard H. Timpson, Director Research Administration The University of Utah 302 Park Building Salt Lake City, Utah 84112

TASK ORDER NO. 2 WITH UNIVERSITY OF UTAH RESEARCH INSTITUTE UNDER SUBCONTRACT NO. C85-110763 WITH THE UNIVERSITY OF UTAH FOR SOIL SAMPLING AND ANALYSIS - N1DL-102-86

Dear Mr. Timpson:

1. This Task Order No. 2, effective July 1, 1986 is issued in accordance with:

A. The terms of Subcontract C85-110763.

B. Research Institute Proposal dated June 30, 1986.

2. As a result of this Task Order No. 2, U of U Research Institute will provide support for a study on soil samples and analysis. The work to be provided shall be in accordance with Attachment A, Scope of Work.

3. EG&G Idaho Administration

A. Contractual responsibilities under this Task Order shall be administered by Ann Rydalch.

B. A11 work to be performed under this Task Order shall be under the technical jurisdiction and direction of J. Poland.

4. University of Utah Administration

A. University of Utah subcontractual responsibilities under this Task Order No. 2 shall be administered by Richard Timpson.

B. Technical Administration: All work to be performed under this Task Order shall be under the technical jurisdiction and direction of J. N. Moore.

n err: r:Idaho Inc P.O. Box 1625 Idaho Falls, ID 83415 ** Mr. Richard Timpson The University of Utah O July 1, 1986 C: MDL-102-86 Page 2

5. Subject to the terms and conditions of Subcontract No. C85-110763, The University of Utah shall use all reasonable efforts to complete the Scope of Work by August 1, 1986.

6. The total estimated cost and ceiling amount for this Task Order No. 2 is $16,736.00.

The amount currently obligated for performance of this Task Order is the maximum amount obligated and must not be exceeded without the prior approval of the Subcontract Administrator designated herein. If at any time the Subcontractor has reason to believe that the total cost to the Contractor will be greater than the obligated amount and/or ceiling amount shown on this Task Order, the Subcontractor shall notify the Contractor in writing to that effect, giving the revised estimate of such total cost for the performance of the Task Order.

7. The Patent Rights Article under this Task Order is deleted.

8. Monthly invoices for services provided under this Task Order must be accompanied by a certified statement of costs in the format set forth in Appendix B.

The original and two copies of this Task Order No. 2 are forwarded. Please execute the original and one copy and return them to EG&G Idaho, Inc. The remaining copy, executed by EG&G Idaho, Inc., may be retained for your records.

EG&G IDAHO, INC. THE UNIVERSITY OF UTAH

Ae:1-c"---Cr..,_-___cs By By M. D. Lovejoy Title Subcontract Soecialist Title

AVR:dkw cc: J. N. Moore W. Forsberg J. Poland, WINCO ATTACHMENT A C85-110763-002

SCOPE OF WORK

The Subcontractor shall provide services to include the following:

1. Coordinate the collection of a total of 50 soil samples (25 organic and 25 inorganic, actual collection by others).

2. QA services for all sample handling, analysis and reporting activities including EPA chain-of-custody.

3. Handling, transportation and refrigeration of samples from collection point to laboratory per EPA requirements.

4. Laboratory analysis of the 50 samples for toluene, benzene, xylene, Ba, Cr, As, Ag, Pb, Hg, Se and Cd and reporting analysis results.

Services shall include providing sample containers and preparation of containers to preserve samples. A11 analysis will be in accordance with EPA approved methods and guidelines and shall be finished and reported by August 1, 1986. c c /NEL/daho National Engineering Laboratory 1-+ — - — _ 1.; December 15, 1986

Mr. Richard H. Timpson, Director Research Administration The University of Utah 302 Park Building Salt Lake City, Utah 84112

MODIFICATION NO. 1 TO TASK ORDER NO. 2 FOR SOIL SAMPLING & ANALYSIS UNDER SUBCONTRACT NO. C85-110763 WITH THE UNVIERSITY OF UTAH RESEARCH INSTITUTE CDC-121-86

Dear Mr. Timpson:

1. This Modification No. 1 to Task Order No. 2, Subcontract No. C85-110763, effective August 1, 1986, is issued in accordance with the following:

A. The terms of Subcontract No. C85-110763.

B. UURI's additional proposal request dated September 4, 1986, and further verbally clarified December 9, 1986.

2. As a result of this Modification No. 1 to Task Order No. 2, Subcontract No. C85-110763 is modified as follows:

A. Paragraph 5, "Term of Performance" is changed to read:

The UURI shall use all reasonable efforts to complete the scope of work by December 31, 1986.

B. Paragraph 6 is changed to read:

The total estimated cost and ceiling amount for this Modification No. 1 is $21,082.00. With this additional $21,082.00, the cost and ceiling amount is increased from 516,736.00 to $37,818.00.

The amount currently obligated for performance of this Task Order is the maximum amount obligated and must not be exceeded without the prior approval of the Subcontract Administrator designated herein. If at any time the Subcontractor has reason to believe that the total cost to the Contractor will be greater than the obligated amount and/or ceiling amount shown on this Task Order, the Subcontractor shall notify the Contractor in writing to that effect, giving the revised estimate of such total cost for the performance of the Task Order.

n =neatIdano Inc P.O. Box 1625 Idaho Falls, ID 83415 ** CD CD Mr. Richard H. Timpson December 15, 1986 CDC-121-86 t‘: Page 2

C. Attachment A — Scope of Work is modified to include, but not be limited to, the following:

1. Collect and soil sample 67 soil samples and decontaminate the sampling equipment. Determine the vertical extent of contamination and background levels of toxic metals and organic compounds.

2. Organic and inorganic (heavy metal) analyses of background samples (4).

3. A complete organic scan of the "worst" case sample to determine the range of contaminants that could be present (1).

4. Determination of cyanide in the creosote—bearing sample.

5. Four additional organic analysis for benzene, xylene, and toluene.

6. Seven additional heavy (10 metal) analyses.

7. Ten additional lead analyses.

8. Additional sample preparation (preparation of four composite samples, determination of dry weight).

The results of the data will be statistically evaluated and described in a final report to WINCO by December 31, 1986.

3. Except only as changed by this Modification No. 1, all of the terms and conditions relating to Task Order No. 2 to Subcontract No. C85-110763 shall remain unchanged and continue in full force and effect.

4. Please sign and return two copies of this Modification No. 1. The third copy, which has been signed by EG&G Idaho, Inc. may be retained for your records.

EG&G IDAHO, INC. THE UNIVERSITY OF UTAH

By By C. D. Cutler, Manager Title R&D Subcontracts Title

AR:pjd

cc: W. L. Forsberg J. N. Moore D. J. Poland FORM NONG1-404(5131 REQUISITION FOR MATERIAL MID Splyi-CE: ogi(eor- T. ORDER TYPE 1ST INPUT BY ---,:- Din 2ND PS er , - PO NO - ... ., ,. .. ..,......

EIPANew PR COMPANY • DELIVER TO LOCATION E VE E - 4 C7 • V IIS/RiES N/A - «.:. . a 1 ,..... '0' - Tit, ITIFEO. OFG. CST EL WE DGE NEEDED 4.. T16110010 30 - 03.03-67, 03-16-67 r •••• ''' REQUESTER . LOCATION -PROPERN CUSTDOIAN : NUMBER • /Ili:. Grp D.J.Polend CPP-630 6-3650 N/A 4- Cia4..4, CD APPROVER SIGNATURE PROPERTY REVIEW r. i I' N 4 SUETY REVIEW ,..EPA. LEVEL OA PLAN NO,-, REG INSP LOCATION WINC0-5730 lawm N/A N/A ' lOuDIHONE - WA ' it/A V 0 KO Y 0 N O . i -i - I PRIOFUTY COOE PRODUOI SVC COOE .•ESr. PRICE REM' OTY UNIT (NOUN) (AEU.) MODEL I 0 2 0 3 0 _ 00 '( UNIT) UNIT PRICE MPG PRICE I PART NUMBER •• Provide services to include: collectiol anees and ...- coordinating Of a the collection total ,I it af 60 soil samples; 46 services for all,I sample handling, analysis, and reporting

activities including EPA chain-of- I custody; handling,transporiStion and ,1 refrigeration Of samples from collection point to laboratory per EPA requiromentn;

... laboratory analysis of 60 samples for I I ---1,11 20 samples for Bat Cr, As, Ag, PbI I END USE 7-- ..,.._ ..-- NOM ORDER NO. • ,„:10 A Call. COED ''"". C PLIOLISTTED PRICES t* ....., ._. ., ... -.1..t, . ID a pis puRomsEs 0 EXPERIENCE 8 KNOMEDGE WA .. SUGGESTEDSUPPLIERS universtty.of Utan. (Ex sting Oat Contract CEILING PRICE EST ISM. PRICE - 4AJOIG PRICE _.. University Outreach Progno) i ...... $24.2640 ..-- 111114 FOB PREPAID 0 SHIP WA SHP 10 CONFIRAIING TO -7 - Y El N 0 0 OEST couccr 0. - ❑ - 0 OM MEW & An0 n - - , _ - PMCUREMENT CODING FISCAL WI ORDERED DATE P D BUYER MUM MCC Me 01 COMP arR VEAR BUS nn .... — .,. ,. . .. _ , . —, 6:4,-2;,,Ft ac s I I I °re I . I I. I I '' 7* 4;. SOL Y 0 N0 . . - - '' WIRING 504.‘,.-4,C,•,L.,i"."..- ...... A.S.ItOr.1 RECEIPT NG ITEM MAMMY sJTEM OUANTTIY 7 2 3 NO. 4 DATE 'RECEIVED' *UNIT - NOt 'DATE RECEPIElie *I. WSW - RECIW 2.. 7- PPO. . .. COLLECT 7 ...... —WE ..- IN 4; ^ -, ... . .4, REJECT .!. . . T •••••••.* ....' '1r* PEONS SIJP 11 Waif CHARMS OWN& CLASS - ...... 7.,;k:7-

4. S. REOEIVINa & REQUESTER 1 *FIECEIVING',.; (pInk) IIEWESTER'S COPY "; DISTRIBUTION OF SUBCONTRACTS, PURCHASt OKDERS:7 AND MODIFICATIONS FOR WINCO

TITLE: AC-A:f JACIt /14.7 o:4-4

NO. .55"1.2 .1)I Ili- co 1 TO MCD CA: L____ ORIGINAL COPIES

Subcontractor ,/ //t Subcontract Administra or :4.A.A.„ j >c (,---Irequester C. i2,e_tk,/ (LP, 0 1 Quality Engineer 1

EG&G IDAHO G. R. Thomas - w/1097 1 M. S. Quigley - w/1097 X Accounts Payable 1 J. E. White (GFM) 1 R. E. Gray (S/C personnel at INEL) 1 X Receiving/Inspection w/1097 CF-6018 1 1099 eligible - other compensation form

WINCO E. L. Kopp (FAST Project Only) w/5730 1 P. E. Thornock (If FAST Project, cross off) w/5730 1 X Accounts Payable - N. M. Petersen 1 J. M. Cleveland 1

DOE-ID 1 Chicago Patent Office (if Patent Rights Article Applicable) 2 Other Department of Labor (over $10,000 - SF 99 - hardware)

Effective Date 0 ti S1 Del ivery Date [:)(.. Dollar Value $2_27,21/ Charge No. -r-76 // co/a Requisition No. b---a /3n/77:2 Vendor No. (22 di" --33 de3

Distributed: Date -5/ 7 By 771 , (Joe,- c c

INELldaho Nationai Engineering Laboratory 1).) CC

April 14, 1987

Mr. W. L. Forsberg, Director Administrative Services University of Utah Research Institute 391 Chipeta Way, Suite C Salt Lake City, UT 84108

TASK ORDER NO. 1 WITH UNIVERSITY OF UTAH RESEARCH INSTITUTE UNDER SUBCONTRACT NO. C87-101314 FOR SOIL SAMPLING AND ANALYSIS - CDC-56-87

Dear Mr. Forsberg:

1. This Task Order No. 1, effective April 6, 1987 is issued in accordance with:

A. The terms of Subcontract C87-101314

B. Research Institute Proposal dated March 31, 1987. .S ..Thsz Atte 2. As a result of this Task Order No. 1, U of U Researctxwill provide the Vriril" support for a study on soil samples and anaysis. The work to be provided shall be in accordance with Attachment A, Scope of Work.

3. EG&G Idaho Administration

A. Contractual responsibilities under this Task Order shall be administered by Ann Rydalch.

B. All work to be performed under this Task Order shall be under technical jurisdiction and direction of J. Poland. Pesedavt-4 -twat;trite 4. University of Utah4Administration Resecre-4 A. University of UtahAsubcontractual responsibilities under this Task Order No. 1 shall be administered by W. L. Forsberg.

B. Technical Administration: All work to be performed under this Task Order shall be under the technical jurisdiction and direction of J. N. Moore.

GJEGrG Wino. Inc. P.O. Box 1625 Idaho Falls, ID 83415 c Mr. W. L. Forsberg University of Utah April 14, 1987 CDC-56-87 N: Page 2

5. Subject to the ter47and iicsialitiws of Subcontract No. C87-101314, University of UtalisAll'use alT reasonable efforts to complete the entire Scope of Work by June 15, 1987.

6. The total estimated cost and ceiling amount for this Task Order No. 1 is $22,200.00.

The amount currently obligated for performance of this Task Order is the maximum amount obligated and must not be exceeded without the prior approval of the Subcontract Administrator designated herein. If at any time the Subcontractor has reason to believe that the total cost to the Contractor will be greater than the obligated amount and/or ceiling amount shown on this Task Order, the Subcontractor shall notify the Contractor in writing to that effect, giving the revised estimate of such total cost for the performance of the Task Order.

7. The Patent Rights Article under this Task Order is deleted.

8. Monthly invoices for services provided under this Task Order must be accompanied by a certified statement of costs in the format set forth in Appendix B.

9. The original and two copies of this Task Order No. 1 are forwarded. Please execute the original and one copy and return them to EG&G Idaha, Inc. The remaining copy, executed by EG&G Idaho, Inc., may be retained for your records.

EG&G IDAHO, INC. UNIVERSITY OF UTAH RESEARCH INSTITUTE

By

C. D. Cutler, Manager Title R&D SUBCONTRACTS Title President

AVR:pjd cc: J. N. Moore J. Poland, WINCO C87-101314 T. O. #1 Attachment A

SCOPE OF WORK

The Scope of Work shall include, but not be limited to, the following:

Provide services to include: collection and coordinating the collection of a total of 60 soil *samples; QA services for all sample handling, analysis, and reporting activities including EPA chain-of-custody; handling, transportation and refrigeration of samples from collection point to laboratory per EPA requirements; laboratory analysis of 60 samples for pH and nitrate, 20 samples for Ba, Cr, As, Ag, Pb, Hg, Se, Cd, aluminum and 4 samples for fluoride, 4 background samples for fluoride and nitrate, Ba. Cr, As, Ag, Pb, Hg, Se, Cd; and reporting analysis results. Also, laboratory analysis of 20 samples (collected by others) for pH, 7 samples for Ba, Cr, As, Ag, Pb, Hg, Se, Cd, and aluminum and nitrate. All sample preparation (water extraction). Services shall include providing sample containers and preparation of containers to preserve samples. All anlaysis will be in accordance with EPA approved methods.

*Will provide all necessary sampling protocol, grid plan and sample locations.

The results of the data will be described in a final report to WINCO by June 15, 1987. - , ------, 2:1=- rft- c:1".' -f---- se -- r- ----,.... -7 —__ t. ,-,- „ CD 0 I—• ./4/4 0 ci ' ' - , CD 1 `94; Cz k.. r• i ' -•,‘ hr.....: caor,;),1

EARTH SCIENCE LABORATORY UNNFRSTTY nF UTAH RESEARCH INSTITUTE 391 Chipeta Way, Suite C Salt Lake City. Utah 84108 (801) 524-3422

jod W I NIC (*..) TO ORG./LOCATION TELEPHONE NUMBER

C.0(,-, R. I 5; - q 9 FROM ORG./LOCATION TELEPHONE NUMBER

THIS TRANSHITTAL CONSISTS OF 4- PAGES. (excluding cover sheet)

VERIFICATION TELEPHONE NO. (801) 524-3437 EARTH SCIENCE LABORATORY

UNIVERSITY OF UTAH RESEARCH INSTITUTE 391 Chipeta Way, Suite C Salt Lake City, Utah 84108

March 31, 1987

UNIVERS/TY OF UTAH Office of Research Administration 304 Park Building Salt Lake City, Utah 84112

Title: INEL Samples Analyses - Task Order No. 2, Modification No. 2 to the University of Utah Subcontract No. C-85110763

Type of Request: Contract Modification

Amount Requested: $26,640

Joseph N. Moore James J. Brophy, President Principal Investigator University of Utah Research Institute SCOPE OF WORK

Provide services to include: collection and coordinating the collection of a total of 60 soil *samples; QA services for all sample handling, analysis, and reporting activities including EPA chain-of-custody; handling, transportation and refrigeration of samples from collection point to laboratory per EPA requirements; laboratory analysis of.60..ssmples.fos_OLond.nitrate, 20 samples for Ba, Cr, As, Aq, Pb, Hg, Se, Cd, aluminum and 4 samples for fluoride, 4 background samples for fluoride and nitrate, Ba, Cr,

As, Ag, Pb, Hg, Se, Cd; and reporting analysis results. Also, laboratory analysis of 20 samples (collected by others) for pH, 7 samples for Ba, Cr, As, Ag, Pb, Hg, Se, Cd, and aluminum and nitrate. A11 samples will be analyzed for percent moisture soil pH and sample preparation (water extraction). Services shall include providing sample containers ana preparation or uvatainere to preserve samples. A11 analysis will be in accordance with EPA approved methods. Services will also include the issuance of a formal final report.

*Will provide all necessary sampling protocol, grid plan and sample locations. o BUDGET Cr; Ca Amount

A. Salaries and Wages: $6,629

1. Salaries a. J. N. Moore 88 hours b. R. L. Kroneman 124 hours c. K. R. Yorgason 122 hours d. J. L. Johnston 84 hours

B. Employee Benefits:

1. 39.9% 2,645

C. Subcontract - EnviroSearch, Inc.:

1. David Nelson - 48 hours 2,640

D. Travel:

1. Per Diem and Lodging - 6 days $ 300 2. Car Rental - 6 days 300

Total 600

E. Supplies:

1. Safety Clothing $ 155 2. Chemicals and Misc. 400

Total 555

F. Total Direct Coats: $13,069

G. Indirect Costs:

1. 42.9% of F 5,607

H. G & A Costs:

1. 18.1% of F 2 365

I. Total Direct, Indirect 6 G&A Costs: $21,041 o CD

Ca J. Fee: 159 1. 5.5% of 1 1

$22,200 K. Total Project Price - UURI:

L. University of Utah Indirect Costs: 4 440 1. 20% of K

$26 640 M. Total Project Price: • E 4 4 1 1 .) now er-wed-619:(sae REQUISITION FORMATc'RIAL-AND SERVICE Page of P°"°. r n r, r : ORCER TYPE 1ST INPuT By DATE 2ND INPUT BY ; DATE VENDOR Ntl ..w, ---- .1 u s, '- •- f.. 417, , _ -... 4 , ID 'OMPANY DELIVER TO LOCATION ;RHONE VENDOR NAME --..,._ -.....-..,...... , 0 1,- iLISIRLES N/A , 144, .... hi u A CD CHARGE NO WO ORG CST EL. BATE DATEi NEEDED i ' }-41 ,I. T16110015 T530 1997 / m REQUESTER LOCATION PHONE PROPERTY CUSTODIAN NDLABER 1 , r . U.J.Poland CPP-630 6-3660 N/A .:7:------.44 IVA APPROVER SIGNATURE PROPETIRY-GEVIENI Y..,bir g it Lei ., .„ , / OcAo1Y beta/ , 1 SAFE Y REVIEW OA LEVEL ' (4111feyriceit2 REC INSP LOCATION wiNal 5730 ANCHMENTS N/A ,/, ,•-", N/A 1 E a E m D iv cij -. -whet 4 7N/A yoNt yt:i4Nci / 1 / PRIORITY CODE PRODUCT SVC CODE EST PRICE

ITEM COY UNIT (ROLM) IADJI MOOEL - 1E2E30 ______00 (UNIT) UNIT PRICE IDEAL PRICE

/1 ri V "4 PART NUMBER 2 Modify requisitionl#30596 to -Include additional sampling, analysts, and,

coordination of cleanup in the CPP-621

area. Specifically add the following. Provide services to include: collection

and coordinating the collecOon of4an

— additional 30 soil samples (contractor will provide all necessary sampling : protocol, grid plan and sample lecationl): QA services for all sample handling, I ENO USE ♦

BASIS FOR ESTIMATE c WORK OROER NO. - 4 E -A DETAIL ATTIGHED „ii C PUBLISHED MIS E. 0 EXPERIENCE & KNOWLECGE LI 8 PAST PURCHASES / sunGESTED SUPPLIERS ,. CEILING PRICE EST TOTAL PRICE ItiAL PRICE r ,i i .?. $ $4,000.00

TERMS ; F0E1 PREPAID 0 SHIP VIA. SHIP TO CONFIRMING TO PO YE NO 4 D CiESTI-. mulct 0 : 44 ;.- CFP-654 0❑ 0 ORIG PREPW & too 0 i Omer PROCUREMENT COOING FISCAL OXIE ORDERED 1.- DICE PROMISED BUYER axe . woos we Ex COmP arR YEAR -Bus TYPE i. --- .1 •--- IT ---.-'3717 '-r r7 -- r hel-rA— liwt T '1'. ' - -- '.. SBEA V 0❑ N 0❑ : . _ GSA CONT GS OCS EXPIRING

FIECEIPC NO • 1 2 ITEM OUANTITY REM OUANTITy NO DATF RECEIVED UNIT NO. DATE RECEIVED UNIT FREOIT RECEIPT

.1 PPO -

031.1ECT

0/1

BY

2 \ REACT'

METHOD PACKING SLIP FREIGHT CYIARGES EXPENSE CLASS II,

1 I d. S. RECEIVING 6. REOUESTER & RECEIVING 7. (pink) REOUESTERS COPY d• • to ,t.nrinouse !clam) Nucien Company. Inc. REQUISITION FOR MATERIAL AND SERVICES f• • orINC 7-6150A (Rev. 3-84) (INTER-OFFICE USE ONLY)

KO ORO CST EL DELIVER TO LOCATION PHONE if Ho ri IT 753r) 4i/A ifkr77aggitteffilifiA N CR CCMPANE DATE DATE NEEDED .% NCO/ oiFFF L9CATION PHONE PROPERTV CUSTODIAN NUMBER r, 71 0_,91) &it 1..-N.5-0 C--Y000O ',RRRrRx•lo: wrF SIGNA I URE

. Il RVNEW SA ETY REVIEW 0 A RELATED O.A. PLAN NO REC. INSP LOCATION WINC0-5730 000rEffiiik a:AK AnrnsreO:E Ai/ A 0 14/51( Al/74 A1/4 /-• /' 1.1 •- N 4 Aiwpow,,k °:<$1 UT? UNIT INOUPOIACU I MOOEUPT NO attPWOmtv:

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'ce I i` cc/ "'NJ

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o7,5OATE MJR NO. AT'ACHID C PUBLISHED PRICES Ft Rip.P,FS 0 EXPERIENCE & RAULEDGE • 't !..PPLIERS EST oft. TOTAL 2R a TOTAL PRICE

DATE PLACED DATE DUE Nodify Requisition # 30596 to include the addition of the following:

services to include: collection and coordinating the collection of EIL;Itional 70 soil samples (contractor will provide all necessary r„:1Ing protocol, grid plan and sample locations); OA services for all I e handling, analysis, and reporting activities including EPA ,fl-o-f-custody; handling, transportation and refrigeration of samples t collection point to laboratory per EPA requirements; laboratory isis of 70 samples for Hg; and reporting analysis results. Services c.l include providing sample containers and preparation of containers to -i-erve samples. si)A kample analysis will be in accordance with EPA !rods. Services 9VAPPIr also include guidance by UURI to WINCO on the :val of CPP-A'l contaminated soil. The guidance for t e removal of +rom the CPP-621 hree luminum nitrate French drains be based the UURI analysis resu ts. Services A.443 also include the issuance ot +Inal r ep or t 14H2 SAALF/ Ia., 02-7 1 / / E--cLreji,nad/2_ a-zeztto--ce-— fitodo /14

o DISTRIBUTION OF SUBCONTRACTS, PURCHASE ORDERS AND MODIFICATIONS FOR WINCO 1\7; TITLE: La_ 1c„,„A iaci_ Cl NO • C 75-2 Z. C. L L z cii oc

ORIGINAL COPIES

Subcontractor >1- Subcontract Administrator ,4z. 1 c4 Requester .112. 0P 1 Quality Engineer Al 4 1

EG&G IDAHO G. R. Thomas - w/1097 1 M. S. Quigley - w/1097 1 X Accounts Payable 1 J. E. White (GFM) 1 R. E. Gray (S/C personnel at INEL) 1 X Receiving/Inspection w/1097 CF-601B 1 1099 eligible - other compensation form

WINCO E. L. Kopp (FAST Project Oniy) w/5730 1 P. E. Thornock (If FAST Project, cross off) w/5730 1 X Accounts Payable - N. M. Petersen 1 J. M. Cleveland 1

DOE-ID 1 Chicago Patent Office (if Patent Rights Article Applicable) 2 Other Department of Labor (over $10,000 - SF 99 - hardware)

Effective Date6 g_-.7 Delivery Datec: -731 El -77 Dollar Value S 44=0 pc. Charge No. 7-74 / / 00/5— Requisition No. ira Caeri, 5.4// Vendor No. 0 2025-33 63

Distributed: o o

INESIdaho Narional Engweenng Lahr:yawn' June 29, 1987 CJ1

Mr. W. L. Forsberg, Director Administrative Services University of Utah Research Institute 391 Chipeta Way, Suite C Salt Lake City, UT 84108

MODIFICATION NO. 1 TO IASK ORDER NO. 1 UNDER SUBCONTRACT NO. C87-101314 WITH THE UNIVERSITY OF UTAH RESEARCH INSTITUTE FOR SOIL SAMPLINGAND ANALYSIS - AR-112-87

Dear Mr. Forsberg:

1. This Modification No. 1 to Task Order No. 1, effective June 11, 1987 is issued in accordance with the following:

A. The terms of Subcontract No. C87-101314.

B. Oral agreement between UURI, D. J. Poland of WINCO and EG&G Idaho's Ann Rydalch on June 11, 1987, relative to providing additional funds and extending the term of performance for continuation of work presently being performed.

2. As a result of this Modification No. 1 to Task Order No. 1, to Subcontract No. C87-101314 is modified as follows:

A. Paragraph 5, "Terms of Performance" is changed to read:

University of Utah Research Institute shall use all reasonable efforts to complete the scope of work by July 31, 1987.

B. Paragraph 6 is changed to read:

The total estimated cost and ceiling amount for this Modification No. 1, Task Order No. 1 is S4,000. With this additional $4,000, the total Task Order No. 1 cost and ceiling amount is increased from S22,200 to 526,200.

The amount currently obligated for performance of this Task Order is the maximum amount obligated and must not be exceeded without the prior approval of the Subcontract Administrator designated herein. If, at any time, the Subcontractor has reason to believe that the total cost to the Contractor will be greater than the obligated amount and/or ceiling amount shown on this Task Order, the Subcontractor shall notify the Contractor in writing to that effect, giving the revised estimate of such total cost for the performance of the Task Order.

P. O. Box 1625 Idaho Falls, ID 83415 C: O Cr; University of Utah June 29, 1987 CA AR-112-87 Page 2

Monthly, trimester, and a yearly progress report will be delivered to coincide with the INEL reporting schedule for the Bureau of Mines and is to be finished by April 30, 1987.

3. Except only as changed by this Modification No. 1, all of the..terms. and conditions relating to Task Order No. 1 to Subcontract No. C87-101314 shall remain unchanged and continue in full force and effect.

4. Please sign and return two copies of this Modification No. 1. The third copy, which has been signed by EG&G Idaho, Inc., may be retained for your records.

EG&G IDAHO, INC. UNIVERSITY OF UTAH RESEARCH INSTITUTE

BY / .(4441..ie 6 ANN RYDALCH JAMES /BROP TITLE SUBCONTRACT ADMINISTRATOR TITLE PRESIDENT

mi

cc: D. J. Poland, WINCO J. N. Moore, UURI FORM' erli-6198 (8-86) REQUISITION FOR MATERIA Page of __ )NO ORDER TYPE 1ST INPUT BY DATE 2ND INPUT BY DATE fVEND N0. --...... , G.'ii 7

LIAN 0 ------/ 7 DELIVER 10 LOCATION PHON VE OGFINAME c..) COMPANY - ., 1 1997 / , ijii.iii..At..... A/A C7 r Y -'.-----.. -...__, 1,-- CNARGE NO RED ORO CST EL. DATE DATE NEEDED 4. tie.r -----....J . ?Cr ,... ,- C) f J.. AO-30 -St li -09-87 . 4... ,.... '-'-',-..„... •.., 4..., > C.:: EECUESTER LOCATION PHONE PROPERTY CUSIOOIAN NUMBER ---...,...... __E ''''R . .. p,;:aod rii.v...1t, o-a-,Lt.,, N/A APPROVER SIGNATURE PROPERTY REVIEW

(faun REVIEW &Amy Rae/ 0 A LEVEL 0 A PLAN NO. REC. INSP LOCA ION WINCO-5730 ATTACHM NTS Ni A i 0 c 0 lc 0 ni a N/A rt/A Y 0 N RI Y 0 N El 1 i PRIORITY CODE PRODUCT SVC CODE EST PRICE (TEM OTY UNIT {NOUN) IA0.1.1 MODEL 1 f:1 2 El 3 CI _____ 00 (UNIT) UNIT PRICE TOTAL PAIGE

PART NUMBER ?rcv..; ;critco; ;(1 rat:ludo: coilectior

,...;ic :.4,,,intil'A ..; Cy .17:1 :.-C; I 1 'jr:t ii:1 oi IT

,i, .. ni ..:: ies ;,ampiine protocai, 1

...Trio , an 41%6 5ampit !ccatizals; nA I

lcrvicet i'.”. al .; iampie hanO;ing, 1

on.liysis ,-3nO reporting activities I irt]ilinl A chain-at-custody: handlirp, _

:rinspoe: jil 4.nt.: r*trit,ar.i‘iati oi I

samp,es from collection point Lotaboratcry per EPA reo.:

140orary asaiysis of IU somples tor 1 icontinued is ENO USE

GAGS FOR ESTIMATE WORK ORDER ND ;I. A DETAIL ATTACBIE0 2 C PUBLISHED PRICES J 8 PAST FIJRCHASES EI D EXPERIENCE & KNOWLEDGE SUGGESTED suppuss Liil I v..: n t Lje u; u it‘41) da 1 tit. ti i LI ...EL A L.,;g4tr 1. A. CEIUNG PRICE EST. TOEAL PRICE TOIAL PRICE +iersisy Outreuch Prot:yr% a $ 11,000

TERMS I Fil, PREPAID 0 SHIP VIA SHIP TO CONFIRMING TO PO V 0 N 0 COLLECT 0 CPN64 0 I 0{-- DESTORIG PREPAY 8. ADO 0 Other PROCUREMENT CCOING FISCAL DATE ORDERED DATE PROMISED BUYER CDS Paws moo cc cos ivPE SQE am YEAR BUS. lYPE

I , I ‘.1 I l I I I NSA . Y in N D GSA CONT GS-OCIS EXPIRING

ITEM OUANTITY ITEM OUANTITY RECEIPT NO 1 2 3 NO. DATE RECEIVED UNIT No. DATE RECEIVED UNIT FREIGHT RECEIPT

PPO

GOV'

OA

SY

Rua

MEUCCI POCKING SLIP FREIGHT CHARGES EXPENSE CLASS _ N

4. 5. RECEIVING 6. REOUESTER 6 RECEIVING 7. (pink) REQUESTER'S COPY EG&G (1/87)

DISTRIBUTION OF SUBCONTRACTS, PURCHASE ;ORDERS---- AND MODIFICATIONS FOR WINO O JALI 4 1991 O TITLE: 5-efr;" c7.1 NO. C / %Vie C"; Ti5

ORIGINAL COPIES Subcontractor Q Subcontract Administrator d"- A..A.- Requester Pt 9, ted., tfi3e, 1 Quality Engineer 1

EG&G IDAHO G. R. Thomas - w/1097 1 M. S. Quigley - w/1097 1 X Accounts Payable 1 J. E. White (GFM) 1 R. E. Gray (S/C personnel at INEL) 1 Receiving/Inspection w/1097 CF-601B 1 1099 eligible - other compensation form

WINCO E. L. Kopp (FAST Project Only) w/5730 1 P. E. Thornock (If FAST Project, cross off) w/5730 1 X Accounts Payable - N. M. Petersen 1 J. M. Cleveland 1 011111••••••

DOE-ID 1 Chicago Patent Office (if Patent Rights Article Applicable) 2 Other Department of Labor (over $10,000 - SF 99 - hardware)

Effective Date 11 0 %_:27 Delivery Date pi :F,7, Dollar Value $ /C Charge No. "t—/ L //e 41/JC-- Requisition No. 2.7.1rj- _52315.-.717 Vendor No.e);;c2.1:5-37:3 C1,3;

Distributed: Date ///k 5-F7 By Lt, c c

/dahoWEL National Engineering Laboratory

November 6, 1987

Mr. W. L. Forsberg, Director Administrative Services University of Utah Research Institute 391 Chipeta Way, Suite C Salt Lake City, UT 84108

TASK ORDER NO. 2 WITH UNIVERSITY OF UTAH RESEARCH INSTITUTE UNDER SUBCONTRACT NO. C87-101314 FOR SOIL SAMPLING AND ANALYSIS - AR-280-87.

1. This Task Order No. 2, effective November 6, 1987, is issued in accordance with:

A. The terms of Subcontract No. C87-101314

B. University of Utah Research Institute Proposal dated November 6, 1987.

2. As a result of this Task Order No. 2, U of U Research Institute will provide the service necessary in support for collection and coordinating of soil samples and analyzing. The work to be provided shall be in accordance with Attachment A, Scope of Work.

3. EG&G Idaho Administration:

A. Contractual responsibilities under this Task Order No. 2, shall be administered by Ann Rydalch.

B. A11 work to be performed under this Task Order No. 2 shall be under the technical jurisdiction and direction of J. Poland.

4. University of Utah Research Institute Administration:

A. University of Utah Research Institute subcontractual responsibilities under this Task Order No. 2 shall be administrated by W. L. Forsberg.

B. Technical Administration - A11 work to be performed under this Task Order No. 2 shall be under the technical jurisdiction and direction of J. N. Moore.

**EMSIdaho. Inc. P.O. Box 1625 ldaho Falls, ID 83415 o o

Mr. W. L. Forsberg November 6, 1987 AR-280-87 Page 2

5. Subject to the terms and conditions of Subcontract No. C87-101314, University of Utah Research Institute shall use all reasonable efforts to complete the Scope of Work by September 30, 1988.

6. The total estimated cost and ceiling amount for this Task Order No. 2 is $10,976.00.

The amount currently obligated for performance of this Task Order is the maximum amount obligated and must not be exceeded without the prior approval of the Subcontract Administrator designated herein. If at any time the Subcontractor has reason to believe that the total cost to the Contractor will be greater than the obligated amount and/or ceiling amount shown on this Task Order, the Subcontractor shall notify the Contractor in writing to that effect, giving the revised estimate of such total cost for the performance of the Task Order.

7. The Patent Rights Article is not applicable on this Task Order and has been deleted.

8. Monthly invoices for services provided under this Task Order may be accompanied by a certified statement of costs in the format set forth in Appendix B, but must accompany the final invoice.

The original and two copies of this Task Order No. 2 are forwarded. Please execute the original and one copy and return them to EG&G Idaho, Inc. The remaining copy, executed by EG&G Idaho, Inc. may be retained for your records.

EG&G IDAHO, INC. UNIVERSITY OF UTAH RESEARCH INSTITUTE

BY (Ln;Er4Zt BY

Ann Rydalch Treasurer TITLE Subcontract Administrator TITLE Wilford L. Forsberg tls cc: J. N. Moore J. Poland, WINCO A o Attachment o C87101314 Task Order 2

Scope of Work

The Scope of Work shall include, but not be limited to the following:

The Subcontractor shall collect and coordinate the collection of 10 soil samples; QA services for all sample handling, analysis and reporting activities including EPA chain-of custody. This shall also include handling, transportation and refrigeration of samples from collection point to laboratory per EPA requirements.

Laboratory analysis shall be conducted on 10 samples for ph, Ba, Cr, As, Ag, Pb, Hg, Se, Cd, F, and sample preparation (water extraction).

Services shall include providing sample containers and preparation of containers to preserve samples. All analysis will be in accordance with EPA approved methods.

The results of the data will be described in an interim report to WINCO by January 4, 1988. 6 444.7 The term of performance on this Task Order No. 2 is November 7, 1987 through 4it September 30, 1988 unless otherwise changed. RESEAPCB ACCOUNTING

UNIvERSITY 416 PARK BUILDING }--A SALT LAKE CITY uTAH 84112 OF UTAH I %lit_ 801-581.7346 c INVOICE °EC 5 so AGENCY ADDRESS it-AGENCY ID NUMBER S/C C85 110763 T/0 t2 ,GE & G Idaho, Inc. sac VOUCHER NO 1 !? a 1110 Box 1625 Gv n tinn-u 2 final Idaho Falls. Idaho 83415 UNIVERSITY ACCOUNT NC 5-25187 DATE December 11 1986

DESCRIPTION

INEL Samples Analysis

Requesting payment for the Period: August 1, 1986 In the amount of S10.305.91

rota] Due SI0,305.91

total Paid Not Including This Invoicot $ AUTHORFY I SIGNATURE DATE CONSTRUCTt:' OA Di CERT. OF ReASONA1LEN.S5 OF LIRL.Cf CHARGES EG&G IDAHO, INC. 71 ,7 / / TECHNICAL APPROVAL // EG&G IDAHO, INC. MITCOMMACTS SECTION APPI*VAL MR PAYMENT

certify io the nest ot my knowleage that all expenditures

repared a payments reaueSted cre fp apPrOrthate PurPoses

ana in canphance with the provisions Of the apaication ana

owara agreements

University of Utah

AOGO1 APPENDIX B EG & G IDAHO. INC. STATEMENT OF COSTS 1 U of U Account No.5-25187. VO No. 2

1. Name and Address of Subcontractor: Lniversity of Utiahliwbcontroc Accowfling 418 Park Building Salt Lake City, Utah 84112 C: C: 2. Subcontract Number S/C C85 110763 T/O c2 r•••••• •.• 3 Beginning and ending date of c.o.; pertinent subcontract period 7-01-86 to 8-01-86

4 Costs incurred during the pertinent subcontract period

List only those costs which are to be reimbursed by the contractor or proportionately shared by the parties:

Cost Cetegorifts: Amount

a. Salaries and Wages

Equipment (List separately the cost of each piece of equipment)

c. Travel (show amounts for both foreign and domestic. Ifnone. state none

Domestic

Foreign

Total Travel d. Other Dlrect Costs 8,588.59 e. Total Direct Expenditures 8,588.59 f. Indirect Charges 1.717.32 (Indicate percent and expenditures to which percent is applied.) 20% C: 5. Tota1 Costs for Items for pertinent per od 10.305.91c

6. Support cost for the pertinent period set forth in Article 3. chargeable to the CO contractor for the pertinent period.

7. Cumulative costs (Contractor costs under this statement plus costs for previous periods). 16,736.00

8. Cost Ceiling in Article 5 16,736.00

9. The difference between lines 7 and 8

10. Provide information regarding contributions by the subcontractor of items listed in Article 5.E during pertinent period. State the extend of Subcontractor's actual contribution, the measure of such contributions should be in the same terms as the subcontractor's commltment under Article 5.E: e.g., time, dollar, etc..

11. Actual outstanding commitments for goods or services at the end of the period covered by this statement.

1 dhill,_Manager 12-11-86 Name and Title f an Authorized Representative S ' V o C: “CON NUti.EMODA.110 COMPANY,Inc. Distribution. ternal Correwc.mdence CO D. L. Condotta crs. it/ B. R. Dickey J. Dugone Date: March 8, 1012%, K. L. Johnson 2:99, -WartSvs•Neciitxionl-- To: Distribution • G. F. Offutt From: P. W. Smith B. R. Wheeler 1/L- Committee Members File (2) Subject: HNO Spill/ Wlr-30-82 3 f

.uzCLIVED to-tb MAR 8 1982

yfir, W. S. NECHODOM /4"1:' L"J

As you know, the nitric acid storage tank at CPP-621 was overflowed March 6, 1982, doing possible damage to some construction concrete. The following people are hereby appointed to investigate this in- cident to determine why it happened and what can be dane to make sure it doesn't happen again:

Chairman R. J. Marchinko D. L. Olsen W. L. Antonson N. P. Willis

Please have your investigation completed by March 20, 1982.

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The following procedures need to be followed for the removal of the soil contaminated with Nitric Acid at CPP-621.

1. All contaminated soil will be placed into poly lined drums (available at CFA) for disposal. (30 gallon size recommended but not required.)

2. Areas where the acid pooled, allowing for the absorption of the acid into the ground, will require the removal of the majority of contaminated soil. This involves primarily the area along the concrete wall south of CS151 (the horizontal nitric acid tank).

a) The amount of soil to be removed will be dependent on the amount of absorption that took place. Contact Rochelle Honkus at 6-3206 or Bob Marcinko at 6-3590 for any questions.

b) The amount of soil to be removed from the area south of CS151 will need to extend to the base of the recently poured concrete retaining wall.

c) The area to the south east of CS151 along the north/south running trench presently under construction needs to be cleaned up initially. This will include the removal and disposal of the polyethlene sheeting, the wood forms and the surface layer of soil (approximately 1-2 inches of soil).

3. Following the clean up procedures, the area shall be thoroughly flushed with water. Contact with Rochelle Honkus or Bob Marcinko shall be made prior to the wash down procedure to ensure sufficient soil has been removed.

4. Personnel exposed to the contaminated soil (those removing it and filling the drums) shall wear as a minimum the following personnel protective equipment: acid boots, disposable acid clothing, acid gloves, full face respirators with combination cartridges.

5. All drums prior to being sealed will need to be checked for its acid concentration. This will be done with pH paper under the direction of Rochelle Honkus or Bob Marcinko. Drums that contain soil that is still acidic will need to have a layer of soda ash added to the surface.

6. Wood forms and any other materials that are suspect of acid contamination shall be disposed of in non compactable waste containers. Jot.% YZUla Oiev /1,01 IVIMIPI I CAIPAINIleC JUD rituuta I WUHK PALKAlat Orme! 1 ol 1 ShonTale 13. Priority 14. MJR Nb Excavate & Dispose of HNO3 Soaked Gravel Dirt

2 Date or Request 3 Date Required 4. Equipment ID No. 15. Job Type Area 5. GWA No. 0 OM 0 Scheduled 12301-230-251 3-09-82 03-23-82 0 Emergency O u nequested By Ext. 7. Work Package Contents (Attached) Mall No. Material List Yes No D. L. Olsen 1 3220 8. MJR is Limited to Ho 10 ize ALARA Yes No and S Materi Drawings Yes No

Req uester 11 M IR Requirements- 21. Planner 9 Job Location: n Sate Wolk Permit Required Identify Area, Bidg Room Goriogivalion Change 621 Area UA t 0 A ne ❑ C 0 HP Permit

12 pexnpuon ol WWk The acid spill near CS-151 vessel has seeped into the ground. The soil/gravel that has had at( acid on it must be excavated & placed in poly lined barrels for disposal at the Hazardous Material Disposal area. The biggest accumulation of liquid occurred at the corner of the con- crete dike due south of CS-151. The soil in this area must be excavated down to the footings. The soil in the surrounding areas must be excavated as deep as the acid seeped. Safety will monitor the soil removal so that non acidic dirt is not removed, but all of the acid contaminat ion is removed. The poly lined barrels are available at CFA warehouse. The 30 gallon drum si, ,is cataloged as 17 H. Procurement spec is Es50421. The gasket spec is Es504422. The 55 gent drum size is cataloged as 17 C. Procurement spec is ES 50365. The gasket spec is ES50656. Please excavate dirt and dispose of as outlined. Contact Bob Marciltko at 3590 or Dave Olsen at lext 6-3220 if additional information is required. Disposal to be in accordance with appropiatt pr-cedures and regulations as specified by Safety.

;)

i tE. Workers and *Exposure: 18. Ready to 19. Latest Malt Schedule Date Delivery Date 1 1 1 . •Hot Jobs I L1L. Craft 20. Reviews Technical Ii Est. Hours Actual Hours Foreman OA & S&S HE I Signature 22 Job Completed as Marked: (Foreman Check One). 23. Job Completed OA 0 Per Work Package With No Changes Engineering Per Drawings & DCN's (attached) Requester Approval

Responsible Foreman Date Requester (or Shift Ropy or Alternate) , - Date " W „

1-1 ',a • - /0 CRITERIA O ,9, ‘,,DESTGN CO / FOR SECONDARY CONTAINMENT VAULTS

PREPARED FOR THE U.S. DEPARTMENT OF ENERGY IDAHO OPERATIONS OFFICE IDAHO FALLS, IDAHO

Prepared by:

DATE//ds ---

APPROVALS:

ZYV1Ail °t11146;6 DATE /III )f• PROJECTS DEPT. DA TE /OA/kr ENGI2ING FDP Startup DEPT. awAl. DATE A)/2--V135 c46011C(<1

T- DATE ÍCi /534,5 TECHN AL af-

DATE //6 3-01-

DATE /044S

DATE /2- a 3 -5/5--

DATE /21/4 -54:4-

DATE //

k5 4.4--itrrfavfn.6 5 CP-7;_7 - o MI5 —C PP - 77 —53 5(0 o 53 Co 5 7 S I 52-

- 7 f 3 - I Oci

1.0 INTRODUCTION

2.0 FUNCTIONAL REQUIREMENTS 1

3.0 GENERAL DESIGN REQUIREMENTS 2

3.1 Operational Requirements 2 3.2 Maintenance Requirements 6 3.3 Design Life Requirements 6 3.4 Structural Requirements 6 3.5 Safety Requirements 6 3.6 Quality Assurance Requirements 7 3.7 Codes and Standards 9

4.0 COMPONENT DESIGN REQUIREMENTS 10

4.1 Containment Vaults 10 4.2 Materials of Construction 11 4.3 Alarm 11 4.4 Electrical Power 12 4.5 Ladder 12 4.6 Nuts and Bolts 12 C: o

1. INTRODUCTION 00

There are several acid storage tanks (VES-CS-151 & 100, nitric acid; VES-CS-164, sulfuric acid; VES-CS-167, hydrochloric acid; VES-CS-169, hydrofluoric acid; VES-CS-101,102, & 152, aluminum nitrate; VES-CS-EAST and WEST, ) located at ICPP. Currently there are inadequate and unacceptable provisions for the collection and holding of the contents of these tanks should they rupture or leak.

Consequently, these storage tanks do not meet the environmental impact requirements for hazardous chemical storage as mandated in 40 CFR 260 - 264:6iVironmental Protection Agency.

This project will build seParate acid containment vaults for ./47C /..4..SCT -/Je hydrofluoric, sulfuric, and hydrokloric acid. The project will build a common vault for the three aluminum nitrate tanks, a common vault for to903-the two pilot plant feed tanks, and a common containment vault for the -- -- two nitric acid tanks. The vaults will be used to contain liquids that may escape from the primary tanks.

2. FUNCTIONAL REOUIREMENTS

The proposed acid secondary containment vaults will contain leaks or spills from the primary tank and prevent the acid from escaping to the ground and contaminating it.

The containment vaults shall be designed to hold 110 % of the liquid volume of a storage tank; however, whenever one vault contains more than one tank, the vault shall be designed to contain 100 % of the liquid volume of the largest tank and 10 % of any other tank contained by the enclosure.

1 o 3. GENERAL DESIGN REQUIREMENTS o 3.1 Operational Requirements GO

The new containment vaults shall provide sufficient and safe storage of acids leaking from the primary tanks. They shall meet the following operational requirements.

3.1.1 aluminum nitrate, VES-CS-101,102, and 152. These three tanks will have one common vault. The vault shall contain 100% of the largest tank (CS-101) plus 10% of the volume of one of the remaining two tanks. The engineered concrete containment vault shall be 54 feet by 15 feet by 3.1 feet inside dimension (ID), and shall safely contain 18,663 gallons of liquid.

3.1.1.1 These tanks are presently situated on a compacted sand base. The concrete vault shall replace the compacted sand base as the foundation for all three aluminum nitrate tanks. The A-E shall determine the most economical way of accomplishing this.

3.1.1.2 The drain lines of each vessel shall be modified will drain into the containment CpLf f/c/i°5 : such that they vault.

3.1.1.3 The process supply lines of each vessel shall be modified such that they will not breach the containment vault wall.

2 o CD 3.1.2 nitric acid, VES-CS-151, VES-CS-100. The engineered concrete containment vault shall be 65.5 feet by 22 feet CD by 3.75 feet ID. The southeast corner of the containment CO vault shall be configured such that it will extend beyond the perimeter of the vessel and conform to the configuration of the pump house. A small passage way between the containment vault and pump house shall be provided if possible. The finished vault shall safely contain a minimum of 36,200 gallons of liquid.

3.1.2.1 VES-CS-100 is a 34,000 gallon stainless steel tank situated on a compacted sand foundation. The concrete containment vault shall provide the new foundation for the vessel. The A-E shall determine the most economical method for accomplishing this.

3.1.2.2 The drain lines of each vessel shall be modified such that they will drain into the containment vault.

3.1.2.3 The process supply lines of each vessel shall be modified such that they will not breach the containment vault wall.

3.1.3 sulfuric acid, VES-CS-164. At present a concrete berm exists around three sides of the storage tank. This existing berm shall be used as part of the containment vault. A fourth side and a concrete slab shall be added to complete the containment vault. The engineered concrete containment shall be 18.6 feet by 14 feet by 3.1 feet ID to hold 6039 gallons of liquid. The primary tank support occupies 1474 gallons. Consequently, the completed containment vault will safely hold 4565 gallons of liquid. 3.1.3.1 The concrete support for this tank is only under the outer perimeter of the tank. To prevent any acid from contacting the soil, concrete and liner material will need to be placed in the void space.

3.1.4 hydrochloric acid, VES-CS-167. At present a concrete berm exists around three sides of the storage tank. The addition of a fourth side for the sulfuric acid vault will be the fourth side for this vault. The existing berm shall be used as part of the containment vault. A concrete slab shall be added to complete the containment vault. The engineered concrete containment shall be 18.6 feet by 14 feet by 2.5 feet ID to hold 4870 gallons of liquid. The primary tank support occupies 1190 gallons. The finished containment will safely hold 3680 gallons of liquid.

3.1.4.1 The concrete support for this tank is only under the outer perimeter of the tank. To prevent any acid from contacting the soil, concrete and liner material will need to be placed in the void space.

3.1.5 hydrofluoric acid, VES-CS-169. At present a concrete containment pit is located underneath the hydrofluoric acid tank. A concrete slab shall be placed in the bottom of the pit to form the containment vault. This concrete containment vault shall be 27 feet by 16 feet by 8.75 feet ID, having a capacity of 28,278 gallons.

3.1.5.1 The drain lines currently emptying liquids into this vault will remain. o )-- 3.1.5.2 A permanently mounted ladder from the top of the -.1 o containment vault to a distance of 2 feet from CO the bottom of the vault shall be provided.

3.1.6 Pilot Plant Feed Tanks, VES-CS-EAST and WEST. These two tanks are used to conta feed stoc solution for the research facilities. They -ach con ain 1000 gallons. The vault shall be 12 feet by 12 feet by 1.5 feet and hold 1616 gallons of liquid.

3.1.6.1 The drain lines of each vessel shall be modified such that they will drain into the containment vault.

3.1.6.2 The process supply lines of each vessel shall be modified such that they will not breach the containment vault wall.

3.1.7 General.

3.1.7.1 The containment vaults shall be lined with an acid resistant material to prevent corrosion of the concrete. The coating shall cover the bottom and extend approximately 6 inches up the inside walls.

3.1.7.2 The floor of each vault shall have a slope of 1.5 inches in 12 feet towards the low point. o o 3.1.7.3 Each containment vault shall be equipped with an audio-type alarm. The annunciators for the O CO aluminum nitrate, hydrochloric, sulfuric, nitric and hydrofluoric acid shall be located in the FAST (bldg 666) control room. The pilot plant feed tank alarm annunciator shall be located in the 637 Low Bay.

3.1.7.4 A11 features of the design shall incorporate maximum personnel safety during operation.

3.2 Maintenance Requirements The acid containment vauits and associated equipment shall be designed for ease of maintenance to minimize operating cost and equipment downtime. Equipment shall be chosen on the basis of what is presently in use at ICPP to minimize the requirement for spare parts and craft training.

3.3 Design Life Requirements The acid containment structure shall have a minimum design life of 20 years.

3.4 Structural Requirements The acid containment vaults shall be designed to meet the requirements for seismic zone III in the latest (1982) edition of the Uniform Building Code (UBC).

3.5 Safety Requirements

3.5.1 Construction. Safety requirements during construction are controlled by the Morrison-Knudsen Company Inc., Construction Safety Management Plan.

6 o CD 3.5.2 Operation - 1 CD 3.5.2.1 A safety shower and an eyewash station are Co located adjacent to the present structure.

3.5.2.2 Removable hand rails shall be installed on the berms.

3.5.2.3 A ladder shall be installed in the hydrofluoric acid containment vault for entry and exit. The ladder shall extend from the top of the containment vault to approximately two feet from the bottom of the containment vault.

3.6 Quality Assurance Requirements

3.6.1. Level This project is classified as "Quality Level III " as defined in WINCO QMP 3-1.

3.6.2. A-E Responsibility

3.6.2.1 The A-E shall prepare and implement procedures to control activities affecting quality during design as stipulated in WINCO QMP 3-1.

3.6.2.2 The project shall be designed and constructed to meet the requirements of the INEL Quality Manual for construction.

7 o o 3.6.2.3 The design documents (e.g., drawings and specifications) shall include appropriate C Cc inspection requirements and acceptance criteria in sufficient detail so that the quality of construction can be verified.

3.6.2.4 A vendor data schedule indicating the required data submittals, submitted dates, and approved authority shall be prepared and submitted to the WINCO Project Manager for review and approval during Title II design.

3.6.3 Inspection and Testing Requirements

3.6.3.1 A systems operating test shall be performed to verify that the level alarms and annunciators function properly. The test shall be included in the project specification and shall be performed by the subcontractor. WINCO Quality Assurance shall witness the test.

3.6.3.2 The foliowing tests shall be performed on the concrete:

1. Slump test in accordance with ASTM C143

2. Air Content test in accordance with ASTM C173

3. Compressive strength test in accordance with ASTM C39

4. Concrete temperature test. 5. Concrete uniformity test for adequacy of mixing equipment in accordance with ASTM C94 0 CO

3.7 Codes and Standards.

3.7.1 General. Design, construction, testing, and operation of the acid containment vault shall be accomplished in compliance with current INEL Architectural Engineering Standards and other DOE, WINCO, federal, state, and local regulations, standards, and codes, as well as approved WINCO Standard Operating Procedures. Where regulations conflict, their order of priority shall be as listed in the preceding sentence. Specific regulations and standards which are directly applicable are referenced below. The latest editions or issues shall be used.

