HAZEN RESEARCH, INC. Analytical Department Superfun4Recoi er SITE: J 4601 Indiana St., Golden, CO 80403 303-279-4501 BREAK: OTHER:
QUALITY MANUAL
Radiochemistry and Uranium Laboratories
Policies and Procedures Established to meet NELAC Quality Systems Standards
Reviewed, Acknowledged, and Approved by: Signature Date
Bill Youngclaus Bench Chemist
Richard Oberto Senior Chemist
Ann Strapac Lab Technician
Eve DelaFuente Group Supervisor s* 'A*/ Robert Rostad Laboratory Manager
John C. Jarvis Laboratory Director QA Officer
Eleventh Revision, 3/8/2000 Quality Manual Page 1 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
TABLE of CONTENTS
1.0 Laboratory Description and Quality Statement
1.1 Laboratory Profile 4 1.2 Management Quality Statement 4 1.3 Laboratory Organization 5
2.0 Personnel
2.1 Job Descriptions and Responsibilities 5 2.2 Training 5 2.3 Resumes 6 2.4 Director's Certifications 6 2.5 Employee Signatures and Initials 6
3.0 Facilities
3.1 General Description 6 3.2 Hazen Campus Map 7 3.3 Analytical Department Floor Plan 7
4.0 Licenses and Laboratory Certifications 7
5.0 Methodology
5.1 Standard Operating Procedures 8 5.2 Radium-226 (ZnS scintillation counting) 8 5.3 Radium-226 (alpha spectrometry) 8 5.4 Radium-228 8 5.5 Thorium-230 9 5.6 Polonium-210. 9 5.7 Lead-210 10 5.8 Gross Alpha, Beta 10 5.9 Uranium 10 5.10 Radiocesium 11 5.11 Radiostrontium. 11 5.12 Tritium 12 5.13 Radon 12 5.14 Method Exceptions and Departures 12 5.15 Employee SOP Certification 13
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TABLE of CONTENTS Page 2
6.0 Equipment and Instrumentation 13
7.0 Reference Standards and Traceability 13
8.0 Sample Management
8.1 Sample Preservation 14 8.2 Sample Receiving, Acceptance, and Log-in 16 8.3 Sample Storage and Disposal. 16 8.4 Chain of Custody 17
9.0 Data Management
9.1 Worksheets, Calculations 17 9.2 Data Validation 17 9.3 Reporting 17 9.4 Storage and Disposal of Records 18 9.5 Security and Confidentiality 18
10.0 Quality Management
10.1 Instrument Checks 18 10.2 Batch Quality control 19 Control Standards 19 Duplicate Samples 19 Spikes 19 Blanks 20 10.3 Acceptance Criteria 20 10.4 Corrective Action s 20 10.5 Proficiency Testing ____ _ 21 10.6 Internal Audits 21 10.7 Customer Complaint s 21
11.0 Appendices
Appendix A Organizational Chart 22 Appendix B Method Proficiency Demonstration Form 24 Appendix C StafFResumes 26
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TABLE of CONTENTS Page 3
Appendix D Hazen Campus, Analytical Lab Floor Plan ..33 Appendix E Detection Limits and Sample Volumes 36 Appendix F Sample Acceptance and Log-in Flowchart. 38 Appendix G Chain of Custody and Sample Receipt Forms .41 Appendix H Worksheets, Reports 44 Appendix I Security and Confidentiality .47 Appendix J Instrument Control Charts 51 Appendix K Performance Test Procedure, Gas Flow Counter 54 Appendix L Performance Test Procedure, Alpha Spectrometer.... .57 Appendix M Performance Test Procedure, Liquid Scintillation 60 Appendix N Performance Test Procedure, Gamma Spectrometer. 67 Appendix O Performance Test Procedure, Scintillation Counter.. 69 Appendix P Control Standard Chart .72 Appendix Q Duplicate Analysis Chart .74 Appendix R Spiked Sample Tabulation. .78 Appendix S Blank Sample Tabulation .80 Appendix T Internal Audit Checklist 82 Quality Manual Page 4 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
1.0 Laboratory Description and Quality Statement
1.1 Laboratory Profile
Hazen Research Inc. has operated a commercial analytical laboratory for more than thirty years, in support of the chemical, mining, and mineral processing industries. A part of Hazen's laboratory has been devoted to radiochemical assay of environmental and process samples, as a means of monitoring radioactive contaminants resulting from mining and mineral processing operations. This capability has been extended to include a general testing and analysis service available to municipalities, governmental agencies, and private individuals.
1.2 Management Quality Statement
The following is excerpted from the Hazen Corporate Statement of Principles and Values:
Our objectives are:
To achieve and maintain leadership in the business area we serve. To maintain an environment in which employees can find well- paying, stimulating and meaningful work and in which they feel they have an influence over their conditions and future prospects.
The following principles will govern our conduct in achieving these objectives:
We will maintain the finest staff possible in all job categories. This will be accomplished by a combination of recruiting, training, and specific employee development programs to help employees grow in knowledge and ability.
We are dedicated to the concept that quality implies meeting or exceeding the clients' expectations. This concept incorporates the principle of excellence with technical expertise. Implicit in this policy is the need for timeliness, cost control, and excellent client relations.
The highest ethical standards will be maintained in service to clients, relations with the community, compliance with the law, and dealings with each other.
We will constantly seek ways to increase our productivity. This means finding ways to increase the quantity and quality of Quality Manual Page 5 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
knowledge produced per client dollar. We will constantly examine our methods in order to be more effective in every aspect of the business.
1.3 Laboratory Organization
The Analytical Department Organizational Chart is found in Appendix A.
2.0 Personnel
2.1 Job Descriptions and Responsibilities
The following job classifications describe the organization of the radiochemistry laboratory and the responsibilities and minimum requirements of the various levels of activity:
The Laboratory Analyst has a minimum of a B.S. degree in chemistry, or related field, and is responsible for performing analyses according to the procedures outlined in this manual.
The Radiochemistry Group Supervisor has a minimum of a B.S. degree in chemistry, or related field, and is responsible for training analysts, scheduling work, supervising the application of the quality control measures outlined in this manual, and for reviewing all data produced in the radiochemistry section.
The Laboratory Manager has a minimum of a B.S. degree in chemistry, or related field, and is responsible for coordination of activities among the various lab groups, client contact and service, and enforcement of the quality control measures specified in this manual.
The Laboratory Director has a minimum of an M.S. degree in chemistry, or related field, and has responsibility of insuring that the laboratory staff is aware of, and acting upon, new regulatory requirements in the field of radiochemistry. The laboratory director will conduct periodic inspections of the quality control procedures being used in the radiochemistry laboratory to insure that they comply with the requirements outlined in this manual. The laboratory director will act as the quality assurance officer for the radiochemistry group.
2.2 Training
Training in analytical techniques is generally performed at the Group Supervisor level, or by the individual who is most familiar with the techniques involved. Seminars and formal courses conducted by Quality Manual Page 6 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
equipment manufacturers and vendors are also used for employee training. The company safety officer conducts yearly OSHA approved training courses on workplace safety. Specialized radiation safety training is given to employees who are working with radioactive materials.
Analysts are required to demonstrate proficiency in a method before they are considered trained. This proficiency is documented using the Demonstration of Capability form, a copy of which is found in Appendix B.
Employees are required to read the essay entitled Ethics in Science, by Henry H. Bauer. Improper, unethical, or illegal actions on the part of an employee can result in immediate termination of employment. By signing the cover page of this document, the empoyee acknowledges that he or she has read the Bauer essay, and has understood the statement of punishment and penalty stated here.
2.3 Resumes of individuals currently performing radiochemistry lab functions are found in Appendix C.
2.4 The Laboratory Director's Certification of Personnel Qualifications can be found in the QC documentation files located in the radiochemistry office.
2.5 The log o employef e names and initials can be found in the QC documentation files located in the radiochemistry office.
3.0 Facilities
3.1 General Description
The Analytical Department consists of approximately 9,000 square feet of finished laboratory space. Additional space is available from adjoining Company operations, and such space can be used for overflow work or special projects.
Fume hoods are available for performing evaporations, extractions, acid digestions, and dry ashing. Included are three large stainless steel perchloric acid fume hoods.
A dedicated laboratory refrigerator is available for storage of temperature sensitive reagents.
Flammable reagents and chemicals are stored in a commercial steel cabinet designed for this purpose. Quality Manual Page 7 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Standard laboratory services include bench mounted compressed air, vacuum, natural gas, and 110/220 v electrical supply.
A deionized water system, utilizing three mixed bed ion exchange resin tanks in series, provides a high purity water of 2 micro mho per centimeter or less conductivity. This water is used to prepare reagents, standards and dilutions, and to clean glassware. The water is monitored continuously by means of an online conductivity indicator, and is checked daily with a laboratory conductivity meter. The measurements are recorded in a notebook.
