NRC-05-0034, Semi-Annual Quality Assurance Status Report, July - December 2004
| ML051240121 | |
| Person / Time | |
|---|---|
| Site: | Fermi |
| Issue date: | 12/31/2004 |
| From: | AREVA, Framatome ANP |
| To: | Office of Nuclear Reactor Regulation |
| References | |
| NRC-05-0034 | |
| Download: ML051240121 (137) | |
Text
A AR EVA ANALYTICAL SERVICES SEMI-ANNUAL QUALITY ASSURANCE STATUS REPORT July - December 2004 QUALITYASSURANCE TRENDING ANALYSIS i :
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- OCT JANiE FES MAR APR AY FRAMATOMEANP, INC.
ENVIRONMENTAL LABORATORY 29 Research Drive Westborough, MA 01581-3913 Telephone: (508) 898-9970 Fax: (508) 836-9815
A AR EVA FRAMATOME ANP ENVIRONMENTAL LABORATORY ANALYTICAL SERVICES SEMI-ANNUAL QUALITY ASSURANCE STATUS REPORT JULY-DECEMBER 2004 EL 027105 Date:
/.7 1o Prepared By:
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Reviewed By: -
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Date:
Date:
3J 1(/c So Framatome ANP Environmental Laboratory 29 Research Drive Westborough, MA 01581-3913
TABLE OF CONTENTS Page INTRODUCTION.................................................
1 A.
Quality Control Program Scope................................................
1
- 1.
Inter-laboratory and Third Party................................................
1
- 2.
Intra-laboratory............................................... 2 B.
Quality Assurance Program (Internal and External Audits)................................ 2 II.
Performance Evaluation Criteria................................................
3 A.
Acceptance Criteria...............................................
3
- 1.
Internal Process Control Samples.................................3
- 2.
Backgrounds...........................................................................................5
- 3.
Blanks.................................
5
- 4.
NRC Resolution Criteria..................................
5
- 5.
DOE Evaluation Criteria..................................
5
- 6.
ANSI 13.30 Relative Bias Criteria for Bioassay..................................
6 B.
QC Investigation Criteria and Result Reporting...............................................
6
- 1.
QC Investigation Criteria...............................................
6
- 2.
Reporting of Analytical Results to Laboratory Customers............
.......... 7
- 3.
Self-Assessment Program...............................................
7 111. ANALYTICAL SERVICES QUALITY CONTROL SYNOPSIS........................................ 7 A.
Result Summary............................................
7
- 1.
Radiological Environmental Services Quality Control............................. 7
- 2.
Part 50/61 Quality Control...........................................
10
- 3.
Bioassay Quality Control...........................................
12 B.
Status of Condition Reports (CR)...........................................
12 C.
Status of Audits/Assessments...........................................
12
- 1.
Internal...............................................................................................;.. 12
- 2.
External................................................................................................. 13 IV.
UPDATED PROCEDURES ISSUED DURING JULY-DECEMBER 2004.................... 13 V.
REFERENCES....................................................
13 F:AADMIN\\CORREM\\EL 027-05
-ii-
TABLE OF CONTENTS (continued)
APPENDIX A INTER/INTRA-LABORATORY, ENVIRONMENTAL MONITORING: ANALYTICS, DOE, ERA AND NIST QUALITY CONTROL PROGRAM RESULTS APPENDIX B EFFLUENT MONITORING AND WASTE CHARACTERIZATION QUALITY CONTROL RESULTS (10CFR PART 50/61)
APPENDIX C BIOASSAY QUALITY CONTROL PROGRAM RESULTS ATTACHMENT I RESULTS OF THE BLIND DUPLICATE PROGRAM F:ADMINMCORRES\\EL 027-05
_jjj-
LIST OF TABLES
- 1.
Analytics Environmental Crosscheck Program Results by Framatome ANP Environmental Laboratory Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 2.
Framatome ANP Environmental Laboratory Analytics Environmental Cross-Check Program Performance Evaluation
- 3.
NIST Environmental Analysis Results by Framatome ANP Environmental Laboratory Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 4.
Summary of Framatome ANP Environmental Laboratory, National Institute of Standards and Technology (NIST), Traceability Results, July-December 2004
- 5.
Environmental Measurements Laboratory Quality Assessment Program
- 6.
Department of Energy Mixed Analyte Performance Evaluation Program (MAPEP-04-12)
- 7.
Environmental Resource Associates Proficiency Test Results Framatome ANP Environmental Laboratory
- 8.
Intra-laboratory Environmental Process Control Results by Framatome ANP Environmental Laboratory Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 9.
QC Charcoal Activity Screening Results
- 10.
Framatome ANP Environmental Laboratory, Environmental Intra-Laboratory and Inter-Laboratory Data Summary, Bias and Precision by Media, July-December 2004
- 11.
Framatome ANP Environmental Laboratory, Environmental Intra-Laboratory and Inter-Laboratory Data Summary, Bias and Precision by'Analysis Type, July-December 2004
- 12.
Environmental Bias and Precision by Year
- 13.
Analytics Radiochemistry Crosscheck Results by Framatome ANP Environmental Laboratory Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 14.
Framatome ANP Environmental Laboratory Analytics Radiochemistry Cross-Check Performance Evaluation
- 15.
NIST Part 50/61 Analysis Results Breakdown by Framatome ANP Environmental Laboratory, Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 16.
Summary of Framatome ANP Environmental Laboratory, National Institute of Standards and Technology (NIST), Part 50/61 Traceability Results, July-December 2004
- 17.
Intra-laboratory Part 50/61 Process Control Results Breakdown by Framatome ANP Environmental Laboratory, Acceptance Criteria, Media and Measurement Categories, July-December 2004 FAADMIN\\CORRE5\\EL 027-05
-iv-
LIST OF TABLES
- 18.
Part 50/61 Analysis Results Breakdown by Framatome ANP Environmental Laboratory, Acceptance Criteria, Media and Measurement Categories, July-December 2004
- 19.
Part 50/61 Bias and Precision by Year
- 20.
Bioassay Analysis Results Breakdown By Framatome ANP Environmental Laboratory Acceptance Criteria, Media, and Measurement Categories, July-December 2004
- 21.
Lawrence Livermore National Laboratory (LLNL) Bioassay Thyroid Radioiodine Intercomparison Project (TRIP)
- 22.
Condition Report (CR) Status, July-December 2004
- 23.
Updated Instrumentation Group/Analytical Services Section Procedures Issued During July-December 2004 FMADMIN\\CORRES\\EL 027-05
I.
INTRODUCTION This report covers the Quality Assurance (QA) Program for the Analytical Services function of the Framatome ANP Environmental Laboratory (E-LAB) for the second half (July-December) of 2004. Due to the broad scope of QC inter-comparison programs in which the E-LAB participates, the report consolidates wherever possible, text and results into three service categories: Radiological Environmental Monitoring, Part 50/61, and Bioassay.
This report includes:
intralaboratory QC results analyzed during the reporting period, interlaboratory QC results, analyzed prior to the reporting period, for which
'known values" were not previously available, and interlaboratory QC results, analyzed during the reporting period, for which
'known values" were available.
Any other inter-laboratory QC results will be included in the next semi-annual report.
Manual 100, Revision 8 (Reference 1) became effective on September 10, 2004. The text of this report reflects the latest revision of this manual, as do the trending graphs and any data evaluations performed after the effective date. Any data evaluations performed prior, however, were conducted in accordance with Manual 100, Revision 7.
A.
Quality Control Program Scope
- 1.
Inter-laboratory and Third Party The Framatome ANP Environmental Laboratory QC Program is designed to monitor the quality of analytical processing associated with environmental, bioassay, effluent (10CFR Part 50), and waste (IOCFR Part 61) sample analysis.
Inter-laboratory and third party quality control programs for environmental radioanalyses include: the Environmental Crosscheck Program, administered by Analytics, Inc., the National Institute of Standards and Technology (NIST) Measurement Assurance Program (MAP), the Environmental Resource Associates (ERA) Proficiency Test (PT)
Program, the Department of Energy (DOE) Mixed Analyte performance Evaluation Program (MAPEP).
The QAP program administered by the (DOE) Environmental Measurements Laboratory (EML) was suspended by the Department of Homeland Security following the results of QAP 60 (contained in the first half 2004 report). The MAPEP program is administered by the Radiological and Environmental Sciences Laboratory (RESL) and consists of four media (water, soil, vegetation, and air filter) submitted twice each year. The MAPEP samples are designed to evaluate the ability and quality of analytical facilities performing sample measurements that contain hazardous and radioactive (mixed) analytes. The ERA PT FAADMIN\\CORRESTEL 027-05 program consists of radionuclides in water submitted twice per year. This program is used to maintain certification with the National Environmental Laboratory Accreditation Program (NELAP). The certification is necessary to perform analysis for projects that must meet EPA regulations for the Clean Water Act (CWA), Resource Conservation &
Recovery Act (RCRA), or the Safe Drinking Water Act (SDWA).
Inter-laboratory and third party quality control for Part 50/61 radioanalyses, is provided by the Radiochemistry Crosscheck Program, administered by Analytics, Inc. and the NIST MAP.
- 2.
Intra-laboratory The internal Quality Control program is designed to include QC functions such as instrumentation checks (to insure proper instrument response),
blank samples (to which no analyte radioactivity has been added),
instrumentation backgrounds, duplicates, as well as overall staff qualification analyses and process controls. Both process control and qualification analyses samples seek to mimic the media type of those samples submitted for analysis by the various laboratory clients. These process controls (or process checks) are either actual samples submitted in duplicate in order to evaluate the precision of laboratory measurements, or blank samples which have been "spiked" with a known quantity of a radioisotope that is of interest to Laboratory clients. These QC samples, which represent either 'single" or 'double blind" unknowns, are intended to evaluate the entire radiochemical and radiometric process.
To provide a sense of direction and consistency in administering the quality control program, E-LAB has developed and follows an annual quality control and audit assessment schedule (Reference 2). The plan, which is approved on or before January 15th of each year and reviewed for adequacy at monthly LQARC meetings, describes the scheduled frequency and scope of Quality Assurance and Control actions considered necessary for an adequate program. The magnitude of the process control program combines both internal and external sources targeted at 5% of the routine sample analysis load.
B.
Quality Assurance Program (Internal and External Audits)
During each semi-annual reporting period at least one internal assessment is conducted in accordance with the pre-established E-LAB Quality Control and Audit Assessment Schedule. In addition, the Laboratory may be audited by prospective customers during a pre-contract audit, and/or by existing clients who wish to conduct periodic audits in accordance with their contractual arrangements. A National Environmental Laboratory Accreditation Program (NELAP) audit is performed every two years as part of maintaining certification to perform EPA-related analyses.
FMADMIN\\CORRES\\EL 027-05 II.
PERFORMANCE EVALUATION CRITERIA A.
Acceptance Criteria The E-LAB has adopted a QC acceptance protocol based upon two performance models:
For those inter-laboratory programs that already have established performance criteria (i.e., MAPEP, ERA, and TRIP), the Laboratory will utilize the criteria for the specific program.
For inter-laboratory or third party QC programs that have no preset acceptance criteria (e.g. the Analytics Crosscheck Programs, NIST MAP),
results will be evaluated in accordance with E-LAB internal acceptance criteria.
1.
Internal Process Control Samples Internal Process Control (PC) results are evaluated in accordance with two separate E-LAB acceptance criteria. A full discussion of the analytical services acceptance criteria can be found in Reference 1. The first criterion concerns bias, which is defined as the deviation of any one result from the known value. The second criterion concerns precision, which deals with the ability of the measurement to be faithfully replicated by comparison of an individual result with the mean of all results for a given sample set. Quality control deviations falling outside the Laboratory acceptance criteria are discussed in the appendices.
(a)
Bias For each analytical measurement tested, the bias is the percent deviation of the reported result relative to the expected value (value of the spike known by comparison with or derivation from a standard reference material). The percent deviation relative to the known is calculated as follows:
(H' ;HI '100 Hi where:
H= the value of the it measurement in a category being tested Hi = the actual quantity in the test sample as defined by the spike The Laboratory internal criterion for bias is that an analysis is considered in agreement if the value is within +/-15% of the known value. If this condition is not met, the two-sigma range about the analyzed value is established. If the known value falls within the specified range, the analysis is considered in agreement.
FHADMIN\\CORRES\\EL 027-0S Deviations from this general criterion, for specific radionuclides, are given in Tables 1 and 13 and Reference 1.
E-LAB acceptance criteria are applied when the sample concentration is 10 or more times the method MDC. Otherwise, the 'known value" and associated uncertainty are compared to the measured result and uncertainty using a two-tailed standard statistical test at the 95% confidence level.
(b)
Precision For a group of test measurements containing a given spiked level, the precision is the percent deviation of individual results relative to the mean reported measurement. At least two values are required for the determination of precision. The percent deviation relative to the mean reported measurement is calculated as follows:
(Hi' RH100 where:
H=
the reported measurement for the ith analytical measurement H = the mean analytical measurement Ft =
H(
n =
the number of samples in the test group The Laboratory criterion for precision is that an analysis is considered in agreement if the individual value is within +/-15% of the mean value. If this condition is not met, the two-sigma range about the analyzed value is established. If the mean value falls within the specified range, the analysis is considered in agreement. In the case of duplicate or replicate analyses where there is no "known" value, the two-sigma range is established for each duplicate analysis (three-sigma range for replicates) for each analysis. If the ranges overlap, the analyses are considered in agreement for precision.
Deviations from this general criterion, for specific radionuclides, are given in Tables 1 and 13 and Reference 1.
F:\\ADMIN\\CORRES\\EL 027-05 (c)
Mean Bias For each group of analytical measurements tested, the mean bias is the percent deviation of the mean reported result relative to the expected value. The mean percent deviation relative to the expected value is calculated as follows:
[((Hi)X 0
where:
H = the mean analytical measurement Hi = the actual quantity in the test sample as defined by the spike
.2.
