~ AP42 Section: 1 .I Reference: 67
Title: Results of the March 1990 Trace Metal Characterization Study on Unit 3 at the Sherburne County Generating Station. Interpoll Laboratories, Circle Pines, Minnesota.
June 7,1990. RESULTS OF THE UARCH 1990 TRACE METAL CHARACTERIZATION STUDY ON UNIT 3 AT THE SHERWRKE COUNTY GENERATING STATIM
i
I- - Interpc!’ Lsboratories, Inc. 4500 Ball Road N.E. Circle Pines, Minnesota 55014-1819
TEL: (612) 78’6-6020 FAX: (612) 786-7854
RESULTS OF THE MARCH 1990 TRACE METAL CHARACTERIZATION STUDY ON UNIT 3 AT THE SHERBURNE COUNTY GENERATING STATION
Submitted to:
NORTHERN STATES POWER COMPANY West of Highway 10 Becker, Minnesota 55308
Attenti on:
Bob Catron
Approved by:
Report Number 0-3005 June 7, 1930 PL/prp TABLE OF CONTENTS
1 INTRODUCTION I
2 SUMMARY AND DISCUSSION 4
3 RESULTS E, 3.1 Results of Orsat and Moisture Analyses 10 3.2 Results of Multi Metal Modified Method 5 Sampling 14 3.3 Results of the Hexavalent Chromium Sampling 17
APPENDICES:
A - Sampling Train Calibration Data B - Location of Test Ports C - 4M5 Field Data Sheets - SDA Inlet D - 4M5 Field Data Sheets - Stack E - Chromium Sampling Train Field Data Sheets F - Laboratory Data Sheets for Method 3 G - Results of Trace Metal Analysis H - Results of Lime Analysis I - Results of Trace Metals Analyses on Csal Sample J - Procedures K - Calculsrior Equeti~xs
ii ABBREVIATIONS
ACFH actual cubic feet Der mlnute cc tml) cubic centimeter (milliliter) DSCFH standard cubic foot of dry gas per minute DSHL drv standard milliliter DEG-F (OF) degrees Fahrenheit DIA. d iame ter FP finished Droduct for plant FT/SEC feet Der second gram GPH gallons per minute GR/ACF grains per actual cubic foot GR/DSCF grains per dry standard cubic foot g/dscm grams per dry standard cubic meter HP horsewwer HRS hours IN. inches IN.HG. inches of mercury IN.WC. inches of water LB DOUnd LB/DSCF pounds wr dry standard cubic foot LB/HRC pounds per hour LW10 BTU pounds Der million British Thermal Units heat input LB/HHBTU pounds per million British Thermal Unlts heat input LTPD long tons per day MW megawatt mg/Nm: milligrams per dry standard cubic meter uq/Nm' micrograms per dry standard cubic meter microns (urn) micrometer UIN. minutes ns nanograms ohm-cm ohm-centimeter PH particulate matter PPH pounds per hour PPH parts per million DDmC parts Der million carbon DDm.d Darts per million. dry DDm.W Darts Der million. wet QDt Darts per trillion PSI pounds oer sauare inch SP.FT. sauare feet T PD tons per day US micrograms v/v percent by volume w/w percent by weight < -< (when following a number)
Standard conditions are defined as 68 OF (20 OC) and 29.92 IN. of mercury pressure.
iii 1
Jeff Cole, RTI, says this is a dry bottom boiler, according to I the UDI/EEI database. Jeff has been working with the NSP data for five years and, therefore, I am taking his word on this. 4 Jj
1 1 I' 1 INTRODUCTION
?r H?rci 27, !9W. Int2rzc! 1 i3isratsr:er personnel 23ndgcted a trace ?letal characterization study on the Unit 3 Dry Scrubbing System at the NoTtnern States Pcwer :Company (NSP) Sherburne County Ceneraticg Stst:sn loc3T.ea ii: Pxk2r, M:nne;c.ta. 3n-s;:e t2sting was performed by 3. 'Vu Koever, E. Tr~bridge, Y. k'aehler axd C. 3ainville. Cocrdinstizr be-ween testicg act7v:ties and Jlan'. operation w2s provided by Bob Cat:on of NS?.
IJn't 3 is a Babcock and Wilcou. 8€0 MW boiler which came on lice In 1927. The boiler is flred with Fulvsriiad subSituminous :oal from
Montma. Particulate and sulf?lr dioxid? ecjssims are ccntrolled b:: 3 dry scrubber consisting af a sprzy dryer abjorber (SIX) and tagP.cuse.
Scrubbed flue gas is exhausted t3 the atmos3here by a 952-foot high radial brick-lined corcrete .stack.
Yulti-Metal Modified Method 5 (4ME) sampling train was used to isokinetica!ly collect sclid and vapor phase trace metals. The samples 'were crrllected and analyzed as per the EPA Draft Method "Methodology far the Determination of Metals Emissions in Exhaust Gases from Stationary Source Combustion Processes". The aerosol or solid phase trace metal samples were collected on high purity Pallflex' filters. The vapor phase trace metals were collected in an all glass impinger train. The first and second impingers each contained :00 cc of a mixture of 5% HNO? and 10% H,O,... The third and fourth impingers contained 100 cc cf a mixture of 4% KMnC, and 10% H,SO:. These impingers collect any elemental mercury which might penetrate the first two impingers.
The recovered four-part trace metal samples ware returned to the laboratory where the prob? rinse, filter and nitric acid impinger cat.:h &re smbined, dissc:ve,j in acid (inclJd:;.c the gls; fiber fiiter! and 5na:yied by Inductively Coupled Argon Plasma Emission Speztrometry (ICP). I
In scme cases, the same here reanalyzed by grachite furnace atonic li absorption spectrometry fer grezter sensitivity. The permanganate mersiry catch and en a?icuot of the frcnt balf. cz:ccI were enalyred by .:olb vap?r s atomic abscratior. spectrometry :CV/AC;. Twc field-biased b:anks 'e?~ collected and recovered at each test site and analyzed with the field 1' samples.
?he CrlVI) samples *e-e co??ected*.ith ? Modified Method I? sampling Y train withcut the cptional filter. Pallflex'. Type 2500 QAT ultrapure filters were used in the post-impinger filter holder in place of the normal glass fiber fllters. The sampling train was rigorously cleaned prior to sampling to remove any traces cf organic materials which react rapidly tc reduce Cr(V1) to Cr(II1). In addition, nonorganic vacuum grease was used to sea! all ground glass joints in the sampling train.
A heated glass-lined silmpling probe was used to extract the samplos from the stack. The first two impingers were charged with 1 N NaOH which acts as a preservative. The samples were collected following Method 5 sampling protxol. After completion of sampling, the frc4 half of the train was recovered using 0.5% Na,CO:... The backhalf was recovered using 0.1 N Na@H. The recovered samples were stored at 4 'C until analysis.
In the laboratory, the three-part field sample was combined, pH adjusted, APDC chelating agent added and extracted with MiBK. The MiBK was then evaporated and the residue taken up in nitric acid. The extract was then analyzed by ICP in accordance with EPA Method 6010.
An integrated flue gas sample was extracted simultaneously with each particulate and sulfur dioxide sample using a specially designed gas sampling system. Integrated flue gas samples were collected in 44-liter Tedlar bags housed in a protective aluminum housing. After sampling was complete, the bags were sealed and returned to the laboratory for Orsat aralysis. Priyr to sampling, tne Tedlsr bags are leak, checked at 1:.
2 IN.HI;. v3cuum w3;h a? in-line -stmeter. 332s with any detectable inleakage are discarded.
Testing on the SDA Inlet was conducted using a singls point traverse. Each test run was 60 minutes in duratior. Testing cnthe Stack was conducted from four test ports oriented at 90 degrees. These test ports are ,located seven stack diameters downstream of the breeching inlet and eievsn diameters upstream of the stack exit. 4 16-ooint traverse was used to extract representative trace metals and chromium VI samples. Each traverse point was sampled four minutes to give a tota? sampling time of 64 minutes per run.
The important results of the test are summarized in Section 2. Detailed results are presented in Section 3. Field data and all other supporting information are presented in the appendices.
3 2 SUMMARY AND DISCUSSION
The results of the trace metals determinations are summarized in Tables 1 and 2. Chromium VI results are DreSented in Table 3.
The mass rates of trace metals determined at the Inlet sampling location, when stoichiometrically converted to the appropriate or actual species, and adjusted for unanalyzed species such Si02, Ti02 SOj and P20j give total particulate mass flow rates which agree very well with the total inlet particulate mass flows measured on August 9, 1988 when a complete duct traverse (48-points) was performed as shown below:
Particulate Mass Rate LB/HR Calculated from Measured Trace Metals Run 3-27-90 8-9-86 1 32300 44300 2 472@0 4420@
Average 39700 42300
The above calculated mass rates for 3-27-90 do not exhibit good agreement with the particulate mass rate calculated directly from a gravimetric analysis of the trace metal samples (71,000, 67000 and 28000 LB/HR). This is not surprising inasmuch as the 3-27-90 sampling consisted of a 3-point traverse. This data suggests a severe stratification of particulate mess flaw in the inlet dxting.
Some contaminatiop occurred of the Run 1 sample :,Zliected at the stack test site uh:ch invalidated the Run ! results for arsenic, cadmium and zinc. This contaninaticn did nct effect cther trace Elements nor vas it observed in the subseqirent test rcns.
P No other difficulties were encountered in the field or in th6 la’soratsry eveluation of the samples. On the basis of this fact ane a complete review of the entire data and results, it is our opinion, subject to the above qualifications, that the results reported herein are accurate and closely reflect the actual values which existed at the time the test was performed.
E Table 1. Results of the March 27, 1990 Trace Metal Determinations on the Unit 3 Dry Scrubber System at the NSP Sherburne County Station in Becker, Minnesota.