The analytical laboratory uses five microcomputer workstations operating on a Novell network to standardize laboratory functions. Sample logging, container labeling, calculations, report generation, and general laboratory management functions are performed using these systems.
A complete library of reference materials is located adjacent to the main laboratory facility. Method manuals published by the EPA, APHA, AOAC, and ASTM are available. These publications are the primary source of analytical methodology used in routine laboratory operations.
3.2 Hazen Campus Map (see Appendix D)
3.3 Analytical Department Floor Plan (see Appendix D)
4.0 Licenses and Laboratory Certifications
Hazen Research Inc. operates the radiochemistry laboratory in compliance with Colorado State Rules and Regulations Pertaining to Radiation Control. Colorado is an NRC agreement state, and has issued license Colo. 77-02SF to govern our activities in this area.
The radiochemistry laboratory currently holds drinking water radiochemistry certifications in the following states:
Colorado Massachusetts Wyoming Connecticut Utah Kentucky North Dakota Kansas South Dakota Illinois Montana Indiana New York Michigan New Hampshire Ohio Wisconsin Quality Manual Page 8 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
5.0 Methodology
5.1 Standard Operating Procedures
Detailed information about the methods used for radiochemistry can be found in the laboratory's procedure manual, which contains the current Standard Operating Procedures (SOPs) for the various analytes. The following discussion provides a brief summary of the methods and the literature references upon which they are based.
5.2 Radium-226: Radium-226 is isolated by double precipitation using lead and barium sulfate. The resulting precipitate is mounted on a counting planchet and the activity of radium-226 is determined using scintillation counting.
Reference:
American Public Health Association, Standard Methods for the Examination of Water and Wastewater. 17th Ed., Method 7500 Ra B (1989).
5.3 Radium-226: The radiochemistry laboratory is also equipped to assay radium-226 using alpha spectrometry. The procedure is a modification of the American Public Health Association method for total radium assay, where radium isotopes are isolated by multiple precipitations using lead and barium sulfate. A reduced amount of barium is used so that the precipitate can be mounted on a membrane filter and analyzed by alpha spectrometry. The yield of each barium precipitate is measured by spiking the sample with a known amount of barium-133, a gamma emitter, and measuring its gamma activity in the final precipitate.
References:
American Public Health Association, Standard Methods for the Examination of Water and Wastewater. 17th Ed., Method 7500 Ra B (1989).
Lim, T.P., and Dave, N.K., A Rapid Method of Radium-226 Analysis in Water Samples Using an Alpha Spectroscopic Technique. CIM Bulletin vol. 74, no. 833, pp. 97-105 (Sept. 1981).
5.4 Radium-228: Radium-228 is isolated by coprecipitation on barium sulfate. The coprecipitate is purified by several dissolutions and reprecipitations using DTPA reagent and pH control. The resulting solution is aged for 36 hours to allow ingrowth of actinium-228. Radium-228 is removed from Quality Manual Page 9 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
solution by reprecipitation. Actinium-228 is extracted from the solution using bis (2-ethylhexyl) phosphoric acid, and back extracted into an aqueous phase. The aqueous phase is evaporated onto a counting planchet, and the actinium-228 activity determined by gas flow proportional counting.
References:
Brooks and Blanchard, USEPA/EMSL, Radiochemical Determination of Radium-228 in Water Samples. Method Ra-05 (a modification of the Percival and Martin procedure) (1981).
Percival, Donald R., and Martin, Don B., Sequential Determination of Radium-226. Radium-228. Actinium-227. and Thorium Isotopes in Environmental and Process Waste Samples. Analytical Chemistry, 46, pp. 1742-1749 (Oct. 1974).
5.5 Thorium-230: Thorium-230 is separated from other alpha emitting radionuclides by collection on Dowex AG 1-X8 ion exchange resin. The thorium-230 is eluted and the eluate evaporated to a volume of 15 ml. The thorium-230 is coprecipitated on barium sulfate, redissolved in alkaline EDTA, and carried on eerie hydroxide. The eerie hydroxide is mounted on a membrane filter and subjected to alpha spectrometry.
References:
Latimer, J.N., et al, Handbook of Analytical Procedures. RMO-3008, USAEC, Grand Junction Office/Analytical Laboratory (Feb. 1970).
Sill, Claude W., and Williams, Rodger L., Preparation of Actinides for Alpha Spectrometry Without Electrodeposition, Analytical Chemistry, 53, pp. 412-415(1981).
5.6 Polonium-210: Polonium-210 is precipitated as the sulfide using bismuth as a carrier. The precipitate is mounted on a membrane filter and its alpha activity measured using a gas flow proportional counter.
References:
Rosholt, J.N. Jr., Quantitative Radiochemical Method for Determination of Major Sources of Natural Radioactivity in Ores and Minerals. Analytical Chemistry, 26, pp. 1307-1311 (1954). Quality Manual Page 10 Radiochemistry Laboratory Revisio n11 Hazen Research Inc. 3/8/2000
United Kingdom Atomic Energy Authority, Analytical Method for the Determination of Polonium-210, Thorium-230 in Uranium Ores. Concentrates, and Plant Liquors. PG Report 356 (S).
5.7 Lead-210: Lead contained in the sample, along with lead added as a carrier, is collected on an anion exchange resin (Dowex 1-X8). The lead is eluted and precipitated as the chromate. The lead chromate is allowed to age to permit ingrowth of bismuth-210. The beta activity of the lead 210 and bismuth-210 is measured using low background gas flow proportional counting. Recovery is determined by weighing the final lead chromate precipitate and comparing it to the theoretical 100% yield. Recovery corrections are made.
Reference:
United States Geological Survey, Methods for Determination of Radioactive Substances in Water and Fluvial Sediments, Techniques of Water Resources Investigations of the United States Geological Survey, Chapter A5( 1977).
5.8 Gross Alpha, Beta: An aliquot of water is evaporated onto a stainless steel counting planchet. Alpha and beta activity is measured using low background gas flow proportional counting. Thorium-230 and strontium 90 standards are used for alpha and beta calibrations, respectively.
Reference:
USEPA Environmental Monitoring and Support Laboratory, Prescribed Procedures for Measurement of Radioactivity in Drinking Water. EPA 600/4-80-032, Method 900.0 (Aug. 1980).
5.9 Uranium: Natural uranium is determined by fluorimetry. The uranium is concentrated and separated from matrix interferences by solvent extraction (ethyl acetate). A portion of the uranium bearing organic phase is aliquoted onto a sodium fluoride pellet. The pellet is fused at 1000 deg. C for 3 minutes in a propane flame. The fluorescence of the pellet when exposed to ultraviolet radiation is measured. The intensity of the fluorescence is proportional to the uranium concentration.
References:
American Society for Testing of Materials, Test Methods for Microquantities of Uranium in Water by Fluorimetry. Annual Book of ASTM Standards, Method D 2907-91. Quality Manual Page 11 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Department of Mines and Technical Surveys, Ottawa, Canada, Manual of Analytical Methods for the Uranium Concentrating Plant. Mines Branch Monograph 866 (1959).
Fisher Scientific Company, Jarrell-Ash Division, Instruction Manual. Model 26-000 Fluorimeter (Dec. 1971).
5.10 Radiocesium: Radioactive cesium is isolated by the use of a phosphomolybdate precipitation and a chloroplatinate precipitation. Non radioactive cesium is used as a carrier. The final precipitate is counted for beta activity to measure 'total radiocesium'.
References
American Public Health Association, Standard Methods for the Examination of Water and Wastewater. 17th Ed., Method 7500-Cs B (1989).
USEPA Environmental Monitoring and Support Laboratory, Prescribed Procedures for Measurement of Radioactivity in Drinking Water. EPA 600/4-80-032, Method 901.0 (1980).
5.11 Radiostrontium: Radioactive strontium is isolated by use of sequential carbonate and nitrate precipitations. Non-radioactive strontium and barium are used as carriers. The final precipitate is counted for beta activity to measure 'total radiostrontium'.
If strontium-90 is to be determined, the precipitate is allowed to age for several weeks to permit ingrowth of yttrium-90, redissolved, and spiked with non-radioactive yttrium. The yttrium is then precipitated as oxalate and the precipitate counted for beta activity to measure, indirectly, strontium-90 via its daughter yttrium-90.
Strontium-89 is calculated as the difference between the total radiostrontium and the strontium-90. Because strontium-89 has a short half life (about 50 days), a decay calculation must be applied to correct the strontium-89 activity to the time of sample collection.
References:
American Public Health Association, Standard Methods for the Examination of Water and Wastewater. 17th Ed, Method 7500-Sr A (1989). Quality Manual Page 12 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
USEPA Environmental Monitoring and Support Laboratory, Prescribed Procedures for Measurement of Radioactivity in Drinking Water. EPA 600/4-80-032, Method 905.0 (1980).