Backgrounds As discussed in Reference 1, backgrounds represent the ambient signal response, recorded by measuring instruments, which is independent of radioactivity contributed by the radionuclides being measured in the sample. Backgrounds will not normally contain any three-sigma statistically positive activity of the target parameters. The background signal is subtracted from the sample's signal.
- 3.
Blanks Wherever possible equivalent media for preparing laboratory processing blanks will be used. Synthetic matrices may be used for bioassay if equivalency is proven.
- 4.
NRC Resolution Criteria Some Laboratory clients use the NRC Resolution Criteria to evaluate double blind Part 50 performance. NRC Resolution Criteria are based on an empirical relationship that combines prior experience and the accuracy needs of the program' As "Resolution" increases, the acceptability of one's measurement becomes more selective. Conversely, as "Resolution" decreases, agreement levels are widened to account for the increase in uncertainty.
- 5.
DOE Evaluation Criteria (a)
The Environmental Measurements Laboratory (EML) test program (DOEQAP) was cancelled by the Department of Energy in 2004.
A future test program may become available if deemed necessary by the Department of Homeland Security.
(b)
The Radiological & Environmental Sciences Laboratory (RESL) inter-comparison program, MAPEP, defines three levels of FAADMIN\\CORRE5\\EL 027-05 performance: Acceptable (flag = 'A"), Acceptable with Warning (flag = 'W"), and Not Acceptable (flag = "N"). Performance is considered acceptable for a mean with a bias *20% of the reference value for the analyte. Performance is acceptable with warning for a mean result bias of >20% but *30% of the reference value. If the bias is greater than 30% the results are deemed not acceptable.
- 6.
ANSI 13.30 Relative Bias Criteria for Bioassay The relative bias statistic is defined for the ith measurement in a category with respect to the expected value (value of the spike known by comparison with or derivation from a standard reference material) is defined as:
13 (Ai - Air)
Where:
A, = the value of the ith measurement in a category being tested A,, = the actual quantity in the test sample, as defined by the spike In order to avoid the expense of a large number of replicates at each radioactivity level in each category, the relative bias B, is calculated from the individual relative biases Bi and defined as I, (BN )
Br =
Where: N is the number of test samples measured by an individual service laboratory in a given test category.
For testing purposes Br shall be within -0.25 to +0.50 B.
QC Investigation Criteria and Result Reporting
- 1.
QC Investigation Criteria Summarized below are the investigation criteria applied to QC analyses that failed E-LAB bias criteria. The Condition Report process tracks investigation results.
(a)
No investigation is necessary when an individual QC result falls outside the QC performance criteria for bias.
(b)
Investigations shall be initiated when the mean of a QC process batch or the mean of three consecutive individual QC processes is outside the performance criterion for bias.
F:AADMIN\\CORRE5XEL 027-05 (c)
An investigation shall be initiated when the trending of at least 12 consecutive results for a given process indicates that the mean bias from the known is greater than 60% of the bias performance criterion.
- 2.
Reporting of Analytical Results to Laboratory Customers A similar set of guidelines was developed, applicable to reporting of results. The guidelines are as follows:
If an investigation is required for a process (normally after consecutive QC process check failures), and if the QC results requiring the investigation have a mean bias from the known of greater than +/- (applicable E-LAB bias criterion +5%) for environmental and bioassay processing and +/- (applicable E-LAB bias criterion +10%) for Part 50/61 processing, then the LQARC shall meet to determine the disposition of client results.
- 3.
Self-Assessment Program In accordance with Reference 1, E-LAB has established a Self-Assessment policy where all Laboratory staff members are strongly encouraged to continually evaluate laboratory activities for quality enhancements, cost savings, and time savings.
Ill.
ANALYTICAL SERVICES QUALITY CONTROL SYNOPSIS A.
Result Summary Two-year (2003-2004) trending graphs are provided in Appendices A-C of this report to give temporal perspective regarding possible trends or bias. In the event an analysis does not meet E-LAB performance criteria, the individual analysis sheet(s), in addition to a brief explanation, are included to augment the graph. It should be noted that DOE and ERA samples are evaluated against criteria specific to the DOE samples. Therefore, only sample results which fell in the "Warning" or Non-Agreement" categories will be addressed in the Appendices. If any questions arise regarding previous analyses, please refer to the semi-annual status report corresponding to the sample analysis date. In all cases an analysis sheet is available for each individual analysis to back-up the data, presented on the graph.
- 1.
Radiological Environmental Services Quality Control During this semi-annual reporting period, twenty-six nuclides associated with media types were analyzed by means of the Laboratory's internal process control, DOE, NIST, ERA and Analytics quality control programs.
Media types representative of client company analyses performed during this reporting period were selected. Presented below is a synopsis of the media types evaluated.
Air Filter Sediment/soil Charcoal (Air Iodine)
Water F:\\ADMIN\\CORRESMEL 027-05 Milk (a)
Analytics Environmental Cross Check Program During this semi-annual period the Analytics Cross Check Program provided 154 individual environmental analyses for bias and 154 for precision evaluation (Table 1). Of the 154 analyses evaluated for bias, 100% (154/154) of all results fell within E-LAB acceptance criteria. Of the 154 analyses evaluated for precision, 100% (1 54/154) came within E-LAB tolerance limits. Appendix A graphically summarizes the results by two-year trending graphs.
Table 2 provides a report of the Laboratory's participation in the Analytics' cross check program for the second and third quarters of 2004. Using the Laboratory's internal acceptance criteria as the basis of evaluation, all 53 of mean results came within agreement criteria.
Due to problems encountered during the dissolution steps of the E4185-162 Sr-89/90 filter for the second quarter 2004, a replacement Sr-90 filter from the MAPEP second half samples was included in the results table. The Sr-90 result was within the MAPEP acceptance criteria. An Analytics replacement Sr-89/90 filter, E4340-162, was successfully analyzed and is included in Table 2.
(b)
National Institute of Standards and Technology (NIST)
Measurement Assurance Program (MAP)
The E-LAB has been a participant in the Nuclear Energy Institute (NEI)/National Institute of Standards and Technology (NIST)
Measurements Assurance Program since June of 1987.
Continued participation is documented by dated Reports of Traceability issued for particular radionuclides, which indicate the deviation of the participant's reported value for a given measurement technique from that measured and certified by the NIST.
During this reporting period there were two NIST MAP samples received. The water sample consisted of 3 radionuclides and 36 measurements performed. The filter sample consisted of 5 radionuclides and 30 measurements performed. Detailed information on Environmental NIST MAP data is provided in Tables 3 and 4. All of the 66 measurements met the E-LAB acceptance criteria and 14 of 22 mean results met the administrative limit of +/-5%. NIST traceability certificates will be issued for all detector/nuclide combinations.
FMADMIN\\CORRES\\EL 027-05 (c)
Summary of Participation in the Department of Energy (DOE)
Monitoring Programs During this semi-annual reporting period, a combination of three different media types and twelve different radionuclides were analyzed for the semi-annual Mixed Analyte Performance Evaluation Program (MAPEP-04-12, Table 6). All but one of the 23 mean results were evaluated as "Acceptable." Two of the 23 tests were acceptable false positive tests. The Pu-238 in water test fell in the uWarning" range with a bias of -20.6% (with an acceptance limit of 20%). CR 04-17 was initiated to investigate the failure.
(d)
Environmental Resource Associates (ERA) Proficiency Test (PT)
Program During this semi-annual period, a total of 9 mean results (n=3) were evaluated by ERA. Using the evaluation criteria set by NELAP, 88.9% (8/9) of the radionuclides were in 'Agreement."
The single failure, Co-60 in water, was caused by a data entry error in the ERA internet database. The analyzed result was well within the acceptance criteria. Appendix A graphically summarized the results by two-year trending graphs. Table 7 provides a report of the Laboratory's participation in the PT program.
The Framatome ANP Environmental Laboratory (Lab ID# 11823) maintained NELAP accreditation from the New York State Department of Health through the Environmental Laboratory Approval Program for the following methods for both potable and non-potable waters:
Gross Alpha, Method EPA 900.0 Gross Beta, Method EPA 900.0 Iodine-131, Method ASTM D4785-88 Photon Emitters, Method EPA 901.1 Radioactive Cesium, Method EPA 901.1 Tritium, Method EPA 906.0 (e)
Intra-Laboratory Process Control Program The Environmental Laboratory internal process control program evaluated 452 individual analyses for bias and 219 analyses for precision. Trending graphs associated with the performance results for this program are given in Appendix A, and the results are summarized in Table 8.
Of the 452 internal process control analyses evaluated for bias, 99.1 % met Laboratory acceptance criteria. Also, 100% of the 219 results for precision were found to be acceptable.
F:AADMIN\\CORREM\\EL 027-05
_9 _
Table 9 lists QC samples used to qualitatively screen calibrated geometry air charcoals for activity above the Minimum Detectable Concentration (MDC). All 78 QC charcoals evaluated during this semi-annual period reported positive activity as expected. The bias data for each individual measurement is presented in Table 9.
(f)
Analytical Blanks During this semi-annual reporting period, none of the 163 environmental analytical blanks analyzed reported positive activity, greater than three (3) times the standard deviation.
(g)
Instrumentation Backgrounds None of the instrumentation backgrounds processed between July-December 2004 reported activity that was above the three standard deviation investigation level.
(h)
Blind Duplicate Results Blind duplicate results for 2004 are presented in Attachment 1.
Based upon the summary evaluation, 99.6% of all paired measurements met the acceptance criteria. This data is not included in the summary tables (Tables 10-12).
(i)
Overall Data Summary for the Reporting Period July-December 2004 The compilation of intra-and inter-laboratory comparison data by analyzed matrix for this reporting period is summarized in Table 10. Table 11 presents the same data grouped according to analysis type. In either case, the cumulative bias for the three programs evaluated to internal E-LAB performance criteria shows 99.4% of the 672 individual results were observed to fall within the E-LAB bias acceptance criteria, while 100% of the 439 analyses passed the acceptance criteria for precision.
(j)
Summary of Environmental Quality Control Results by Year The historical summary of the E-LAB process control program performance for the environmental monitoring function is provided in Table 12. For the second half of 2004, 99.4% of the analyses fell within the E-LAB acceptance criteria for bias as compared to a historical percentage of 96.7. Similarly, 100% of the analyses evaluated for precision met the E-LAB acceptance criteria as compared to 99.4% of analyses for the 27-year operating history.
- 2.
Part 50/61 Quality Control During this semi-annual reporting period, twenty-one nuclides were analyzed by means of the Laboratory's internal process control, National FAADMIN\\CORREM\\EL 027-05 Institute for Standards and Technology Measurement Assurance Program (NIST MAP) measurements of Part 50/61 radionuclides, and the Analytics Radiochemistry Crosscheck Program.
(a)
Analytics Radiochemistry Cross Check Program During this semi-annual period the Analytics Cross Check Program provided 18 individual analyses to be evaluated for bias and precision (Table 13). Of the 18 analyses, 100% fell within the E-LAB acceptance criteria for bias and 100% for precision..
Appendix B graphically summarizes the results by two-year trending graphs.
Table 14 provides a report of the Laboratory's participation in the Analytics' cross check program for the second half of 2004. Using the Laboratory's internal acceptance criteria as the basis of evaluation, all 6 results passed the agreement criteria.
(b)
NIST Measurement Assurance Program (MAP)
During this reporting period there were two NIST MAP samples received. The water sample consisted of 3 radionuclides and 36 measurements performed. The filter sample consisted of 5 radionuclides and 30 measurements performed. Detailed information on NIST MAP data is provided in Tables 15 and 16.
All of the 66 measurements met the E-LAB acceptance criteria and 14 of 22 mean results met the administrative limit of +/-5%.
NIST traceability certificates will be issued for all detector/nuclide combinations.
(c)
Intra-Laboratory Process Check Program There were 91 internal Laboratory QC process control analyses evaluated for bias and 78 for precision during the second half of 2004 in the Part 50/61 area. Of these, 91.2% (83/91) met the E-LAB acceptance criteria for bias. A total of 100% (78/78) Part 50/61 process control samples met E-LAB acceptance criteria for precision (Table 17).
(d)
Analytical Blanks During this semi-annual reporting period, none of the 160 Part 50/61 analytical blanks analyzed reported positive activity greater than three (3) times the standard deviation.
(e)
Instrumentation Backgrounds One hundred percent (100%) of the instrumentation backgrounds processed between July-December 2004 reported activity that was below the three standard deviation investigation level.
FMADMIN\\CORRES\\EL 027-05 (f)
Overall Data Summary for the Reporting Period July-December 2004 The compilation of intra-and inter-laboratory comparison data by analyzed matrix for this reporting period is summarized in Table 18. The cumulative bias shows 95.4% (167/175) of the individual results fell within E-LAB acceptance criteria for bias. A total of 100% (162/162) of the results met Laboratory precision criteria.
(g)
Summary of Part 50/61 Quality Control Results by Year The historical E-LAB summary of process control performance for the Part 50/61 monitoring program is provided in Table 19. For the calendar year 2004, 95.0% of the QC analyses fell within E-LAB acceptance criteria for bias as compared to the sixteen year historical percentage of 94.0. For precision, 100% of the results met the precision acceptance criteria as compared to 99.2%
historically.
- 3.
Bioassay Quality Control There were no bioassay QC analyses performed during this semi-annual period as indicated in Table 20.
For the past several years, the E-LAB has participated in the Lawrence Livermore National Laboratory (LLNL) Thyroid Radioiodine Intercomparison Project (TRIP). This program allows laboratories and facilities to self-assess their performance for in-vivo measurements of radioiodine isotopes in the thyroid. The LLNL established the intercomparison project to provide participating facilities with an independent means of evaluating their thyroid radio-iodine measurement using the IAEA/ANSI thyroid calibration neck phantom and well characterized NIST-traceable isotopes for 1-125 and 1-131. As shown in Table 21, TRIP 0504-52 was conducted during this semi-annual period.