Concentrat ion ( udNm3) Run 1 Run 2 Run 3 Element Inlet Stack Inlet Stack Inlet Stack
Aluminum 1 .39X105 261 2.56X105 67 1 .87X105 101 Arsenic 69.6 X 66.0 c.056 83.6 <.056 Boron 8430 2620 8270 445 10900 1890 Barium 10300 t6.5 15800 t6.5 10300 t6.5 Beryllium 22.9 .0022 24.9 .0067 26.5 .0135 Calcium 3.33X105 465? 6.O6X1O5 259 3.97X105 251 Cadmium 8.15 X 8.23 11.8? 7.34 6.84 Chromium 266 15.6 281 9.26 316 7.07 Copper 587 108 555 52.2 748 25.6 Iron l.38X1O5 143 l.lOXl0~ 103 1. 58X105 33.7 Potassium 51700 251 48500 84.8 58300 81.9 Magnesi urn 20000 40.3 30000 16.7 30400 29.2 Manganese 5450 7.73 5210 51.9 6280 5.16 Molybdenum 64.5 (4.4 47.2 t4.4 87.1 (4.4 Sodl um 84900 949? 1.12x105 627 1.19x105 653 Nickel 204 10.9? 174 10.0 237 3.59 Lead 640 16.9 494 5.35 654 t4.5 Sel eni urn 45.4 (2.72 32.2 (2.79 58.5 t2.81 Antimony 83.8 .97 58.1 0.22 93.9 t.20 Stronti um 19900 1.63 11700 5.50 24700 5.61 Vanadi um 704 t.ll 643 t.ll 836 <.11 Zinc 264 X 2 58 35.6 256 23.4 Mercury 7.88 5.62 7.56 2.34 4.95 4.6 Silver 2.29 <.33 2.31 t.33 2.30 t.34
x = Result invalidated due to field contamination ? = Result may be high due to field contamination
6 uu$1 I
mw01 mn -n a -L clJ NU)
7 Table 3 Summary of the Results of the March 27. 10'30 Hexavalent Chromium (CrVI) Determinations on the Unit 3 Stack at the KSP Sherburne County Station.
Concentration Emission Rate Test/Run (us/Nm') (LB/HR) 2/ 1 1.30 0.0095 2/2 0.39 0.0028 2/3 1.41 0.0100 Avg 1.03 0.0074
8 3 RESULTS
The results of all field and laboratory evaluations are presented in this section. Gas composition (Orsat and moisture) are presented first followed by the computer printout of the trace metals and chromium VI sampling data. Preliminary measurements including test port locations are given in the appendices.
The results have been calculated on a personal computer using programs written in Extended BASIC specifically for source testing cal- culations. EPA-published equations have been used as the basis of the calculation techniques in these programs.
The emission rates have been calculated using the product of the concentration times flow method. 3.1 Results of Orsat and Moisture Analyses
10 Interpol 1 Report No. 0-3005 Northern States Power - Sherco Becker. Minnesota
Test No. 1 Unit 3 SOA Inlet
Results of Orsat & Moisture Analyses----- Methods 3 6 4(?v/v)
Run 1 Run 2 Run 3 Date of run 03-27-90 03-27-90 03-27-90
Dry basis (orsat)
carbon dioxide...... 13.30 13.40 13.50 oxygen ...... 6.70 6.50 6.40 carbon monoxide...... 0.00 0.00 0.00 nitrogen...... 80.00 80.10 80.10
Wet basis (orsat)
carbon dioxide ...... 12.03 12.05 12.06 oxygen...... 6.06 5.84 5.72 carbon monoxide ...... 0.00 0.00 0.00 nitrogen...... 72.38 72.02 71.54 water vapor...... 9.53 10.09 10.68
Dry molecular weight ...... 30.40 30.40 30.42 Wet molecular weight ...... 29.21 29.15 29.09 Specific gravity ...... 1.009 1.007 1.005 Water mass flow ...... (LB/HR) 662829 695254 743527
11 1.068 1.075 1.074 I Interpoli Report No. 0-3005 Northern S:3.t?s P3wcr - Snercc ‘I Becker, Minnesota Test NO. i 1 Unit 3 Stack I Results of Orsat B Moisture Analyses-----Methods 3 B 4(tv/v) Run 1 Run 2 Run 3 1 Date of run 03-27-90 @3-27-96 03-27-90
1 Dry basis (orsat) 1 carbon dioxide ...... 13.50 13.80 13.90 oxygen ...... 6.50 6.20 6.10 I carbon monoxide ...... 0.00 0.00 0.00 c nitrogen...... 80.00 80.00 80.00 1 Wet basis (orsat) 4 carbon dioxide...... 11.43 11.75 11.89 oxygen...... 5.50 5.28 5.22 I carbon monoxide...... 0.00 0.00 0.00 nitrogen ...... 67.70 68.13 68.42
I water vapor ...... 15.37 14.84 14.47
I Dry molecular weight ...... 30.42 30.46 30.47 Wet molecular weight ...... 28.51 28.61 28.66
I Specific gravity ...... 0.985 0.988 0.990 I Water mass flow ...... (LB/HR) 0.00 0.00 0.00 1 I
1.067 1.365 1.265 I 12 'I
Interpol1 Report No. 0-3005 Northern States Power - Sherco Becker. Minnescta
Test No. 2 unit 3 Stack
Results of Orsat 6 Moisture Analyses----- Wethods 3 6 4(Zv/v)
Run 1 Run 2 Run 3 Date of run 03-27-90 03-27-90 03-27-90
Dry basis (orsat)
carbon dioxide...... 13.60 13.60 13.60 I I 6.00 I oxygen ...... 6.10 6.10 I carbon monoxide ...... 0.00 0.00 0.00 I nitrogen ...... 80.30 80.30 00.40
Wet basis (orsat)
carbon dioxide ...... 11.68 11.61 11.58 oxygen ...... 5.24 5.21 5.11 carbon monoxide...... 0.00 0.00 0.00 nitrogen...... 68.98 68.55 68.46 water vapor...... 14.10 14.63 14.85
Dry molecular weight ...... 30.42 30.42 30.42 Wet molecular weight ...... 28.67 28.60 28.57 Specific gravity ...... 0.990 0.988 0.987 Water mass flow ...... (LB/HR) 0.00 0.00 0.00 t I I I 1 I I I
I 3.2 Results of the Multi Metal Modified Method 5 (4M5) SamDling I I I I I I I I 1
I 14 I
Interpoll Report No. 0-3005 I Northern States Power - Sherco Becker. Minnesota
I Test NO. 1 Unit 3 SOA Inlet
I Results of the Multi Metal Modified Method 5 (4M5) Sampling I Run 1 Run 2 Run 3 I Date of run 03-21-90 03-21-90 03-21-90 Time run start/end.. ...(HRS) 840/ 940 1025/1125 1210/1310 1 Static pressure ...... (1N.WC) -13.20 -13.20 -13.20 Cross sectional area (SQ.FT) 1090.00 1090.00 1090.00 Pitot tube coefficient...... 840 .040 .E40
I Water in sample gas condenser...... (HL) 0.0 0.0 0.0 impingers...... GRAMS) 65.0 82.0 90.0 I desiccant...... GRAMS) 28.0 16.0 15.0 total ...... GRAMS) 93.0 98.0 105.0 I
Gas meter coefficient...... 0.9992 0.9992 0.9992 I Barometric pressure. .(IN.HG) 29.12 29.12 29.12 Avg . orif .pres .drop. . (IN. WC) 1.69 1.67 1.70 I Avg. gas meter temp..(DEF-F) 01.7 87.5 90.4 Volume through gas meter.. .. at meter conditions ...(CF) 43.75 43.76 4q.20 I standard conditions.(DSCF) 41.63 41.20 41.39 Total sampllng time .... (MIN) 60.00 60.00 60.00 Nozzle diameter ...... (IN) .249 .249 .249 I Avg.stack gas temp ..(DEG-F) 200 200 2 80 Volumetric flow rate...... I actual ...... (ACFH) 3691895 3660354 3697315 dry standard...... (DSCFH) 2243426 2209850 2216340 I Isokinetic variation..... (%) 99.1 100.2 100.4 1 I
I 15 Interpoll Report No. 0-3005 Northern States Power - Sherco Becker. Minnesota
Test No. I Unit 3 Stack
Results of the Multi Metal Modified Method 5 (4M5) Sampling
Run 1 Run 2 Run 3 Date of run 03-27-90 03-27-90 03-27-90
Time run start/end.. ... (HRS) 840/ 954 1025/1139 1210/1324 Static pressure ...... (IN.WC) -0.72 -0.72 -0.72 Cross sectional area (SQ.FT) 683.49 683.49 683.49 Pitot tube coefficient...... 840 .840 .E40
Water in samp e gas condenser...... (ML) 0.0 0.0 0.0 impingers...... (CRAMS) 115.0 110.0 109.0 desiccant...... (GRAMS) 10.0 7.0 4.0 total ...... (CRAMS) 125.0 117.0 113.0
Gas meter coefficient...... 0.9980 0.9980 0.9980 Barometric pres sure.. (IN. HG) 28.98 28.98 28.98 Avg. orif. pres .drop.. (IN. WC) 0.88 0.83 0.83 Avg. gas meter temp..(DEF-F) 63.4 62.8 64.0
Volume through gas meter.... at meter conditions. ..(CF) 33.22 32.38 32.27 standard conditions.(DSCF) 32.45 31.67 31.49
Total sampling time ....(MIN) 64.00 64.00 64.00 Nozzle diameter...... (IN) ,178 .178 .I78 Avg.stack gas temp ..(DEC-F) 167 166 166
Volumetric flow rate...... actual...... (ACFM) 2829194 2829323 2811269 dry standard ...... (DSCFM) 1950168 1965867 1962255
Isokinetic variation.....(%) 102.9 99.6 99.2 I I I I I I I I
1 3.3 Results of the Hexavalent Chromium (Cr VI) SamDling I I I I I I I I I
I 17 Interpol1 Report No. 0-3005 Northern States Power - Sherco Becket-. Minnesota
Test No. 2 Unit 3 Stack
Results of Hexavalent Chromium (Cr VI) Sampling
Run 1 Run 2 Run 3 Date of run 03- 2 7 -90 03-27-90 03-27-90
Time run start/end.. ... (HRS) 1430/1540 1550/1659 1710/1820 Static pressure ...... (IN.WC) -0.72 -0.72 -0.12 Cross sectional area (SQ.FT) 683.49 683.49 683.49 Pitot tube coefficient...... 840 .840 .840
Water in sample gas condenser ...... (ML) 0.0 0.0 108.0 impi nge rs ...... (GRAMS) 104.0 106.0 8.0 desiccant ...... (GRAMS) 5.0 8.0 0.0 total ...... (GRAMS) 109.0 114.0 116.0
Gas meter coefficient...... 0.9980 0.9980 0.9980 Barometric pressure.. (IN.HG) 28.80 28.80 28.80 Avg. orif.pres.drop..(IN.WC) 0.83 0.83 0.84 Avg. gas meter temp..(DEF-F) 70.1 67.2 74.1
Volume through gas meter.... at meter condltlons ... (CF) 32.66 32.55 32.92 standard conditlons.(DSCF) 31.30 31.37 31.32