5.12 Tritium in Water: Water samples are distilled under basic, oxidizing conditions to remove potential interferences. The distillate is collected and an aliquot taken for liquid scintillation analysis. Tritium contained in the water is determined by measurement of its weak beta emission.
References:
American Public Health Association, Standard Methods for the Examination of Water and Wastewater. 17th Ed., Method 7500-3H B (1989).
USEPA Environmental Monitoring and Support Laboratory, Prescribed Procedures for Measurement of Radioactivity in Drinking Water. EPA 600/4-80-032, Method 906.0 (1980).
5.13 Radon in Water: Water samples are collected using an apparatus designed to minimize loss of dissolved radon gas. An aliquot of water is equilibrated with an immiscible organic liquid scintillator in a glass liquid scintillation vial. Radon is extracted into the organic phase. The mixture is allowed to age for three hours to allow ingrowth of short half life daughters, and counted using a liquid scintillation counter.
Reference:
USEPA-LV Environmental Monitoring Systems Laboratory, The Determination of Radon in Drinking Water by Liquid Scintillation Counting. Method 913.0 (May, 1991).
5.14 Method Exceptions and Departures.
Occasionally samples are received which cannot be processed using the approved methods because of matrix interferences, inadequate sample volumes, expired preservation times, or other circumstances. When, in the judgement of the laboratory manager, useful data can still be obtained by use of a modification to the standard method, the customer will be contacted and the options explained. The lab manager will explain to the customer that the results will not be considered valid for regulatory purposes, and that the report will carry a disclaimer to this effect. The customer will decide if the work is to proceed. Quality Manual Page 13 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
5.15 Employee SOP Certification
Employees signing this document (cover page) certify that they have read, understood, and agree to perform the most recent version of all SOP's.
6.0 Equipment and Instrumentation
The following items of equipment are available for use by the radiochemistry group:
(one) Tennelec LB 4000 low background alpha/beta gas flow proportional counter
(one) E.G.&G. Ortec multichannel analyzer w/Maestro spectrum software
(one) Ortec Model 7150 multichannel analyzer with Ortec amplifiers
(one) Canberra model 7401VR alpha spectrometer with 450 cm2 PIPS detector
(two) 3 in. x 3 in. sodium iodide gamma detector
(one) Houston Omnigraphic 2000 X-Y plotter
(one) Northgate 386/SX computer with Epson 5000 printer
(one) Jarrell-Ash Model 26-000 fluorimeter
(one) Packard 1600 TR liquid scintillation counter
(two) Sartorius A200S electronic analytical balances
(one) Ludlum Model 43-10 alpha scintillation counter with Model 1000 sealer
7.0 Reference Standards and Traceability
Instruments are calibrated with reference standards that are provided by the National Institute of Standards and Technology (NIST) or the New Brunswick Laboratories (NBL). The following reference materials are used:
Analysis Isotope Form Source Ra-226 Ra-226 solution NIST Ra-228 Ra-228 solution NIST Th-230 Th-230 solution NIST Po-210 Po-210 solid NBLnNBL no< . 6-A pitchblende ore Pb-210 Pb-210 solid NBLnNBL no< . 6-A pitchblende ore Quality Manual Page 14 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Gross alpha Th-230 solution NIST Gross beta Y-90/Sr-90 solution NIST Uranium U3O8 solid NIST no. 950a black oxide Radiocesium Cs-137 solution NIST Radiostrontium Y-90/Sr-90 solution NIST Tritium H-3 solution NIST Radon Ra-226 solution NIST
8.0 Sample Management
8.1 Sample Preservation
The majority of samples sent to Hazen are collected by the client or his representative. Hazen Research can assist the client in sample site selection, collection methods, and preservation techniques. We can provide a field sampling crew and all necessary supplies, including sample containers, preservatives, and labels. The client is encouraged to check with the lab manager prior to beginning a sampling program so that sample collection, preservation, and shipping logistics can be finalized.
Sample preservation techniques must be used to insure that the sample is stabilized prior to being analyzed. The following general guidelines apply:
Air Particulates: To avoid loss of particulate material contained on 8 x 10 inch high-vol filters, they should be folded once to enclose the exposed side of the paper and placed in an appropriately sized folder and labeled envelope. The laboratory can provide folders and envelopes for this purpose. The folders serve as a form to record flow data, sampling time, dates, and other pertinent information. Low-vol filters should be shipped to the lab in their original cassettes or in sealed petri dishes.
Drinking Water: Except for samples to be analyzed for radon or tritium, water samples must be acidified with reagent grade nitric acid to pH less than 2 within 5 days of collection, and then allowed to stand for a minimum of 16 hours prior to analysis. If this is not done, regulatory requirements specify that the sample must be rejected, and a new one collected. The laboratory manager will be responsible for notifying the customer when this occurs.
Water samples collected for radon analysis require a special sampling apparatus and bottles. Instructions and equipment for collecting radon samples are available from the laboratory. Quality Manual Page 15 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Water samples collected for tritium analysis require no special preservatives, filtration, or sample handling. These samples must be collected in a glass bottle.
Wastewater and Effluent Samples: If dissolved radionuclides only are to be determined, the sample should be filtered on site using a 0.45 micron membrane filter, and acidified with reagent grade concentrated nitric acid to pH less than 2. Plastic bottles should be used as sample containers.
If'potentially dissolved' radionuclides are to be determined, the sample should be acidified immediately after collection with reagent grade concentrated nitric acid to pH less than 2 and allowed to stand for at least 16 hours. The lab will then filter the sample and determine the recoverable radionuclide content.
If both dissolved and suspended radionuclides are to be determined, the sample should be filtered on site using a 0.45 micron membrane filter and the filtrate acidified to pH less than 2 using reagent grade nitric acid. The filtrate and filter will be analyzed separately. The volume of sample treated should be recorded so that the suspended radionuclide concentration can be calculated. If field filtration is not possible, the sample should be transported to the lab as quickly as possible, with no treatment. The lab will filter the sample and use the filtered residue to determine suspended radionuclides, and will acidify the filtrate for determination of dissolved radionuclides.
'Total' radionuclides are determined by filtering the sample, digesting the filter, and adding the resulting digest back to the filtrate.
Additional discussion of sample preparation and reporting bases can be found in SOP Waterprep-1, Preparation of Water Samples for Metals Analysis.
Samples should not be allowed to sit in direct sunlight or near a source of heat above normal room temperature. Conversely, samples should not be allowed to freeze.
The laboratory may require up to four gallons or more of water to complete the full suite of radiochemical analyses, including all QC requirements, and separate samples must be collected for radon and tritium. The volume of sample used for each analysis is listed in Appendix E. Laboratory customers are encouraged to contact the lab manager to discuss sample volume and preservation requirements prior to submission of samples. Work will not begin on a set of samples if there is Quality Manual Page 16 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
insufficient material available to meet regulatory requirements for sample size and QC.
Vegetation, Soil. Sediments: These samples should be sealed in plastic bags and shipped immediately to the lab. The client should specify if the analyses are to be done on an as-received (wet) basis or on a dry basis. Dry basis analyses will normally be done unless other instructions are received.
8.2 Sample Receiving, Acceptance, and Log-in
The Hazen laboratory operates a networked microcomputer laboratory management system that supports the SOP for receiving and logging samples and analytical requests. This SOP is described graphically in the flowchart contained in Appendix F. The system provides administrative record keeping so that sample and associated data are documented and traceable through the analytical process. Such information as received dates, analysis requests, methods, ID numbers, and completion dates are easily accessible. The computer data are backed up daily by hard copy reports.
The system is used daily by the laboratory managers and supervisors to help plan work assignments, and to monitor individual group status and performance.
8.3 Sample Storage and Disposal
Hazen Research Inc. employs a full time safety/environmental compliance engineer whose responsibilities include oversight of disposal of hazardous wastes and samples from laboratory and pilot plant operations. This responsibility includes training of lab personnel in proper disposal methods, and interaction with regulatory agencies to insure that disposal is carried out according to current regulatory requirements. Additionally, Hazen employs a radiation safety officer whose responsibilities include oversight of the radioactive materials license, which covers inventory and disposal of radioactive materials.
The labeling and storage requirements for radioactive materials and samples can be found in the Hazen Research Inc., Radiation Protection Program manual.
Analytical pulps and water samples are stored for three months, or longer if requested by the client, before disposal. Quality Manual Page 17 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
8.4 Chain of Custody
Chain of Custody procedures are facilitated via the use of either the client's COC form, or via Hazen's COC form. A copy of the latter is contained in Appendix G, along with a copy of Hazen's Sample Receipt Form.