3.7.2 Department of Energy. The following documents are referenced for their applicability to the design of the facility and shall be utilized.

(1) Order 6430.1, "General Design Criteria Manual."

(2) DOE-ID, Order 5480.1A, Chap. I, "Environmental Protection, Safety, and Health Protection Standards."

(3) DOE-ID, ID-12044, Operational Safety Design Criteria Manual.

(4) DOE-ID, INEL Architectural Engineering Standards, Rev.5.

3.7.3 WINCO, ICPP Supplement to DOE-ID Architect-Engineering Standards for the Idaho National Engineering Laboratory. o o —1 3.7.4 Federal CD Cc

(1) 29 CFR Part 1926, Occupational Safety and Health Administration Standards.

(2) 29 CFR 1910, Industry Standards.

(3) 40 CFR 260, 261, 262, and 264 Environmental Protection Agency.

3.7.5 National. The following national cohsensus codes and standards will be utilized in the design where applicable:

(1) ANCR-1218, Human Factors in Design.

(2) Uniform Building Code.

(3) National Electrical Code, ANSI-C 1.

(4) National Electrical Manufactures Association (NEMA) Standards.

(5) American Construction Institute, (ACI).

(6) American Society for Testing Materials, (ASTM).

10 o o 1-4 4.0 COMPONENT DESIGN REQUIREMENTS -1 C: CO

4.1 Containment Vaults. The secondary containment vaults shall be made of 3000 pounds per square inch compressive strength concrete and designed to have a slope of 1.5 inches in 12 feet to the lowest design point. They shall have a minimum capacity of 110 % of each individual separate tank; however, when more than one tank occupies a vault, the design shall be 100 % of the largest tank and 10 % of the volume of any other tanks.

4.2 Materials of Construction. The following materials of construction have been determined to be compatible with the different acids (nitric, hydrochloric, aluminum nitrate, sulfuric, hydrofluoric and pilot plant feed) and shall be used.

4.2.1 Liner: The liner material for the containment vaults shall be:

1. hydrochloric acid, Swindress Bond concete liner.

2. hydrofluoric acid, Ceilcote 6650B reinforced polyester.

3. sulfuric acid, Swindress Bond concrete liner.

4. nitric acid, Swindress Bond concrete liner.

5. aluminum nitrate, Swindress Bond concrete liner.

6. pilot plant feed, Ceiicote 66508 reinforced polyester.

11 4.3 Alarm. The containment vaults for aluminum nitrate, hydrochloric, sulfuric, nitric and hydrofluoric acid shall be equipped with an audio-type alarm and an annunciator. The alarm shall be local for each containment vault and the annunciator shall be located in the FAST (bldg 666) control room. The containment vault for the pilot plant feed tanks shall be equipped with an audio-type alarm and an annunciator. The alarm shall be local to the containment vault and the annunciator shall be located in CPP-637 Low Bay.

4.4 Electrical Power. Electrical power needs will be established by the A-E. Possible sources are CPP-621 or FAST Acid Storage Pump Building, MCC-CS-407. All electrical equipment shall be rated for outdoor service.

4.5 Ladder. The ladder shall be made of carbon steel.

4.6 Nuts and Bolts The nuts and bolts shall be made of carbon steel.

12 I00 Final Report

HYDROFLUORIC ACID STORAGE TANK AREA IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, NC.

Earth Science Laboratory

Unlversity or Utah Research Institute 391 Chipeta Way.Suite C Salt Lake City, Utah 84108 (801)324-3422

Dece,Irnber, 1987 \co FINAL REPORT

HYDROFLUORIC ACID STORAGE TANK AREA

IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

TABLE OF CONTENTS

1.0 Introduction 1

2.0 Site Description 1

3.0 Site Geology 2

4.0 Sample Procedures 2

5.0 Analytical Procedures and Results 3

5.1 Analytical Results 3

6.0 Data Quality 4

7.0 Evaluation of Results 5 LIST OF FIGURES

Figure 1 Map of the CPP complex showing the location

of the project area 7

Figure 2 Map of the Chemical Storage Area 8

Figure 3 Sample locations at the Hydrofluoric Acid

Storage Tank Area 9

LIST OF TABLES:

T.able 1 Metal, fluoride, pH, and moisture contents

of samples 10

Table 2 Precision and accuracy data of analytic 11

Table 3 Analyses of field duplicate samples 12

Table 4 Background concentrations determined from

samples taken in the vicinity of the CPP

complex 13

Table 5 Ranges of concentrations in volcanic

soils 14

LIST OF APPENDICES

Appendix 1 Chain of Custody form

Appendix 2 Quality control data

ii 1.0 INTRODUCTION

This report presents the results of a preliminary character- ization of potential soil contamination at the Hydrofluoric Acid

Storage Tank Area (CPP-727) at the Idaho Chemical Processing

Plant (CPP) complex (Figs. 1 and 2). The plant, managed by the

Westinghouse Idaho Nuclear Company, Inc. (WINCO), is located approximately 50 miles west of Idaho Falls, Idaho. The project was undertaken to identify the nature and levels of hazardous constituents that may be present in the soils at this storage facility. The characterization is based on chemical analyses of soil samples collected by personnel and associates of the

University of Utah Research Institute (UURI) on November 16,

1987.

2.0 SITE DESCRIPTION

The Hydrofluoric Acid Storage Tank Area is a concrete lined

excavation approximately 16 feet by 28 feet by 12 feet deep

located at the southern end of the Chemical Storage Area (Fig.

2). The floor of the excavation contains two concrete footings

that are each approximately 7 feet 10 inches wide by 10 feet

long. The remaining portions of the base of the excavation are

covered with gravel-rich soil. Prior to sampling, the excavation

was filled with limestone to neutralize any acid that may have

spilled during the operation of this facility. A drain located

on the north wall presently discharges steam condensate into the

excavation. The drain is enclosed within a metal cage that

1 extends to within several inches of the base of the excavation.

The soil beneath the drain has collapsed into a small pit

approximately 1 foot across.

No detailed site history documenting the extent of chemical

discharges to the ground at the Hydrofluoric Acid Storage Tank

aaArea is available. However previous sampling indicated that

the fluoride contents of the soils at this storage facility were

above background levels (refer to UURI Final Report: Chemical

Storage and Zirconium Feed Tank Storage Areas, Idaho Chemical

Processing Plant: Sept. 1987).

3.0 SITE GEOLOGY

The sampling sites are underlain by sand, gravel and clay-

rich sediments which unconformably overlie basalt. The sediments

in nearby excavations on the CPP site are approximately 40 feet

thick. The thickness of the basalt has not been established. A

three foot thick clay horizon above the basalt was previously

sampled in one of the excavations and mineralogically analyzed at

UURI. X-ray diffraction analysis of this sample indicates that

it consists of approximately 25% quartz, 10', plagioclase, 5%

potassium feldspar, 15% smectite, 5% illite, 1% chlorite, 1%

kaolinite, and 36% glass.

4.0 SAMPLING PROCEDURE

The soil sampling techniques and procedures employed during

the project are described in the accompanying Quality Assurance

2 o o cn

Sampling Plan. The locations of the soil samples collected from iC

the Hydrofluoric Acid Storage Tank Area are shown in Figure 3.

5.0 ANALYTICAL PROCEDURES AND RESULTS

The samples collected during this study were analyzed for

soil pH, fluoride (F; water extractable) and heavy metals (total

metal analysis) which may have been discharged to the soils or

leached by the acids. These metals include arsenic (As), barium

(Ba), chromium (Cr), lead (Pb), mercury (fig), selenium (Se), and

silver (Ag). Soil moisture was also determined in order to

relate the analytic concentrations, determined on the basis of

dry weight, to in-situ weight concentrations.

5.1 Analytical Results

Analysis of the soils was performed by the University of

Utah Research Institute (UURI) located in Research Park at 391

Chipeta Way, Suite A, Salt Lake City, Utah. This laboratory is

certified in the State of Utah by the State Health Laboratory,

Bureau of Laboratory Improvement for the recuired metal analyses.

Utah is a "Primacy" state in which EPA RCRA programs are managed

at the state level by authorized state agencies. The Chain of

Custody (COC) form for samples submitted to this laboratory are

contained in Appendix 1.

The analytical results are presented in Table 1. Note that

values for moisture are expressed as percentage levels (%), Hg

and Se are expressed in parts per billion (ppb ), and the

3 o o CD ka remaining elements are given in parts per million (ppm). A11 analyses are reported on a weight per dry weight basis. The EPA- approved methods utilized for these analyses are described in the accompanying Quality Assurance Sampling Plan.

6.0 DATA QUALITY

The precision and accuracy of the analyses were determined from a statistical evaluation of field and laboratory quality control samples. Precision data were obtained from duplicate analyses of field and laboratory quality control samples.

Accuracy data were obtained from analyses of standard reference materials, spiked field samples, and laboratory standard samples.

EPA has nominally established control limits for precision and accuracy as plus or minus three standard deviations about the mean. Analytical data produced while quality control data

remains within this limitation meet the EPA-recommended 95%

Confidence Limit for data acceptability. Quality assurance data for project analyses are contained in Appendix 2 and summarized

in Table 2. These data indicate that the analyses of project samples fall within acceptable quality assurance limits.

Soil samples are heterogeneous and thus present inherent

analytical problems. Often very small particles of a particular

contaminant are not uniformly present throughout the sample

causing anomalies in the data which must be verified through

additional analyses. The UURI Earth Sciences Laboratory

4 performed multiple analyses and a thorough quality assurance evaluation in order to validate the precision and accuracy of its reported data.

Two of the field samples were collected in duplicate to assess the heterogeneity of the soils. Chemical analyses of the field duplicates are presented in Table 3. The duplicate samples were composited in a stainless steel bucket and split into two plastic containers at the time of collection.

7.0 EVALUATION OF RESULTS

The results of the sample analyses have been statistically compared to the concentrations found in previously collected background samples (Tables 4) to determine the distribution of anomalous values. Concentrations exceeding a value equal to the background mean + 2 standard deviations are underlined in Table

1. For comparison the range of metal contents typically found in soils over volcanic rocks is shown in Table 5.

The data show that all of the soil samples collected from the Hydrofluoric Acid Storage Tank Area are characterized by anomalous F contents. In addition, anomalous concentrations of

As, Ba, Cr, Pb, and Se occur in the soils sampled below the drain. The elevated concentrations of these metals are

consistent with the low pH of sample 8. Elevated concentrations

of As (samples 1,3,4, and 5), Ba (samples 3 and 5), Cr (samples

1, 3, 4, and 5), Pb (samples 1, 4, and 5) and Hg (sample 2) in

other samples in contrast, do not appear systematic and are

5 within the range of values typical of soils overlying volcanic

terrains.

6 SAMPLING AREA

F IGURE - 1 Sludge Pit

CPP 621 Trench Trench

Nitric Chemical Chemical

Chemical Trench/

CPP-727

Condensate Dry Well ietp

CPP 607

SCALE o 10 20 Ft

Map of the Chemical Storage Area FIGURE 2 Drain I I I I I 8 3• 2 6

Si

4

"----"--<-----Concrete Wall

1 2 4 • Feet N • Sample Locations

Figure 3 - Hydrofluoric Acid Tank Storage Area (CPP727) TABLE!

Chetical analyses of soils troll the Hydrofluoric Acid Storage Tank Area.

61TE i DEPTH MOISTIME pH Hg As Se Ea Cr Pb Cd Ag (inches) l%) (pp() (ppb) (ppm) (ppb) (pp) (ppm) (pips) (ppm) (pa)

1 0-6 4.58 8.53 191.0 40 9.0 125 230 41 30 <4 2

1 24 3.51 9.30 62.0 54 4.0 125 ' 110 14 <8 <4 2

2 0-6 4.19 9.73 34.6 21 8.0 267 190 27 <8 <4 2

2 24 4.11 8.08 30.4 93 6.0 142 190 28 <6 <4 2

3 0-6 5.03 8.55 24.8 25 9.0 142 250 37 9 <4 2

3 10-15 5.55 7.09 55.7 <20 10.0 330 44 <8 (4 2

4 4-6 4.29 8.03 35.4 41 8.8 198 44 19 <4 2

4 18-21 3.06 7.51 23.2 22 6.0 t93 172 28 <8 (4 2 m 5 4-6 6.47 7.00 29.2 <20 8.8 195 390 43 22 <4 L

5 18-24 2.88 6.60 45.0 <20 10.0 280 400 28 <8 <4 <1.6

6 4-6 4.09 6.59 42.2 <20 5.3 160 253 31 <8 <4 <1.8

.1 a 19 4.37 6.58 33.9 35 6.0 408 22'7 <8 <4 2

8 0-6 24.91 4.24 74.4 <20 40.0 2909 693 100 821 <4 2 cn o

(LI TABLE 2

Precision and accuracy data for analyses.

PRECISION DATA ACCURACY DATA

95% 95% Confid Confid % Mean RSD Limit % Mean RSD Limit

As 100 38.6 11.6 99.8 3.78 11.4

Ba 100 9.48 28.4 98.0 3.34 10.0

Cd 100 0.71 2.13 10.0.7 3.82 11.5

Cr 100 8.52 25.6 100.9 3.57 10.7

F 100 2.10 6.30 100.9 4.40 13.2

Pb 100 4.55 13.7 99.0 4.34 13.0

Hg 100 6.53 19.6 100.E 8.60 25.8

Se 100 7.80 23.4 100.9 10.5 31.5

Ag 100 4.77 14.3 98.0 4.87 14.6 TAKE 3

Tank Area. Chemical analyses of duplicate soil samples from the Hydrofluoric Acid Storage

Cd Ag SITE 11 DEPTH MOISTURE pH F Hg As Se 8a Cr Pb (ppm) (inches) (s) (ppml (pphl (ppm) (ppbl (ppm) (ppm) (ppm) (ppm)

8 <4 <1.6 6 4-6 4.89 6.69 42.2 <20 4.6 146 290 35

<8 <4 2 6 Duplicate 5.09 6.48 42.0 <20 6.0 174 : 210 25

835 4 2 8 0-6 23.22 4.06 74.6 <20 40.0 3250 840 t10

89 761 0 2 8 Duplicate 26.60 4.4( 74.6 <20 40.0 2565 555 TABLE 4 9ackground concentrations of NO3, F, Al, Sa, Cr, Pb, Cd, Ag, Zr, Hg, As, and Se in soils sappled at locations outside of the CPP complex.

NO3 F Al Ra Cr Ph Cd Ag Zr Hg As Se SAMPLE (%) (pin) (%) (ppm) (ppm) (ppm) (ppal (ppal (ppa) (ppb) (ppa) (ppb)

Skg 1' 200 25 12 <5 <2 43 5.6 484

Ekg 2' 270 32 16

8kg 3' 270 33 17 <5 (2 27 6.5 467

Bkg 4' 250 34 12 (5 <2 28 7.0 341

860258 0.86 0.15 1.21 280 28 <10 <5 <2 <5 25 5.6 113

880253 0.72 0.32 0.81 380 25 <10 <5 (2 10 57 7.6 252

860260 0.41 3.12 1.60 240 28 <10 CS (2 9 23 6.4 695

1261 0.43 0.42 0.79 220 16 <10 <5 <2 12 30 6.2 236

<160284 0.27 4.00 1.60 230 28 <10 <5 <2 7 21 6.0 102

860265 0.25 0.28 0.75 210 20 <10 <5 (2 10 46 7.6 227

Average (X1 0.49 0.88 1.14 255 27 12 (5 (2 9 32 6.4 332

5l.Dev.(5.0.1 0.25 1.53 0.41 51 5 3 2 13 0.8 184

X • 2f(5.3.) 0.98 3.94 1.96 358 38 17 14 57 8.0 701

7 TABLE 5

Ranges of average concentrations in ppm of Cr, Ni, As, Ag, Cd, Pb, and Ba and in ppb of Hg and Se in soil overlying volcanic terrains.

ELEMENT RANGE MEAN

Cr 20-700 85

Ni 7-150 30

As 2.1-11.0 5.9

Se 10d-500 200

Ag 0.01-8.0

Cd 0.1-0.5

Hg 10-180 50

Pb 10-70 20

Ba 500-1500 770

Data on Cr, Ni, As, Se, Ag, Hg, Pb, Ba from wedepohl, K. H., ed., Handbook of Geochemistry, Springer-Verlag, New York, N. Y.

Data on Cd from Kabata-Pendias, A., and Pendias, H., 1984, Trace elements in soils and plants: CRC Press, Inc., Boca Raton, Florida, 315 p. cn cJ hti

c LT)

ARSENIC FFECISION

DATE TYPE MEAS. 1 MEAS.2 RECZ1 REC%2

1 22-Ju1-E6 REF 9 ry 100.0 100.0 _ 2E-Ju1-66 REF 6 6.2 38.4 101.6 23-Ju1-66 REF 7.2 100.0 100.0 4 79-Ju1-26 REP 7 100.0 100.0 c 7 7• -, Oth-Jun-87 REP 7.7 101.5 98.=. 6 06-Jun-87 REP 7.7 7.1 101.6 96.4 06-Jun-S7 REF 7.1 36.4 101.6, , 0 06-Jun-R7 REF .‘., .‘./ 100.0 100.0 24-Jun-87 REP 1 1 100.0 100.0 10 24-Jun-E7 REF 7.8 a 98.7 101.7,

n MEAN LCL UCL 100.0 1.1 R.5.7 107.7

atIOV14TT,1 o o

c." 1,-)

ARSENIC PRECISION

DATE TYPE MEAS. 1 MEAS.2 REC%1 RECY.2

1 78-Tu1-5,6 REP 5 9 100.0 100.0 .,,_ 28-Jul-SS REP 6 6.2 98.4 101.6 7 Z3-Jul-86 REP 7.2 7.2 100.0 100.0 4 22-Ju1-26 REP 7 J 100.0 100.0 r... 06-Jun-87 REP 7.7 7.7 101.5 a 06-Jun-07 REP 3.7 7.1 101.6 98.4 7 06-Jun-87 REP 3.1 Z. 98.4 , 3 06-Jun-87 REF 100.0 100.0 9 24-Jun-87 REP 1 1 100.0 11::0 10 24-Jun-37 REP 7.8 3 58.7 101.3

n MEAN = LCL UCL 100.0 1.1 cA.7 107.7

APPENDIX 2 MtECOVglri' — 11 104 102 107 109 100 101 1138 103 105 108 r 05 ea ea 114 82 ea 90 B3 81 0 1.1 1 — -1 — — — —I — — — — —

LCAE P. C0 , ▪ 14 T APSE A.PPENDI 111C Sjad 5 PREPS* LE 2 i r▪ PREP. a CGMTPC-i. s 10 PiRCCOVLPI

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110

115

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100

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9 Aq ACCURACY

DATE TYPE MEAS. TRUE REC%

1 T8-Jul-86 ST 0.0 =.0.0 100.0 ":. 20-Jul-86 ST 50.0 cn n 100.0 7 28-Jul-86 ST 51.0 50,0 102.0 28-JU1-86 ST 50,0 =I2 0 100.0 ' 09-Dec-86 SP 2 ^ 2.1 101.4 ..,.. 09-Dec-86 ST 2.1 . ".0 107.0 7 29-Apr-87 ST 2.0 ce 0 100.0 8 06-Jun-87 ST 99.0 100.0 99.0 9 06-Jun-87 ST 101.0 100.0 101.0 10 06-Jun-87 SP 94.0 100.0 94.0 11 06-Jun-87 9P 99.0 100.0 89.0 .",.. 24-Jun-87 ST 99.0 100.0 99.0 17 24-Jun-87 SP 94.0 100.0 94.0 14 24-Jun-87 9T 101.0 100.0 101.0 If, 24-Jun-87 :.-.r- qt..° 100.0 91.0 16 24-Jun-87 ST 59.0 100.0 99.0 17 24-Jun-87 SP R7,,0 100. cc n 18 24-Nov-87 ST 79.0 40.0 97.5 1C 24-Nov-87 ST 40.0 40.0 100.0 ^0 24-Nov-87 SP 42.0 42.0 100.0

n MEAN LCL UCL 20.0 97.8 4.7 847.6 112.0

APPENDIX 2 SbeCCOVE V;

130

115

110

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05

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80

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DATE TYPE MEAS. 1 MEAS.2 REC%1 REr7.2

1 24-Jun-S7 REP 101 99 101.0 99.0 ^ 24-Jun-87 REF' 99 .17Q 100.0 100.0 ,. 24-Jun-87 REP 101 92 101.0 99.0 4 24-Nov-67 REP 1.5 114.3 65.7 -, e-J 24-Nov-27 REF' - - 100.0 100.0 6 ERR ERR ERR ERR ERR ERR a ERR ERR 10 EF:R ERR

n MEAN LOL IJOL 20.0 ERR PPR PPR ERR MICCOVLITI 110 120 115 105 05 ea 00 95 90 LOWEP 1 I il l 7 COW 3 TP.0 _ 4 _ e 7 i i I i i SELENIUM i I e t I I I I I i 1 1 I I ta SAUPLE AGMS/it( 11111W1 1 a 11 12 i I i 13 t., 3. 14 UPPER 15 18 COWTPCit i ll r 17 1 I i 1 1 i ll I I i 18 i t 1 r 1 1 18 l i I i I i t i t 20 i i iV 00 " t:) I _ c•-

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DATE TYPE MEAS. 1 REC%1 = 1 10-Aug-S6 REP 290 :05 102.5 10-Aug-86 REP 400 450 94.1 105.9 ,.... 10-Aug-86 REP 724 400 89.5 110.5 4 10-Aug-S6 REP 715 471 85.6 114.4 =-,=.- c.., 10-Aug-SO REP 472 89.7 110.7 6 10-Aug-S6 REP 446 488 95.5 104.3 7 10-Au9-36 REP 741 77T 104.5 8 74-Nov-S7 'REP 2770 :r50 92.0 108.0 9 24-Nov-87 REP 197 207 96.5 103.5 10 24-Nov-87 REP 146 174 91.7: 10S.8

n MEAN s L7L LICL 20.0 100.0 8.4 74.9 125.1

APPENOIX 2 A(1GCOVLNf O 05 80 85 GO Ltuier- -

1 CI 2 CO W 5 T PCLL 4 5 E 7 LEP CURT g SAIRI

ACC le CAA LI 11 PA Or 12 11 14. 15 1 3

ER 18 CC447 17 151 18 20 OOÐE)2

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APPENDIX 2 Pb ACCURACY

DATE TYPE MEAS. TRUE PEC%

1 2S-Ju1-G6 ST 49 ,-.0 98.0 - ZS-Ju1-86 ST 45 50 90.0 3 23-jul-S6 ST =7 50 106.0 4 28-Ju1-E6 ST 49 50 92.0 .., 28-Jul-8S SP 51 47.5 107.4 -o- -- 6 28-Ju l-S6 r 74 107.0 7 28-Jul-S6 ,,r 44 47., 102.3 8 28-Jul-86 -SP 40 41 37.6 9 10-Au9-26 SF 76 40 90.0 10 10-Au9-66 ET 49.6 50 99.2 ,-, 11 09-Dec-86 .a 07 96.6 ,-, 12 09-Dec-86 ST 2.1 ... 10Ft. 0 13 11-Dec-S6 E= mg 234.5 97.2 14 11-Dec-86 196 -'00 99.0 15 11-Dec-S6 oo 196 207 9s.7 16 11-Dec-86 ST TOO '700 100.0 ., 17 29-Apr-87 CT .... 100.0 18 24-Jun-97 ST 99 100 99.0 19 -74-Jun-87 94 100 94.0 ,-- '70 24-Jun-S7 o p 100 100 100.0

MEAN LCL UCL 20.0 9S.S 4.6 85.0 112.6

Pb ACCURACY

DATE TYPE MEAS. TRUE REC%

1 24-Jun-87 SP 95 100 rC 0 24-Jun-87 ST 100 100 100.0

APPENDIX 2 %PCCOVCIr( — 110 100 105 115 110 05 00 95 90 WEAN 1 -1 -.I --1 ,_-- cowrPcm_ Ci1041014 MMOV‘11-11",, SJSIPLE 5 PPE1:1110W a PPE!? COW Tpoi 9 la o

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cAnmaim PRECISION

nATE TYPE MEAS.1 MEAS.2 RECZ1 REC%2

1 24-Jun-87 REP 101 99 101.0 93.0 _ 24-Jun-E7 REP 100 93 100.5 99.5 -. 24-Jun-S7 REP 100 100 100.0 100.0 4 24-Nov-87 REP 0 0 ERR ERR 5 24-Nov-87 REP 0 " 0 100.0 100. 0 ERR 6 ERR ERR 7 ERR B ERR ERR 0 ERR ERR ERR 10 ERR

n MEAN LCL UCL 20.0 ERR ERR ERR ERR

APPENDIX 2 OiPECOVEV.-.'

115

120 100

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10

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Ba ACCURACY

DATE TYPE MEAS. TRUE REC%

1 06-Jun-87 SP 0.04 0.04 100.0 2 24-Jun-87 ST 0.02 0.03 96.0 3 24-Jun-87 SP 0.05 0.05 99.0 4 24-Jun-87 ST 0.03 0.03 100.0 5 24-Jun-87 SP 0.04 0.05 96.7 6 24-Jun-87 ST 0.03 0.Q3 100.0 7 24-Jun-87 SP 0.02 0,03 96.0 8 24-Nov-87 ST 400.0 400.0 100.0 9 24-Nov-87 ST 400.0 400.0 100.0 10 24-Nov-87 SP 590.0 590.0 100.0 11 24-Nov-87 SP 955.0 940.0 101.6 12 ERR 13 ERR 14 ERR 15 ERR 16 ERR 17 ERR 18 ERR 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

APPENDIX 2 c

C

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115 —

110

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SAW LE YEAI L43)*EP COI:TPOL UPPEP CC44TPC4-

APPENDIX 2 BARIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%L REC%2

1 24-Jun-87 REP 0.021 0.02 102.4 97.6 2 24-Nov-87 REP 180 190 97.3 102.7 3 24-Nov-87 REP 5S0 560 99.1 100.9 4 ERR ERR 5 ERR ERR 6 ERR ERR 7 ERR ERR 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

APPENDIX 2 12a J.PSE WIC ACCU PACT

115 -

110

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Lim 100 r

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APPENDIX 2 o o h Pl C.. o Pl 'CI 0 0 ff) 1). 1/1 ill 0

0 re) N.. (..4, o 0) V) r. in r• o- .0 ui o o o o o C o o o- v-4 v-4 •-• 1-1 w Cr Cr. In Ul h N CA Ui U7 11 ID r I CA nCl W C.9 I) 4'") -0 C I CI C.1 CA V) ', 65 ei5

0000000 Kt w w o 0 (9 ci Cr. -0 I9 CO C.1 r) to ci (.4 tt U7 r, rJJ Ell C.1 (.1 CJ C.I r•-• •-•

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-0 -0 -0 -I) -o -0 -0 -CI V- h r- N r-- I-- V- C CD CO 03 CO 0) CO Ql W CO (A CO CO 0) ID CO 0) CO CO CO O) 1111111111111111 1111 • w -4 -1 4-4 4-4 •-• *-1 U U C C C C C> > > e) 1- :1 in 70.11D0_77777170.0 Is 47 4-)4-1 1-0 41 1-)0041 4-0 1-.1 4-1,4 4-)ZZZ IIIIIIIIIIIIIIIIIIII 01WCO CO 03 CO 0) co cr-, -40 40 tt eV et Ct mt CA CI CA CA CA CA r4 CA CA C? C9 C.1 C9 C9 CA CI CI rA (A

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LEAD. PRECISION 110 102 108 ,,---M.

aa l as 1 0.0. 103 102 101 100 9111

PMECOVEIr; g3 (17 g8 g5 Em. 03 92 91 80 2 3 5 10

SAW P - LI 1J4.14 LOKI! CONTROL FF1EP CON'POL.

APPENDIX 2 LEAD PRECISION

DATE TYPE MEAS.1 MEAS.2 FEr7.1 RECZ2

28-Jul-86 REP 17 IS 97.1 102.9 1 - , 28-Ju1-86 REP 3'7 98.5 101.5 , 28-Jul-86 REP 11 13 91.7 108.3 4 10-Aus-86 REP 16 19 91.4 108.4 100.6 .Jc 11-Dec-86 REP 267 270 =-, 0 101.4 6 11-Dec-86 REP : 54.3 98.6 101.0 7 11-Dec-86 REF' 19A )700 99.0 ERR 8 24-Nov-87 REP 0 0 ERR ERR 9 24-Nov-87 REP 0 ERR ERR 10 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

APPENDIX 2 SWPECOVIFF;

102 110

lac 114 lia 108 104 112

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APPENDI x 2 Quality Assurance Sampling Plan for tlze HYDROFLUORIC ACID STORAGE TANK AREA IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

Earth Science Laboratory

University of Utah Research Institute 391 Chlpeta Way.Suite C Salt Lake Clty, Utah 84108 (801)5243422

December, 1987 QUALITY ASSURANCE SAMPLING PLAN

FOR THE

HYDROFLUORIC ACID STORAGE TANK AREA

IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

TABLE Or CONTENTS

1.0 Introduction 1

2.0 Objectives and Scope 1

3.0 Project Organization 1

4.0 Site Description 2

5.0 Sampling Rational 2

6.0 Sampling Procedures 3

6.1 Soil Sampling 3

6.2 Sampling Equipment Decontaminition 4

6.3 Sample Containers 5

6.4 Sample Container Labels and Seals 5

6.5 Sample Handling and Transport 5

6.6 Field Quality Assurance/Quality Control

Procedures 6

6.7 Field Log Book 6

7.0 Sample Custody 7

8.0 Analytical Procedures 7

9.0 Laboratory Quality Assurance/Quality

Control Procedures 8 10.0 Data Review and Validation 8

11.0 Corrective Action 9

11.1 Laboratory Corrective Action 9

11.2 Project Corrective Action 10

12.0 Preventive Maintenance 10

13.0 Reporting 10

ii LIST OF FIGURES

Figure 1 Map of CPP Facility

Figure 2 Map of Chemical Storage Area

Figure 3 Map of Hydrofluoric Acid Storage Tank Area

Figure 4 Project Organization

Figure 5 Chain-of-Custody Form

LIST OF APPENDICES

Appendix 1 Analytical Methods

1.1 Method 3050: Acid digestion of sludges

1.2 EPA 200.7 (ICP)

1.3 SW-846 7060 (Arsenic)

1.4 SW-846 7471 (mercury)

1.5 SW-846 7741 (Selenium)

1.6 Method 340.2 (Fluoride)

iii CD o ff17.

C)

1.0 INTRODUCTION

This plan contains the quality assurance guidelines for sampling, analysis, and data reporting activities for the preliminary characterization of soil contamination at the

Hydrofluoric Acid Storage Tank Area (CPP-727; Figs. 1-3) of the

Westinghouse Idaho Nuclear Company, Inc. (WINCO).

2.0 OBJECTIVES AND SCOPE OF THE PROJECT

This soil sampling and analysis project will be conducted by personnel of the University of Utah Research Institute (UURI) to characterize the upper two feet of soils beneath the Hydrofluoric

Acid Storage Tank Area (CPP-727). This project plan is designed to identify the nature and quantity of hazardous constituents that may be present in the soils as a result of past operations.

3.0 PROJECT ORGANIZATION AND RESPONSIBILITY

The project organization is shown in Figure 4. The

Principal-In-Charge will have overall responsibility for:

1. direction of the project;

2. communication with local, state, and federal regulatory

agencies and;

3. data and project reporting.

The Project Manager will be responsible for:

1. the preparation of project plans;

2. execution of all activities in accordance with project

plans and;

1 3. communica_lon with the Principal-In-Charge.

The Project Quality Assurance Officers will _e responsible for:

1. preparation of the Quality Assurance/Quality Control

for Plan

2. evaluation of sampling procedures,

3. coordination of all laboratc y analytical procedures,

4. assessment of the validity, precision, and accuracy of

all analytical data, including quality control samples

and,

5. recommendations for corrective action or further data

collection.

4.0 SITE DESCRIPTION

The Hydrofluoric Acid Storage Tank Area is a concrete lined excavation approximately 16 feet by 28 feet by 12 feet deep. The

base of the excavation contains two concrete footings that are each approximately 7 feet 10 inches wide by 10 feet long.

Otherwise, the base of the excavation is unlined. The excavation

was filled with limestone to neutralize any acid that may have

spilled during operation of the facility. A drain located on the

north wall discharges steam condensate to the base of the pit.

5.0 SAMPLING RATIONALE

Surface sampling (0-4 inches) will be conc__:ted to

positively identify areas potentially impacted by the past

2 CD CD Cn CD handling practices associated with the chemicals stored in this area.

Subsurface soil samples will be collected 24 inches below each surface sampling site to assess the potential extent of downward migration.

A11 pertinent data, observations, and unusual conditions will be recorded in the field log book (see Section 6.7). A11 rationale for on-site decisions and implementation of action deviating from this sampling plan will be documented.

Additional'samples will be collected from any soils located in the sampling area that visually appear to be contaminated as indicated by dark stains, discoloration, odors, etc.

6.0 SAMPLING PROCEDURES

6.1 Soil Sampling

Throughout the sampling area, soil sampling will be

conducted at sites having the highest potential to exhibit

contamination. The proposed sampling locations are shown on

Figure 3.

A11 soil samples will be collected utilizing stainless steel

hand tools which have been decontaminated in accordance with

EPA-recommended procedures prior to the collection of each

sample. Augering to reach the subsurface soil sampling depth of

24 inches will be accomplished using a stainless steel hand

auger. If the hand auger is also to be used for sample

3 collection, it will again be decontaminatc:. prior c_ sample collection. The soil will be placed in a decontaminated stainless steel bucket until sufficient material has been collected from each sampling horizon. The soil will then be gently mIxed with a stainless steel spoon to homogenize the sample before being placed in an appropriate sampling container.

The sample container will then be properly labeled and prepared for transportation to the laboratory.

6.2 Sampling Equipment Decontamination

An area will be established at the site for the decontamination of a11 sampling equipment and protective clothing that may come in contact with hazardous ccnstituents. The decontamination area will be equipped with the necessary reagents, non-leaking containers, brushes and other appropriate equipment. Decontamination will involve (in order):

1. scrubbing with culinary water,

2. culinary water rinse,

3. acid rinse,

4. distilled water rinse,

Hand tools employed for sampling will be decontaminated

between each use and after sampling.

Protective clothing will be decontaminated, if required and

possible, or iisposed of along with the residues, solutions and

materials resulting from decontamination operations.

4 6.3 Sample Containers

Soil samples for inorganic analysis will be placed in

chemically clean, one pint, wide-mouth, plastic containers. A11

sample containers will be prepared by the laboratory for sampling

in accordance with EPA-approved protocols for the analytical

methods listed in Attachment 1.

6.4 Sample Container Labels and Seals

A11 sample containers will be sealed at the time of

collection with a non-tearable seal which bears the sampler's

name, date, and sample number. The seal shall be placed over the

lid and threaded ring to ensure that the sample has not been

tampered with prior to delivery to the laboratory.

A11 sample containers shall be labeled at the time of

collection with indelible ink pens. Sample labels will contain

the following information:

-Site number or project code

-Sample description

-Date of collection

-Time of collection

-Sample number

-Sample collector(s)

-Requested analyses

6.5 Sample Handling and Transport

5 After sealing and labeling, sample containers will immediately be placed in a cooler, and cooled to four degrees

Centigrade. The samples will be kept out of direct sunlight.

The cooler shall be suitable for vehicular transportation to the laboratory.

6.6 Field Quality Assurance/Quality Control Procedures

A blank sample will be taken in the field and handled along with the field samples and analyzed to assess cross contamination due to sample Ilindling practices.

A duplicate field sample will be collected and analyzed for each set of 20 or fewer samples to assess sampling, sample handling, and laboratory analytical performance.

6.7 Field Log Book

A field log book with bound, consecutively numbered pages, will be maintained by project personnel uncle:. Chain-of-Custody procedures. The information, logged on a daily basis, will include:

-Date and time of entry

-Purpose of sampling

-Name and address of field contacts

-Type of waste, if known or suspec:ed

-Description of sample(s)

-Number and size of sample(s) taken

6 :0 CD

-Description of sampling point(s)

-Collector(s) name(s) and signature(s)

-References such as maps, etc.

-Field observations, including unusual conditions

-weather conditions

-Any field measurements

- Equipment maintenance performed

- Decontamination procedures

- Record of attending personnel, including visitors.

7.0 SAMPLE CUSTODY

To establish the documentation necessary to trace sample possession from the time of collection through completion of analysis, the Chain-of-Custody form (Fig. 5) will be filled out.

It will accompany the samples to the laboratory and be signed and dated by the laboratory agent accepting delivery of the samples.

Prior to sample transfer, all samples will be inspected for damage or tampering. The Chain-of-Custody form will be retained with the samples until the analyses have been completed. The form will then be returned to the sampler with a copy of the analytical results.

8.0 ANALYTICAL PROCEDURES

A11 analytical work will be performed by UURI. This facility is located in the University of Utah Research Park, Salt

Lake City, Utah and is EPA-certified to perform the required

7 analyses through the Utah State Health Laboratory, Bureau c

Laboratory Improvement. A11 analyses will be performed uti__zing

EPA-approved methods.

9.0 LABORATORY QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES

Laboratory QA/QC procedures will be those outlined in the

written quality assurance plan this laboratory has on file with

the Utah St a Health Labo - ory, Bur au of Laboratory

Improvement. Copies of these plans may be obtained from the laboratory or bY writing to:

Bureau of Laboratory Improvement

State Health Laboratory

44 Medical Drive, Salt Lake City, Utah 84113.

This plan conforms with the requirements contained in "Rules

for t. a Certification of Environmental Laboratories," Utah,

January 3, 1986. This regulation outlines the minimum EPA and

state quality assurance activities necessary for environmental

laboratory certification.

10.0 DATA REVIEW AND VALIDATION

The results of the -ample analyses and the field and

laboratory quality contr _ checks will be reviewed and validated

by a Project Quality Assurance Officer. Laboratory control

checks will include duplicate analyses, matrix spikes, and the

8 c c

analysis of standards and standard reference materials as required by the EPA approved methodologies and the laboratory quality assurance plans.

Data from field and laboratory duplicates will be used to assess precision. The mean and relative standard deviation will be calculated and compared with EPA-recommended criteria to evaluate data acceptability.

Data from the analysis of standards, standard reference materials and matrix spikes will be used to evaluate data accuracy. The Mean and relative standard deviation will be calculated and compared with EPA-recommended criteria to evaluate acceptability.

A Project Quality Assurance Officer will prepare a written report on the analytical data for the Project Manager. The report will review the validity, quality, and completeness of the data and if necessary, make recommendations for corrective action, further sampling or additional analytical data.

11.0 CORRECTIVE ACTION

11.1 Laboratory Corrective Action

Laboratory corrective action taken to ensure data quality is

outlined in the written laboratory quality assurance plans on

file with the Utah State Health Laboratory, Bureau of Laboratory

Improvement.

9 11.2 Project Corrective Action

Corrective action will be initiated when the project objectives, as outlined in Section 2.0 are not met or when assessment of data quality reveals data of questionable or unknown quality.

Corrective action may be initiated by any individual on the project subject to approval by the Principal-In-Charge. These corrective actions .1 include, but are not limitea to, modifications of th_ ampling procedure or additional sampling, modifications o'f analytical techniques within EPA-approved guidelines, and modification of data reporting procedures.

12.0 PREVENTIVE MAINTENANCE

A11 equipment used in the field for this project will be

maintained in accordance with the manufacturer's recommendations.

Cleaning and necessary maintenance will be accomplished prior to

and after sam_ling. A11 maintenance will be recorded in the

field log book as described in Section 6.7.

13.0 REPORTING

After the analytical results for the samples have been

evaluated, a written report on the data will be prepared. The

report will contain the analytical results and an assessment of

the data quality. To ensure against errors in transcription, the

reported data will be checked by at least two individuals for

accuracy. The Project Manager or his designated representative

10 will submit the report to the Principal-In-charge for final comment.

11 b

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iv \ ' • Y;1/4 • . anal 9? r'r Dr. SAMPLING AREA a-77, n •- _ussi

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Map of the Chemical Storage Area FIGURE 2 Drain

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Concrete Concrete Footing Footing

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2 4

Fee: - Proposed Sample Locations

Figure 3 - Hydrofluoric Acid Tank Storage A-3,-c (CPP727) c

Project Organization*

Principal-In-Charge Joan Poland (WINCO)

Project Manager Joseph Moore (UURI)

Project Quality Sampling and Assurance Decontamination Officers Joseph Moore Gary Colgan (UURI) Ralph Helfer Gary Colgan (EnviroSearch) (EnviroSearch)

Inorganic Analyses (UURI)

* Abbreviations: WINCO,Westinghouse Idaho Nuclear Company Inc.; UURI, University of Utah Research Institute.

FIGURE 4 UNIVERSITY OF UTAH RESEARCH INSTITUTE U 391 CHIPETA WAY, SUITE C SALT LAKE CITY, UTAH 84108-1295 TELEPHONE 801-524-3422

SAMPLE CUSTODY CONTROL RECORD

SAMPLE DATE:

WELLS OR MAT'LS SAMPLED: SAMPLE NUMBERS

PARAMETERS FOR ANALYSIS

SPECIAL INSTRUCTIONS:

SAMPLE COLLECTION DRESERVATION

I certify that these samples were collected by me in accordance with EP' procedures and guidelines.

Name Signature Date/Time

RECEIPT ACKNOWLEDGEMENT (LABORATORY)

I received the designated samples from at am/pm (date). They were properly sealed

Name Signature Oate/Time

FIGURE 5 c

METHOD 3050

ACID DIGESTION OF SLUDGES

1.0 Scope and Application

1.1 Method 3050 is an acid digestion procedure used ta prepare sludge- type and soil samples for analysis by flame or furnace atomic absorption spectroscopy (AAS) or by inductively coupled argon plasma spectroscopy (ICP). Samples prepared by Method 3050 may be analyzed by AAS or 1CP for the following metals:

Antimony Lead Arsenic Nickel Barium Selenium Beryllium Silver Cadmium Thallium Chromium Zinc Copper

1.2 Method 3050 may also be applicable to the analysis of other metals in sludge-type samples. However, prior to using this method for other metals, it must be evaluated using the specific metal and matrix.

2.0 Summary of Method

2.1 A dried and pulverized sample is digested in nitric acid and hydrogen peroxide. The digestate is'then refluxed with either nitric acid or hydrochloric acid. Hydrochloric acid is used as the final reflux acid for the furnace analysis of Sb or the flame analysis of Sb, Ba, 8e, Cd, Cr, Cu, Pb, Ni, and Zn. Nitric acid is employed as the final reflux acid for the furnace analysis of As, Ba, Be, Cd, Cr, Cu, Pb, Ni, Se, Ag, 71, and Zn or the flame analysis of Ag and Tl.

3.0 Interferences

3.1 Sludge samples can contain diverse matrix types, each of which may present its own analytical challenge. Spiked samples and any relevant standard reference material should be processed to aid in determining whether Method 30S0 is applicable to a given waste. Nondestructive techniques such as neutron activation analysis may also be helpful in evaluating the applicabil- ity of this digestion method.

4.0 Aoparatus and Materials

4.1. 125-ml conical Phillips' beakers.

4.2 Watch glasses.

A 'OA 4.3 Drying ovens that can be maintained at 30' C.

4.4 Thermometer that covers range of 0' to 200' C.

4.5 Whatman No. 42 filter paper or equivalent.

5.0 Reagents

5.1 ASTM Type II water (ASTM 01193): Water should be monitored for impurities.

5.2 Concentrated nitric acid: Acid should be analyzed to determine level of impurities. If impurities are detected, all analyses should be blank corrected.

5.3 Concentrated hydrochloric acid: Acid should be analyzed to deter- mine level of impurities. If impurities are detected, all analyses should be blank corrected.

5.4 Hydrogen peroxide (307): Oxidant should be analyzed to determine level of impurities. If impurities are detected, all analyses should be blank corrected.

6.0 Sample Collection, Preservation, and Handling

6.1 All samples must have been collected using a sampling plan that addresses the considerations discussed in Section One of this manual.

6.2 A 1 sample containers must be prewashed with detergents, acids, and distilled deionized water. Plastic and glass containers are both suitable.

6.3 Nonaqueous samples shall be refrigerated when possible, and analyzed as soon as possible.

7.0 Procedure

7.1 Weigh and transfer to a 125-ml conical Phillips' beaker a 1.0-9 portion of sample which has been dried at 60' C, pulverized, and thoroughly mixed.

7.2 Add 10 ml of 1:1 nitric acid (HNO3), mix the slurry, and cover with a watch glass. Heat the sample at 95' C and reflux for 10 min. Allow the sample to cool, add 5 ml of conc. HNO3, replace the watch glass, and reflux for 30 min. Do not allow the volume to be reduced to less than 5 ml while maintaining a covering of solution over the bottom of the beaker.

Revised 4/84 APPENDIX 1.1 Cont. o o

CD 7.3 After the second reflux step has been completed and the sample has cooled, add 2 ml of Type 11 water and 3 ml of 30% hydrogen peroxide (H202). Return the beaker to the hot plate for warming to start the peroxide reaction. Care must be taken to ensure that losses do not occur due to excessively vigorous effervescence. Heat until effervescence subsides, and cool the beaker.

7.4 Continue to add 30% H202 in 1-ml aliquots with warming until the effervescence is minimal or until the general sample appearance is unchanged. (NOTE: Do not add more than a total of 10 ml 30% H202.)

7.5 If the sample is being prepared for the furnace analysis of Ag and Sb or direct aspiration analysis of Ag, Sb, Ba, Be, Cd, Cr, Cu, Pb, Ni, Tl, and Zn, add 5 ml of 1:1 HCI and 10 ml of Type II water, return the covered beaker to the hot plate, and heat for an additional 10 min. After cooling, filter through uhatman No. 42 filter paper (or equivalent) and dilute to 100 ml with Type II water (or centrifuge the sample). The diluted sample has an approximate acid concentration of 2.51 (v/v) HC1 and 0.5% (v/v) HNO3 and is now ready for analysis.

7.6 If the sample is being prepared for the furnace analysis of As, Ba, Be, Cd, Cr, Cu, Pb, Ni, Se, T1, and Zn, continue heating the acid-peroxide digestate until the volume has been reduted to approximately 2 ml, add 10 ml Type II water, and warm the mixture. After cooling, filter through datman No. 42 filter paper (or equivalent) and dilute to 100 ml with Type 11 water (or centrifuge the sample). The diluted digestate solution contains approximately 2% (v/v) HNO3. For analysis, withdraw aliquots of appropriate volume, add any required reagent or matrix modifier, and analyze by method of standard additions.

8.0 Quality Control

8.1 For each group of samples processed, procedural blanks (Type II water and reagents) should be carried throughout the entire sample-preparation and analytical process. These blanks will be useful in determining if samples are being contaminated.

8.2 Duplicate samples should be processed on a routine basis. Duplicate samples will be used to determine precision. The sample load will dictate the frequency, but 111% is recommended.

8.3 Spiked samples or standard reference materials should be employed to determine accuracy. A spiked sample should be included with each group of samples processed and whenever a new sample matrix is being analyzed.

8.4 The concentration of all calibration standards should be verified - - inst a quality control check sample obtained from an outside source.

8.5 The method of standard addition shall be used for the analysis of all EP extracts and whenever a new samP le matrix is being analyzed.

APPENDIX 1.1 Cont. Revised 4/84 United States Environmental Monitoring and Environmental Protection Support Laboratory Agency Cincinnati OH 45268

Research and Oavelopment sEPA Test Method

inductively Coupled Plasma— Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes Method 200.7

1. Scope and Application added as rnore information becornes available and as required 1 1 This metnod may be used for the determination of dissolved. 1.5 Because of the differences suspended. or total elements in between various makes and models of .drinking water, surface water. satisfactory instruments. no detailed domestic and industrial wastewaters. instrumental operating instructions can be provided. Instead. the analyst 1.2 Dissolved elements are is referred to the instructions provided determined in filtered and acidified by the rnanufacturer of the particular samples. Appropriate steps must be instrument. taken in all analyses to ensure that potential interference are taken into 2. Summary of Method account. This is especially true when dissolved solids exceed 1500 mg/L. 2.1 The method describes a (See 5.) technique for the sirnultaneous or sequential muftielement 1.3 Total elements are determined determination of trace elements in after appropriate digestion procedures solution. The basis of the method is are performed. Since digestion the measurement of atomic emission techniques increase the dissolved by an optical spectroscopic technique. solids content of the samples. Samples are nebulized and the appropriate steps must be taken to aerosol that is produced is transported correct for potential interference to the plasma torch where excitation effects.(See 5.) occurs. Characteristic atomic-line emission spectra are produced by a radio-frequency inductively coupled 1.4 Table 1 lists elements for which plasma (ICP). The spectra are this method applies along with dispersed by a grating spectrometer recommended wavelengths and and the intensities of the lines are typical estimated instrumental monitored by photomultiplier tubes. detection limits using conventional The photocurrents from the pneumatic nebulization. Actual photomultiplier tubes are processed working detection limits are sample and controlled by a computer system. dependent and as the sample matrix A background correction technique is varies. these concentrations may also required to compensate for variable vary. In time. other elements may be background contribution to the

Merals-20 Dec. 1982

R nrs••• tr.• %. determination uf trace elements. verify background and interelement unresolved overlap of molecular band Background must be measured correction factors.(See 7.6.2) spectra; 3) background contribution adjacent to analyte lines on samples from continuous or recombination during analysis. The position selected 3.9 Quality control sample - A phenomena: and 4) background solution obtained from an for the background intensity outside contribution from stray light frorn the measurement. on either or both sides source having known, concentration line emission of high concentration of the analytical line. will be values to be used tO verify the elements. The first of these effects determined by the complexity of the calibration standards.(See 7.6.3) can be compensated by utilizing a spectrum adjacent to the analyte line. cornputer correction of the raw data, 3.10 Calibration standards - a The position used rnust be free of requiring the monitoring and series of know standard speCtral interference and reflect the solutions measurement of the interfering used by the analyst for calibration of same change in backgraund element. The second effect may the instrument (i.e.. preparation of the intensity as occurs at the analyte require selection of an alternate analytical curve). ISee 7.4) wavelength measured. Background wavelength. The third and fourth of effects can usually be compensated by correction is not required in cases 3.17 Linear dynamic range - The broadening background a background correction adjacent to line where a concentration range over which the the analyte line. In addition. users of correction measurement would analytical curve rernains linear. actually degrade the analytical result. simultaneous multielement The possibility of additional 3.12 Reagent blank - A volume of instrumentation must assume the interferences named in 5.1 (and tests deionized. distilled water containing responsibility of verifying the absence (or their presence as described in 5.2) the same acid matrix as the of spectral interference from an should also be recognized and calibration standards carried through element that could occur in a sample appropriate corrections made. the entire analytical scheme.(See but for which there is no channel in 7.5.2) the instrument array. Listed in Table 2 3. Definitions are some interference effects for the 3.13 Calibration blank - A volume recomrnended wavelengths given in 3.1 Dissolved - Those elements of deionized. distilled water acidified Table 1. The data in Table 2 are which will pass through a 0.45 pm with HNO3 and HCI. (See 7.5.1) intended for use only as a membrane filter. rudimentary guide for the indication of 3.14 Method of standard addition - potential spectral interferences. For 3.2 Suspended - Those elements The standard additian technique this purpose, linear relations between which are retained by a 0 45 prn involves the use of the unknown and concentration and intensity for the -nembrane filter. the unknown plus a known amount of analytes and the interferents can be standard. (See 10.6.1) assumed. 3.3 Total - The concentration The interference information, which determined on an unfiltered sample 4. Safety was collected at the Ames Laboratory.' following vigorous digestion (9.3). or is expressed at analyte concentration the sum of the dissolved plus 4.1 The toxicity or carcinogenicity of eqivalents (i.e. false analyte concen- suspended concentrations 19.1 plus each reagent used in this rnethod has trations) arising frorn 100 rng/L of the 9.21 not been precisely defined; however, interferent element. The each chemical compound should be suggested use of this inforrnation is as 3.4 Total recoverable - The treated as a potential health hazard. follows: concentration determined on an From this viewpoint. exposure to Assume that arsenic (at 193.696 PM) is to be determined in a unfiltered sampte following treatment these chemicals must be reduced to sample containing approximately 10 mg/L of with hoz dilute mineral acid (9.4). the lowest possible level bv whatever According to means available. The laboratory is aluminum. Table 2. 100 mg/L of aluminum would 3.5 Instrumental detection limit - responsible for maintaining a current yield a false The concentration sIgnal for arsenic equivalent to a awareness file of OSHA regulations equivalent to approximately 1.3 mg/L signal, due to the analyte. which is regarding the safe handling of the Therefore. l 0 rng/L of aluminum would result in equal to three times the standard chemicals specified in this method. A a false signal for arsenic deviation of a series of replicate reference We of material data equivalent to approxirnately 0.13 mg/L The reader measurements of a reagent blank handling sheets should also be made is cautioned that signal at the same wavelength. available to all personnel involved in other analytical may the chemical analysis. Additional svstems exhibit somewhat 3.6 Sensitivity - The slope of the different levels of references to laboratory safety are interference than analytical curve. i.e. functional those shown in available and have been identified Table 2, and.that the relationship between emission interference effects must be evaluated (14.7, 14.8 and 14.91 for the intensity and concentration. for each individual system. information of the analyst. 3.7 instrument check standard - A 5. Interferences Only those interferents listed were multielement standard of known investigated and the blank spaces in concentrations prepared by the 5.1 Several types of interference Table 2 indicate that measurable inter- analyst to monitor and verify effects may contribute to inaccuracies ferences were not observed for the instrument performance on a daily in the determination of trace interferent concentrationa listed in .is. (See 7.6.1) elements. They can be summarized as Table 3. Generally, interferences were follows: discerniblp if they produced peaks or .d interference check sample - A background shifts corresponding to solution containing both interfering 5.1.1 Spectra/ interferences can be 2-5% of the peaks generated by the and analyte elements of known categorized as 1) overlap of a spectral lAmeg Laboratory. USDOE. knoll Slat• UniVanity. concentration that can be used to line from another element: 21 Ames lowa SOW t

Der. 1982 Metals-21 analyte concentrations also listed in imally a factor of 10 above the instru- responsibility of the analyst to verify Table 3. mental detection limit after dilution), that the instrument configuration a, At present, information on the listed an analysis of a dilution should agree operating conditions used satisfy thc are silver and potassium wavelengths wimin 5 % of the original determina- analytical requirements and to not available but it has been reporteo tion (or within some acceptable con- rnaintain quality control data that second order energy from the trol limit (14.3) that has been estab- confirming instrument performance magnesium 383.231 nm wavelength lished for that matrix). If not. a and analytical results. interferes with the listed potassium line chemical or physical interference ef• at 766 491 nm. lect should be sqspected. 7. Reagents and standards 7.1 in the 5.1.2 Physical interferences are 5.2.2 Spike addition—The recovery Acids used preparation and for generally considered to be effects ol a spike addition added at a of standards sarnple processing associated with the sample nebuliza- rninirnurn level of 10X the in- rnust be ultra-high purity grade or tion and transport vocesses. Such strumental detection limit (maximum equivalent. Redistilled acids are properties as change in viscosity and 100X) to the original determination acceptable. surface tension can cause significant should be recovered to within 90 to 7.1.1 Acetic acid. conc (sp gr 1.06). inaccuracies especially in samples 110 percent or within the established which may contain high dissolved control limit for that matrix. If not. a 7.1.2 Hydrochlonc acid. conc. (sp gr solids and/or acid concentrations. The matrix effect should be suspected. The 1.19) use of a peristaltic purnp may lessen use of a standard addition analysis these interferences. If these types of procedure can usually cornper- ate for 7. " 3 Hydrochlor: acid. (141): Adn interferences are operative, they must this effect Caution: The stanc.: ad- 50_, mL conc. HCI t-ap gr 1.19) to 4C be redL :ed by dilution of the sample dition te": - nique does not dete-- coin- mL aeionized, distrilled water and and/or utilization of standard addition cident scactral overlap. If suspected, dilute to 1 liter. techniques. Another problem which use of computerized cornpensatiort, an can occur from high dissolved solids alternate wavelength, or comparison 7.1.4 Nitric acid. conc. (sp gr 1.411. is salt buildup at the tip of the with an alternate rnethod is recom- 7.1.5 Nitric acid,(1+1): Add nebulizer. This affects aersol flow-rate mended. ;See 5.2.3) 500 rnL causing instrumental drift. Wetting conc. HNO) (sp. gr 1 41) to 400 mL the argon prior to nebulization, the 5.2.3 Comparison with alternate deionized. distilled water and dilute to use of a tip washer. or sampte dilution method o/ analysis—When investi- 1 liter. have been used to control this gating a new sample matrix. compan- 7.2 Dionized, distilled water: Prepare problem. Also, it has been reported son tests may be performed with other by passing distilled water through a that better control of the argon flow analytical techniques such as atomic mixed bed of C3tion and anion ex• rale improves instrument absorption spectrometry, or other change resins. Use deionized. perforrnance. This is accomplished approved methodology. distilled water for the preparation of all with the use of mass flow controllers. 5.2.4 Wavelength scanning a reagents. calibration standards and as 5.7.3 Chemical interferences are analyte line region—lf the appropriate dilution water. The purity of this water characterized by molecular compound equipment is available. wavelength must be equivalent to ASTM Type II formation, ionization effects and scanning can be performed to detect reagent water of Specification 0 1193 solute vaporization effects. Normally Potential spectral interferences. (1 4.6) these effects are not pronounced with 7 3 Standard stock solutions may be the ICP technique, however. if 6. Appara 3 purchased or prepared "cm ultra high observed they can be minimized by 6.1 Inductivet.. Loupled Plasma- purity grade chernicals ..r metals. All careful selection of operating Atomic Emission Spectrometer. salts must be dried for 1 h at 105°C conditions (that is. incident power, unless otherwise specified. observation position, and so forth), by 6.7.1 Computer controlled atomic (CAUTION: Many rnetal salts are ex- buffering of the sample. by matrix emission spectrometer with background tremely toxic and may be fatal if swal- matching. and by standard addition correction. lowed. Wash hands thoroughly after procedures. These types of handling.) Typical stock solution pre- interferences can be highly dependent 6.1.2 Radiofrequency generator. paration procedures follow: on matrix type and the specific analyte element. 6.1.3 Argon gas supply, welding 7.3,1 Aluminum solution, stock 1 grade or better. rnL = 100 pg Al: Dissolve 0.100 g of 5.2 It is recommended that aluminum metal in an acid mixture of 4 whenever a new or unusual sarnple 6.2 Operating conditions — Because mL of (1+1) HCI and 1 mL of omit. HNOs matrix is encountered, a series of of the differences between various in a beaker. Warm gently to effect tests be performed prior to reporting makes and models of satisfactory on. When solution is complete, concentration data for analyte nstruments, no detailed operating er quantitatively to a liter flask, elements. These tests, as outlined in Istructions can be provided. Instead, an additional 10 mL of (1«1) HCI 5.2.1 through 5.2.4, will ensure the .ne analyst should follow the and dilute to 1.000 mL with deionized, analyst that neither positive nor instructions provided by the distilled water. negative interference effects are manufacturer of the particular operative on any of the analyte el- instrument. Sensitivity, instrumental 7.3.2 Antimony solution stock. 1 rnL ements thereby distvting the detection limit. precision. linear dy- = 100 Ng Sb: Dissolve 0.2669 g K(5130) accuracy of the reported values. namic range, and interference effects C.1-1406 in deionized distilled water. must be investigated and established add 10 mL (1+1) HCI and dilute 5.2.1 Serial dilusion—lf the analyte for each individual analyte line on that to 1000 mL with deionized. distilled concentration is sufficiently high (min• particular instrument. It is the water.