Total sampling time .... (MIN) 64.00 64.00 64.00 Nozzle diameter ...... (IN) .178 .I78 .I78 Avg.stack gas temp ..(DEG-F) 164 164 163 Volumetric flow rate...... actual ...... (ACFH) 2801458 2808571 2804604 dry standard ...... (OSCFM] 1957528 1950487 1944863
Isokinetic variation.....(*) 98.9 99.5 99.6
18 I I I I I I
APPENDIX A
... 1 SAMPLING TRAIN CALIBRATION DATA I I I I C YIYI CUI- e. <& 6s UV 2% 1 0 'it J .1 m a Um ll $I V C a U 0 m m d 3 0 5 c 5 U s 8 2 f I n a .J .I- U 0 -0 nL 48 0 .P U e uiui Y) H a mWN a 0 c V 0 C II c m ? L I-YI V U U L "8%m II 8 !i V r: a A& D ae 1 I U
Ea II V e m 0 a . > -I- e WN c 0 m SI U 11 V 0 Cl rr I- a ll 0 2: C II
I1 A- 1 I. I I I 0
A- 2 I Interpoll Laboratories, Inc. (612) 786-6020
Nozzle Callbratlon Data Sheet
Date or Calibration: Manh 27. 1990 Nozzle Number 5-4 Technician: E. Trowbridge
Nozzle rotated by 60 degree increments and diameter measured to nearest 0.001 inch. Observed readings and average:
Pos 1t 1on 01 ameter ( 1nches )
1 0.249
2 0.250
3 0.249
Average: 0.249
A- 3 I:
Interpol 1 Laboratories II (612)786-6020 S-Type Pitot Tube Inspection Sheet I'I Pitobe No. //-/7 I Pitot tube dimensions: 1. External tubing diameter (Dt) , 3,' IN. 0 2. Base to Side A opening plane (PA) .+4D IN. Base to Side B opening plane (P,) Yd/ 3. - IN. I I' 4. 5. 1:
6. 7. I-
8. I 9. I Distance from Pitot to Probe Components: 10. Pitot to 0.500 IN. nozzle *7sB/ IN. I
11. Pitot to probe sheath It&d IN. 12. Pitot to thermocouple (parallel to probe) x@BIN. I 13. Pitot to thermocouple (perpendicular to probe) ~A~IN.I
Date of Inspection: Inspected by : I /z-g-sp I I
A- 4 I n 3 c 0
x 8 N VI i 2 VI n .I U . 0 m 3 -I 8 0 V c E a a i e -3 0 c c s a Y c I c Y c L t aI n : si c P s -1 r c V L < 0 r a U 28s... 0 m Y VIO-I 0 e Y 0 P -IN- n 0 V c r il Y n II 6 U L n z V V C a c L n O P d L II r z 0 r Y c xP t a!k s II a8 a - s (D z II Y t! t! a d V r z n a g II e r i 0 a L c V V 0 Y I- m 2 0 C II
31 A- 5 c L a u
al -n m al I-1 U m L I-
v) m z PI Y I.I
U 111 -E m cn m
Q, W -m w m a sm E c c 0 c
L al U 2 Y r" wl al . c, Y QJ I 0 N I A 4 c . 0 ..U -0 \. al -m m I
A- 6 1 Interpoll Laboratories, Inc. (612) 786-6020
Nozzle Callbration Data Sheet
Date of Calibration: March 27. 1990 Nozzle Number 4-3 Technic4 an: 0. Van Hoever
Nozzle rotated by 60 degree increments and diameter measured to nearest 0.001 inch. Observed readings and average:
Pos iti on Diameter ( 1nches )
0.175
0.177
0.180
Average : 0.178
A- 7 Interpol1 Laboratories (612)786-6020
S-Type Pitot Tube Inspection Sheet Pitobe No. g- 14
Pitot tube dimensions:
1. External tubing diameter (Dt) * 31d IN. 2. Base to Side A opening Plane (PA) f& ir, IN. 3. Base to Side B opening plane (p,) * vd> IN.
6. B1 < so- / 7. B2 C So /
.. 8. z <.125’ ,33 9. W <.0625” *a&
Distance from Pitot to Prc-r Components: .. 10. Pitot to 0.500 IN. nozzle , 7/a IN. 11. Pitot to probe sheath 7.A4 IN. 12. Pitot to thermocouple (parallel to probe) x8L@ IN.
13. Pitot to thermocouple (perpendicular to probe) . 74 W.
Date of Inspection: Inspected by:
/2 -8-84
A- 8 I EFCI Method 5 Gas Meterinq Svstem 6uality Control Check Data Sheet
Instructions: @perate the control module at a flow rate equal tu .'''He for 10 minuter before attaching the um- bilical. Eecord the following data:
Meter Temp. (OF) Ti me Vol wne !min) (CF) Inlet Out 1 et
Calculate Y,, as follows:
I+ 'T'=- i=, nut within the range uf C1.5'7 to l.OTI., "the volume niete:ing system shot.tld be investigated before beginning. " i,ctsrps!l1 .. Ls~c.ratot-i~~.lnc.
;.L.LL.1 I r') ys&-..+:)&,<:!
E_F'n Method 5 Gas Metering Svstem Ckiality Control Check Data Sheet
Instructions: Operate the control module at a flow rate equzl to ,';HE for 1Q minutes before attaching the um- bilical. F:ecord the following data:
.-
Calculate Y,, as follows:
0 .5 Y," = 1.786 [I (t, p,+ 460)] r v- Ixterpoll Laboratories. inc. ie.12) 73&--&<1&,:)
EFQ Method 5 Gas Metering Svstem Rxality Control Check Data Sheet
Instructions: Operate the control module at a flow rate equal to ."'.Hefor 10 minutes before attaching the um- bilical. Record the following data:
Meter Temp. (OF) Ti me Vol un1e !min) (CF) Inlet Outlet
Calculate Y,, as follows:
I+ Y,, iE, no.t within the range of 0.97 tu l.OZ, "the volume nieter.ing s.ystem shsuld he investigated before beginning. "
CFR Title 40, Part 50. Appendix A, Mettiud 5, Section 4.4. 1 5-432R A-11 Interpol 1 Laboratories, Inc. Temperature Measurement Device )t Calibration Sheet
I unit under test: TI Vendor /&-&A!! Model 357k3-T Serial !umber hr-/ Range -//a.6 -F rf * /99g OF Thermocouple Type Date of calibration z-s-fa Techni c I an KTh ~4dkfb 40 .I
Method of Calibration: [7 Comparison aqains; ASTW mercury in glass thermometer usinq a theroostarted and insulated alulinum block design to provide uniforl temnerature. The temperature i8 adjusted by adjustlnq the voltage on the block hem cartridqe. D Ome$a Model CL-300 Tpe & Ihermcouple Simulator ihich orovides 21 precise temoerature eouivalent lillivo $ignrls. The CL-300 is cold junction comnensated. Calibratlon accuracy is 0.11 of soan (210O0Ft 1 dew ifor neqativs teioeraturei add ?. 2 deqrees. The CL-300 simulates exactly the milllvoltage of a lvne K thermocouole at the indicated temoerature. 'I .~
~~ Des1red Temperature of Response of Devi ion d--' Temp (OF) standard or Unit ilnder lest Nanlna1 Simulated Temp (OF) (9)
0 100 200 300 400 500 600
1000 1100 1200 1300 1400 1500 1600 1700 1800
2000 2100
1 OF = off scale response by unit under test (OF) X dev = 100 At / (460 + t) &' unit in tolerance Unit was not in tolerance: recalibrated - See new calibration sheet.
A- 12 Interpol1 Laboratories, Inc.
Jemwrature Measurement Cevlce Fallbration Sheet
Unlt under test: Vendor - Serial Wunber Mode 1 ?9A 4-r - x /8T - v Range - //> .b Y ?J j- /9W '/ OF Thermocouple Type Cr- 3rB - Date of Callbration Z --i -9d Technlclan
Method of Callbratlon: a Caipiricon iqiinct ASTI1 urcury in qlics thermetir osing I thermostatted and inrulited iluiinui block designe8 to provide mifori teineriture. The tomperiture is idjosted by idjnstia9 the voltage on the block beiter cirrridge. Omega Rodel CL-300 I!pe I Therwcauole Siiulitor which ororides 22 priciie teioeritore eouirtlent iillirolt & ciqntlc. The CL-~OO is cold junction cointnrited. Cilibrition accuracy is: 0.11 of spin 12100~12 1 degree Ifor neqitire teineratures tdd f 2 degrees. The Cl-100 timuliter exictly the iilliroltiqc of I Iyne I theriocouDle it the indicate0 teaoeriture.
Desirfd Temperature of Response of Devlc Temp (F) Standard or Unit Under Test Nominal Simulated Tmv (OF) ('5) At (OF)
0 100 200 300 400 600 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000
2100 ~ I I 1 I I Averages: I d.?b OF = off scale response by unlt under test (OF)
X dev = 100 At~ / (460 t) unit In tolerance Unit was not in tolerance: recalibrated - See new calibration sheet. 5-433 A- 13 Interpol1 Laboratories, Inc.
Temperature Measurement Oevlce Calibration Sheet
Unlt under test: Vendor GoRDOd Model 53 In K Serial Number PDT - /b Range -1Iz'F .Ib fqqq.r OF Thermocouple Type &_ Date of Ca::bratlon 3 -€--IO Technlclan 5.aa Id# /LLP ti Method of Callbratlon: a Comparison apains: ASTW mercury in glass thermoseter uslnp a thermostatted and insulated alumlnul block design; 1II to provide uniform tenotrature. The temperature IS tdpstcd by adjusting the voltage on the block beittr cartridge. $i Ole98 Model CL-300 TyDe I Therwcouple Simulator which orovides 22 precirc tenoerature eouivalent Illli~Ol signals. The EL-300 is cold junction comoensated. Calibrstlon accuracy is 0.11 of soan (210041 f. 1 degree . ifor neqative temoeratures add $ 2 degrees. The CL-300 simulates clactly the millivoltage Of I Tvoe I @ 1 thermocouole at the indicated teaoerature.
Desired I Temperature of Response of Devia ion Temp (Of) standard or Unit Under Test Nmlnal I slmulated Temp (OF) (OF) At (%I
0 . .s 100 47.7 200 & 300 298 400 39s- 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000 2100 Averages:
OF = off scale response by unit under test (OF) X dev = 100 At / (460 + t) unlr In tolerance unit was nor in tolerance: recalibrated - See new calibration sheet. 5-434
B
. . ~.. .. . _. . . - ...... APPENDIX B .. LOCATION OF TEST PORTS ...... ~ B-1 33 Y
... ..