The 1-125 and 1-131 biases were well within the acceptance criteria.
B.
Status of Condition Reports (CR)
Table 22 provides a synopsis of CR activity for sample processing during the second half of 2004. Fifteen items were closed and fifteen were opened during this reporting period. As of December 31, 2004, a total of three CRs remain open, none of which are older than 6 months.
C.
Status of Audits/Assessments
- 1.
Internal Corporate QA Audit 04-29 Framatome ANP Quality Assurance audited the E-LAB during the period December 13-21, 2004.. The audit scope included verification of FAADMIN\\CORRE5\\EL 027-05 compliance with the applicable quality requirements of the Laboratory QA, Safety, and Condition Report manuals. A total of five findings were issued and are summarized as CRs 04-20 through 04-24 in Table 22.
Three of these CRs have been closed and the remaining two are pending closure following procedure revisions to enhance the noted areas. The auditor concluded that "... individuals in the Marlborough and Westborough offices are effectively implementing the quality requirements..."
2.'
External There were no external audits conducted during this semi-annual period.
IV.
UPDATED PROCEDURES ISSUED DURING JULY-DECEMBER 2004 A list of Analytical Services Section procedures, which were updated during this semi-annual period, is included in Table 23.
V.
REFERENCES
- 1.
Framatome ANP Environmental Laboratory Manual 100 'Laboratory Quality Assurance Plan", Revision 8, September 10, 2004.
- 2.
Framatome ANP Environmental Laboratory 2004 Quality Control and Audit Assessment Schedule.
- 3.
Framatome ANP Quality Assurance Audit Report, File T5.4, Audit Number 04-29, dated January 20, 2005.
F:AADMIN\\CORRE5\\EL 027-05 TABLE I ANALYTICS ENVIRONMENTAL CROSSCHECK PROGRAM RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA, AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 4
1 2
3 4
I. Air Particulate Alpha 5
1 0
0 6
00 0
Beta 6
0 0
0 6
0 0
0 Gamma 14 11 2
0 26 1
0 0
Sr-89 1
0 0 0
0 0
0 0
0 Sr-90 1
0 0
0 0
02 0
0
- 11. Milk X
Gamma 44 11 53 4
3 0
0 0
5 0
0 0
Sr-89 2
1 0
0 2
1 0
0 Sr-90 2
1 0
0 3
0 0
0 III. Water Alpha 3
0 0
0 3
0 0
0 Beta 1
2 0
0 2
1 0
0 Gamma 21 7
2 0
26 3
1 0
H-3 3
0 0
0 3
0 0
1 0
1 2
0 0
Sr-89 Sr-90 Total Number in Range:
107 36 11 0
136 14 4
0 Percentage of Total Processed:
69.5 23.4 7.1 0.0 88.3 9.1 2.6 0.0 Sum of Analyses:
154 154 (1) Percent Bias by Deviation Category as noted in Table 1, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 1. Footnote (2)
- Total may not equal 100 due to rounding FAADMIN\\CORRES\\EL 027-05
-Al-
TABLE 1 ENVIRONMENTAL PROCESS CONTROL ANALYSIS RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 (Continued)
(1)
Percent Bias by Deviation Category 1 = >0 and <5 2 = >5 and <10 3 = >10 and <15 (or within 2 sigma of known, see Reference 1)
For Gross Alpha and Beta In water 3 = >10 and <25 (or within 2 sigma of known)
For Sr-89/90 mixtures 3 = >10 and <25 (or within 2 sigma of known)
For Alpha Spectrometry*,
3 = >10 and <20 (or within 2 sigma of known)
For Uranium-Total, Pu-241, Zn-65 on an air filter 3 = >10 and <20 (or within 2 sigma of known) 4 = Outside criteria (2)
Percent Precision by Deviation Category I =>0 and <5 2=>5and<10 3 = >10 and <15 (or within 2 sigma of mean, see Reference 1). Exceptions as above.
4 = Outside criteria Isotopic Uranium (U-234, 235, 238)
Isotopic Thorium (Th-230, 232)
Np-237 Am-241/Cm-242, 243/244 Pu-alpha (Pu-238, 239, 240)
Ra-226 Total may not equal 100 due to rounding.
FAADMIN\\CORRES\\EL 027-05
-A2-
TABLE 2 FRAMATOME ANP ENVIRONMENTAL LABORATORY ANALYTICS ENVIRONMENTAL CROSS CHECK PROGRAM PERFORMANCE EVALUATION Ratio Sample Quarter/
Sample Reported Known E-LAB/
Number Year Media Nuclide Units Value Value Analytics Evaluation E4182-162 2nd/04 Water H-3 pCi/L 11680 11900 0.98 Agreement E4183-162 2nd/04 Filter Gross Alpha pCi 46.8 48.8 0.96 Agreement E4183-162 2nd/04 Filter Gross Beta pCi 156 160 0.98 Agreement E4184A-162 2nd/04 Filter Ce-141 pCi 86 88.3 0.97 Agreement E4184A-162 2nd/04 Filter Cr-51 pCi 127 128 0.99 Agreement E4184A-162 2nd/04 Filter Cs-1 34 pC!
54 56.9 0.94 Agreement E4184A-162 2nd/04 Filter Cs-137 pCi 90 87.8 1.03 Agreement E4184A-162 2nd/04 Filter Co-58 Pci 27 26 1.03 Aqreement E4184A-162 2nd/04 Filter Mn-54 pCi 42 39.7 1.06 Agreement E4184A-162 2nd/04 Filter Fe-59 pCi 27 25.1 1.09 Agreement E4184A-162 2nd/04 Filter Zn-65 pCi 62 56 1.11 Agreement E4184A-162 2nd/04 Filter Co-60 pCi 92 96.8 0.95 Agreement E4185-162 2nd/04 Filter Sr-89 pCi (1)
E4185-162 2nd/04 Filter Sr-90 pCi (1)
E4186-162 2nd/04 Milk 1-131 pCi/L 55 58.2 0.95 Agreement E4186-162 2nd/04 Milk I-131 LL pCi/L 59 58.2 1.01 Agreement E4186-162 2nd/04 Milk Ce-141 p0i/L 165 157 1.06 Agreement E4186-162 2nd/04 Milk Cr-51 pCi/L 241 228 1.06 Agreement E4186-162 2nd/04.
Milk Cs-1 34 pCi/L 99 101 0.98 Agreement E4186-162 2nd/04 Milk Cs-137 pCi/L 157 156 1.01 Agreement E4186-162 2nd/04 Milk Co-58 pCi/L 46 46.2 1.00 Agreement E4186-162 2nd/04 Milk Mn-54 pCi/L 73 70.5 1.04 Agreement E4186-162 2nd/04 Milk Fe-59 pCi/L 48 44.5 1.08 Agreement E4186-162 2nd/04 Milk Zn-65 pCi/L 100 99.3 1.01 Agreement E4186-162 2nd/04 Milk Co-60 pCi/L 175 172 1.02 Agreement RdF12 May-04 Filter Sr-90 pCi 20.3 22.4 0.91 Agreement (2)
(1) - Problems encountered in filter dissolution, filter re-ordered.
(2) - Replacement filter for first half 2004 from DOE MAPEP F:\\ADMINMCORRESXEL 027-05
-A3-
TABLE 2 (Continued)
FRAMATOME ANP ENVIRONMENTAL LABORATORY ANALYTICS RADIOLOGICAL ENVIRONMENTAL CROSS-CHECK PERFORMANCE EVALUATION Ratio Sample Quarter/
Sample Reported Known E-LABI Number Year Media Nuclide Units Value Value Analytics Evaluation E4269-162 3rd12004 Water Gross Alpha pCi/L 41.3 42.7 0.97 Agreement E4269-162 3rd/2004 Water Gross Beta pCiIL 214 225 0.95 Agreement E4270-162 3rd/2004 Water 1-1 31 LL pCi/L 67.8 70.8 0.96 Agreement E4270-162 3rd/2004 Water 1-131 pCVL 70.5 70.8 1.00 Agreement E4270-162 3rd/2004 Water Ce-141 pCVL 258 250 1.03 Agreement E4270-162 3rd/2004 Water Cr-51 pCi/L 230 223 1.03 Agreement E4270-162 3rd/2004 Water Cs-1 34 pCi/L 93.4 96.4 0.97 Agreement E4270-162 3rd/2004 Water Cs-137 pCi/L 217 215 1.01 Agreement E4270-162 3rd/2004 Water Co-58 pCi/L 93.4 94.6 0.99 Agreement E4270-162 3rd/2004 Water Mn-54 pCi/L 181 181 1.00 Agreement E4270-162 3rd/2004 Water Fe-59 pCi/L 95.2 91.6 1.04 Agreement E4270-162 3rd/2004 Water Zn-65 pCUL 180 178 1.01 Agreement E4270-162 3rd/2004 Water Co-60 pCiUL 126 125 1.01 Agreement E4271-162 3rd/2004 Filter Gross Alpha pCi 38.3 36.8 1.04 Agreement E4271-162 3rd/2004 Filter Gross Beta pCi 191 194 0.98 Agreement E4272-162 3rd/2004 Milk 1-131 LL pCi/L 79.4 83.5 0.95 Agreement E4272-162 3rd/2004 Milk 1-131 pCiUL 81.1 83.5 0.97 Agreement E4272-162 3rdl2004 Milk Ce-141 pCi/L 240 235 1.02 Agreement E4272-162 3rd/2004 Milk Cr-51 pCUL 214 210 1.02 Agreement E4272-162 3rd/2004 Milk Cs-1 34 pCiUL 89.5 90.6 0.99 Agreement E4272-162 3rd/2004 Milk Cs-137 pCUL 204 202 1.01 Agreement E4272-162 3rd/2004 Milk Co-58 pCiQL 90.9 89 1.02 Agreement E4272-162 3rd/2004 Milk Mn-54 pCiUL 173 171 1.01 Agreement E4272-162 3rd/2004 Milk Fe-59 pCUL 91.3 86.1 1.06 Agreement E4272-162 3rd/2004 Milk Zn-65 pCi/L 169 167 1.01 Agreement E4272-162 3rd/2004 Milk Co-60 pCiUL 116 118 0.98 Agreement E4273-162 3rd/2004 Milk Sr-89 pCi/L 99.2 102 0.97 Agreement E4273-162 3rd/2004 Milk Sr-90 pCVL 23.4 24.5 0.96 Agreement E4340-162 3rd/2004' Filter Sr-89 pCUL 151 152 1.00 Agreement E4340-162 3rd/2004' Filter Sr-90 pCUL 53.5 58.8 0.91 Agreement
- Replacement filter for lost 2nd quarter filter.
FAADMIN\\CORRES\\EL 027-05
TABLE 3 NIST MAP ANALYSIS RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA, AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 4
1 2
3 4
I. Water I
Gamma 15 17 4
0 36 0
0 0
II. Filter I
I Gamma 26 4
0 0
30 0
0 0
Total Number in Range:
41 21 4
0 66 0
0 0
Percentage of Total Processed:
62.1 31.8 6.1 0.0 100.0 0.0 0.0 0.0 Sum of Analyses:
66 66 (1) Percent Bias by Deviation Category as noted in Table 1, Footnote (1)-
(2) Percent Precision by Deviation Category as noted in Table 1, Footnote (2)
- Total may not equal 100 due to rounding F:AADMIN\\CORRES\\EL 027-05
-A5-
TABLE 4
SUMMARY
OF FRAMATOME ANP ENVIRONMENTAL LABORATORY NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY (NIST)
TRACEABILITY RESULTS JULY-DECEMBER, 2004 NIST Reference E-LAB Mean Percent Standard Date of Measurement Deviation From Number Standard Radionuclide Matrix Technique NIST 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy Env. #2
-6.62 1680-5 27-Apr-04 Cd-I 09 Liquid Gamma Spectroscopy Env. #2
-7.88 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy Env. #2
-9.30 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy #2
-5.04 1680-5 27-Apr-04 Cd-109 Liquid Gamma Spectroscopy #2
-10.67 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy #2
-8.75 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy #4
-0.88 1680-5 27-Apr-04 Cd-I 09 Liquid Gamma Spectroscopy #4
-3.85 1680-5 27-Apr-04 AC-241 Liquid Gamma Spectroscopy #4
-3.02 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy #5
-2.86 1680-5 27-Apr-04 Cd-109 Liquid Gamma Spectroscopy #5
-6.92 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy #5
-4.57 1686-8 24-Jun-04 Co-57 Filter Gamma Spectroscopy #2
-0.16 1686-8 24-Jun-04 Co-60 Filter Gamma Spectroscopy #2
-0.13 1686-8 24-Jun-04 Cd-I 09 Filter Gamma Spectroscopy #2
-3.98 1686-8 24-Jun-04 Cs-1 34 Filter Gamma Spectroscopy#2
-4.34 1686-8 24-Jun-04 Am-241 Filter Gamma Spectroscopy #2
-1.44 1686-8 24-Jun-04 Co-57 Filter Gamma Spectroscopy #4
-1.30 1686-8 24-Jun-04 Co-60 Filter Gamma Spectroscopy #4 0.74 1686-8 24-Jun'04 Cd-I 09 Filter Gamma Spectroscopy #4
-6.05 1686-8 24-Jun-04 Cs-I 34 Filter Gamma Spectroscopy #4
-4.16 1686-8 24-Jun-04 Am-241 Filter Gamma Spectroscopy #4
-1.50 Data on NIST MAP program is repeated in Table 16 for Part 50/61 QC data.