Metals-22 On. 7982 7.3.3J. Arsenic solution. stock. 1 rrt = 7.3.12 Iran solution. stock. 1 mL 7.3.23 Thallium solution. stock. 1 100 itt4 As. Dissolve 0.1320 g of 44/03 = 100 pg Fe: Dissolve 0.1430 g mL = 100 pg TI: Dissolve 0.1303 g in 100 mL of deionized. distilled water Fe303 in a warm mixture of 20 mL TINO3 in deionized, distilled water. containing 0.4 g NaOH. Acidify the (1+1) HCI and 2 mL of conc. HNO,. Add 10.0 mL conc. HNO, and dilute solution with 2 mL conc. HNO3 and Cool, add an additional 5 mL of conc. to 1,000 mL with deionized, distilled dilute to 1.000 mL with deiOnized. HNO3 and dilute to 1000 mL with water. tlisGlled water. deionized. distilled water. 7.3.24 Vanadium solution. stock, 1 7.3.4 Barium solution, stork. 1 nt 7.3.13 Lead solution. stock. 1 rnL mL = 100 pg V: Oissolve 0.2297 = 100 pg 8a: Dissolve 0.1516 g BaC13 = 100 pg Pb: Dissolve 0.1599 g NH.V03 in a minimurn amount of (dried at 250°C lor 2 hrs) in 10 mt_ Pb(N0313 in minirnum amount of conc. HNO3. Heat to increase rate deionized, distilled water with 1 mL (1+1) HNO3. Add 10.0 mL conc. HNO, of dissolution. Add 10.0 mL conc. (1+1) HCI. Add 10.0 rnL (1+1) HCI and dilute to 1.000 mL with deionized. HNO, and dilute to 1.000 rnL with and dilute to 1.000 rnL with deionized. distilled water. deionized, distilled water. distilled water. 7.3.14 Magnesium solution. stock, 1 7.3.25 Zinc solution. stock, 1 mL 7.3.5 Beryllium solution, stock. 1 rn1.. = 100 pg Mg: Dissolve 0.1658 g = 100 Ang Zn: Oissolve 0.1245 g ZnO mL = 100 pg 8e: Do not dry. Dis- Mg0 in a minimum amount of (1+1) in a minimum amount of dilute HNO,. solve 1.966 g BeSO. - 4 41-430. in HNO3. Add 10.0 rnL conc. HNO, and Add 10.0 mL conc. HNO, and dilute deionized, distilled water, add 10.0 mL dilute to 1.000 mL with deionized, to 1.000 rnL with deionized. distilled conc. HNO, and dilute to 1.000 nt distilled water. water. with deionized. distilled water. 7.3.15 Manganese solution. stock. 1 7.4 Mixed calibration standard so- 7.3.6 Boron solution. stock. 1 rill mL = 100 pg Mn: Dissolve 0.1000 g lutions-Prepare mixed calibration = 100 pg 13: Do not dry Dissolve of manganese metal in the acid mix• standard solutions by combining ap- 0 5716 g anhydrous H3803 in deionized lure 10 rnL conc. HCI and 1 mL conc. propriate volumes of the stock solu- distilled water dilute to 1.000 rnL. HNI03, and dilute to 1,000 mL with tions in volumetric flasks. (See 7.4.1 Use a reagent meeting ACS specifi'ca- deionized, distilled water. thru 7.4.5) Add 2 mL of (1+1) tions. keep the bottle tightly stoppered HCI and dilute to 100 mL with and store in a desiccator to prevent 7.3.16 Molybdenum solution. stock. deionized. distilled water. (See Notes the entrance ol atmospheric moisture. 1 rnL = 100 pg Mo: Dissolve 0.2043 g 1 and 6.) Prior to preparing the mixed (NH.)3Mo0. in deionized. tlistdled standards. each stock solution should 7.3.7 Cadmium solution. stock. 1 water and dilute to 1.000 mL. be analyzed separately to determine mL = 100 tig Cd Dissolve 0.1142 g possible spectral interference or the 7.3.17 stock. 1 Cd0 in a minimum amount of (1+1) Nickel solution, presence of impurities. Care should HNO3. Heal to increase rate of dis- mL = 100 rig Ni. Dissolve 0.1000 g be taken when preparing the mixed solution. Add 10 0 rnL conc. HNO3 of nickel metal in 10 rnL hot conc. standards that the elements are com- and dilute to 1.000 mL with deionized. HNO3. cool and dilute to 1.000 mL patible and stable. Transfer the mixed distilled water. with deionized, distilled water. standard solutions to a FEP fluoro- carbon or unused polyethylene bottle 7.3.18 Potassium solution stock, 1 7.3.8 Calcium solution, stock. 1 mL for storage. Fresh mixed standards mL = 100 pg K: Dissolve 0.1907 g = 100 pia Ca: Suspend 0.2498 g should be prepared as needed with KCI, dried at 110°C. in deionized. CaCO3 dried at 180°C lor 1 h before the realization that concentration can distilled water dilute to 1.000 mL. weighing in deionized. distilled water change on aging. Calibration stand- and dissolve cautiously with a min• 7.3.19 Selenium solution. stock. 1 ards must be initially verified using imum amount of (1+1) HNO3. Add a quality control sample and moni- 10.0 mL conc. mL = 100 pg Se: Oo not dry. Dissolve HNO3 and dilute to tored weekly for stability (See 7.6.3). 1.000 rnL with 0.1727 g Hae(33(actual assay 94.6%) deionized, distilled Although not specifically required. water. in deionized, distilled water and dilute to 1.000 mL. some typical calibration standard corn• binations follow 7.3.9 Chromium solution. stock, 1 when using those specific wavelengths listed in Table rnL = 100 pg Cr: Oissolve 0.1923 7.3.20 Silica solution, stock. 1 mL 1. g of Cr03 in deionized. distilled = 100 pg SiO3: Do not dry. Oissolve water. When solution is complete, 0.4730 g NazSiO3 • 9H,0 in deionized. acidify with 10 mL conc. HNO3 and distilled water. Add 10.0 mL conc. 7.4.1 Mixed standard solution /- dilute to 1.000 mL with deionized, HNO, and dilute to 1.000 mL with Manganese. beryllium. cadmium. lead. distilled water. deionized, distilled water. and zinc. 7.3.2 f Silver solution, stock, 1 7.3.10 Cobalt solution. stock, 1 7.4.2 solution II- mL = 100 pg Ag: Dissolve 0.1575 g Mixed standard mL 2 100 pg Co: Oissolve 0.1000 g Barium, copper, iron, vanadium. and AgN0,in 100 mL of deionized. dis• of cobalt metal in a rninirnum amounl cobalt. of (1+1) HNO,. Add 10.0 mL (1+1) HCI tilled water and 10 mL conc. HNO,. with deionded. and dilute tn 1,000 mL with deionized. Oilute to 1,000 mL distilled water, distilled water. 7.4.3 Mixed standard solution In- Molybdenum, silica. arsenic, and '.3.11 Copper solution, stock, 1 7.3.22 Sodium solution. stock 1 selenium. tL = 100 pg Cu: Dissolve 0.1252 g mL = 100 pg Na: Oissolve 0.2542 g Cu0 in a minimum amount of (1+1) NaCI in deionized. distilled water. HNO, Add 10.0 mL conc. HNO3 and Add 10.0 mL conc. HNO, and dilute 7.4.4 Mixed standard solution IV- dilute to 1.000 mL with deionized, to 1.000 mL with deionized. distilled Calcium. sodium, potassium, alumi- distilled water. water. num. chromium and nickel.

On 1982 Metals-23 7.4.5 Mixed standard snlinion V— detection limits given in Table 1. (For an active analytical quality control Antimony, boron .nagnesium. silver. effluent samples of expected high program using spiked samples and re- and thallium, concentrations ,zoike at an agent blanks. that certain steps in the NOTE 1: lf the :ion of silver appropriate lev- !I the type of cleaning procedure are not required for to the recommer acid combination samples analy: ire varied. a routine samples. those steps may be results in an unit. ecrpitation. synthetically pr ared sample may be eliminated from the procedure. add 15 mL cat deto-ized distilled used if the above criteria and intent water and warm the flask until the are met. A limited supply of a 8.2 Before collection of the sample a solution clears. Cool and dilute to 100 synthetic interference check sample decision must be made as to the type mL with deionized. distilled water. For will be available from the Quality of data desired. that is dissolved. this acid combination the silver con- Assurance Branch of EMSL- suspended or total, so that the appro- centration should be limited to 2 Cincinnati. (See 12.1.2) priate preservation and pretreatment mg/L. Silver under these conditions steps may be accomplished. Filtration, is stable in a tap water matrix 7,6.3 The quality control sample acid preservation. etc.. are to be per. Mr 30 days. Higher concentralions should be prepared in the same acid formed at the time the sample is of silver require additional HCI matrix as the calibration standards coliected or as soon as possible at a concentration near 1 mg/L and in thereafter. 7.5 Two types ol blanks are tequired accordance with the instr ::ions for the analysis. The calibration blank provided by lhe supplier. e Quality 8.2.1 For the deterrnination of dis- (3.131 is used in establishing the Assurance Branch of EMSL-Cincinnati solved elernents the si—ole must be analytical curve while the reagent will either supply a quality control filtered through a 0.4 rnembrane blank (3.12) is used to correct for sample or information where one of filter as soon as pract 3fter collec- possible contamination resulting from equal quality can be procured.(See lion. (Glass or plastic ,ring appara- varying amounts oi the acids used in 12.1.3) tus are recommended lo avoid possi- the sarnple processing ble contamination.) Use the first 50- 100 mL to rinse the filter flask. Dis- 8. Sample handling an 7.5.1 The calibration blank is pre. , card this portion and collect the preservation pared by diluting 2 mL ol (1 • 1) HNO3 required volume of filtrate. Acidify the and 10 mi. of (1•1) HO to 100 mt.. filtrate with (1 41) HNC), to a pH of 2 8.1 For the determination of trace wilh deionizo4 distilled water. (See or less. Norrnally. 3 mL of (1+1) acid elements. contamination and loss Note 6 I Prepare a sufficient Quantity are per liter should be sufficient to pre- of prime concern. Dust in the labora- to be used to flush the system be- serve the sample. tory environment, impurities in tween standards and samples. reagents and impurities on laboratory 8 2.2 For the determination of sus- apparatus which the sample contacts 7.5.2 The reagent blank must con- oended elements a measured volume are all sources 01 potential contain all the reagents and in the of unpreserved sample must be fil- contamination. Sample containers can same volumes as used in the pro- tered through a 0.45-pm membrane introduce either positive or negative cessing of the samples. The reagent f titer as soon as practical after errors in the measurement of blank must be carried through the trace collection. The filter plus suspended elements by (a) contributing con• complete procedure and contain the material should be transferred to a taminants through leaching or same acid concentration in the final surface suitable container for storage and/or desorption and (b) by depleting solution as the sample solution shipment. No preservative is required. used for analysis concentrations through adsorption. Thus the collection and treatment of 8.2.3 For the determination of total 7.6 In addition to the calibration the sample prior to analysis requires or total recoverable elements. the standards, an instrument check stan- particular attention. Laboratory sample is acidified with (1+1) HNO3 dard (3.7), an interference check glassware including the sample bottle to ple 2 or less as soon as possible, sample (3.8) and a quality control (whether polyethylene. polyproplyene p-eferable at the time of collection. sample (3.9) are also required for the or FEP-fluorocarbon) should be The sample is not filtered before analyses. thoroughly washed with detergent processing. and tap water: rinsed with (1+1) nitric 7.6.1 The instrument check standard acid. tap water,(1+1) hydrochloric 9. Sample Preparation is prepared by the analyst by com- acid, tap and finally deionized. distilled 9.1 For the determinations of dis- bining compatible elermintS lila con- water in that order (See Notes 2 and solved elements. the filtered, centration equivalent to the midpoint 31. preserved sample may often be of their respective calibration curves. NOTE 2: Chromic acid may be useful to analyzed as received. The acid matrix (See 12.1.1) remove organic deposits from glass- and concentration of the samples and ware; however, the analyst should be calibration standarrts rnust be the 7.6.2 The interference check sample be cautioned that the glassware must sem.- 3ee Note 6.. precipitate is prepared by the analyst in the be thoroughly rinsed with water to forrr . upon acidification of the following rnanner. Select a remove the last traces of chromium. sarnime or during transit or storage, it representative sample which contains This is especially important if chromium rnust be redissolved before the minimal concentrations of the is to be included in the analytical analysis by addir additional acid analytes of interest by known con- scheme. A commercial product. NOCH- and/or by heat described in 9.3. centration of interfering elernents that ROMIX. available from Godax Labor- will provide an adequate lest of the atories, 6 Vatic* St.. New York. NY 9.2 For the determination of sus- correction factors. Spike the sarnple 10013. may be used in place of pended elements, transfer the mem- with the elements of interest at the chromic acid. Chomic acid should not brane filter containing the insoluble approximate concentration of either be used with plastic boffin. material to a 150-ml Griffin beaker 100 zig/t.. or 5 times the estimated NOTE 3: If it can be documented through and add 4 mL conc. HNO3. Cover the

Metals-24 Dec 1982 c CJ with II Waidi if mid heel clog the nebulizer.(See Note 4.) Adjust sample. Concentration values obtained C77. y it I ly I lie wain acid wilt soon dis• the sample to a predetermined volume should not deviate from the actual

SI.' Ir the membrane based on the expected concentrations values by more than ± 5 percent 1*.Crease the temperature ol the of elements present. The sample is (or the established control limits hr.. plate and digest the material. now ready lor analysis (See Note 6). whichever is lower). If they do. follow Mien the acid has nearly evaporated. Concentrations so determined shall be the recommendations of the instru- cool the beaker and watch glass and reported as "total." ment manufacturer to correct for this acid another 3 mL of conc. HNOs NOTE 5: If low determinations of condition. Cover and continue heating until the boron are critical. quartz glassware digestion is complete, generally indi- should be use. 10.5 Begin the sample run flushing cated by a light colored &gestate. NOTE 6: If the sample analysis solution the system with the calibration blank Evaporate to near dryness (2 mLl, cool. has a ditferent acid concentration solution (7.5.1) between each sample. add 10 rnLI-ICI (1.1) and 1 5 all from that given in 9.4, but does not (See Note 7.) Analyze the instrument deionized. distilled water per 100 rnL introduce a physical interference or check standard (7.6.1 ) and the calibra- dilution and warm the beaker gently affect the analytical result, the same tion blank (7.5.1) each 10 samples for 15 min to dissolve any precipi- calibration standards may be used. 10.6 If it has been found that tated or restdue material. Allow to method of standard addition are cool. wash down the watch glass and 9.4 For the determination of total required. the following procedure is beaker walls with deionized distilled recoverable elements. choose a mea- recommended. water and filter the sarnple to rernove sured volume of a well mixed. acid insoluble material that could ctog the preserved sample appropriate for the 10.6.1 The standard addition tech- nebulizer. (See Note 4 ) Adlust the expected level of elements and trans- nique (14.2) involves preparing new volume based on the expected con- fer to a Griffin beaker. (See Note 5.) standards in the sample matrix by centrations of elements present. This Add 2 mt. of (14.1) HNO,and 10 rnL adding known amounts of standard 10 volume will vary depending on the of (141) HCI to the sample and heat one or more aliquots of the processed elements to be determined (See Note on a steam bath or hot plate until the sample solution. This technique com• sample is now ready for volume 6). The has been reduced to near 25 pensates for a sample constituent that Concentrations so determined mL making analysis. certain the sample does enhances Or depresses the analyte not shall be reported as -suspended." boil After this treatment. cool signal thus producing a different slope 4 of filtering, NOTE In place the the sample and filter to remove inso- from that of the calibration standards. diluting and mixing sample after may luble material that could clog the It will not correct for additive inter- be centrifuged or allowed to settle bv nebulizer.(See Note 4.) Adjust the ference which causes a baseline shift. gravity overnight to remove insoluble volume to 100 mL and mix. The sample The simplest version of this technique material. is now ready for analysis. Concentra- is the single-addition method. The tions so deterrnined shall be reported procedure is as follows. Two identical total 9.3 For the determination of as -total.- aliquots of the sample solution. each elements, choose a measured. volume of vOlurrie V.. are taken. To the well 10. Procedure of the mixed acid preserved first (labeled A) is added a small sample appropriate for the expected volume V, of a standard analyte level of elements and transfer to a 10.1 Set up instrument with proper operating parameters established in solution of concentration c,. To the Griffin beaker. (See Note 5.) Add 3 mL second (labeled B) is added the same conc. HNO3. Place the beaker on 6.2. The instrument must be allowed of volume V, of the solvent. The analy- to near dry- to becorne thermally stable before be- a hot plate and evaporate tical signals of A and B are measured ness cautiously. making certain that ginning. This usually requires at least 30 min. of and corrected for nonanalyte signals. the sample does not boil and that no operation prior to calibra• hon. The unknown sample concentration of the area bottom of Me beaker is c, is calculated: allowed to go dry. Cool the beaker and 10.2 Initiate appropriate operating add another 5 mL portion of conc. configuration of computer. cx = SeVsCs HNO3. Cover the beaker with a watch (SA • Sa) Vx glass and return to the hot plate. 10.3 Profile and calibrate instru- Increase the temperature of the hot ment according to instrument where S. and Se are the analytical plate so that a gentle reflux action manufacturer's recommended signals (corrected for the blank) of occurs. Continue heating, adding addi- procedures, using the typical mixed solutions A and B. respectively. Vs tional acid as necessary, until the calibration standard solutions and cs should be chosen so that SA digestion is complete (generally indi- described in 7.4. Flush the system is roughly twice S.on the average. lt cated when the digestate is light with the calibration blank (7.5.1) is best if v5 is made much less than in color or does not change in appear- between each standard.(See Note 7.) Vs.and thus es is much greater than ance with continued refluxing.) Again, (The use of the average intensity of cc to avoid excess dilution of the evaporate to near dryness and cool multiple exposures for both sample matrix. If a separation or the beaker. Add 10 mL of 1.1 HCI standardization and sample analysis concentration step is used. the and 15 mL of deionized. distilled has been found to reduce random additions are best made first and water per 100 mL of final solution error.) carried through the entire procedure. and warm the beaker gently for 15 NOTE 7: For boron concentrations For the results from this technique to min. to dissolve any precipitate or greater than 500 pg/L extended flush be valid. the following limitations residue resulting from evaporation. times of 1 to 2 min. may be required. must be taken into consideration: Allow to cool, wash down the beaker 1. The analytical curve must be linear. walls and watch glass with deionized 10.4 Before beginning the sample 2. The chemical form of the analyte distilled water and filter the sample to run. reanalyze the highest mixed added must respond the same as the remove insoluble material that could calibration standard as if it were a analyte in the sample.

Lac. 1982 Metals-25 3. The interference effect must Lie standards. A fresh dilution of this constant over the working range of sample shall be anlayzed every week concern. thereafter to monitor their stability. if 4 The signal must be corrected for the results are not within -±5% of the any additive interference. true value listed lor the control sample. prepare a new calibration 11. Calculation standard and recalibrate the correct the 11.1 Reagent blanks (7.5.21 should instrument. 11 this does not problem. prepare a new stock be subtracted from all samples. This is standard and a new Calibration particularly important for digested standard and repeat the calibration. samples requiring large quantities of acids to complete the digestion. Precision and Accuracy were performed, 11.2 if dilutions 13.1 In an EPA round robin phase 1 applied the appropriate lactor must be study, seven laboratories applied the to sample values. ICP technique to acid-distilled water matrices that had been dosed with 11.3 Oala should be rounded to the various rnetal concentrates. Table 4 thousandth place and all results lisis the true value. the mean reported should be reported in rng/L up to value and the mean % relative three significant figures. standard deviation. Quality Control 12. References (Instrumental) 1. Wing& V J. Peterson. and 12.1 Check the instrument V.A. FASC141. "inductively Coupled standardization by analyzing Plasma-Atomic Erntssion aopropriate quality control check Spectroscopy: Prominent Lines.- EPA- standards as follow: 600/4-79 -017.

12.1.1 Analyze an appropriate 2. Winelordner, J D , "Trace instrument check standard (7.6.1) Analysis Spectroscopic Methods for containrng the elements of interest at Elements." Chemical AtialysIs. Vol. a frequency of 10%. This check 46. pp. 41-42 standard is used to determine 3. Handbook tor instrument drilt. If agreement is not AnalyttCal Quality Control in Water and Wastewater within ±5% of the expected values or Laboratories. within the established Control limitS. EPA-600/4-79-019. whicnever is lower, the analysis is out 4. Garbarino. J R. and Taylor. H.E.. control. The analysis should be of -An lnductively-Coupled Plasma terminated. the problem corrected, Atomic Emission Spectrometric the instrument recalibrated. and Method for Routine Water Quality Analyze the calibration blank 1 7.5.1/ Testing." Applied Spectroscopy 33. at a frequency of 10%. The result No. 30979/. should be within the established control limits of two standard devia- 5. "Methods for Chernical Analysts of tions ol the mean value. If not, repeat Water and Wastes." EPA-600/4-79- the analysis two more times and 020. • average Me three results. If the average is not within the control limit. 6 Annual Book of ASTM Standards. terminate the analysis, correct the Part 31. ;floblem and recalibrate the instrument. 7. "Carcinogens - Working With Carcinogens." Department of Health. I 2.1.2 To verify interelement and Education. and Welfare, Public Health background correction factors amity** Service, Center for Disease Control. the interference check sample (7.15.2) National institute for Occupational at the beginning, end. and at periodic Safety and Health, Publication No. 77- intervals throughout the sample run. 206. Aug. 1977. Results should fall within the established control limits of 1.5 times 8. ''OSHA Safety and Health Stan- the standard deviation of the mean dards. General industry. 29 CFR value. II not. terminate the analysis, 1910i. Occupational Safe ind Health correct the problem and recalibrate Administration. OSHA (Revised. the instrument. January 1976).

12.1.3 A quality control sample 9. "Safety in Academic Chemistry 7.6.3) obtained from an outside Laboratories. American Chemical So- fource must first be used for the ciety Publication, Committee on initial verification ol the calibration Chemical Safety, 3rd Edition. 1979.

Merels.26 Dec. 1982 CY: Tab/e 2. Analyre Concentration Equivalents Img/LI Arising From Inierlerents at the 100 mg/L Level Analyte Wavelength. nm Interlerent cn Al Ca Cr Cu Fe Mg Mn Ni Ti V Aluminum 308.215 ------0.21 - - I.4 Antimony 206.833 0.47 - 2.9 - 0.08 - - - .25 0 45 Arsenic 193.696 1.3 - 0.44 ------1.1 Barium 455.403 ------Beryllium 313.042 ------0.04 0.05 Boron 249.773 0.04 - - - 0.32 - - - - -

Cadmium 226.502 - - - - 0.03 - - 0.02 - - Calcium 317 933 - - 0.08 - 0.01 0.01 0.04 - 0.03 0.03 Chromium 267.716 - - - 0.003 - 0.04 - - 0.04

Cobalt 228.616 - - 0.03 - 0 005 - - 0.03 0.15 - Copper 324.754 - - - 0 003 - - 0.05 0 02 Iron 259.940 - - - - - 0.12 - - - Lead 220.353 0.17 - Magnesium 279.079 0.02 0.11 0.13 0.25 - 0.07 0.12 Manganese 257.610 0.005 - 0.01 0.002 0.002 - Molyhdenum 202.030 0.05 - - - 0.03 Nickel 231.604 - - - - - Selenium 196 026 0.23 - - - 0.09

Silicon 288 158 - - 007 ------0.01 Sodium 588.995 ------0 08 - Thallium 190 864 0 30 ------Vanadium 292.402 0.05 aoos - 0.02 Zinc 213 856 0 14 0.29 -

Table J. Interlerent and Analyre Eleniental Concen. trations Used for Interference Measurements in Table 2.

Analytes Img/L) Mtederents /mg/Ll Al 10 AI 7000 As 10 Ca 1000 8 10 Cr 200 Ba l Cu 200 Be l Fe 1000 Ca 1 Mg 1000 Cd 10 Mn 200 Co 1 Ni 200 Cr 1 Ti 200 Cu 1 V 200 Fe 7 Mg 1 Mn 1 Mo 70 Na 70 Ni 10 Pb 10 Sb 10 Se 10 Si 1 TI 10 1 10

metals.28 Dee 7982

APPENDIX 1.2 Con t. Table 4 1CIN Precision and Accuracy Data Sample p 1 Sample 42 Sample 43 Mean Mean Mean True Reported Mean True Reported Mean True Reported Mean Vahm Value Percent Va/ue Value Percent Va/ue Value Percent Element po/L pg/L RSD tig/L po/L RS.7 pg/L pg/L RSO Be 750 733 6.2 20 20. 9.c 760 176 5.2 Mn .350 345 2.7 15 15 6.7 100 99 3.3 V 750 749 1.8 70 69 2.9 170 169 1 1 As 200 208 7.5 • - 7_ 19 23 60 63 17 Cr 150 149 3.8 '0 10 18 50 50 3 3 Cu 250 235 5.1 11 11 40 70 67 7.9 Fe 600 594 3.0 20 19 15 180 178 60 .41 700 696 5.6 60 62 33 160 161 13 Cd 50 48 12 2.5 2.9 16 14 13 16 Co 500 512 10 20 20 4.1 120 108 21 Att 250 245 5.8 30 23 11 ---1 55 14 Pb 250 236 16 24 30 32 80 14 In 200 201 5.6 76 19 45 82 9.4 Se 40 32 21.9 6 8.5 4i 10 8 5 8.3 Not all e/ements were analyzed by all laboratories.

APPENDIX 1.2 Cont.

Dec.1982 Metals-29 ARSENIC

Method 206.4 (Spectrophotometric-SDDC)

STORET NO. 01002 Inorganic, Dissolved 00095 Inorganic. Total 00997 Inorganic , Suspended 00996 l. Scope and Application 1.1 The silver diethyldithiocarbamate method determines inorganic arseni.: when present in concentrations at or above 10 ug/ I. The method is applicable to drinking water and most fresh and sa1ine waters in the absence of high concentrations of chromium, cobalt, copper, mercury, molybdcnum, nickel, and silvcr. Domestic and indui.:rial wastes may also be analyzed after digestion (see 3.3). 1.2 Difficulties may be encountered with certain industrial waste ma:trials containing volatile substances. High sulfur content of wastes may exceed remo‘ll capacity of the lead acetate scrubber. 2. Summary of Method 2.1 Arsenic in the sample is reduced to arsine, AsH j. in acid solutic in a hydrogen generator. The arsine is passed through a scrubber to remove sulfide an:: is absorbed in a solution of silver diethyldithiocarbamatc dissolved in pyridine. The rrd cornplex thus formed is measured in a spectrophotometer at 535 nrn. 3. Comments 3.1 In analyzing drinking water and most surface and ground waters, interferences are rarely encountered. Industrial waste samples should be spiked with a known acnount of arsenic to establish adequate recovery. 3.2 It is essential that the system be airtight during evolution of the arsine, t.r. avoid losses. 3.3 If concentration of the sample and/or oxidation of any organic matter is required, refer to Method 206.5.[Standard Methods, I4th Edition, Method 404B, p. 21z4, Procedure 4.a (1975)]. For sample handling and preservation, see part 4.1 of the Atz‘rnic Absorption Methods section of this manual. 3.31 Since nitric acid gives a negative interference in this test, use s lfuric acid as a preservative if only inorganic arscnic is being rneasured. 3.4 l-Ephedrine in chloroform has been found to be a suitable cc:vent for silver diethyldithiocarbarnate if the analyst finds the odor of pyridine obje-ztionable [Anal. Chem. 45, 1786(1973)]. 3.5 For quality control requirements and optional recommendations for use in drinking water analyses, see part 10 of the Atomic Absorption Methods section cf t his manual.

Approved for NPDES and SDWA Issued 1971 APPENDIX 1.3 Editorial revision 1974

206.4- a. Precision and Accuracy 4.1 In a round•robin study reported by Standard Methads a synthetic unknown sample containing 40 ug/I, as As, with other metals was analyzcd in 46 laboratorics. Relativc standard deviation was t 13.8% and relative error was 0%. 5. Reference 5.1 The procedure to be used for this determination isfound in: Standard Methods for the Examination of Water and Wastewater, 14th Edition, p. 283, Method 404A (1975).

APPENDIX 1. 3 Cont.

206.4-2 c c

METHOD 7471

MERCURY TN SOLID OR SEMISOLID WASTE (MANUAL COLD-VAPOR TECHNIOUE)

1.0 Scope and Application

1.1 Method 7471 is approved for measuring total mercury (organic and inorganic) in soils, sediments, bottom deposits, and sludge-type materials. A11 samples must be subjected to an appropriate dissolution step prior to analysis.

2.0 Summary of Method

2.1 Prior to analysis the samples must be prepared according to the procedures discussed in this method.

2.2 Method 7471, a cold-vapor atomic absorption method, is based on the absorption of radiation at the 253.7-nm wavelength by mercury vapor. The mercury is reduced to the elemental state and aerated from solution in a closed system. The mercury vapor passes through a cell positioned in the light path of an atomic absorption spectrophotometer. Absorbance (peak height) is measured as a function of mercury concentration.

2.3 The typical detection limit for this method is 0.0002 mg/1.

3.0 Interferences

3.1 Potassium permanganate is added to eliminate possible interference from sulfide. Concentrations as high as 20 mg/1 of sulfide as sodium sulfide do not interfere with the recovery of added inorganic mercury from Type II water.

3.2 Copper has also been reported to interfere; however, copper concen- trations as high as 10 mg/1 had no effect on recovery of mercury from spiked samples.

3.3 Seawaters, brines, and industrial effluents high in chlorides require additional permanganate (as much as 25 ml) since, during the oxi- dation step, chlorides are converted to free chlorine which also absorbs radiation 4E153 nm. Care must therefore be taken to ensure that free chlorine tlialitent before the mercury is reduced and swept into the cell. This may be accomplished by using an excess of hydroxylamine sulfate reagent. (25 ml). In addition, the dead air space in the BOO bottle must be purged before adding stannous sulfate. 8oth inorganic and organic mercury spikes have been quantitatively recovered from seawater using this technique.

3.4 Certain volatile organic materials that absorb at this wavelength may also cause interference. A preliminary run without reagents should determine if this type of interference is present.

APPENDIX 1.4 4.0 Apparatus and Materials

4.1 Atomic absorption spectrophotometer or equivalent: Any atomic absoption unit having an open sample presentation area in which to mount the absorption cell is suitable. Instrument settings recommended by the particular manufacturer should be followed. Instruments designed specifically for the measurement of mercury using the cold-vapor techntque are commercially available and may be substituted for the atomic absorptinn spectrophotometer.

4.2 Mercury hollow cathode lamp or electrodeless discharge lamp.

4.3 Recorder: Any multirange variable speed recorder that is compatible with the UV detection system is suitable.

4.4 Absorption cell: Standard spectrophotometer cells 10 cm long having quartz end windows may be used. Suitable cells may be constructed from plexiglass tubing, 1 in. 0.0. x 4.5 in. The ends are ground perpendicular to the longitudinal axis and quartz windows (1 in. diameter x 1/16 in. thickness) are cemented in place. The cell is strapped to a burner for suPport and aligned in the light beam by use of two 2-in. x 2-in. cards. One-in.-diameter holes are cut in the middle of each card. The cards are then placed over each end of the cell. The cell is then positioned and adjusted vertically and hor",zontally to give the maximum transmittance.

4.5 Air p.mp: 'Any peristaltic pump capable of delivering 1 liter 3ir/min may be used. A Masterflex pump with electronic speed control has been fou7d to be Satisfactory.

4.6 Flowmeter: Capable of me2,:uring an air flow of 1 liter/min.

4.7 Aeration tubing: A straight glass frit having a coarse porosity. Tygon tubing is used for passage of the mercury vapor from the sample bottle to the absorption cell and return.

4.8 Drying tube: 6-in. x 3/4-in.-diameter tube containing 20 g of magnesium perchlorate or a small reading lamp with 60-W bulb which may be used to prevent condensation of moisture inside the cell. The lamp should be positioned to shine on the absorption cell so that the air temperature in the cell is about 10. C above ambient.

4.9 The cold-vapor generator is assembled as shown in Figure 1.

4.10 The apparatus shown in Figure 1 is a closed system. An open system, where the mercury vapor is passed through the absorption cell only once, may be used instead of the closed system.

APPENDIX 1.4 Cont. Jc Scrubber Cnnl skiing a Met ciii y Absoibing Media Sampla SnWon In ROO fiords

Houra 1. Apparalus Inr nameless mercury delerrninalion. 4.11 Because mercury ..apor is toxic, precaution must be taken to avoid its inhalation. Therefore, a bypass has been included in the system to either vent the mercury vaper into an exhaust hood or pass the vapor through Some absorbing media, such as:

1. equal volumes of 0.1 M KMn04 and 10: H2SO4

2. 0.25; iodine in a 3% KI solution

A specially treated charcoal that will adsorb mercury vapor is also available from Barnebey and Cheney, E. 8th Ave. and N. Cassidy St., Columbus, Ohio 43219, Cat. #580-13 or #580-22.

5.0 Reagents

5.1 ASTM Type II wa - (ASTM 01193): Water should be monitored for impurities.

5.2 Aqua regia: Pre,:,a.-e immediately cefore use by carefully adding three volumes of conc. HCI to one volume of conc. HNO3.

5.3 Sulfuric acid, 0.5 N: Dilute 14.0 ml of conc. sulfuric acid to 1 liter.

5.4 Stannous sulfate: Add 25 g stannous sulfate to 250 ml of 0.5 N sulfuric acid. This mixture is a suspension and should te stirred continu- ously during use. A 10% solution of stannous chloride can be substituted for stannous sulfate.

5.5 Sodium chloride-hydroxylamine sulfate solution: Dissolve 12 g of sodium chloride and 12 g of hydroxylamine sulfate in Type 11 water and dilute to 100 ml. Hydroxylamine hydrochloride may be used in place of hydroxylamine sulfate.

5.6 Potassium permanganate, 5: solution ,w/v): Dissolve 5 g of potassium permanganate in 100 ml of Type 11 water.

5.7 Mercury stock solution: Dissolve 0.1354 g of mercuric chloride in 75 ml of distilled water. Add 10 ml of conc. nitric acid and adjust the volume to 100.0 ml (1.0 ml = 1.0 mg Hg).

5.8 Mercury working standard: Make successive dilutions of the stock mercury solution to obtain a working standard containing 0.1 ug/ml. This working standard and the dilution of the stock mercury solutions should be prepared fresh daily. Acidity of the working standard should be maintained at 0.15: nitric acid. This acid should be acded to the flask as needed before adding the aliquot. c METHOD 7741

SELENIUM (ATOMIC ABSORPTION, GASEOUS HYDRIDE)

1.0 Scope and Application

1.1 Method 7741 is an atomic absorption procedure which is approved for determining the concentration of selenium in wastes, mobility procedure extracts, soils, and groundwater, provided that the sample matrix does not contain high concentrations of chromium, copper, mercury, silver, cobalt or molybdenum. All samples must be subjected to an appropriate dissolution step prior to analysis. Spiked samples and relevant standard reference materials are employed to determine applicability of the method to a given waste.

2.0 Summary of Method

2.1 Samples are prepared according to the nitric/sulfuric acid digestion procedure described in this method. Next, the selenium in the digestate is reduced to the +4 form ustng tin chloride. The +4 selenium is then converted to a volatile hydride with hydrogen produced from a zinc/HC1 reaction.

2.2 The volatile hydride is swept into an argon-hydrogen flame located in the optical path of an atomic absorption spectrophotometer, and the resulting absorbance is proportional to the selenium concentration.

2.3 The typical detection limit for this method is 0.002 mg/1..

3.0 Interferences

3.1 High concentrations of chromium, cobalt, copper, mercury, molybdenun nickel, and silver can cause analytical interferences.

3.2 Traces of nitric acid left following the sample workup can result in analytical interferences. Nitric acid must be distilled off by heating the sample until fumes of S03 are observed.

3.3 Elemental selenium and many of its compounds are volatile and therefore certain samples may be subject to losses of selenium during sample preparation.

4.0 Apparatus and Materials

4.1 100-ml beaker.

4.2 Electric hot plate.

4.3 A commercially available zinc slurry hydride generator or a generator constructed from the following material (see Figure 1).

'nne.,m,"V 1 5.6 Potassiun iodide solution: Oissolve 20 g CI in 100 ml Type 11 ' water.

5.7 Stannous chloride solution: Oissolve 100 g SnCl2 in 100 ml of conc. HCI.

5.8 Selenium standard stock solution: 1000 mg/liter solution may be purchased, or prepared as follows. Oissolve 0.3453 g of selenious acid (assay 94.61 of H2Se03) in Type 11 water. Add to a 200-ml volumetric flask and bring to volume (I ml = 1 mg Se).

6.0 Sample Collection, Preservation. and Handling

6.1 A11 samples must have been collected using a sampling pian that addresses the considerations discussed in Section One of this manual.

6.2 All sample containers must be prewashed with detergents, acids, and Type 11 water. Plastic and glass containers are both suitable.

6.3 Special containers (e.g., containers used for volatile organic analysis) may have to be used if very volatile selenium compounds are to be analyzed.

6.4 Aqueous samples must be acidified to a pH of less than 2 with nitric acid.

6.5 Nonaqueous samples shall be refrigerated where possible, and analyzed as soon as possible.

7.0 Procedure

7.1 Sample preparation

7.1.1 To a 50 ml aliquot of digested sample (or in the case of EP extracts a 50-ml sample) add 10 ml conc. HNO3 and 12 ml of 18 N H2SO4. Evaporate the sample on a hot plate until white S03 fumes are observed (a volume of about 20 ml). Do not let it char. If it chars, stop the digestion, cool and add additional HNO3. Maintain an excess of HNO3 (evidence of brown fumes) and do not let the solution darken, because selenium may be reduced and lost. When the sample remains colorless or straw yellow during evolution of S03 fumes, the digestion is complete.

7.1.2 Cool the sample, add about 25 ml distilled deionized water and again evaporate to SO3 fumes just to expel oxides of nitrogen. Cool. Add 40 ml conc. HCI and bring to a volume of 100 ml with distilled deionized water.

1.5 Cont. ,evised 4/84 APPENDIX 7.2 Prepare working standards from the standard stock solutions. The following procedure provides standards in the optimum working range.

7.2.1 Pipet 1 ml stock solutlon into a 1-liter volumetric flask. Bring to volume with Type 11 water containing 1.5 ml conc. HNO3/liter. The concentration of thls solution is 1 mg Se/liter (1 ml = 1 pg Se).

7.2.2 Prepare six working standards by transferring 0, 0.5, 1.0, 1.5, 2.0 and 2.5 ml of the selenium stock standard (see Section S.8) into a 100-ml volumetric flasks. Bring to volume with diluent. The concentrations of these working standards are 0, S, 10, 15, 20 and 25 pg Se/liter.

7.3 Standard additions

7.3.1 Take the 15-, 20-, and 25-pg standards and transfer quanti- tatively 25 ml from each into separate 50-ml volumetric flasks. Add 10 ml of the prepared sample to each. Bring to volume with Type 11 water containing 1.5 ml HNO3/liter.

7.3.2 Add 10 ml of prepared sample to a 50-ml volumetric flask. Bring to volume with Type 11 water containing 1.5 ml H1103 per liter. This is the blank.

7.4 Follow the manufacturer's instructions for operating an argon- hydrogen flame. The argon-hydrogen flame is colorless so it may be useful to spirate a lowconcentration of sodium to ensure that ignition has occurred.

7.5 The 196.0-nm wavelength shall be used for the analysis of selenium.

7.6 Transfer a 25-ml portion of the digested sample or standard to the reaction vessel. Add 0.5 ml SnC12 solution. Allow at least 10 min for the metal to be reduced to its lowest oxidation state. Attach the reaction vessel to the special gas inlet-outlet glassware. Fill the medicine dropper with 1.50 ml zinc slurry that has been kept in suspension with the magnetic stirrer. Firmly insert the stopper containing the medicine dropper into the side neck of the reaction vessel. Squeeze the bulb to introduce the zinc slurry into the sample or standard solution. The metal hydride will produce a peak almost immediately. When the recorder pen returns partway to the base line, remove the reaction vessel.

7.7 Analyze. by the method of standard additions, all EP extracts, all samples analyzed as pert of a delisting petition, and all samples that suffer from matrix interferences.

7.8 Duplicates, spiked samples, and check standards should be routinely analyzed.

APPENDIX 1.5 Cont. FLUORIDE

Method 340.2 (Potentiometric, Ion Selective Electrode)

STORET NO: Total 00951 Dissolved 00950

I. Scope and Application 1.1 This method is applicable to the measurement of fluoride in drinking, surface and saline waters, domestic and industrial wastes. 1.2 Concentration of fluoride from 0.1 up to 1000 mg/liter may be measured. 1.3 For Total or Total Dissolved Fluoride, the Bellack distillation is required for NPDE.S monitoring but is not required for SDWA monitoring. 2. Summary of Method 2.1 The fluoride is determined pot.:atiometrically using a fluoride electrode in conjunction with a standard single junction sleeve-type reference electrode and a pH meter having an expanded millivolt scale or a selective ion meter having a direct concentration scale for fluoridc. 2.2 The fluoride electrode consists of a lanthanum fluoride crystal across which a potential is developed by fluoride ions. The cell may be represented by Ag/Ag Cl, 0-(0.3), F(0.001) LaF/test solution/SCE/. 3. Interferences 3.1 Extremes of pH interfere; sample pH should be between 5 and 9. Polyvalent cations of Si'', Fe•' and Al" interfere by forming complexes with fluoride. The degree of interference depends upon the concentration of the complexing cations, the concentration of fluoride and the pH of the sample. The addition of a pH 5.0 buffer (described below) containing a strong chelating agent preferentially complexes aluminum (the most common interference), silicon and iron and eliminates the pH problem. 4. Sampling Handling and Preservation 4.1 No special requirements. 5. Apparatus 5.1 Electrometer(pH meter), with expanded mv scale, or a selective ion meter such as the Orion 400 Series. 5.2 Fluoride Ion Activity Electrode,such as Orion No.94-09'. 5.3 Reference electrode, single junction, sleeve-type, such as Orion No. 90-01, Beckman No. 40454, or Corning No. 476010. 5.4 Magnetic Mixer, Teflon-coated stirring bar.

Approved for NP DES and SDWA Issued 1971 Editorial revision 1974

APPENDIX 1. 6 340.2-1 6. Reagents 6.1 Buffer solution, pH 5.0-5.5: To approximately 500 ml of distilled water in a I liter beaker add 57 ml of glacial acctic acid, 58 g of sodium chloride and 2 g of CDTA'n. Stir to dissolve and cool to room temperature. Adjust pH of solution to between 5.0 and 5.5 with 5 N sodium hydroxide (about 150 ml will be required). Transfer solution to a 1 liter volumetric flask and dilute to the mark with distilled water. For work with brines, additional NaCI should be added to raise the chloride level to twice the highest expected level of chloride in the sample. 6.2 Sodium fluoride, stock solution: 1.0 ml = 0.1 mg F. Dissolve 0.2210 g of sodium fluoride in distilled water and dilute to l liter in a volumetric flask. Store in chemical-resistant glass or polyethylene. 6.3 Sodium fluoride, standard solution: 1.0 ml = 0.01 mg F. Dilute 100.0 ml of sodium fluoride stock solution (6.2) to 1000 ml with distilled water. 6.4 Sodium hydroxide, 5N: Dissolve 200 g sodium hydroxide in distilled water, cool and dilute to l liter. 7. Calibration 7.1 Prepare a series of standards using the fluoride standard solution (6.3) in the range of0 to 2.00 mg/1 by diluting appropriate volumes to 50.0 ml. The following series may be used:

Millimeters of Standard Concentration when Diluted (1.0 ml = 0.01 rng/F) to 50 ml, rng F/liter

0.00 0.00 1.00 0.20 2.00 0.40 3.00 0.60 4.00 0.80 5.00 1.00 6.00 1.20 8.00 1.60 10.00 2.00

7.2 Calibration of Electrometer: Proceed as described in (8.1). Using semilogarithmic graph paper, plot the concentration of fluoride in mg/liter on the log axis vs. the electrode potential developed in the standard on the linear axis, starting with the lowest conceranthoo at the bottom of the scale. Calibration of a selective ion meter: Follow the directiantofthe manufacturer for the operation of the instrument. 8. Procedure 8.1 Place 50.0 ml of sample or standard solution and 50.0 ml of buffer (See Note)in a 150 ml beaker. Place on a magnetic stirrer and mix at medium speed. Immerse the electrodes in the solution and observe the meter reading while mixing. The electrodes must remain in the solution for at least three minutes or until the reading has stabilized. At concentrations under 0.5 mg/liter F, it may require as long as five minutes to reach a stable meter reading; high concentrations stabilize more quickly. If a pH meter is used, record thc potential measurement for each unknown sample and conven the potential

340.2-2 APPENDIX 1.6 Cont. reading to the fluoride ion concentration of the unknown using the standard curve. If a selective ion meter is used, read the fluoride level in the unknown nple di -tly in mg/l on the fluoride scale. NOTE: For industrial waste samples, this amount of buffer may not be adequate. Analyst should check pH first. If highly basic( > 9), add 1 N HCI to adjust pH to 8.3. 9. Precision and Accuracy 9.1 A synthetic sample prepared by the Analytical Reference Service, PHS, containing 0.85 mg/1 fluoride and no interferences was analyzed by 111 analysts; a mean of 0.84 mg/1 with a standard deviation of t0.03 was obtained. 9.2 On the same study, a synthetic containing 0.75 mg./1 fluoride, 2.5 mg/1 polyphosphate and 300 mg/1 alkalinity, was analyzed by the same I 1 1 analysts; a rnean of0.75 mg/1 fluoride with a standard deviation of t0.036 was obtained.

Bibliography

I. Patent No. 3,431,182(March 4, 1969). 2. CDTA is the abbreviated designation of 1, 2-cyclohexylene dinitrilo tetraacetic acid, (Matheson, Coleman & Bell, Cat. No. P8661)or cyclohexane diamine tetraacetic acid,(Merck- Titriplex IV or Baker Cat. No. G083). 3. Standard Methods for the Examination of Water and Wastewaters, p 389, Method No. 414A, Preliminary Distillation Step ()knack), and p 391, Method No. 414B, Electrode Method, 14th Edition (1975). 4. Annual Book of ASTM Standards, Pan 31, "Water, Standard D1179-72, Method B, p 312 (1976).

APPENDIX 1.6 cont. 340.2-3

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1 000 er.e . I Tat 57.40 Z. 470 en. W771771. • #4. men NW! WO 0•601.1 dc-t.77,17h, c9 AW577 OWWW- -1P1NE AT VE5 AA -1 . AVM Mil A WW-6-.0.W7A 4.4-7 17/2.—L4w4,,- reenZL S 407 J arreArr lc 2 C93N )",,-.4or zewr TITLE I _toe /I 44 WO 0 1_ TITLE II • .2.2";;;;;;;..270 171303 ! 3 Lae. — p z recraw/7\ •WIDION ott ca. I mu \r, ▪ oo s 4 3 2 8 7 6 5

Locnnot Pee) 15 St. N P LeNC ?EC CD _noWEL National Engineering Laboratory BCol-05 -91

From B. L. Cole Phone 6-8520/MS-5117 Date March 14, 1991 Subiect Results Of Observation During Excavation Of Asphalt At CPP- 621

To .M. L. Nelson

cc: B. L. Cole-2 C. S. Wellard A. B. Culp J. L. Williams H. Roberts D. J. Williamson A. H. Owen

On March 14, 1991, John Wozniewics, Golder Associates Inc., and Brenda Cole, Environmental Restoration, observed the Excavation of asphalt south of CPP-621 and adjacent to Solid Waste Management Unit (SWMU) CPP-45. We were asked to observe for any discolored soil and run detector tube tests for hydrofluoric acid. The detector tubes were specific to hydrofluoric acid. Their expiration date was April 1992 and their range was 0-25 ppm.

The soil did not appear to show any signs of contamination. The detector tube was placed within 1-2 inches above the soil and below the surface of the soil in 5-6 different locations. The results of the detector tube testing indicated that hydrofluoric acid was not present.

At this time, I see no reason why excavation work can not continue for your project.

If you have any questions or comments, please feel free to contact me at 526-8520.

Thank-you

Brenda L. Cole, Project Engineer Environmental Restoration

\blc

(4)) Westinghouse Idaho Nuclear Company. Inc. ?eF ta o- kr.:C.E :V LI re;t• L JAN 0 4 1991

Final Report

CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC,

Earth Science Laboratory

University of Utah Research Institule 391 Chipela Way, Suite C Salt Lake City. Utah 84108 (801) 524-3422

September, 1987

REF. VI iiLL - Cpp. o o isf-7/9 - o

Final Report

CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

September, 1987 o c - c FINAL REPORT c CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS

IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

TABLE OF CONTENTS

1.0 Introduction 1

2.0 Site Location 1

3.0 Site Geology 2

4.0 Sample Procedures 2

5.0 Analytical Procedures and Results 3

6.0 Data Quality 5

7.0 Evaluation of Results 6 o o

C). LIST OF FIGURES o ,d

Figure 1 Map of CPP facility showing location of

project area and background samples 7

Figure 2 Sample locations at the Chemical Storage

Area 8

Figure 3 Sample locations at the Zirconium Feed

Tank Storage Area 9

LIST OF TABLES

Table 1 Metal, nitrate, pH, and moisture contents

of samples 10

Table 2 Precision and accuracy data for

analyses 18

Table 3 Background concentrations from samples

taken in the vicinity of CPP 19

Table 4 Ranges of concentrations in volcanic

soils 20 LIST OF APPENDICES

Appendix 1 Chain of Custody forms 21

Appendix 2 Quality control data 26 1.0 INTRODUCTION

This report presents the results of a preliminary character- ization of potential soil contamination at the Chemical Storage

Area and the Zirconium Feed Tank Storage Area at the Idaho

Chemical Processing Plant (CPP complex; Fig. 1). The complex, managed by the Westinghouse Idaho Nuclear Company, Inc. (WINCO), is located approximately 50 miles west of Idaho Falls, Idaho.

The project was undertaken to identify the nature and levels of potential hazardous wastes that may have been spilled during the storage and transfer of chemicals at the Chemical Storage Areas.

The characterization is based on results from the chemical analysis of soil samples collected by personnel and associates of the University of Utah Research Institute (UURI) between April 13 and 16, 1987. In addition, analyses of drillcore collected by • WINCO personnel from the chemical storage area are given in this report. The analyses of these drillcore samples were performed according to EPA protocol and with approved methods. However, the drilling was not performed by UURI and UURI has no direct knowledge of the sampling procedures followed. Thus, drillcore data are presented for comparison only, and are not here represented aS being valid for submittal to EPA for regulatory

purposes.