8- 2 ...... APPENDIX C
4M5 FIELD DATA SHEETS - SDA INLET INTERPOLL LQBDRATOHIES EPR HE 'HOD 2 FIELD DnTQ SHEET Job &d-5&&& Source &a fl3 A2-NLrr Test 1Hun Date 3-27-& Stack dimen. 3&&!4 c/36 IN. Dry bulb OF Wet bulb 'F nanometer: @Reg. 0 Exp. 0 Elec. Barometric pressure A'flbZ in Hg Static pressure -/X Z- in wc Operators Kr/a,v&,oge -**,e Schematic of F'ltot No. /7-//v Cp s% Cross Section
Port (in) INTERPOLL LABORATORIES EPCI METHOD 5/17 SAMPLE LOG SHEET I \~
Job d5f/cHcAc 0 Date 3-27-96Test Run 4-1 Source *(HI ?-3 6P4 L-A Le? No. of traverse points 3 Method %td- Filter holder: -nht 5s Filter type: Ss ZNsnwX
Sample Train Leak Check:
Pretest: ( 0.02 cfm at 15 in. Hg. (vac) Postest : - cfm at Kin. Hg. Bc (vat) 4
Particulate Catch Data:
NO.S of filters used: Recovery solvent (5)
5s *do Q acetone 0 otherts)
No. of probe wash bottles: / Sample recovered by: E7
Condensate Data:
Integrated Gas Sampling Data:
Bag Material: 5-layer CIluminized Tedlar Size: 5 Pretest lea): check: @ cc/min at /rin. Hg. Time start: &q/ (HRS) Time end: d)yJy (HRS) Sampling rate: 4/lc0 cc/min Operator: Za-- S/N of O= Analyzer used to monitor train outlet: 7 CF-02:
c- 2 S-0046RR I c- 3 I INTERPOLL LABORATORIES EVA METHOD 5/17 SAMPLE LOG SHEET ,~
Job &.g//k-#//Cfl Date 3-s7-98 Test -f Run 3!I source Y#/T~SOP ZA’LI~ No. of traverse points 3 Method dlV5 Filter holder: YMrrrrC-fx Filter type: $3
Sample Train Leak Check:
Pretest: ( 0. 3 cfm at 15 in. Hg. (vac) Postest : - 2 cfm at dn.Hg. (vac)
Particulate Catch Data:
NO.S of filters used: Recovery solvent (s) ssi# a3 p( acetone 0 other(6) No. of probe wash bottles: / Sample recovered by: Fr -
Condensate Data:
Impinger No. 2 2- I Impinger -No. 3 7 I z@lI-~ Condenser
Desiccant /L/// 139s /4
Integrated Gas Sampling Data:
Bag Pump NO. /39’ ox NO. 2 8 Bag NO. 4
Bag Material: 5-layer aluminized Tedlar Size: 4s Pretest leal: check: cc/min at /rin. Hg. - Time start: ,Qzb (HRS) Time end: //zf(HF?S) Sampling rate: U/BO cc/min Operator: F7 S/N uf O= Analyzer used to monitor train Outlet: 2 I c-4 S-0046RR so.- n I. &e- 0-.
c- 5 INTERPOLL LABORATORIES EPA METHOD 5/17 SAMPLE LOG SHEET 1,
NO. or rraverse poinrs Zilter holder: S&'IZ#cX-S5 Filter type: 5s-
Sample Train Leak Check:
Pretest: ( 0.02 cfm at 15 in. Hg. (vac) Po6 test : - A cfm at J1/ in. ~g.(vac)
Particulate Catch Data: No.s of filters used: Recovery solvent (s)
SSzZ/S- & acetone 0 otherts) / No. of probe wash bottles: Sample recovered by: --
Condensate Data:
Difference
esiccan
Integrated Gas Sampling Data: ~agPump NO. 39 BO,: NO. rD Bag NO. 3
Bag Material: 5-layer CIluminized Tedlar Size: 4s Pretest leal: check: J cc/min at 1~ in. ~g. - Time start: />I/ (HRS) Time end: /T/f (HRS) Sampling rate: +'& cc/min Operator: Fr
S/N Of O= Analyzer used to monitor train Outlet:
CF-t:iZT - I C-6 S-0046RR-
I 1 I B 1 I 1
... i. 1 APPENDIX D
1 45 FIELD DATA SHEETS - STACK ! I 1 1 I I I 1 I Job dS3 / .5HlEP/ 0 r Source IJAJ IT d- 3 STAC IC Test Hun Q Date 3-27-CiQ Stack dimen. 354 IN. Dry bulb' 'F Wet bulb- 'F Manometer: meg. 0 Exp. 0 Elec. Barometric pressure 2h?Fr in Hg A & 72- -I Static pressure in WC 0;FLEVA'TOR Operators 3 gd d Fraction Distance Distance of from Stack from End of Diameter Mall (in) Port (in) I 9- I I I A 7 1; I U I I U 1 I I I I I ll I I n I a Temp. meic. tool :- SiN: Time End: hrsl f< GT r.cthincj= reg. n.;r,mneter: 5-u-1 e.,panaed: .' E = electronic 5-392.1 INTERPOLL LABORATORIES EPA METHOD 5/17 SAMPLE LDG SHEET 1, Job ds? / 5k/15RC 0 Date Source UN/ 7 UT Method 4 Lhr Fi1 ter holder: 35 Filter type: 4 / / Sample Train Leak Check: Pretest: ( 0.02 cfm at 15 in. Hg. (vac) Postest : - -8 cfm at in. Hg. Particulate Catch Data: No.6 of filters used: Recovery solvent (6) No. of probe wash bo Sample recovered by: - Condensate Data: Impinger NO. 2 ' 5/r 4/m /i 5- Impinger -No. 3 <' Condenser a, Desiccant L49f /Y SY /o I Integrated Cas Sampling Data: Bag Pump No. -zHT Box No. i7 Bag No. / Bag Material: Slayer Aluminized Tedlar i=e: Pretest leal: check: in. Hg. D cc/min at rfz, p3 Time start: @a+% (HRS) Time en&/ ( HRS- ) Sampling rate:76 cc/min Operato S/N of o= Analyzer used to monltor train outlet: &-' D- 2 S-0046RR I D- 3 INTERPOLL LABORATORIES EPA METHOD 5/17 SAMPLE LOG SHEET I! Job /45P $Heco -f// - Date Source u.c/rr-3 &of- Method 4%- Filter holder: 5s I Sample Train Leak Check: Pretest: ( 0.02 cfm at in. Hg. (vac) Postest: - 601;fm at 2 in. Hg. Particulate Catch Data: N0.s of filters used: Recovery solvent (5) ch\r8 acetone I #, other(s) N ,-/c No. of probe wash bottles: / I Sample recovered by: - Condensate Data: I . ~~ I I I I r n I I I I Integrated Gas Sampling Data: Bag Pump No. 3,'5 Box No. Bag NO. / 1 Bag Material: %layer aluminized Tedlar Size: Pretest leal: check: D cc/min at i+ in. Hg. I 53 39 Time start: io (HHS) Time end: I1 ( HRS ) Sampling rate: 3(00 cc/min Operator: GI&-- I S/N of Oa Analyzer used to monltor train outlet: 7- I CF-i:iZ? D-4 S-0046RR I D- 5 ~ INTERPOLL LARORATORIES EVA METHOD 5/17 SAMPLE LOG SHEET 1, Job Source NIvLr 3 3-’ 62LK Method 4M7 Filter holder: -77 Filter type: Sample Train Leak Check: pretest: ( 0.02 cfm at IS in. H;. (vac) & Postest: acfm at in. Hg. (vac) +- Particulate Catch Data: No.5 of filters used: very solvent (5) 0108 cetone - other (6) ,4f /%G? 1L / No. of probe wash bottl n Sample recovered by: Q 7;CY7 - Condensate Data: ~~ - .- . . Difference Impinger -No. 3 i Condenser Desiccant Y B / Integrated Gas Sampling Data: 3 Hag pump No. 3? Bo,: No. /7 Bag No. Bag Haterial: 5-layer Aluminized Tedlar Size: 43 Pretest leal: check: 3 cc/min at /Y in. ~g. S/N of O= Analy-er used to monitor train outlet: I CF- 1:123 - D-6 S-0046RR I 0- 7 -- APPENDIX E CHROMIUM SAMPLING TRAIN FIELD DATA SHEETS INTERPOLL LFIBORATORIES EPA METHOD 2 FIELD DnTA SHEET Job /4f5 P s&5'R..o Source gA/YjT*3 S&,C Test 3 Hun 2 Date 3/27/4D r Stack dimen. 3 F? GT r.cthlnc;= reg. n.ar,~rneter- S= e::psndEd: E = electronic S-SSi t- 1 INTERPOLL LABORaTORIES €PA METHOD 5/17 SCIMPLE LOG SHEET I ~~ Source - No. of traverse points /b - Method Fi 1ter hol der: 3-5- Filter type: +dJ/eq - Sample Train Leak Check: Pretest: ( 0.02 cfm at 15 in. Hg. (vac) Postest: Oxcfm at - in. Hg. (vac) I Particulate Catch Data: N0.s of filters used: Recovery solvent (5) 0 acetone I. p-othercs) /x/ No. of probe wash bottles: / I Sample recovered by: 3ycp- Condensate Data: I Weight (g) 1: Final Dif f erencE Imp i nger No. =%=I==- I Impinger No. I Condenser - I I I Integrated Gas Sampllng Data: Hag Fump No. a/, Box No. cz- Bag No. ' I Hag Material: 5-layer Aluminized Tedlar Size: 43 Pretest leak check: 0 cc/min at J# in. Hg. I - Time start: /q30 (HRS) Time end: /Y%d (HRS) Sampl i ng rate: 40 cc/min Operatow 1 S/N of O= Analyzer used to monitor train outlet: 7- CF-02; - E-2 S -0046RR I L. P =- E-3 INTERFOLL LARORATORIES EVA METHOD 5/17 SAMPLE LOG SHEET 1, Sample Train Leak Check: I Pretest: ( 0.02 cfm at 15 in. Hg. (vac) Postest : - cfm at 2 in. Hg. (vac) % Particulate Catch Data: ~0.sof filters used: Recovery solvent (5) 0 aceton_e 7-other(s) c/tJ.rgCC No. of probe wash bottles: / I' Sample recovered - Condensate 'Data: I -1 ~~ . - [=I . _.. Ii .- I~ I- 1 '1 Integrated Gas Sampling Data: Bag Pump No. F3 BO,: NO. Bag No. 7 Bag tlaterial: 5-layer Clluminised Tedlar Size: 4- Pretest leal: check: 0 cc/min at in. Hg. li Time start: l(a (HRS) Time end: HRS 1 Sampling rate: 400 cc/min operatoa- 11 S/N of Orr Analyzer Used to monitor traln outlet: 8' CF-t:iZS - E-4 S-0046RR II E- 5 INTERPOLL LABORATORIES EPA METHOD 5/17 SAMPLE LOG SHEET I Job Al. 5.P. s AEfh Date 3/7-7/q‘’ Test - Run 4 Source NIT No. of traverse points Hethod FL!llter h?lZr: 5 5 Filter type: feffebv Sample Train Leak Check: c Pretest: .( 0.02 cfm at 15 in. Hg. (vac) /$‘ Postest: cfm at in. Hg. Particulate Catch Data: No.s of filters used: Recovery solvent (5) 0 acetone I: ;Et/other(s) - No. of probe wash bot I’ Sample recovered by: - .. - .. Condensate D-ata: I ~~ ~ .~~ .~ . ~ 1: .- I. 1. I I I Integrated GP6 Sampling Data: Bag Pump No. BOX NO. ZZ Bag NO. 3 Bag Material: %layer Plluminized Tedlar Size: 42 Pretest leal: check: 9 cc/min at in. Hg. I - Time start: /7/0 (HRS) Time end: /8ZQ (HRS) Sampling rate: duo cc /mi n Oper-mH’ I S/N of O= Analyzer used to monltor train outlet: z CF-I:~~: I - E-6 S-0046RR I APPENDIX F LABORATORY DATA SHEETS FOR METHOD 3 I Interpoll Laboratories (612) 706-6020 I Chain of Custody Sample Deposition Sheet I 3 ob A&?