F:\\ADMIN\\CORRES\\EL 027-05
-A6-
TABLE 5 ENVIRONMENTAL MEASUREMENTS LABORATORY QUALITY ASSESSMENT PROGRAM REPORTED EML REPORTED MATRIX/
RADIO-MEAN VALUE REPORTED VALUE EML TO KNOWN UNITS NUCLIDE BqIUnits ERROR Bq/Unlts ERROR RATIO EVALUATION EML has notified the industry that QAP 60 (March 2004) was the final set of samples to be issued. Further information may be found on the EML website, URL http://www.eml.doe.gov/qap/
F:AADMIN\\CORRES\\EL 027-05
-A7-
TABLE 6 DEPARTMENT OF ENERGY MIXED ANALYTE PERFORMANCE EVALUATION PROGRAM (MAPEP-04-12)
MATRIX/
RADIO-E-LAB MAPEP BIAS UNITS NUCLIDE MEAN VALUE VALUE Evaluation Filter (Bq total)
Sr-90 0.75 0.83
-9.6 Agreement Soil (Bqlkg)
Am-241 59.5 67
-11.2 Agreement Soil (Bqlkg)
Cs-1 34 455 414 9.9 Agreement Soil (Bqlkg)
Cs-1 37 893 836 6.8 Agreement Soil (Bqgkg)
Co-57 420 400 5.0 Agreement Soil (Bq/kg)
Co-60 567 518 9.5 Agreement Soil (Bqlkg)
Mn-54 534 485 10.1 Agreement Soil (Bqgkg)
Pu-238 38.33 35.4 8.3 Agreement Soil (Bq/kg)
Pu-239/240 41.66 41.8
-0.3 Agreement Soil (Bq/kg)
K-40 666 604 10.3 Agreement Soil (Bqgkg)
Sr-90 2.3+/-1.2 False Positive Test N/A Agreement Soil (Bq/kg)
Zn-65 781 699 11.7 Agreement Wate (Bq/L Am-241 0.5202 0.59
-11.8 Agreement Water (Bq/L)
Cs-1 34 197 208
-5.3 Agreement Water (Bq/L)
Cs-1 37 232 250
-7.2 Agreement Water (Bq/L)
Co-57 170.6 185
-7.8 Agreement Water (Bq/L)
Co-60 157.4 163
-3.4 Agreement Water (Bq/L)
H-3 87 82.9 4.9 Agreement Water (Bq/L)
Mn-54 257 267
-3.7 Agreement Water (Bq/L)
Pu-238 0.984 1.27
-20.6 Warning*
Water (Bq/L)
Pu-239/240 0.0070+/-0.0048 False Positive Test N/A Agreement Water (Bq/L)
Tc-99 10.66 10.4 2.5 Agreement Water (Bq/L)
Zn-65 207 208
-0.5 Agreement
- CR 04-17 Issued for Warning result for Pu-238. See Table 22 For details F:AADMIN\\CORRES\\EL 027-05
-A8-
TABLE 7 ENVIRONMENTAL RESOURCE ASSOCIATES PROFICIENCY TEST RESULTS FRAMATOME ANP ENVIRONMENTAL LABORATORY ERA REPORTED ERA ERA ERA LOT #l MATRIX RADIO-MEAN VALUE VALUE CONTROL WARNING REF. DATE UNITS NUCLIDE pCIIL pCIIL LIMITS LIMITS EVALUATION RAD-59 November 2004 Water pCi/L Gross Alpha 27.7 31.7 18.045.4 22.5-40.9 Agreement RAD-59 November 2004 Water pCiIL Gross Beta 32.9 36.3 27.645.0 30.5-42.1 Agreement RAD-59 November 2004 Water pCi/L Tritium 21300 20700 17100-24300 18300-23100 Agreement RAD-59 November 2004 Water pCi/L Ba-133 76.3 78.4 64.8-92.0 69.3-87.5 Agreement RAD-59 November 2004 Water pCi/L Cs-134 42.4 42.9 34.2-51.6 37.1-48.7 Agreement RAD-59 November 2004 Water pCiIL Cs-137 61.2 60.1 51.4-68.8 54.3-65.9 Agreement RAD-59 November 2004 Water pCi/L Co-60 116 11.7 3.04-20.4 5.93-17.5 (1)
RAD-59 November 2004 Water pCi/L Zn-65 52 50.9 42.1-59.7 45.0-56.8 Agreement RAD-59 November 2004 Water pCi/L 1-131 20.2 22.1 16.9-27.3 18.6-25.6 Agreement (1) - Analyzed value of 11.6 pCiIL was entered into ERA database as 116 pC/L.
F3\\ADMIN\\CORRES\\EL 027-05
-A9-
TABLE 8 INTRA-LABORATORY ENVIRONMENTAL PROCESS CONTROL RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA, AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2), (3) 1 2
3 4
1 2
3 4
I. Air Particulate Beta 112 8
0 0
0 0
0 0
Gamma
- 11. Air Charcoal Gamma-Quantitative 4
0 0
0 0
0 0
0 Gamma - Screening 58 14 6
0 0
0 0
0 Ill. Milk Gamma 6
l
_0
_0 0
_9 l
_0
_0_
l 0
l l
l Sr-89 7
1 I
I I
I Sr-90 l
l l
l l
l IV. Water Am-241 1
8 5
0 4
6 4
0 C-14 4
4 4
0 0
0 12 0
Fe-55 9
5 0
0 0
0 14 0
Gross Alpha 6
10 13 0
0 0
16 0
Gross Beta 7
7 17 4
4 6
6 0
Gamma 23 5
0 0
0 0
28 0
1 0
9 3
1 0
Ni-63 11 2
1 0
0 0
14 0
Pu-238 6
6 2
0 0
0 14 0
Pu-241 6
6 2
0 0
2 12 0
Sr-90 6
1 9
0 0
0 16 0
Tritium 19 3
3 0
7 2
14 0
Tc-99 9
4 3
0 0
0 16 0
Total Number 296 86 66 4
33 19 167 0
in Range:
Percentage of 65.5 19.0 14.6 0.9 15.1 8.7 76.3 0.0 Total Processed:
-07 Sum of Analyses:
452 219 (1) Percent Bias by Deviation Category as noted in Table 1, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 1, Footnote (2)
(3) Most Precision data generated from non-positive client samples for specific contractual evaluation
- Total may not equal 100 due to rounding F:ADMIN\\CORRES\\EL 027-05
-A10-
TABLE 9 QC CHARCOAL ACTIVITY SCREENING RESULTS SPIKE FILTER ANALYSIS ACT.
NUMBER LSN TYPE DATE REPORTED
% BIAS 68474162-C L7638-01 SAIC-1 1-Jul-04 YES 4.09 L7670-01 SAIC-1 7-Jul-04 YES 1.39 L7690-01 SAIC-1 14-Jul-04 YES 0.86 L7761-01 SAIC-1 23-Jul-04 YES 1.81 L7798-01 SAIC-1 28-Jul-04 YES' 1.43 L7836-01 SAIC-1 2-Aug-04 YES 1.58 68474162-E L7638-03 SAIC-2 1-Jul-04 YES 8.53 L7670-03 SAIC-2 7-Jul-04 YES 1.37 L7690-03 SAIC-2 14-Jul-04 YES 11.95 L7761-03 SAIC-2 23-Jul-04 YES 11.93 L7798-03 SAIC-2 28-Jul-04 YES 12.05 L7836-03 SAIC-2 2-Aug-04 YES 5.23 68474162-D L7638-02 SAWC 1-Jug-04 YES
-1.94 L7638-02 SAWC 7-JuA-04 YES
-2.37 L7690-02 SAWC 13-Jug-04 YES 0.17 L7761-02 SAWC 22-Jug-04 YES
-1.01 L7798-02 SA2C 28-JuS-04 YES
-3.83 L7836-02 SA2C 2-Aug-04 YES
-3.31 68474162-K L7874-01 SAIC-1 13-Aug-04 YES 2.27 L7907-01 SAIC-1 19-Aug-04 YES 3.05 L7935-01 SAIC-1 23-Aug-04 YES 4.05 L7978-01 SAIC-1 30-Aug-04 YES 2.18 L8016-01 SAIC-1 8-Sep-04 YES 2.04 L8041 -01 SAIC-1 13-Sep-04 YES 3.82 68474162-L L7874-02 SAl2 13-Aug-04 YES
-4.58 L7907-02 SAW2 19-Aug-04 YES
-2.31 L7935-02 SAW2 23-Aug-04 YES
-0.55 L7978-02 SAC2 30-Aug-04 YES
-1.04 L8016-02 SAW2 8-Sep-04 YES
-0.14 L8041-02 SA2C 13-Sep-04 YES
-3.18 68474162-M L7874-03 SAIC-2 12-Aug-04 YES 2.21-L7907-03 SAIC-2 19-Aug-04 YES 4.40 L7935-03 SAIC-2 23-Aug-04 YES 8.74 L7978-03 SAIC-2 30-Aug-04 YES 7.27 L8016-03 SAIC-2 8-Sep-04 YES 10.21 L8041 -03 SAIC-2 13-Sep-04 YES 8.80 FAADMIN\\CORRES\\EL 027-05
-All-
TABLE 9 (continued)
QC CHARCOAL ACTIVITY SCREENING RESULTS SPIKE FILTER ANALYSIS ACT.
NUMBER LSN TYPE DATE REPORTED
% BIAS 69182162-A L8082-01 SAIC-1 20-Sep-04 YES
-0.04 L8133-01 SAIC-1 29-Sep-04 YES
-1.27 L8171-01 SAIC-1 4-Oct-04 YES
-3.53 L8214-01 SAIC-1 12-Oct-04 YES
-3.57 L8246-01 SAIC-1 19-Oct-04 YES
-7.69 L8298-01 SAIC-1 27-Oct-04 YES
-7.96 69182162-B L8082-02 SA2C 20-Sep-04 YES 1.70 L8133-02 SA2C 29-Sep-04 YES 0.91 L8171-02 SA2C 4-Oct-04 YES 1.62 L8214-02 SA2C 12-Oct-04 YES 2.04 L8246-02 SA2C 19-Oct-04 YES
-4.42 L8298-02 SA2C 27-Oct-04 YES
-0.66 69182162-C L8082-03 SAIC-2 20-Sep-04 YES 3.61 L8133-03 SAIC-2 29-Sep-04 YES 1.61 L8171-03 SAIC-2 4-Oct-04 YES 4.27 L8214-03 SAIC-2 12-Oct-04 YES 2.95 L8246-03 SAIC-2 19-Oct-04 YES 12.03 L8298-03 SAIC-2 27-Oct-04 YES 4.09 69182162-J L8365-01 SAIC-1 2-Nov-04 YES 1.64 L8403-01 SAIC-1 9-Nov-04 YES 1.92 L8441 -01 SAIC-1 15-Nov-04 YES 1.85 L8471-01 SAIC-1 23-Nov-04 YES 0.23 L8502-01 SAIC-1 30-Nov-04 YES 1.84 L8530-01 SAIC-1 6-Dec-04 YES 2.79 69182162-K L8365-03 SA2C 2-Nov-04 YES
-5.37 L8403-03 SA2C 9-Nov-04 YES
-3.81 L8441-03 SA2C 15-Nov-04 YES
-4.45 L8471-03 SAW2 23-Nov-04 YES
-4.37 L8502-03 SA2C 2-Dec-04 YES
-3.29 L8530-03 SA2C 7-Dec-04 YES
.- 5.76 69182162-L -L8365-02 SAIC-2 2-Nov-04 YES 5.56 L8403-02 SAIC-2 9-Nov-04 YES 8.33 L8441-02 SAIC-2 15-Nov-04 YES 7.96 L8471-02 SAIC-2 23-Nov-04 YES 8.98 L8503-02 SAIC-2 30-Nov-04 YES 10.42 L8530-02 SAIC-2 7-Dec-04 YES 8.50 F:V'ADMIN\\C0RRES\\EL 027-05 A2
-A12-
TABLE 9 (continued)
QC CHARCOAL ACTIVITY SCREENING RESULTS SPIKE FILTER ANALYSIS ACT.
NUMBER LSN TYPE DATE REPORTED
% BIAS 69484162-D L8561-01 SAIC-1 14-Dec-04 YES
-0.77 L8599-01 SAIC-1 22-Dec-04 YES 2.96 69484162-E L8561-03 SA2C 14-Dec-04 YES 0.28 L8599-03 SA2C 21-Dec-04 YES 0.83 69484162-F L8561-02 SAIC-2 14-Dec-04 YES 3.40 L8599-02 SAIC-2 22-Dec-04 YES 3.36 F:iADMIN\\CORRES\\EL 027-05
-A13-
TABLE 10 FRAMATOME ANP ENVIRONMENTAL LABORATORY ENVIRONMENTAL INTRA-LABORATORY AND INTER-LABORATORY DATA
SUMMARY
BIAS AND PRECISION BY MEDIA JUNE-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2), (3) 1 2
3 4
1 2
3 4
I. Air Filter Gross Alpha 5
1 0
0 6
0 0
0 Gross Beta 118 8
0 0
6 j
0 0
0 Gamma 40 15 2
0 56 1
0 0
Sr-89 0
0 0
0
° 0
0 0
Sr-90 I
0 1
0 0
2 0
0 il. Charcoal Gamma-Quantitative 4
l 0
0 0
0 0
0 0
Gamma-Screening 58 14 6
0 0
0 0
0 Ill. Milk Gamma 50 11 5
0 62 T
4 3
0 0
1 0 0
0 Sr-89 2
1 0
0 2
1 0
0 Sr-90 2
1 0
0 3
0 0
0 IV. Soll/Sediment Am-241 0
1 0 0
0 0
0 0
1 0
Gamma 0
0 0
0 0
0 0
0 V. Water Am-241 1
8 5
0 4
6 4
0 C-14 4
4 4
0 0
0 12 0
Fe-55 9
5 0
0 0
0 14 0
Gross Alpha 9
10 13 0
3 0
16 0
Gross Beta 8
9 17 4
6 7
6 0
Gamma 59 29 6
X 0
62 3
29 0
2 0
10 5
1 0
NI-63 11 2
1 0
0 0
14 0
Pu-238 6
6 2
0 0
0 14 0
Pu-241 6
6 2
0 0
2 12 0
Sr-89 0
0 0
0 0
0 0
0 Sr-90 6
1 9
0 0
0 16 0
Tritium 22 3
3 0
10 2
14 0
Tc-99 9
4 3
0 0
0 16 0
Total Number in 444 143 81 4
235 33 171 0
Range:
Percentage of 66.1 21.3 12.1 0.6 53.5 7.5 39.0 0.0 Total Processed:
Sum of Analyses:
672 439 (1) Percent Bias by Deviation Category as noted In Table 1, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 1, Footnote (2)
(3) Most Precision data generated from non-positive client samples for specific contractual evaluation
- Total may not equal 100 due to rounding.