2.0 SITE LOCATION

The Chemical Storage Area (Fig. 2) is approximately 130 feet

by 90 feet and encompasses the Chemical Storage Pump House o o

Cn (CPP-621), the Nitric Acid Storage Tank Area (CPP-719) and o adjacent sludge pit, the Aluminum Nitrate Storage Tank Area

(CPP-720), the Hydrofluoric Acid Storage Tank Area (CPP-727), the

Sulfuric Acid and Hydrochloric Acid Tank Area (CPP-759), and the chemical drain lines servicing these areas.

The Zirconium Feed Tank Storage Area (CPP-637) is located approximately 675 feet north-northwest of the main Chemical

Storage area. A 30 x 30 foot was sampled at this facility (Fig.

3).

3.0 SITE GEOLOGY

The sampling sites are underlain by sand, gravel and clay-

rich sediments which unconformably overlie basalt. The sediments

in nearby excavations on the CPP site are approximately 40 feet

thick. The thickness of the basalt has not been established. A

three foot thick clay horizon above the basalt was previously

sampled in one of the excavations and mineralogically analyzed at

UURI. X-ray diffraction analysis of this sample indicates that

it consists of approximately 25% quartz, 10% plagioclase, 5%

potassium feldspar, 15% smectite, 5% illite, 1% chlorite, 1%

kaolinite, and 36% glass.

4.0 SAMPLING PROCEDURE

The soil sampling techniques and procedures employed during

the project are described in the accompanying Quality

2 o o

Cn Assurance/Quality Control Sampling Plan (refer to Volume 1). -1 Soil sample locations are shown in Figs. 1 through 3.

Three background soil samples were collected from areas outside the CPP complex (Fig. 1) utilizing the same sampling techniques. Background Site 1 (samples 860258 and 860259) was located in an area approximately 300 feet southeast of the

wastewater treatment facility and 35 feet east of the dirt road.

Background Site 2 (samples 860260 and 860261) was located in an area approximately 730 feet east-northeast of the coal-fired steam plant. Background Site 3 (samples 860264 and 860265) was

located in an area west of the western CPP access road and 180

feet away from a white shack. Precise locations of these

background sites have been determined by WINCO personnel and are

available from them.

5.0 ANALYTICAL PROCEDURES AND RESULTS

Aluminum nitrate and various acids including nitric,

sulfuric, hydrofluoric, and hydrochloric acid, have been stored

at the Chemical Storage Area. The available data indicates that

aluminum nitrate and nitric acid have been discharged to the soil

through french drains as a result of spills and leaks. The

largest reported spill occurred in 1982, and involved

approximately 1200 gallons of nitric acid. The extent of leaks

or spills involving other chemicals at the Chemical Storage Area

is not known.

3 o o

Cn No detailed site history documenting the extent of chemical o

discharges to the ground in the Zirconium Feed Tank Storage Area

is available. However, 450 gallons of zirconium feed is reported

to have spilled from one of the tanks in November, 1978.

Based on this information, the samples collected during

this study were analyzed for soil pH, nitrate (NO3 -N), aluminum

(A1), and heavy metals which may have been discharged to the

soils or leached by the acids. These metals are barium (Ba),

chromium (Cr), lead (Pb), silver (Ag), zircon (Zr), mercury (Hg),

arsenic (As), and selenium (Se). Soil moisture was also

determined in order to relate the analytic concentrations,

determined on the basis of dry weight, to in-situ weight

concentrations.

5.1 Analytical Results

Analysis of the soils was performed by the University of

Utah Research Institute (UURI) located in Research Park at 391

Chipeta Way, Suite A, Salt Lake City, Utah. This laboratory is

certified in the State of Utah by the State Health Laboratory,

Bureau of Laboratory Improvement for the required metal analyses.

Utah is a "Primacy" state in which EPA RCRA programs are managed

at the state level by authorized state agencies. Chain of

Custody (COC) forms for samples submitted to this laboratory are

contained in Appendix 1.

The analytical results are presented in Table 1 and the

locations of the samples are shown in Figs. 2 and 3. Note that

4 o o values for moisture, Al and Ba are expressed as percentage levels Cn o ,d (%), Hg and Se are expressed in parts per billion (ppb), and the remaining elements are given in parts per million (ppm). A11 analyses are total constituent analyses and are reported on a weight per dry weight basis. The EPA-approved methods utilized for these analyses are listed in "Test Methods for Evaluating

Solid Wastes (SW-846), Second Edition Revised, EPA, April 1984

(refer to Vol. 1, Appendix 1).

6.0 DATA QUALITY

The accuracy and precision of the analyses were determined from a statistical evaluation of the quality control samples.

Accuracy data were obtained from the analysis of standard reference materials, spiked field samples and standards analyzed along with the project samples. Precision data were obtained from duplicate analyses of field samples and standards analyzed with project samples. Control limits for accuracy and precision

are nominally established by the EPA to be equal to the mean + 3 standard deviations. Quality control data for the analyses are

contained in Appendix 2. These data indicate that the analyses

fall within acceptable limits. A summary of the precision and

accuracy data for the analyses is presented in Table 2.

Soil samples are heterogeneous and thus present inherent

analytical problems. Often very small particles of a particular

contaminant may not be present uniformly throughout the sample

causing anomalies in data which must be verified through addi-

5 o o tional analysis. The UURI Laboratory performed many additional o analyses to confirm the accuracy of all data.

7.0 EVALUATION OF RESULTS

The results of the sample analyses have been statistically

compared to the concentrations found in the background samples

(Tables 3) to determine the distribution of anomalous values. o cr Concentrations exceeding a value equal to the background mean + 2

standard deviations are underlined in Table 1. For comparison

the range of metal contents typically found in soils over

volcanic rocks is shown in Table 4.

The data show that anomalous metal, F, and NO3 -N concentra-

tions in soil from the Chemical Storage Facility are found in

areas where the discharge of acids or aluminum nitrate is known

to have occurred. These areas include the french drains,

chemical trench, hydrofluoric acid containment area and the

sludge pit. In addition, the majority of the core samples

submitted for analysis are also enriched in NO3 -N. The highest

concentrations of NO3 -N in the core samples occur in the deepest

samples, suggesting that the nitrate has been leached downward.

Soil samples collected from the Zirconium Feed Tank Storage

Area contain anomalous concentrations of Zr (860242, 860243,

860246, 820251 to 860254, 860257), A1 (860251), Cr (860242,

860243, 860251) and As (860257).

6 X Bkg. (860258) (860259)

Bkg. (860260) X (860261)

100).14 •041

POCCUPOI

7-1909 Bkg. X (860264) (860265) F IGURE - 1 LO9T00 Sludge FD = French Drain Pit Sample Location CPP 621 * 232

230 200 * 201

204 205 228 217 229 FD 227 Al Nit a) 218, 219 19 FD F— rci 220, 221(i FD _c FD 222 224 223 0 225 209 210 Chemical Trench

211,213 208 212 214 Condensate Dry Well 0 206, 207

CPP 607

SCALE

0 10 20 Ft

Sample locations at the Chemical Storage Area FIGURE 2 247 244(245) 242 248 246 243

249 251 253(254) 250 252 257

Sample locations at the Zirconium Feed Tank Storage Area (CPP 637)

10' SCALE i 10'

• , Approximate location of zircon storage tanks

(222) Duplicate samples in parentheses

FIGURE 3 TABLE 1. Analytical Data

Sample Moisture NO3 - N Soil Sample ft Depth (%) (ppm) pH (ppm)

4-16 4.5' 4.01 0.24 9.11 4-19-2 18-20' 0.51 82.00 8.01 4-22-2 18-20' 4.73 256.00 6.57 4-23-1 8-10' 0.23 85.30 7.90 4-24A 13-15' 9.55 909.00 6.32 4-28 6' 1.69 8.73 4-30 4-5' 5.34 2.63 8.65 4-1-1 3-5' 1.51 29.40 8.45 4-3-1 8-10' 2.22 9.90 8.78 4-3-2 18-20' 0.67 7.55 4-8-2 13-15' 0.41 0.55 8.66 4-14 3' 0.33 1.57 8.37 4-17-2 18-20' 0.94 0.25 9.09 4-22-1 8-10' 4.62 6.30 8.38 4-37 3' 3.19 8.79 4-28 6' 1.69 8.73 4-5-2 18-20' 2.07 0.45 8.62 4-16 5' 2.27 <0.1 8.98 4-30 4-5' 5.34 2.63 8.65 4-34 4' 1.72 1.45 8.58 860200 0-4" 15.4 6990.00 2.80k 860201 24" 9.14 6910.00 3.07 860202 0-4" 5.99 3200.00 2.62 ti5C-' 860203 24" 5.77 636.00 2.58)k 860204 0-4" 0.85 140.00 3.91 L.860205 24" 4.17 3.59 5.34 860206 0-4" 3.88 0.58 8.57 860207 24" 5.96 0.23 8.48 860208 0-4" 0.59 9.29 30 860209 0-4" 11.6 2.79 2900 860210 0-4" 37.8 3.41 88 860211 0-4" 1.78 1.13 8.78 860212 0-4" 2.33 1.14 8.85 860213 24" 3.86 0.17 9.21 860214 24" 4.72 0.60 8.45 860215 0-4" 19.1 2.13 6.72 860216 24" 6.41 0.63 6.53 860217 24" 6.43 0.62 6.49

10 Sample Moisture NO3 AS N Soil Sample # Depth (%) (ppm) PH (ppm)

860218 0-4" 18.8 0.62 5.88 860219 24" 7.1 0.17 5.75 860220 0-4" 19.6 0.57 6.20 4) 860221 24" 6.48 0.58 7.06 AyT860222 0-4" 2.11 8.10 L860223 24" 4.67 9.04 860224 0-4" 1.68 8.48 860225 24" 4.92 5.45 8.51 0-4" 9.46 27.50 5.25-1 , 860227 24" 6.73 3.10 4.30 C7\--1 )4 :66:22:: 0-4" 0.72 1.51 8.64 C} 860229 24" 2.44 1.25 9.15 860230 0-4" 0.37 4.12 7.56 I° (I 24" 2.02 1.12 8 860232 0-4" 34.9 8720.00 3.30 SaLaits6 \At- * 860233 0-4" 1.16 8.05 86024 24" 2.74 0.16 8.67 86025 0-4" 0.47 0.44 8.15 86026 24" 9.46 0.46 8.85 860242 0-4" 0.082 860243 24" 6.97 860244 0-4" 0.33 860245 0-4" 0.35 860246 24" 7.7 860247 0-4" 2.02 860248 24" 5.53 860249 0-4" 1.28 860250 9" 3.93 860251 0-4" 9.34 860252 24" 8.06 860253 0-4" 0.71 860254 0-4" 0.6 860255 blank 0.40 6.10 860257 24" 11.8 860258 0-4" 1.41 0.86 6.59 0.15 860259 24" 2.69 0.72 7.88 0.32 860260 0-4" 2.74 0.41 6.65 0.12 860261 24" 2 0.43= 7.99 0.42 860264 0-4" 3.19 0.27 7.30 4.00 860265 24" 2.78 0.25 8.29 0.28 Sludge Pit 3.5' 18.8 5200.00 2.61 Sludge Pit 2.5' 46.7 6080.00 2.55

11 Sample # Depth Al(%) Da(%) Cr(ppm) Pb(ppm) 4-16 4.5' 0.913 0.017 25 <10.0 4-19-2 18-20' 0.818 0.015 20 <10.0 4-22-2 18-20' 1.330 0.015 25 <10.0 4-23-1 8-10' 0.788 0.016 11 <10.0 4-24A 13-15' 3.100 0.017 25 <10.0 4-28 6' 0.975 0.028 33 <10.0 4-30 4-5' 1.080 0.020 24 <10.0 4-1-1 3-5' 4-3-1 8-10' 0.727 0.039 18 <10.0 4-3-2 18-20' 0.860 0.012 21 <10.0 4-8-2 13-15' 4-14 3' 4-17-2 18-20' 4-22-1 8-10' 4-37 3' 4-28 6' 4-5-2 18-20' 4-16 5' 4-30 4-5' 4-34 4' 60200 0-4" 0.938 0.010 13 <10.0 60201 24" 0.798 0.008 8 <10.0 860202 0-4" 0.442 0.031 25 <10.0 860203 24" 0.285 0.007 10 <10.0 860204 0-4" 0.746 0.021 33 97 mt 860205 24" 0.625 0.010 15 <10.0 860206 0-4" 0.863 0.021 29 62 860207 24" 0.601 0.018 13 <10.0 860208 0-4" 860209 0-4" 860210 0-4" 860211 0-4" 860212 0-4" 860213 24" 860214 24" 860215 0-4" 1.050 0.023 26 14 860216 24" 1.340 0.029 40 <10.0 860217 24" 1.260 0.017 23 <10.0 860218 0-4" 1.930 0.017 50 16 860219 24" 1.060 0.015 17 <10.0 860220 0-4" 1.210 0.014 32 20 5 860221 24" 1.120 0.047 29 <10.0 k.)• 860222 0-4" cO L860223 24" 860224 0-4" ,860225 24" 860226 0-4" 0.399 0.026 9 <10.0 860227 24" 0.398 0.026 10 <10.0 860228 0-4"

12 860229 24" 860230 0-4" Sample ample # Depth Al(%) Be(%) Cr(ppm) Pb(ppm) 60231 24" 860232 0-4" 6 090* <.001 9 <10.0 szoi...Q0 860233 0-4" 86024 24" 86025 0-4" 86026 24" 860242 0-4" 0.734 0.015 41 <10.0 860243 24" 1.200 0.020 43 <10.0 860244 0-4" 0.425 0.008 17 <10.0 860245 0-4" 0.473 0.013 16 <10.0 860246 24" 1.370 0.016 37 <10.0 860247 0-4" 0.870 0.018 22 <10.0 860248 24" 0.956 0.018 24 <10.0 860249 0-4" 0.759 0.033 23 <10.0 860250 9" 1.170 0.025 25 <10.0 860251 0-4" 2.120 0.032 139 <10.0 860252 24" 1.240 0.026 31 <10.0 860253 0-4" 0.327 0.005 23 <10.0 860254 0-4" 0.251 0.005 22 <10.0 860255 blank <0.5 <0.5 <0.04 <0.2 860257 24" 1.470 0.033 40 <10.0 860258 0-4" 1.310 0.028 28 <10.0 860259 24" 0.812 0.038 26 <10.0 860260 0-4" 1.550 0.024 28 <10.0 860261 24" 0.788 0.022 18 <10.0 860264 0-4" 1.600 0.023 28 <10.0 860265 24" 0.748 0.021 20 <10.0 Sludge Pit 3.5' 2.320 0.009 27 <10.0 Sludge Pit 2.5' 5.840 <0.001 <5.0 <10.0

13 Sample Sample # Depth Cd(ppm) Ag(ppm) Zr(ppm) Hq(ppb) 4-16 4.5' <5.0 <2.0 9 4-19-2 18-20' <5.0 <2.0 <5.0 4-22-2 18-20' <5.0 <2.0 <5.0 4-23-1 8-10' <5.0 <2.0 7 4-24A 13-15' <5.0 <2.0 <5.0 4-28 6' <5.0 <2.0 12 4-30 4-5' <5.0 <2.0 14 42 4-1-1 3-5' 4-3-1 8-10' <5.0 <2.0 8 46 4-3-2 18-20' <5.0 <2.0 8 4-8-2 13-15' 4-14 3' 4-17-2 18-20' 4-22-1 8-10' 4-37 3' 4-28 6' 4-5-2 18-20' 4-16 5' 4-30 4-5' 42 4-34 4' 860200 0-4" <5.0 <2.0 9 <50 860201 24" <5.0 <2.0 <5.0 <50 860202 0-4" <5.0 <2.0 8 <50 860203 24" <5.0 <2.0 <5.0 <50 860204 0-4" <5.0 <2.0 9 <50 860205 24" <5.0 <2.0 9 <50 Cill860206 0-4" <5.0 <2.0 12 <50 860207 24" <5.0 <2.0 <5.0 <50 860208 0-4" 25 860209 0-4" 14 860210 0-4" 59 860211 0-4" 55 860212 0-4" 56 860213 24" 82 860214 24" 14 860215 0-4" <5.0 <2.0 16 2340 860216 24" <5.0 <2.0 9 428 860217 24" <5.0 <2.0 <5.0 439 860218 0-4" <5.0 <2.0 10 2040 860219 24" <5.0 <2.0 -7 495 860220 0-4" <5.0 <2.0 8 697 860221 24" <5.0 <2.0 <5.0 <50 :5 F860222 0-4" 66* fr L860223 24" 25 860224 0-4" 48 860225 24" 19 860226 0-4" <5.0 <2.0 7 <50 {860227 24" <5.0 <2.0 <5.0 <50 860228 0-4" 47

14 860229 24" 25 860230 0-4" 38 Sample Sample # Depth Cd(ppm) Ag(ppm) Zr(ppm) Hg(ppb) 41.860231 24" 21 4.) ) A: '0 860232 0-4" <5.0 <2.0 8 109 t9.1.4%,A dk- 860233 0-4" 37 86024 24" 21 86025 0-4" 23 86026 24" 20 860242 0-4" <5.0 <2.0 123 860243 24" <5.0 <2.0 174 860244 0-4" <5.0 <2.0 7 860245 0-4" <5.0 <2.0 6 860246 24" <5.0 <2.0 85 860247 0-4" <5.0 <2.0 <5.0 860248 24" <5.0 <2.0 6 860249 0-4" <5.0 <2.0 <5.0 860250 9" <5.0 <2.0 7 860251 0-4" <5.0 <2.0 15762 860252 24" <5.0 <2.0 18 860253 0-4" <5.0 <2.0 129 860254 0-4" <5.0 <2.0 161 860255 blank <0.05 <0.04 <0.1 <0.001 860257 24" <5.0 <2.0 14 860258 0-4" <5.0 <2.0 <5.0 25 860259 24" <5.0 <2.0 10 57 860260 0-4" <5.0 <2.0 9 23 860261 24" <5.0 <2.0 12 30 860264 0-4" <5.0 <2.0 7 21 860265 24" <5.0 <2.0 10 46 Sludge Pit 3.5' -- <5.0 <2.0 12 Sludge Pit 2.5' <5.0 <2.0 6

15 Sample Sample # Depth As(ppm) Se(ppb) 4-16 4.5' 7.6 329 4-19-2 18-20' 3.2 190 4-22-2 18-20' 4.6 194 4-23-1 8-10' 5.0 654 4-24A 13-15' 6.0 148 4-28 6' 5.8 292 4-30 4-5' 5.6 243 4-1-1 3-5' 4-3-1 8-10' 7.8 963 4-3-2 18-20' 8.0 289 4-8-2 13-15' 4-14 3' 4-17-2 18-20' 4-22-1 8-10' 4-37 3' 4-28 6' 292 4-5-2 18-20' 4-16 5' 4) 4-30 4-5' 243 4-34 4' 860200 0-4" 3.8 218 860201 24" 3.0 121 860202 0-4" 7.6 549 860203 24" 3.8 423 4 860204 0-4" 6.2 330 60205 24" 5.8 241 860206 0-4" 14.0 926 860207 24" 5.6 450 860208 0-4" 860209 0-4" 860210 0-4" 860211 0-4" 860212 0-4" 860213 24" 860214 24" 860215 0-4" 6.5 218 860216 24" 6.3 250 860217 24" 6.6 199 860218 0-4" 7.2 161 860219 24" 6.4 293 860220 0-4" 6.8 188 #0 860221 24" 5.8 362 ,,,N, p60222 0-4" 860223 24" 860224 0-4" 860225 24" 42 1 r860226 0-4" 3.8 329 43 860227 24" 2.4 329 860228 0-4"

16 860229 24" 860230 0-4" Sample liample # Depth As(ppm) Se(ppb) L860231 24" 860232 0-4" <1.0 101 cla.A4-ct#52_ e-kt 860233 0-4" 86024 24" 86025 0-4" 86026 24" 860242 0-4" 3.0 38 860243 24" 5.6 107 860244 0-4" 1.8 78 860245 0-4" 4.0 53 860246 24" 4.4 72 860247 0-4" 7.0 141 860248 24" 6.8 45 860249 0-4" 5.4 20 860250 9" 8.0 23 860251 0-4" 1.6 48 860252 24" 6.0 31 860253 0-4" 1.4 51 860254 0-4" 1.6 81 860255 blank <0.001 860257 24" 15.0 48 860258 0-4" 5.6 113 860259 24" 7.6 252 860260 0-4" 6.4 695 860261 24" 6.2 236 860264 0-4" 6.0 102 860265 24" 7.6 227 Sludge Pit 3.5' 4.4 215 Sludge Pit 2.5' 1.0 153

17 TAsLs 2

Precision and accuracy data for analyses.

PRECISION DATA ACCURACY DATA

% MEAN RELATIVE 95% % MEAN RELATIVE 95% RECOVERY ST.DEV.(%) CONFID. RECOVERY ST.DEV.(%) CONFID.

A1 99.6 1.6 4.8 100 3.5 10.5

As 100.4 3.9 11.7 100 1.1 3.3

Be 98.2 1.9 5.7 100 3.1 9.3

Cd 100.7 4.1 12.3 100 0.7 2.1

Cr 101.6 3.4 10.2 100 7.1 21.3

Pb 98.8 4.6 13.8 100 4.9 14.7

Hg 100.5 9.0 27.0 100 7.2 21.6

Se 98.2 7.5 22.5 100 7.5 22.5

Ag 97.6 5.1 15.3 100 0.9 2.7

Zr 100.5 7.4 22.2 100 0.7 2.1

NO3 100.1 2.9 8.7 100 3.3 9.9 - N

F 100.9 4.4 13.2 100 2.1 6.3

18 TABLE 3

Background concentrations of NO3-11, F, Al, Ba, Cr, Pb, Cd, Ag, Zr, Hg, As, and Se in soil sampled from locations outside of the CPP complex.

NO3-N F Al Ba Cr Pb Cd Ag Zr Hg As Se SAMPLE (ppm) (%) (%) (ppm) (ppm) (ppm) (ppm) (ppm) (ppm) (ppm) (ppb)

Bkg 1' 200 25 12 <5 <2 43 5.6 484

Bkg 270 32 16 <5 <2 19 5.1 405

Bkg 34 270 33 17 <5 <2 27 6.5 467

Bkg 44 250 34 12 <5 (2 28 7.0 341

860258 0.86 0.15 1.31 280 28 <10 <5 <2 <5 25 5.6 113

860259 0.72 0.32 0.81 380 26 <10 <5 <2 10 57 7.6 252

860280 0.41 0.12 1.60 240 28 <10 (5 (2 9 23 6.4 695

860261 0.43 0.42 0.79 220 18 <10 <5 <2 12 30 6.2 236

860264 0.27 4.00 1.60 230 28 <10 <5 <2 7 21 6.0 102

860265 0.25 0.28 0.75 210 20 <10 <5 <2 10 46 7.6 227

Average (X) 0.49 0.88 1.14 255 27 12 <5 (2 9 32 6.4 332

St.Dev.(s.d.) 0.25 1.53 0.41 51 5 3 2 13 0.8 184

X f 2(s.d.) 0.98 3.94 1.96 358 38 17 14 57 8.0 701

A. Refer to Final Report: FPR karehous Site, Idaho Chemical Processing Plant: Earth Science Laboratory, Sept. 1986 for the locations of samples Bkg 1 to 4.

lc, EP T,A

19 TABLE 4

Ranges of average concentrations in ppm of Cr, Ni, As, Se, Ag, Cd, Pb, and Ba and in ppb of Hg in soil overlying volcanic terrains.

ELEMENT RANGE MEAN

Cr 20-700 85 Ni 7-150 30 As 2.1-11.0 5.9 Se 0.1-0.5 0.2 Ag 0.01-8.0 Cd 0.1-0.5 Hg 10-180 50 Pb 10-70 20 Ba 500-1500 770 A1 0.45-10% Zr 70-500 195

Data on Cr, Ni, As, Se, Ag, Hg, Pb, Ba from Kabata-Pendias, A., and Pendias, H., 1984, Trace elements in soils and plants: CRC Press, Inc., Boca Raton, Florida, 315 p.

Data on Cd from Wakita, H., and Schmitt, R. A., 1978, Behavior during weathering and alteration of rocks in Handbook of Geochemistry, Wedepohl, K. H., ed., Springer-Verlag, New York, N. Y., p. 48-G-1.

20 .L -L

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Ag ACCURACY

DATE TYPE MEAS. TRUE REC%

1 28-Jul-86 ST 50.0 50.0 100.0 2 28-Jul-86 ST 50.0 50.0 100.0 3 28-Jul-86 ST 51.0 50.0 102.0 4 28-Ju1-86 ST 50.0 50.0 100.0 5 09-Dec-86 SP 2.2 2.1 101.4 6 09-Dec-86 ST 2.1 2.0 103.0 7 29-Apr-87 ST 2.0 2.0 100.0 8 06-Jun-87 ST 99.0 100.0 99.0 9 06-Jun-87 ST 101.0 100.0 101.0 10 06-Jun-87 SP 94.0 100.0 94.0 11 06-Jun-87 SP 89.0 100.0 89.0 12 24-Jun-87 ST 99.0 100.0. 99.0 13 24-Jun-87 SP 94.0 100.0 94.0 14 24-Jun-87 ST 101.0 100.0 101.0 15 24-Jun-87 SP 91.0 100.0 91.0 16 24-Jun-87 ST 99.0 100.0 99.0 17 24-Jun-87 SP 85.0 100.0 85.0 18 ERR 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

26 5WECUVIVY' 115 120 100 105 110 90 95 96 gs LIFWEP - 1 2 DOWTP0.1 ,... 3 4 5 5 ;" 8 SLYER 9 SAUTLE 27 AMLIPACY 146.4.9 10 11 12 NJ 13 14 t 1 1 1 PPEP 1 1 15 1 1 r i i 16 r CO6T70C 1 1 1 1 11 1 1 1 1 1 '1 17 1 9

1 9

20 SILVER PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 24-Jun-87 REP 101 99 101.0 99.0 2 24-Jun-87 REP 99 99 100.0 100.0 3 24-Jun-87 REP 101 99 101.0 99.0 4 ERR ERR 5 ERR ERR 6 ERR ERR 7 ERR ERR 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

28 SILVEP PPECISILIU 120

115

110

105

gs

90

115

BO 1 2 3 5 5 9 10

GAO LE Ld EA.111 DIYHEP (1114TPOL PPEP COILITPOL

29 A1 ACCURACY

DATE TYPE MEAS. TRUE REC%

1 09-Dec-86 SP 8.8 8.6 102.3 2 09-Dec-86 ST 8.2 8.0 102.5 3 29-Apr-87 ST 7.9 8.0 98.8 4 29-Apr-87 SP 12.4 12.3 100.8 5 06-Jun-87 ST 0.4 0.4 99.8 6 06-Jun-87 ST 0.4 0.4 99.3 7 06-Jun-87 SP 1.7 1.8 96.7 8 06-Jun-87 SP 1.1 1.1 99.1 9 24-Jun-87 ST 0.4 0.4 97.5 10 24-Jun-87 SP 1.6 1.6 99.4 11 24-Jun-87 ST 0.4 0.4 100.0 12 24-Jun-87 SP 1.2 1.2 99.5 13 24-Jun-87 ST 0.4 0.4 100.2 14 24-Jun-87 SP 6.1 6.3 98.2 IS ERR 16 ERR 17 ERR 18 ERR 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

30 ALE11410 Ltd 41:1:11 PAZ( 120

1 1 —

45

40

05 —1

80 1 2 3 4 5 5 r 8 9 10 11 12 13 14 15 15 17 18 19 20

&MAPLE O 1.001EP 131}14T — Lt LL14 UPPEP C414TP.0=1.

31 ALUMINIUM PRECISION

DATE TYPE MEAS. 1 MEAS.2 RECX1 RECX2

29-Apr-87 REP 4.3 4.2 101.2 98.8 06-Jun-87 REP 1.38 1.34 101.5 98.5 3 06-Jun-B7 REP 0.695 0.643 103.9 96.1 4 24-Jun-87 REP 1.17 1.13 101.7 98.3 5-, 24-Jun-87 REP 0.748 0.704 10:c. 0 97.0 6 24-Jun-87 REP 5.84 5.78 100.5 99.5 7 24-Jun-87 REP 0.87.9 0.812 101.6 98.4 8 24-Jun-87 REP 0.788 0.728 104.0 96.0 9 24-Jun-87 REP 1.46 1.26 107.4 9?.6 10 24-Jun-87 REP 0.748 0.695 103.7 96.3

n MEAN s LCL UCL 20.0 100.0 3.5 89.5 110.5

zz ALUM W111141 PPEDISlek 120

115

110 - — — 1

105 — -J _ ----- — --- --

95

90 --

115 —

BO 3 5 15 IdSPtE UEAW LOWE P W TNA PPEP DINH!sgt

33 c c tea. c. MERCURY PRECISION c

DATE TYPE MEAS.1 MEAS.2 REC7.1 RECX2

1 24-Jun-27 REP 264 256 101.5 99.5 2 24-Jun-97 REP 38 89.2 111.8 - 24-Jun-07 REP ;: 103.6 94.4 4 24-Jun-87 REP 27 ,.., 96.4 103.6 5 24-Jun-S7 REP 29 29 100.0 100.0 6 24-Jun-87 REP 61 59 101.7 98.3 7 24-Jun-37 REP 78 74 102.6 97.4 8 24-Jun-B7 REP 38 30 111.9 98.2 9 24-Jun-87 REP 29 27 103.6 96.4 10 24-Jun-87 REP 19 17 105.6 94.4

n MEAN s LCL UCL 20 -00 100 6 92 118

73 Ba ACCURACY

DATE TYPE MEAS. TRUE REC%

1 06-Jun-87 SP 0.04 0.04 100.0 2 24-Jun-87 ST 0.02 0.03 96.0 3 24-Jun-87 SP 0.05 0.05 99.0 4 24-Jun-87 ST 0.03 0.03 100.0 5 24-Jun-87 SP 0.04 0.05 96.7 6 24-Jun-87 ST 0.03 0.03 100.0 7 24-Jun-87 SP 0.02 0.03 96.0 8 ERR 9 ERR 10 ERR 11 ERR 12 ERR 13 ERR 14 ERR 15 ERR 16 ERR 17 ERR 18 ERR 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

34 ROLM AJt1114..CY 120

115

110 -I

105 a T /

1 MI

95

90 -

95 -

90 1 2 3 4 6 1 n 11 12 13 14 15 15 17 18 19 20

3.419LE 0 LOWEP. L931i1T9•04_ JODY .2.1 11 P PEP C•041T17.0L

35 BARIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 28-Jul-86 REP 310 320 98.4 101.6 2 28-Jul-86 REP 320 330 98.5 101.5 3 28-Jul-86 REP 300 300 100.0 100.0 4 28-Jul-86 REP 250 250 100.0 100.0 5 11-Dec-86 REP 2.22 2.27 98.9 101.1 6 11-Dec-86 REP 3920 4090 97.9 102.1 7 11-Dec-86 REP 2.48 2.53 99.0 101.0 8 06-Jun-87 REP 0.029 0.03 98.3 101.7 9 06-Jun-87 REP 0.016 0.019 91.4 108.6 10 24-Jun-87 REP 0.024 0.025 98.0 102.0

n MEAN s LCL UCL 20.0 100.0 3.1 90.7 109.3

BARIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 24-Jun-87 REP 0.021 0.02 102.4 97.6 2 ERR ERR 3 ERR ERR 4 ERR ERR S ERR ERR 6 ERR ERR 7 ERR ERR 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

BARIUM PRECISION

16 PPECISION 120

115

11 0 -dr i lr -7.., ...,..

105 ...... _ -- 1 00 ____ _ UN -..------.., ...... a ... 95

so r •

85

eu 2 3 4 5 C 10

1.16PLE LOWT.P. C1041701.11. a. 11 PPER 0:951.11.001

37 Cr ACCURACY

DATE TYPE MEAS. TRUE REC%

1 28-Jul-86 ST 49.0 50.0 98.0 2 28-Jul-86 ST 50.0 50.0 100.0 3 28-Jul-86 ST 50.0 50.0 100.0 4 28-Jul-86 ST 50.0 50.0 100.0 5 28-Jul-86 SP 63.0 60.0 105.0 6 28-Ju1-86 SP 53.0 51.0 103.9 7 28-Jul-86 SP 58.0 53.5 108.4 8 28-Jul-86 SP 67.0 63.5 105.5 9 28-Jul-86 SP 53.0 50.0 106.0 10 09-Dec-86 SP 2.0 2.0 100.0 11 09-Dec-86 ST 2.1 2.0 103.5 12 29-Apr-87 ST 2.0 2.0 98.5 13 29-Apr-87 SP 2.3 2.2 106.0 14 24-Jun-87 ST 100.0 100.0 100.0 15 24-Jun-87 SP 123.0 125.0 98.4 16 24-Jun-87 ST 100.0 100.0 100.0 17 24-Jun-87 SP 114.0 119.0 95.8 18 24-Jun-87 ST 100.0 100.0 100.0 19 24-Jun-87 SP 133.0 130.5 101.9 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

38 FiF.SC at'gr ❑ 110 120 115 195 1 85 90 BS BO BO LOWE - - 1 P 2 DOMTPH 3 4 5 6 CH110411114 q S+YIPLE

39 LILO 1n ACCI1PAC? 11 12 13 14 UPPEP 15 16 CONTPC11. 17 19 19 2n CHROMIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 28-Jul-86 REP 40 40 100.0 100.0 2 28-Jul-86 REP 28 28 100.0 100.0 3 28-Ju1-86 REP 35 34 101.4 98.6 4 28-Jul-86 REP 34 33 101.5 98.5 5 29-Apr-87 REP 0.15 0.14 103.4 96.6 6 06-Jun-87 REP 40 30 114.3 85.7 7 06-Jun-87 REP 23 17 115.0 85.0 8 24-Jun-87 REP 25 25 100.0 100.0 9 24-Jun-87 REP 20 18 105.3 94.7 10 24-Jun-87 REP 31 30 101.6 98.4

n MEAN s LCL UCL 20.0 100.0 7.1 78.8 121.2

40 gincovsvc 11 1 130 120 90 70 BO OD 0 - 2 3 LO'REP CO 4 T PAR HUHU 41 1114114 5 P P LE PECIS 5 'th PPEP ti, DINITPOL ,t 9 1 0 Cd ACCURACY

DATE TYPE MEAS. TRUE REC%

1 28-Jul-86 ST 50.0 50.0 100.0 2 28-Jul-86 ST 50.0 50.0 100.0 3 28-Jul-86 ST 51.0 50.0 102.0 4 28-Jul-86 ST 50.0 50.0 100.0 5 28-Jul-86 SP 20.0 20.0 100.0 6 09-Dec-86 SP 2.1 2.0 104.0 7 09-Dec-86 ST 2.1 2.0 105.0 8 29-Apr-87 ST 1.9 2.0 95.0 9 06-Jun-87 ST 100.0 100.0 100.0 10 06-Jun-87 ST 100.0 100.0 100.0 11 06-Jun-87 SP 100.0 100.0 100.0 12 06-Jun-87 SP 114.0 100.0 114.0 13 24-Jun-87 ST 99.0 100.0 99.0 14 24-Jun-87 SP 98.0 100.0 98.0 15 24-Jun-87 ST 100.0 100.0 100.0 16 24-Jun-87 SP 96.0 100.0 96.0 17 24-Jun-87 ST 99.0 100.0 99.0 18 24-Jun-87 SP 100.0 100.0 100.0 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

42 CADS] II A =I rate 120

115

I t I I 'i 110 1 1 I 1 1 . i 105 ll II I i I / .1 II

95

90

95

an 7 3 4 5 fi 7 9 10 11 12 13 14 15 15 17 19 19 2n

`aka P LE O 1269itt! CONTROL "CAN PPEP. C.-{WTP131

43 CADMIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 24-Jun-87 REP 101 99 101.0 99.0 2 24-Jun-87 REP 100 99 100.5 99.5 3 24-Jun-87 REP 100 100 100.0 100.0 4 ERR ERR 5 ERR ERR 6 ERR ERR 7 ERR ERR 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

44 NPLCQVGIT' 115 105 120 110 1 00 90 95 B5 BO - — — — — — — 2 3 LOWE P COPT it CALL11014 POL SAbitIPLE 5 45 PPEDISIOW L. ,

PPCP B T P .13t 9 10 NRGCOVEVY 0 100 110 105 120 115 05 0 90 gs 11 LOY101 - - — 1 1 a DDMTPOL I I 1 I 1 I 3 • i l. . 1 . 4 i 5 5 . 7 1 0 LEAD 9 4 1.1.411PLE 6 1 ACC 10 I LIPAC - 11 . . 12 13 _ 14 . UPPEP 15 . 15 CD.4TP4L 17 .... 113 .

.. 19 20 Pb ACCURACY

DATE TYPE MEAS. TRUE REC%

1 28-Jul-86 ST 49 50 98.0 2 28-Jul-86 ST 45 50 90.0 3 28-Jul-86 ST 53 50 106.0 4 28-Jul-86 ST 49 50 98.0 5 28-Jul-86 SP 51 47.5 107.4 6 28-Jul-86 SP 34 33 103.0 7 28-Jul-86 SP 44 43 102.3 8 28-Jul-86 SP 40 41 97.6 9 10-Aug-86 SP 36 40 90.0 10 10-Aug-86 ST 49.6 50 99.2 11 09-Dec-86 SP 2 2.07 96.6 12 09-Dec-86 ST 2.1 2 105.0 13 11-Dec-86 SP 228 234.5 97.2 14 11-Dec-86 ST 196 200 98.0 15 11-Dec-86 SP 196 207 94.7 16 11-Dec-86 ST 200 200 100.0 17 29-Apr-87 ST 2 2 100.0 18 24-Jun-87 ST 99 100 99.0 19 24-Jun-87 SP 94 100 94.0 20 24-Jun-87 ST 100 100 100.0

n MEAN s LCL UCL 20.0 98.8 4.6 85.0 112.6

Pb ACCURACY

DATE TYPE MEAS. TRUE REC%

1 24-Jun-$7 SP 95 100 95.0 2 24-Jun-87 ST 100 100 100.0 3 24-Jun-87 SP 81 100 - 81.0 4 ERR 5 ERR 6 ERR 7 ERR

4 7 NRGCVV:E{

--

115

110

120 105

100

95

85

90

rso

IiEAJd

2

/

3

LO9NER

COW

4

T

KN.

15-01.0.

fQ16,1811

48

PRECISION

9

PPEP.

DORTP.OL

9 LEAD PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 28-Jul-86 REP 17 18 97.1 102.9 2 28-Jul-86 REP 32 33 98.5 101.5 3 28-Jul-86 REP 11 13 91.7 108.3 4 10-Aug-86 REP 16 19 91.4 108.6 S 11-Dec-86 REP 267 270 99.4 100.6 6 11-Dec-86 REP 52.8 54.3 98.6 101.4 7 11-Dec-86 REP 196 200 99.0 101.0 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

49 21.5.E.50+41 US IC DI PAM' 211 1 I I 1 1 115 -I I I i il

110 i 1 11 1 1 1 105 —1 i , I 1 rig [II 60 I

I I I I

E5 —

Ea - -1 2 .3 4 5 ; 10 11 12 13 14 15 15

5A5IPLE LOWL.1.1 MCP% — tiEd+.14 1100E5 0.1051.PAIL

50 ZIRCONIUM ACCURACY

DATE TYPE MEAS. TRUE REC%

1 24-Jun-87 ST 98.0 100.0 98.0 2 24-Jun-87 SP 100.0 106.5 93.9 3 24-Jun-87 ST 100.0 100.0 100.0 4 24- Jun-87 SP 97.0 100.0 97.0 5 24-Jun-87 ST 99.0 100.0 99.0 6 24-Jun-87 SP 115.0 100.0 115.0 7 ERR 8 ERR 9 ERR 10 ERR 11 ERR 12 ERR 13 ERR 14 ERR 15 ERR 16 ERR 17 ERR 18 ERR 19 ERR 20 ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

51 11PC*101.111.1 PPLC2111111

115 --I

1

105

g5 _

_

BS H

-r- , i 2 4 5

;4W1 P LE -- LOW:: MMTPOL 1.1 p PE P E`..{;51211-1.

52 ZIRCONIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 24-Jun-87 REP 99 99 100.0 100.0 2 24-Jun-87 REP 100 98 101.0 99.0 3 24-Jun-87 REP 100 99 100.5 99.5 4 ERR ERR 5 ERR ERR 6 ERR ERR 7 ERR ERR 8 ERR ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

53 F ACCURACY

DATE TYPE MEAS. TRUE REC%

..)9-Dt?c-36 ST 1.0 1.0 100.0 09-Dec-86 ST 1.0 1.0 92.0 09-Dec-26 ST 1.0 1.0 101.0 09-Dec-86 ST 1.0 1.0 98.0 09-Dec-86 ST 1.0 1.0 101.0 09-Dec-86 ST 1.0 1.0 95.0 14-jan-27 ST 1.0 1.C) 100.0 14-Jan-87 ST 1.0 1.0 100.0 9 14-Jan-87 ST 0.5 0.5 106.0 10 14-Jan-87 ST 1.0 1.0 97.0 11 14-Jan-27 ST 1.C) 1.0 100.0 12 04-Apr-87 ST 1.0 1.0 99.0 1: 06-Jun-87 ST 1. 0 1.0 101.0 14 06-Jun-87 ST 1.0 1.0 100.0 15 06-Jun-87 ST 1.0 1.0 102.0 16 06-Jun-87 ST 1.2 1.0 115.0 17 ERR la ERR 9 ERR 20 ERR

n MEAN LCL urL 20.0 EF:R ERR ERR ERR

54 %RECOVERY 0 110 105 120 115 100 90 95 80 85 LOWER 1 ',.., 2 CONTROL / A 3 \ \ 4 / 7., 5 \ \ \ 6 / / _ FLUORIDE 8 ' / / / 1 \ 9 I SAMPLE

\

1 55 \ 11/". 10 MEAN ACCURACY 11 12 13 -___, A 14 ,--- UPPER ..- 15 16 CONTROL 17 18 19 20 FLUORIDE PRECISION

DATE TYPE MEAS.1 MEAS.2 REC%1 REC%2

1 REF 15 15.5 98.4 101.6 2 14-Jim-97 REF 0.57 0.59 94.6. 105.4 7 14Jan-97- REP 2 100.0 4 14-Jan-87 REP 3.55 =:(;)7 99,3 5 14-Jan-87 REP 4.1 4 101.2 99.8 6 14-Jan-27 REP 85 as 101.7 7 14-Jan-87 REP 7.5 3.4 1r,: ,; 98.6 8 06-Jun-87 2.6 2.7 98.1 101.9 9 06-jun-87 o.9e 1 101.0 10 06-Jun-87 4.95 4.9 X:gi 99.5

MEAN s LCL UCL 100.0 2.1 93.6 106.4.

FLUORIDE PRECISION

DATE TYPE MEPIS.1 MEAS.2 RFC%1 REC7,2

1 06-Jun-67 4 4.5 94.1 105.9 2 06-Jon-27 96 3.8 102.1 97.9

56 %RECOVERY — 110 100 115 105 120 85 90 95 80 MEAN - i- ---,, ------2 N/ / ., / N 3 LOWER ,______CONTROL 4 I FLUORIDE - SAMPLE 5 1"---- 57 „..- PRECISION ------„. -1... 4 o I --. --, ------.. t A L. , URPEP „------1--- 8 I CONTROL 1 ____------, 10 %RECOVERY O 120 100 110 130 80 90 70 LOWER - - - -41 1 ` a 2 CONTROL 3 4 5 6 SELENIUM a 8 -4 9 SAMPLE

58 10 MEAN ACCURACY 11 12 13 14 UPPER 15 16 a CONTROL 17 18 19 a.. 20 Se ACCURACY

DATE TYPE MEAS. TRUE REM.

1 10-flo...71-2.6 5;7 1.1 I. -.0 10-Auq-26 ST 2.0 2.0 100.0 10-Aug-86 ST 2.0 2.0 102.6 4 Icy-Aus-86 sT 3.1 3.0 103.3 S 10-Aug-86 ST 4.1 4.0 102.5 6 10-Aug-86 ST 3.9 4.0 57.5 7 1.0-Au9-86 ST 4.8 5.0 96.0 8 10-Auq-86 SP 660.0 593.0 111.3 9 10-Au9-86 SP 597.0 637.0 93.4 10 10-Aug-86 SP 732.0 826.0 88.6 11 10-Au5-86 SF' 766.0 782.0 98.0 12 10-Au9-86 SP 653.0 690.0 94.6 13 09-nec-96 SE 3.2 106.7 14 29-Apr-87 ST 0::(7:11 100.0 15 06-Jun-27 ST 1;-_)?10 10.0 100.0 16 06-Jun-87 ST 18.6 20.0 93.0 17 06-Jun-87 ST 30.8 30.0 102.7 18 06-Jun-87 360.0 418.0 86.1 17 Ok-jun-S7 SP 511.0 556.0 97.1 20 06-Jun-87 SP 17.0 50.9 81.3

n MEAN s LCL UCL 20.0 98.2 7.5 75.8 120.7

oe ACCURACY

DATE TYPE MEAS. TRUE R5C74

1 06-Jun-87 SP 55.2 10.0 84.0 06-Jun-87 28.6 127.1 6-Jyn-S7 SR 575.0 449.0 127.4 4 24-J6n-27 SP 57.6 27.2 101.5 5 24-Jun-87 SF' 29.9 35.9 74.9 6 24-Jun-87 SP 40.6 41.4- 92.1 7 24-Jun-27 SP 21.0 22.7 72.5

59 %RECOVERY 100 120 110 130 80 90 70 MEAN - I r ------.-"'-----, _,.---- _,,,,,_ a 2 -,--"'- --- 0 - .--'''. 3 LOWER -.-...,_, _.,____------__,_ '-'------CONTROL 4 2 SELENIUM __ _---- SAMPLE -VVV- 5 a 60 PRECISION c 2 A a UPPER 8 a CONTROL _------______---c: -----____ 9 a 10 2 Se PRECISION

DATE TYPE MEA9.1 MEAS.2 REC7:1 RECX2 ------10-Aug-96 REP 306 392 87.7 112.3 10-Oug-84 REP 731 964 91.7 108.3 10-Au5-96 REP 273 159 96.5 113.5 4 10-Aug-B6 REP 959 1020 96.9 101.1 cr 10-Aug-96 REP 1010 1020 99.5 100.5 6 10-Aug-86 REF' 1020 1200 71.9 109.1 7 10-Aug-86 REP 1260 1440 97..7 106.7 8 I0-Aug-86 REP 433 450 99.1 101.9 9 10-Aug-86 REP 368 777' 99.5 ' 100.5 10 10-Au9-86 REP 304 341 94.3 105.7

n MEAN s LCL UCL 100.0 7 77.0 123.0

Se PRECISION

DATE TYPE MEAS.1 MrAS.2 RECXI REG%

1 10-Aug-24 REP 290 305 97.5 10-Aus-86 REP 400 450 94.1 105.9 10-Aug-86 REP 124 400 99.5 110.'D 4 10-Aug-86 REP 115 421 95.6 114.4 ,,) 10-Aus-84 REP 432 535 69.: 110.7 10-Aus-96 REP 446 488 95.5 104.5 10-Aug-84 REP 341 373 95.5 06-Jun-97 REP 411 469 95.8 104. 9 06-Jun-87 REP 218 223 92.9 10 06-Jun-87 REP 250 247

MEAN LCL UCL. 10u.0 7.5 77.6

SELENIUM PRECISION

DATE TYPE MEAS.1 MEAS.2 PECX1 RE ---

1 06-jun-97 REP 421 373 104.3 93.7 -... 06-Jun-87 REP 930 922 100.4 99.6 24-Jun-37 REP 253 227 105.4 94.6 4 24-Jun-87 REP 270 259 102.1 97.9 5 24-Jun-87 REP 296 295 100.2 99.9 6 24-Jun-87 REP 244 227 103.6 96.4 7 24-Jun-87 REP 258 236 104.5 95.5 8 24-Jun-87 REP 208 190 104.5 95.5 9 24-Jun-87 REP 295 289 101.0 99.0 10 E

61 OCR ECOV ERY O 110 120 115 105 100 90 95 80 85 LOWER - 1 ..-- 2 \ CONTROL \ v 3 / / I\ 4 \ \i/ 5 I , ,.. . ARSENIC 8 / /. 9 \ SA

kipLe V ACCURACY 10 MEAN 62 /, , 11 \ \\ 12 N. N 13 14 / / UPPER A / 15 / /\ 16 CONTROL \ \ \ 17 18 19 20 As ACCURACY

DATE. TYPE MEAS. TRUE REC%

1 28-Ju1-84 SP 29.0 29.0 100.0 28-Ju1-86 SP 26.0 25.4 101.6 3 28-Jul-86 SP 23.0 92.0 4 28-Jul-86 SP 29.0 2/.0 103.7 5 28-Ju1-84 SP 34.0 37.0 97.7 28-Jul-86 ST 2.0 100.0 7 28-Jul-84 ST 5.0 = 100.0 8 28-Jul-86 ST 4.9 5. u 98.0 9 28-Jul-86 ST 3.1 3.0 107.7 10 09-Dec-86 SP ,J.4 97.6 11 09-Dec-84 ST 2.1 2.0 105.0 1'7 29-Apr-87 ST 2.0 2.0 100.0 13 06-Jun-87 SP 7.8 8.0 97.5 14 04-Jun-87 SP 7.8 8.0 97.5 15 04-Jun-87 SP 10.2 10.0 102.0 16 24-Jun-87 SP 4.1 107.7 1/ 24-Jun-87 SP 5.("i 4.9 102.0 18 ERR 17 ERR 20 ERR

n MEAN LCL UCL 20.0 ERR ERR. ERR ERR

63 CD CD

CM ARSENIC PRECISION CD

DATE TYPE NEA8.1 MEAS.2 RECX1 RECX2 ------22-J:t1-86 REP 9 9 100.0 28-Jul-86 REP 6.2 78.4 101.6 2S-Jul-86 REP 7.2 100.0 100.0 4 22-Jul-86 REP 7 . 100.0 5 06-Jun-87 REP r 101.5 98.5 06-Jun-87 REF. 3.1 101.6 98.4 / 66-iun-87 REP 1.1 98.1. 101.6 B 06-Jun-87 PEP '7.7 2.7 100.0 100.0 9 24-Jun-87 REP 1 1 100.0 100.0 10 24-Jun-87 REP 7.8 8 98.7 101.3

n WEAN LCL UCL 7'0.0 100.0 1.1 96.7 103.3

64 %RECOVERY - 105 104 103 102 107 109 100 108 106 101 110 93 92 95 98 94 96 97 99 91 90 MEAN - . -....__ ...„- . --... -....., -- 0 .- -..._ --- --. 3 LOWER C ONTROL 4 -----... ARSENIC _ --,_ ---- ...,.. SA 5 65 kIPLE PRECISION 6 a / ... / N l.\ / \ T i I

- — UPPER -;> 8 1 CONTROL 9 10 %RECOVERY

O

120

115

110

100

105

95

85

90

80

LOWER

_Z\

1

2

CONTROL

3

4

5

6

7

NITRATE

8

9

SAMPLE

66

ACCURACY

10

MEAN

✓---"--....."--,

11

12

13

a

14

UPPER

15

16

CONTROL

17

18

19

20

0

o

1-'

C)

o

-a O O CI") NITRATE ACCURACY

DATE TYPE MEAS. TRUE REC.%

i 06-Jun-87 SF 3.8 3.8 .. 06-Jun-87 SP 2.9 2.9 102. 4 3 06-Jun-87 ST 3.0 99,0 4 06-Jun-87 ST 3.0 3.0 9E3. 7 5 06-Jun-87 ST 3. 1 3.0 102.0 6 06-Jun-87 sT 4.0 4.0 99.0 7 06-Jun-87 ST 4.9 F3.0 98.6 8 06-Jun-87 ST 1. 0 1 .0 95.0 9 06-Jun-E7 ST 2.1 2.0 107.0 1C) 06-Jun-87 ST 7.. C.) 3,0 99.3 11 06-Jun-87 ST 4. C) 4. C) 100.8 12 06-Jun-87 ST 5.0 5.0 99.2 13 ERR 14 ERR 15 ERR 16 ERR 17 ERR 18 ERR 19 ERR 20 ERR

n MEAN L.Ci UCL 70.0 ERR ERR ERR ERR

67 %R (COVERT — 120 115 100 110 105 85 90 95 80 MEAN <, o 3 LOWER CONTROL 4 NfTRATE SAMPLE 5 e PRECISION n 6 A 7 UPPER 8 CONTROL 9 10 NOS PRECISION

DATE TYPE MEAS.1 MEAS.2 RECX1 REC-42

1 :)9-Dec-86 REF 0.09 0.09 100.0 100.0 2 21-Feb-87 REP 2.12 1.98 10S.4 96.6 3 21-Feb-87 REF ..r..4 2.95 107.1 4 15-Apr-87 REP 0 99.4 177):: ,.. 06-Jun-87 REF' 1.94 98.5 101.5 6 06-Jun-87 REP 1.1 101.9 9E.1 7 06-jun-87 REP 0,52 99.0 liDi.0 8 ERR: ERR 9 ERR ERR 10 ERR ERR

n MEAN s LCL UCL 20.0 ERR ERR ERR ERR

69 O

c c ,.;! tal9 r mr.: r,Aut 120 I1 . I 1 I I 1 F i1 1 . 1 -1 1 1 1 i 115 1 J. _I_ 1 1------. 1 if -1 IL ---Lt- - t 1 -r- T-41 1 t 1 , 1 : 1 I Ii, 110 . 1 I I I I 1 ,I 1 I I I 1 I I i i 1 i I I •• . I I I I I 1115 I I i I I I I I ; I 1 . I I 1 I i ,L. I • 1 Il 'I ; I I l I 1.3 I _--4. I 1 1 i .• r,', I : ;••• I :-.--• t I III , !I I i I L. 1 1 100 4- 1 C .-.1 L' ' i :.•' I I 7-f I- I : ) -r ri ' .1 1. i I I I Ilii I / y. I II-III I F....-.. ii il i .1 1 1 II I 1 95 1 I 'c I 'II ,I,./ 1 I ii 1 i, ill , t I 00 - I I I 1 I C3— 44-41-- -11 33 --EP EIL .____./- 93I _4_RI.._.._.il 85 I: V i I I i I r I ' I I I I 1 i i I 1 I - --- -1.-- i 4- I . -i-- I- 1i 1 --I-4 3 4 5 5 • 2 9 15 11 12 15 14 15 15 17 1E1 19 21.1

0.A.19 LE 1.1.1.90 1:,5141.1 PAX ------WI PPEP

70 c c i--. C.: Hg ACCURAC'Y CM sed

DATE TYPE MEAS. TRUE REC.%

1 30-Jul-e ST 27.1 97.S 2 30-jui-86 ST 29.5 31 95.2 3 12-Aug-SO ST 29.3 31.6 92.7 4 127f:Iu9-36 ST 30.6 31.6 96.8 ,., 12-Aug-E6 ST 31.6 101.3 6 12-Aug-86 ST 33.3 31.6 105.4 7 12-Aug-Bs 51 31.2 31.6 98.7 8 12-Auq-86 9T 30 30 100.0 9 12-Aug-SS ST 31.3 31.6 99.1 10 12-Aug-96 9T 71.3 31.6 99.1 11 09-Dec-26 ST 10 30 100.0 17 29-:zyr-87 ST 30 30 100.0 13 06-J,R-e7 ST 49..7 50 99.4 14 06-jun-S7 ST 49.7 50 99.4 IS 06-Jun-87 ST 200 95.2 16 06-1.m-87 ST 49.'7 98.4 17 0-6J7 un-e SP 492 -)5 98.4 18 24-jun-B7 SF 29 27.8 104.3 19 24-Jun-B7 SP 42.7 43.2 c?6,8 20 24-Jun-87 SP 30 28.3 106.0

rl MEAN s LCL UCL 20 99.3 3.2 89.6 109.0

71 NR6CQVilrf- 120 100 105 SS B5 Ott BO - - T 3 LThiet:P. ,o DI3 , 102.04. LAC 1;!E:11 5 72 PRECIOIOJA LI OPER C:01 , 1 1 10 o o o ,c),Aiickcuoil_0 k:7,.:[:\ilit 0.__, cr: cp [JAN 0 4 L91 cr)

QUALITY ASSURANCE SAMPLING PLAN

CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, /NC,

Earth Science Laboratory

University of Utah Research Institute 391 Chipeta Way, Suite C Salt Lake City, Utah 84108 (801) 524-3422

September, 1987

skt b QUALITY ASSURANCE SAMPLING PLAN

CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

September, 1987 o o cn o cr) QUALITY ASSURANCE SAMPLING PLAN

FOR THE CHEMICAL STORAGE AND ZIRCONIUM FEED TANK STORAGE AREAS

IDAHO CHEMICAL PROCESSING PLANT

WESTINGHOUSE IDAHO NUCLEAR COMPANY, INC.