/ 5u Eem Source UN I T *3 Team Lead& D Vl4 Test Site STACK Date Submitted 3 - 2 7 - 4 0 Date of Test 3 . 2 7. '7 0 I Test No. 1 No. of Runs Completed 9 I I I .S. Thimble I I PA M-6 or 8 cid Gases I I I I I 1 Audit Samples pulfur Dioxide 01% per €PA M-6 OOxides of Nit. Up15 per EPA M-?A I pther OOther Source Information I 1) Type o+ Source-.&&iler 0 Asphalt Plant 1 Incinerator 1 Dryer 0 Other 2) Fuel&oal 0 Wood 0 Gas 0 Oil 0 RDF 0 Other I 3) 1s sample combust~ble~o0 Yes 4) Does sample need special handllng?+o 0 Yes If yes, explain S-278RRK'R I F- 1 Interpoll Laboratories (612) 706-601U EPA Method 5 Data Reporting Sheet Oroat CInrlvsir c\ir QA Check EPA Method I Quidelines Orsat Analyzer System Leak Check Fuel Type F0 Range Within EPA H-3 Guidelines Coal f - Anthracite/Lignite 1.016-1.130 for fuel type. Bituminous 1.083-1.2Z0 I Where F,= 20.9-Ot Oil: COI Distillate 1.260-1.41: Wesi. ___~dual 1.2 10-1.370 Gas: Natural' I .600-1. ax si Propane 1 .434-1.596 F=Flask (250 cc all glass) Butane 1.405-1.553 H=Tedlar Hag (S-layer) wood/Wood Bark 1.050-1.150 F-2 LSC-04-BR I I Interpoll Laboratories (612) 796-4020 ‘I Chain of Custody Sample Deposition Sheet I A Source Team Leader Test Site Date Submit I Test No. 1 No. of Runs Completed 3 Type of Sample Analysi E Required Comments 1 Ws::,,:: 1 n 1 per EPA M-5 I 04s per €PA M-5 S. Thimble s per €PA M-17 I &her I Impinger Catch: plN Protocol OD.’. Water PI Protocol I 03” H=OI OEPA M-6 or 8 04M5 Hg Only pcid Gases RM5 Metal5 Formaldehyde I 01.0 N NaOH IjMetals pther ~C.’:her I Integrated per €PA M-3 Gas sample %@A per EPA M-10 Wther I psper €PA M-74 Time (HHS) I OAttached fuel Form #S-0163RRR OX-Hay Sediqraph I OBahco Method I Dother psper EPA M-5 s of Nit. oc\s per EPA M-7A I OOther u Source Xnf or mat ion I 1) Type of Source: Boiler 0 Asphalt Plant 0 Incinerator 0 Dryer 0 Wood 0 Gas 0 Oil 0 RDF 0 Other I 0 No 0 Yes 4) Does sample need special handling? 0 No 0 Yes Ifyes, explain S-278HHRR I F-3 - Interpol 1 Laboratorleo (612) 786-6070 €PA Method 3 Data Reporting Sheet I Orsat Analysis Job dsg /ShcPy 'CC TestSource Site 3' kS Team Leader ET ubl,s *3 I- DatR Submitted 3-17-ic Date of Test J -11 - ic No. of Runs Frpleted 3 Technician I I--m2 I dfimbient Rip QA Check EPA Method 5 Quidelines mrsat Analyzer System Leak Check Fuel Type F0 Range -dF- Within EPA PI-3 Guidelines Coal : for fuel type. finthracite/Lignite 1. 016-1.130 Bituminous 1. 08z-1.2;0 I Where Em= 20.9-0 Oil: Di st i 11ate 1.260-1.412 e Res1dual 1.210-1.370 Qas: Natural 1.600-1 - 855 Propane 1.434-1 - 585 F=Flask (250 cc all glass) Butane 1.405-1.55; B=Tedl ar' Hag (5-layer) Wood/WoOd Bark 1.000-1.11.0 I F-4 LSC-04-BR I Interpol1 Laboratories (612) ?SA-6020 'I Chain or Custody Simp1 e Deposi tion Sheet I Job k.S,?. 5Ha2LCO Source LZ-,~ 3 Team Leader Test Site 5-i-a d.. Date Submitted 31 27/43 Date of Test 31Z1140 I Test No. t I No. of Runs Completed 3 I Type of Sample I I AS per EPA M-5 I psper EPA M-17 I I I I I I I I I Source Information 1) Type of Sourcemoiler 0 Asphalt Plant 0 Incinerator 0 Dryer 0 Other oal 0 Wood I combustible? 4) Does sample need spe S-27BRRRR I F- 5 Interpol 1 Laboratories (613) 766-6020 .€Pa Method 3 Data Reporting Sheet Orsrt Analysis No. of Run I mbient nir 04 Check €PA nethod 3 Quidolines Orcat nnalvzmr Svstem Loak Check Fuel Two F0 Range- I - --- I--. -I------.. - B F- Within EPA R-3 Guidelines Coal : for fuel type. finthracite/Lignite 1.016-1.130 Bituminous 1.003-1.250 Where F,= 20;;;01 Oil8 Distillate 1.268-1.4 1z Residual 1.210-1.;70 Gas: Natural I. b08- 1.056 Propan e 1.4Z4-1.586 F-Flask (250 cc all glass) Butane 1.405-1.555 B=Tedlar Bag (!?,-layer) Wwd/Wood Bark 1.008-1.130 I r-o LSC-04-BR - B I I 8 E 1 I 1 r APPENDIX 0 E RESULTS OF TRACE METAL ANALYSIS I I I I I II I I I INTERPOLL LABORATORIES. INC. (612)786-6020 NSP/Sherco Laboratory Log No. 9242 Results of Trace Metal Analysis Test: 1 Source: Unit No. 3 Stack Sample Type: 4M5 Train Catch Total Mass of Trace Metal in Samole (uq) Trace Metal EPA Method Field Blank Run 1 Run 2 Run 3 (Log No.) (9242-39) (9242-40) (9242-41) (9242-42) A1urni nurn SW-846. 6010 270 510 3 30 360 Arsenic SW-846. 7060 0.17 0.10 < 0.05 < 0.05 Boron SW-846. 6010 33 2420 408 1690 Barium SW-846. 6010 8.1 12.5 10.6 9.5 Beryllium SW-846. 7091 0.018 0.020 0.024 0.030 Cal ciurn SW-846. 6010 247 608 413 405 Cadmi urn SW-846. 6010 237 27 11 6.5 Chromi um SW-846. 6010 3.9 15 19 7.0 Copper SW-846. 6010 40 102 50 26 Iron SW-846. 6010 60 169 130 68 Potassium SW-846, 6010 110 295 140 137 Magnesium SW-846. 6010 25 62 40 51 Manganese SW-846. 6010 15 7.6 47 5.1 Molybdenum SW-846. 6010 26 32 28 30 Sodi urn SW-846. 6010 540 1030 720 7 40 Nickel SW-846. 6010 29 11 10 4.2 Lead SW-846. 6010 5.2 19.5 8.8 5.9 Seleni um SW-846. 7740 < 2.5 < .2.5 < 2.5 < 2.5 Antimony SW-846. 7041 0.21 1.1 0.41 0.17 Strontium 3500-sr. <5 6.5 <5 <5 Vanadium SW-846. 6010 < 0.1 < 0.1 < 0.1 < 0.1 Zinc SW-846. 6010 180 117 41 30 Mercury SW-846. 7470 < 0.1 0.96 < 0.4 < 0.2 Si 1ver SW-846. 6010 < 0.3 < 0.3 < 0.3 < 0.3 'Standard Methods, 17th Edition. G- 1 I INTERPOLL LABORATORIES. INC. (612)786-6020 Ii -. NSP/Sherco Laboratory Log No. 9242 li Results of Trace Metal Analysis Test: 1 Source: Unit No. 3 Stack Sample Type: Permanganate Impinger Catch Total Mass of Trace Metal in Sample (ua) Trace Metal EPA Method Field Blank Run 1 Run 2 Run 3 (Log NO.) (9242-23) (9242-27) (9242-31) (9242-35) 87 Mercury SW-846. 1470 0.80 5.0 2.9 4.9 1 I I I I t 1' G- 2 L INTERPOLL LABORATORIES, INC. (612)786-6020 NSP/SherCO Laboratory Log No. 9242 Results of Trace Metal Analysis Test: 1 Source: Unit No. 3 SDA Inlet Sample Type: Inlet Train Catch Total Mass of Trace Metal in Sample lua) Trace Metal EPA Method Run 1 Run 2 Run 3 (Log No.) (9242-06) (9242-10) (9242-14) A1uml num SW-846, 6010 164000 299000 219000 Arsenic SW-846, 6010 82 77 98 Boron SW-846, 6010 9940 9640 12820 Barium SW-846. 6010 12150 18440 12100 Beryl1 ium SW-846, 6010 27 29 31 Calcium Sd-846. 601.:) 392000 707000 465000 Cadmium SW-846, 6010 10 10 9 Chromium SW-846. 6010 313 328 310 Copper SW-846. 6010 695 650 880 Iron SW-846. 6010 162000 128000 185000 Potassium SW-846. 6010 60900 56600 68300 Magnesi um SW-846. 6010 23600 35100 35600 Manganese SW-846. 6010 6420 6080 7360 Molybdenum SW-846. 6010 109 88 135 Sodi um SW-846. 6010 1oooM) 13oooO 139000 Nickel SW-846. 6010 242 204 279 . Lead SW-846. 6010 758 580 770 Selenium SW-846. 6010 56 40 71 Antimony SW-846. 6010 99 68 110 Stront ium SW-846. 6010 23400 13700 28900 Vanadium SW-846. 6010 830 7 50 980 Zinc SW-846. 6010 320 3 10 320 Mercury SW-846, 7470 0.29 0.32 0.25 Silver SW-846. 6010 c 3.0 c 3.0 3.0 6-3 INTERPOLL LABORATORIES. INC. (612)786-6020 NSP/Sherco Laboratory Log No. 9242 Results of Trace Metal Analysis n 'c .i lest: 1 Source: Unit No. 3 SDA Inlet Sample Type: Permanganate Implnger Catch . Total Mass of Trace Metal In Sample (ua) Trace Metal EPA Method Field Blank Run 1 Run 2 Run 3 - (Log No.) (9242-50) (9242-51) (9242-52) (9242-53) m Mercury SW-846. 7410 0.22 9.8 9.3 6.6 I,/ I\ a c 1 1 1, B (4 I NSP Sherco Unit 3 March 90 All ICP Met hod Hi stori ca 1 Measured Used Run 1 Run 3 Run 3 ICP 375 A1 270 270 510 33c 360 GF.'AA (5 As 0.17 .05 X <.05 c.05 ICP 9 B 33 9 2420 408 1690 ICP 12 Ba 8.1 8.1 12.5 10.6 9.5 GF/AA <.1 Be .018 .018 .020 .024 .030 ICP 181 Ca 247 181 608? 41 3 405 ICP c.4 Cd 237 c.4 X ll? 6.5 ICP c.7 Cr 3.9 <.7 15 9 7 ICP 3.2 cu 40 3.2 102 50 26 ICP 38 Fe 60 38 169 130 68 ICP 64 K 110 64 295 140 137 ICP 25 Mq 25 25 62 40 51 ICP <.5 Mn 15 <.5 7.6 47 5.1 ICP 33 MO 26 33 32 28 30 ICP 158 Na 540 158 1030? 720 740 ICP <1 Ni 29 (1 1 .I? 10 4.2 ICP t4 Pb 5.2 <4 19.: 8.8 5.9 GF/AA (5 Se (2.5 t2.5 (2.5 (2.5 t2.5 GF/AA c.5 Sb .21 .21 1.1 0.41 0.17 GF/AA c5 Sr t5 (5 6.5 (5 t5 ICP <.1 V <.l <.1 <.1 C.1 <.l ICP 9.1 Zn 180 9.1 X 41 30 Cold Vapor c.4 Hg <.1 c.4 .96 <.4 <.2 ICP c.6 A9 c.3 t.3 <.3 c.3 <.3 Cold VaDor Hq .80 .8 5.0 2.9 4.9 Total Train Hg c.9 .8 5.96 2.9 4.9 x = Invalidated due to field contamination (3) ? = Result may be high due to field contamination (3) *Prepared by P. Lonnes May 1990 Total analyses = 72 G-5 APPENDIX H RESULTS OF LIME ANALYSIS INTERPOLL LABORATORIES. INC. (612)786-6020 NSP/Sherco Laboratory Log No. 9242 Results of Trace ktals Analysis Source: Unlt No. 3 Sample Type: Llme Concentratlon of Trace Metal Metal EPA Method In SarnDle (ua/a) (Log No.) (9242-73) Arsenlc SW-846, 6010 < 5.0 Beryl 1I um SW-846. 