- Totals summarize Internal PCs, NIST MAP, and Analytics Cross Check programs FRADMIN\\CORRES\\EL 027-05
-A14-
TABLE 11 FRAMATOME ANP ENVIRONMENTAL LABORATORY ENVIRONMENTAL INTRA-LABORATORY AND INTER-LABORATORY DATA
SUMMARY
BIAS AND PRECISION BY ANALYSIS TYPE JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2), (3) 1 2
3 4
1 2
3 4
I. Gross Alpha Air Filter 5
1 0
0 l
6 0
0 0
Water 9
10 13 0
3 0
16 l
0 II. Am-241 Water 1
8 5
0 4
6 4
0 III. C-14 Waterl 4
1 4
l 4
1 0
1 0
1 0
1 12 T
0 IV. Fe-55 Waterl 9
1 5
1 0
1 0
I 0
1 0
1 14 1
0 V. Gross Beta Air Filterl 118 l
8 0
l 0
6 0
0 0
Water 8
9 17 4
6 7
6 0
VI. Gamma Air Filterl 40 15 2
0 56 1
0 0
Charcoal-Quantitativel 4
0 I
0 I
0 1
0 1
0 1
0 1
0 Charcoal-Screeningl 58 14 I
6 I
0 I
0 I
0 l
0 1
0 MilkI 50 1
11 1
5 1
0 l
62 1
4 l
3 l
0 Water 59 29 6
0 1
62 1
3 1
29 1
Milk 3
2 1
0 0
1 5
0 0
0 Waterl 1
1 3
l 2
1 0
10 5
1 1
0 Vil. Ni-63 Waterl 11 2
1 1
1 0
1 0
l 0
1 14 0
[X. Pu-238 Waterl 6
1 6
1 2
1 0
1 0
1 0
1 14 0-X. Pu-241 Waterl 6
1 6
1 2
1 0
I 0
1 2
1 12 1
0 Xi. Sr-89 Air Flterl 0
1 0
0 1
0 1
0 1
0 1
0 1
0 Milkj 2
1 1
1 0
0 2
1 0
0 XII.
Sr-90 Air Fliterl I
I 0
1 1
l 0
1 0
1 2
1 0
1 0
Milk' 2
l 1
l 0
l 0
l 3
0 0
0 Waterl 6
1 9
0 1
0 1
0 1
16 1
0 XA r_.
Tritium Waterl 22 1
3 3
1 0
1
'0 0
2 1
64 1
° XIV. Tc-99 Water 9
4 3
0 0
0 16 0
Total Number in 444 143 81 4
235 33 171 0
Range:
j Percentage of 66.1 21.3 12.1 0.6 53.5 7.5 39.0 0.0 Total Processed:
6 439 Sum of Analyses:
6 62 r439 (1) Percent Bias by Deviation Category as noted In Table 1. Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 1, Footnote (2)
(3) Most Precision data generated from non-positive client samples for specific contractual evaluation
- Total may not equal 100 due to rounding.
- Totals summarize Internal PCs, NIST MAP, and Analytics Cross Check programs F:\\ADM1MCORRES\\EL 027-05
-A15-
TABLE 12 ENVIRONMENTAL BIAS AND PRECISION BY YEAR Percent Bias Percent Precision Deviation from Known Deviation from Mean Bias Criteria* 1_)Precision Criteria* (2)
Outside Outside Criteria
% Within Criteria
% Within Year 1
2 3
4 Criteria 1
2 3
4 Criteria 2004 849 273 172 10 99.2 439 60 362 2
99.8 2003 572 182 74 13 98.5 354 55 106 1
99.8 2002 619 170 74 7
99.2 411 44 16 3
99.4 2001 383 115 80 22 96.3 330 45 19 2
99.5 2000 368 143 63 18 97.0 342 70 36 1
99.8 1999 323 100 44 13 97.3 301 46 10 2
99.4 1998 375 100 21 7
98.6 355 56 21 4
99.1 1997 351 118 46 11 97.9 -
306 46 11 1 0
100.0 1996 616 187 104 24 97.4 696 71 33 3
99.6 1995 291 75 37 12 97.1 200 43 24 0
100.0 1994 359 116 54 14 97.4 265 61 10 1
99.7 1993 262 121 60 29 93.9 227 59 26 1
99.7 1992 438 206 84 21 97.2 656 112 29 1
99.9 1991 504 174 92 19 97.6 710 82 30 4
99.5 1990 519 153 56 34 95.5 644 97 20 2
99.7 1989 448 171 70 28 96.1 599 76 35 4
99.4 1988 425 141 66 22 96.6 536 76 20 1
99.8 1987 450 187 65 27 96.3 623 80 15 3
99.6 1986 558 185 70 27 96.8 700 82 33 0
100.0 1985 449 177 92 25 96.6 561 93 28 0
100.0 1984 479 254 104 31 96.4.
699 127 24 0
100.0 1983 475 211 108 36 95.7 639 113 46 4
99.5 1982 341 109 135 30 95.1 496 112 135 12 98.4 1981 175 116 152 29 93.9 286 72 46 1
99.8 1980 160 115 167 37 92.3 335 96 59 1
99.8 1979 80 51 68 20 90.9 230 73 51 16 95.7 1978 112 90 40 20 92.4 259 73 29 14 96.3 1977 28 18 12 8
87.9 75 39 5
7 94.4 Total #
11,009 4,058 2,210 594 96.7 12,274 2,059 1,279 90 99.4 in Range:
III
% of all 61.6
.22.7 12.4 3.3 78.2 13.1 8.1 0.6 Analyses In Range*
Total Number 17,871 15,702 I Total may not equal 100 due to rounding.
(1) Deviation Categories 1-3 as noted in Table 1, Footnote (1)
(2) Deviation Categories 1-3 as noted in Table 1, Footnote (2)
F:\\ADMIN\\CORRES\\EL 027-05
-A16-
TABLE 13 ANALYTICS RADIOCHEMISTRY CROSSCHECK PROGRAM RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA, AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 4
1 2
l 3
4 I. Water Fe-55 2
2 2
0 6
0 0
0 Sr-89 3
2 1
0 3
3 0
0 Sr-90 3
3 0
0 3
3 0
0 Total Number in 8
7 3
0 12 6
0 0
Range:
I
___I_
Percentage of 44.4 38.9 16.7 0.0 66.7 33.3 0.0 0.0 Total Processed:
I Sum of Analyses:
18 18 (1) Percent Bias by Deviation Category as noted in Table 12, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 12, Footnote (2)
- Total may not equal 100 due to rounding F:HADMIN\\CORRES\\EL 027-05
-A17-
TABLE 13 PART 50/61 PROCESS CONTROL ANALYSIS RESULTS BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 (Continued)
(1)
Percent Bias by Deviation Category 1 = >0 and *5 2 = >5 and *10 3 = >10 and *15 (or within 2 sigma of known, see Reference 1)
For Gross Alpha and Beta In water, 3 = >10 and *25 (or wi, For Alpha Spectrometry*,
3 = >10 and *20 (or wil For Uranium-Total, Pu-241, Zn-65 on an air filter, C-14, 3 = >10 and *20 (orwi[
4 = Outside criteria (2)
Percent Precision by Deviation Category 1 =>0 ands5 2=>5and*10 3 = >10 and *15 (or within 2 sigma of mean, see Reference 1) 4 = Outside criteria thin 2 sigma of known) thin 2 sigma of known) thin 2 sigma of known)
Isotopic Uranium (U-234, 235, 238)
Isotopic Thorium (Th-230, 232)
Np-237 Am-241/Cm-242, 243/244 Pu-alpha (Pu-238, 239, 240)
Ra-226 Total may not equal 100 due to rounding.
F:ADMIN\\CORRES\\EL 027-05
-Al18-
TABLE 14 FRAMATOME ANP ENVIRONMENTAL LABORATORY ANALYTICS RADIOCHEMISTRY CROSS-CHECK PERFORMANCE EVALUATION Mean Ratio I
_I Sample Quarter/
Sample Reported Known E-LAB/
I Number Year Media Nuclide Units Value Value Analytics Evaluation Al 8332-162 3rd/2004 Liquid Fe-55 uCi/cc 3.91 E-04 4.08E-04 0.96 Agreement A18333-162 3rd/2004 Liquid Sr-89 uCi/cc 1.83E-03 1.90E-03 0.96 Agreement A18333-162 3rd/2004 Liquid Sr-90 uCi/cc 3.07E-04 3.16E-04 0.97 Agreement A18656-162 4th/2004 Liquid Fe-55 uCi/cc 3.94E-04 4.44E-04 0.89 Agreement Al 8657-162 4th/2004 Liquid Sr-89 uCi/cc 3.75E-03 3.55E-03 1.06 Agreement A18657-162 4th/2004 Liquid Sr-90 uCi/cc 2.85E-04 2.82E-04 1.01 Agreement FA\\ADMIN\\CORRES\\EL 027-05
-A19-
TABLE 15 NIST MAP ANALYSIS RESULTS BREAKDOWN BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 l
4 1
2 3
4 I. Water Gamma 15 17 4
0 36 0
0 0
II. Filter Gamma 26 4
0 0
30 0
0 0
Total Number in Range:
41 21 4
0 66 0
0 0
Percentage of Total Processed:
62.1 31.8 6.1 0.0 100.0 0.0 0.0 0.0 Sum of Analyses:
66 66 (1) Percent Bias by Deviation Category as noted in Table 1, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 1, Footnote (2)
- Total may not equal 100 due to rounding F:AADMIN\\CORRES\\EL 027-05
-A20-
TABLE 16
SUMMARY
OF FRAMATOME ANP ENVIRONMENTAL LABORATORY NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY (NIST)
TRACEABILITY RESULTS JULY-DECEMBER, 2004 NIST Reference E-LAB Mean Percent Standard Date of Measurement Deviation From Number Standard Radionuclide Matrix Technique NIST 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy Env. #2
-6.62 1680-5 27-Apr-04 Cd-1 09 Liquid Gamma Spectroscopy Env. #2
-7.88 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy Env. #2
-9.30 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy#2
-5.04 1680-5 27-Apr-04 Cd-109 Liquid Gamma Spectroscopy #2
-10.67 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy #2
-8.75 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy #4
-0.88 1680-5 27-Apr-04 Cd-109 Liquid Gamma Spectroscopy #4
-3.85 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy#4
-3.02 1680-5 27-Apr-04 Co-57 Liquid Gamma Spectroscopy #5
-2.86 1680-5 27-Apr-04 Cd-109 Liquid Gamma Spectroscopy #5
-6.92 1680-5 27-Apr-04 Am-241 Liquid Gamma Spectroscopy#5
-4.57 1686-8 24-Jun-04 Co-57 Filter Gamma Spectroscopy #2
-0.16 1686-8 24-Jun-04 Co-60 Filter Gamma Spectroscopy #2
-0.13 1686-8 24-Jun-04 Cd-1 09 Filter Gamma Spectroscopy #2
-3.98 1686-8 24-Jun-04 Cs-134 Filter Gamma Spectroscopy #2
-4.34 1686-8 24-Jun-04 Am-241 Filter Gamma Spectroscopy#2
-1.44 1686-8 24-Jun-04 Co-57 Filter Gamma Spectroscopy #4
-1.30 1686-8 24-Jun-04 Co-60 Filter Gamma Spectroscopy #4 0.74 1686-8 24-Jun-04 Cd-1 09 Filter Gamma Spectroscopy #4
-6.05 1686-8 24-Jun-04 Cs-1 34 Filter Gamma Spectroscopy #4
-4.16.
1686-8 24-Jun-04 Am-241 Filter Gamma Spectroscopy#4
-1.50 Data on NIST MAP program is repeated in Table 4 for Environmental QC data.
F:ADMINCORRES\\EL 027-05 21
-A21-
TABLE 17 INTRA-LABORATORY PART 50161 PROCESS CONTROL RESULTS BREAKDOWN BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 l
4 1
2 3
4 I. Soil Alpha 0
0 0
0 0
0 0
0 Am-241 0
0 0
0 0
0 0
0 Fe-55 0
0 0
0 0
0 0
0 Gamma 3
0 0
0 0
0 0
0 Sr-89 0
0 0
0 0
0 0
0 Sr-90 0
° 0
1 0
0 0
0 0
0 II. Liquid Alpha 1
5 0
0 0
0 0
0 Am-241 0
2 4
0 6
0 0
0 Beta 1
0 0
0 0
0 0
0 C-14 0
0 3
0 0
1 2
0 Cm-24314 2
4 0
0 6
0 0
0 Fe-55 0
3 0
3 6
0 0
0 Gamma 6
0 0
0 6
0 0
0 H-3 4
2 0
0 6
0 0
0 1-129 0
0 1
5 5
1 0
0 Ni-63 3
3 0
0 6
0 0
0 Np-237 1
2 0
0 3
0 0
0 Pu-238 6
0 0
0 6
0 0
0 Pu-241 0
2 1
0 3
0 0
0 Sr-89 3
8 1
0 5
3 1
0 Sr-90 4
2 0
0 5
1 0
0 Tc-99 1
4 1
0 5
1 0
0 Total Number 35 37 11 8
68 7
3 0
in Range:
Percentage of 38.5 40.7 12.1 8.8 87.2 9.0 3.8 0.0 Total Processed:
Sum of Analyses:
91 78 (1) Percent Bias by Deviation Category as noted in Table 13, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 13, Footnote (2)
- Total may not equal 100 due to rounding.