TABLE OF CONTENTS

1.0 Introduction 1

2.0 Objectives and Scope 1

3.0 Project Organization 1

4.0 Site Description 2

5.0 Sampling Rational 3

6.0 Sampling Procedures 4

7.0 Sample Custody 9

8.0 Analytical Procedures 10

9.0 Laboratory Quality Assurance/Quality

Control Procedures 10

10.0 Data Review and validation 11

11.0 Corrective Action 11

12.0 Preve.ntive Maintenance 12

13.0 Reporting 13 LIST OF FIGURES

Fig. 1 Map of CPP Facility 14

Fig. 2 Map of Chemical Storage Area 15

Fig. 3 Map of Zirconium Feed Tank Storage Area 16

Fig. 4 Project Organization 17

Fig. 5 Chain-of-Custody Form 18

LIST OF APPENDICES

Appendix 1 Analytical Methods

1.1 Method 3050: Acid digestion of sludges

1.2 EPA 200.7 (ICP)

1.3 SW-846 7060 (Arsenic)

1.4 SW-846 7471 (Mercury)

1.5 SW-846 7741 (Selenium)

1.6 EPA 353.3 (Nitrate) 1.0 INTRODUCTION

This plan contains the quality assurance guidelines for sampling, analysis, and data reporting activities for the preliminary characterization of soil contamination at the

Chemical Storage and Zirconium Feed Tank Storage Areas (Figs. 1-

3) of the Westinghouse Idaho Nuclear Company, Inc. (WINCO).

2.0 OBJECTIVES AND SCOPE OF THE PROJECT

This soil sampling and analysis project will be conducted by personnel of the University of Utah Research Institute (UURI) to characterize the upper two feet of soils beneath the Chemical

Storage and Zirconium Feed Tank Storage Areas. This project plan is designed to identify the nature and quantity of hazardous constituents that may be present in the soils as a result of past

Operations.

3.0 PROJECT ORGANIZATION AND RESPONSIBILITY

The project organization is shown in Figure 4. The

Principal-In-Charge will have overall responsibility for:

1. direction of the project;

2. communication with local, state, and federal regulatory

agencies and;

3. data and project reporting.

The Project Manager will be responsible for:

1. the preparation of project plans;

1 0 o Fy c: o 2. execution of all activities in accordance with project cr) plans and;

3. communication with the Principal-In-Charge.

The Project Quality Assurance officers will be responsible for:

1. preparation of the Quality Assurance/Quality Control

Project Plan

2. evaluation of sampling procedures,

3. coordination of all laboratory analytical procedures,

4. assessment of the validity, precision, and accuracy of

all analytical data, including quality control samples

and,

5. recommendations for corrective action or further data

collection.

4.0 SITE DESCRIPTION

The Chemical Storage Area (Fig. 2) is approximately 130 feet by 90 feet and encompasses the Chemical Storage Pump House

(CPP-621), the Nitric Acid Storage Tank Area (CPP-719) and adjacent sludge pit, the Aluminum Nitrate Storage Tank Area

(CPP-720), the Hydrofluoric Acid Storage Tank Area (CPP-727), the

Sulfuric Acid and Hydrochloric Acid Tank Area (CPP-759), and the chemical drain lines servicing these areas.

An additional 30 by 30 foot sampling area (Fig. 3), containing the Zirconium Feed Tank (CPP-637), located

2 c c

Cr) c approximately 675 feet north-northwest of the main Chemical CD

Storage area, will also be sampled.

The Chemical Storage Area has been utilized since the late

1970's to store various acids and aluminum nitrate in large metal and fiberglass tanks encircled by earth berms. In March 1982, a nitric acid spill of approximately 1200 gallons occurred in the

Chemical Storage Area at CPP-719. The acid was neutralized utilizing soda ash and soils known to be contaminated were excavated for disposal. Zirconium compounds have been stored at the Zirconium Feed Tank Storage Area in free-standing tanks. In

November, 1978, 450 gallons of zirconium feed spilled from one of the tanks.

5.0 SAMPLING RATIONALE

Surface sampling (0-4 inches) will be conducted to positively identify areas potentially impacted by the past handling practices associated with the chemicals stored in this area.

Subsurface soil samples will be collected 24 inches below each surface sampling site to assess the potential extent of downward migration.

A11 pertinent data, observations, and unusual conditions will be recorded in the field log book (see Section 6.7). A11 rationale for on-site decisions and implementation of action deviating from this sampling plan will be documented.

3 Background subsurface soil samples, geologically identical to soils in the sampling area, will be collected and analyzed.

Background samples will be taken in areas that are far enough away from the sampling site to preclude the effects of contamination. These samples will be analyzed to establish background levels of inorganic constituents in soils on the CPP facility.

Additional samples will be collected from any soils located in the sampling area that visually appear to be contaminated as indicated by dark stains, discoloration, odors, etc.

6.0 SAMPLING PROCEDURES

6.1 Soil Sampling

Throughout the sampling area, soil sampling will be conducted at sites having the highest potential to exhibit contamination. The following list identifies the sampling areas and number of samples to be collected:

AREA 0-4" 24" Total

CPP-719 14

Nitric Acid Storage Tank drains 2 2

Nitric Acid Storage area 4 4

Sludge Pit 1 1

CPP-720 6

4 O O

C7% c, Aluminum Nitrate Tank drains 3 3 co

CPP-727 6

Hydrofluoric Acid Storage area 3 3

CPP-759 4

Sulfuric Acid Tank area 1 1

Hydrochloric Acid Tank area 1 1

CPP-637 12

Zirconium Feed Tank area 6 6

:hemical Drain Lines 7 7 14

Sackground 3 3 6

Grand Total 62

A11 soil samples will be collected utilizing stainless steel

:and tools which have been decontaminated in accordance with

:PA-recommended procedures prior to the collection of each

:ample. Augering to reach the subsurface soil sampling depth of

24 inches will be accomplished using a stainless steel hand luger. If the hand auger is also to be used for sample

:ollection, it will again be decontaminated prior to sample

:pllection. The soil will be placed in a decontaminated

flainless steel bucket until sufficient material has been

5 zollected from each sampling horizon. The soil will then be gently mixed with a stainless steel spoon to homogenize the sample before being placed in an appropriate sampling container.

The sample container will then be properly labeled and prepared for transportation to the laboratory.

5.2 Sampling Equipment Decontamination

An area will be established at the site for the decontamination of all sampling equipment and protective clothing

:hat may come in contact with hazardous constituents. The iecontamination area will be at least 10 by 10 feet, and plastic

Tined. Its perimeter will be bermed to contain all materials generated during decontamination. The decontamination area will be equipped with the necessary reagents, non-leaking containers, brushes and other appropriate equipment. Decontamination will involve (in order);

1. scrubbing with water and detergent,

2. culinary water rinse,

3. acid rinse,

4. deionized water rinse,

5. hexane rinse and,

6. a final deionized or distilled water rinse.

Hand tools employed for sampling will be decontaminated

2etween each use and after sampling.

Protective clothing will be decontaminated, if required and

6 o o

o possible, or disposed of along with the residues, solutions and dr; materials resulting from decontamination operations.

6.3 Sample Containers

Soil samples for inorganic analysis will be placed in chemically clean, one pint, wide-mouth, plastic containers and the mouth will be covered with Teflon.

A11 sample containers will be prepared by the laboratory for sampling in accordance with EPA-approved protocols for the analytical methods listed in Appendix 1.

6.4 Sample Container Labels and Seals

A11 sample containers will be sealed at the time of collection with a non-tearable seal which bears the sampler's name, date, and sample number. The seal shall be placed over the lid and threaded ring to ensure that the sample has not been

tampered with prior to delivery to the laboratory.

A11 sample containers shall be labeled at the time of

collection with indelible ink pens. Sample labels will contain

the following information:

-Site number or project code

-Sample description

-Date of collection

-Time of collection (military 24 hr)

-Sample number

-Sample collector(s)

7 o o

C") -Requested analyses o CD

6.5 Sample Handling and Transport

After sealing and labeling, sample containers will immediately be placed in a cooler, and cooled to four degrees

Centigrade. The samples will be kept out of direct sunlight.

The cooler shall be suitable for vehicular transportation to the laboratory.

6.6 Field Quality Assurance/Quality Control Procedures

A blank sample will be taken in the field and handled along with the field samples and analyzed to assess cross contamination due to sample handling practices.

A duplicate field sample will be collected and analyzed for each set of 20 or fewer samples to assess sampling, sample

handling, and laboratory analytical performance.

6.7 Field Log Book

A field log book with bound, consecutively numbered pages,

will be maintained by project personnel under Chain-of-Custody

procedures. The information, logged on a daily basis, will

include:

-Date and time of entry

-Purpose of sampling

-Name and address of field contacts

8 o o

-Type of waste, if known or suspected Cn o CO -Description of sample(s)

- Number and size of sample(s) taken

-Description of sampling point(s)

-Collector(s) name(s) and signature(s)

-References such as maps, etc.

- Field observations, including unusual conditions

-Weather conditions

-Any field measurements

-Equipment maintenance performed

-Decontamination procedures

-Record of attending personnel, including visitors.

7.0 SAMPLE CUSTODY

To establish the documentation necessary to trace sample possession from the time of collection through completion of analysis, the Chain-of-Custody form (Fig. 5) will be filled out.

It will accompany the samples to the laboratory and be signed and dated by the laboratory agent accepting delivery of the samples.

Prior to sample transfer, all samples will be inspected for damage or tampering. The Chain-of-Custody form will be retained with the samples until the the analyses have been completed. The form will then be returned to the sampler with a copy of the analytical results.

9 8.0 ANALYTICAL PROCEDURES

A11 analytical work will be performed by UURI. This facility is located in the University of Utah Research Park, Salt

Lake City, Utah and is EPA-certified to perform the required analyses through the Utah State Health Laboratory, Bureau of

Laboratory Improvement. A11 analyses will be performed utilizing

EPA-approved methods.

9.0 LABORATORY QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES

Laboratory QA/QC procedures will be those outlined in the

written quality assurance plan this laboratory has on file with

the Utah State Health Laboratory, Bureau of Laboratory

Improvement. Copies of these plans may be obtained from the laboratory or by writing to:

Bureau of Laboratory Improvement

State Health Laboratory

44 Medical Drive, Salt Lake City, Utah 84113.

This plan conforms with the requirements contained in "Rules

for the Certification of Environmental Labor-atories," Utah,

January 3, 1986. This regulation outlines the minimum EPA and

state quality assurance activities necessary for environmental laboratory certification.

10 o o

10.0 DATA REVIEW AND VALIDATION C.) CO The results of the sample analyses and the field and laboratory quality control checks will be reviewed and validated by a Project Quality Assurance Officer. Laboratory control checks will include duplicate analyses, matrix spikes, and the analysis of standards and standard reference materials as required by the EPA approved methodologies and the laboratory quality assurance plans.

Data from field and laboratory duplicates will be used to assess precision. The mean and relative standard deviation will be calculated and compared with EPA-recommended criteria to evaluate data acceptability.

Data from the analysis of standards, standard reference materials and matrix spikes will be used to evaluate data accuracy. The mean and relative standard deviation will be calculated and compared with EPA-recommended criteria to evaluate acceptability.

A Project Quality Assurance Officer will prepare a written report on the analytical data for the Project Manager. The report will review the validity, quality, and completeness of the data and if necessary, make recommendations for corrective action, further sampling or additional analytical data.

11.0 CORRECTIVE ACTION

11.1 Laboratory Corrective Action

11 o o

Laboratory corrective action taken to ensure data quality is o CO outlined in the written laboratory quality assurance plans on file with the Utah State Health Laboratory, Bureau of Laboratory

Improvement.

11.2 Project Corrective Action

Corrective action will be initiated when the project objectives, as outlined. in Section 2.0 are not met or when assessment of data quality reveals data of questionable or unknown quality.

Corrective action may be initiated by any individual on the project subject to approval by the Principal-In-Charge. These corrective actions will include, but are not limited to, modifications of the sampling procedure or additional sampling, modifications of analytical techniques within EPA-approved guidelines, and modification of data reporting procedures.

12.0 PREVENTIVE MAINTENANCE

A11 equipment used in the field for this project will be maintained in accordance with the manufacturer's recommendations.

Cleaning and necessary maintenance will be accomplished prior to and after sampling. A11 maintenance will be recorded in the field log book as described in Section 6.7.

12 CD CD

CD 13.0 REPORTING O Cfl After the analytical results for the samples have been evaluated, a written report on the data will be prepared. The report will contain the analytical results and an assessment of the data quality. To ensure against errors in transcription, the reported data will be checked by at least two individuals for accuracy. The Project Manager or his designated representative will submit the report to the Principal-In-Charge for final comment.

13 411

SAMPLING AREAS

F IGURE - 1 909j00 Siudge FD = French Drain Pit CPP 621 o Proposed Sample Location

•FD

FD

•FD Trench •FD Chemical FD

Chemical Trench

7;ondensate Dry Well ietz) a

CPP 607

SCALE 0 10 20 Ft

Proposed sample locations at the Chemical Storage Area FIGURE 2 o o 0-) o crp

Proposed sample locations at the Zirconium Feed Tank Storage Area (CPP 637)

10' rSCALE I 10'

Approximate location of zircon storage tanks

Figure 3 o Project Organization* o o Principal-In-Charge cr) Joan Poland (WINCO)

Project Manager Joseph Moore (UURI)

Project Quality Sampling and Assurance Decontamination Officers Keith Yorgason David Nelson (UURI) Ralph Helfer Ralph Helfer (EnviroSearch) (EnviroSearch)

Inorganic Analyses (UURI)

-.Loreviations: WINCO,Westinghouse Idaho Nuclear Company Inc.; UURI, University of Utah Research Institute.

Figure 4 o UNIVERSITY OF UTAH RESEARCH INSTITUTE o CM o UURI CM 391 CHIPETA WAY,SUITE C SALT LAKE CITY, UTAH 84108-1295 TELEPHONE 801-524-3422

SAMPLE CUSTODY CONTROL RECORD

L4FLE DATE: zaLS OR MAT'LS SAMPLED: SAMPLE NUMBERS

:r1IMETERS =71 ;NALYSIS

TE:AL .:77:UCTIONS:

..7711 COLLECTION & PRESERVATION

:actify that these samples were collected by me in accordance with EPA -..—_adures. and guidelines.

Name Signature Date/Time

_:T ACKNOWtEDGEMENT (LABORATORY)

--nz.ived the designated samples from

am/pm (date). They were properly sealed

Name Signature Date/Time

Figure 5 Appendix 1.1

METHOD 3050

ACID DIGESTION OF SLUDGES

1.0 Scope and Application

1.1 Method 3050 is an acid digestion procedure used to prepare sludge- type and soil samples for analysis by flame or furnace atomic absorption spectroscopy (AAS) or by inductively coupled argon plasma spectroscopy (ICP). Samples prepared by Method 3050 may be analyzed by AAS or ICP for the following metals:

Antimony Lead Arsenic Nickel Bari um Selenium Beryllium Silver Cadmi um Thallium Chromium Zinc Copper

1.2 Method 3050 may also be applicable to the analysis of other metals in sludge-type samples. However, prior to using this method for other metals, it must be evaluated using the specific metal and matrix.

2.0 Summary of Method

2.1 A dried and pulverized sample is digested in nitric acid and hydrogen peroxide. The digestate is'then refluxed with either nitric acid or hydrochloric acid. Hydrochloric acid is used as the final reflux acid for the furnace analysis of Sb or the flame analysis of Sb, Ba, Be, Cd, Cr, Cu, Pb, Ni, and Zn. Nitric acid is employed as the final reflux acid for the furnace analysis of As, Ba, Be, Cd, Cr, Cu, Pb, Ni, Se, Ag, T1, and Zn or the flame analysis of Ag and Tl.

3.0 Interferences

3.1 Sludge .samples can contain diverse matrix types, each of which may present its own analytical challenge. Spiked samples and any relevant standard reference material should be processed to aid in determining whether Method 30S0 is applicable to a given waste. Nondestructive techniques such as neutron activation analysis may also be helpful in evaluating the applicabil- ity of this digestion method.

4.0 Apparatus and Materials

4.1. 125-ml conical Phillips' beakers.

4.2 Watch glasses.

19 Revised 4/84 o _ Jrying ovens that can be maintained at 30' C. o

Thermometer that covers range of 0' to 200' C. o -= Whatman No. 42 filter paper or equivalent.

ASTM Type II water (ASTM 01193): Water should be monitored

'I Concentrated nitric acid: Acid should be analyzed to determine impurities. If impurities are detected, all analyses should be it:ratted.

Concentrated hydrochloric acid: Acid should be analyzed to deter- -IF E'rei of impurities. If impurities are detected, all analyses should be 22-ected.

Hydrogen peroxide (30%): Oxidant should be analyzed to determine — impurities. If impurities are detected, all analyses should be 2:727-ected.

"c_.-:e Collection, Preservation, and Handling

All samples must have been collected using a sampling plan that - the considerations discussed in Section One of this manual.

:I All sample containers must be prewashed with detergents, acids, 22r:7:led deionized water. Plastic and glass containers are both

Nonaqueous samples shall be refrigerated when possible, and soon as possible.

4eigh and transfer to a 125-ml conical Phillips' beaker a 1.0-9 - sample which has been dried at 60' C, pulverized, and thoroughly

Add 10 ml of 1:1 nitric acid (HNO3), mix the slurry, and cover -a:ch glass. Heat the sample at 95' C and reflux for 10 min. Allow -7: to cool, add 5 ml of conc. HNO3, replace the watch glass, and 30 min. Do not allow the volume to be reduced to less than 5 ml -a-ltaining a covering of solution over the bottom of the beaker.

- 34 20 o o 7.3 After the second reflux step has been completed and the sample has cooled, add 2 ml of Type 11 water and 3 ml of 30% hydrogen peroxide (H202). 'eturn the beaker to the hot plate for warming to start the peroxide reaction. o are must be taken to ensure that losses do not occur due to excessively Cl) vigorous effervescence. Heat until effervescence subsides, and cool the beaker.

7.4 Continue to add 30% H202 in 1-ml aliquots with warming until the effervescence is minimal or until the general sample appearance is unchanged. (NOTE: Do not add more than a total of 10 ml 30% H202.)

7.5 If the sample is being prepared for the furnace analysis of Ag and Sb or direct aspiration analysis of Ag, Sb, Ba, Be, Cd, Cr, Cu, Pb, Ni, T1, and Zn, add 5 ml of 1:1 HC1 and 10 ml of Type 11 water, return the covered beaker to the hot plate, and heat for an additional 10 min. After cooling, filter through Whatman No. 42 filter paper (or equivalent) and dilute to 100 ml with Type 11 water (or centrifuge the sample). The diluted sample has an approximate acid concentration of 2.5% (v/v) HC1 and 0.5% (v/v) HNO3 and is now ready for analysis.

7.6 If the sample is being prepared for the furnace analysis of As, Ba, Be, Cd, Cr, Cu, Pb, Ni, Se, 71, and Zn, continue heating the acid-peroxide digestate until the volume has been reduced to approximately 2 ml, add 10 ml nf Type 11 water, and warm the mixture. After cooling, filter through Whatman No. 42 filter paper (or equivalent) and dilute to 100 ml with Type Il water (or centrifuge the sample). The diluted digestate solution contains Approximately 2% (v/v) HNO3. For analysis, withdraw aliquots of appropriate lume, add any required reagent or matrix modifier, and analyze by method of _andard additions.

8.0 Quality Control

8.1 For each group of samples processed, procedural blanks (Type II -eater and reagents) should be carried throughout the entire sample-preparation and analytical process. These blanks will be useful in determining if Lamples are being contaminated.

8.2 Duplicate samples should be processed on a routine basis. Duplicate :amples will be used to determine precision. The sample load will dictate :he frequency, but 10% is recommended.

8.3 Spiked samples or standard reference materials should be employed to determine accuracy. A spiked sample should be included with each group of :amples processed and whenever a new sample matrix is being analyzed.

8.4 The concentration of all calibration standards should be verified mainst a quality control check sample obtained from an outside source.

8.5 The method of standard addition shall be used for the analysis all EP extracts and whenever a new sample matrix is being analyzed.

21 Revised 4/84 Appendix 1.2 United States Environmental Monitoring and Envoi onmental Protection Support Laboratory Aycncy Cincinnati OH 45268

Research and Development

Test Method

inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes Method 200.7

1. Scope and Application added as more information becomes available and as required. 1.1 This method may be used for the determination of dissolved. 1.5 Because of the differences suspended. or total elements in between various makes and models of drinking water, surface water, satisfactory instruments, no deiailed domestic and industrial wastewaters. instrumental operating instructions can be provided. Instead. the analyst 1.2 Dissolved elements are is referred to the instructions provided determined in filtered and acidified by the manufacturer of the particular samples. Appropriate steps must be instrument. taken in all analyses to ensure that potential interference are taken into 2. Summary of Method account. This is especially true when dissolved solids exceed 1500 mg/L. 2.1 The method describes a (See 5.) technique for the simultaneous or sequential multielement 1.3 Total elements are determined determination of trace elements in after appropriate digestion procedures solution. The basis of the rnethod is are performed. Since digestion the measurement of atomic emission techniques increase the dissolved by an optical spectroscopic technique. solids content of the samples. Sarnples are nebulized and the appropriate steps must be taken to aerosol that is produced is transported correct for potential interference to the plasma torch where excitation effects.(See 5.) occurs. Characteristic atomic-line emission spectra are produced by a radio-frequency inductively coupled 1.4 Table 1 lists elements for which plasma (ICP). The spectra are this method applies along with dispersed by a grating spectrometer recommended wavelengths and and the intensities of the lines are typical estimated instrumental monitored by photomultiplier tubes. detection limits using conventional The photocurrents from the pneumatic nebulization. Actual photomultiplier tubes are processed working detection lirnits are sample and controlled by a computer system. dependent and as the sample matrix A background correction technique is varies. these concentrations may also required to compensate for variable vary. In tirne, other elements may be background contribution to the

Metals-20 Dec. 1982

22 determination 01 trace elements verify background and interelement unresolved overlap o1 molecular band f3ackground most be measured correction factors. (See 7 6 2) snactra, 3) background contribution adjacent to analyte lines on samples from continuous or recombination during analysis. The position selected 3.9 Duality control sample - A phenomena; and 4) background the background intensity solution obtained from an outside contribution from stray light from the surement, on either or both sides source having known, concentration line emission of high concentration .te analytical line. will be values to be used tO verify the elements. The first of these effects determined by the complexity of the calibration standards.(See 7.6.3) can be compensated by utilizing a spectrum adjacent to the analyte line. computer correction of the raw data. 3.10 Calibration standards - a The position used must be free of requiring the monitoring and know spectral interference and reflect the series of standard solutions measurement of the interfering used by the analyst for calibration of same change in background element. The second effect may the instrument (1.e . preparation of the intensity as occurs at the analyte require selection of an alternate analytical curve). (See 7.4) wavelength measured. Background wavelength. The third and fourth effects can usually be compensated by correction is not required in cases of 3.11 Linear dynamic range - The a background correction adjacent to line broadening where a background concentration range over which the the analyte line. ln addition, users of correction measurement would analytical curve rernains linear. actually degrade the analytical result. simultaneous multielement The possibility ol additional 3.12 Reagent blank - A volume of instrumentation must assume the interferences named in 5.1 (and tests deionized. distilled water containing responsibility of verifying the absence for their presence as described in 5.2) the same acid matrix as the of spectral interference frorn an should also be recognized and calibration standards carried through element that could occur in a sample appropriate corrections made. the entire analytical scheme.(See but for which there is no channel in 7.5.2) the instrument array. Listed in Table 2 3. Definitions are some interference effects for the 3.13 Calibration blank - A volume recomrnended wavelengths given in 3.1 Dissolved - Those elements of deionized. distilled water acidified Table 1. The data in Table 2 are which will pass through a 0.45 prn with HNO3 and HCI. (See 7.5.1) intended for use only as a membrane fitter. rudimentary guide for the indication of 3.14 Method of standard addition - potential spectral interferences. For 3.2 Suspended - Those elernents The standard addition technique this purpose, linear relations between which are retained by a 0.45 pm involves the use of the unknown and concentration and intensity for the membrane filter. the unknown plus a known arnount of analytes and the interferents can be standard.(See 10.6.1) assurned. Total - The concentration 3.3 The interference information, which determined on an unfiltered sample 4. Safety was collected at the Ames Laboratory.' 'owing vigorous digestion (9.3), or is expressed at analyte concentration sum of the dissolved plus 4.1 The toxicity or carcinogenicity of eqivalents (i.e. false analyte concen- .....ispended concentrations. (9.1 plus each reagent used in this method has trations) arising from 100 mg/L of the not been precisely defined; however, 9.2.) interferent element. The suggested use each chemical cornpound should be of this information is as follows: 3.4 Total recoverable - The treated as a potential health hazard. Assume that arsenic (at 193.696 nm) concentration determined on an From this viewpoint, exposure to determined in a sarnple unfiltered sample lollowing treatment these chemicals must be reduced to is to be containing approximately 10 mg/L of with hot. dilute mineral acid (9.4). the lowest possible level by whatever aluminum. According to Table 2. 100 means available. The laboratory is yield a false 3.5 Instrumental detection limit - responsible for maintaining a current mg/L of aluminum would signal for arsenic equivalent to The concentration equivalent to a awareness file of OSHA regulations approximately 1.3 mg/L. Therefore, signal, due to the analyte. which is regarding the safe handling of the 10 mg/L of aluminum would result in equal to three times the standard chemicals speci(ied in this method. A signal for arsenic equivalent to deviation of a series of ten replicate reference file of material data a false reader measurements of a reagent blank handling sheets should also be made approximately 0.13 mg/L. The other analytical signal at the same wavelength. available to all personnel involved in is cautioned that systems may exhibit somewhat the chemical analysis. Additional 3.6 Sensitivity - The slope of the different levels of interference than references to laboratory safety are analytical curve, i.e. functional thOse shown in Table 2, and that the available and have been identified relationship between emission interference effects must be evaluated (14.7, 14.8 and 14.9) for the intensity and concentration. for each individual system. information of the analyst.

3.7 Instrument check standard - A 5. Interferences Only those interferents listed were multielement standard of known investigated and the blank spaces in concentrations prepared by the 5.1 Several types of interference Table 2 indicate that measurable inter- analysl to monitor and verify effects may contribute to inaccuracies ferences were not observed for the instrument performance on a daily in the determination of trace interferent concentrationS listed in basis. (See 7.6.1) elements. They can be summarized as Table 3. Generally, interferences were follows: discernible if they produced peaks or 3.8 Interference check sample - A background shifts corresponding to solution containing both interfering 5.1.1 Spectral interferences can be 2-5% of the peaks generated by the I analyte elements of known categorized as 1) overlap of a spectral 'Ames Laboratory. USDOE. lowa Sta:e University. tentration that can be used to line from another element; 2) Ames Iowa 50011

Dec. 1982 Metals-21

23 analyie concentrations also listed in irnally a lactor ol 10 above the instru- responsibility of the analyst to verify Table 3. mental detection lirnit after dilution), :hat the instrument configuration and At present. information on the listed an analysis of a dilution should agree operating conditions used satisfy the silver and potassiurn wavelengths are within 5 % of the original determina- analytical requirements and to not availablc but it has been reported tion (or within some acceptable con- maintain quality control data tat second order energy horn the trol limit (14.3) that has been estab- confirming instrument perforrnance tagnesium 383.231 nm wavelength lished for that matrix). If not, a and analytical results. interferes with the listed potassium line chemical or physical interference ef- at 766 491 inn, fect should be suspected. 7. Reagents and standards 7.1 Acids used in the preparation 5.1.2 Physical interferences are 5.2.2 Spike addition—The recovery of standards and for sample proccssing generally considered to be effects of a spike addition added at a purity grade or associated with the sample nebuliza- minimum level of 10X the in- must be ultra-high tion and transport proccsses. Such strumental detection lirnit (maximum equivalent. Redistilled acids are properties as change in viscosity and 100X) to the original deterrnination acceptable. surface tension can cause significant should be recovered to within 90 to 7.1.1 Acetic acid, conc. (sp gr 1.06). inaccuracies especially in samples 110 percent or within the established which may contain high dissolved control limit for that matrix. If not. a 7.1.2 Hydrochloric acid. conc. (sp gr solids and/or acid concentrations. The matrix effect should be suspected. The 1.19). use ol a peristaltic pump rnay lessen use of a standard addition analysis these interferences. If these types of procedure can usually cornpensate for 7.1.3 Hydrochloric acid, (1+1): Add interferences are operative. they must this effect. Caution: The standard ad- 500 int conc. HCI (sp gr 1.19) to 400 be reduced by dilution of the sample dition technique does not detect coin- mL deionized, distrilled water and and/or utilization of standard addition cident spectral overlap. If suspected, dilute to 1 liter. techniques. Another problem which use of computerized compensation. an can occur from high dissolved solids alternate wavelength, or comparison 7.1.4 Nitric acid, conc. (sp gr 1.41). is salt buildup at the tip of the with an alternate method is recom- 7.1.5 Nitric acid,(1+1): nebulizer. This affects aersol flow-rate mended.(See 5.2.3) Add 500 mL causing instrumental drift. Wetting conc. HNO3 (sp. gr 1.41) to 400 mL the argon prior to nebulization, the 5.2.3 Comparison with alternate deionized, distilled water and dilute to use of a lip washer. or sample dilution method of analysis—Wlien investi- 1 liter. have been used to control this gating a new sample matrix, compari- 7.2 Dionized, distilled water: Prepare problem. Also, it has been reported son tests may be performed with other by passing distilled water through a that better control of the argon flow analytical techniques such as atomic mixed bed of cation and anion ex- rate improves instrument absorption spectrometry. or other change resins. Use deionized, distilled performance. This is accomplished approved methodology. water for the preparation of all vith the use of mass flow controllers. 5.2.4 Wavelength scanning of reagents, calibration standards and as 5.1.3 Chernica/ Interferences are analyte line region—lf the appropriate dilution water. The purity of this water characterized by molecular compound equipment is available, wavelength must be equivalent to ASTM Type II formation, ionization effects and scanning can be performed to detect reagent water of Specification I) 1193 solute vaporization effects. Normally potential spectral interferences. (14.6). these effects are not pronounced with 7.3 Standard stock solutions rnay be the ICP technique. however. if 6. Apparatus purchased or prepared from ultra high observed they can be minimized by 6.1 Inductively Coupled Plasma- purity grade chernicals or metals. All careful selection of operating Atomic Emission Spectrometer. salts rnust be dried for 1 h at 105°C conditions (that is. incident power, unless otherwise specified. observation position. and so forth), by 6.1.1 Computer controlled atomic (CAUTION: Many metal salts are ex- buffering of the sample. by matrix emission spectrometer with background tremely toxic matching, and by standard addition and may be fatal if swal- correction. lowed. Wash hands thoroughly after procedures. These types of handling.) Typical stock solution pre- interferences can be highly dependent 6.1.2 Radiofrequency generator. paration procedures on matrix type and the specific follow: analyte element. 5.1.3 Argon gas supply, welding 7.3.1 Aluminum solution, stock, 1 grade or better. ..ml = 100 pg Al: Dissolve 0.100 g of 5.2 It is recomrnended that -7-aluminum metal in an acid mixture of 4 whenever a new or unusual sample 6.2 Operating conditions — Because mL of (1+1) HCI and 1 mL of conc. HNO3 matrix is encountered. a series of of the differences between various in a beaker. Warm gently to effect tests be performed prior to reporting makes and models of satisfactory solution. When solution is complete, concentration data for analyte instruments, no detailed operating transfer quantitatively to a liter flask, elements. These tests. as outlined in instructions can be provided. Instead, add an additional 10 mL of (1+1) HCI 5.2.1 through 5.2.4, will ensure the the analyst should follow the and dilute to 1.000 mL with deionized, analyst that neither positive nor instructions provided by the distilled water. negative interference eflects are manufacturer of the particular operative on any of the analyte el- instrument. Sensitivity. instrumental 7.3.2 Antimony solution stock, 1 mL ements thereby distorting the detection limit, precision, linear dy- = 100 pg Sb: Dissolve 0.2669 g K(Sb0) accuracy of the reported values. namic range, and interference effects C.H.06 in deionized distilled water, must be investigated and established add 10 mL (1+1) HCI and dilute `.2.1 Serial dilution—lf the analyte for each individual analyte line on that to 1000 mL with deionized, distilled mcentration is sufficiently high (min- particular instrument. It is the water.

Metals-22 Dec.1962

24 7.3.3 • Al Wine soltaloll„CloCk. 1 inL = 7.3.12 lron solutoon, stock. 1 nil_ 7.3.23 Thallium solution, stock. 1 100 /tit As. Dissolve (11320 y of As203 = 100 py Fe: Dissolve 0 1430 g .niL = 100 py Tl: Dissolve 0.1303 y in 100 mL of deionized. distillcd water Fe203 in a warrn mixture of 20 niL IMO,in deionized. distilled water. o containing 0 4 g NaOH. Acidify the (1•1) HCI and 2 mL of conc. HNO3 Add 10 0 mL conc. HNO3 and dilute solution with 2 mL conc. HNO, and Cool, add an additional 5 mL of conc. to 1,000 mL with deionized, distilled o dilute to 1.000 mL with deionized. HNO, and dilute to 1000 mL with water. distilled water. deionized. distilled water. ce, 7.3.24 Vanadium solution, stock. 1 o 7.3.4 Barium solution. stock. 1 rnL 7.3.13 Lead solution, stock. 1 mL mL = 100 pg V: Dissolve 0.2297 cr;. = 100 py Da: Dissolve 0.1516 g BaCl2 = 100 pg Pb: Dissolve 0.1599 g NH4V03 in a minimum amount of (dried at 250°C for 2 hrs) in 10 mL Pb(NO3)3 in minimum amount of conc. HNO3. Heat to increase rate deionized, distilled water wiM 1 nil (1+1) HNO3. Add 10.0 rnL conc. HNO3 of dissolution. Add 10.0 rnL conc. (1.1) FICI. Add 10.0 mL (1+1) Ho and dilute to 1,000 mL with deionized. HNO3 and dilute to 1.000 mL with and dilute to 1,000 rnL with deionized, distilled water. deionized, distilled water. distilled water. 7.3.14 Magnesiurn solution, stock, 1 7.3.25 Zinc solution, stock, 1 mL 7.3.5 Beryllium solution. stock. 1 mL = 100 pg Mg: Dissolve 0.1658 g = 100 pg Zn: Dissolve 0.1245 g ZnO mL = 100 pg Be: Do not dry. Dis- Mg0 in a minimum amount of (1+1) in a minimum amount of dilute HNO3. solve 1.966 g DeS0. • 4 4H20. in HNO3. Add 10.0 mL conc. HNO3 and Add 10.0 mL conc. HNO, and dilute deionized, distilled water. add 10.0 mL dilute to 1,000 mL with deionized, to 1.000 mL with deionized, distilled conc. HNO3 and dilute to 1,000 mL distilled water. water. with deionized, distilled water. 7.3.15 Manganese solution. stock, 1 7.4 Mixed calibration standard so- 7.3.6 Boron solution, stock, 1 mL mL = 100 pg Mn: Dissolve 0.1000 g lutions-Prepare mixed calibration = 100 pg B: Do not dry. Dissolve of manganese metal in the acid mix- standard solutions by combining ap- 0.5716 g anhydrous H3803 in deionized ture 10 mL conc. HCI and 1 mL conc. propriate volumes of the stock solu- distilled water dilute to 1,000 mL. HNO3, and dilute to 1.000 ml. with tions in volumetric flasks. (See 7.4.1 Use a reagent meeting ACS specifica- deionized, distilled water. thru 7.4.5) Add 2 mL of (1+1) tions. keep the bottle tightly stoppered HCI and dilute to 100 mL with and store in a desiccator to prevent 7.3.16 Molybdenum solution. stock. deionized, distilled water. (See Notes the entrance of atmospheric moisture. 1 mL = 100 pg Mo: Dissolve 0.2043 g 1 and 6.) Prior to preparing the mixed (Nf-1.),Mo04 in deionized, distilled standards. each stock solution should 7.3.7 Cadmium solution, stock, 1 water and dilute to 1.000 mL. be analyzed separately to determine mL = 100 pg Cd: Dissolve 0.1142 g possible spectral interference or the Cd0 ip a minimum amount of (1+1) 7.3.17 Nickel solution. stock. 1 presence of impurities. Care should HNO3. Heat to increase rate of dis- mL = 100 pg Ni: Dissolve 0.1000 g be taken when preparing the mixed solution. Add 10.0 mL conc. HNO3 of nickel metal in 10 mL hot conc. standards that the elements are com- and dilute to 1.000 mL with deionized, HNO,. cool and dilute to 1,000 mL patible and stable. Transfer the mixed distilled water. with deionized. distilled water. standard solutions to a FEP fluoro- carbon or unused polyethylene bottle 7.3.1 6 Potassium solution. stock, 1 7.3.B Calcium solution, stock, 1 mL for storage. Fresh mixed standards mL = 100 pg K: Dissolve 0.1907 g = 100 pg Ca: Suspend 0_2498 g should be prepared as needed with KCI, dried at 110°C, in deionized. CaCO3 dried at 180°C for 1 h before the realization that concentration can distilled water dilute to 1.000 mL. weighing in deionized, distilled water change on aging. Calibration stand- and dissolve cautiously with a min- ards must be initially verified using imum 7.3.19 Selenium solution, stock. 1 amount of (1+1) HNO,. Add a quality control sample and moni- 10.0 mL conc. HNO3 and dilute to mL = 100 pg Se: Do not dry. Dissolve 0.1727 g H2Se03(actual assay 94.6%) tored weekly for stability (See 7.6.3). 1,000 mL with deionized, distilled Although not specifically required. water. in deionized. distilled water and dilute to 1.000 mL. some typical calibration standard com- 7.3.9 Clwomium solution, stock. 1 binations follow when using those mL = 100 pg Cr: Dissolve 0.1923 7.3.20 Silica solution, stock. 1 mL specific wavelengths listed in Table g of Cr03 in deionized. distilled = 100 pg Si02: Do not dry. Dissolve 1. water. When solution is cgmplete, 0.4730 g Na3SiO3 - 9H30 in deionized, acidify with 10 mL conc. HNO3 and distilled water. Add 10.0 mL conc. 7.4.1 Mixed standard solution 1- dilute to 1,000 mL with deionized. HNO, and dilute to 1.000 mL with : Manganese, beryllium, cadmium, lead, distilled water. deionized, distilled water. . and zinc.

7.3.10 Cobalt solution. stock. 1 7.3.21 Silver solution, stock. 1 mL = 100 pg Ag: Dissolve 0.1575 g 7.4.2 Mixed standatd solution 11- mL = 100 pg Co: Dissolve 0.1000 g Barium. copper, iron, vanadium, and of cubalt metal in a minimum amount AgN0.3 in 100 mL of deionized, dis- tilled water and 10 mL conc. HNO3. cobalt. of (1+1)1-1NO3. Add 10.0 mL (1 ) NCI and dilute to 1,000 mL with deionized, Dilute to 1,000 mL with deioniied. distilled water. distilled water. 7.4.3 Mixed standard solutioll Molybdenum, silica, arsenic, and 7.3.11 Copper solution. stock, 1 7.3.22 . Sodium solution. stock, 1 selenium. mL = 100 fig Cu: Dissolve 0.1252 g mL = 100 pg Na: Dissolve 0.2542 g CuO in a minirnum amount of (1 +1) NaCI in deionized, distilled water. HNO3. Add 10.0 mL conc. HNO3 and Add 10.0 mL conc. HNO3 and dilute 7.4.4 Mixed standard solution 1V- dilute to 1,000 mL with deionized, to 1,000 mL with deionized. distilled Calcium, sodium, potassium, alumi- distilled water. water. num. chromium and nickel.

Dec. 1982 Metals-23

25 7 4.5 A4iwil standa,rt snlution V— detection limits given in Table 1 (For an active analytical quality control Antemony. boron, magnesium. silver. effluent samples of expected high plograin using spiked samples and re- o and thallium concentrations, spike at an agent blanks. that certain steps in the o NOTE 1:11 the addition ol silver appropriate level.) If the type of cleaning procedure are not required for to the recommended acid combination samples analyzed are varied. a routine samples, those steps may be results in an initial precipitation, syntheticalty prepared sample may be eliminated from the procedure. add 15 inL of deionized distilled used if the above criteria and intent o water and warm the flask until the are met. A limited supply of a 8.2 Before collection of the sample a (Jr, solution clears. Cool and dilute to 100 synthetic interference check sarnple decision rnust be rnade as to the type inL with deionized. distilled water. For will be available from the Ouality of data desired, that is dissolved, this acid combination the silver con- Assurance Branch of EMSL- suspended or total, so that the appro- centration should be limited to 2 Cincinnati. (See 12.1.2) priate preservation and pretreatment mg/L. Silver under these conditions steps may be accomplished. Filtration, is stable in a tap water matrix 7.6.3 The quality control sarnple acid preservation, etc.. are to be per- fru 30 days. Higher concentrations should be prepared in the same acid formed at the time the sample is of silver require additional HCI. rnatrix as the calibration standards coliected Pr as soon as possible at a concentration near 1 mg/L and in thereafter. 7.5 Two types of blanks are required accordance with the instructions for the analysis. The calibration blank provided by the supplier. The Ouality 8.2.1 For the determination of dis- (3.13) is used in establishing the Assurance Branch of EMSL-Cincinnati solved elements the sample must be analytical curve while the reagent will either supply a quality control filtered through a 0.45-pm membrane blank (3.12) is used to correct for sample or information where one of filter as soon as practical after collec- possible contamination resulting from equal quality can be procured.(See tion.(Glass or plastic filtering appara- varying amounts of the acids used in 12.1.3) tus are recommended to avoid possi- the sample processing. ble contarnination.) Use the first 50- 100 mL to rinse the filter flask. Dis- 8. Sample handling an 7.5.1 The cahhratton blank is pre- card this portion and collect the pared by diluting 2 mL of (1+1) HNO3 preservation required votume of filtrate. Acidify the and 10 mL of (1.1) HCI to 100 mL filtrate with (1+1) HNO3 to a pH of 2 8.1 For the with deinnized. distilled water. (See determination of trace or less. Normally, 3 mL of (1+1) acid elements, contamination and loss are Note 6.) Prepare a sufficient quantity per liter should be sufficient to pre- of prime concern. Dust in the to be used to Ilush the system be- labora- serve the sample. tory environment, impurities in tween standards and samples. reagents and impurities on laboratory 8.2.2 For the determinalion of sus- apparatus which the sample contacts 7.5.2 The reagent blank must con- pended elements a measured volurne are all sources of potential contain all the reagents and in the of unpreserved sample must be fil- contamination. Sample containers can same volumes as used in the pro- tered through a 0.45-pm membrane introduce either positive or negative cessing of the samples. The reagent filter as soon as practical after errors in the measurement ot trace blank must be carried through the collection. The filter plus suspended elements by (a) contributing con- complete procedure and contain the material should be transferred to a taminants through leaching or surface sarne acid concentration in the final suitable container for storage and/or desorption and (b) by depleting solution as the sample solution shiprnent. No preservative is required. used for analysis. concentrations through adsorption. Thus the collection and treatment of 8.2.3 For the deterrnination of total 7.6 In addition to the calibration the sample prior to analysis requires or total recoverable etements. the particular standards, an instrument check stan- attention. Laboratory sample is acidified with (1+1) HNO, dard (3.7), an interference check glassware including the sample bottle to pH 2 or less as soon as possible, sample (3.8) and a quality control (whether polyethylene. polyproplyene preferable at the time of collection. sample (3.9) are also required for the or FEP-fluorocarbon) should be The sample is not filtered before analyses. thoroughly washed with detergent processing. and tap water; rinsed with (1+1) nitric 7.6.1 The instrument check standard acid, tap water,(1+1) hydrochloric 9. Sample Preparation is prepared by the analyst by:com- acid. tap and finally deionized, distilled 9.1 For the determinations of .dis- bining compatible elemenls at a con- water in that order (See Notes 2 and solved elements, the filtered, centration equivalent to the midpoint 3). preserved sample may often be of their respective calibration curves. NOTE 2: Chromic acid may be useful to analyzed as received. The acid matrix (See 12.1.1) remove organic deposits from glass- and concentration of the samples and ware; however, the analyst should be calibration standards must be the The 7.6.2 interference check sample be cautioned that the glassware rnust same.(See Note 6.) If.a precipitate is prepared by the anatyst in the be thoroughly rinsed with water to formed upon acidification of the following manner. Select a remove the last traces of chrornium. sample or during transit or storage, it representative sample which contains This is especially important if chrornium must be redissolved before the minimal concentrations of the is to be included in the analytical analysis by adding additional acid analytes of interest by known con- scheme. A commercial product, NOCH- and/or by heat as described in 9.3. centration of interlering elements that ROM1X, available from Godax Labor- will provide an adequate test of the atories, 6 Varick St.. New York, NY 9.2 For the determination of sus- correction factors. Spike the sample 10013, may be used in place of pended elements. transfer the mem- with the elements of interest at the chromic acid. Chomic acid should not brane filter containing the insoluble oproxirnate concentration of either be used with plastic bottles. material to a 150-mL Griffin beaker 00 pg/L or 5 times the estimated NOTE 3: if it can be documented through and add 4 mL conc. HNO3. Cover the

Metals-24 Oec. 1982

26 values 1,, •• r V/1111 u ..AI:11( It and clog the nebulizer (See Note 4.) Adjust sample. Concentration obtaineq= c) Qt.•-lii hi' ill:Al will Nuoll the sample to a predetermined volume should not dcviate from the actual the membrane based on the expected concentrations - values by inore than ± percent V—"'" on:lease the termirraitire ol the of elements present. The sample is (or the established control limits hi.• plate and digest the material. now ready for analysis (See Note 6). whichever is lower). If they do. follow Cr) w,,,fn the acid has nearly evaporated. Concentrations so determined shall be the recommendations of the instru- cool the beaker and watch glass and reported as "total." ment manufacturer to correct tor this 0 add another 3 mL of conc. HNO, NOTE 5: If low determinations of condition. Cover and continue heating until the boron are critical, quartz glassware digestion is complete, generally indi- should be use. 10.5 Begin the sample run flushing cated by a light colored digestate. NOTE 6: If the sarnple analysis solution the system with the calibration blank each saniple. Evaporate to near dryness (2 mL). cool. has a different acid concentration solution (7.5.1) between add 10 mL HCI (1+1) and 15 int_ from that given in 9.4. but does not (See Note 7.) Analyze the instrument deionized. distilled water per 100 mL introduce a physical interference or check standard (7.6.1) and the calibra- dilution and warrn the beaker gently affect the analytical result, the same tion blank (7.5.1) each 10 sarnples. for 15 min. to dissolve any precipi- calibration standards may be used. 10.6 If it has been found that tated or residue material. Allow to rnethod of standard addition are cool, wash down the watch glass and 9.4 For the determination of total required. the following procedure is beaker walls with deionized distilled recoverable elements, choose a rnea- recornmended. water and filter the sample to rernove sured volume of a well mixed, acid insoluble rnaterial that could clog the preserved sample appropriate for the 10.6.1 The standard addition tech- nebulizer. (See Note 4.) Adjust the expected level of elements and trans- nique (14.2) involves preparing new volume based on the expected con- fer to a Griffin beaker.(See Note 5.) standards in the sample matrix by centrations of elernents present. This Add 2 mi. of (1+1) HNO3 and 10 rnL adding known amounts of standard to volurne will vary depending on the of (1+1) HCI to the sample and heat one or more aliquots of the processed elements to be determined (See Note on a steam bath or hot plate until the sample solution. This technique com- 6). The sample is now ready tor volume has been reduced to near 25 pensates for a sample constituent that analysis. Concentrations so determined mL making certain the sample does enhances or depresses the analyte shali be reported as "suspended." not boil. After this treatment, cool signal thus producing a different slope NOTE 4: In place of filtering. the the sample and filter to remove inso- from that of the calibration standards. sample after diluting and rnixing may luble material that could clog the lt will not correct for additive inter- be centrifuged or allowed to settle by nebulizer.(See Note 4.) Adjust the ference which causes a baseline- shift. gravity overnight to rernove insoluble volume to 100 mL and mix. The sample The simplest version of this technique material. is now ready for analysis. Concentra- is the single-addition method. The tions so determined shall be reported procedure is as follows. Two identical 9.3 For the determination ol total as "total." aliquots of the sample solution, each elements. choose a measured, volume of volume V., are taken. To the 10. Procedure of the well mixed acid preserved first (labeled A) is added a small sarnple appropriate for the expected 10.1 Set up instrument with proper volurne V, of a standard analyte level of elements and transfer to a solution of concentration c,. To the Grilfin beaker.(See Note 5.) Add 3 mL operating parameters established in 6.2. The instrument second (labeled B) is added the same of conc. HNO3. Place the beaker on must be allowed to become thermally stable before be- volume V, of the solvent. The analy- a hot plate and evaporate to near dry- tical signals of A and B are measured cautiously, ginning. This usually requires at least ness making certain that and corrected for nonanalyte signals. the sample does not boil and that no 30 min. of operation prior to calibra- tion. The unknown sample concentration area of the bottom of the beaker is c, is calculated: allowed to go dry. Cool the beaker and 10.2 Initiate appropriate operating add another 5 mL portion of conc. configuration of computer. Cx = SoVsCs HNO3. Cover the beaker with a watch (SA - Se) Vx glass and return to the hot plate. 10.3 Profile and calibrate instru- Increase the temperature of the hot ment according to instrument where SA and SB are the analytical plate so that a gentle reflux action manufacturers recommended signals (corrected for the blank) of occurs. Continue heating. adding addi- procedures, using the typical mixed solutions A and El, respectively. Vs necessary, tional acid as uMil the calibration standard solutions and cs should be chosen so that S. digestion is complete (generally indi- described in 7.4. Flush the systern is roughly twice SI3 on the average. It cated when the digestate is light with the calibration blank (7.5.1) is best if Vs is made much less than in color or does not change in appear- between each standard. {See Note 7.) \ix, and thus cs is much greater than ance with continued refluxing.) Again, (The use of the average intensity of cx. to avoid excess dilution of the evaporate to near dryness and cool multiple exposures for both sample matrix. If a separation or the beaker. Add 10 mL of 1+1 HCI standardization and sample analysis concentration step is used, the and 15 mL of deionized. distilled has been found to reduce randorn additions are best rnade first and water per 100 mL of final solution error.) carried through the entire procedure. and warm the beaker gently for 15 NOTE 7: For boron concentrations For the results from this technique to min. to dissolve any precipitate or greater than 500 pg/t. extended flush be valid. the following limitations residue resulting from evaporation. times of 1 to 2 min. may be required. must be taken into consideration: Allow to cool, wash down the beaker 1. The analytical curve must be linear. walls and watch glass with deionized 10.4 Before beginning the sample 2. The chemical form of the analyte distilled water and filter the sample to 'run, reanalyze the highest mixed added must respond the same as the remove insoluble material that could calibration standard as if it were a analyte in the sample.

Get. 1982 Metals-25 27 e 3 The interference cow must b standards. A fresh dilution of this constant Dye/ the workfny range of sample shall be anlayzed every week concern. thereafter to monitor their stability. If 4 The signal must be corrected for the results are not within -±5% of the any addillve interference. true value listed for the control Calculation sample. prepare a new calibration 1 1. standard and recalibrate the correct the 1.1 Reagent blanks (7.5.2) should instrurnent. If this does not oe subtracted frorn all samples. This is problem, prepare a new stock particularly important for digested standard and a new calibratMn samples requiring large quantities of standard and repeat the calibration. acids to complete the digestion. Precision and Accuracy 11.2 If dilutions were performed. 13.1 In an EPA round robin phase 1 appropriate factor must be applied the study, seven laboratories applied the sample values. to ICP technique to acid-distilled water matrices that had been dosed with 11.3 Data should be rounded to the thousandth place and all results various metal concentrates. Table 4 should be reported in mg/L up to lists the true value, the mean reported relative three significant figures. value and the mean % standard deviation. 12. Quality Control References (Instrumental) 1. Winge. R.K.. V.J. Peterson. and 12.1 Check the instrument V.A. Fassel. "Inductively Coupled standardization by analyzing Plasma-Atomic Emission appropriate quality control check Spectroscopy: Prominent Lines," EPA- standards as follow: 600/4-79-017.

12.1.1 Analyze an appropriate 2. Winefordner. J.D.. •Trace instrument check standard (7.6.1) Analysis: Spectroscopic Methods for containing the elements of interest at Elements." Chemical Analysis, Vol. a frequency of 10%. This check 46, pp. 41-42. standard is used to determine instrurnerit drift. If agreement is not 3. Handbook for Analytical Quality within t5% of the expected values or Control in Water and Wastewater within the established control limits. Laboratories. EPA-600/4-79-019. 'thever is lower, the analysis is out 4. Garbarino. J.R. and Taylor. H.E.. ontrol. The analysis should be "An Inductively-Coupled Plasma „aminated. the problern corrected. Atomic Emission Spectrornetric and the instrurnent recalibrated. Method for Routine Water Quality Analyze the calibration blank (7.5.1) Testing." Applied Spectroscopy 33. al a frequency of 10%. The result No. 3(1979). should be within the established control limits of two standard devia- 5 "Methods for Chemical Analysis of tions of the mean value. If not. repeat Water and Wastes." EPA-600/4-79- the analysis two more times and 020. average the three results. If the average is not within the control limit, 6. Annual Book of ASTM Standards, termiinate the analysis. correct the Part 31. probiiern and recalibrale the instrument. 7. "Carcinogens - Working With CarcinogensS Department of Health. 12.1..2 To verify interelernent end Education, and Welfare. Public Health bacloround correction factors analyze Service. Center for Disease Control, :he interference check sarnple (7.6.2) • National Institute for Occupational at the beginning. end. and at periodic Safety and Health, Publication No. 77- .ntencals throughout the sample run. 206. Aug. 1977. Resulns should fall wilhin the ?.stabkished control limits of 1.5 times 8. "OSHA Safety and Health Stan- he standard deviation of the mean dards, General Industry."(29 CFR /Mut If no(. terminate the analysis, 1910), Occupational Safety and Health :orrec the problem and recalibrate Administration, OSHA 2206. (Revised. 'le instrument. January 1976).