6010 < 0.1 Cadrnl urn SW-846. 6010 c 0.2 Chrornl um SW-846. 6010 15.3 Nickel SW-846. 6010 3.2 Lead SW-846. 6010 c 2.5 Selenium SW-846, 6010 < 5.0 Mercury SW-846. 7470 0.01 H-1 APPENDIX I RESULTS OF TRACE METALS ANALYSES ON COAL SAMPLE INTERPOLL LABORATORIES. INC. (612)786-6020 NSP/Sherco Laboratory Log No. 9242 Results of Trace Metal s Anal ysi s Source: Unit 3 Sample Type: Coal Concentratlon of Trace Metal Metal Methoda in Samle (ua/a) (Log No.) (9242-74) Arsenic SW-846. 7060 0.70 Beryllium SW-846. 7091 0.32 Cadml um SW-846. 7131 0.06 Chroml um SW-846. 6010 4.4 Nickel SW-846. 6010 2.3 Lead SW-846. 6010 9.1 Sel enium SW-846. 7740 < 1.6 Mercury ASTM D3684 0.02 'Sgmple prepped by ASTM Method D3683. APPENDIX J PROCEDURES Trace Hetals (4W51 Procedures J-1 TIETHODOLOGY FOR THE DETERMINATION OF WETALS EMISSIONS IN EXHAUST GASES FROM STATIONARY SOURCE COMBUSTION PROCESSES 1. Applicability and Principle 1.1 Applicability. This method is applicable for the determination of total chromium (Cr). cadmium (Cd). arsenic (As). nickel (Ni). manganese (Mn). beryllium (Be), copper (Cu). zinc (k).lead (Pb). selenium (Se). phosphorus (P), thallium (Tl). silver (Ag). antimony (Sb). barium (Ba). and mercury (Hg) 1. -1 emissions from municipal waste incinerators, sewage sludge incinerators, and hazardous waste incinerators. This method may also be used for the 1 determinaeion of particulate emissions following the additional procedures described. Modifications to the sample recovery and analysis procedures I described~- in this protocol .for the purpose of determining particulate emissions may potentially impact the front half mercury determination.. 1.2 Principle. Particulate and gaseous metal emissions are withdrawn 1- isokinetically from the source and collected on a heated filter, and in a series of chilled impingers containing a solution of dilute nitric acid in i hydrogen peroxide in two impingers. and acidic potassium permanganate solution in two (or one) impingers. Sampling train components are recovered and I digested in separate front and back half fractions. Materials collected in the sampling train are digested with acid solutions to dissolve inorganics and to 1 remove organic constituents that may create analytical interferences. Acid digestion is performed using conventional Par$ Bomb or microwave digestion techniques. The nitric acid and hydrogen peroxide impinger solution. the I acidic potassium permanganate impinger solution, and the probe rinse and digested filter solutions are analyzed for mercury by cold vapor atomic I absorption spectroscopy (CVAAS). Except for the permanganate solution, the I 'Field tests to date have shown that of the total amount of mercury measured by the method, ply 0 to <2Z was measured in the front half. Therefore, it is tentatively concluded, based on the above data, that particulate emissions may I be measured by this train. without significantly altering the mercury results. remainder of the sampling train catches are analyzed for Cr. Cd. Ni. Wn. Be. Cu, Zn. Pb. Se. P. T1. Ag. Sb. Ba. and As by inductively coupled argon plasma emission spectroscopy (ICAP) or atomic absorption spectroscopy (AAS). Graphite furnace atomic absorption spectroscopy (GFAAS) is used for analysis of antimony. arsenic. cadmium. lead. selenium. and thallium. if these elements require greater analytical sensitivity than can be obtained by ICAP. Additionally, if desired. the tester may use AAS for analyses of all metals if the detection limits meet the goal of the testing program. For convenience, aliquots of each digested sample fraction can be combined proportionally for a single analytical determination. The efficiency of the analytical procedure is quantified by the analysis of spiked quality control samples containing each of the target metals including actual sample matrix effects checks. 2. Range, Sensitivity, Precision. and Interferences 2.1 Range. For the analyses described in this methodology and for similar analyses. the ICAP response is linear over several orders of magnitude. Sam- ples containing metal concentrations in the nanograms per milliliter (ng/ml) to micrograms per milliliter (ug/ml) range in the analytical finish solution can be analyzed using this technique. Samples containing greater than approximately 50 ug/ml of chromium, lead, or arsenic should be diluted before analysis. Samples containing greater than approximately 20 ug/ml of cadmium should be diluted before analysis. 2.2 Analytical Sensitivity. ICAP detection limits in the analytical solution (based on SW-846. Method 6010) are approximately as follows: Sb (32 ng/ml). As (53 ng/ml). Ba (2 ng/d). Be (0.3 ng/d). Cd (4 ng/ml). Cr (7 ng/ml). Cu (6 ng/ml). Pb (42 ng/ml). Mn (2 ng/d). Ni (15 ng/ml). P (75 ng/ml). Se (75 ng/ml). Ag (7 ng/ml). Ti (40 ng/d). and Zn (2 ng/ml). The actual method detection limits are sample dependent and may vary as the sample matrix may affect the limits. The detection limits for analysis by direct aspiration AAS (based on SW-846. Method 7000) are approximately as follows: Sb (200 ng/ml), As (2 ng/ml). Ba (100 ng/ml). Be (5 ndml). Cd (5 ng/ml), Cr (50 ng/ml). Cu (20 ng/ml). Pb (100 ng/ml). Mn (10 ng/ml). Ni (40 ng/ml). Se (2 ng/ml). Ag (10 ng/ml). Tl (100 ng/ml). and Zn (5 ng/ml). The detection limit for mercury by CVAAS is approximately 0.2 ng/ml. The use of GFAAS can give added sensitivity compared to the use Of direct aspiration AAS for the following metals: Sb (3 ng/ml). As (1 ng/ml). Be (0.2 ng/d). Cd (0.1 ng/ml). qb&m*nt 5 Is.benmtnary mi: 2 " not b~ryreteased b, sp* *M *odd not nt this .tags conn'JcI, 'epr-t Mq POIIC~. tt IS twr; drcu(.~tor =vent on ~tsmztm:m 5-3 ~u~wY-UQ Imoliatic>r Cr (1 ng/ml). Pb (1 ng/ml). Se (2 ng/=l), and T1 (1 ng/=l). To ensure the possibility of optimum ease in obtaining accurate me8surements. the concentration of target metals in samples should be at least ten times the detection limit. Under certain conditions. and with greater care in the analytical procedure. this concentration can be as low as approximately three It times the detection limit. However. the scatter of such data may render them unacceptable or may require many analyses before the desired reliability of tj analytical data is obtained. Using the procedures described in this method, the theoretical analytical 11 detection limits shown above, a volume of 300 ml for the front half and 150 ml for the back half samples. and a Stack gas Sample volume of 1.25 m3. the 11 corresponding in-stack detection limits are presented in Table A-1 and X5b dDculmn( b b .&l88dNfgdn(L calculated as shown: has not been formally released bl EPA -*XBSD and should nm et rhb be Construe3 II C P rcpre?.rrt Aqeno) pollcy. It 8% Fewg qr...,i>~.- t(ir ,-omme-( pr :.- .. -4- .--. .I. ., I..... where: A = analytical detection limit, ug/ml. tl ~ B = volume of sample prior to aliquot for analysis. ml. C = stack sample volume. dscm. m3. D = in-stack detection limit. up@. c I1 Values in Table A-1 are calculated for the front and back half and/or the total train. it Actual method in-stack detection limits are based on actual test values. If required, this method's in-stack detection limits listed can be improved for II a specific test by using one or more of the following options: o A normal 1-hour sampling nul collects a stack gas sampling volume of 41 about 1.25 m3. If the sampling time is increased and 5 m3 is collected, the in-stack method detection limits would be one fourth of I I the values shown above (this means that with this change. the method is four times more sensitive than normal). o The in-stack detection limits assume that all of the sample is digested II (with exception of the aliquot for mercury) and the final liquid volume for analysis is 300 ml for the front half and 150 ml for the back half 41 sample. .If the front half volume is reduced from 300 ml to 30 ml, the front half in-stack detection limits would be one tenth of the values #I shown above (ten times more sensitive). If the back half volume is reduced from 150 m1 to 25 ml the in-stack detection limits would be one 11 sixth of the above values. Matrix ecfects checks are necessary on mb &cbnTrbnl L L'.