FAADMIN\\CORRES\\EL 027-05
-A22--
TABLE 18 PART 50/61 ANALYSIS RESULTS BREAKDOWN BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JULY-DECEMBER 2004 Bias Criteria (1) lPrecision Criteria (2)l I 0 2
3 4
1 0
3 4
- 1. Filter Gamma4 26 4
0 0
30 0
1 0
0 II. Soil Gammal 3
1 0 4 0 l
0 4 0 2 0
1 0
1 0
- 11. Liquid Alpha 15000 0
Am-241 0
2 4
0 6
0 0
0 Beta 1
0 0
0 0
0 0
0 C-14 10 0
3 0
0 1
2 0
Cm-243/4 2
4 0
0 6
0 0
0 Fe-55 2
5 2
3 12 0
0 0
Gamma 21 17 2
0 42 6
0 H-3 4
2 0
0 6
0 0
0 1-129 1
4 1
0 5
1 0
0 Ni-63 33006 0
Np-237 1
2 0
0 3
0 0
0 Pu-238 6
0 0
0 6
0 0
0 Pu-241 021 0
3 0
00 Sr-89 6
10 2
0 8
6 1
0 Sr-90 7
5 0
840 Tc-99 1
4 1
0 5
1 0
0 Total Number 84 65 18 8
146 13 3
0 in Range:
Percentage of 48.0 37.1 10.3 4.6 90.1 8.0 1.9 0.0 Total Processed:
Sum of Analyses:
175 162 (1) Percent Bias by Deviation Category as noted in Table 13, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 13, Footnote (2)
- Total may not equal 100 due to rounding.
- Totals summarize Internal PCs, NIST MAP, and Analytics Cross Check programs F:AADMIN\\CORRESXEL 027-05
-A23-
TABLE 19 PART 50161 BIAS AND PRECISION BY YEAR (1)
Percent Bias Percent Precision Deviation from Known Deviation from Mean Bias Criteria 2
- 2)
Precision Criteria (2)
Outside Outside Criteria
% Within Criteria
.% Within Year 1
2 3
4 Criteria 1
2 3
4 Criteria 2004 157 110 54 17 95.0 286 23 4
0 100.0 2003 144 91 51 9
96.9 249 18 2
0 100.0 2002 215 94 49 8
97.8 300 24 5
2 99.4 2001 159 90 46 24 92.5 238 46 6
0 100.0 2000 151 72 28 23 91.6 220 38 16 4
98.6 1999 111 59 14 7
96.3 168 13 5
2 98.9 1998 90 68 24 7
96.3 160 22 7
0 100.0 1997 99 43 33 8
95.6 168 13 2
0 100.0 1996 194 80 33 17 94.8 285 31 8
0 100.0 1995 112 47 35 7
96.5 173 15 4
0 100.0 1994 125 39 25 5
97A 158 22 5
1 99.5 1993 154 51 32 17 93.3 208 34 7
0 100.0 1992 116 86 38 7
97.2 207 27 5
0 100.0 1991 126 77 53 35 88.0 223 28 10 5
98.1 1990 116 65 31 21 91.0 199 35 6
0 100.0 1989 73 71 51 26 88.2 152 40 24 8
96.4 1988 30 19 13 13 82.7 43 13 6
9 87.3 Total#
2,172 1,162 610 251 94.0 3,437 442 122 31 99.2 in Range:
%of all 51.8 27.7 14.5 6.0 85.2 11.0 3.0 0.8 Analyses in Range' Sum of Analyses 4,195 4,032
- Total may not equal 100 due to rounding.
(1) This breakdown excludes the 71 verification analyses associated with the startup of this area of the Laboratory during 1988-89.
(2) Deviation Categories 1-4 as noted in Table 13, Footnote (1)
F:\\ADMIN\\CORRES\\EL 027-05
-A24-
TABLE 20 BIOASSAY ANALYSIS RESULTS BREAKDOWN BY FRAMATOME ANP ENVIRONMENTAL LABORATORY ACCEPTANCE CRITERIA, MEDIA AND MEASUREMENT CATEGORIES JANUARY-JUNE 2004 Bias Criteria (1)
Precision Criteria (2) 1 2
3 4
1 2
3 4
I. Urine (3)
Gamma H -3+00 Total Number In Range:
0 ° 0
0 0
0 0
0 Percentage of 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 Total Processed*:
Sum of Analyses:
0 0
(1) Percent Bias by Deviation Category as noted in Table 13, Footnote (1)
(2) Percent Precision by Deviation Category as noted in Table 13, Footnote (2)
(3) There were no internal or external bioassay QC samples analyzed during this period.
- Total may not equal 100 due to rounding FAADMIN\\CORRESMEL 027-05
-A25-
TABLE 21 LAWRENCE LIVERMORE NATIONAL LABORATORY (LLNL)
BIOASSAY THYROID RADIOIODINE INTERCOMPARISON PROJECT (TRIP)
F:=ADMIN\\CORRES\\EL 027-05
-A26-
TABLE 22 CONDITION REPORT (CR) STATUS (JULY-DECEMBER 2004)
(OPEN)
(CLOSED)
INITIATION CLOSE-OUT CR #
DATE DATE DESCRIPTION STATUS AS OF 06130104 Client requested investigation Into Required MICs for these samples were all met, several though did not meet concerns over timeliness of sample the specific time frames. Management Is monitoring the processing of these processing and explanation of several special samples during routine sample status meetings. Each unusual CR 04-06 16-Apr-04 7-Sep-04 sample results.
sample result was investigated and explanation provided.
Process chedk for Fe-55 failed with A new NIST Fe standard was obtained. The new calibration curve nessaive bias.
eliminated most of the negative bias on subsequent Fe-55 analyses.
CR 04n8 25-May-04 8-Sep-04 Training on the findings was provided to all chemists.
Four water samples analyzed for I-The Individual who mis-entered the data Into LIMS and the Individual
.131LL could not meet the required performing verification review were counseled concerning the need for self-MDC due to delay in performing the checking. Final results and an explanatory letter have been provided the analysis. Delay was determined to be client.. Supervisor performed review of sample receipt process and Is CR 04-09 1 0-Jun-04 8-Nov-04 data entry error currently performing independent review of all sample log-in data.
LIMS fields for the chemical carrier ID The individual Involved has been counseled. All chemists were reminded to and expiration date for some ensure all LIMS fields are verified prior to completing data entry. All carrier analyses were not updated as infomation in LIMS has been verified to be corred CR 04-10 6-Jul-04 5Oct-04 required.
Intenalprocss heckforSr-8/90 A detailed Investigation Into the strontium process was conducted. The Sr-Internal process check for Sr-89t90 89 calibration on LKB #1 was performed. The tracer was successfully failed to meet the bias acceptance validated, the procedure process was reviewed acceptably, samples were
- limits, reprocessed successfully, and subsequent process check was acceptable.
CR 04-11 15-Jul-04 7-Dec-04 Two dient samples being saved for Composite samples have been completed with appropriate notes about the future composite were unable to be missing samples. A separate storage area has been provided for holding located.
the samples until ready for compositing.
CR 04-12 23-Jul-04 4-Aug-04 The filter was independently analyzed by garmma spectroscopy to validate Analytics air particulate sample for the known value. With a cited known value of 59 pCi, the gamma spec gross alpha failed to meet the E-LAB alysis Indicated 50 pCi, which Is similar to the gross alpha analysis result.
acceptance cniteria for bias.
The filter has been re-analyzed by Analytics and the new known' validates a.
the original E-LAB analytical results. The subsequent Analytics filter for CR 04-13 27-Jul-04' 28-Jan-05 gross alpha had a -4% bias, well within the acceptance criteria.
Only the mounts for counting the filter for 1-131LL were found to be Several samples were found to have contaminated. Samples were either re-mounted or re-analyzed. Clients cstarier were notified If their samples were unable to analyzed to the required MDC.
been contaminated during camer A revision of the carrier verification method and a review of source verification testing.
preparation methods has been completed to add new controls to this CR 04-14 3-Aug-04 7-Dec-04 process.
Excessive cream and curdling of milk samples Is the major cause of the low Eight milk samples for Sr-89190 had recoveries. A refrigerator has been designated for storage in an attempt to Eightally milk samlesovery ves.
retard curdling of milk samples. Several chemicals used In the process have unusually low recovery values, been verified or re-made to ensure the proper pH or molarity. A blank milk CR 04-15 8-Sep-04 S
IIsample was run through the process with an acceptable -70% recovery.
F:AADMIN\\CORRES\\EL 027-05
-A27-
TABLE 22 (continued)
CONDITION REPORT (CR) STATUS (JULY-DECEMBER 2004)
(OPEN)
(CLOSED)
INITIATION CLOSE-OUT CR #
DATE DATE DESCRIPTION STATUS AS OF 06130104 Seveal Prt 1 Fe55 nd N-63 A review of the handling and review process was conducted. No historical Sev eral Part 61 Fe-55 and Ni-63 problems were noted. The liquid scintillation procedure was revised to samples were sitched during liquid require a post-count verification of the proper protocol plug. All samples CR 04-16 20-Sep-04 2
ct-04 ilaon analsis.
were re-counted using the appropriate method and reported to the client.
MAPEP-04-MaW12 water sample for A single analysis was performed of the Pu-238 sample. A subsequent Pu-238 fell In the Waming' range recount was statistically similar to the original count and also passed the with a -20.8% bias (limit of +1-20% for MAPEP acceptance criteria. No problems were noted with the process CR 04-17 30-Nov-04 26-Jan-05 Waming).
history.
Internal process checks for 1-129 for the first and second quarters of 2004 Testing Indicates that a bias exibsthratit.h A new NIST source has been had positive biases greater than the ordered for further testingo acceptance limit.
CR 04-18 30-Nov-04 All samples were re-processed with successful control spike. Chemist was Two consecutive gross beta control found to have been overheating planchet. causing Cs-137 volatization.
spikes (water) failed with large Chemist has been counseled on proper heating of planchets to prevent negative biases.
volatization of cesium. A precaution was added to the procedure and all CR 04-19 30-Nov-04 7-Feb-05 chemists were trained to the revision.
Puche Od i
f t filed Purchase Order review form completed (address changes only). A reminder PufohaseOrder revi ew fom nn fd to personnel Involved In the P.O. review process was provided by the for revision to existing P.O.
Laboratory Manager.
CR 04-20 15-Dec-04 17-Jan-05 Chemist was trained to the appropriate Information. Additional Read & Sign Read & Sign training not completed training forms were not completed as required. These have now been for a new chemist, completed. The training procedure Is being revised specifically for the indoctrination training of new employees.
CR 04-21 1 5-Dec-04 Pipet QC check log corrected. Review of all documents Indicate this was an Pipet failed daily QC check due to isolated Instance. Management reviewed the process of document control incorrect acceptance range listed on for pipet and balance OC checks. A modification of document control was
- form, made to Include frequent supervisory review and submittal for final records CR 04-22 15-Dec-04 3-Feb-05 retention.
A software V&V for spreadsheets The personnel performing the revision (late 2002/early 2003) failed to used In Part 50/61 processing update the spreadsheet footer with the new revision number. The V&V contained Incorrect reference to the documentation has been updated and was also verified to have been revision number.
performed on the correct revision.
CR 04-23 15-Dec-04 13-Jan-05 Three weaknesses noted In Safety Threel weplaknese notedwnafet Al personnel have been retrained to the OSHA requirement for flushing
.Manual compliance (eyewash eyewashes. The hazardous chemnical list has been reviewed and updated.
flushing, NFPA labels missing on Chemical labeling has been verified. A revision to the requirements for chemicals hazardous chemical list labeling Is In progress.
CR 04-24 15-Dec-04 F:\\ADMIN\\CORRES\\EL 027-05
-A28-
TABLE 23 UPDATED INSTRUMENTATION GROUP/ANALYTICAL SERVICES SECTION PROCEDURES ISSUED DURING JULY-DECEMBER 2004 PROCEDUR TITLE REVISION APPROVA EFFECTIVE E NUMBER NUMBER LDATE DATE The Determination of Tritium in 373 Environmental Samples Using the 1
10/19/04 10/26/04 Micro Distillation Apparatus Operation and Calibration of the 480 EG&G Ortec Octete-PC Alpha 7
07/27/04 07/27/04 Spectrometry Detector System Operation And Calibration Of The 490 Wallac Model 1414/1415 5
10/06/04 10/06/04 Liquid Scintillation Counter 715 Preparation of Tolerance Charts 18 07/27/04 07/27/04 730 Standardization and Verification of 16 10/29/04 10/29/04 Carriers__
The Determination of lodine-1 29 in 1192 10 CFR 50 and 10 CFR 61 Samples 0
07/27/04 07/27/04 Using the Micro Distillation Apparatus Operation and Calibration of the LKB 1210 Model 1219 SM Liquid Scintillation 11 10/06/04 10/06/04 Counter F:AADMIN\\CORRES\\EL 027-05 A-29
APPENDIX A INTER/INTRA-LABORATORY, ENVIRONMENTAL MONITORING ANALYTICS, DOE, ERA AND NIST QUALITY CONTROL PROGRAM RESULTS F:UADMIN\\CORRESMEL 027-05
.-. t....-..-..-.....-J.