9.0 Data Management
9.1 Worksheets, Calculations
Data collected during the course of an analysis are recorded on a standard worksheet form that is keyed to a computer program used to calculate the final results. Included in the hardcopy data file for each analysis are copies of alpha or gamma spectra, where applicable, instrument printouts, and results obtained on spiked samples, standard reference samples, duplicate analyses, and blanks. A copy of a typical worksheet is contained in Appendix H.
9.2 Data Validation
Calculations and computer inputs are checked for transcription accuracy by the radiochemistry group supervisor, who initials each page of checked data. The laboratory manager reviews all data, with respect to appropriate quality control and consistency of results, prior to release of a final report to the client. The laboratory manager will initial and date each page of checked data.
9.3 Reporting
Results of analyses are reported on Hazen letterhead paper. Reports will include the date of sample receipt, date of report issue, Hazen identification numbers, client sample identification numbers, Hazen project number, client purchase order number, reporting units of the listed results, method references, and analyst initials.
Radiochemical results are always accompanied by their statistical counting uncertainty at the 95% confidence level. An estimate of the overall analytical uncertainty is not normally reported, but is available from the laboratory manager, if required by the client for reporting purposes.
All reports are reviewed by the laboratory manager as a final check before the data are forwarded to the client.
A typical report is contained in Appendix H. Quality Manual Page 18 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
9.4 Storage and Disposal of Records
Analytical data, chain of custody and sample receipt forms, and reports are stored for a period often years.
9.5 Security and confidentiality
New employees are instructed in the company security and confidentiality policies immediately upon hire. All employees are reminded of the policies at least once per year, thorough re-issue of the written security policy. A copy of this policy is contained in Appendix I.
10.0 Quality Management
10.1 Instrument Checks
Instrumentation is serviced and checked periodically to maintain optimal performance.
Analytical balances are maintained under contract with a reputable balance service company. They are cleaned and adjusted twice each year, or more often if required. Balances are checked daily with two class S check weights, and the results recorded.
The gas flow proportional counter is checked at the beginning of each day of use with americium-241 and strontium-90 reference sources to insure that instrument performance has not deteriorated. Background counts are taken each day that the instrument is in use. The results of these tests are recorded in a notebook, and plotted on control charts for easy visual determination of variability (see Appendix J). The procedure for performing these checks is contained in Appendix K.
The alpha spectrometer is energy calibrated at the beginning of each day of operation using an amerecium-241 reference source. The alpha spectra are displayed and integrated on a CRT, so that the analyst can note any abnormal characteristics (such as excessive tailing) that may affect the validity of the results. A background determination is made once per week and plotted on a control chart. The procedure for performing these checks is contained in Appendix L.
The liquid scintillation counter is checked at the beginning of each day of use with a carbon-14 and a tritium check source to insure that instrument performance has not deteriorated. Background counts are taken each day that the instrument is in use. The results of these tests are tabulated in a Quality Manual Page 19 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
notebook, and examined to confirm correct operation of the instrument prior to counting samples. The procedure for performing these checks are contained in Appendix M.
The gamma spectrometer used for measuring barium-133 spike recoveries is energy calibrated at the beginning of each day of operation using a New England Nuclear barium-133 solution. The detector is checked once a month for resolving capability using a cobalt-60 sealed source. Spectra are displayed and integrated on a CRT so that the analyst can note any abnormal characteristics that may effect the validity of the results. The procedure for performing these checks are contained in Appendix N.
The scintillation (ZnS) counter is checked at the beginning of each day of use with a thorium-230 reference source to insure that instrument performance has not deteriorated. Background counts are taken each day that the instrument is in use. The procedure for performing these checks are contained in Appendix O.
10.2 Batch Quality Control
A batch of samples is defined as twenty samples or less, processed together. Each batch of samples will contain a minimum number of quality control samples. These QC samples will include:
Control Standards
NIST and NBL reference materials are used as control standards which are carried through each procedure along with unknowns to check recovery and bias. Each batch of samples will be accompanied by at least one of these standards.
Duplicate Samples
Each batch of samples containing less than 10 samples will contain at least one duplicate sample. Batches of 10 or more samples will contain at least two duplicate samples.
Each batch of samples will contain one spiked sample to check analyte recovery. Quality Manual Page 20 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Each batch of samples will contain at least one blank sample consisting of deionized water. The blank sample will be carried through all of the chemical processes that are applied to the batch samples.
10.3 Acceptance Criteria
Results obtained on control standards are tabulated and charted. Appendix P contains a typical chart showing results of control standard analyses. The results are considered acceptable if they He within the control limits provided by the chart.
Duplicate analyses are tabulated and charted. Appendix Q contains a typical chart showing results of duplicate analyses. Pass/Fail criteria for duplicate analyses are also contained in this appendix.
Spiked sample results are tabulated. Acceptable spike recovery is 80% to 120%. Appendix R contains a typical table showing spike recovery results.
Blank sample results are tabulated. Acceptable results are defined as values that are less than 2 x the method detection limit (MDL). Appendix S contains a typical table showing blank analysis results and pass/fail criteria.
10.4 Corrective Actions
Instrument function that deviates from established control limits will result in repair, cleaning, or recalibration of the instrument to restore proper operation.
Batch QC results that are out of established control limits will result in review of all the data associated with that batch. The Lab Manager and/or the Lab Director will perform this review. If the problem cannot be found and corrected, the batch will be completely or partially rerun. Exceptions may be made, based on the professional judgement of the reviewers. Such exceptions might include: insufficient sample for rerun; the batch does not contain results that are close to or above the regulatory limits for the analyte in question; the deviation from the control limit is not considered large enough to materially effect the validity of the batch. The reviewer will note on the data sheet the reason for any exceptions that are made. Quality Manual Page 21 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
10.5 Proficiency Testing
The Hazen laboratory participates in the Environmental Resource Associates RadCheM Proficiency Testing Program, and the New York State Potable Water Proficiency Testing Program. Reports from these providers are available for client inspection, if requested.
10.6 Internal Audits
The quality assurance officer will conduct yearly audits of the quality control system to insure that procedures outlined in this manual are being followed. This process will be facilitated and documented by the use of a checklist. The checklist is contained in Appendix T.
10.7 Customer Complaints
Customer complaints may include issues related to turnaround time, responsiveness, quality of results produced, pricing, and inquiry followup. The first level of responsibility for responding to customer complaints lies with the laboratory manager. If the issue cannot be resolved at this level, then it is the responsibility of the laboratory director to intervene and resolve any problem that still exists. The laboratory director is authorized to use any and all company resources that can be applied to the problem. This includes consulting with the company president or any of the senior managers who may have experience in resolving a particular kind of problem. Quality Manual Page 22 Radiochemistry Laboratory Revision 11 Hazen Research Inc. . 3/8/2000
Appendix A
Organizational Chart APPENDIX A
HAZEN RESEARCH, INC. ANALYTICAL DEPARTMENT ORGANIZATIONAL CHART March 8, 2000
N. Hazen, President, Hazen Research, Inc.
J. Jarvis, Quality Assurance Manager, Analytical Dept.
• J. Jarvis, Director, Analytical Department
R. Rostad, Manager, General Analytical
P. Ware, AA Group Supervisor
•B. Youngclaus
L. Hartan,, Wevveit Chemistry Group Supervisor I- H. Melikean E. Dela Fuente, Radiochemistry Group Supervisor
' A. Strapac
• R. Oberto
• B. Youngclaus
'D. Yheaulon, Water Lab Supervisor
C. Henry, ICP Spectroscopy
R. Bauman, Fire Assay
B. Stewart, Secretary
D. Christensen, Sample Logging
•G. Cunningham, Manager, Fuels Lab
V. Hebel
T. Demouth Quality Manual Page 24 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix B
Demonstration of Capability Form Quality Manual Page 25 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
DEMONSTRATION OF CAPABILITY
Analyst:
Analyte:
Method Reference:
SOP No. and Revision:
Date of Demonstration:
PE or QC Sample Used:
Acceptable Range of Results:
Results Obtained by Analyst:
We, the undersigned, certify that:
The analyst identified above, using the cited test method, which is in use at this facility for the analyses of samples under the National Environmental Laboratory Accreditation Program, have met the Demonstration of Capability.
The test method was performed by the analyst identified on this certification.
A copy of the test method and the laboratory-specific SOP is available for all personnel on-site.
The data associated with the demonstration of capability are true, accurate, complete, and self-explanatory.
All raw data (including a copy of this certification form) necessary to reconstruct and validate these analyses have been retained at the facility, and that the associated information is well organized and available for review by authorized assessors.