-mlIrnfnrv em% 3 hsnd been released €PI is and should nor at Stage be mmruc: -n represent Agcnq pollcy. tt is tc:T 3rculatcd for conynsnt on Its tecp.iICy" 5-4 --am- ma y-llcy lrnollutions 1 - TABLE A-1. IN-STACK METHOD DETECXION LWTS (ug/m3) FOR TRAIN FRACTIONS USING ICAP AND AFS Front Half Back ndf1 Back Half2 Fraction 1 Fraction 2 Fraction 3 Total Train Metal Probe and Filter Impingers 1-3 Impingen 4-5 Antimony 7.7 (0.7)' 3.8 (0.4)' 11.5 (1.1)' Arsenic 12.7 (0.3)' 6.4 (0.1)' 19.1 (0.4)' Barium 0.5 0-3 0.8 Beryllium 0.07 (0.05)' 0.04 (0.03)' 0.11 (0.08). Cadmium 1.0 (0.02)' 0.5 (0.03). 1.5 (0.3). Chromium 1.7 (0.2)' 0.8 (0.1)' 2.5 (0.3)' Copper 1.4 0.7 2.1 Lead 10.1 (0.2)' 5.0 (0.1)' 15.1 (0.3). Manganese 0.5 (0.2)' 0.2 (0.1). 0.7 (0.3)' Mercury 0.05** 0.03" 0.03" 0.11- Nickel 3.6 1.8 5.4 Phosphorus 18 3 27 Selenium 18 (0.5)' 9 (0.3)' 27 (0.8)' Silver 1.7 0.9 2.6 Thallium 9.6 (0.2)' 4.8 (0.1)' 14.4 (0.3)' Zinc 0.5 0.3 0.8 ( )* Detection limit when analyzed by GFAAS. ** Detection limit when analyzed by CVAAS. Actual method in-stack detection limits are based on actual test values. analyses of samples and typically are cf greater significance for samples that have been concentrated below the normal sample volume. A volume less than 25 ml may not allow resolubilization of the residue and may increase interference by other compounds. o When both of the above two improvements are used on one sample at the same time. the resultant improvements are multiplicative. For example. where stack gas volume is increased by a factor of five and the total liquid sample digested volume of both the front and back halves is reduced by factor of six, the in-stack method detection limit is reduced by a factor of thirty (the method is thirty times more sensitive). o Conversely. reducing stack gas sample volume and increasing sample liquid volume will increase limits. The front half and back half1 samples '(Fractions 1 and 2) can be combined prior to analysis. The resultant liquid volume (excluding Fraction 3 which must be analyzed separately) is recorded. Combining the sample as described does not allow determination (whether front or back halfl) of where in the train 4 5-5 the sample WBS captured. The in-stack method detection limit then becomes a single value for all metals. except mercury for which the contribution of Fraction 3 must be considered. o The above discussion assumes no blank correction. Blank corrections are discussed later in this method. 2.3 Precision. The precisions (relative standard deviation) for each metal detected in a method development test at a sewage sludge incinerator, are as follows: Sb (13.9%). As (13.5%). Ba (13.1%). Cd (11.5%). Cr (12.5%). Cu (11.9%). Pb (11.6%). Ni (7.7%). p (13.52). Se (15.3%). T1 (12.3%). and Zn (11.8%). Beryllium. manganese and silver were not detected in the tests: however, based on the analytical sensitivity of the ICAP for these metals, it is assumed that their precisions should be similiar to those- for the other metals. 2.4 Interferences. Iron can be a spectral interference during the analysis of arsenic. chromium. and cadmium by ICAP. Aluminum can be a spectral interference during the analysis of arsenic and lead by ICAP. Generally. these interferences can be reduced by diluting the sample. but this increases the method detection limit. Refer to EPA Method 6010 (SW-846) for details on potential interferences for this method. For all WAAS analyses. matrix modifiers should be used to limit interferences. and standards should be matrix matched. I 3. Apparatus 3.1. Sampling Train. A schematic of the sampling train is shown in Figure 1 A-1. It is similar to the Method 5 train. The sampling train consists of the following components. I- 3.1.1 Probe Nozzle (Probe Tip) and Borosilicate or Quartz Glass Probe Liner. Same as Method 5. Sections 2.1.1 and 2.1.2. Glass nozzles are required unless an alternate probe tip prevents the possibility of contamination or I interference of the sample with its materials of construction. If a probe tip other than glass is used, no correction of the stack sample test results can be 1 made because of the effect on the results by the probe tip. 3.1.2 Pitot'Tube and Differential Pressure Gauge. Same as Method 2. I Sections 2.1 and 2.2, respectively. 3.1.3 Filter Holder. Glass. same as Method 5. Section 2.1.5. except that I a Teflon filter support may be used. if desired, to replace the glass frit. 5 nb *.merit b F.bnmtMW e. 11 * ken hllyNhEEd Epb should not at thb rtage M tD,,,tUtNtO p revem1 bnqpoky. tt IC Mlng urcdJted for comynent on tts 1e:hnlSY I 5-6 =uT.CY *M Y-licy lmpllsltlonr 5-7 ~~ ~ ~~ ~~ Interpoll Laboratorles. Inc. (612)786-6020 11 Determinat 1 on of Hexavalent Chmaiua i in sarpllng Train Sawles I 1 Interpol1 Method I: 6010-mS EPA Reference Method I: SW-846. 6010 I I Version 1.0 I June 20. 1990 I i J-8 I 1 APPLICATION Thls method is appllcable to the detennlnatlon of hexavalent chromium In stationary source samples collected by a sampllng traln. Method No. 6010-WS Revlsion No. 0 Date June 20. 1990 1-1 3-9 ~ ~~~ - 2 RANGE I1 The range of thls method extends from a detection limlt of 0.05 ug to 50 ug. The upper range can be greatly extended through dllutlons. I1 YI II Method No. 6010-MM5 Revlslon No. 0 Date June 20. 1990 2-1 J-10 3 WPLE HAHILING AND PRESERVATION 3.1 Samples should be analyzed as soon as possible. 3.2 To retard the chemical activity of hexavalent chromium. the samples should be transported and stored until the time of analysis at 4%. Method NO. 601O-MMS Revision No. 0 Date June 20. 1990 3-1 J-11 1 4 su+uRYOFWETHoD The probe wash and filter of the sampling traln are combined, digested. and flltered. The filtrate is combined with the impinger catch. the pH of this solution is adjusted to 2.4. and chelated using APDC. Adjust the solution pH agaln to 2.8 and @xtractwith MIBK. This isolates the Cr(V1) fmm the other Cr species. The MIBK Is evaporated and the residue taken up In nitric acid. The solution Is then analyzed by ICP or GF/M. Method No. 6010-MM5 Revision No. 0 Date June 20. 1990 4-1 J- 12 5 INTERFERENCES Cr(V1) reacts with most organtc compounds and surfaces. Wethod NO. 6OlO-Hn5 Revlslon No. 0 Date June 20. 1990 5-1 5-13 6 APPARATUS AND GLASSWARE 6.1 For GF/AA analysis: 6.1.1 Chromium hollow cathode lamp. ' 6.1.2 Wavelength: 357.9 nm. 6.1.3 Furnace Program: Drying time 30 sec. Drying temp. 125'C . Ashing time 30 sec. Ashi ng temp. lOoo0C Atom1 zing t 1me 10 sec. Atomizing temp. 2700'C 6.2 For ICP analysis: 6.2.1 Them Jarrell Ash ICAP 61 Plasma Spectrometer. 6.2.2 Optical system: 0.75 meter Paschen-Runge mount with a 25 micron entrance sllt and 50 micron exit slits. 6.2.3 Detectors: Hamamatsu Side Window 1/2 inch (1.3 cm) diameter; R300. R427. R306. RB89. 6.2.4 Computer: IW R/AT 640K RAM. 30 WByte Winchester hard drive. 1.44 MByte floppy drive, enhanced color display. 6.3 Hot plate. Method No. 6010-HM5 Revision No. 0 Date June 20. 1990 6- 1 5-14 6.4 Volumetric flasks: 100 mL. 250 mL. and lo00 mL. for preparation of standards and sample dilution. 6.5 Graduated cylinders: For preparation of reagents. 6.6 Mlcrowave digester: CEH HDS-81D. Teflon PFA vessels (120 mL size) with pressure relief valve, digestion turntable. capping station. 6.7 Beakers and watch glasses: 250 mL beakers for sample digestion with watchglasses to cover the tops. 6.8 RIng stands and clamps: For securing equlpment. 6.9 Filter funnels. 6.10 Glass fiber filters. 6.11 Dlsposable Pasteur pipets and bulbs. 6.12 Volumetric pipets. 6.13 Separatory funnels. Method No. 6010-MM5 Revision No. 0 Date June 20. 1990 6-2 J-15 7 REACENE4 7.1 Amnonlum pyrrolidlne dlthlocarbamate (APDC) solutlon. Dissolve 1.0 gram APDC In demlnerallzed water and dilute to 100mL. Prepare fresh dally. 7.2 Potassiumdichromate stock solutlon: Dissolve 141.4 mg of drled potasslum dichromate. K1Crl4 (analytical reagent grade), in Type I1 water and dilute to 1 liter (1 mL = 50 ug Cr). 