• 2.1.3 A quality control sample 9. ''Safety in Academic Chemistry 7.6.3) obtained from an outside Laboratories. American Chernical So- aurce rnust first be used for the ciety Publication, Committee on aitial werification of the calibration Chemical Safety, 3rd Edition, 1979.

Metals-26 Dec.1982

28 Berummended Wavelengths' and Estimated Instrumental r.r. -pints O O Estimated detection ant Wavelength run pg/L 2 an 308.215 45 o MC 193.696 53 411111111117 206.833 32 asi.- 455.403 2 ramie 313.042 a3

t 249 773 5 721mia 226.502 4 lamer 317.933 10 ;Sr 267.716 7 ' ain 228.616 7

Tiour 324.754 6 a 259.940 7 220.353 42 279.079 30 ZaTimiese 257.610 2

tarn 202.030 8 231.604 15 766.491 see3 196.026 75 288.158 58

:Sr 328.068 7 _an- 588.995 29 TS- 190.864 40 Aar 292.402 8 It- 213.856 2 --narelengths hated are recommended because of their sensitivity and anacceptance. Other wavelengths may be substituted if they can vase rhe needed sensitivity and are treated with the same corrective =Jaffaes tor spectral interference. (See 5.1.1.1. riesated instrumental detection limits as shown aretaken from "rely Coupled Plasma-Atomic Emission SpectroscOpy-Prominent -a-EPA-600/4-7.9-017. They are given as a guide for an instrumental air -Y.:e actual method detection limits are sample dependent and may vary -zrzemple matrix varies. anc.eoendent on operating conditions and plasma position.

Dec.! 982 Meta/s-27

29 Analyle Concentranen Equiva lents fing/L) Arising from biles-totems at the 100 mg/L Level o Wavelength. fen Inteilerent c:: Al Ca Cr Cu fe Mg Mn Ni Ti V Fj "-mar 308.215 ------0.21 - - 1.4 'cram 206.833 a47 - 2.9 0.08 - - .25 0.45 o air 193.696 /.3 - 0.44 - - - - - 1.1 CT% -Aber 455.403 -"rms 313.042 0.04 0.05 AIMS< 249.773 0.04 0.32 -

,ss•eter 226.502 - - - 0.03 - - 0.02 - as, 317.933 - - 0.08 - 0.01 0.01 004 - 0.03 0.03 its...r 267.716 a003 0.04 - 0.04 as- 228.616 - - a03 - 0.005 - ao3 0.15 iair- 324.754 - a003 - a05 0.02 259.940 - - - - - 0.12 -

_LC 220.353 0.17 ------ametaer 279.079 - 0.02 0.1 1 - a13 0.25 - 0.07 0.12 amme 257.610 a005 - 0.01 a002 0.002 - - der 202.030 0.05 - 0.03 - Sur 231.604 ------lac- 196.026 0.23 - - - 0.09 - - - :St 288.158 - 0.07 - - - - - aor .:ism- 588.995 - - - - - 0.08 - Ister 190864 0.30 - - -

as 292.402 - 0.05 - a005 - - 0.02 21:c 213.856 - - - 0.14 - 0.29 -

Jai utederent and Analyte Elemental Concen- -attons Used ler lntederence Measurements a rable 2.

Aar -ag/L1 Intederents (mg/L1 A 10 Al 1000 70 Ca 1000 ;0 Cr 200 :- ..., 1 Cu 200 1 Fe 1000 - 1 Mg 1000 '0 Mn 200 1 Ni 200 7 Ti 200 1 V 200 ‘-- 1 ac 1

.0 '.7. '0 -0

Metals-28 Dec.1982

30 Table 4. l03 Precision and Accuracy Data

Sample t$ 1 Sample tt 2 Smnple o Mean Mean Mean True Reponed Mean True Reported Mean flue Reported Mean Value Value Percent Value Value Percent . Value Value Percent Element pg/L pg/L RSD pg/L pg/L RSD pg/L pg/L RSD o Be 750 733 6.2 20 20. 9.8 180 176 5.2 c) Mn 350 345 2.7 15 15 6.7 100 99 3.3 V 750 749 1.8 70 69 2.9 170 169 1.1 As 200 208 7.5 22 19 23 60 63 17 0 150 749 3.8 10 70 18 50 50 3.3 Cu 250 235 5.7 11 11 40 70 67 7.9 fe 600 594 3.0 20 19 15 180 178 6.0 Al 700 696 5.6 60 62 33 160 161 13 Cd 50 48 72 2.5 2.9 16 14 13 16 Co 500 512 10 20 20 4.1 120 108 21 Ni 250 245 5.8 30 28 11 60 55 14 Pb 250 236 16 24 30 32 80 80 14 Zn 200 207 5.6 16 19 45 80 82 9.4 Se 40 32 21.9 6 8.5 42 10 8.5 8.3 Not all elements were analyzed by all laboratories.

Dec. 1987 Meta/s-29 31 Appendix 1.3

O O

O ARSENIC Cr)

Method 206.4 (Spectrophotometric-SDDC)

STORET NO. 01002 Inorganic, Dissolved 00095 Inorganic.. Total 00997 Inorganic, Suspcnded 00996

Scope and Application 1.1 The silver diethyldithiocarbamate method determines inorganic arseni: when present in concentrations at or above 10 ug/1. The method is applicable to drinkinz water and most fresh and saline waters in the absence of high concentrations of C:.Tomium,- cobak, copper, mercury, molybdenum, nickel, and silver. Domestic and indus:rial wastes may also be analyzed after digestion (see 3.3). 1.2 Difficulties may be encountered with certain industrial waste mat:Hats containing volatile substances. High sulfur content of wastes may exceed remoN al capacity of the lead acetate scrubber. Summary of Method 2.1 Arsenic in the sample is reduced to arsine, AsE13, in acid solutic7. in a hydrogen generator. The arsine is passed through a scrubber to remove sulfide ar.:.! is absorbed in a solution of silver diethyldithiocarbamate dissolved in pyridine. The :-.td cornplex thus formed is measured in a spectrophotorneter at 535 nm. Comments 3.1 In analyzing drinking water and most surface and ground waters, intern:- rences are rarely encountered. Industrial waste samples should be spiked with a known ccriount of arsenic to establish adequate recovery. 3.2 It is essential that the system be airtight during evolution of the arsine, lc avoid losses. 3.3 If concentration of the sample and/or oxidation of any organic matter Es required, refer to Method 206.5.[Standard Methods, 14th Edition, Method 404B, p. 2.1'4, Procedure 4.a (1975)]. For sample handling and preservation, see part 4.1 of the At..Nmic Absorption Methods section of this manual. 3.3.1 Since nitric acid gives a negative interference -`in this test, use silfuric acid as a preservative if only inorganic arsenic is being measured. 3.4 1-Ephedrine in chloroform has been found to be a suitable sc:vent for silver diethyldithiocarbamate if the analyst finds the odor of pyridine obknionable [Anal. Chem.45, 1786(1973)]. 3.5 For quality control requirements and optional recommendations for use in drinking water analyses, see part 10 of the Atomic Absorption Methods section cf this manual. coved for NPDES and SDWA r.v-th 1971 al-orial revision 1974 32 206.4-1 c Precision and Accuracy 4.1 In a round-robin study rcportcd by Standard Mcthods a synthetic unknown sample containing 40 ug/l, as As, with othcr metals was analyzed in 46 laboratories. Rclativc standard dcviation was t 13.8% and relative crror was 0%. Reference 5.1 Thc procedure to be used for this determination is.found in: Standard Mcthods for the Examination of Watcr and Wastcwatcr, 14th Edition, p. 283, Mcthod 404A (1975).

206.4-2 33 Appendix 1.4

METHOD 7471

MERCURY IN SOLID OR SEMISOLID WASTE (MANUAL COLD-VAPOR TECHNIQUE)

1.0 Scope and Application

1.1 Method 7471 is approved for measuring total mercury (organic and inorganic) in soils, sediments, bottom deposits, and sludge-type materials. All samples must be subjected to an appropriate dissolution step prior to analysis.

2.0 Summary of Method

2.1 Prior to analysis the samples must be prepared according to the procedures discussed in this method.

2.2 Method 7471, a cold-vapor atomic absorption method, is based on the absorption of radiation at the 253.7-nm wavelength by mercury vapor. The mercury is reduced to the elemental state and aerated from solution in a closed system. The mercury vapor passes through a cell positioned in the light path of an atomic absorption spectrophotometer. Absorbance (peak height) is measured as a function of mercury concentration.

2.3 The typical detection limit for this method is 0.0002 mg/1.

3.0 Interferences

3.1 Potassium permanganate is added to eliminate possible interference from sulfide. Concentrations as high as 20 mg/1 of sulfide as sodium sulfide do not interfere with the recovery of added inorganic mercury from Type II wate

3.2 Copper has also been reported to interfere; however, copper concen- trations as high as 10 mg/1 had no effect on recovery of mercury from spiked samples.

3.3 Seawaters, brines, and industrial effluents high in chlorides require additional permanganate (as much as 25 ml) since, during the oxi- dation step, chlorides are converted to free chlorine which also absorbs radiation of 253 nm. Care must therefore be taken to ensure that free chlorine is absent before the mercury is reduced and swept into the cell. This may be accomplished by using an excess of- hydroxylamine sulfate reagent (25 ml). In addition, the dead air space in the BOO bottle must be purged before adding stannous sulfate. Both inorganic and organic mercury spikes have been quantitatively recovered from seawater using this technique.

3.4 Certain volatile organic materials that absorb at this wavelength may also cause interference. A preliminary run without reagents should determine if this type of interference is present.

34 o o 4.0 Apparatus and materials O 4.1 Atomic absorption spectrophotometer or equivalent: Any atomic Cr; absoption unit having an open sample presentation area in which to mount the absorption cell is suitable. Instrument settings recommended by the particular manufacturer should be followed. Instruments designed specifically for the measurement of mercury using the cold-vapor technlque are commercially available and may be substituted for the atomic absorpti.on spectrophotometer.

4.2 Mercury hollow cathode lamp or electrodeless discharge lamp.

4.3 Recorder: Any multirange variable speed recorder that is compatible with the UV detection system is suitable.

4.4 Absorption cell: Standard spectrophotometer cells 10 cm long having quartz end windows may be used. Suitable cells may be constructed from plexiglass tubing, 1 in. 0.0. x 4.5 in. The ends are ground perpendicular to the longitudinal axis and quartz windows (1 in. diameter x 1/16 in. thickness) are cemented in place. The cell is strapped to a burner for support and aligned in the light beam by use of two 2-in. x 2-in. cards. One-in.-diameter holes are cut in the middle of each card. The cards are then placed over each end of the cell. The cell is then positioned and adjusted vertically and horizontally to give the maximum transmittance.

4.5 Air p-mp: 'Any peristaltic pump capable of delivering 1 liter air/min may be used. A Masterflex pump with electronic speed control has been foird to be satisfactory.

4.6 Flowmeter: Capable of measuring an air flow of 1 liter/min.

4.7 Aeration tubing: A straight glass frit having a coarse porosity. Tygon tubing is used for passage of the mercury vapor from the sample bottle to the absorption cell and return.

4.8 Drying tube: 6-in. x 3/4-in.-diameter tube containing 20 g of magnesium perchlorate or a small reading lamp with 60-W bulb which may be used to prevent condensation of moisture inside the cell. The lamp should be positioned to shine on the absorption cell so that the air temperature in the cell is about 10' C above ambient.

4.9 The cold-vapor generator is assembled as shown in Figure 1.

4.10 The apparatus shown in Figure 1 is a closed system. An open system, where the mercury vapor is passed through the absorption cell only once, may be used instead of the closed system.

35 Alr Pump

(J.)rn Jc Desiccant Scrubber Altsmplinn Cnll CnnteinIng El 4— Bubbler 0 4 Melon), AbsotbIng Metlia Semple Solu lon In ',pi-)fintile

F igura 1. Appnratus for [tameless mercury determination.

n9 T 00 o 4.11 mercury ‘dpor is toxic, precaution must be taken to o Because avoid 1-4 its inhalation. Therefore, a bypass has been included in the system to -ither vent the mercury vaper into an exhaust hood or pass the vapor through o ome absorbing media, such as: cn

1. equal volumes of 0.1 M KMn04 and 10% H2SO4

2. 0.25% iodine in a 3% KI solution

A specially treated charcoal that will adsorb mercury vapor is also available from Barnebey and Cheney, E. 8th Ave. and N. Cassidy St., Columbus, Ohio 43219, Cat. #580-13 or #580-22.

5.0 Reagents

5.1 ASTM Type II water (ASTM D1193): Water should be monitored for impurities.

5.2 Aqua regia: Prepare immediately before use by carefully adding three volumes of conc. HC1 to one volume of conc. HNO3.

5.3 Sulfuric acid, 0.5 N: Dilute 14.0 ml of conc. sulfuric acid to 1 liter.

5.4 Stannous sulfate: Add 25 g stannous sulfate to 250 ml of 0.5 N sulfurjc acid. This mixture is a suspension and should be stirred continu- ously during use. A 10% solution of stannous chloride can be substituted for tannous sulfate.

5.5 Sodium chloride-hydroxylamine sulfate solution: Dissolve 12 g of sodium chloride and 12 g of hydroxylamine sulfate in Type II water and dilute to 100 ml. Hydroxylamine hydrochloride may be used in place of hydroxylamine sulfate.

5.6 Potassium permanganate, 5% solution (w/v): Dissolve 5 g of potassium permanganate in 100 ml of Type II water.

5.7 Mercury stock solution: Dissolve 0.1354 g of mercuric chloride in 75 ml of distilled water. Add 10 ml of conc. nitric acid and adjust the volume to 100.0 ml (1.0 ml = 1.0 mg Hg).

5.8 Mercury working standard: Make successive dilutions of the stock mercury solution to obtain a working standard containing 0.1 pg/ml. This working standard and the dilution of the stock mercury solutions should be prepared fresh daily. Acidity of the working standard should be maintained at 0.15% nitric acid. This acid should be added to the flask as needed before adding the aliquot.

37 METHOD 7741 Appendix 1.5 SELENIUM (ATOMIC ABSORPTION, GASEOUS HYDRIDE)

.0) Scope and Application

1.1 Method 7741 is an atomic absorption procedure which is approved for determining the concentration of selenium in wastes, mobility procedure extracts, soils, and groundwater, provided that the sample matrix does not contain high concentrations of chromium, copper, mercury, silver, cobalt or molybdenum. All samples must be subjected to an appropriate dissolution step prior to analysis. Spiked samples and relevant standard reference materials are employed to determine applicability of the method to a given waste.

2.0 Summary of Method

2.1 Samples are prepared according to the nitric/sulfuric acid digestion procedure described in this method. Next, the selenium in the digestate is reduced to the +4 form using tin chloride. The +4 selenium is then converted to a volatile hydride with hydrogen produced from a zinc/HC1 reaction,

2.2 The volatile hydride is swept into an argon-hydrogen flame located in the optical path of an atomic absorption spectrophotometer, and the resulting absorbance is proportional to the selenium concentration.

2.3 The typical detection limit for this method is 0.002 mg/1.

3.0 Interferences

3.1 High concentrations of chromium, cobalt, copper, mercury, molybdenun nickel, and silver can cause analytical interferences.

3.2 Traces of nitric acid left following the sample workup can result in analytical interferences. Nitric acid must be distilled off by heating the sample until fumes of S03 are observed.

3.3 Elemental selenium and many of its compounds are volatile and therefore certain samples may be subject to losses of selenium during sample preparation.

4.0 Apparatus and Materials

4.1 100-m1 beaker.

4.2 Electric hot plate.

4.3 A commercially available zinc slurry hydride generator or a generator constructed from the following material (see Figure 1).

38 7.2 Prepare working standards from the standard stock solutions. The following procedure provldes standards in the optimum working range.

7.2.1 Pipet 1 ml stock solution into a 1-liter volumetric flask. Bring to volume with Type II water containing 1.5 ml conc. HNO3/liter. The concentratlon of this solution is 1 mg Se/liter (1 ml = 1 pg Se).

7.2.2 Prepare six working standards by transferring 0, 0.5, 1.0, 1.5, 2.0 and 2.5 ml of the selenium stock standard (see Section 5.8) into a 100-m1 volumetric flasks. Bring to volume with diluent. The concentrations of these working standards are 0, 5, 10, 15, 20 and 25 pg Se/liter.

7.3 Standard additions

7.3.1 Take the 15-, 20-, and 25-pg standards and transfer quanti- tatively 25 ml from each into separate 50-ml volumetric flasks. Add 10 ml of the prepared sample to each. Bring to volume with Type II water containing 1.5 ml HNO3/liter.

7.3.2 Add 10 ml of prepared sample to a 50-ml volumetric flask. Bring to volume with Type 11 water containing 1.5 ml HNO3 per liter. This is the blank.

7.4 Follow the manufacturer's instructions for operating an argon- hydrogen flame. The argon-hydrogen flame is colorless so it may be useful to aspirate a low- concentration of sodium to ensure that ignition has occurred.

7.5 The 196.0-nm wavelength shall be used for the analysis of selenium.

7.6 Transfer a 25-ml portion of the digested sample or standard to the reaction vessel. Add 0.5 ml SnC12 solution. Allow at least 10 min for the metal to be reduced to its lowest oxidation state. Attach the reaction vessel to the special gas inlet-outlet glassware. Fill the medicine dropper with 1.50 ml zinc slurry that has been kept in suspension with the magnetic stirrer. Firmly insert the stopper containing the medicine dropper into the side neck of the reaction vessel. Squeeze the bulb to introduce the zinc slurry into the sample or standard solution. The metal hydride will produce a peak almost immediately. When the recorder pen returns partway to the base line, remove the reaction vessel.

7.7 Analyze, by the method of standard additions; all EP extracts, all samples analyzed as part of a delisting petition, and a11 samples that suffer from matrix interferences.

7.8 Duplicates, spiked samples, and check standards should be routinely analyzed.

39 o o 5.6 Potassiun iodide solution: Dissolve 20 g

5.8 Selenium standard stock solution: 1000 mg/liter solution may be purchased, or prepared as follows. Dissolve 0.3453 g of selenious acid (assay 94.6% of N2Se01) in Type II water. Add to a 200-ml volumetric flask and bring to volume (1 ml = 1 mg Se).

6.0 Sample Collection, Preservation, and Handling

6.1 All samples must have been collected using a sampling plan that addresses the considerations discussed in Section One of this manual.

6.2 All sample containers must be prewashed with detergents, acids, and Type II water. Plastic and glass containers are both suitable.

6.3 Special containers (e.g., containers used for volatile organic analysis) may have to be used if very volatile selenium compounds are to be analyzed.

6.4 Aqueous samples must be acidified to a pH of less than 2 with nitric acid.

6.5 Nonaqueous samples shall be refrigerated where possible, and malyzed as soon as possible.

.0 Procedure

7.1 Sample preparation

7.1.1 To a 50 ml aliquot of digested sample (or in the case of EP extracts a 50-ml sample) add 10 ml conc. NNO3 and 12 ml of 18 N H2SO4. Evaporate the sample on a hot plate until white S03 fumes are observed (a volume of about 20 ml). Do not let it char. If it chars, stop the digestion, cool and add additional HNO3. Maintain an excess of HNO3 (evidence of brown fumes) and do not let the solution darken, because selenium may be reduced and lost. When the sample remains colorless or straw yellow during evolution of S03 fumes, the digestion is complete.

7.1.2 Cool the sample, add about 25 ml distilled deionized water and again evaporate to SO3 fumes just to expel oxides of nitrogen. Cool. Add 40 ml conc. NCI and bring to a volume of 100 ml with distilled deionized water.

'sed 4/84 40 Appendix 1.6

NITROGEN, NITRATE

Method 352.1 (Colorimetric, Brucine)

STORET NO. Total 00620

1. Scope and Application 1.1 This mcthod is applicablc to the analysis of drinking, surface and saline waters, domestic and industrial wastes. Modification can be made to remove or correct for turbidity, color, salinity, or dissolved organic compounds in the sample. 1.2 The applicable range of concentrations is 0.1 to 2 mg NO3—N/liter. 2. Summary of Method 2.1 This method is based upon the reaction of the nitratc ion with brucine sulfate in a 13 N I-12SO,solution at a temperature of 100°C. The color of the resulting cornplex is measured at 410 nrn. Temperature control of the color reaction is extremely critical. 3. Sample Handling and Preservation 3.1 Analysis should be made as soon as possible. If analysis can be made within 24 hours, the sample should be preserved by refrigeration at 4°C. When samples must be stored for more than 24 hours, they should be preserved with sulfuric acid (2 ml conc. H2SO4 per liter) and refrigeration. 4. Interferences 4.1 Dissolved organic matter will cause an off color in 13 N H2SO4 and must be compensated for by additions of all reagents except the brUcine-sulfanilic acid reagent. This also applies to natural color present not due to dissolved organics. 4.2 The effect of salinity is eliminated by addition of sodium chloride to the blanks, standards and samples. 4.3 A11 strong oxidizing or reducing agents interfere. The presence of oxidizing agents may be determined with a total residual chlorine test kit. 4.4 Residual chlorine interference is eliminated by the addition ofsodium arsenite. 4.5 Ferrous and ferric iron and quadrivalent manganese give slight positive interferences, but in concentrations less than 1 mg/I these are negligible. 4.6 Uneven heating of the samples and standards during the reaction time will result in erratic values. The necessity for absolute control of ternperature during the critical color t development period cannot be too strongly emphasized. 5. Apparatus 5.1 Spectrophotometer or filter photorneter suitable for measuring absorbance at 410 nm. 5.2 Suflicient nurnber of 40-50 ml glass sample tubes for reagent blanks, standards and samples. 5.3 Neoprene coated wire racks to hold sample tubes. 5.4 Water bath suitable for use at 100°C. This bath should contain a stirring mechanism so that all tubes are at the same tcmperature and should be of sufficient capacity to accept

Approved for NPDES and SDWA Issued 1971

352A-I

41 the rcquircd numbcr of tubcs without significant drop in temperature when thc tubes are O immersed. O 5.5 Water bath suitabk for usc at 10-15t. 6. Reagcnts O 6.1 Distilled water free of nitrite and nitrate is to be used in preparation of aIl reagents and standards. 6.2 Sodium chloride solution (30%): Dissolve 300 g NaCI in distilled water and dilute to 1 liter. 6.3 Sulfuric acid solution: Carefully add 500 ml conc. H2S0, to 125 ml distilled water. Cool and kecp tightly stoppered to prevent absorption of atmospheric moisture. 6.4 Brucine-sulfanilic acid reagent: Dissolve 1 g brucine sulfate [(C231426N2002-H2SO4-7H20] and 0.1 g sulfanilic acid (NEI,C61-14S03H-H20) in 70 ml hot distilled water. Add 3 ml conc. HCI, cool, mix and dilute to 100 ml with distilled water. Store in a dark bottle at 5t. This solution is stable for several months; the pink color that develops slowly does not effect its usefulness. Mark bottle with warning CAUTION: Brucine Sulfate is toxic; take care to avoid ingestion. 0 6.5 Potassium nitrate stock solution: 1.0 ml = 0.1 mg NO3-N. Dissolve 0.7218 g anhydrous potassium nitrate(KNO 3)in distilled water and dilute to 1 liter in a volumetric flask. Preserve with 2 ml chloroform per liter. This solution is stable for at least 6 months. 6.6 Potassium nitrate standard solution: 1.0 ml = 0.001 mg NO3-N. Dilute 10.0 ml of the stock solution (6.5) to I liter in a volumetric flask. This standard solution should be Y-7 C prepared fresh weekly. \j/ ,/1 6.7 Acetic acid (1 + 3): Dilute 1 volume glacial acetic acid (CH3COOH)with 3 volumes of -3 /0 distilled water. 6.8 Sodium hydroxide(IN): Dissolve 40 g of NaOH in distilled water. Cool and dilute to 1 liter. 7. Procedure 7.1 Adjust the pH of the samples to approximately 7 with acetic acid (6.7) or sodium hydroxide(6.0. If necessary, filter to remove turbidity. 7.2 Set up the required number of sample tubes in the rack to handle reagent blank, standards and samples. Space tubes evenly throughout the rack to allow for even flow of bath water between the tubes. This should assist in achieving uniform heating of all tubes. 7.3 If it is necessary to correct for color or dissolved organic matter which will cause color on heating, a set of duplicate samples must be run to which all reagents except the brucine- sulfanilic acid have been added. 7.4 Pipette 10.0 ml of standards and samples or an aliquot of the samples diluted to 10.0 ml into the sample tubes. 7.5 If the samples are saline, add 2 ml of the 30% sodium chloride solution (6.2) to the reagent blank, standards and samples. For fresh water samples, sodium chloride solution may be omitted. Mix contcnts of tubes by swirling and place rack in cold water bath (0-10t).

352.1-2 42 c c 7.6 Pipcttc 10.0 ml of sulfuric acid solution (63)into cach tube and mix by swirling. Allow tubes to come to thermal equilibrium in the cold bath. Be sure that temperatures have equilibrated in all tubes before continuing. 7.7 Add 0.5 ml brucine-sulfanilic acid reagent (6.4) to each tube (except the interference control tubes, 7.3)and carefully mix by swirling, thcn place the rack of tubes in the 100t watcr bath for exactly 25 minutes. Caution: Immersion of the tube rack into thc bath should not decrease the temperature of the bath more than I to 2°C. In order to kecp this temperature decrease to an absolute minimum,flow of bath water bctween the tubes should not be restricted by crowding too many tubes.into the rack. If color development in the standards reveals discrepancies in the procedure, the operator should repeat the procedure after reviewing the temperature control steps. 7.8 Remove rack of tubes from the hot water bath and immcrse in the cold water bath and allow to reach thermal equilibrium (20-25°C). 7.9 Read absorbance against the reagent blank at 410 nm using a 1 cm or longer cell. 8. Calculation 8.1 Obtain a standard curve by plotting the absorbance 'of standards run by the above procedure against mg NO3-N/1.(The color reaction does not always follow Beer's law). 8.2 Subtract the absorbance of the sample without the brucine-sulfanilic reagent from the absorbance of the sample containing brucine-sulfanilic acid and determine mg NOrN/1. Multiply by an appropriate dilution factor if less than 10 ml of sample is taken. 9. Precision and Accuracy 9.1 Twenty-seven analysts in fifteen laboratories analyzed natural water samples containing exact increments of inorganic nitrate, with the following results:

Increment as Precision as Accuracy as Nitrogen, Nitrate Standard Deviation Bias, Bias, mg N/liter mg Miter % mg N/liter

0.092 -6.79 -0.01 0.19 0.083 +830 +0.02 1.08 0.245 +4.12 +0.04 L24 0.214 +2.82 +0.04

(FWPCAMethod Study 2, Nutrient Analyses).

Bibliography

1. Standard Methods for the Examination of Water and Wastewater, l4th Edition, p 427, Method 4 I9D (1975). - 2. Annual Book of ASTM Standards, Part 31,"Water", Standard D 992-71, p 363(1976) 3. Jenkins, D., and Medsken, L.,"A Brucine Method for the Determination of Nitrate in Ocean, Estuarine, and Fresh Waters", Anal Chem., 36, p 610,(1964).

352.1-3

43

RECEIVLD

C:=1 JAN 0 4 1991 01 CO RC FL: copy 00 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #t-3 AT cPP 637 APRIL 3, 1986

DATE TIME SAMPLE DEPTH BLOW COUNTS

032086 8:00 a.m. On site, get tooling from decon room. 032086 8:00 to 11:00 Wait for holes to be marked. 032086 11:00 to 12:145 We had a real concern about overhead and possible underground lines at hole number 1. Our choice 4 was to wait until we could reach Joan or Birney for clarification. n32086 1:00 p.m. On hole #4-3, ready to drill 2086 1:30 8 to 10 feet 17/15//6/18 ..j2086 1:50 18 to 20 feet 3940/65/86 At 15 feet we encountered a very hard material which appeared to be compacted sand and gravel. 032086 2:15 to 3:15 Wait for hole to be ntarked.

Total Depth: 20 feet Total Standby: 51 hours

sic- sec poctioast co 17 13

R.tt o o cn co co

260 So. 1400 West PINGREE, IDAHO 832620

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-2 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032086 3:20 p.m. On hole, begin drilling. 032086 3:36 8 to 10 feet 11/2040/37 032086 3:45 Finish for the day 032186 8:00 On site, get set up 032186 8:13 Begin drilling 032186 8:35 13 to 15 feet 111/27/26/214 032186 We had wet material at 36 feet Rossible as there was no auger return. At 16 feet, we had fine grained material, and at about V5 feet we were into a clay layer. 032186 10:32 Bedrock at 61 feet.

Total Depth: 61 feet Total Standby: 0 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-4 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032186 10:40 Begin drilling. 032186 At about 1 foots we hit a wet clay-like material. 032186 12:45 13 to 15 feet 63/84/65/95 032186 1:15 23 to 25 feet 18/27/30/30

Total Depth: 25 feet Total Standby: 0 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPOIff JOB NO. 2517.2 DRILL HOLE #4-5 AT CPP 637

DATE TIME SAMPLE DEPTH BIAW COUNTS

032186 2:00 p.m. On hole, begin drilling. 032186 2:20 8 to 10 feet 16/19/33/39 032L86 2:50 18 to 20 feet 13/20/27/42 032186 3:30 Finish for the day.

Total Depth: 20 feet Total Standby: 0 c: co cn oo oo

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-6 AT cPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032486 8:22 On site, ready to drill 032486 9:25 13 to 15 feet 38/50/52/34 032486 10:00 23 to 25 feet 26/54/72/80

Total Depth: 25 feet Total Standby: 0 o o

C.1 CO CO

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-8 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032486 10:15 On hole, ready to drill. 032486 At 8 to 10 feet, we were in moist material. 032486 10:45 8 to 10 feet 4/3/2/10 032486 11:15 13 to 15 feet 41/35/50/72 032486 12:00 Pulled tooling, ready to move.

Total Depth: 15 feet Total Standby: 0 260 So. 1400 West PINGREE, IDAHO 83262,

(208) 684-5490

DRILL REPORf JOB NO. 2517.2 DRILL HOLE #4-7 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032486 12:45 On hole, begin drilling. 032486 1:45 18 to 20 feet 26/24/35/74 032486 2:15 23 to 25 feet 31/25/35/42 032486 3:40 Bedrock at 613,- feet, had a clay layer at 14 4 feet. n32586 8:00 a.m. On site, pulled tooling.

Total Depth: 614 feet TotaL Standby: 260 So. 1400 West PINGREE, IDAHO 83262,

(208) 684-5490

DRILL REPOFC JOB NO. 2517.2 DRILL HOLE #4-12 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032586 9:00 to 10:00 No hoLes marked. 032586 10:00 On hole) begin drilling. 032586 10:45 13 to 15 feet 44/64/56/49 032586 11:30 23 to 25 feet 29/36/48/48 032586 Had a clay layer at 43 feet. ?586 2:15 p.m. Bedrock at 59 3/4 feat.

Total Depth: 59 3/4, feet Total Standby: 1 hour o o CI CO 00

260 So. 1400 West PINGREE, IDAHO 83262 .0 (208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLES 1,3 & 130, AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032586 2:30 On hole, ready to drill, Joan had told us to mark the hole 34 ft., 7 in. from #12. 032586 3:00 At 8 feet, when we were trying to take the the first sample, we hit a duct bank, so we moved 3 feet north and began again. 2586 3:25 8 to 10 feet 3/26/86 rtal Depth: 8 feet Total Standby: $

* * * * * * * * * *

032586 3:45 On Hole # 4-13A, ready to drill. 032686 8:00 On site, ready to driLl. 032686 8:24 8 to 10 feet 7/5/475 032686 8:45 18 to 20 feet 27/25/29/36 032686 9:00 to 9:30 HeLp Joan mark hoLes.

Total Depth: 20 feet Total Standby: i hour cc, c) cn co

260 So. 1400 West PINGREE, IDAHO 83262 • (208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-15 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032686 9:45 On hole, ready to drill. 032686 10:15 13 to 15 feet 25/38/4840 032686 10:45 23 to 25 feet 20/27/34/30

Total Depth: 25 feet Standby: 0 o o cn co co

260 So. 1400 West PINGREE, IDAHO 83262

(208) 6845490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-18 AT cPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032686 11:15 On hole, ready to drill 032686 11:45 13 to 15 feet 31/35/42/62 032686 12:15 23 to 25 feet 26/33/28/34

Total Depth: 25 feet Total Standby: 0 o o

00 00

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILLFEPORT JOB NO. 2517.2 DRILL HOLE #4-22 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032686 1:25 On hole, ready to drill 032686 2:00 8 to 10 feet 5/4/8/9 Material was very soft at 8 foot level. 032686 2:30 L8 to 20 feet 49/72/61/96

"otal Depth: 20 feet Total Standby: 0 260 So. 1400 West PINGREE, IDAHO 83262

.12081 684-5490

DRILLREPORT JOB NO. 2517.2 DRILL HOLE #4-23 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032686 3:00 On hole, ready to drill 032686 3:30 8 to 10 feet 28/38/70/63 032786 8:00 On site, get set up. 032786 9:00 18 to 20 feet 61/91/86/56

Total Depth: 20 feet Total Standby: 0 o o F-- Csi CX) 00

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-19 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032786 8:00 to 8:45 Mark holes 032786 9:00 Sample on #4-23 032786 10:00 On hole, ready to drill. 032786 10:24 8 to 10 feet 11/34/33/31 032786 10:54 18 to 20 feet 34/39/45/52

Total Depth: 20 feet Total Standby: 3/4 hour 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-21 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

032786 11:00 On hole, ready to driLl 032786 11:45 Had drilled 8 feet, quit for the day to attend court. 032886 8:17 On site, ready to drill 032886 8:45 13 to 15 feet 37/46/77/100 n32886 9:15 23 to 25 feet 55/100 at 6 inches * note: at 100 counts, we feel that we are only compacting the material, and would be of no benefit to continue a drive sample. 032886 1:00 Bedrock at 59 feet - clay Layer at 43 feet

Total Depth: 59 feet Total Standby: 0 o o

CA CO CO

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB N0. 2517.2 DRILL HOLES #4-24 & 24A AT CPP 637

DATE TINE SAMPLE DEPTH BLOW COUNTS

032886 1:15 On hoLe, ready to drill 032886 1:30 3 to 5 feet 16/16/12/16 032886 At 6 feet, we hit a solid object that caught the augers and killed the engine. We moved 3 feet south, and continued with 24-A

ii-IHI-A-1*-1*****-11-11-14-****

032886 2:00 On hole, begin drilling 032886 2:30 13 to 15 feet 59/51/100 at 5 inches

Total Depth: 15 feet, (24 & 24A combined) Total Standby: 0 o o

CO

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-25 AT CPP 637

DATE TIKE SA14PLE DEPTH BLOW COUNTS

032886 3:00 On hole, ready to drill 032886 3:30 3 to 5 feet 5/4/4/5 033186 8:00 to 10:00 Meeting at MK office. 3186 10:00 to 10:15 Wait for guard. ,3186 10:30 13 to 15 feet 30/38/36/38 033186 11:00 23 to 25 feet 18/33/46/40

Total Depth: 25 feet Total Standby: :I hour o o

00

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE N4-1 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

033186 11:15 On hole, material is very, very soft. 033186 11:30 3 to 5 feet 2/1/1/1 033186 12:15 13 to 15 feet 11/35/33/30 033186 1:30 23 to 25 feet 56/88/70/40 Note: sample at 13 feet had a definite acidic smell. 31116 2:00 Finished, ready to move.

Total Depth: 25 feet Total Standby: fa 260 So. 1400 West PINGREE, IDAHO 83262 I (208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE 04-11 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

033166 2:15 On hole, ready to drill. 033186 2:30 3 to 5 feet 5/h/8/18 033186 3:00 13 to 15 feet 36/55/52/50 033186 3:25 Finished, ready to move 033L86 3:30 We went to 604, got waste barrel and moved it over to 637. 1186 3:45 Finished for the day.

Total Depth: 15 feet Total Standby: 0 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 DRILL HOLE #4-14 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

040186 8:00 On site 040186 8:00 to 8:15 At Joan's office for directions and supplies. 040186 8:45 On hole, ready to drill. 040186 9:30 L8 to 20 feet 20/17/20/14

Total Depth: 20 feet Total Standby: 0 0 1-4 cn CO 00

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPOET JOB NO, 2517.2 DRILL HOLE #6-17 AT CPP 637 #14-17A

DATE TIME SAMPLE DEPTH BLOW COUNTS

040186 10:00 On Hole, ready to drill. 0140186 10:15 At 2 feet, hit a cement trench, moved 3 feet south to miss the trench. n40186 10:30 On hole 14-17A, ready to drill. )186 11:00 18 to 20 feet 33/30/25/19

Total Depth: 14-17 &17A : 22 feet Standby: O O

CO CO 260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPOIff JOB NO. 2517.2 DRILL HOLE #4-20 AT CPP 637

DATE TIME SAMPLE DEPTH BLOW COUNTS

040186 11:30 On hole, ready to drill. 040186 12:00 13 to 1$ feet 19/33/29134 040186 12:30 23 to 25 feet 29A1/37/36 (1140186 1:00 Heady to move

Total Depth: 25 feet Standby: o o cn co co

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 HAND AUGER HOLES AT CPP 637

NOTE: AS THESE HOLES WERE ALL DONE BY A HAND AUGER, NO SAMPLE DEPTHS WILL BE SHOWN.

DATE TIME HOLE NUMBER HOLE DEPTH

040186 2:08 4-33 3 feet 040186 2:38 to 3:10 Made arrangements to get a power auger unit to try on these holes. (11.0186 3:10 Went to MK to talk to Birney 386 8:00 4-33 - tried to used power unit, but it was not big enough to drive augers any further. 040386 8:30 4-31A again tried to use power unit, to no avail 4-31A hand augered 3 feet 040386 9:00 4-31 hole began 6' below 2 feet ground surface. 040386 9:30 4-32 at li feet hit decayed wood, very wet hole was caving in, so only got 2? feet. 040386 10:00 4-34 clay-like material 3 to 4 feet 4 feet 040386 10:15 4-26 had to move 3 times as hole kept caving in li feet li feet 3 feet 040386 10:55 il-2Phole-- was 5 feet from fround surface, li feet his very moist material. 3 feet 040386 11:00 4-28 very soft material 6 feet 040386 11:25 4-29 very hard material 3 feet 040386 11:45 4-30 went 2 feet, found a wooden form, it was very rocky and hard to penetrate 3 feet. o o 1-s cn oo cc

260 So. 1400 West PINGREE, IDAHO 83262

(208) 684-5490

DRILL REPORT JOB NO. 2517.2 HAND AUGER HOLES AT CPP 637

DATE TIME HOLE NUMBER HOLE DEPTH

040386 12:30 4-36 5 feet 040386 12:45 4-37 extremely hard to penetrate, dug 2 feet with shoveL, then augered. 3 feet 040386 1:30 4-10 very wet 3 feet 0386 1:54 4-9 very hard 3 feet 40386 2:08 4-35 very hard 2 feet 040386 2:30 4-16 pit level about 5 feet from ground level 2 feet 040386 3:00 SLudge Pit had 22 feet of white powder, then we got into had carmel colered wet material with sand. ji feet 040386 3:15 4-17 3 feet, were on cement 040386 3:30 4-14 3 feet

Total footage for had augered holes: 63 feet Total Standby: 0 1 • I "ON. -W1514 --4 I. !II

N\ :-.1141-1-05-81-2 4 / N IS 4,875 9 r -„—141

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TR,-,38 i nil _J TR 40 /c------Th n r -11p- TR 34 , ... 1630.L TR:s3jj 5 IR 14 ---i p 16291 PARKING 698 AREA I IYASIEVIATBR TR TREATMEN ii Legend AUXIN ASH )(-- ) BURY EAST PERMET R ROAD A . PIT v33 --,...N. Cleaned Areas ----„ r A Possible sub—surface i contamination to TR 35C CTB-313 /'4 L. Q._ EAST PERW1E ROAO LODGE POE STEET LODGE POLE STREET -- 1R-23 F 689 a be investigated. SS C 1606 ._----j TR_3 56640 3 "4 --..N.) BB BB°a _ : 667 7-2 T-3 CO 1637 0 — 11 • 0 SUBSTABON _ HESILOCK b. on o p 1836 1639 695 96 512 699 691 III 1648 , 712-25n7R-3 E le 7 ,k.?t 1 - PERCOLATION . 8 sc e 4 II CEDAR STR f 1"1 T8-4 6 arW-30 POND 664 _ :64131 SU STAIN 1645 fr t El At ,r ,, , \ il — TR TR-10 , ti.,i±k—d w 1658 .#4(''''', 1R-29 1R-20 1R-22 lia A \ F FN STROT ..,-,. • A 71 X., if./ • -; 855 1 00 E - .eYe ,,' irt-28 693 Z •11 11 67 7R-21 % ..q/ % ''V 0 *•,,f OS-../ / 1603 M _ P/ • ,,i 'r A.'4.44 }ti .)%%A•# ',0 e Adif .e. . ' rfrefi ) el•7 11. OF -2 °V e /10 c. / V-"• ,.1.7 ast BP.1 ; 663 I 655 •• 1 4.4mitams• :007/ j "4 _ • :12A D /if A ,re / „inj 2/./4. 9/ 1/C . 7 9 At,"/ * Pie, 1"5. 4-.11 4 0 45C,V. elIV 5' a -- § Feten-117 - • 11 4/f),,,,4/ ':1 \ / 1649 ,,,,, • - • ,/1 :it, // . RERCO,ATION 1 1647 a .),,, r 1 z 0 r --1 0 ',"1 . N631 V:• ,1 -,:-.,-.... i POND 1W fir i el..!.....-- - , 4 /Ad ' 7,ht: ',7 i 606 1 sal uk"//02.,,-71 •:€ .//: .". r /4 44, 1111 ‘, , Al LE SlREET 2 „. • ',4#. i 1650 1631 672 602 • :Str17,11111, 674D 1604 6 16 "V "?:.:"fflareci 7. '.reA ;"/////// A :,1,%1)2 ,i >ifril511- , 640 6,fie:s I i '',Ile'd P 6210 t.,,,,,, eig,' 20D-1 A .% .1.A.51741#1,AAnAt,"te 1617 ,•,;17/#2,4 4., /41, . .., ° ii' VW/Jr - gc liA n :IF e •'III d d..N, 1..- " 611 gl,...Th Vi'•/2,'.4# Im 1 ri, n33 1644 saw S < ,.•••” \...... i 5 2a 53 U BIRCH f < 6811 --1!"41 Si 161 IE a ??." et " (61 1605 3 'OA 0 es2 161 v,,,,..,.#2, ,1662, 668 4 U 637 ---.--) :1646: VS .frz 4 \ _ 637 651 BAMBOO SnEEf r ?WI; - 'VCCEIEr

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CLEVELAN BLVD ICPP — A—'8740 (11-92) 6 5 4 3 2 (NI NJ MEMO OF CONVERSATION

Date: February 2, 1993 Time: 13:30 hrs Commitment Made [ ] Yes [X] No

Person Calling: Bruce Culp Person Called: Mark Howard

Representing: WINCO ER Representing: WINCO Projects

Purpose of Conversation: Asbestos Abatement in Chemical Trench at CPP-621

Text of Conversation: Mark described the project that took place in the Chemical Trench south of CPP 621. The project took place during the months of September, October and November 1993. The project removed asbestos from lines in the trench and replaced them with nonasbestos insulation. Also during the project approximately 2" of soil was removed from the entire area of the trench to remove any asbestos that may have fallen to the ground. The area within the trench was covered with plastic and sand is planned to be put on top the plastic.

Signedc9r— Date: Et 2 \c)(9.5 )

REP xv 22_

PRELIMINARY INFORMATION UNIVERSITY OF UTAH RESEARCH INSTITUTE UURI EARTH SCIENCE LABORATORY 391 CHIPETA WAY, SUITE C SALT LAKE CITY, UTAH 84108-1295 TELEPHONE 801-524-3422

September 4, 1986

Ms. Joan Poland Westinghouse Idaho Nuclear Co. Box 4000, CPP 630 1955 Fremont Avenue Idaho Falls, Idaho 83403

Dear Joan:

Enclosed, please find a preliminary scope of work and budget for the work you requested UURI perform at CPP site 621. The proposed work is comprehen- sive and has been divided into four components; pre-sampling activities (Phase I), targeted sampling within the site and on its perimeter (Phase II), inter- mediate depth/slant drilling (Phase III), and the preparation of a final report and closure plan (Phase IV). In our opinion, it will be most cost effective to develop a program with these components now if the decision is made by WINCO to bring the site into compliance with EPA standards. This compliance will probably require refurbishing the containment facilities, chemical trenches, and pump houses as well as characterizing and remediating the site. This may be much more difficult and costly if the construction is completed as presently planned. You should, in addition, keep in mind as you review the sampling plan which we have outlined that the layout of the site places limits on the location and depth of the samples that can be collect- ed. Thus, there will be some gaps in the data especially in the central portions of the area and beneath the limestone pits. EPA may require WINCO to close these gaps with additional data before approving any closure plans.

I have included costs for preparing a site safety plan for WINCO's approval as we discussed during our meeting with you last week. However, because WINCO is responsible for overall site safety at the CPP facility, we feel that WINCO should provide a Site Safety Officer during sampling activities, and approve and implement any site safety plans that we prepare at your request. It is our understanding that WINCO will assume the liability for safety on the site. We do, however, want the option of stopping sampling activities by our staff at the site without penalty if, in our opinion, a dangerous situation should develop.

The sampling program we have designed will involve: hand augering; deep augering to approximately 40 feet; and intermediate depth or slant augering to c c 20-30 feet. Samples with a hand auger will be taken at the surface and at a depth of approximately 3 feet throughout the area, including the limestone C- pits, french drains, sludge pit, and chemical trenches. We anticipate collecting approximately 110 hand auger samples. Cc

Deep augering samples will be obtained around the perimeter of the site and if possible, adjacent to and in the limestone pit. Because the clay layer at 40 to 45 feet acts as a barrier to downward percolating contamination, we plan to auger no deeper than the top of this layer. This deep drilling will establish the maximum extent of contamination.

In the center of the site where the space between the tanks is narrow, a small drill rig will be required. We have located a rig suitable for this work but its depth capabilities are limited and because of its small size, drilling will be slow and therefore costly. If possible, use of this rig should be delayed until data from the hand augered and deep samples are obtained, since information on the full extent of contamination in the area may not be needed if contamination exists at depth.

We have assumed in preparing the budget that you will provide the manual labor and construction materials needed to obtain some of the samples. This work will involve: removal of some of the beams and metal posts; removal of the limestone from two sample locations in each of the limestone pits; removal of portions of the trench covers during trench sampling; and pumping and barreling of the sludge in the sludge pit so that the bottom can be sampled.

I understand that the Hawley Bros. would be available to do the deep drilling around the middle of September. The paperwork and hand augering could be started as soon as we have a contract in place. If you need additional information or more detailed cost breakdown please let me know.

Sincerely,

JNM:leo enclosure cc: W. Forsberg A. Rydalch R. H. Timpson P. M. Wright PRELIMINARY INFORMATION SCOPE OF WORK

CPP - SITE 621

UURI:

1. Prepare QA/QC - Sampling plan

2. Prepare site safety plans for approval by WINCO as requested.

3. Subcontract drilling in accordance with approved sampling program.

4. Perform on-site QA/QC activities (document sampling, label and transport samples, maintain chain of custody records).

5. Perform sampling and decontamination activities.

6. Provide sampling and decontamination supplies.

7. Assign samples to laboratories certified for analyses performed.

8. Report analytical data to WINCO.

9. Prepare interim and final reports on analytical data as needed, including statistical evaluation of data, extent and distribution of anomalous concentrations and results of QA/QC samples, but excluding recom- mendations.

10. Prepare closure plans as required. PRELIMINARY INFORM.^,T!ON c BUDGET

Phase I - Pre-Sampling CO Amount A. Salaries and Wages:

1. Salaries $ 1,615 a. J. N. Moore - 60 hours b. Draftsperson - 8 hours c. Secretary - 40 hours

B. Employee Benefits:

1. 42.8% of A1 691

C. Consultant (EnviroSearch, Inc.):

1. David Nelson - 60 hours 3,300

D. Travel:

1. Airfare - INEL site (3) $630 2. Per Diem - 3 days 150 3. Car Rental - 2 days 90

Total 870

E. Supplies:

1. Office Supplies 50

F. Total Direct Costs: $6,526

G. Indirect Costs:

1. 48.4% of F 3,159

H. G & A Costs:

1. 13.5% of F 881

I. Total Direct, Indirect and G&A Costs: $10,566

J. Fee:

1. 5.5% of I 581

K. Total Project Price - UURI: $11,147

L. University of Utah Indirect Costs:

1. 20% of K 2,228

M. Total Project Price: $13,375 o PRELIMINARY INFORMATION o BUDGET CT;

Phase II - Near Surface Sampling/Deep Drilling (X) Amount

A. Salaries and Wages:

1. Salaries $8,605 a. J. N. Moore - 152 hours b. R. L. Kroneman - 160 hours c. K. R. Yorgason - 160 hours d. Draftsperson - 8 hours e. Secretary - 32 hours

2. Wages 1,440 a. Technician - 160 hours

Total 10,045

B. Employee Benefits:

1. 42.8% of A1 $3,683 2. 14.2% of A2 204

Total 3,887

C. Consultant (EnviroSearch, Inc.):

1. David Nelson - 104 hours 5,720

D. Travel:

1. Airfare - INEL site (4) $ 840 2. Per Diem and Lodging - 20 days 1,000 3. Car Rental - 5 days 225

Total 2,065

E. Supplies:

1. Power Auger $200 2. Safety Clothing 150 3. Chemicals and Misc. 675

Total 1,025

F. Subcontracts:

1. Drilling 4,670

G. Total Direct Costs: $27,412 o o H. Indirect Costs: Cn

1. 48.4% of G 13,267 00 I. G & A Costs:

1. 13.5% of G 3,701

J. Total Direct, Indirect and G&A Costs: $44,380

K. Fee:

1. 5.5% of J 2,441

L. Total Project Price - UURI: $46,821

M. University of Utah Indirect Costs:

1. 20% of L 9,364

N. Total Project Price: $56,185 c PRELIMINARY INITRMATION c BUDGET cr

Phase III - Intermediate/Slant Drilling

Amount

A. Salaries and Wages:

1. Salaries $3,120 a. J. N. Moore - 76 hours b. R. L. Kroneman - 40 haurs c. K. R. Yorgason - 40 hours d. Draftsperson - 8 hours e. Secretary - 24 hours

2. Wages 360 a. Technician - 40 hours

Total 3,480

B. Employee Benefits:

1. 42.8% of A1 $1,335 2. 14.2% of A2 51

Total 1,386

C. Consultant (EnviroSearch, Inc.):

1. David Nelson - 52 hours 2,860

D. Travel:

1. Airfare - INEL site (2) $420 2. Per Diem and Lodging - 10 days 500 3. Car Rental - 5 days 225

Total 1,145

E. Supplies:

1. Steam Cleaner $500 2. Safety Clothing 150 3. Chemicals and Misc. 200

Total 850

F. Subcontracts:

1. Drilling 10,375

G. Total Direct Costs: $20,096 H. Indirect Costs: re 1. 48.4% of G 9,726

I. G & A Costs:

1. 13.5% of G 2,713

J. Total Direct, Indirect and G&A Costs: $32,535

K. Fee:

1. 5.5% of J 1,789

L. Total Project Price - UURI: $34,324

M. University of Utah Indirect Costs:

I. 20% of L 6,866

N. Total Project Price: $41,190 PRELIMINARY INFNMATION BUDGET

Phase IV - Reporting

Amount

A. Salaries and Wages:

1. Salaries $2,685 a. J. N. Moore - 94 hours b. Draftsperson - 16 hours c. Secretary - 80 hours

B. Employee Benefits:

1. 42.8% of A1 1,149

C. Consultant (EnviroSearch, Inc.):

1. David Nelson - 170 hours 9,350

D. Supplies:

1. Office and Drafting Supplies 150

E. Total Direct Costs: $13,334

F. Indirect Costs:

1. 48.4% of E 6,454

G. G & A Costs:

1. 13.5% of E 1,800

H. Total Direct, Indirect and G&A Costs: $21,588

I. Fee:

1. 5.5% of H 1,187

J. Total Project Price - UURI: $22,775

K. University of Utah Indirect Costs:

1. 20% of J 4,555

L. Total Project Price: $27,330 __ UNIVERSITY OF UTAH RESEARCH INSTITUTE go.

• -0 • t EARTH SCIENCE LABORATORY 391 CHIPETA WAY, SUITE C SALT LAKE CITY, UTAH 84108-1295 TELEPHONE EV -524-3422

December 1, 1987

Ms. Joan Poland WINCO P. O. Box 1625 Idaho Falls, ID 83403

Dear Joan:

Enclosed please find the chemical analyses of the sample we collected from the fir storage tank area at CPP 621. i have also enclosed a list of the background values for the area. Note that the background F values are in ppm, no %, as was previously indicated.

Sample number 8 was collected beneath the drain in the pit. The remaining samples were collected at various locations around the concrete footings.