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP GROSS ALPHA AIR PARTICULATE RESULT BIAS 100 80 z
0 z
CE 0
11 11 LL IL ni 60 40 20 0
-20
-40
-60 I
I I
I I
I I
I I
I I
I I
I I
11 I,
I, Uaow Contrd Llail (+25_OX) -
IT, Lowo
- oni tion1t r-2.a) - - --- - - --- - - - - - - - - - - - - - - - - - - - - - - - - - -I
-80
-100
+ ERA
- PC A NST v ANALYTOS K
I 1
I I
' I I
I I
I I
w I
I I
1-1 I I I
- 1. I b AAS-
_ S1.
-Wx Al F
MAY a AL
)X SP COT f
((
A HB UM A + W U
.1 U P
I 0 C
ANALYSIS PERIOD 2003-2004
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP GROSS ALPHA WATER RESULT BIAS 100 80 z
60 0
40 1.
Uppr Cowrd LlUt (+259 20 o
0 41
+
IL
-20 li- _40t
(-2-5-) --
>t-----
IL -40
~~~r26)+/---.
R
-60
- *A
-80 _..T
.T ANALYTrS
-100 I,
I, 11I,,,,,,
I I,
l I
I l
- OE ANB iw MA 6ky D
1J a
Oi a
u B
Aa m
y IN a E KG Sp CT to DM ANALYSIS PERIOD 2003-2004
QC CROSS CHECK MALYSIS SHEET SAMPLE TYPE: WAXER ISSUAUCE DATE: 08/04/2004 REF. DATE: 05/26/2004 LAB SAHPLE NO:
751515 ANAL DATE: 07/13/2004 UNI7S:
pCi/L MUCLIDE RESULT I RESULT 2 RESULT 3 MEAN KWOUN X
X X
VALUE DIFF.1 DIFF.2 DIFF.3 Alpha 1 776 s 72 E-01 60.20E 00 28.90 Beta C 519 i 44)E-01 45.40E 00 14.30 Internal spike for Gross Alpha In water was analyzed acwording to specifc dient protocol. The result met the dient's QC citerba.
ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT THOSE NOTED WITH AN ASTERISK
~---
'r*-..
~
- 1....-
1--
QC CROSS CHEOC ANALYSIS SHEET SAMPLE TYPE: UATER ISSUANCE DATE: 11/03/2004 REF. DATE:
03/08/2004 LAS SAMPLE NO:
801802 ANAL DATE:
10/07/2004 UNITS:
pCI/L UIUCLIDE lESULT I REIWLT 2 RESULT 3 MEAN KW=
X X
X VALUE DIFF.1 DIFF.2 DIFF.3 Atpha t 3T1
- 48)E-01 55.40C 00
-33.00 get&
C 638 a 43)E01 59.60E 00 7.00 Internal spike for Gross Alpha In water was analyzed according to specific client protocol. The known value was less than 10 Imes the method MDC. The result met the cient's QC criteria.
ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT THOSE NOTED WITH AN ASTERISK I~-
~-.,..
,......
.'.
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP GROSS ALPHA RESULT BIAS 100 80 z
3:
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ANALYSIS PERIOD 2003-2004
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Am-241 RESULT BIAS 100 80 z
0 z
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Ba-133 RESULT BIAS 100 80 z;
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INTRALABORATR'Y CROSS CHECK ANALYSIS SHEET SAMPLE TYPE; WATER ISSUANCE DATE: 11/19/2004 REF. DATE:
11/19/2003 LAS SAMPLE NO; 821701 ANAL DATE:
10/21/2004 UNITS:
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( 1175T 17)E 00 10.77E 02 9.10
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ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT THOSE NOTED WITH AN ASTERISK t
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09/28/2004 UNITS:
pci/L
~w..................................
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X X
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- 28.40*
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.1 I.
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1-INTRALABORATORY CROSS CHECK AUALYSIS SHEET SAMPLE TYPE: WATER ISSUANCE DATE: 11/19/2004 REf. DATE: 11/19/2003 LAB SAXPLE No:
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1-
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. -1 INTRALABORATORY CROSS CHECK ANALYSIS SHEET SAMPLE TYPE: WATER ISSU.NCE DATE: 01/182005 REF. DATE:
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12/21/2004 UNITS; pCf/L NUCLIDE RESULT 1 RESULT 2 RESULT 3 MEAN KNCM4N X
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-10.60 Beta
( 592 1 10)E 00 82.00E 01
-27.80*
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ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT TNOsE NOTED WITH AN ASTERISK I
r-...
r-.---.,-..-,--
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP C-14 RESULT BIAS 100 80'
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP CHARCOAL RESULT BIAS 100 80 z
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Cs-134 RESULT BIAS 100 I
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP H-3 RESULT BIAS 100 80.
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP 1-131 (Gamma) RESULT BIAS 100
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Pu-238 RESULT BIAS 100 80 77z0 B7z 0T-
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-.- I 2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Pu-241 RESULT BIAS 100 80 0
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS.
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Sr-90 RESULT BIAS 100 80 z
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c QC COSS CMECK AMALYSIS SHEET SAMLE TYPE: WATER ISSUANCE DATE: 08112/2004 REF. DATE: 0610312004 LAS SAMPLE NO; 754312 ANAL DATE:
0810312004 UNITS: pCi/L NUCLIDE RESULT I RESULT 2 RESULT 3 KMA K310WM I
VALLE DIFF.1 DIFF.2 DIFF.3 Sr*90 C 510 +/-55)E-01 6018 0*5.10 Internal spike for Sr-90 In water was analyzed according to specific client protocol. The known vakie was less than 10 tkmes the method MDC. The result met the client's QC crttria and met the E-LAB acceptance criteria using the 2-sigma test ALL RESULTS PASSED CA PERFORHANCE CRITERIA EXCEPT THOSE NO TED WITH AN ASTERISK
V..
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09/23/2004 UNITS:
pCl/L NUCLIDE RESULT I RESULT 2 RESULT 3 NEAI KOUI X
X X
VALUE DIFF.1 DIFF.2 DIFF.3 Sr-90 C 492 a 56)E*0i 63.60E 00
-22.60 Internal spike for Sr-90 In water was analyzed according to specific client protocol. The known value was less than 10 times the method MDC. The result met the cient's QC criteria.
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.I
.. 4 S.._.
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QC CROSS CHECK AMALYSIS SHEET SANPLE TYPE: WATER ISSUALCE DATEs 12/08/2004 REF. DATE: 0310812O34 LAB SAMPLE NO:
808302 ARAL DATE:
10/27n/004 UNITS: PCl/L UCLIDE RESULT 1 RESULT 2 RESULT 3 PA" KHOI XX VALUE DIFF.1 DiFf.2 DIFF.3 Sr-90 C 787 I 58)E-O1 63.601 00 23.70 Internal spike for Sr-90 In water was analyzed according to specific client protool. The known value was less than 10 times e metd MDC. The result met the clients QC criteria.
ALL RESULTS PASSED GA PERFORMANCE CRITERIA EXCEPT THOSE NOTED WITH AN ASTERISK
1 - -
-,
.. l-l..
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Sr-89 (COMBINED WITH Sr-90) RESULT BIAS 100 80 z
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Tc-99 RESULT BIAS-II :
z 0z y
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100 80 60 40 20 0
-20
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-60
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1 2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP U-234 RESULT BIAS 100 80 I,
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-40 20 0
-20
-40
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP U-238 RESULT BIAS 100 0
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80 60 40 20 0
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0 z
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-20
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS REMP Zn-65 RESULT BIAS 100 80 0
Uy-60 40 20 0
-20
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ANALYSIS PERIOD 2003 2004
APPENDIX B EFFLUENT MONITORING AND WASTE CHARACTERIZATION QUALITY CONTROL RESULTS (10CFR PART 50/61)
FMADMIN\\CORESMEL 027-05
9.S.,
'.._A 1-...
............ ___r----
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Gross Alpha RESULT BIAS 100:
80 I
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S.~-~*-X 2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Am-241 RESULT BIAS 100
.80 z7 0
0 Ll-60 40 20 0
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.6-L-2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Ba-133 RESULT BIAS
'100 80 z
0 z
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-20 I
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0 z
\\110 I I 60 40 20 0
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b 2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 C-14 RESULT BIAS 100 80 0
U-LL Ul-60 40 20 0
-20
-40
-60 I I I
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ANALYSIS PERIOD 2003-2004
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PART 50/61 CROSS CHECK ANALYSIS SHEET SAXPLE TYPE: LIQUID ISSUANCE DATE: 11/30/2004 REF. DATE:
08/04/2004 LAB SAlPLE NO:
Z22128 ANAL DATE:
10/29/2004 LAB S&PLE MO:
Z22129 ANAL DATE:
10/29/2004 LAB SA1PLE NO:
Z22130 ANAL DATE:
10/29/2004 UNITS:
uCI/g MUCLIDE RESULT 1 RESULT 2 RESULT 3 WUAN KN OUI X
VALUE DIFF.1 DIFF.2 DIfF.3 H-3 (1137 t
29)E-05 (1134 t
29)E-05 (1118 a 28)E-05 10.66E-03 6.70 6.40 4.90 X DIFF FROM KW; 11.30E-03 0.60 0.40
-1.00 C-14 C 271 t Z0)E-04 C 370 a 27)E*04 C 242 a 18)9-04 30.8E-03
- 12.20 19.90
-21.60*
X DIFF FROM KEA:
29.43E-03
- 7.90 25.70*
- 17.80 Tc-99
( 270
- 24)E-06 C 276 a 18)E-06 272 a 18)E-06 30.115-05
-10.30
-8.30
- 9.70 X DIFF FROM KMEA:
27.27E-05
-1.00 1.20
-0.20 1-129
( 320 t 19)E-06
( 313 a 19)E-06 C 352
- 21)E-06 27.58E-05 16.00' 13.50 27.60*
X DIFF FROM MEAN:
32.83E-05
- 2.50
-4.70 7.20 A single Pail 61 Process Check sample for C-14 fell outside the 209% bias acceptance lmit. No CR was Issued since the mean of the three samples (-4.6%) fell within the acceptance llmtt.
ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT THOSE MOTED WITH AN ASTERISK
- 1. -
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.PART 50/61 Cd-109 RESULT BIAS 100 80 z~
0 0
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Cm-243/244 RESULT BIAS 100 80 z
0 z
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- 1.
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Co-57 RESULT BIAS 100 80 0
0mr ILI ILI ILI 60 40 20 0
-20
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Co-60 RESULT BIAS 100 80 60 40 0
0 20
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Cs-134 RESULT BIAS I -
z 0
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Cs-137 RESULT BIAS 100 80 z
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60 40 20 0
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. - I-2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Eu-152 RESULT BIAS 100 80 I
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. .... 1.....,. -
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 Fe-55 RESULT BIAS
-'100 80 z
0 z
0 LL To 60 40 20 0
-20
-40
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PART 50/61 CROSS CHECK ANALYSIS SkEET SAMPLE TYPE: LIQUID ISSUANCE DATE: 02/J4/2005 REF. DATE:
11/02/2004 LAB SAMPLE NO:
Z22525 LAB SAMPLE NO:
Z22526 LAB SAMPLE NO:
Z22527 ANAL DATEs 12/18/2004 ANAL DATE:
12/18/2004 ANAL DATE:
12/18/2004 LIITS:
uCI/g NUCLIDE RESULT 1 RESULT 2 RESULT 3 mum
. KNO VALUE X
X X
DIFF.1 DIFF.2 DIFF.3 Fe-55
( 810 a 66)E-05
( 818 I 66)E-05
( 860 a 70)E-05 10.13E-03
- 20.00*
- 19.204
-15.100 X DIFF FROM MEAN:
82.93E-04
-2.30
( 17Z a 1l)E-05 C 791 1 62)E-05 C 1059 a 51)E-05
( 172 I 10)E-05
( 792 a 62)E-05 X DIFF FROM MEAN:
C i103 a 54)E-0S X DIFF FROI MEAN:
( 182 a 11)E-05 X DIFF FROM MEANs 86.00E-04 78.93E-04 11.33E-03
-8.70
-8.00
-7.90
-0.50 0.20 0.30
-8.30
- 6.50
- 2.60
- 2.60
-0.70 3.40
- 4.10
- 4.10 1.50
-1.90
-1.90 3.W0 10.67E-03 17.93E-04 17.53E-04 Pu-238 C 2215 a SO)E-09 C 2185 a 49)E-09
( 2146 a 49)E-09 X DIFF FROM MEAN:
21.11E-07 4.90 3.50 1.70 1.50 0.10
-1.60 21.82E-07 A set of three Part 50161 Process Check samples for Fe-55 fell outside the +/-15% bias acceptance limit. CR 05-08 was Issued to Investigate the negative bias. The Initial Investigation Indicated a potential problem with the Fe-55 source used to prepare the process check.
ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT TROSE NOTED WITH AN ASTERISK I
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 H-3 RESULT BIAS 100 80 z
0 11 z
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60 40 20 0
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Lower Contl Ltnit (-150f%-
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 1-129 RESULT BIAS 100 zr 0
0ffi LL LL 80 60 40 20 0
-20
-40
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PART 50/61 CQRSS CHECK AMALYSIS SHEET SAMPLE TYPE: LIQUID ISSUANCE DATE: 11/19/2004 REF. DATE: 03/19/2004 LAS SAMPLE NO:
221444 LAS SAMPLE NO:
ZZ1445 LAS SAHPLE MO: Z2146 ANAL DATEt 10/02/2004 ANAL DATEI 10/02M2004 ANAL DATEM 10/02/2004 UNITS:
uCI/g NUCLIDE RESULT I RESULT 2 RESULT 3 a^N KO X
X VALUE DIFF.1 DlFf.2 DIFF.3 h-3 C 489 a 13)9-05 C 466 2 12)E-05 C 473 a 13)1-05 4.391-04 1.10
- 3.70
-2.30 X DIFF FRaO 1EAM:
47.60E-04 2.70
-2.10
( 310 a 23)E-04 C 307 2 21)E-06 t 222 a 13)E-06 C 273 a 20)1-04 X DIFF FRDW HkW:
C 316 2 21)E-06 X DIFF FR4N W.A":
C 225 a 15iE-06 X DIFF FRO0 I0JM.