7.3 Potasslum dlchromate standard solution: Dilute 10.00 mL potasslum dichromate stock solutlon to 100 mL (1 mL = 5 ug Cr). 7.4 Sulfuric acid. 10 t (v/v): Dilute 10 mL of dlstilled reagent grade sulfurlc acid, HISO,. to 100 mL with Type I water. 7.5 Hethyl Isobutyl ketone (MIBK) 7.6 Sulfuric acid. 0.1211: Slowly add 6.5 mL concentrated H2S0, to demineralized water and dllute to 1 llter. 7.7 NItrlc acld. concentrated 7.8 Sodlum Hydmxlde solutlon. 1 M: Dlssolve 40 grams NaOH In demlnerallzed water and dilute to 1 liter. 7.9 Digestion Solution: MIX 20 grams NaOH and 30 grams NalCOI and dilute to 1 llter wlth demlnerallzed water. Method No. 6010-MM5 Revlslon No. 0 Date June 20. 1990 7-1 5-16 Normal. accepted laboratory safety practices should be followed. No known carclnogenlc materials are used In thls method. Method No. 6010-MH5 Revlsion No. 0 Date June 20. 1990 8- 1 5-17 9 PROCEDURE II 9.1 Combine the probe rlnse and the fllter from the sample traln In a beaker. 1.1 9.2 Add 40 mL of the dlgestlon solution. I-I 9.3 Heat beaker on hot plate for 30 minutes. The solutlon should not be taken to dryness. 11 9.4 After cooling. the mixture is flltered uslng a distilled-water II preeuashed glass flber fllter using vacuum filtratlon. 1-1 9.5 Comblne the flltrate (which contalns the CrVI) with the implnger catch and adjust the pH to 2.4 using HtSO,. 9.6 Add 5 mL of APE per 100 mL of solutlon. 17 9.7 Transfer to scparatcry funnel and extract ulth 10 mL of MIBK per 100 mL of solution. Shake vlgonxrsly for 5 minutes. Allow layers to II separate (10 - 15 mlnutes). Remove MIBK layer into a flask. Repeat the above two more times and put MIBK into the same flask. II 9.8 Evaporate the HIBK on a hot plate almst to dryness. I' 9.9 Add 25 mL of 5% "01and heat for 45 mlnutes. 9.10 Transfer to a 25 mL volumetrlc flask and bring to volume wlth 52 HNOl. Method NO. 6010-W5 li Revision No. 0 Date June 20. 1990 I' 9- 1 J- 18 1 9.11 Analyze by ICP. (If samples are below the ICP detection limlt. 1 reanalyze by GF/AA with Zeeman background correction if required). 9.12 Sample Analysis: The prepared sample is analyzed by ICP for b Hexavalent Chromium. The wavelength is 267.716 nm. I 9.12.1 Instrument Set-up: The instrument is set-up and profiled as described in the ICP Standard Operating Procedure I (Interpol1 Method Number ICP-ILL). I 9.12.2 Instrumental Callbration: Following set-up, the instrument Is calibrated using a blank and a solution containing 100 I mg/L of chromium. 1 I I I I I 1 1 1 Method No. 6010-MM5 Revision No. 0 I Date June 20. 1990 I 9-2 I J-19 10 CALCULATION To calculate results in total ug. use the followlng equation: ug/mL Cr x (Dilution Factor) x Volume of Sample (mL) = total ug where: ug/mL Cr = read off ICP prlntout %. volume of Sample = flnal volume of sample after preparatlon (Liters) Dllutlon Factor = any dilutions required to bring the 11 concentratlon of Cr within the calibration range or to remove Interferences I I I Method No. 601O-C(n5 I Revislon No. Date June 20. 1990"I 10-1 3-20 11 QUALIlY COHTROL PROCEDURES 11.1 To verlfy the absence of matrlx interferences. at least one matrlx splke nust be performed. If not enough sample was submltted. an Instrument splke must be run. Percent recovery nust meet control llmlts for the method. 11.2 One splke nust be performed In order to determine extractlon eff lclency . 11.3 One dupllcate must be run per batch. The Percent Relatlve Difference nust meet the control llmlts for the method. If there isn't enough sample, an Instrument dupllcate wlll be run. 11.4 A method blank nust be run to verify that the method is performing to speclflcations. \ 11.5 Any sample above the llnear range of the instrument mst be dlluted and reanalyzed. 11.6 Two callbratlon blanks are analyzed wlth each analytlcal batch. One Is analyzed at the beglnnlng of the run and the other at the end. 11.7 Tw Instrument check standards should be analyzed during an analytlcal run. One at the beglnnlng and another at the end. These standards verlfy the accuracy of the Instrument calibration. Method No. 6010-MHS Revlsion No. 0 Date June 20. 1990 11-1 5-21 12 ACCURACY AND PRECISIOH 12.1 The accuracy llmits for thls method ape from 80 to 120 percent recovery. 12.2 The precision limit for this method Is 10 relative percent difference. 12.3 Check standards nust be within 2 10t of thelr true value or the data associated with them Is considered Invalid. ~ .. Method No. 6010-HM5 Revlsion No. 0 Date June 20. 19% 12-1 13 REFEREKXS 13.1 EPA Method 6010; Test Methods for Evaluating Solid Waste (SW- 846); U.S. EPA Office of Solid Waste and Emergency Response; Novenher 1986. 13.2 EPA Method 7191; Test Methods for Evaluating Solid Waste (SW- 846); U.S. EPA Office of Solid Waste and Emergency Response; November 1986. 13.3 EPA Method 7197; Test Methods for Evaluating Solid Waste (SW- 846); U.S. EPA Office. of Solid Waste and Emergency Response; Noveder 1986. 13.4 Draft Method Wethodology for the Determlnat$on of Metals Emlssions in Exhaust Gases from Stationary Sources of Combustion Processes.; received April, 1989 from Source Methods Standardization Branch. US €PA Atmospheric Research and Exposure Assessment Laboratory; Research Triangle Park, NC 27711. Method No. 6010-MHS Revision No. 0 Date June 20. 1990 13-1 5-23 APPENDIX K CALCULATION EQUATIONS I 1 CALCULATION EQUATIONS I METHOD 2 I VS I I ,d I 60 vs A 1 Qa 1 4.935 Qs,d Gd % - 3ws I I RH* I I B:S I I I I *Alternate equations for calculating moisture content from wet bulb and I dry Suld data. I K- 1 CALCULATION EQUATIONS METHOD 3 lOO(X0~- ).5% CO) %EA = 1) 264% N2 - %02 + 0.5% CO O.44(%CO2) 0.32 (%02) + 0.28 %CO ) + Bws) 0.18 - C-1 "wIstd1 'w(std) + "m(std) I 1 K-2 I I I CALCULATION EQUATIONS METHOD 5 Pbar + m/13.6 = 17.65 V, Y ( 1 I 'm( std) 'm(avg) = 0.0472 VIS I 'w( std) ,I z V Ts(avg) m(std) I = 0.0944 (p - c s "s A" bws)' c 15.43 M, 3 M Ps - 272.3 c 'a Ts( avg) ('w( stdf 'm( std)) b ($)I = 8.5714 X io'3 Cs Qs,d ! - 1.3228 x 10-1 Mp A MP12 - I O A" c iI c t K- 3 - I I, SYUBOLS I A = Cross sectional area of stack, SQ. FT. I An = Cross sectional area of nozzle, .SQ. FT. I = Water vapor in gas stream, proportion by volume Bws I CP = Pitot tube coefficient, dimensionless Ca = Concentration of particulate matter in stack gas, I wet basis, GR/ACF I -CS = Concentration of particulate matter in stack gas, dry basis, corrected to standard conditions, GR/DSCF .- I- EA = Excess air, percent by volume I Y = Dry test meter correction factor, dimensionless 1'J Gd = Specific gravity (relative to air), dimensionless I = Isokinetic variation, percent by volume I Md = Molecular weight of stack gas, dry basis, g/g - mole. I = Mass flow of wet flue gas, LB/HR I mp = Particulate mass flow, LB/HR I MS = Molecular weight of stack gas, wet basis. g/g. mole. I MP = Total amount of particulate matter collected, g I Pbar = Atmospheric pressure, IN. HG. (uncompensated) 1 pg = Stack static gas pressure, IN. WC. I K- 4 PS = Absolute pressure of stack gas, IN.HG. Pstd = Standard absolute pressure, 29.92 IN. HG. Aa Actual volumetric stack gas flow rate, ACFM Qs .d = Dry volumetric stack gas flow rate corrected to standard conditions, DSCFY RH = Relatlve humidity, X Tdb = Dry bulb temperature of stack gas. OF TW3 = Wet bulb temperature of stack gas, OF Tm(avg) = Absolute average dry gas meter temperature, 02 - TS(avg) = Absolute average stack temperature, OF Tstd = Standard absolute temperdture, 528 OF (68 OF) e = Total sampling time, min. v1 c = Total volume of liquid collected in impingers and silica gel, ml Vm Yslume of gas sample as measured by dry gas meter, CF Vm(std) = Volume of gas sample measured by the dry gas meter corrected to standard conditions, DSCF Vw(std) = volume of water vapor in the gas sample corrected to standard conditions, SCF - vs = Average actual stack gas velocity. FT/SEC VPtdb = Vapor pressure at Tdb. IN. HE. K- 5 I I VPtwb = Vapor pressure at Twb. IN. HG I m = Average pressure differential across the orifice meter. IN. WC. I AP = Velocity pressure of stack gas, IN. WC. I Y = Dry test meter correction coefficient, dimensionless I P = Actual gas density, LS/ACF I I I I I I I I I I I e I