Sincerely,

oseph N. Moore

JNM:kr encl. (k,-V

\ v.' C.7 U,A?(' ,t ' CI o SITE M DEpTH IN INCHES % MO/STURE Ph Prim F ppb Hg F-J. „I -a 0-6 4.68 8.53 191 40 CA.) lb 24 3.51 9.30 62 54 w:a 2a 0-6 4.19 9.73 34.6 21 2b 24 4.11 8.08 30.4 93 3a 0-6 5.08 8.55 24.8 25 3b 10-15 5,58 7,09 56.7 <20 4a 4-6 4.29 8.03 35.4 41 4b 18-21 3.06 7.61 23.2 22 5a 4-6 6,47 7.00 29.2 <20 5b 18-24 3.88 6.60 45.0 <20 6a 4-6 4.99 6.59 42.2 <20 6b 18 4.37 6.68 33.9 35 8a 0-6 24.91 4.24 55.7 <20

S/TE 4 ppm As ppb Se ppm Ba ppm Cr ppm Pb ppm Cd ppm Ag la 9.0 125 230 41 30 <4 2 lb 4.0 125 110 14 <8 <4 2 2a 8.0 267 190 27 <8 <4 2 2b 6.0 142 190 28 <8 <4 2 3a 9.0 142 250 37 9 <4 2 3b 10 330 360 44 <8 <4 2 4a 8.8 198 180 44 19 <4 2 b 6.0 193 170 28 <8 <4 2 a 8.8 195 390 43 22 <4 2 5b 10 280 400 28 <8 <4 <1.6 6a 5.3 160 250 31 <8 <4 <1.8 6b 6.0 408 290 28 <8 <4 2 8a 40 2908 693 100 821 <4 2 TABLE 3

Background concentrations of 140,-A, F, Al, Ba, Cr, Pb, Cd, Ag, Zr, Hg, As, and Se in soil sampled froa locations outside ot the CPP coeples,

NO3-N F Al la Cr Pb Cd Ag Zr Hg As Se 5AMPLE Opel (rpm) (X) (PIA) (1110, (15Poi (PPA) (wpm) (OW (PA) (ppm) (nob)

Bkg 1" -- 200 25 12 <5 <2 43 5.6 484

Bkg 2" 270 32 16 <5 <2 19 5.t 405

8kg 3" 270 33 17 <5 (2 27 6.5 467

Bkg 4' 250 34 12 (5 (2 28 7.0 341

860258 0.86 0,15 1,31 280 28 <10 <5 (2 <5 25 5.6 113

860259 0.72 0.32 0.81 380 26 <10 <5 <2 10 57 7.6 252

860260 0.41 0.12 1.60 240 28 <10 (5 <2 9 23 6.4 695

0261 0.43 0.42 0.79 220 18 (10 <5 (2 12 30 6.2 236

860264 0.27 4.00 1,60 230 <10 <5 <2 7 21 6.0 102

060265 0.25 0.28 0.75 21, <10 <5 <2 10 46 7,6 227

Average (X) 0.49 0.88 1.14 255 27 12 <5 <2 9 32 6.4 332

St.Oev.(s.d.) 0.25 1.53 0.41 51 5 3 2 13 0.8 184

1 4 2ial.) 0.98 3.94 1.96 358 38 17 - 14 57 8.0 701 t A. Defer to Final Report: PPR Warehous Site, Idaho Chemical Processing Plant: Earth Science Laboratory, Sept. 1986 for the locations of samples 8kg t to 4.

19 ~ '71 C. ri. I. _, C I 1-- ,-- INELm National Engineering Laboratory 1_ kJefil‘ir 0 4 '11)E1 1-- DJP-01-87 c:

From D. J. Poland ERC r COPY Phone : 6-3650/CPP-630 Nm . September 1, 1987 SuNect Characterization of the CPP-621/637 Areas

(Of"' Ra, c1, To J. W. Ruffner GP&CE Projects

The characterization of the solid waste man gement units (SWMUs), CPP-621 chemical storage area and the CPP-637 courtyard (spill 1978), requested by Projects because of pending construction (secondary containments) and conducted by the University of Utah Research Institute (UURI) (report attached), has been completed and the following is a summary of this characterization:

• Sample analyses have been statistically compared to the concentrations found in the background samples. These analyses indicated higher than background levels of mercury In the three aluminum nitrate French drains, higher than background levels of fluoride in the hydrofluoric acid containment, higher than background levels of nitrate and lead in the chemical trench, and higher than background levels of nitrate in the sludge pit. The analyses results of the soil samples collected from the CPP-637 courtyard area indicate higher than background levels of zirconium, aluminum, chromium, and arsenic.

A cleanup was conducted in the CPP-621 aluminum nitrate French drains. This remedial action (conducted by UURI) draft final report is attached and states in part the following:

• Soil excavated from the three aluminum nitrate French drains contained mercury at greater than background levels.

• The average mercury concentration of unexcavated soil is <58.3 ppb. This value is approximately equal to the background mean + 2 standard deviations and is within the range of Hg contents of soils developed over volcanic rocks.

In conclusion, the following assumptions can be made:

• The aluminum nitrate French drains have been cleaned up to background levels. Construction may proceed in this area but be aware that construction in a solid waste management unit is always at a risk without prior EPA approval. See attached letter from A. J. Matule to

®! Westinghouse Idaho Nuclear Company. Inc. cep: zs C: J. W. Ruffner C OJP-01-87 September 1, 1987 Page 2 cr

P. I. Nelson for information on risks involved. Since the characterization of the sites following cleanup has been conducted by a recognized expert with experience in these activities, Environmental Engineering believes the risks of non approval by EPA to be minimal.

Further characterization and/or cleanup is necessary in the HF containment, chemical trench, sludge pit, and CPP-637 courtyard. However, in the CPP-637 courtyard a temporary stainless steel catch basin may be installed under the two zirconium feed tanks until a characterization/cleanup has been conducted. Additional guidance for the HF pit will be forthcoming.

No hazardous constituents above background levels were detected in the area of the nitric acid tanks and sulfuric and hydrochloric acid containment. Construction may proceed in these areas but be aware that construction in a solid waste management unit is always at a risk without prior EPA approval. However, because the characterization was conducted by a recognized expert with experience in these activities, Environmental Engineering believes the risk of non approval by EPA to be minimal.

If you have any further questions concerning the above, please call me at 526-3650.

D. J. Po4/and, Environmental Engineer R&ES Environmental Engineering

/tlr

Attachment 3- (v 001.49

CPP-621 PRELIMINARY LABORATORY ANALYSIS RESULTS

SAMPLE #

ANALYSIS #8-1 #1-2 #31 #27 #33 Bkg #1 Bkg #2 Bkg #3 Bkg #4

pH 8.95 9.02 5.23 4.26 8.47 8.70 8.58 8.47 8.48

*Ba 0.73 0.084 0.28 0.194 0.76 200 270 270 250

*Cr 0.027 0.026 0.010 0.011 0.015 25 32 33 34

*Pb <0.054 <0.054 0.069 <0.054 0.11 12 16 17 12

*Cd 0.005 0.007 0.035 0.014 0.009 <5 <5 <5 <5

*Ag <0.004 <0.004 <0.004 <0.004 <0.004 <2 <2 <2 <2

*Nitrate 7.33E-1 3.74E+0 1.95E+0 2.71E+2 2.52E+0 1.3 2.0 2.8 2.2

*Fluoride 0.3 0.3 0.15 0.15 0.4 0.12 0.58 0.58 0.46

*Chloride 4.23E-1 3.27E-1 <1.8E-1 9.94E-1 2.39E-1 0.7 1.0 1.0 0.7

*Sulfate 3.71E+0 2.67E+0 8.07E-1 1.21E+0 3.71E+0 1.6 1.4 <1.0 2.0

*A1 0.44 0.52 0.41 0.18 0.43 ------

* Units = ppm C IrObon C0055110.01 mere err,

&miffs 50 Beira 1000 Cameo 1 0 Ovesroyy• 5 0 WI 10 martin 0 3 0.11flig• 1 0 1.1V01 1 0 loony 0 02 1.•0•1•11 0 4 666660 11.•0 1 W 10 0 1•. why,. 0 f a D 00 :4 1 1, 1 0

1 41 re 1 1 Contittttt a lad C ttttt union For If le 00000 y 3/246 /6 ir ge16-:±a

/-,.? /2.).5 34//eg /0?: /S- nt

47/- 171-16 [A) 9/34.6 015 0-n— zi/e cia /L.

5- ro ct., ;cc( r 9 4046 /0:5-5 1 V.2- rAzi 0 e- 4-i;

cep- #33 /86 ?

5,17-2,1&E )/43-444 a -bit 7r7trient e7 41 I / FL-Je, gc_,,//ftiSt „0--x.c+FA 44)._ 5r /19,-. 41/e tu; Ltut „,41- • /3 ) sp--5

1/6

347

/ • 45-

31.7 0- /0 / •d-o

9/2-6 Q-01- / as /d a:to .2,2- _2_ a, -lc

344 0R.S. 3;3c

341? 423. -2_ to-z; ,) ,_el tip' I 4 /irk* D4ipt 3-5 - 9 -/ r 9- a- i -i0 ( /6 I-- /0 -/ 3-5 -a 01_ i.a le • g--io CO i\k-- iy iv( iii-/ -/.0 0,1 /7 1 ,- / --/,0

.26- / E - /6

26 -/ 3-s - .24 -0?__ Se- -/0 .2; la 43--.71-/ -..S ‘>2.7 dol. a- / 0 .28 021-1 3-c- ,2-g-,Z, S- /0 .2Y' .29- / 3 - s— a9- a_ E.-ft) 30 3o - / 3 5- 3o -..Z_ a-io 3/ 3/ - / 3-5 - avarafiro2._ E--/c 3 Sa-/ 3-S- 32-,2,4 0- - / 6 33 3- / 3-5 - • "33-,2_ E--/O 3el :34/ -/ 3-5 --- 3Y-a-.. 2-10 aS" e5 _ 1 3 S-- s-- .z... E-- /6 36 36 -/ .-,s - 36-0,1_ 2-. I 0

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04 gigs- toa 5.a2 *Si 8.41 E.70 2,57 2,41 gslig .....0 ti P3a- -0,73 0,0E11 04 - -0-igy 046 2..0.0 alo C4.0- ago - 1-4. _ %a 1-1 el 0.0,a? 0,61.24 S.0/0 o.eme. o.ofs- 425-: -132_ 1, 33 3lit Uti

g"l -`%°.°5,`4'0.051 -6. de?40.as, . 0./f /2- /4 / /.2_

e-cl. 0 005 0,607 0,035 0.0y O.067 45- 45 C5 4 C d- C- /la 4a cby

Vr' Flmortie, 0,3 0.3 0,15 04.0 a SI 0.12_ 0 55/ 0.58 0 '4

it thooift V.23E-1 3.27g-I 4/SE-1a2.396-I 0,7 1.0 1,o 0,7 A , Sa Rile, .316-to 2-416-to 8.076•1 hal Ef0 3,71E4-0 1. 6 /. 4

‘7"--

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,F6(346 705zz azre dere/ a-et S lo 6E6 V ea-a/CS:00 64,1

#F60;s-,cy 02 1.° Steric;e_ 73 3t7 64'6 /0" eiz7/9 sE. 10a/774eid.fece

c.763 //oZY 7343. f..3 cR7 aZ,' AL) //A/6 el 34. ket) Saceetc, 3`Ler ( . 4-0:e1) igr-P-4A+e Pirc yorcei [lkA;\ Westinghouse Idaho T c-- , 7:,- . \ -a- Nuclear Company. Inc. rt '.1 1 77- ; (-) I FORM WrJCO-5351 (966) REQUEST FOR CHEMICAL ANAL ?IS t. t 1 ri i INSTRUCTIONS ON REVERSE SIDE — PRINT CLEARLY — ON oHAI4ACTiR PR 130X ' . c.o 'I CI \ ?: !, i — 1 I rii 1 i i i 1 g ,---. = Assigned by Analytical. All others roust be completed. * Log Number 1 —..i t , xx---... ,„...___— -- it 1 I it'll Title for this Request 13,1(61), 1,- ,q, , , , i Batch Number (if any))t_..----7 -- ---

GWA Number 1/ 4,1 ,) A -,c,31C, 70, /,o, *Log Coordinator 11111111.11

Requester ,15, ,S, ,Pic, L-4611A),/, 11111 Telephone i i i 1:1 -,3,6 50,

Address le,PIP- ,6,3,0„ , 1 Samples/Data Classified? 0 Yes fell No

Quality Level: E I 0 II E III LI IV EPA Procedures Required? 1 Yes 0 No (See Instructions) (See Chain-oVCustody on back)

Sample Radioactivity (See Instructions) HP Initials'i t— i 4P•I , , i mR/h

*Hazard Index . 1111111 Alpha Emitters Present? E Yes /No

Total U235 Coment: Concentration i , i 1 1_4 mg/mL Volume of Sample , i ) i 1 4, i_i mL

Comments (Include hazardous chemicals — HF, Cd, strong acids, etc. — matrix of samples. expected concentrations, special instructions, etc.):

771.-1, /IA

ANALYSIS DESIRED 0 Sample Name ef 5ofre— Rt ski las Sr-90 Pc -.7.3"i Anv?S‘i ,7 IR 6-,, 01,;', 4,5T , , 1 i -z--I ,...--1. ,..,- ‘z oy 1 fr-C•16,0,..Z 6, V, , , , , —CI _i__I LI __Lzi e're,10 14„.;6,0, , , , , / / LI LI / 2_1

/ / 6. ---.1 ikle.., 10 ic;21-6 I 0711 I 1111-1 /----1 4Z—I v 71 IF1610 14;1157% a I I I I z--/I 47_1 .Z_I .Z_1 / / v ii40 i.:2141 i 1- 1 1 -i 1 --I .Z_I _Li Filni010-2.15781 1 1 i 1 i / _Li / v

/1 / IM6 101.11,31 I I I I —Z—I

11111111111

1111111111( —I _I

Approved Date ),-,/;),) wisp) 5351 (9-86) (back) REQUEST FOR CHEMICAL ANALYSIS

INSTRUCTIONS SAMPLE ACTIVITY: If not radioactive, enter "COLD", if less than background and the origin of the sarnple is unknown enter a

HAZARD INDEX: A calculated number which is used as a guideline in determining the appropriate type of radionuclide work place. This will be calculated oy Radiation Technology personnel at the request of Analytical Chemistry personnel. The Requester must supply the following information for the calculation: 1) The quantity of radionuclides present 2) The physical/chemical form of radionuclides present 3) Type of sample container.

ALPHA EMITTERS PRESENT: If the sample contains any alpha emitting radionuclides, please check "yes", even if the sample contains a very small quanti- ti Also list the quantity and type (if known, or your estimate if unknown) in the comment seclion.

COMMENT LINES: Provide information related to the request. If more space is needed, attach a separate sheet.

ANALYSES DESIRED: List the analyses to be perforrned at the top of the table and check (.-) in the small box opposite the sample name, those analyses :o oe performed on each sample. SAMPLE NAME: If names containing more than 10 characters are used, the requester will be asked to code the samples when they are delivered to the laboratory. ne code number will be used in the computer and on the final report form so the customer should keep his copy of the code.

OUALITY LEVEL: See SOP WE-1, Quality Level Designation. requirements. Analytical Quality Levels I, II. and III provide the level of quality listed below. Levels I. It and III require negotiation with Analytical to establish a quality control program suitable for your samples. Most non-process related samples are Duality Level IV. °utility Level I: Results are produced by two independent analysis methods which are tested statistically against pre-established limits at specified con- fidence levels. Level IL Results are produced with a bias correction and precision estimate obtained through a quality control program and the results are tested against pre-established limits at specified confidence levels. Level III. Results are produced with a bias correction and precision estimate obtained through a quality control program. Lt, JO IV: Results are produced without bias correction and precision estimate.

CHAIN OF CUSTODY RECORD (Required for all EPA Analyses) SArnalers ISig Lure) )1010.. Date/Tim SwF!. _ed _i_ 4//647 I 42:e4"ciaelL- /art La. Pe'narks gsr,(2 s, ,.. 119-1e,,S n nq s ec by. (Signatt. c_nnre. j Dai /Time Received by: (Signature) f rd...... , K/cg e X? ; 2 I /42 : RS 190 . Re.alqUIS Dy' (Signature) Dale/Time Received by: (Signature)

I Reiinquisned by (Signature) Date/Time Received by: (Signature)

I Reonquisnea by. (Signature) Date/Time Received GT (Signature)

I Relinquished by: (Signature) Dale/Time

I artet.to lor Laboratory by: (Signature) Date/Time

±1a--tC2i/e 4/% 0 I/ 7771; 10 ovs A-ct-ed- /i e Lie vet( (72._)_/&

UNIVERSITY OF UTAH RESEARCH INSTITUTE

EARTH SCIENCE LABORATORY 391 CHIPETA WAY SUITE C SALT LAKE CITY, UTAH 84108-1295 TELEPHONE 801-524-3422

January 20, 1987

Westinghouse Idaho Nuclear Company 1955 Fremont Ave. P.O. Box 4000 CPP 630 Idaho Falls, ID 83403

Attention: Joan Poland

REPORT

Sample pH ppm ppm PPm ppm Cl F SO4 NO3

Background 1 8.70 0.7 0.12 1.6 1.3 Background 2 8.58 1.0 0.58 1.4 2.0 Background 3 8.47 1.0 0.58 < 1.0 2.8 Background 4 8.48 0.7 0.46 2.0 2.2

These numbers represent hot water soluble fraction in the solid sample. 100 g of each sample was leached with 100 ml of water.

/9„,...LAZ Ruth L. Kroneman Chemist

RLK/cd

/ (A1.- '/

FINAL report, for SOIL CPR621 , r..‘- / ', - .e> ‘.<:- ` i dic• „ REPORT FOR : DJ POLAND LOG NUMÐE.R -. : 1A(357',. /.\ ADDRESS : CPP 630 PHONE NUWER.1.4 6-3t50 \\ \\ \ - / • S. N, / DATE RECEIVED : 11/25/86 DATE COMPLETEDr. .01/15127., , TIME RECIEVED : 15:17 TIME COMPLETED:\C 111N / 7 \ .., \ 6/ GWA CHARGED : 16110-530-010 REVIEWED BY : R.,1. DE/MHER \./ MSA MR/HR : COLD SIGNATURE:

HAZARD INDEX: NONE

'YSIS METHOD SAMPLE ANALYST RESULTS FOR 11257

NITRATE 8978 4-8-1 CGC 7,3263E-01 UG/ML NITRATE 8978 4-1-2 CGC 3.7445E+00 UG/ML NITRATE 8978 4-31 CGC 1.9537E+00 UG/ML NITRATE 8978 4-27 CGC 2.7066E+02 UG/ML NITRATE 8978 4-33 CGC 2.5235E+00 UG/Mi. FLUORIDE 8973 4-8-1 CGC 0,3 UG/ML FLUORIDE 8973 4-1-2 CGC 0.3 IJG/ML FLUORIDE 8973 4-31 CGC 0.15 UG/ML FLUORIDE 8973 4-27 CGC 0.15 UG/Mt FLUORIDE 8973 4-33 CGC 0.4 UG/ML CHLORIDE 8974 4-8-1 CGC 4.2308E-01 UG/ML CHLORIDE 8974 4-1-2 CGC 3.2697E-01 UG/ML CHLORIDE 8974 4-31 CGC 1.8072E-01 UG/ML CHLORIDE 8974 4-27 CGC 9.9377E-01 UG/ML CHLORIDE 8974 4-33 CGC 2.3850E-01 UC/ML SULFATE 8979 4-8-1 CGC 3.7140E+00 UG/ML SULFATE 8979 4-1-2 CGC 2.6644E+00 UG/ML SULFATE 8979 4-31 CGC 8,0740E-01 UG/ML SULFATE 8979 4-27 CGC 1.2111E+00 UG/ML SULFATE 8979 4-33 CGC 3,7140E+00 UG/ML PH 8010 4-8-1 JHG 8.95 PH 8010 4-1-2 JHG 9.02

REP 27 O O r- ANOL YSIS LLi ANALYST RESULTS FOR 11257 001726 000 C4 . CO c' ODCDCOC4 CO c> Cu IIIIIIIIIIIIIII111111111!1111111111111 , . - 2 C. CD c>c).-1 r C4 Cr CL , 0 • ' D 7 - r. c CO CD cr 1-4 CL • Ol D 0 0000 7 7 7»> 6 = '0 I: ZZZZ C7C7L^CDL^ 03 it cococorococr 1Y. IC ZD hi _J -

:7 6 111 CJ cn _J C4 CC ZD cc Fi D: JJJ GQG6 C4 1 . 6 7 :3 7 riCCOC.4 cn CC H cr 1: C4 CO ri - -1 3 7 I: c Z r.700G ZD 04 H co _J C4 CC ZD N ri 6 7 I: ZD Z L _ CC CO O 1: C4 CO C ZD J hi O' 0=000 6 0 = /7" r, 1: 03 CD cr 1: C4 C4 CC CO ZD ri Fl CD 6 0 (-3 2222 C4 CD IC CC O cr C4 C4 C4 CC CD hi yr 1 . 6 0 CD 03 cr C4 C4 3: ZD OC. H c- CC CD -1 z c C) CD 1: C4 CC CO ZD H cr cr C4 C4 CD CC C> 0 0 2 ,-1C0000-. 0 Z N. cr cr C4 C4 CC CO CC CO C> O cr cr rq L C2 CO C.) 0 6 .4 OCO.N00 • in CD _J C4 OC cr cr r CJ CD /7 CD ,J C3 CC CO CO Tr C4 C2 yr 6 0 C> CD N, CC CO yr cr C4 C4 yr CD CC CO cr cr C4 CO Z> Li! 6 7777 C ID ca CC CO r, cn cr FA -J Ld C4 C> yr :7 O c> CD CC CO r, cr -4 LU C4 CO C> Z> cn Fi yr :a 6 "N. ZD O Uj CC CO r, cr En LU C4 C.4 hi N., yr 6 0 CD O c> -a col CC CO r,cocoonco Z> cr C4COCOCOODCO LO CO CO hi yr • '40 trIZZZ z C.4 Ul cr W _J C4 JJ C4 CD OD LULLILUWIJJ CD W CD cn ID- cr -J Ld C4 CO C.J h- C> • 11111

0 0 C4 CO - = CO N.. F- C4 CD ZC or... W -04 cr cn C3 C4 C4 CD h- U. 1..• a 0 0 r. -43 C4 CD CO O r< la_ _J - CC W CD CD T rn -J __I cn a: cr C4 CL h- W 0 D 0 7 0 tiCJ r• 2 /: C4 c) - cc. C3 14.1 C4 CO h- No CD CD 0, r, __I C4 cr -j a: F- Lu C4 CL CJ • D

-J CN ,-1 CJ CD 41 t- I: NO - = CO CO CD Ci_ 7: CD _4 LD H co co cr cn Ld CL CO C> CJ >< _4 D Log Number: 11257 Page..: 1 of 5 •eated by..:D,R. TRAMMELL Date Cr..:11/25/86 — Time Cr..:15:17

1 Request Name:SOIL CPP621 G,WA/....“4716110-530-010 3 MSA...:COLD mr/hr 4 Requestor...:DJ POLAND Address1CPP 630 6 Phonet6-2650 O O HAZARD INDEX; NONE 10 F. 11 F IU oo 12 F 13 B 14 W 15 W 16 W L157 C e Index Meth Name of Results anallysis name EH]

1 9 8978 NITRATE 4-8-1 CGC +7.32625E-01 UG/ML 20 8978 NITRATE 4- 1 -2 CGC +3,74452E+00 UG/ML 21 8979 NITRATE 4-31 A CGC +1.95367E+00 UG/ML 22 3978 NITRATE 4-27 CGC +2.70664E+02 UG/ML 23 8978 NITRATE 4-33 CGC +2.52349E+00 UG/ML 24 8973 FLUORIDE 4-8-1 CGC 0.3 UG/ML -7= 8973 FLUORID9. 4-1-2 CGC 0.3 UG/ML 8973 :LUORIDE t CGC 0,15 UG/ML 8973 FLUORIDE 4-27 A CGC 0.15 UG/ML 29 8973 FLUORIDE 4-33 1 CGC 0.4 UG/ML 29 8974 CHLORIDE 4-3-1 CGC +4.23077E-01 UG/ML 30 8974 CHLORIDE CGC +3.26923E-01 UG/ML 31 8974 CHLORIDE 4-31 CGC 180723E-01 UC/ML 32 8974 cH1ORI9F CGC +9.913770E-01 UG/ML 33 8974 CHIORIDF 4-33 t CGC +2.33505E-01 UG/ML 34 8979 SULFATE 4-8-1 x CGC +3,71404E+00 UG/ML aa 8979 SHLFATP t CGC +2.66442E+00 UG/ML 36 9979 SULFATF t CGC +8.07400E-01 HG/ML 27 8979 SULFATE 4-27 t CGC +1.21110P+00 UG/MI 38 8979 SUIFATE 4-32 t CGC +2.71404E+00 UG/ML 39 8010 PH 4-8-1 A JHG =2,95 40 8010 PH 4-1-2 x JHG =9.02 41 8010 PH (-21 JHG -C.23 42 8010 PH 4-77 JHG =4,26 43 8010 PH 4-33 JHG =8.47 44 2130 ALUMINUM 4-8-1 RAS .44 UG/ML 45 2130 ALUMINUM RAS .52 UG/ML 46 2130 ALUMINUM 4-31 RAS .41 UG/ML 47 2130 ALUMINUM 4-27 RAS .18 UG/ML 48 2130 ALUMINUM 4-33 RAS .43 UG/ML 49 2240 CHROMIUM 4-8-1 RAS .027 UG/ML 50 2240 CHROMIUM 4-1-2 RAS .026 UG/ML 2. 2240 CHROMIUM 4-31 RAS .010 UG/ML 2240 CHROMIUM 4-27 RAS .011 UG/ML 2240 CHROMIUM 4-33 RAS .015 UG/ML 54 2560 BARIUM 4-8-1 RAS .73 UG/ML 55 2560 BARIUM 4-1-2 RAS .084 UG/ML -,c- 56 2560 BARIUM 4-31 RAS .28 UG/ML 57 2560 BARIUM 4-27 RAS .194 UG/ML 58 2560 RARTum 4-31 RAS RAs >069 ML

62 2820 LEAD 4-27 RAS <.054 UG/ML 3 2820 LEAD 4-33 RAS ,11 UG/ML 4 2480 CADMIUM 4-B-1 RAS 4005 UC/ML 65 2480 CADMIUM 4-1-2 RAS .007 UG/ML 66 2480 CADMIUM 4-31 RAS .035 UG/ML 67 2480 CADMIUM 4-27 RAS .014 UG/ML 68 2480 CADMIUM 4-33 RAS .009 UG/ML 69 2470 SILVER 4-8-1 RAS < .000 UG/ML 70 2470 SILVER 4-1-2 RAS <4004 UG/ML 71 2470 SILVER 4-31 RAS < .004 UG/ML 72 2470 SILVER 4-27 RAS < ,004 UG/ML 73 2470 SILVER 4-33 RAS < .004 UG/ML 82 8982 EP-TOX-LCH 4-8-1 314G =rnMPLrTED, 128 42 G / 2568 ML. 83 8982 EP-TOX-LCH 3HG =COMPLETED. 129.37 G / 2587 ML 34 8982 EP-TOX-LCH 4-31 JHG =COMPLETED, 131.70 G / 2634 ML 85 8982 EP-TOX-LCH 4-27 I JHG =COMPLETED. 120.66 G / 2417 ML, 66 8982 EP-TOX-LCH 4-33 3HG =COMPLETED. 131.39 G / 2629 ML WeslInghouse Idaho Nuclear Company, Inc. SPECTROCHEMICAL ANALYSIS FORM WINCO-5352 (12-84)

-ORD N 1r /9O LOG 0 &L I/Pis-7. '•;/ ANALYZED BY /161- - Ain' SPL. CODE Cia3b42 //,-/ APPROVED BY Qeyg DATE CHARGE N /6 //e, — — 020

SPL. ACTIVITY (mR/hr) REQUESTED BY fe c

30 DETERMINATIONS / •,- -erg /21 MC MAJOR = >5% NUMERALS = /in/ frc c.rc( ,-*e m = MINOR = < 5%> 0.1% t = TRACE = <0.1% it -e--/ t-/-2- -/-3/ 4-2-? i-z3

cc/ a , oer 0,0,7 0,033- 0, 6/1 1- 0, 009

& 0, 73 o. egg o • Lff v • /91- o ,"7e. C,-- o . oz7 a . att. 0. 0/0 (Lod 0.6 16—

re (v. oft •<- 6,, es21- a f en,9 1 0-0.64 O .//

ne !6.00 4 4 c-ocir e e...) 1- . o.o,016 <0.00f— A ,,ii- 0.5 -2-- 0.1-/ o ,ir a . 4-3

e-,4C.--- c c~ RENO OF CONVERSATION

Date: February 1, 1993 Time: 1400 hrs Commitment Made [ ] Yes [X] No

Person Calling: Bruce Culp Person Called: Joseph Moore

Representing: WINCO Representing: University of Utah Research Institute

Purpose of Conversation: Source of 4-X-X sample analysis in Chemical Storage And Zirconium Feed Tank Storage Area Final Report (September 1987)

Text of Conversation: I asked Joe about the chronology of sampling activities at the ICPP that UURI did in 1986 & 87. Joe referred to a report as we talked and confirmed that the samples in the September 87 final report were analyzed by UURI at the same time that the samples taken by UURI in April 87 were analyzed. He confirmed that these samples were not taken by UURI but were given to him by Joan Poland. He remembered Joan discussing that the samples were taken before by Hawley Bros. and remembered looking at the sampling locations still visible in the roadways. (These were the drill locations done by Hawley in March and April of 86, WINCO ERC DCN #01588).

Signedc Date: Feb 1, 1993

C-t-E 251) 0- NI /1 Golder Associates Inc. CONSULTING ENGINEERS

REPORT FOk THE IDAHO CHEMICAL PROCESSING PLANT DRILLING AND SAMPLING PROGRAM FOR ACID STORAGE TANK VAULTS CPP-757 AND CPP-727 AT SOLID WASTE MANAGEMENT UNIT CPP-45

Prepared for:

EG&G Idaho, Inc/Westinghouse Idaho Nuclear Company, Inc.

Prepared by:

Golder Associates Inc. Redmond/Richland, Wa

January 1991 893-1195.900

GOLDER ASSOCIATES INC. • 4104 . 148TH AVENUE N.E., REDMOND (SEATTLE), WASHINGTON, U.S.A. 98052 • TEL. (206) 883-0777 • FACSIMILE (206) 882-5498 • TELEX: 5106002944

OFFICES IN UNITED STATES • CANADA • UNITED KINGDOM • SWEDEN • GERMANY • ITALY • AUSTRALIA January 31, 1991 i 893-1195.900

TABLE OF CONTENTS Page No.

1. INTRODUC110N 1

1.1 Objectives 1 1.2 Organization of the Report 1

2. SITE BACKGROUND AND PHYSICAL SETTING 2

2.1 Idaho Chemical Processing Plant 2 2.1.1 Regional Geology 2 2.1.2 Regional Hydrology 2 2.2 Solid Waste Management Unit(SWMU) CPP-45 4 2.2.1 Location and Description of SWMU CPP-45 4 2.2.2 Location and Description of Acid Storage Tank Vault CPP-757 4 2.2.3 Known or Suspected Wastes Associated with Acid Storage Tank Vault CPP-757 4 2.2.4 Location and Description of Acid Storage Tank Vault CPP-727 8 2.2.5 Known or Suspected Wastes Associated with Acid Storage Tank Vault CPP-727 8

3. SAMPLING AND ANALYSIS 10

3.1 Objectives 10 3.2 Soil Sampling Methods and Locations 10 3.2.1 Sample Collection at SWMU CPP-45 Acid Storage Tank Vault CPP-757 10 3.2.2 Sample Collection at SWMU CPP-45 Acid Storage Tank Vault CPP-727 10 3.3 SWMU CPP-45 Site Geology 12 3.3.1 SWMU CPP-45 Acid Storage Tank Vault CPP-757 Site Geology 12 3.3.2 SWMU CPP-45 Acid Storage Tank Vault CPP-727 Site Geology 12 3.4 SWMU CPP-45 Sample Handling and Analysis 13 3.4.1 Sample Handling and Analysis, CPP-757 13 3.4.2 Sample Handling and Analysis, CPP-757 15 3.5 Quality Assurance/Quality Control 15 3.5.1 Blanks 16 3.5.2 Field Duplicates 16 3.5.3 Performance Audit Samples 19 3.6 Data Validation 19 3.6.1 Holding Times 19 3.6.2 Instrument Calibrations 19 3.6.3 Project Detection Limit Goals 20 3.6.4 Quality Control Data 20 3.6.5 Blank Data 20

Golder Associates January 31, 1991 ii 893-1195.900

TABLE OF CONTENTS (Continued)

4. NATURE AND EXTENT OF CONTAMINATION 22

4.1 Assessrnent of Background Data 22 4.2 Results of Inorganic Analysis for Solid Waste Management Unit CPP-45 24 4.3 Results of Organic Analysis 24 4.4 Results of General Chemistry Analysis 24

5. HEALTH AND ENVIRONMENTAL ASSESSMENT 26

5.1 Identification of Toxic Contaminants 26 5.2 Identification of Exposure Pathways 27 5.3 Identification of Receptor Populations 28 5.4 Human Health Assessment 28 5.5 Environmental Assessment 30

6. SUMMARY AND CONCLUSIONS 31

6.1 Summary 31 6.2 Conclusions 31

7. REFERENCES 32

LIST OF TABLES

2-1 Analysis of Preliminary Surface Sampling SWMU-45 Add Storage Tank Vaults CPP-757 and 727 7 3-1 Target Compounds/Analyte List, Solid Waste Management Unit CPP-45 14 3-2 Field Duplicate Analysis Results, Solid Waste Management Unit CPP-45 17 3-3 Performance Audit Sample Analysis Results, Solid Waste Management Unit CPP-45 18 4-1 Background Concentrations of Metals in Soils Sampled from Outside the ICPP Fadlity and One-sided Normal Tolerance Interval(s) 23 4-2 Solid Waste Management Unit CPP-45 Sample Analysis Results (results in mg/Kg) 25 5-1 Summary of Health and Environmental Assessment for SWMU CPP-45 29

Golder Associates Tanuary 31, 1991 iii 893-1195.900

TABLE OF CONTENTS (Continued)

LIST OF FIGURES

2.0 Site Plan 3 2.1 Solid Waste Management Unit CPP-45, ICPP Site Plan 5 2.2 Solid Waste Management Unit CPP-45, Site Plan 6 2.3 Previous Sampling Locations at SWMU CPP-45 HCl/I-12SO, and HF Storage Tank Vaults 9 3.0 Sampling Locations at SWMU CPP-45 HCl/H2SO4 and HF Storage Tank Vaults 11

UST OF APPENDICES

APPENDIX A Borehole Logs APPENDIX B List of Compounds Analyzed APPENDIX C Laboratory Reports Part 1, Laboratory Inorganic Analysis Results Part 2, Laboratory Organic Analysis Results Part 3, Laboratory Method Blank DatWField Blank Data

Golder Associates January 31, 1991 1 893-1195.900

1. INTRODUCTION

1.1 Objectives

The objectives of the sampling and analysis program conducted by Golder Associates Inc. (Golder Associates) at the Solid Waste Management Unit(SWMU) CPP-45 were to evaluate the nature and extent of soil contamination of the known or suspected wastes in the add storage vaults CPP-757 and CPP-727 and in doing so characterize the vaults to determine whether any remediation under RCRA is required. This work was performed in accordance with the Technical Work Plan for the Idaho Chemical Processing Plant Soil Sampling and Analysis Program at Solid Waste Management Unit CPP-45 (Golder Associates 1990a, 1990b).

1.2 Organization of the Report

This report presents general information on the site and the physical setting, a description of sampling and analysis procedures, a description of the nature and extent of the contamination, a health and environmental assessment and a summary and conclusions. The conclusions detail our recommendations for further work at the site. Borehole logs and laboratory analytical results are presented in the Appendices.

Golder Associates January 31, 1991 2 893-1195.900

2. SITE BACKGROUND AND PHYSICAL SETTING

2.1 Idaho Chemical Processing Plant

2.1.1 Regional Geology

The Idaho Chemical Processing Plant (ICPP) is located in the southern portion of the Idaho National Engineering Laboratory (INEL) site that occupies approximately 890 square miles of the northwestern portion of the Eastern Snake River Plain in southeast Idaho (Figure 2.0). The plain is a structural and topographic basin approximately 200 miles long and 50 to 70 miles wide. Surficial sediments range from 0 to 345 feet thick at the INEL. Underlying the surficial sediments are 2,000 to 10,000 feet of basalt flows, rhyolitic rocks, tephra, and interbedded alluvium and lacustrine deposits (Mundorff et al., 1964; Bartholomay et al., 1989; Pittman et al., 1988).

The ICPP is located on alluvial sediments deposited by the Big Lost River or on fill materials. Surficial sediments at the ICPP can be divided into two distinct layers. The coarse grained surficial layer extends to a depth of 35 to 40 feet and is composed of sands and gravels with a trace of silt and clay. The underlying layer is made up of clayey sands and sand-clay mixtures and ranges from zero to ten feet in thickness and overlies the Snake River Plain basalts. The contact between the basalts and the overlying sediments generally occurs at a depth of 45 to 50 feet below the original land surface (WINCO 1989a, 1989b).

Sedimentary interbeds are common within the Snake River basalts. In the area of the ICPP, a 15 to 30 foot thick clayey interbed occurs at a depth of approximately 110 feet below land surface. The sequence of interbedded basalts and sedimentary interbeds continues to well below the water table. There is evidence of a sedimentary interbed at a depth of 750 feet below land surface (WINCO, 1989a, 1989b).

2.1.2 Regional Hydrology

Surface Water

The Big Lost River is the major surface water feature on the INEL with its headwater located west of the site. The Big Lost River flows to the southeast past the town of Arco, Idaho onto the Snake River Plain then turns to the northeast flowing onto the INEL and terminating in three playa lakes. Where the river flows onto the plain, the main channel branches into many distributaries and the flow is spread broadly, losing water by infiltration into the channel bottom (Pittman et al., 1988). The Big Lost River is ephemeral with flow onto the site only during periods of high runoff. The INEL Diversion Dam is located approximately 9 miles upstream from the ICPP and was designed to control flooding on the INEL site by diverting water into designated spreading areas.

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SIC SOUTHERN ROTE O tc. wa.riono, EXPLANATION Selected Facilities at the Idaho National Engineering Laboratory

CFA - CENTRAL.FACILITIES AREA EBR-1 EXPERIMENTAL BREEDER REACTOR N NO. I ICPP - IOAHO CHEMICAL PROCESSING PLANT CTF CONTAINED TEST FACIUTV NRF - NAVAL REACTORS FACILITY 4ra. (formerly cad Loss of RWMC RADIOACTIVE WASTE MANAGEMENT Fluid Test Facility—WET) COMPLEX INEL BOUNDARY TAN - TEST AREA NORTH a FACILITIES TRA . TEST REACTORS AREA V TOWNS ANL-W ARGONNE NATIONAL LABORATORY-WEST

FIGURE 2.0 SITE PLAN (atter Bareciomay, et al. 1989) EG&G/DRILL & SAMPLE SUMMARY SWMU CPP-45/10 PROJECT P. 8911193900 DWG.tC.254720ME laain DRAWN DC Golder Associates January 31, 1991 4 893-1195.900

Hydrogeology

The depth to the water table of the Snake River Plain aquifer in the area of the ICPP is approximately 455 feet below land surface based on 1990 water level measurements made by Golder Associates. The direction and rate of groundwater movement in the vicinity of the ICPP is documented from monitoring contaminant plumes in the Snake River aquifer. The rate of flow ranges from 5 to 15 ft/day in a direction from north-northeast to the south- southwest (Pittman et aL, 1988).

Two perched water tables are known to exist at the ICPP. The geologic layers responsible for these water thbles are at the interface between the surficial sediments and the top of the uppermost basalt layer, and at the interface between the 110 foot interbed and the overlying basalts. The direction of flow and extent of these perched zones is not known.

2.2 Solid Waste Management Unit(SWMU) CPP-45

2.2.1 Location and Description of SWMU CPP-45

SWMU CPP-45 is located north of the CPP-607 building at the ICPP and is illustrated on Figures 2.1 and 2.2. Acid storage tank vaults CPP-757 and CPP-727 are located in the south portion of SWMU CPP-45. The storage tanks have been removed from storage vault CPP- 757 only.

2.2.2 Location and Description of Add Storage Tank Vault CPP-757

Acid storage tank vault CPP-757 is located in the southeast portion of SWMU CPP-45. The storage vault walls are constructed of concrete with an uneven, coarse gravel floor. The vault is approximately 14 feet wide and 39 feet long with a maximum depth of about 6 feet.

The vault once contained hydrochloric acid (HO) and sulfuric acid (H2SO4)storage tanks. The tanks have since been removed and the vault is presently empty.

2.2.3 Known or Suspected Wastes Associated with Acid Storage Tank Vault CPP-757

A spill of about 300 gallons of concentrated sulfuric add reportedly occurred in 1986. Other spills of hydrochloric ac➢d or sulfuric add may have occurred within the vault and not been reported. Hydrochloric add and sulfuric add could be classified as characteristic hazardous wastes (D002) due to corrosivity.

Preliminary surface sampling of the soils at two locations underlying the storage tank vault (Figure 2-3) had been performed prior to this investigation (UURI 1987). Analysis of these samples for pH, mercury, and nitrate-nitrogen indicated the presence of low concentrations of mercury and nitrates. Mercury concentrations were above a preliminary determination of background levels at one location (Table 2-1).

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FIGURE 2-1 SOLID WASTE MANAGEMENT UNIT CPP-45 ICPP SITE PLAN EG&G/DRILL 8SAMPLE SUMMARY SWMU CPP-45/ID PROJECT NO. 993.1195100 DWG. NO. 29484 DATE 129/90 DRAWN TK Golder Associates FD = French Drain

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FIGURE 2-2 SOLID WASTE MANAGEMENT UNIT CPP-45 SITE PLAN EG&G/DRILL & SAMPLE SUMMARY SWMU CPP-45/1D PROJECT NO B*11-1191.Z0 DWG. NO tarn DATE 1/28.111 DRAWN DC Golder Associates 893-1195.900

TABLE 2-1

ANALYSIS OF PRELIMINARY SURFACE SAMPLING SWMU-45 ACID STORAGE TANK VAULTS CPP-757 AND CPP-727*

Acid Storage Tank Vault CPP-757

Sample No. Sample Depth Soil pH No3-N (ppm) Hg (ppb) 860211 0-4" 8.78 1.13 55 860212 0-4" 8.85 1.14 56 860213 24" 9.21 0.17 82 860214 24" 8.45 0.60 14

Acid Storage Tank Vault CPP-727

Sample No. Sample Depth Soil pH F (ppm) Hg (ppb) 860208 0-4" 9.29 30 25 860209 0-4" 2.79 2900 14 860210 0-4" 3.41 88 15

"UURI 1987a

Golder Associates lanuary 31, 1991 8 893-1195.900

2.2.4 Location and Description of Acid Storage Tank Vault CPP-727

Acid storage tank vault CPP-727 is located in the southwest portion of SWMU CPP-45. The vault walls are constructed of concrete with a flat, native soil floor with a cover of limestone rock directly below the tank The vault is approximately 16 feet wide, 27 feet long and 8 feet deep.

The vault contains a horizontal hydrofluoric add storage tank. Associated valves are located at the northwest and northeast portions of the vault.

2.2.5 Known or Suspected Wastes Associated with Acid Storage Tank Vault CPP-727

A documented spill of approximately 4 gallons of hydrofluoric acid occurred at the west end of the vault and other spills may have occurred but are not recorded. Hydrofluoric acid is classified as a listed waste (U134).

Preliminary surface sampling of the soils at three locations within the vault (Figure 2-3) had been performed prior to this investigation (UURI 1987). Analysis of these sample for pH, metals and fluoride ions indicated the presence of hydrofluoric acid in the western and northern portions of the vault (Table 2-1).

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I 860212 860214 J Condensate Dry Well \\NN Approximate SWMU Boundary

CPP 607

0 10 20 Feet • Borehole Locations

FIGURE 2.3 PREVIOUS SAMPLING LOCATIONS AT SWMU CPP-45 HCl/H 2SO4 AND HF STORAGE TANK VAULTS EG&G/DRILL a SAMPLE SUMMARY SWMU CPP-45AD PROJECT NQ 003-1195.903 DWG. NO 26473 DATE yam DRAWN DC Golder Assor' 'Is lanuary 31, 1991 10 893-1195.900

3. SAMPLING AND ANALYSIS

3.1 Objectives

The objective of the sampling effort at SWMU CPP-45 acid storage containment vault CPP- 757 and vault CPP-727 was to determine if adds or miscellaneous chemicals have been released to the soil and are presently in concentrations above regulatory action levels requiring RCRA remediation prior to any further construction activities.

The characterization efforts focused on the tank and valve locations within the containment vault, considered the most likely sources of potential contamination.

3.2 Soil Sampling Methods and Locations

3.2.1 Sample Collection at SWMU CPP-45 Add Storage Tank Vault CPP-757

The chosen method of sampling in vault CPP-757 was hand augering. This method was chosen over hollow stem auger drilling due to limited accessibility in the vault.

Soil sample locations are shown on Figure 3.0. The individual locations were chosen in areas of the vault that were near low points, in close proximity to valves or where discoloration in the soil was noted. All borings were augered to a depth of six feet or until refusal. Sample collection intervals were 0-2 feet, 2-4 feet, and 4-6 feet. Samples were taken with either a 0.41 foot, 0.33 foot or a 0.15 foot diameter auger. All samples were screened by WINCO Health Physics personnel to detect radiation levels above background level.

Sampling equipment and sample preparation tools were decontaminated between each sample interval to minimize the potential for cross contamination. Augering and sampling decontamination procedures are referenced in Section 4.6 of the Technical Work Plan, Volume II (Golder Associates 1990b).

3.2.2 Sample Collection at SWMU CPP-45 Add Storage Tank Vault CPP-727

The chosen method of sampling in vault CPP-727 was hand augering. This method was chosen over hollow stem auger drilling due to limited accessibility in the vault.

Soil sample locations are shown on Figure 3.0. The individual locations were chosen in areas of the vault that were near low points in dose proximity to valves or where discoloration in the soil was noted. All borings were augered to a depth of six feet or until refusaL Sample collection intervals were 0-2 feet, 2-4 feet, and 4-6 feet. Samples were taken with either a 0.41 foot, 0.33 foot or a 0.15 foot diameter auger. All samples were screened by WINCO Health Physics personnel to detect radiation levels above background level.

Golder Associates Acid Storage Tank Vault CPP-727

192 Chernical Trench 10.9 CPP Acid Storage Tank 45-01 Vault CPP-757 CPP 45-01A CPP 45-03 CPP 45 05 .05 CPP 45-04 2.75' e 7 7.4N MCL 2S0 12.3' I ---- 1.\tr---- .# 4-1 saa Condensate Dry Wei Approximate SWMU Boundary

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FIGURE 3.0 PLANNED SAMPLING LOCATIONS AT SWMU CPP-45 HCl/H2S0 4 AND HF STORAGE TANK VAULTS EG&G/DRILL & SAMPLE SUMMARY SWMU CPP-05/I0 PROJECT NO. NO. 29470 893.1105.930 OWCI. DATE 1/28/91 DRAWN DC Golder Associates January 31, 1991 12 893-1195.900

Sampling equipment and sample preparation tools were decontaminated between each sample interva] to minimize the potential for cross contamination. Augering and sampling decontamination procedures are referenced in Section 4.6 of the Technical Work Plan, Volume II (Golder Associates 1990b).

3.3 SWMU CPP-45 Site Geology

3.3.1 SWMU CPP-45 Acid Storage Tank Vault CPP-757 Site Geology

CPP-757 is located on about six inches to one foot of granular fill which overlies alluvial sediments deposited by the Big Lost River. The fill material is comprised of sands similar in compositions to those found in the native alluvium and was probably derived from a local source.

Two six foot borings (CPP45-03 and CPP45-04) and one three foot boring (CPP45-05) were augered and sampled in the vault. The alluvial sediments in the vault generally consisted of well graded fine to coarse gravel and medium to coarse sand. No groundwater was encountered in the borings.

Upon completion of the drilling and sampling the borings were left open since weather conditions were unfavorable for filling the holes and forthcoming construction activities would excavate beyond the depths of the borings.

3.3.2 SWMU CPP-45 Acid Storage Tank Vault CPP-727 Site Geology

CPP-727 is located on about six inches to one foot of granular fill which overlies alluvial sediments deposited by the Big Lost River. The fill material is comprised of sands similar in compositions to those found in the native alluvium and was probably derived from a local source. Directly below and adjacent to the arid storage tank the vault bottom was lined with a layer of 4 inch or greater limestone cobble.

Three borings (CPP 45-01, CPP 45-02 and CPP 45-03) were augered to approximately 1.5 feet but terminated due to ground conditions or underground wiring. Two additional borings (CPP 45-01A and CPP 45-02A) were augered to a depth of 6 feet. The alluvial sediments in the vault generally consisted of well graded fine to coarse gravel and medium to coarse sand. No groundwater was encountered in the borings.

Upon completion of the drilling and sampling the borings were left open since weather conditions were unfavorable for filling the holes and forthcoming construction activities would excavate beyond the depths of the borings.

Golder Associates January 31, 1991 13 893-1195.900

3.4 SWMU CPP-45 Sample Handling and Analysis

3.4.1 Sample Handling and Analysis, CPP-757

Samples were obtained by augering to the desired sampling interval and, using a decontaminated hand auger, sampling one auger volume of the boring material. Samples were obtained from borings 03 and 04 from the surface to 2 foot, 2 to 4 foot and 4 to 6 foot intervals and from boring 05 from the surface to 2 foot and 2 to 4 foot intervals. Samples were processed on a fresh length of protective plastic on the processing table. The upper two inches of material in the auger was discarded. The sample was then placed into a decontaminated stainless steel mixing bowl, mixed thoroughly using decontaminated stainless steel utensils, and granular material larger than two inches was discarded. Sample was then transferred to two 8 ounce glass jars for analysis for total metals, pH, chloride and sulfate.

Samples from the surface to 2 foot interval on boring 5 were also prepared for Appendix VIII analyses. Grab samples were immediately taken for Appendix VIII volatile organics and placed in 8 ounce glass jars. Sample was placed in the containers such that little or no headspace was present, the containers were immediately sealed with a teflon lined lid and temporarily placed in the shipping containers. Ambient temperatures were such that no coolant was required in the shipping containers prior to actual shipment to the laboratory.

The remaining sample material was transferred to a plastic container for Appendix VIII pH, CI, SO„ metals, cyanide and sulfide analyses and to two 8 ounce glass jars for Appendix VIII semivolatiles, pesticides and herbicides and Appendix VIII dioxins and furans. Any remaining sample material was discarded into a 50 gallon waste container for subsequent disposal by WINCO personnel. All samples were labeled and placed into the appropriate shipping container with the necessary amount of coolant for maintaining the samples at 4°C. Sample were packed in bubble wrap for protection during shipment. Samples were then transferred by overnight carrier under chain-of-custody to the analytical laboratory.

All samples obtained were analyzed by Pacific Northwest Environmental Laboratory, Inc. (PNELI) of Redmond, Washington for the constituents listed in Table 3-1 with the exception of the surface sample obtained from boring 05. The surface to 2 foot sample collected from boring 05 was analyzed by Gulf South Environmental Laboratory, Inc.(GSELI) of New Orleans, Louisiana and by Southwest Laboratory of Oklahoma, Inc(SWLO) of Tulsa, Oklahoma for the 40 CFR Part 261 Appendix VIII constituents.

Results of the analysis indicating the target compounds detected and the range of values are presented in Table 4-2. Copies of all laboratory data reports are provided in Appendix C. A discussion of the analytical results is presented in Section 4.

Golder Assoclates TABLE 3-1 893-1195.900

Target CompoundWAnalyte List Solid Waste Management Unit CPP-45

Inorganic Metals Conventional Parameters Total Arsenic pH Total Barium Soluble Chloride Total Cadmium Soluble Sulfate Total Chromium Soluble Fluoride Total Lead Total Mercury Total Selenium Total Silver

Golder Associates January 31, 1991 15 893-1195.900

3.4.2 Sample Handling and Analysis, CPP-757

Samples were obtained by augering to the desired sampling interval and, using a freshly decontaminated hand auger, sampling one auger volume of the boring material. Samples were obtained from borings 01, 02 and 06 from the surface to 2 foot depth and from borings 01A and 02A from the 2 to 4 foot and 4 to 6 foot intervals. Samples were processed on a fresh length of protective plastic on the processing table. The upper two inches of material in the auger was discarded. The sample was then placed into a decontaminated stainless steel mixing bowl, mixed thoroughly using decontaminated stainless steel utensils, and granular material larger than two inches was discarded. Sample was then transferred to two 8 ounce glass jars for analysis for total metals, pH, and fluoride.

Samples from the surface to 2 foot interval on boring 06 were also prepared for Appendix VIII analyses. Grab samples were immediately taken for Appendix VIII volatile organics and placed in 8 ounce glass jars. Sample was placed in the containers such that little or no headspace was present, the containers were immediately sealed with a teflon lined lid and temporarily placed in the shipping containers. Ambient temperatures were such that no coolant was required in the shipping containers prior to actual shipment to the laboratory.

The remaining sample material was transferred to a plastic container for Appendix VIII pH, Cl, SO„ metals, cyanide and sulfide analyses and to two 8 ounce glass jars for Appendix VIII semivolatiles, pesticides and herbicides and Appendix VIII dioxins and furans.

Any remaining sample material was discarded into a 50 gallon waste container for subsequent disposal by WINCO personnel. All samples were labeled and placed into the appropriate shipping container with the necessary amount of coolant for maintaining the samples at 4°C. Sample were packed in bubble wrap for protection during shipment. Samples were then transferred by overnight carrier under chain-of-custody to the analytical laboratory.

All samples obtained were analyzed by Pacific Northwest Environmental Laboratory, Inc. (PNELI) of Redmond, Washington for the constituents listed in Table 3-1 with the exception of the surface sample obtained from boring 06. The surface to 2 foot sample collected from boring 06 was analyzed by Gulf South Environmental Laboratory, Inc. (GSELI) of New Orleans, Louisiana and by Southwest Laboratory of Oklahoma, Inc(SWLO) of Tulsa, Oklahoma for the 40 CFR Part 261 Appendix VIII constituents.

Results of the analysis indicating the target compounds detected and the range of values are presented in Table 4-2. Copies of all laboratory data reports are provided in Appendix C. A discussion of the analytical results is presented in Section 4.

3.5 Quality Assurance/Quality Control

Quality assurance/quality control procedures were implemented during the sampling and analysis program. These procedures are summarized below.

Golder Associates lanuaty 31, 1991 16 893-1195.900

• A trip blank and an equipment blank were collected and analyzed to monitor potential contamination that may have been introduced from the decontamination procedures and shipping process (see section 3.5.1).

• A field duplicate sample was collected to measure overall field and laboratory precision (see Table 3-2).

• A blind reference performance audit sample was prepared and submitted for metals analysis to determine laboratoty accuracy (see Table 3-3).

3S.1 Blanks

A trip blank was included in the sample shuttle for organic analysis. Methylene chloride (20 uWL) was detected in the trip blank sample and also detected in the volatile method blanks at 14 and 7 ug/L respectively.

An equipment blank was submitted for one sampling round for metals and conventional parameters. The blank was prepared by thoroughly cleaning the drilling and sampling equipment prior to each sampling event as described in Section 4.6 of the Quality Assurance Project Plan (Golder Associates, 1990) followed by a final rinse with deionized water and collection of the rinseate in the proper containers for metals and conventional parameters analysis (Ph, chloride, sulfate, fluoride). Barium and iron were detected in the equipment blank at 16.8 ug/L and 62.5 ug/L respectively. Both of these values reported are obtained from a reading that was less than the Contract Required Detection Limit(CRDL) but greater than or equal to the Instrument Detection Limit (IDL). Iron is commonly found in the alloys used for fabrication of drilling and sampling equipment. Fluoride and chloride were reported at 0.531 mWL and 0.120 mg/L. These levels are significantly lower than the levels found in the soil samples collected at the site.

3.5.2 Field Duplicates

Field duplicate results from SWMU CPP-45 are presented in Table 3-2. The samples were collected and prepared as described in Section 4.4 of the Quality Assurance Project Plan (Golder Associates, 1990). The table presents the relative percent difference (RPD) between duplicate samples for analyses that exhibit results greater than the sample detection limit. Although no data quality criteria exist for field duplicates, the EPA recommends that the RPD for laboratory duplicates fall within a control limit of +/-20% for water samples and +/-35% for soils when sample values are 5 times the sample detection limit. (EPA, 1988b).