Name, Director, Analytical Dept. Signature Date
Name, Quality Assurance Officer Signature Date
Attach all supporting backup data and worksheets. Quality Manual Page 26 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix C
Staff Resumes Quality Manual Page 27 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
John C. Jarvis, Director, Analytical Department
Academic History:
M.S. Analytical Chemistry, 1973 Colorado School of Mines
B.S. Chemistry, 1970 Colorado State University
Professional History:
Hazen Research Inc., Golden, Colorado, 1972 to present
Director, Analytical Department Laboratory Manager Group Supervisor Chemist—radiochemistry, wet chemistry
Special Fields:
Rare earth element geochemistry Instrumental methods of analysis X-Ray fluorescence and microprobe spectroscopy Neutron activiation analysis Microcomputer laboratory applications Fire assay Laboratory management Radiation safety Quality Manual Page 28 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
Robert R. Rostad, Laboratory Manager
Academic History:
M.S. Analytical Chemistry, 1974 Colorado School of Mines
B.S. Chemistry, 1970 Colorado School of Mines
Professional History:
Hazen Research Inc., Golden, Colorado 1974 to present.
Laboratory Manager Group Supervisor Chemist—radiochemistry, wet chemistry, atomic absorption
Special Fields:
ICP spectroscopy AA spectroscopy Wet chemistry X-Ray fluorescence spectroscopy Laboratory Management Quality Manual Page 29 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
Eve DelaFuente, Supervisor, Radiochemistry Laboratory
Academic History:
B.S. Chemical Engineering, 1965 Cebu Institute of Technology, Phillipines
Professional History:
Hazen Research Inc., Golden, Colorado 1976 to present.
Supervisor, Radiochemistry Section Chemist—wet chemistry, atomic absorption spectroscopy
Special Fields:
General wet chemistry Atomic absorption spectroscopy Radiochemistry of naturally occurring radionuclides Quality Manual Page 30 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
Richard P. Oberto, Senior Chemist
Academic History:
B.A. Chemistry, 1970 University of Colorado
Professional History:
Hazen Research Inc., Golden, Colorado 1970 to present.
Group Supervisor, Wet Chemistry, Radiochemistry Senior Chemist
Lucius Pitkin, Inc. (USAEC), Grand Junction, Colorado ,1957-1969
Chemist, uranium processing
Special Fields:
Wet chemistry—colorimetry, titrimetry, gravimetry Atomic absorption spectroscopy Radiochemistry of naturally occurring radionuclides Quality Manual Page 31 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
Ann M. Strapac, Lab Technician
Academic History:
B.S. Biology University of Oregon, Eugene Oregon
Professional History:
Hazen Research Inc., Golden, Colorado, 2/20/1998 to present
Lab Technician, Radiochemistry
University of Oregon, Eugene, Oregon, 1/1996 to 6/1996
Research Assistant
Special Fields:
Radiochemistry of naturally occurring radionuclides Uranium by fluorimetry Quality Manual Page 32 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
APPENDIX C
STAFF RESUMES
Youngclaus, William M.
Academic History.
Metro State College, Denver, CO Courses in chemistry and math
Professional History:
Hazen Research Inc., Golden, Colorado, 12/1996 to present
Bench Chemist
ActLabs, Wheat Ridge, Colorado, 2/1/95 to 3/1/95
Lab Technician
Skyline Labs, Wheat Ridge, Colorado, 5/1/77 to 2/1/95
Lab Technician
Barringer Laboratories, Lakewood, Colorado, 6/2/92 to 6/1/93
Lab Technician
Special Fields:
General wet chemistry Atomic absorption spectrophotometry ICP spectrophotometry Fluorimetric uranium analysis Quality Manual Page 33 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix D
Hazen Campus, Analytical Lab Floor Plan 'IS VNVIdNI
\ BLDG.1 MAIN LABORATORY FLOOR PLAN Quality Manual Page 36 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix E
Detection Limits and Sample Volumes Detection Limits for Radiochemical and Uranium Analyses
The following detection limits are calculated based on the detection limit definition given in EPA-600/4-80-032, Prescribed Procedures for Measurement of Radioactivity in Drinking Water. Appendix C, Method HI
The detection limit is defined as follows:
LLD= 1 OOP xf7.681 xB/T/T)*0'3 2.22 xVxE
Where: LLD = The lower limit of detection in pCi/1 B = Instrument background count T = Time of background count, min. V = Sample volume, in milliliters E = Counter efficiency
Sample volumes and counting times routinely used by the Hazen Lab are as follows:
Sample Counting Detection Radionuclide Volume, ml (me) Time, min. Limit, pCi/1 (s)
Radium-226 1000 33.3 0.2 Radium-228 1000 60.0 1.0 Thorium-230 500 33.3 0.4 Lead-210 500 60.0 2.0 Polonium-210 500 60.0 0.3 Gross Alpha 200 60.0 0.8 Gross Beta 200 60.0 4.0 Radon 15 50.0 8.0 Tritium 4 100.0 600.0 Strontium-90 1000 60.0 1.0 Strontium-89 1000 60.0 2.0 Radiocesium 1000 60.0 1.0
The detection limit for uranium by fluorimetry is 0.002 mg/1 (1.3 pCi/1). Quality Manual Page 38 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix F
Sample Acceptance and Log-in Flowchart RADIOCHEMISTRY SAMPLE ACCEPTANCE AND LOGIN FLOWCHART
SAMPLE RECEIVED LAB 1 WITHIN FORWAR DTO LAB'S N SUBCOf*JTRACTO R OR ^ CAPABILITY? RETURN TO CLIENT Y
SAMPLE PROC:EE D VOLUME N >. ANYV VAY7 N ADEQUATE? Y Y 1 SEALED NOTE REASON ON FINISHED SAMPLE RECEIVED PRODUCT? SHEET N 1 ARRIVED ACID FIED pH<2? TO N N —* f O O pH < Y \f 1 . \V PRESERVED PROC:EE D WITHIN —. ANYVVi//\ M YT ?: MIN 5 DAYS ? >I Y 1 NOTE REASON ON SAMPLE RECEIVED SHEET ir ir PROCEED REJECT WITH SAMPLE(S) LOGIN LOGIN
NEW ASSIGN v fc, PROJECT ? ' W PROJECT NO. N 1
ASSIGN LAB CONTROL NO.
SAMPLE ANALYTICAL COMPILE k. RECEIVED W FORM L \ ' \ ANALYSIS LAB REQUEST MANAGER FORM REVIEW 1 OK LOGIN CLIENT WORKSHEETS
ANALYSTI S LOGOFF
CALCULATE RESULTS
OK
SUPERVISO1R LAB CHECK OK MANAGER REVIEW
c:\excel\radchk.lst Quality Manual Page 41 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix G
Chain of Custody and Sample Receipt Forms a o o DC o 0 • o o in I DC 1 i > g o fr 3T a *• 1 3 i (D f i a i 8 ao o & LL i O c o z i 5 >. < a. §s 1 0 o 2 0 a sc ja ^ 1 E c S r i t t .y
> 1 1 or or | £ £ £ •si o o 2 i; Z c • * jj a O 1 f £ c w •9» -S> o J2. 52. C £ o >« >, H •g f •p S" J3 i J J 2 O
5o5 (C • u> i * 2 S 0. 0 z|S 2 "^ 1 "^ 5^« t> a I s" I F I iii^ a . 2 } I ^^ I » 5* £ j^ £. S 1 1 C n « i 0 o §• cr & ^~ z c c c CB |' J 25 & £ £ HAZEN RESEARCH INC. ANALYTICAL DEPARTMENT Lab Control No. 4601 Indiana St. Golden, CO 80403 (303)279-4501 SAMPLE RECEIPT FORM
Submitter HRI Proj. Address: Date Rec'-d. Rec'd By Ship Via Contact: Cust PO
FAX Results (Y/N)_ FAX No.
Special Instructions
Arrived Adj. to Within Lab No. Prep. pH<2? pH<2?|five Daysl Bottles Reg? Client ID (Y/N)
Checked By: Quality Manual Page 44 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000
Appendix H
Worksheets, Reports Hazen Research, Inc. DATE Octobers, 1999 4601 Indiana Street • Golden, CO 80403 HRI PROJECT 002-3AZ Tel: (303) 279-4501 HRI SERIES NO. X003/99 Fax-(303) 278-1528 DATEREC'D 08/17/1999 OUST. P.O.* None Rec'd
John Smith's Testing Company John Smith 12345 West 60th Avenue Littletown, TX 84569 REPORT OF ANALYSIS
SAMPLE NO. X003/99-1
SAMPLE IDENTIFICATION: Sample # 1 - Well Water - collected on 10/01/99 @ 1300 by John Smith
DETECTION ANALYSIS PARAMETER RESULT LIMIT METHOD DATE ANALYST
Gross Alpha (+-Precision*), pCi/l (D) 35(+-7) 1 EPA 900.0 09/07/1999 EOF @0645 Gross Alpha (^-Precision*), pCi/l (D)*** 1{+-7) 1 EPA 900.0 09/07/1999 EDF @0645 Gross Beta (^-Precision*), pCi/l (D) 18(+-4) 3 EPA 900.0 09/07/1999 EOF @0645 Uranium, mg/l (D) 0.051 0.002 ASTM D2907-91 08/27/1999 AS @1423 Uranium, pCi/l (D)** 34 1 ASTM D2907-91 08/27/1999 AS @1423
'Variability of the radioactive decay process (counting error) at the 95% confidence level, 1.96 sigma. Certification ID's: CO/U.S. EPA Region VIII - XM; CT - PH-0152; KY - 90076; KS - E-10265; NH - 232897-A; NY ELAP -11417; PA DEP 68551; Wl - 99837610
"Uranium results reported assuming the activity of natural U = 6.77 x 10-7 Ci/gm. ***Less Radon and Uranium.