27.43E-03 30.631E-OS 22.431-05 30.65U-03 30.54Z-05 19.12E-05
-20.20*
3.10
-9.20
-12.50 13.00
.0.50
-3.10 0.50 3.50
-3.40 0.20 3.20 18.20*
16.10*
17.70*
0.70.
-1.00 0.30 ALL RESULTS PASSED QA PIRFOR4ANCI CRITERIA EXCEPT THOSE NOTED UITH AN ASTERISK A set of three Part 61 Process Check samples for 1-129 fell outside the +/-15% bias acceptance limit. CR 04.18 was Issued to Investigate the positive bias.
r...
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-i-
,w#--*
PART 50/61 CROSS CMECK AMALYSIS SNEET SAWPLE TYPEz LIQUID ISSUANCE DATEM 11/30/2004 RIF. DATEs 08/04/2004 LAW SAWLE NO:
Z22125 AIAL DATEt 10/29/2004 LAB SAPLE Ua:
222129 ANAL DATE 10/29/2004 LAB SAKPLE NO:
222130 AXAL DATEs 10/29/2004 UNITS:
utf/g WUCLIDE RESULT I REULT 2 RESULT 3 MEAN KNO X
X VALUE DIFF.1 DIFF.2 DIFF.3 1K-3 C 1137 a 29)E-05 C 1134 a 29)E-05 1118 a 28)1.05 10.668-03 6.70 6.40 4.90 X DIFF FROM MIEAIs 11,30E-03 0.60 0.40
- 1.00 C-14 C 271
- 20)E-04 30 1 27)E-04 2 242 a 18)1-04 3061-03
-12.20 19.90
.21.60*
X DIFF FRC1 KEAN:
29.431-03
-7.90 25.70*
-17.50 Tc-99 C 270 a 24)E-06 C 276 a 18)E-06 t272 18)1-06 30.111-05
- 10.30
-5.30
-9.70 X DIFF FRCH MEANt 27.27E-05
-1.00 1.20
-0.20 1-129 C 320a 19)E-06 C 313 S 19)1*06 C 352 a 21)E-06 27.58E-05 16.00*
13.50 27.0*U X DIFF FIRI MEAN:
32.31E-05
.2.50
-4.70 7.20 A set of three Part 61 Process Check samples for 1-129 fell outside the +/-15% bias acceptance limit. CR 04-18 was issued to Investigate the positive bias.
ALL RESULTS PASSED QA PERFORANCE CRITERIA EXCEPT TROSE NOTED WITII AN ASTERISK
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/61 1-131 (Gamma) RESULT BIAS' 100 80 z7 0
0 LL ILuL 60 40 20 0
-20
-40
-60 Upper ContrL Urrill (.150X)
Lower Control Urnrt (-15.0%)
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ANALYSIS PERIOD 2003-2004
~~~~~~~~~~~~
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 50/6 1 Mn-54 RESULT BIAS 100 80 I
I z7 0
0 LL LL 60 40 20 0
-20
-40
-60 Upp& ContraI Urnit (+ 1 bL)%
Lc~ar Control LUmit
(-15-OX
-i ANST
-80
-100 V ANALYWIS
- PC A OTHER ANALYSIS PERIOD 2003-2004
2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PARTP50/61 Ni-63 RESULT BIAS 100 80 z
0 z
0mr ILI ILI LL 60 40 20 0
-20
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2003-2004 QUALITY ASSURANCE TRENDING ANALYSIS PART 60/6 1 Np-237 RESULT BIAS 100 80 z
0 0
U-r IL u-60 40 20 0
-20
-110
-60 Utpa Cntri Unmit
(*20.0X)
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2003-2004. QUALITY ASSURANCE TRENDING ANALYSIS PART 50/6 1 Pu-238 RESULT BIAS 100 80 0
0 LL LL 60 40 20 0
-20
-40
-60 Upper Control Urnit (.200%)
CoorcoMrol&,i
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-80
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PART 50/61 CROSS CHECK ANALYSIS SHEET SAMPLE TYPE: LIQUID ISSUANCE DATE: 11/19/2004 REF. DATE:
08/26/2004 LAB SAMPLE NO:
XZ2Z17 LAS SAMPLE NO:
X22218 LAS SAMPLE NO:
X22219 ANAL DATE: 09/10/2004 ANAL DATE: 09/10/2004 ANAL DATE:
09/10/2004 UNITS: uCl/g KUCLIDE R WULT 1 USULT Z XWSULT 3 mmA K
X XX VALUE DIFF.1 DIFF.2 DIFF.3
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A single Part 50/81 Process Check sample for Sr.89 fell outside the :15% bias acceptance limit. No CR was issued since the mean of the three samples (+1.6%) fell within the acceptance limit ALL RESULTS PASSED QA PERFORMANCE CRITERIA EXCEPT TNOSE NOTED WITH AN ASTERISK
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APPENDIX C BIOASSAY QUALITY CONTROL PROGRAM RESULTS FHADMIN\\CORES\\EL 027-05
There are no charts for the bioassay quality control program for this semi-annual report period.
F:AADMIN\\CORES\\EL 027-05
ATTACHMENT 1 RESULTS OF THE LABORATORY BLIND DUPLICATE PROGRAM FX\\ADMIN\\CORES\\EL 027-05 ATTACHMENT I
AR EVA March 1, 2005 EL 026/05 Distribution
Subject:
Second Half of 2004, Blind Duplicate Program Results The Framatome ANP Environmental Laboratory (E-LAB) participates in a Blind Duplicate Program administered by the participating utility companies. For the second half of calendar year 2004, 99.6% of the paired sample measurement results were within the program's criteria for acceptance.
The Blind Duplicate Program began in 1979 as a cooperative effort among the participating companies. Samples are collected and split in the field and submitted to the E-LAB for analysis. The E-LAB Quality Assurance Officer verifies and reports the program results to the participants. The results are evaluated against the E-LAB acceptance criterion established in Reference 1, which states that a paired measurement is in agreement if the individual values are within +/-15% of the mean value. If this condition is not met, a two-sigma range is established for each of the results, which are in agreement if the two ranges overlap.
Table I summarized the types of media submitted as part of the Blind Duplicate Program by each participant for a total of 12 paired samples.
Table 2 presents the results of the Blind Duplicate Program by analysis type for each participating company. For the second half of 2004 program, 99.6% of the paired measurements met the acceptance criteria as specified in Reference 1. The number of paired measurements falling outside the acceptance criteria is listed before the dash (JI in each company column. For example, the number 112 should be interpreted as I paired measurements out of 2 falling outside the acceptance criteria. Totals are presented for each participating company as well as for the entire program.
REFERENCES
- 1. Framatome ANP Environmental Laboratory Manuall10, tory 99ality Assurance Plan,' Revision 8, September 10, 2004.
tistopher S~lton Quality Assurance Officer Framatome ANP Environmental Laboratory CAS/cas Attachment Distribution:
J. Raimondi J. Pelczar N. Panzarino E. Mercer (MY)
D. Perkins (SB 02-12)
M. Strum D. Montt (YR)
E. Moreno FRAMATOME ANP.
ENVIRONMENTAL LABORATORY: 29 Research Drive, Westborough, MA 01581-3913 Phone: 508 898-9970 Fax: 508 836-9815 www.us.framatome-anp.com
EL 026105 March 1, 2005 Table 1 Summary of Paired Samples Submitted July through December 2004 Sample Yankee Maine Seabrook Total Media Atomic Yankee Station Ground Water 1
0 0
1 Surface Water 2
3 4
1 9
Algae 0
0 1
1 Mussel 0o 0
1 1
Total
.3 3
1 6
12 Table 2 Summary of Paired Measurements Analyzed July through December 2004(1)
Analysis Yankee Maine Seabrook Total Type Atomic Yankee Station Ga mmF7 0178 1/52 0/104 1/234 Gross Beta 0/3 0/0 0/0 0/3 Sr-89/90V3 )
0/0 0/0 0/2 0/2 Tritium 0/3 0/1 0/2 0/6 Total 0/84 1/53 0/108 1/245 (1)The number of measurements that fail to meet the acceptance criteria is shown before the slash.
(2)The gamma numbers represent the total radionuclide measurements in a gamma isotopic analysis.
(3)The Sr-89/90 numbers represent an independent evaluation for each strontium isotope.
Appendix G Meteorological Data
Ferni 2 - 2004 Annual Radioactive Effluent Release and Radiological Environmental Operating Report In accordance with Section 5.9.1.8 of the Fermi 2 Offsite Dose Calculation Manual (ODCM), a summary file of required meteorological data for 2004 is retained on site and available upon request.
G-1
Appendix H Plant Related Isotope Detected In Environmental Air Sampling Media
Fermi 2-2004 Annual Radioactive Effluent Release and Radiological Environmental Operating Report Plant Related Isotope Detected In Environmental Air Sampling Media
==
Introduction:==
Framatome ANO, Inc., the REMP analytical laboratory, notified Detroit Edison that cobalt-60 was detected in the API-1 third quarter 2004 particulate composite air sample. API-I is located in the community of Estral Beach, NE Sector (390), approximately 1.4 miles from the Fermi 2 reactor. The laboratory was instructed to recount the sample on different equipment to confirm the activity. The sample was recounted and the count confirmed the cobalt-60 activity.
Cobalt-60 is a long lived neutron activated isotope with a half-life of 5.27 years. Cobalt-60 is periodically detected in Fermi 2 airborne effluents. In accordance with procedure 62.000.203, REMP Results Analysis - Review and Action, Section 3.3.3, if isotopes related to plant effluents are detected in environmental sample media, an investigation in the form of a situational surveillance must be initiated. The following discussion is the investigation into cobalt-60 activity detected in the third quarter particulate composite air sample of API-1.
Investigation:
The laboratory was instructed to "decomposite" the weekly air samples to determine which week the activity had been deposited. The lab counted each filter individually and determined that the filter was from the sampling period beginning on August 24, 2004. However, due to an electrical storm, API-I only operated for 25 hours2.893519e-4 days <br />0.00694 hours <br />4.133598e-5 weeks <br />9.5125e-6 months <br /> before loosing power because of a blown fuse.
Normally, a sample with this low of a volume is considered not representative and not sent to the laboratory for analysis. The individual analysis showed activity not only for cobalt-60, but also for manganese-54 at concentrations of 3.9E-1 pCi/cubic meter and 6.8E-2 pCi/cubic meter respectively. To determine if the activity detected at API-I originated from Fermi 2's effluents, two sources of data were reviewed, effluent release data and meteorological data.
Review of the effluent data for the time period of August 24 to August 31, 2004 showed no detectable activity for cobalt-60 or manganese-54. To determine what activity would had to have been released during the sampling period, to produce the measured concentrations at API-1, the following calculation was used:
Activity Released
=
Activity Concentration at Sampler Dispersion Factor (XIQ)
The following assumptions and values were used to perform the calculations:
Activity concentrations detected at API-I = 3.90E-1 pCi/cubic meter Co-60 and 6.80E-2 pCi/cubic meter Mn-54.
X/Q = 1.25E-6 sec/cubic meter.
Sampling Period = 9.23E+4 seconds (25 hours2.893519e-4 days <br />0.00694 hours <br />4.133598e-5 weeks <br />9.5125e-6 months <br /> and 39 minutes).
H-1
Fermi 2 - 2004 Annual Radioactive Effluent Release and Radiological Environmental Operating Report Co-60 Calculation:
3.90E-1 pCi/M3 = 3.90E-7 uCi/m3 3.90E-7 uCi/m3 1.25E-6 sec/m3 x 9.234E+4 sec = 2.88E+4 uCi or 28.8 mCi Mn-54 Calculation:
6.80E-2 pCi/m3 6.80E-8 uCi/m3 6.80E-8 uCi/m3 /1.25E-6 sec/m3 x 9.234E+4 sec = 5.02E+3 uCi or 5.02 mCi Review of the meteorological data indicated that the wind was not blowing in the direction of API-I during the sampling period. Figure I graphically shows the 10 meter wind rose of the wind direction during the sampling period.
10 Meter Wind Rose Wind Direction Frequency (N
41%
5.
Figure 1 H-2
Fermi 2 - 2004 Annual Radioactive Effluent Release and Radiological Environmental Operating Report
==
Conclusion:==
After evaluating the information from the investigation, it was determined that the activity detected by the laboratory in the third quarter composite air sample of API-I was not a result of Fermi 2 airborne effluents. This determination was based on the following reasons:
- 1. After the sample was "decomposited" to determine the week in which the activity was deposited, no cobalt-60 or manganese-54 activity was detected in the weekly SPING effluent sample.
- 2. The amount of activity that would had to have been released to produce the concentrations of cobalt-60 and manganese-54 at API-I was calculated to be 28.8 mCi and 5.02 mCi respectively. This amount of activity is greater than 100 times the total activity released in 2004. The total cobalt-60 activity released was 0.12 mCi and the total manganese-54 released was 0.04 mCi for 2004.
- 3. The meteorological data indicated the wind was not blowing in the direction of API-I during the sampling period.
The most probable source of the cobalt-60 and manganese-54 on the air sample media is from cross-contamination. When the air samples are collected in the field, they are sealed in petri dishes at the sample location and shipped to the lab from Warehouse B. Because the samples are sealed at the sampling location, it is highly unlikely they could become cross-contaminated during packaging and shipping. The air sample was most likely accidentally cross-contaminated at the laboratory.