All RPD's for the duplicate sample analysis were below the control limits for both metals and conventional parameters.

Golder Assoclates TABLE 3-2 893-1195.900

Field Duplicate Analysis Results Solid Waste Management Unit CPP-45

Golder ID CPP45-03-M-3-2 CPP45-03-M-3-2-F Relative CPP45-03-pH/C1/S-3-2 CPP45-03-pH/CVS-3-2 Percent Difference

Date Sampled 11/12/90 11/12/90 Inorganic Metals (Results in mWKg) Arsenic 3.7 4.1 10.3 Barium 75.7 69.9 8 Cadmium 1.1U 1.0U NC Chromium 16.0 17.9 11.2 Iron 8680 8640 0 Lead 5.1 5.1 0 Mercury 0.06 0.08 NC Nickel 14.6 14.5 0.7 Selenium 0.64 0.64 NC Silver 2.1U 2.1U NC General Chemistry Analysis (Results in mWKg) pH 6.88 6.81 1.0 Chloride 10.6U 10.7U NC Sulfate 0.532U 0.530U NC Fluoride

RPD - Relative percent difference is calculated by taking the absolute value of the difference between two measurements divided by the average of the two measurements, multiplied by 100.

NC - The result(s) is not calculated due to one or both of the measurements at or below the sample detection limit or not detected.

U - lndicates that analyte was analyzed for but not detected. The number is the minimum attainable detection limit for the sample.

Golder Associates TABLE 3-3 893-1195.900

Performance Audit Sample Analysis Results Solid Waste Management Unit CPP-45

Laboratory Sample ID: 2775-01 Golder Sample ID: CPP45-07-EB Date Sampled: 11/16/90

------Compound/Analyte Reported Value ug/L True Value ug/L Percent Control Unit 1) Recovery Arsenic 92.0 100 92 75-125 Barium 98.9 100 99 75-125 Cadmium 109 100 109 75-125 Chromium 106 100 106 75-125 Lead 106 100 106 75-125 Mercury 95.3 100 95 75-125 Selenium %.8 100 97 75-125 Silver 102 100 102 75-125

1) Control Limits for Inorganic Compounds EPA, 1988a

Golder Assoclates lanuary 31, 1991 19 893-1195.900

3S3 Performance Audit Samples

One performance audit sample was prepared as described in Section 4.4 of the Quality Assurance Project Plan (Golder Associates, 1990) and shipped to the laboratory for metals analysis. The results of the analysis are presented in Table 3-3. The sample was prepared by spiking laboratory prepared deionized water with a known concentration of target analytes. The sample analysis results submitted by the laboratory were within the EPA recommended limits of 75-125 percent recovery.

3.6 Data Validation

A total of 53 samples were analyzed by Pacific Environmental Laboratory, Inc. (PNELI), Gulf South Environmental Laboratory, Inc.(GSELI) and Southwest Laboratory of Oklahoma, Inc. (SWLO). Two samples (CPP45•05 and CPP45-06 both at 0-2 foot depth) were analyzed for Appendix VIII constituents which included volatile organics, semivolatile organics, organophosphate pestiddes, organochlorine pesticides, herbicides, metals, and conventional parameters as specified in section 4.4 of the Quality Assurance Project Plan (Golder Assodates, 1990). All sample analysis results were reviewed and validated in accordance with Section 8 of the Quality Assurance Project Plan (Golder Associates, 1990) and with the EPA functional guidelines for evaluating inorganic data and organic data (EPA 1988a and EPA 1988b). Validation performed on each sample delivery group was documented in the specified report format shown on Figures 8.1 and 8.2 in Section 8 of the Quality Assurance Projed Plan (Golder Assodates, 1990). The following sections outline the findings of the validation procedure for this site.

3.6.1 Holding Times

Holding times specified in the functional guidelines were compared to the reported dates of extraction and analysis for organic, inorganic, and conventional fractions. Volatile organic and semivolatile organic extraction and analysis were performed within the specified holding times for both soil and water matrices. Mercury analyses were completed within 28 days from time of sample collection. The holding time for pH analysis was exceeded for Case 2771 (Golder ID CPP45-04-pH/CL/S-3-2, CPP45-04-pH/C1./S-5-2, CPP45-05-pH/CL/S-3-2, and CPP45-04-pH/CL/S-1-1) by one day, however, data was acceptable for use as reported.

3.6.2 Instrument Calibrations

Instrument calibrations were checked for each fraction with no anomalies noted. Samples were analyzed within the appropriate time windows for each calibration. Organic analyses were performed within the specified time windows for tuning criteria, and both initial and continuing calibration criteria were met as specified in the USEPA Contract Laboratory Program Statement of Work (CLP/SOW)(EPA, 1990a and 1990b).

Golder Assoclates January 31, 1991 20 893-1195.900

The inorganic data had minor problems assodated with the instrument calibrations. The metals data was flagged as estimated because the matrix spike recovery limits exceeded the recovery windows specified in the CLP/SOW,(EPA, 1990b). Based on the calibration recoveries several sample results were requalified as estimated. These regulations do not affect the use of data for site characterization purposes.

3.6.3 Project Detection Limit Goals

Detection limit goals were met for volatile analysis (EPA method 8240) and semivolatile analysis (EPA method 8270) where applicable. The samples (CPP45-05 and CPP45-06, both at 0-2 foot depth) analyzed for Appendix VIII compounds were reported with an additional qualifier as to availability of the reference standard compounds and if the compound could only be identified through the use of a spectral library search.

Inorganic detection limit goals were exceeded for mercury, selenium, chloride and fluoride. The project detection limit goals for sulfate were met with the exception of Appendix VIII sample CPP45-05 where the reported detection limit is 50 mWKg. While the detection limit goals for a few of these analytes slightly exceeded the project specific goals set forth in the Quality Assurance Project Plan, the overall project detection limit goals were achieved for the site.

3.6.4 Quality Control Data

Quality control data which included matrix spike/matrix spike duplicate analysis, surrogate analysis, internal standards analysis and blank analysis were reviewed for recovery percentages. Organic quality control data was acceptable and within CLP specified limits. The sunogate percent recoveries were out of spedfication for the organophosphate pestiddes analysis, however, for this type of analysis the surrogates were difficult to analyze for and are not specified in EPA reference method.

Overall, the inorganic quality control data was acceptable. Anomalies noted in the validation process included low spike recoveries for barium, lead, and mercury with assodated data requalified as estimated.

3.6.5 Blank Data

Laboratory blank data was reviewed and compared to the sample data. Volatile organic analysis of the soils identified acetone (10 and 8 ug/L), and methylene chloride (14 and 7 ug/L) in the method blanks. Acetone and methylene chloride that were detected in the associated samples were eliminated from the sample analysis results summary (Table 4-2) in accordance with the data validation guidelines (EPA 1988a). No other target compounds or tentatively identified compounds were reported for the organic analyses.

Golder Associates January 31, 1991 21 893-1195.900

Inorganic preparation blank values contained elemental contamination above the Instrument Detection Limit (IDL) but below the Contract Required Detection Limit (CRDL). Samples with positive results corresponding to the blank contaminants were requalified with LTJ (not detected, estimated quantitation limit).

Golder Assoclates January 31, 1991 22 893-1195.900

4. NATURE AND EXTENT OF CONTAMINATION

4.1 Assessment of Background Data

Background data for metal concentrations in soils at the ICPP were obtained by the University of Utah Research Institute (UURI) during two studies conducted in 1986 and 1987. Background soils data were obtained at four locations outside the ICPP during an investigation of the Fuel Processing Restoration (FPR) Warehouse Site in 1986. According to the Quality Assurance Sampling Plan (QASP) for this study, background subsurface soils collected were to be geologically identical to soils in the FPR site sampling area. The QASP indicated the FPR site soils were to be sampled at depths of 6 inches below the pre-fill surface of the area and at 18-24 inches below the top of the first horizon samples. The actual depth interval sampled for background soils is noted in the QASP or the final report of the investigation (UURI 1986a and UURI 1986b).

In 1987, background data were obtained at three locations outside the ICPP during an investigation of the Chemical Feed and Zirconium Feed Tank Storage Areas. Samples were obtained at surface to 4 inches and at 24 inches at these locations for a total of six samples (UURI 1987a and U1JRI 1987b).

A summary of the background data obtained from the UURI investigations is provided in Table 4-1. Also shown on this table are the one-sided upper tolerance intervals (UTL) for the background data assuming a normal distribution with 95% coverage of the samples at a 95% confidence coefficient. Tolerance intervals establish a concentration range that is constructed to contain a specified proportion of coverage (P%) of the population with a specified confidence coefficient, Y (EPA 1989a).

There are potential limitations that should be considered in the use of the data obtained by UURI for determining action levels based on background concentrations. These limitations include the following:

• All UURI background data were obtained in the shallow surface soils (0 to 24 inches) and may not be representative of other soil types or horizons;

• Many areas of the ICPP have been graded and/or filled. Background soils sampled by UURI may not be representative of soils used for fill at the ICPP; and

• There may be widespread elevated concentrations of certain constituents above natural background at the ICPP from both point and non-point sources as a result of site activities. It is not appropriate to establish action levels for SWMUs based on natural background if there are widespread elevated concentrations of constituents at the ICPP unrelated to releases from the SWMUs.

Golder Associates TABLE 4-1 893-1195900

Background Concentrations of Metals in Soils Sampled from Outside the ICPP Facility and One-Sided Normal Tolerance Intervals(1)

Results in PPM

Sample Arsenk Barium Cadmium Chromium Lead (2) Mercury Selenium Silver

Bkg 1 5.6 200 <5 25 12 BOO 0.484 <2

Bkg 2 5.1 270 <5 32 16 0.019 0.405 <2

Bkg 3 6.5 270 <5 33 17 0.077 0.467 <2

Bkg 4 7 250 <5 34 12 0.028 0.341 <2

258 5.6 280 <5 28 <10 0.025 0.113 <2

259 7.6 380 <5 26 <10 0.057 0.252 <2

0.023 0.695 <2

JapiOD 260 6.4 240 <5 28 <10

261 6.2 220 <5 18 <10 0.03 0.236 <2

264 6 230 <5 28 <10 0.021 0.102 <2

265 7.6 210 <5 71) < 10 0.046 0.727 <2 sewpossy sewpossy Average (x) Std. 6.4 255 <5 77 9 0.032 0.332 <2 Dev.(SD) 0.8 51 -- 5 5 0.013 0.184 — Background 1111 8.7 403 -- 42 24 0.070 0.868 --

1. All samples were col ected by the University of Utah Research Institute, Salt Lake City, UT using EPA methods. Samples Kdg 1-4 were collected for the FPR Warehouse Site, and 258-265 were collected for the Chemical Storage and Zirconium Feed Tank Storage Areas. All analyses are total constituent analyses and are reported on a dry weight basis.

2. Where lead values are listed below detection limit a value of one-half the detection limit was used in the calculation of the average, standard deviation and tolerance limit values.

3. The background one-sided upper tolerance interval (UTL) is (x) + K'SD, where the K value (tolerance factor) for sample size n = 10 is equal to Z911 with a probability level y = 0.95 and coverage P = 95% lanuary 31, 1991 24 893-1195.900

4.2 Results of Inorganic Analysis for Solid Waste Management Unit CPP-45

Detected inorganic analytes of interest are presented in Table 4-2. Arsenic was detected in all boreholes ranging from 2 mg/Kg to 6.7 mg/Kg with the highest reported value in borehole CPP45-01A at the 2 to 4 foot depth. Barium was detected in each of the boreholes with the maximum value (195 mg/Kg) reported in borehole CPP45-02A at a depth of 2 to 4 feet. Cadmium was detected in surface samples from locations CPP45-05 and CPP45-06. The range of chromium was 7.2 mg/Kg to 31.4 mg/Kg and was reported above detection limits in all boreholes. Lead was detected in all boreholes with the maximum value (55.2 mg/Kg) reported in borehole CPP45-02 at the surface. One location (CPP45-01) reported mercury at the detection limit of 0.09 mg/Kg. Selenium was reported at CPP45-05 at the surface with a concentration of 0.48 mg/Kg but this has been requalified as unusable due to matrix spike data. Silver was not detected in any of the boreholes.

4.3 Results of Organic Analysis

There were no organic compounds detected in any of the sampling locations.

4.4 Results of General Chemistry Analysis

General chemistry parameters consisted of pH, soluble chloride, soluble sulfate and soluble fluoride. Soluble chloride was detected (25.1 mg/Kg) in CPP45-05 at the 0 to 2 foot depth. Sulfate levels ranged from below detection limit to 5.92 mg/Kg in CPP45-04 at the 0 to 2 foot depth. Soluble fluoride was detected in three boreholes (CPP45-01, CPP45-02, and CPP45- 06) at each of the sampling intervals. The highest concentration (310 mg/Kg) was at location CPP45-02 at the 0 to 2 foot depth. Fluoride was detected (0.500 mg/Kg) in the equipment blank at a concentration exceeding project detection limit goals, however, considerably lower than fluoride levels detected in soil samples.

Golder Associates seppossv Jappo U N/A - CP91541 C9915-01A CP91502 C994542A CPP1543 CP945-04 CP915-05 CPP11506 Maximum Minimum Background Borehole - Compound Nol applicable V value UT1. lue was Depth analyzed 14 0-2 0-2 14 14 0-2 24 14 0-2 0-2 0-2 24 24 24 2-4 for but Arsenic Total 67 66 11 34 4.8 3.7 3.9 3.6 15 67 1.6 1.7 1.6 3.9 6.7 1.1 2 2 not detected, Barium Total 619 7/7 66.3 81.2 56.2 50.9 71.6 44.11 51.1 41.13 182 195 403 135 144 the 195 73 121 reported Cadmium value To 1.1 1.1 1.1 1.1 1.1 1.1 1.1 033 0.76 N/A I I 1 1 N/A 1 1 - lal U U U U U U U U U U U U U Is the sampk Chromium Total 31.1 203 73.2 228 15.9 221 17.3 13.3 18.6 31.4 21.3 166 7.2 11.1 8.11 7.2 16 42 detection . limit SOLID 11,100 11500 13,800 10,200 10,100 11900 6,230 14,900 10,000 13,2133 Total 7210 8,6110 3,610 6610 8570 7550 Iron 3,610 N/A WASTE SAMPLE (Results Total Lead 55.2 55.2 10.1 17.1 al 18.7 8.2 8.9 5.4 5.1 4.3 3.7 6.6 1.2 5.3 3.7 18 MANAGEMENT 24 ANA TAN in F YSIS mg/Kg) 4.2 Mercury 0.09 0.06 0.09 0.06 0.06 0.01 0.041 0.10 0.07 0.09 0.09 0.10 0.00 0.04 Total 0.09 0.07 0.09 N/A RESULTS 1.1 U U U U U U U U U U U U U UNIT CPP-45 Nkkel 4.1 Total 112 195 18.2 11.6 16.9 N/A N/A 19.7 15.3 17.9 19.1 17.1 175 19.7 7.3 6.1 11 U Selenium 662 663 0.M 0.62 0.63 0.61 0.61 0.62 0.11 0.63 0.65 0.65 0.61 0.61 Total 018 0.87 0.18 N/A U U U U U U U U U U U U U V

0.13 0.11 Sliver 11 Total 12 11 11 11 11 22 20 21 21 2 I N/A N/A 2 2 U U U U U U U U U U U U U U U pH, 657 629 669 644 6.68 6.11 6.31 Son 619 6.99 7.77 7.09 6.39 8.71 7.31 N/A 7 9 9 au Chloride Soluble 11.1 105 106 10.6 10.6 10.1 11 N/A N/A WA al NIA N/A WA N/A N/A N/A WA U U U U U U U Soluble 0319 0.532 Sidle* 0.%2 50 /92 N/A N/A WA 159 184 5.92 N/A NIA N/A 4.11 N/A N/A N/A U U U 8934193903 Fluoride Soluble 615 3.08 12.2 N/A N/A N/A N/A WA 108 N/A N/A N/A 310 253 269 131 N/A 310 January 3L 1991 26 893-1195.900

5. HEALTH AND ENVIRONMENTAL ASSESSMENT

The Health and Environmental Assessment(HEA) is conducted to evaluate the impact of hazardous constituents present at a site. The HEA involves the identification of contaminants of concern, the concentrations of these constituents in the affected environmental media, and the risk to exposed or potentially exposed human or environmental receptors. The essential element of this assessment is the development of an appropriate set of health and envirorunental criteria to which the measured or predicted concentrations of toxic contaminants are compared. These criteria are primarily based on EPA-established chronic exposure limits. When the criteria are exceeded, there is a likelihood of adverse health or environmental effects and additional measures may be required to prevent or reduce these effects.

5.1 Identification of Toxic Contaminants

Analyses of soil samples from shallow boreholes at SWMU CPP-45 were conducted to detennine the presence and concentration of inorganics and organics in the soil. The inorganic analysis results are presented in Table 4-2. Six of the analytes are not included in this HEA. Arsenic, barium, cadmium, chromium, selenium, and silver did not exceed background concentrations or were analyzed for, but not detected, at the given detection limit. Two other analytes, iron and nickel, are also not evaluated further in the HEA. Iron is an essential element for humans that is generally considered non-toxic except under conditions of large, single, and accidental ingestion of medicine or in the presence of specific genetic or medical conditions. Nickel may also be essential to humans for normal growth and development. Median soil concentrations of nickel are typically 26 - 50 mg/kg (ATSDR, 1988). The highest concentration of nickel detected at SWMU-45 was 19.7 mg/kg.

Lead was detected at a concentration greater than background. Lead is a well-documented cumulative toxin that has also been shown in animal studies to produce cancer. Differences between individuals such as age, nutritional status, and other factors can influence the dose at which lead is toxic. Children, for example, are considered a sensitive population because they are particularly susceptible to neurological changes from excess lead intake. Because some of the toxic effects can occur at blood lead levels so low as to be essentially without a threshold, the EPA recommends that neither a chronic reference dose nor a numerical cancer risk be used at this time (EPA, 1991). Although the soil lead concentration of 55.2 mg/kg at SWMU-45 exceeds the background UM,this concentration is significantly less than the soil concentration of >500mg/kg determined necessary to produce an increase in blood lead levels in children exposed to lead containing soil (EPA, 1989a). Therefore, lead is not considered further in this HEA.

Mercury is present at a level slightly higher than the background UTL. This compound has a number of inorganic and organic derivatives, and toxicity is highly dependent on the form and route of exposure. Organic (alkyl) mercury compounds are generally more toxic by ingestion than inorganic (metallic) mercury. Target organs for toxic effects are the central nervous system and the kidney. Mercury has not been classified as to human carcinogenicity. Mercury is included in the HEA for SWMU-45.

Golder Assoclates lanuary 31, 1991 27 893-1195.900

Three additional parameters, sulfate, chloride, and fluoride, were also analyzed for and detected in the soils at SWMU-45. Sulfate, detected at 5.92 mWkg, and chloride, detected at 25.1 mWkg, are present in the soils at the acid storage tank vault CPP-757 site where hydrochloric and sulfuric add were stored. Sulfate toxidty is minimal and usually associated with mild gastrointestinal effects (Gosselin, et al., 1984). Chloride is considered essentially nontoxic. Normal soil concentrations of chloride range from 10 - 100 mg/kg (Dragun,1988). Sulfate and chloride, therefore, are not considered further in this HEA.

Fluoride, detected at 310 mg/kg, is present in the soil at the hydrofluoric add storage tank vault CPP-727. Fluoride toxicity is assodated with any soluble fluoride compound which dissodates to produce fluoride ion (Gosselin et.al., 1984). The type and severity of toxicity varies with the chemical form, the route of exposure, and the duration of exposure. The potential for acute toxic effects from exposure to fluoride found in the soil is minimal since fluoride interacts with the environment and the soil to form relatively stable compounds. However, chronic effects from exposure to low doses of fluoride in these forms, through ingestion or occupational exposure to fluoride-containing dusts, can produce deposition of fluoride in the teeth (dental fluorosis) and the bone (skeletal fluorosis or osteosclerosis) (Baselt and Cravey, 1989). Fluoride is not known to be carcinogenic. fluoride is included in this HEA.

No organic contaminants were detected during the sampling analyses for SWMU CPP-45.

5.2 Identification of Exposure Pathways

The two contaminants of interest detected at SWMU CPP-45, mercury and fluoride, are located in the soils at the hydrofluoric add storage tank vault CPP-727. The vault is approximately 8 ft in depth; soil samples were obtained from boreholes in the vault floor. Mercury was detected at concentrations just above background at a depth of 2 - 4 ft; the highest fluoride concentration was detected in soils at 0 - 2 ft. Thus, the contaminants 11-5 appear to be localized in the upper portion of the soil column in the vault, but Afr \tri p _e_c) approximately 8 - 12 ft below the general ground surface. See Table 4-2. 1\1-1-42-0' p,ky -c1u Soil ingestion or dermal contact with these soils on a regular basis would not occur unless! the soils are disturbed or moved to the surface outside the vault where more frequent contact would be possible. However, very limited exposures may occur for individuals working in the vault.

The depth to groundwater, the lack of surface water bodies in the vicinity of the vault, the limited areal extent of contamination, and the low concentrations of contaminants detected preclude any significant impact on water from SWMU CPP-45. Thus, water is eliminated as a potential exposure pathway.

The inhalation pathway is also inoperative unless the soils are exposed, and even then a significant adverse risk from airborne fluoride or mercury contaminated particulates is improbable given the low concentrations of contaminants detected in the soils and limited areal extent of contamination (i.e., absence of a significant source).

Golder Associates January 31, 1991 28 893-1195.900

5.3 Identification of Receptor Populations

The typical receptors for contaminants present at SWMU CPP-45 are workers with direct access to and work duties at the acid storage tank vault CPP-727. The ICPP is a secured industrial site with limited access.

5.4 Human Health Assessment

No adverse health effects can be attributed to the mercury and fluoride detected in the vault soils without direct exposure to the soil. As discussed in Section 5.2, the soils would have to be excavated or moved outside the vault where workers at the ICPP could have frequent and ongoing exposure to the contaminants through incidental soil ingestion or dermal contact, the two potentially operative exposure pathways.

For the purposes of an initial screening, it is conservatively assumed that the vault soils are accessible. Based on this assumption, the potential human health effects from the concentrations of mercury and fluoride identified at SWMU CPP-45 are assessed. The results of the assessment are summarized in Table 5-1. Both mercury and fluoride are known to have systemic toxic effects if exposures are great enough. The soil concentrations at which no systemic toxicity would be likely to occur for even a sensitive population (16 kg child, ingesting 200 mg soil per day for a 5 year exposure period) were calculated as part of the assessment. This soil concentration, if ingested, would result in an oral dose equivalent to the applicable chronic reference dose (RfD) for each contaminant. The RfD for a contaminant is the daily intake of the contaminant to which even a sensitive individual might be exposed without developing documented critical toxic effects. This screening is conducted as recommended in the RCRA Facility Investigation Guidance (EPA, 1989b).

The equation for calculating the soil screening criterion is given below:

CS = RfD x BW IR x CF where:

CS = Soil concentration screening aiterion RfD = Chronic Reference Dose BW = Body Weight (16 kg) IR = Ingestion Rate (200mg/day) CF = Conversion Factor (1E-06 kg/mg)

None of the soil concentrations detected exceed the maximum allowable soil concentrations based on the RfD (see Table 5-1). Therefore, systemic adverse health effects should not occur in even sensitive individuals exposed to soil contaminants at the levels detected in the soils at SWMU CPP-45. It should be noted that two screening criteria are provided for fluoride. An RfD of 0.06 mg/kg/day is published that reflects the level of exposure children may have without developing dental fluorosis from an excess intake of fluoride (EPA, 1991).

Golder Associates 893-1195.900

TABLE 5-1

SUMMARY OF HEALTH AND ENVIRONMENTAL ASSESSMENT FOR SWMU CPP-45

Constituent Maximum Chronic Soil Detected Soil Oral RfD Concentration = Concentration (mg/kg/d) RfD (mg/kg) (mg/kg) Fluoride 310 6E-021.2 4,800 1.2E-01° 233,333' Mercury 0.09 3E-045 24 IPA, 1991 'Critical effect considered cosmetic rather than an adverse/toxic health effect 'Calculated safe exposure level in adults to prevent skeletal fluorosis 'Assumed Industrial Scenario: 100mWd soil ingestion, 36% frequency, 40 yr exposure, 70 kg body weight 'EPA, 1990

Golder Associates January 31, 1991 30 893-1195.900

This effect is considered a cosmetic effect rather than an adverse or toxic health effect. A second intake level based on an adverse health effect in adults (skeletal fluorosis) is also reported in the Integrated Risk Information System (EPA, 1991) and is presented in Table 5-1. The soil concentrations of fluoride found at SWMU CPP-45 do not exceed the screening criteria corresponding to either of these acceptable intake levels for fluoride.

Mercury and fluoride are not known to be carcinogenic substances. Therefore, no determination of carcinogenic risk from possible exposures is applicable.

For both contaminants, the contribution of dermal contact or inhalation exposures to the overall health risk, although not quantitatively evaluated, would be inappreciable because of the low levels of soil contamination, the lack of ongoing access to the soils, and the depth of the soil contamination.

Given the results of the screening presented above, adverse health impacts to workers in the vicinity of or with direct access to SWMU CPP-45 would not occur from the contaminant concentrations detected.

5.5 Environmental Assessment

SWMU CPP-45 is located within the controlled boundaries of the ICPP and is the site of two acid storage tank containment vaults located 6 - 8 ft below ground level. All detected soil contaminants are located in soils below the floor of these vaults. SWMU CPP-45 does not support any vegetation with roots extending into the area of detected contamination. Large animals and migratory wildlife have no access to or are not known to frequent the immediate area surrounding SWMU CPP-45. Consequently, no adverse impact on terrestrial biota should occur.

The airborne transport of mercury or fluoride located in the soils at SWMU CPP-45 cannot occur because of the depth to the contaminants and the low levels of contaminants present in the soil (i.e. absence of a significant source). Thus, environments downwind from the area will not be impacted via the air pathway.

Low annual rainfall will result in little surface runoff and infiltration. These conditions, in addition to the depth to groundwater (approximately 455 ft) and low level of soil contamination will limit migration of contaminants and any adverse effects on surface waters or groundwater in the vicinity of SWMU CPP-45. Consequently, surface water and groundwater will not be impacted by the levels of soil contamination detected at SWMU CPP-45.

Golder Assoclates January 31, 1991 31 893-1195.900

6. SUMMARY AND CONCLUSIONS

This sections presents a stunmary of the results of investigations at SWMU CPP-45 containment vaults CPP-727 and CPP-757. Condusions regarding the nature and extent of contamination detected and potential health or environmental effects associated with the contaminants detected are also presented. In addition, recommendations for additional investigations or corrective measures are presented.

6.1 Suntmary

Four boreholes were hand augered and sampled to a depth of 6 feet. Three additional boreholes were hand augered and sampled to a depth of 1.5 feet and one borehole was hand augered and sampled to a depth of 4 feet but terminated at these depths due to ground conditions or underground wiring. Samples in containment vault CPP-757 were analyzed for pH, chloride, sulfate, and total metals. Samples in containment vault CPP-727 were analyzed for pH, fluoride, and total metals. One set of surface samples from each vault were also analyzed for the 40 CFR Part 261 Appendix VIII constituents.

Results of the sampling and analysis are summarized below:

Lead and mercury were detected at concentrations higher than the Upper Tolerance Limit (UTL).

Fluoride was detected in containment vault CPP-727.

No organic compounds were detected during the sampling analyses for containment vaults CPP-727 and CPP-757 in SWMU CPP-45.

6.2 Conclusions

The concentrations of the inorganics detected from tank vaults CPP-727 and CPP-757 in SWMU-45 do not pose a risk to human health or the environment and it is unlikely that permissible exposure levels (see Table 5-1) would be exceeded. No organic compounds were detected for either vault. There is no need to conduct additional investigations at these sites. Removal, decontamination, or dosure, under RCRA should not be required.

Golder Associates January 31, 1991 32 893-1195.900

7. REFERENCES

Barraclough, J.T., B.D. Lewis, and R.G. Jensen, 1981, Hydrologic Conditions at the Idaho National Engineering Laboratory, Idaho, Emphasis: 1974-1978, U.S. Geological Survey Water Resources Investigations Open-file Report 81-526 (IDO-226060), U.S. Department of the Interior, Geological Survey, Idaho Falls, Idaho.

Bartholomay, R.C., L.L. Knobel, and L.C. Davis, 1989, Mineralogy and Grain Size of Surficial Sediment from the Big Lost River Drainage and vicinity, with Chemical and Physical Characteristics of Geologic Materials from Selected Sites at the Idaho National Engineering Laboratory, Idaho U.S. Geological Survey Open File Report 89-384, U.S. Department of the Interior, Geological Survey, Denver, Colorado.

EPA, 1988a, Laboratory Data Validation Functional Guidelines for Evaluating Inorganics Analyses U.S. Environmental Protection Agency, Division, Washington, D.C.

EPA, 1988b, Laboratory Data Validation Functional Guidelines for Evaluating Organics Analyses, U.S. Environmental Protection Agency, Division, Washington, D.C.

EPA, 1989a, Statistical Analysis of Ground-water Monitoring Data at RCRA Facilities: Interim Final Guidance U.S. Environmental Protection Agency, Office of Solid Waste, Washington, D.C.

EPA, 1990a, Health Effects Summary Tables - First/Second Ouarter FY 1990, OSWER (05- 230), ORD (RD-689), OERR 9200.6-303 (89-1/2), U.S. Environmental Protection Agency, Environmental Criteria and Assessment Office, Cincinnati, Ohio.

EPA, 1990b, Integrated Risk Information System, access date September 19, 1990, U.S. Department of Health and Human Services, National Library of Medidne Toxicology Data Network (TOXNET), Bethesda, Maryland.

Golder Associates, 1990b, Ouality Assurance Proiect for Drilling and Sampling Activities at Solid Waste Management Unit CPP-45• Technical Work Plan, Volume II Golder Assodates Inc., Redmond, Washington.

Mundorff, M.J., E.G. Crosthwaite, and C. Kilburn, 1964, Ground Water for Irrigation in the Snake River Basin in Idaho U.S. Geological Survey Water Supply Paper 1954, U.S. Department of the Interior, Geological Survey, Reston, Virginia.

Pittman, J.R., R.G., Jensen, and P.R. Fischer, 1988, Hydrologic Conditions at the Idaho National Engineering Laboratory, 1982 to 1985, U.S. Geological Survey Water-Resources Investigation Report 89-4008, U.S. Department of the Interior, Geological Survey, Idaho Falls, Idaho.

UURI, 1986a, Quality Assurance Sampling Plan; FPR Warehouse Site Idaho Chemical Processing Plant, University of Utah Research Institute, Salt Lake City, Utah

UURI, 1986b, Final Report; FPR Warehouse Site Idaho Chemical Processing Plan, University of Utah, Salt Lake City, Utah.

Golder Associates January 31, 1991 33 893-1195.900

UURI, 1987a, Oualibr Assurance Sampling Plan; Chemical Storage and Zirconium Feed Tank Storage Areas, Idaho Chemical Processing Plant, University of Utah Research Institute, Salt Lake City, Utah.

UURI, 1987b, Final Report; Chemical Storage and Zirconium Feed Tank Storage Areas Idaho Chemical Processing Plant, University of Utah Research Institute, Salt Lake City, Utah.

WINCO, 1989a, Oosure Plan for CPP-34 Contaminated Soil Storage Area in the NE Corner of CPP, Westinghouse Idaho Nuclear Company, Idaho Falls, Idaho.

WINCO, 1989b, Oosure Plan for CPP-55 Mercury Contaminated Area (South of ICPPT-15) Westinghouse Idaho Nuclear Company, Idaho Falls, Idaho.

Golder Associates, 1990, Ouality Assurance Project Plan For The Soil Sampling and Analysis Program At Solid Waste Management Unit CPP-45, Golder Associates Inc., Redmond, Washington.

EPA-1988b, Laboratory Data Validation Functional Guidelines for Evaluating Inorganics Analyses, U.S. Envirorunental Protection Agency, Division, Washington, D.C.

EPA 1988a Laboratory Data Validation Functional Guidelines for Evaluating Organics Analyses U.S. Environmental Protection Agency, Division, Washington, D.C.

EPA 1990a, USEPA Contract Laboratory Program Statement of Work For Organic Analysis Sample Management Office, U.S. Environmental Protection Agency, Washington, D.C.

EPA 1990b, USEPA Contract Laboratory Program Statement of Work For Inorganic Analysis Sample Management Office, U.S. Environmental Protection Agency, Washington, D.C.

ATSDR, 1988, Toxicological Profile for Nickel, Agency for Toxic Substances and Disease Registry, U.S. Public Health Service, Atlanta, Georgia.

Baselt, R.C. and R.H. Cravey, 1989 Disposition of Toxic Drugs and Chemicals in Man 3rd Edition, Year Book Medical Publishers, Inc., Chicago, Illinois.

Dragun, James, 1988, The Soil Chemistry of Hazardous Materials Hazardous Materials Control Research Institute, Silver Spring, Maryland.

EPA, 1991, Integrated Risk Information System, access date January 23, 1991, U.S. Department of Health and Human Services, National Library of Medicine Toxicology Data Network (TOXNET), Bethesda, Maryland.

EPA, 1990, Health Effects Summary Tables - Third Ouarter FY 1990, OSWER (05-230), ORD (RD-689), OERR 9200.6-303 (90-3), U.S. Environmental Protection Agency, Environmental Criteria and Assessment Office, Cincinnati, Ohio.

Golder Associates Tanuary 31 1991 34 893-1195.900

EPA, 1989a, Interim Guidance on Establishing Soil Lead Cleanup Levels at Superfund Sites OSWER 9355.4-02, U.S. Environmental Protection Agency, Office of Solid Waste and Emergency Response, Washington D.C.

EPA, 1989b, RCRA Facility Investigation (RFD Guidance, Volume I: Interim Final, EPA/53WSW-89-031, OSWER Directive 9502.00-6D, U.S. Enviromnental Protection Agency, Office of Solid Waste and Emergency Response, Washington, D.C.

Gosselin, R.E., R.P. Smith, and H.C. Hodge, Oinical Toxicology of Commercial Products, 1984, Williams and Willdns, Baltimore, Maryland.

Golder Associates APPENDIX A BOREHOLE LOGS

Golder Associates PROJECT: ICPP RECORD OF BOREHOLE CPP45-01,01A SHEET: 1 Of 1 PROJECT LOCATION: ICPP CP1145 BORING DATE 10 Nov. 90 DATUM: MSL gn PROJECT NUMBER: ass-1 135.9C0 BORING LOCATION: ICPP CPP4.5

9:t PRORLE SAMPLES PlIDOMETER OR p 1 - ELEV 6go isi C RDAARKS DESORPTION BLOWS / N 4 STANDPIPE I Y 1 t a le INSTALLATICN g DEPTH er I 0 - 0 . Laos* 10 compact. dark yellowish brown (10YR412) poody graded, med.SAND. 1 Goa N/A hale gravel. damp (FILL). b

-.. tre Boring CPP45-01 hit refusal al yellowish 1.8 fL Moved and started Loose to compact dark t ' brown(10YR4/2).poody gracled,medium se CPPASCIA. SAND. some gravel. dainp.(ALLLNIUM)

. t D00 I -0C %13 Very loose to loose. Dark yellowish brown (10YR4/2), nett graded, Me to iaso Vo cone SAND and fine to Coarse GRAVEL. ID 0 trace clay, moist(ALLUVIUM) o o 'ca "00 '0% 'a% Po% . 2 '1o o1 'a% io

o '0 '0 '0 - 3 '0 2 Goa N/A . 9, b % 'eo % W/GlAt % 20 o '0 . "0% '0% '.0 '0 'o 'co "0 '0 o '0 - .. 5 "0 io 'ir, Po

0 '0% Is% Vo Gni D 0 3 b - . a 5.CC ENO OF HOLE

- 7 .

* .

DRILL RIG: Hand Anse LOGGED: P. Innis DILUNG CONTRACTOR- Hawley Bera. CHECKED: D. Findlay ODER. L Weems Golder Associates DATE: 10 Nov. 00 PROJECT: Iasi, RECORD OF BOREHOLE CPP45-02,02A SHEET: 1 OF 1 PROJECT LOCATION: ICPP CPP45 BORING DATE: 10 Nov. 90 DATUM MSL gn PROJECT NUMBER: B93-1195.900 BORING LOCATION: )CPP CPP45

SCR PROFILE SAMPLES REZIONETER i0 i ?. REM.ARKS OR 45 g ELF/ ,ffi tu E it 2 DESCRIPTION SLOWS/ N IE. STANDPIPE INSTALLATION § i± Demi 1 t e in (-)IL § 1 C

IT 0 - 1.00•1 to Compact dark yellowish brown (10YR4/2) Katy graded. med.SAND, gP I Grab WA title graver, damp (FILL). • Boring CPP4S02 hit Loose to compact dark yellowish refusal tl 1.0 foot moved brown (10YR4/2).poorty graded. medium 4.3 ft wed end drilled CPP45-02A. SAND. soma gravel. damp.(ALLLNIU14). - - • - - - 1 --- ,,r, -114 '0 yellowish Lem,to compact. Dark e brown (10YR4/2), well graded, fine to cone SAND and fine to coarse GRAVEL. 'o e trace clay. moist (ALLANIUM) e e 'o , e 'o . .- 2 '0 e e ao '02? VitGV%0 e% Vcr Vo .- 3 °o% .. e? e o 2 Gra N/A 'ot b /3.3c, Vo )o% 'oao 'o°0 ?o% - 4 IA 3 0 Gra 3 • N/A 4.1C END OF HOLE

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m a .

- 7 -

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DRUM Hand Auger LOGGED: P. lane OWING CONTRACTOR: Hamay Bras CHECKED: D. Findley CHILLER L Willem Golder Assoclates DATE: 10 Nov. SD 1 PROJECT: ICPP RECORD OF BOREHOLE CPP45-03 SHEET: 1 OF 1 PROJECT LOCATION: ICPP CPP41.5 BORING DATE: 12 Nov. 90 DATUM: MSL gn PROJECT NUMBER: MD1195.900 BORING LOCATION: ICPP CPP45 al

Kt PROFILE SAMPLES I PEDOMETER 1 § OR 2 ElEV D REMARKs FEET CESCRPTCN N .6 STANDPIPE i 1 r 0 In 1 INSTALLATION CP1118 NUMBEFI IY I o De" 1- a Very loose. dark yellowish brown . (10YR4/2) pcorty graded. med.SAND, ..• some gravel, moist (FILL). Gra SP "I 1 b N/A

-c.'• la Loose to compact dark yellowish brown (10YR4/2), well graded. medium SAND and fine warns gravel. moist (ALLUVIUM). II1 2 • i .

.. Loose to compact dark yellowish brown - .; trc (10YRN2).well graded. medium to wane is% SAND and fine to COMO GRAVEL. trace '0% clay. moist (ALLUVIUM) Vo 207 i:. 2 it. - Do 171 *o ic. DO 0 0 .0? b • 3 0 . O 2 Gra O b WA O. O. SW/G4: O. o _o b 4 %:. - °cI Po '.. ,c, '.:i Vo Vo

0)'0 5 O% . Vo ia 1 , Ot Deo Vo .2 coi G•r D 0 3 b N/A 5.70 END OF HOLE 6 .

- 7 -

I DRILL FIG Hand Augr LOGGED: P. Inna DRUM CONTRACTOK Hooey Beet CHECKED: D. Fincliay owtan. L Williefin Golder Associates DATE: 10 Nov.90 PROJECT: ICPP RECORD OF BOREHOLE CPP45-04 SHEET: 1 OF 1 PROJECT LOCATION: ICPP CPP45 BORING DATE: 12 Nov. 90 DATUM: MSL PROJECT NUMBER: 093-1196.900 BORING LOCAIION: ICPP CPP45

BCC PRDFILE SAMPLES PEZOMEIER OR ELEV DESCRIPTION maAs N STANDPIPE 0 INSTALLATION t' DEPTH O A 0 Locos to compact. dwk yellowish brown (10VR4/2) poorly graded, rm.:I:SAND, gravel. damp (FILL). some Grn N/A SP

OSC Very loose to locos. Dark yellowish • t brown (10YR4/2), well graded, medium to cone SAND and fine lo coarse GRAVEL moot(AWJVIUM)

• 2

- 3

2 G. N/A ▪ 4

3 5.80 END OF HOLE

A 7

E

U. RIG dam Auger LOGGED: P. Innis ORLUNG CCNTRACTOR. Harney Bros CHECKED: D Findley ORILLER. L WALarnt Golder Associates DATE: 10 NOII 90 PROJECT: ICPP RECORD OF BOREHOLE CPP45-05 SHEET: 1 OF 1 PROJECT LOCATION: ICPP CPP45 BORING DATE: 13 Nov. 90 DATUM: MSL gin

PROJECT NUMBER: 693-1195.900 BORING LOCATION: ICPP CPP45

SOIL PROFILE SAMPLES 8 PEZOMETER A 1 ce C REMARCI DESCPSPTION 8 g ELEV 5cil &Owe( N ;..1 STANDFIPE S I g F e in M INSTALLATEN i DEPTH Z a o - o - Loose to compact dark yellowish brown (10•194/2) poorly gred. rned.SAND, 1 Ora N/A and fine to come GRAVEL Tram °WY. e dwnp (FILL). •• •• -5O;-5 bed Lome to compact. Detk yellowish &own (10YR4/2), well graded. medium to :2160 cora SAND and fine to coarse GRAVEL tome clay. moot(ALWVIUM) 't• Go - 1 Deo - '0% ‘To L°0 LI, Vo ow IA iA ,°0 - 2 o '0 •0 Po 'o ... F -‘7 —ac Loose to compact. dark yellowish boarn(10YR4/2), well graded med. to Corm SAND. lisle gravel. moist SW 3 (ALLUVIUM) Gm 2 a 14/A 3.22 END OF HOLE

4 .

3 is

r a .

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• -

OPAL MG Mend Auger LOGGED: P. Innis DISL11N3 CONTRACTOR. honey Bros. OIEOCED: 0 Findley DUER: L. Williams Golder Assoclates DATE: 13 Nov so PROJECT: ICPP RECORD OF BOREHOLE CCP45-06,06A SHEET: 1 OF 1

PROJECT LOCATION: ICPP BORING DATE: 13 Nov. 90 DATUM: MSL gn

PROJECT NUMBER: 873-1195.900 BORING LOCATION: ICPP

eta.PROFILE SAMPLES PIEMMETER 1 I g s2 ELEV i REMARKS OR CE9CONTON N g STANDPPE 1 4. 2 i E 3 r Bur:' INSTALL/MN g OWN cc 1 a - 0 Looms to compact, dark yellowish - brown (10YR4/2),poorly graded medium gp • SAND lithe way& darno WILD Ces DX 1 b N/A Loose to compact, dark yellowish - 1 brown (10T114/2), poody graded, medium Three eltx=were required - SAND,some gravel. damp.(ALLLNIUM) due to

im - 2 END OF HOLE

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L. l

a a -

- • -

- 10 -

0 11 -

.12 -

- 13 -

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- 14

CO1U. F03 Hand Amar LCOGED: B. Monism DRUM 031471ACTOR: Howley Bew. CHECKED: D. Fahey MUER L Wilbur. Golder Associates DATE: 13 Noe. SO 1 APPENDDC B LIST OF COMPOUNDS ANALYZED Table B-1

Analytical Categories, Analytes of Interest, Reference Methods and Detection Limit Requirements

Appendix VIII Volatile Organics (EPA Method CLP-VOA, EPA Method 8240)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

1,1-Dichloroethylene 5 5 1,1-Dichloroethane 5 5 1,1,1-Trichloroethane 5 5 1,1,1,2-Tetrachloroethane 5 5 1,1,2-Trichloroethane 5 5 1,1,2,2-Tetrachloroethane 5 5 1,2-Dibromoethane 5 5 1,2-Dibromo-3-chloropropane 5 5 1,2-Dichloropropane 5 5 1,2-Dichloroethane 5 5 1,2,3-Trichloropropane 5 5 2-Picoline 5 5 2-Hexanone 10 10 3,31-Dichlorobenzidine 20 20 4-Methyl-2-pentanone 10 10 Acetone 10 10 Acrolein 20 20 Acrylonitrile 20 20 Allyl chloride 100 100 Benzene 5 5 Bromodichloromethane 5 5 Bromoform 5 5 Carbon disulfide 5 5 Carbon tetrachloride 5 5 Chlorobenzene 5 5 Chloroethane 10 10 Chloroform 5 5 cis-1,3-Dichloropropene 5 5 Dibromochloromethane 5 5 Dichlorodifluoromethane 5 5 Ethyl methacrylate 5 5 Ethyl benzene 5 5 Methacrylonftrile 5 5 Methyl bromide 10 10 Methyl chloride 10 10 Methyl ethyl ketone 10 10 Methyl iodide 5 5 Methylene bromide, Dibromomethane 5 5 Methylene chloride, Dichloromethane 5 5 Table 5-1, Continued

Appendix VIII Volatile Organics (EPA Method CLP-VOA, EPA Method 8240)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

Methyl methacrylate 5 5 Propionitrile; Ethyl cyanide 5 5 Styrene 5 5 Tetrachloroethylene 5 5 Toluene 5 5 trans-1,4-Dichloro-2-butene 5 5 trans-1,3-Dichloropropene 5 5 Trichloroethylene 5 5 Trichlorofluoromethane 5 5 Vinyl acetate 10 10 Vinyl chloride 10 10 Xylene (total) 5 5

Appendix VIE Semivolatiles (EPA Method CLP-SV, EPA Method 8270)

Detection Limit Goals Compound Water, ug/L. Soil, ug/Kg

1-Naphthylamine 20 660 1,2-Dichlorobenzene 10 330 1,2,4-Trichlorobenzene 10 330 1,2,4,5-Tetraclilorobenzene 10 330 1,3-Dichlorobenzene 10 330 1,4-Naphthoquinone 10 330 1,4-Dichlorobenzene 10 330 2-Methylnaphthalene 10 330 2-sec-Buty1-4,6-dinitrophenol 50 1600 2-Chlorophenol 10 330 2-Naphthylamine 10 330 2-Picoline 20 660 2-Chloronaphthalene 10 330 2-Acetylaminofluorene; 2-AAF 10 330 2,3,4,6-Tetrachlorophenol 10 330 2,4-Dinitrophenol 50 1600 2,4-Dinitrotoluene 10 330 2,4-Dimethylphenol 10 330 2,4-Dichlorophenol 10 330 2,4,5-Trichlorophenol 10 330 Table B-1, Continued

Appendix VIII Semivolatile Organics (EPA Method CLP-SV, EPA Method 8270)

Detection Limit Goals Compound Water, ug/L Soil, us/Kg

2,4,6-Trichlorophenol 10 330 2,6-Dichlorophenol 10 330 2,6-Dinitrotoluene 10 330 3-Methylcholanthrene 10 330 3,3'-Dichlorobenzidine 50 1600 3,31-Dimethylbenzidine 20 660 4-Chlorophenyl phenyl ether 10 330 4-Bromophenyl phenyl ether 10 330 4-Nitroquinoline 1-oxide 10 330 4-Aminobiphenyl 20 660 4,6-Dinitro-o-cresol 50 1600 5-Nitro-o-toluidine 10 330 7,12-Dirnethylbenz[a]anthracene 10 330 Acenaphthene 10 330 Acenaphthylene 10 330 Acetophenone 10 330 alpha, alpha-Dimethylphenethylamine 10 330 Aniline 10 330 Anthracene 10 330 Aramite 20 660 Benzo[a]anthracene 10 330 Benzo[a]pyrene 10 330 Benzo(b]fluoranthene 10 330 Benzo[ghi]perylene 10 330 Benzo(k]fluoranthene 10 330 Benzyl alcohol 20 660 Bis(2-chloroethoxy)methane 10 330 Bis(2-chloroethyl)ether 10 330 Bis(2-chloro-l-methylethyl) ether 10 330 Bis(2-ethylhexyl) phthalate 10 330 Butyl benzyl phthalate 10 330 Chrysene 10 330 Di-n-octyl phthalate 10 330 Di-n-butyl phthalate 10 330 Dibenzofuran 10 330 Dibenz[a,h]anthracene 10 330 Diethyl phthalate 10 330 Dimethyl phthalate 10 330 Diphenylamine 10 330 Table B-1, Continued

Appendix VII1 Semivolatile Organics (EPA Method CLP-SV, EPA Method 8270)

Detection Limit Goals Compound Water, ug/L, Soil, ug/Kg

Ethyl methanesulfonate 10 330 Fluoranthene 10 330 Fluorene 10 330 Hexachlorobenzene 10 330 Hexachlorobutadiene 10 330 Hexachlorocyclopentadiene 10 330 Hexachloroethane 10 330 Hexachlorophene 10 330 Indeno(1,2,3-cd)pyrene 10 330 Isophorone 10 330 Isosafrole 10 330 m-Cresol 10 330 m-Nitroaniline 50 1600 m-Dinitrobenzene 10 330 Methapyrilene 10 330 Methyl methansulfonate 10 330 N-Nitrosodimethylamine 10 330 N-Nitrosodi-n-butylamine 10 330 N-Nitrosomorpholine 10 330 N-Nitrosopiperidine 10 330 N-Nitrosopyrrolidine 10 330 N-Nitrosodipropylamine 10 330 N-Nitrosomethylethylamine 10 330 N-Nitrosodiethylamine 10 330 N-Nitrosodiphenylamine 10 330 Naphthalene 10 330 Nitrobenzene 10 330 o-Nitroaniline 50 1600 o-Toluidine 10 330 o-Nitrophenol 10 330 o-Cresol 10 330 O,O,O-Triethyl phosphorothioate 10 330 p-Nitrophenol 10 330 p-Nitroaniline 50 1600 p-Chloroaniline 10 330 p-Chloro-m-cresol 10 330 p-Cresol 10 330 p-(Dimethylamino)azobenzene 10 330 Table B-1, Continued

Appendix VIII Semivolatile Organics (EPA Method CLP-SV, EPA Method 8270)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg p-Phenylenediamine 10 330 Pentachlorobenzene 10 330 Pentachloroethane 10 330 Pentachloronitrobenzene 50 1600 Pentachlorophenol 50 1600 Phenacetin 10 330 Phenanthrene 10 330 Phenol 10 330 Phora te 10 330 Pronamide 10 330 Pyridine 20 660 Pyrene 10 330 Safrole 10 330 sym-Trinitrobenzene 10 330

Appendix VIII Organophosphorus Pesticides (EPA Method 8140)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

Dimethoate 10 330 Disulfoton 10 330 Famphur 10 330 Methyl parathion 10 330 Parathion 10 330 Phorate 10 330 Pronamide 10 330 Tetraethyl dithiopyrophosphate 10 330

Appendix VIII Herbicides (EPA Method 8150)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

2,4-D; 2,4-Dichlorophenoxy acetic acid 10 330 Silvex; 2,4,5-TP 2 200 2,4,5-T; 2,4,5-Trichlorophenoxyacetic acid 2 200 Table B-1, Continued

Appendix VIII Alcohols and Other (EPA Method 8240 or 8015)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

Acetonitrile; methyl cyanide 100 10000 1,4-Dioxane 100 10000 Isobutyl alcohol 50 5000

Appendix VIII Pesticides/PCBs (SW846, EPA Method 8080; EPA, 1986)

Detection Limit Goals Compound Water, ug/L Soil, ug/Kg

4,4'-DDT 0.1 16 4,41-DDE 0.1 16 4,41-DDD 0.1 16 Aldrin 0.05 8 alpha-BHC 0.05 8 beta-BHC 0.05 8 Chlordane 0.5 80 Chloroprene 10 330 Chlorobenzilate 10 330 delta-BHC 0.05 8 Diallate 10 330 Dieldrin 0.1 16 Endosulfan I 0.05 8 Endosulfan sulfate 0.1 16 Endosulfan II 0.1 16 Endrin aldehyde 0.1 16 Endrin 0.1 16 gamrna-BHC; Lindane 0.05 8 Heptachlor 0.05 8 lsodrin 10 330 Kepone 10 330 Heptachlor epoxide 0.05 8 Methoxychlor 0.5 80 PCB 1016 0.5 80 PCB 1242 05 80 PCB 1232 0.5 80 PCB 1221 0.5 80 PCB 1248 0.5 80 PCB 1260 1 160 PCB 1254 1 160 Toxaphene 1 160 Table B-1, Continued

Appendix VIII Inorganics/CLP Target Analytes Detection Limit Goals Compound EPA Method (SW846) Water, mg/L Soil, mg/Kg

Cyanide 9010 0.04 250 Sulfide 9030 10 500

Aluminum 6010 0.2 40 Antimony 6010 0.06 12.0 Arsenic 7060 0.01 2.0 Barium 6010 0.2 40.0 Beryllium 6010 0.005 1.0 Cadmium 6010 0.005 1.0 Calcium 010 5.0 1000 Chromium 6010 0.01 2 Cobalt 6010 0.05 10 Copper 6010 0 025 5.0 Iron 6010 0.05 10.0 Lead 7421 0.005 1.0 Magnesium 6010 5.0 1000 Manganese 6010 0.015 3.0 Mercury 7470 0.0002 0.04 Nickel 6010 0.04 8.0 Potassium 6010 5.0 1000 Selenium 7740 0.005 1.0 Silver 6010 0.01 2.0 Sodium 6010 5.0 1000 Thallium 7841 0.01 2.0 Vanadium 6010 0.08 16.0 Zinc 6010 0.02 4 Table B-1, Continued

Appendix VIII Dioxins/Furans (SW846, EPA Method 8280)

Detection Limit Goals Compound (Totall Water, ug/L Soil, ug/Kg

Tetrachlorodibenzothoxin (TCDD) 0.01 0.5 Pentachlorodibenzodioxin (PeCDD) 0.01 0.5 Hexachlorodibenzodioxin (HxCDD) 0.01 0.5 Heptachlorodibenzodioxin (HpCDD) 0.01 0.5 Octachlorodibenzodioxin (OCDD) 0.01 0.5 Tetrachlorodibenzofuran (TCDF) 0.01 0.5 Pentachlorodibenzofuran (PeCFD) 0.01 0.5 Hexachlorodibenzofuran (HxCDF) 0.01 0.5 Heptachlorodibenzofuran (HpCDF) 0.01 0.5 Octachlorodibenzofuran (OCDF) 0.01 0.5 Table B-1,Continued

Miscellaneous Inorganic Analyses

Parameter Method Detection Limit Goals Water, mg/L Soil, mg/Kg

Acid Digestion SW846, 3050 NA NA Procedure

Arsenic SW846, 7060 0.01 2.0 Barium SW846, 6010 0.2 40 Cadmium SW846, 6010 0.005 1.0 Chromium SW846, 6010 0.01 1.0 Lead SW846, 7421 0.005 1.0 Mercury SW846, 7470 0.0002 0.04 Selenium SW846, 7740 0.005 1.0 Silver SW846, 6010 0.01 2.0 pH SW846, 9040, 9045 - Chloride EPA 300.00 0.015 0.15 Sulfate EPA 300.0 0.200 2.00 Nitrate/nitrite EPA 300.0 0.01 0.10 Fluoride EPA 300.0 0.01 0.10