CODES: By:_ (T) = Total (D) = Dissolved Robert Rostad (S) = Suspended (R) = Total Recoverable Laboratory Manager (PD) = Potentially Dissolved < = Less Than
An Employee-Owned Company VfN \A tsft 0 Vsl N CD O r
Q <0 N N cs *m •NI 0 ra vr> (A vrv tff b tsi Vri CD a. o c
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CO c. 0 o CL to V* o. «a M s> s ra CO ra o (a Q O i 8 > E Vn ro X. s "SJ CO O- TJ Q. < O ^ < ~5 fY * rc 6» CD O CM 0° CO f \\ _ CO O VA Oo (0 NS f d vn eo O oi si \I\ • * NV re c IK E (U nj E xfl xO ro •o •O O o-*-• E CD •a c c s en O) m m CO CO •s .c Q Q. m -c Quality Manual Page 47 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix I Security and Confidentiality HAZEN RESEARCH SECURITY PROCEDURES 1. Employees' Responsibilities New employees must read and sign a memorandum which describes the confi dential nature of Hazen's business. This memo warns employees against revealing information in casual discussions with outsiders or when answering phone calls. Also, employees are advised that people who are not employees are not allowed in pilot plant or laboratory areas unaccompanied by a staff member. This signed memorandum is retained in the personnel file of each employee (copy attached). Each new employee also signs a patent agreement (copy attached). Article (d) of that agreement states, 1 agree, except as the corporation may otherwise consent in writing, not to disclose at any time either during or subsequent to my employment, any information, knowledge, or data of the corporation I may obtain during the course of my employment, relating to formulas, processes, methods, machines, manufactures, compositions, inventions, discoveries or otherwise, which is of a confidential nature." When employees are terminated, all lab notebooks, reports, and keys must be returned to the appropriate supervisor before the final pay check is issued. 2. Buildings, Laboratories, and Private Offices Access to laboratories, pilot plants, and other buildings is restricted to Hazen employees. Visitors are permitted only when accompanied by a Hazen staff member. Sponsors may request that the area where their project is being conducted be restricted to directly-involved employees only. Issuance of keys is limited and recorded. Spare keys are labeled and kept in the vault Private offices are locked, and individuals' report or project files are locked. 3. Sample Handling and Analytical Data Samples coming to Hazen for research and development test work are logged in by date, client name, and nature of the material, e.g., water, drill core, rock, soil, and are assigned a number which becomes the identification attached to the sample as it progresses through sample preparation and testing. Analytical lab personnel maintain lab notebooks which have an identification number. Analysis data are recorded in these notebooks, along with the corre sponding sample numbers. When full, the books are returned to a designated custodian and retained in a locked cabinet. The lab uses "Analysis Worksheets" to record and report some kinds of analyses. These worksheets also contain only the sample numbeKs) and the analytical data associated with the sample(s). The original worksheet is forwarded to the sample submitter (Hazen technician or engineer) and a copy is kept in the Analytical Department's locked files. 4. Laboratory Notebooks Bound notebooks, which are numbered, are issued to technical staff members for recording procedures and test results. Each person to whom a notebook is issued is responsible for its safe handling. All books are placed in locked cabinets or files at the end of each work period. When full, the books are returned to a designated custodian and are retained in a locked cabinet. 5. General Office Procedures Personnel are instructed concerning security and the matter is discussed at frequent intervals. The switchboard operators are instructed to refer all inquiries other than those directed to a specific individual to an officer of the company. The telecopier is near the receptionist's desk and all incoming or outgoing messages are concealed from the casual visitor's glance. Work in progress is placed in locked files overnight, rather than in desks. Desks are left clean and locked. Word processing disks and the disk index are kept in locked files. Confidential material can be stored on a disk which is accessible by an entry code known only to author and operator. Files are kept locked unless the file clerk is working on them. Files may, however, be removed for reading by Hazen staff members unless confidentiality is restricted to certain people. Two copies of all reports are retained, one copy is in locked file cabinets in the general office area and one copy is in a locked file room on the second floor of Building 1. A record of copy distribution is included in each copy. Reports from the general office files may be checked out by staff members unless marked "Confidential." Copies of reports are also distributed to project managers on a need-to-know basis. The file clerk maintains an inventory of such reports and verifies that inventory at regular intervals by contacting each project manager. Retention of report copies by authors is discouraged. The printing equipment is located in a separate room behind the general office. All extra pages are burned once a day in an incinerator on the premises. The original copy of each report is retained in a locked cabinet for two months and then burned. Also, rough drafts of completed reports are burned. On occasion, requests are received by phone or letter from third parties seeking information concerning sponsored work performed by Hazen. In each case the request is handled by an officer of the company who explains that Hazen must receive written authorization from the sponsor of the work for release of any information to a third party. No information can be released without such authorization. 6. Accounting Department All unfiled material in the accounting office is shredded on site. Desks are clean and locked. Only two keys to the building are issued. Quality Manual Page 51 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix J Instrument Control Charts Instrument Control Charts The control chart is a device used to display the performance of an instrument or counting system and to aid in detecting behavior which is outside of accepted limits. A baseline of acceptable performance must first be established by making a minimum of 20 repetitive measurements of equal duration during a period of time when the instrument is functioning properly. From these measurements a mean and standard deviation is calculated. For example, twenty background measurements, of t minutes duration each, are made on the alpha plateau of the gas flow proportional counter. These are tabulated as follows: Count no. Xi ! {Xi X) | (Xi X)*2 1 126 28 784 2 144 10 100 3 169 15 225 4 190 36 1296 5 129 25 625 6 177 23 529 7 140 14 196 8 119 35 1225 9 129 25 625 10 144 10 100 11 161 7 49 12 178 24 576 13 129 25 625 14 192 38 1444 15 188 34 1156 16 157 3 9 17 194 40 1600 18 124 30 900 19 140 14 196 20 157 3 9 Mean (X) = (SUM Xi)/N = 3087/20 = 154 SUM (Xi - X)"2 = 12269 Standard Deviation (sigma) = [12269/(N-l) ] A - 5 = [12269/19] *-5 = 25 counts A value of 2 x sigma is designated as the 'warning level', and a value of 3 x sigma is designated as the 'control limit'. A control chart can now be constructed. A chart is established with the counting rate as the ordinate and the date of the measurements as the abscissa. A horizontal line is drawn at the mean and at the ±2 and ±3 sigma levels. The daily count rates are then plotted on the chart. If the data fall within ±2 sigma, the instrument is considered to be operating acceptably. RADIOCHEMISTRY QUALITY CONTROL CHART Detector ID Radionuclide Count Date 22? Control limit Warning limit_ m 13-1 -1 .2 Warning^ Limit 71 -3 Control Limit S I G M 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 A Count Number x= Sigma= Sigma/4= Quality Manual Page 54 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix K Perfomance Test Procedure Gas Flow Proportional Counter Performance Test Procedure for Tennelec LB-4000 Gas Flow Proportional Counter Initial Instrument Settings: Discriminator Settings: Beta Lower Level 0 Beta Upper Level 1400 Alpha Lower Level 1401 Alpha Upper Level 4095 Threshold 25 Detector Bias: Alpha 502.5 Beta 1401.0 Gas Flow: 1.5 L/M Plateau Curves: Plateau curves are generated so that optimal detector bias settings can be made for alpha particle and beta particle measurements. The LB-4000 instrument has a facility for generating plateau curves automatically. These curves should be established when the instrument is initially set up and after any major repair which might alter the performance of the instrument. Daily Plateau Check: To insure that plateaus have not drifted or changed on a day-by-day basis, check sources are counted each day that the instrument is in operation. A cesium-137 check source is used to check the beta measurement, and an americium-241 check source is used to check the alpha measurement. Obtain a baseline average for each detector by performing 20 successive counts of the source. Construct a control chart according to the procedure outlined in Appendix A. Count the source each day that the instrument is in use and plot the result on the control chart. If the point falls within ± 2 sigma, the instrument is functioning properly. Instrument performance that falls outside of the established control limits will result in repair, cleaning, or recalibration of the instrument to restore proper operation. Daily Background Check A background control chart should be constructed for each detector. To obtain the baseline average, perform 20 successive background counts of 60 minutes duration. Construct a control chart using the procedure outlined in Appendix A. Perform additional background counts each day that the instrument is in use and plot them on the chart. If the data fall within the ± 2 sigma limit, the instrument is functioning properly. Instrument performance that falls outside of the established control limits will result in repair, cleaning, or recalibration of the instrument to restore proper operation. Quality Manual Page 57 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix L Performance Test Procedure Alpha Spectrometer Performance Test Procedure for Canberra 7401 VR Alpha Spectrometer Energy Calibration and Detector Resolution Spectrometer initial settings: Bias setting: set per instructions provided with detector Descriminator: 0.10 mev E.G.& G. Ortec TRUMP Multichannel Analyzer: Horizontal Scale: 204B Vertical Scale: Auto Preset Live Time: 2000 sec. Place the americium-241 source in the counting chamber and evacuate the chamber. Count the source for 40 seconds and terminate the count. Do not clear the spectrum, but leave it in memory. Remove the americium-241 source and replace it with the thorium-230 source and again evacuate the chamber. Count this source for 2000 seconds. Double click on each peak to obtain a FWHM value for each. Print the spectrum. The americium-241 peak is 5.486 MeV. The thorium-230 peak is 4.684 MeV. Energy calibrate the graph and determine the energy span of the FWHM of the 5.486 MeV peak. This value, in MeV, is the detector resolution. Record this value in the Q.A. notebook. Background Performance Check A background control chart will be constructed on each region of I interest in MCA memory. To obtain the baseline average, perform 20 successive 20,000 second background counts, and plot the data on a control chart. If subsequent background data fall within ± 2 sigma, the background count is within expected limits. Appendix A contains additional information concerning construction of control charts. Backgrounds that are out of tolerance will result in repair, cleaning, or recalibration of the instrument to restore proper operation. Quality Manual Page 60 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix M Performance Test Procedure Liquid Scintillation Counter System Normalization QIP/C-14 Efficiency Check Tritium Efficiency Check Background Check CHAPTER 6 QIP/i 4c Efficiency Check 1. Initiate conversation by pressing the EDIT PROT function key (Fl). Once the function key is pressed, the system asks for the protocol number to be edited. 2. Select a protocol number not being used, and enter that number via the keyboard. Press the # COUNTS/VIAL? 3 RADIONUCLTOE? 14C QEP? tSffi 4. Press Fl-EXIT EDIT, twice, to return to Status Page display. 5. Set up th sample e changer as follows: a. Select and insert correct protocol plug into a Varisette cassette. b. Load an unquenched 14C standard (PPN 6008513). c. Initiate counting. 6. Th acceptable e QIP results are 1000 ± 50 (± 5%) for tSEE and 156 ± 8 (±5%) for SIS. The three repeat counts should be repeatable within ± 3%. 7. Calculate the efficiency as follows: CPM of Region A 10Q% DPM of14C Standard The mtniTmim acceptable efficiency for 14C is 95% for large vials and 94% for small vials. \ 8. If the QIP and/or the efficiency results are not within the defined values, ;perfonn a system Self-Normalization and Calibration (refer to page 146) and repeat the test. If the results are still not within the defined limits, call your Packard technical service representative. 170 operation QIP/C-14 Efficiency Checks - Packard 1600 TR Average (i.) (2.) Date CPMA SIS tSIE C-14 Eff.% Repeat. .% Pass/Fail iole./9-T /«••/*/ 7*7 A3 0-7 %*<• A/ 0-7 /*•>- o-l vh/lr ,,, fc/fJ 97? 76.2 73/ o-t, / 43 997 tlJL, /&,/ 0-7 0 -03" 63 9*-. . fc / 0.3 911 1 -2.L 373 O.f .r 0.7 A/ rn Pass Criteria: SIS must be within 148-164 tSIE must be within 950-1050 C-14 efficiency must be 95 % or greater Repeatability must be <= 3 % (1.) C-14 efficiency = CPMA (average)/131,300 X 100 (2.) Repeatability = (largest CPMA - smallest CPMA) / average CPMA X 100 PERFORMANCE VERIFICATION 3H Efficiency Check 1. Initiate conversation by pressing the EDIT PROT function key (Fl). Once the function key is pressed the system asks for the protocol number to be edited. 2. Select a protocol number not being used and enter that number via the keyboard. Press the 4. Press Fl-EXIT EDIT twice. 5. Set up th sample e changer as follows: a. Select and insert correct protocol plug into a cassette. b. Load an unquenched 3H standard. c. Initiate counting. 6. Calculate the efficiency as follows. (Refer to the Tritium Decay Table in Appendix B or use the DECAY function of the instrument to determine the corrected 3H DPM value.) %Eff= 100% Corrected 3H DPM Value x The minimum acceptable efficiency for3H is 60% for large vials and 58% for small vials. 7. If th 3eH efficiency does not meet the minimum, perform a system Self-Normalization and Calibration (refer to page 146) and repeat the test. If the results are still not within the defined limits, call your local Packard technical service representative. operation 171 Tritium Efficiency Checks - Packard 1600 TR Date CPMA H-3 Eff. % Pass/Fail Date CPMA H-3 Eff. % Pass/Fail £.*•'/' / 7£ (76, L/lftl* ^33 Pass Criteria. H-3 efficiency must be 60% or greater (1.) H-3 efficiency = CPMA / 277,700 x 100 CHAPTER 6 Background Check 1. Initiate conversation by pressing the EDIT PROT function key (Fl). Once the function key is pressed, the system asks for the protocol number to be edited. 2. Select a protocol number not being used and enter that number via the keyboard. Press the COUNT TIME? 10 RADIONUCLIDE? Manual Region A: LL = 0, UL=18.6 Region B: LL = 0, UL=156 Region C: LL = 0, UL = 2000 4. Press Fl-EXIT EDIT twice. 5. Set up th sample e changer as follows: a. Select and insert correct protocol plug into a cassette. b. Load an unquenched background standard. c. Initiate counting. 6. Instrument background may vary due to environmental conditions. For example, altitude and background radiation will cause elevated back ground levels. If the background exceeds three times your normal background level, contact your local Packard technical service representa tive. Self-Normalization and Calibration It is recommended that self-normalization and calibration be performed once a day. There are no real operating procedures associated with self-normaliza tion and calibration, other than inserting a special protocol plug (SNC) and an unquenched14C standard into the first sample position ofa cassette and counting that sample. Refer to page 133 for information on IPA and automat ic SNC operation. /72 '- operation Background Checks - Packard 1600 TR Date CPMA CPMB CPMC Pass/Fail f 3 -if..! <> *¥•?<> 37.77 3V 6/.70 34.70 '//3/7J -/D &?• 63-70 37- 37. f 38-r .7 37.9 35. /D 3?. 2-3.60 37.30 ^0.2 Pass Criteria: Background counts should not exceed 3 times the following: CPMA 23 CPMB 36 CPMC 62 Quality Manual Page 67 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix N Performance Test Procedure Gamma Spectrometer Performance Test Procedure for 3" Nal Gamma Spectrometer Energy Calibration and Detector Resolution Instrument setup (initial): Detector high voltage: 890 V Multichannel Analyzer: .Amplifier: "Direct", use external Ortec 485 amp set with gain at 8 and fine gain at 7 LLD: 0.1 tILD: 10 Expand setting: 1 Verticle scale: 500 Memory: Full Digital offset: Off Passive restorer: Off Place the cobalt-60 sealed source in the counting chamber. Count the source for a short period of time to determine in which channel the maximum of the 1173 KeV photopeak lies (largest of the two major peaks) . Adjust the 485 amplifier fine gain to position the peak maximum at or close to channel 817. After this adjustment has been made, count the source for 40 seconds. Plot the spectrum obtained using the X-Y plotter. Determine the full width at half maximum (FWHM) of the 1173 and 1332 KeV photopeaks. Energy calibrate the graph and determine the energy span at the FWHM of the 1173 KeV photopeak. This value, in KeV, is the detector resolution. Record this value in the Q.C. notebook. If this value is more than 15 % different from any of the previous values, or if there seems to be a pattern of worsening resolution, notify the laboratory manager. Quality Manual Page 69 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix O Performance Test Procedure Scintillation Counter Performance Test Procedure for Ludlum Scintillation Counting System Initial Instrument Settings: Voltage Setting: 800 V Scale Setting: 1 Timer Setting: 30 min. Plateau Curve: A plateau curve must be generated manually using the thorium-230 alpha source (inv. no. C-39) . Set the voltage to 500 and count the source for 10 minutes. Record the number of counts. Turn the voltage up by 50 and repeat the count. Continue this procedure until the final voltage is 1000. Plot a graph of counts (Y axis) vs voltage (X axis). Draw a smooth curve connecting the points. Draw a straight line through the horizontally flat portion of the curve. Mark each end of the plateau by noting the points at which the original line intersects the straight line. Determine the midpoint between these endpoints by measuring the distance between the two and dividing by 2. The voltage that corresponds to this midpoint is the plateau voltage to be used for alpha counting. This should be approximately 800 V. Daily Plateau Check: To insure that the plateau has not drifted or changed on a day-by-day basis, a check source is counted each day the instrument is in operation. The thorium-230 source is used for this purpose. Obtain a baseline average by performing 20 successive 10 minute counts of the thorium-230 source. Construct a control chart according to the procedure outlined in Appendix A. Count the source each day that the instrument is in use and plot the result on the control chart. If the point falls within +_ 2 sigma, the instrument is functioning properly. Instrument performance that falls outside of the established control limits will result in repair, cleaning, or recalibration of the instrument to restore proper operation. Daily Background Check A background control chart must also be established. Obtain a baseline average by performing 20 successive background counts of 30 minutes duration each. Construct a control chart using the procedure outlined in Appendix A. Perform additional background counts each day that the instrument is in use and plot them on the chart. If the data fall within the ± 2 sigma limit, the instrument is functioning properly. Instrument performance that falls outside of the established control limits will result in repair, cleaning, or recalibration of the instrument to restore proper operation. Quality Manual Page 72 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix P Control Standard Chart CONTROL CHART - WATER ANALYSIS Date Value a Standard: 1*1 W.I Element: Method: W.7 Analyst; ft.7 to/-/ CL/5 = 3.9 f*C 11.1 no X 0 I O I Quality Manual Page 74 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix Q Duplicate Analysis Chart DUPLICATE ANALYSIS CHART Pass/Fail Criteria Charting of Results Duplicate analyses are considered acceptable (passing) if their respective 95% confidence intervals overlap. The following procedure is used to determine if the confidence intervals overlap, and to provide a mechanism to chart the results for a historical perspective. Using the accompanying Duplicate Analyses - Radiochemistry table, record the date the duplicate analyses were performed in the second column. Record the highest of the two duplicate values in the Replicate 1 column, along with its accompanying counting error. Subtract the error value from the sample value and record this number in the Repl - Error column. Record the second value in the Replicate 2 column, along with its accompanying counting error. Add the error value to the sample value and record this number in the Rep2 + Error column. Subtract B from A and record the result in the C = A - B column. If this value is less than or equal to 0, then the confidence intervals do overlap, and the duplicate analyses pass. Indicate this in the Pass/Fail column. Using the Pass/Fail Chart, 'C' Values, plot the value of C next to the corresponding date. All values that are to the left of the 0 line are acceptable results, and those to the right are unacceptable results. DUPLICATE ANALYSES - RADIOCHEMISTRY HI VALUE LOW VALUE REPLICATE 1 REPLICATE 2 REP1 ERROR REP2 + ERROR C= PASS/FAI1 Date •+-ERROR •+-ERROR B A-B o-s **'/?(, 2.3 -* •*.. o *// 33 - Z. to 07 2.3. - Z.I _/. 3 -2.7L. 30:9 !••* 1-7 10 11 3.7* 2-7 3-3. o-B 12 Sl.7 13 2-7* /.f z-X //-J" 0*7 3.(t> _ 2. 7 14 O 3 7*0. 7 A/ -/.r 15 -0.3 -/.r Ji 7. «? /O -2.c> 17 7-0 2..0 18 •*"• 3.0 ~S3 19 3/W/ffc l-t-i'-/ /-/y// 20 21 0-0 -0,7 22 23 J*. 0.&.J/.3. ±±. 24 0-7 25 7-77«//. oo * te-i -J8.Q 26 D- O -/.&> 27 M o-o „ 2.Q 29 2~ /D-d 30 31 32 t-sr 33 187 f > 1* 34 /. D 0.x -o.r 35 6~O-t-°-7 £>*? -/ 36 * /• O /. D 37 37. £> ^ 27-7 38 Q-otl»V 39 )-•&•* e>>? O.OJ/.Q -/.&, 40 0. o.(, / /. b -. PASS FAIL Quality Manual Page 78 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix R Spiked Sample Tabulation SPTKBD SAMPLE RESULTS PARAMETER: LIMITS: 80 120 % Recovery CONTROL UNSPIKEO SPIKE SPIKED PERCENT PASS/ DATE NUMBER RESULT AMOUNT, PCI RESULT RECOVERY FAIL 60-7 A ^7-i| o-P ? /o /os p, en*-' o-o .os~ o-o ft 9% 0.C, 73 C.87-/ o-O o-'sr O-O 3.O.OO c.no-1 o- o G-0 11. o-O S8-O /7-r 0 U.-r . o O.X/ Vo O-o o.f- 0-&O o .0 /?./ &£?* /ftt fzi-g 0. D ff'T t,/M Quality Manual Page 80 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix S Blank Sample Tabulation BLANK SAMPLE RESULTS PARAMETER MDL BLANK CONTROL VALUF, LIMIT PASS/ DATF PCT/L 2 X HDL FAIL >/¥/ff /•fa 0~O /.£, /•(* o-O /• fc /. fo ff-7 o-o f-C. l-i. f-t, f-6> (•(* £>•/ e-3. o-D 9/f/Pf /•fc -*;»}?? 0-7 *//<>/? f 0-7 *//*/?? o-O /•& o./ £>•£> A Wff 0-7 3/W7 3/4 ff u AD /•L 0-0 P-4 */"/// /Cfc r Quality Manual Page 82 Radiochemistry Laboratory Revision 11 Hazen Research Inc. 3/8/2000 Appendix T Internal Audit Checklist en 1 I CQ O •*•* +rf u 73 • s 2 CX S JS U cu 'g "i PH-1 t—D' 'O S-5 Pi 0< PiH 1 p* • Ml cn en |U cn en en -O T3 .t3 •a •o -o T3 T3 0) CD 32 « CX •CsU CD I II 2 OH "« en i t •4-1 CO O O o o o O O O O g en S CD •f-j bo Q on H^ cn f o H-) en Q 0 IO CO t cx G 2 •o ^ en to 0> •a c/5 0 i AH C a en u 1 1 S 0) 3 Uncert * 0> o, so Referen c 1 nj W g o c cct O CD Superviso r Initia l Countin g Dat a Package s Metho d Reportin g Unit s H vn J -3 fL fj. 5 Q U I ort s ipl e rksheets , Calculati c I O "0 Q Mi O CD « s s C/3 00 on o "^ CN 00 ^ CN m cx> os ^^ Hazen Research Inc, . Radiochemistry Quality Manual Annual Program Review Checklist Page 2 j—t <3 g . ^~-r o J T _ I Status Comments u • « 6 § S a co S "3 *a •£ ^ « •^ cs ed G O *3 1 1 I ro CO Check Sources 1 rt 1 "8 Backgrounds v> CO m 1 04 CO Control Charts 1 I Spectrometer MD 1 CS •o 1 Detector Resolut o c t-~. "8 I Pi CO Check Sources O> CO i o o o o o o o aceabil i CO co CU •Hcd ^3 wj TO "O H % S I. T3 'O & u a c e cx ° a. ~ § u Q 00 ffl o a -K , 6 '§ I «ffl Refe r Profi c P< U O OO O r-s O4 ro ro co •^- ^ Environmental Super fund Records Crater Resources Management SITE: $1*0*tk Cr 8 March 2001 BREAK: ' ^ Z 399 Boylston Street, 6th Floor Boston, Massachusetts 02116 Reference: 215-19 OTHER: ^ (617) 267-8377 (617) 267-6447 (fax) Mr. David Lederer http //www.erm.com United States Environmental Protection Agency - Region I One Congress Street, Boston, MA 02114-2023 RE: Radiological Analyses Standard Operation Procedures Residential Well Sampling Plan Shpack Superfund Site Norton/Attleboro, MA ERM Dear Dave: Please find two copies of Hazen Research, Inc.'s Quality Manual that includes the Standard Operating Procedures for radiological analysis. This information is being provided to supplement the information provided in the Residential Well Sampling Plan dated 28 February 2001. Should you have any questions, please feel free to contact me at 617-267 8377. Sincerely, Steven P. Sacco, P.G. Project Manager cc: David Buckley, DEP (1 copy) Ed Conroy, Metcalf & Eddy (1 copy) Francis Veale, TI (2 copy) File (2 copies)