IR 05000295/1987029

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Insp Repts 50-295/87-29 & 50-304/87-30 on 871005-09.No Violations or Deviations Noted.Major Areas Inspected: Chemistry Program,Including Procedures,Organization & Training & Qa/Qc Program in Lab
ML20236K719
Person / Time
Site: Zion  File:ZionSolutions icon.png
Issue date: 11/04/1987
From: Holtzman R, House J, Schumacher M
NRC OFFICE OF INSPECTION & ENFORCEMENT (IE REGION III)
To:
Shared Package
ML20236K700 List:
References
50-295-87-29, 50-304-87-30, NUDOCS 8711090320
Download: ML20236K719 (14)


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 , .h' Inspection on Octob S N and 15, 1987 (Reper'ts<No. 50-295/87029(DRSS);           s   1
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O: (No. 50-304/87030(DRSS)) y Areas Inspected: . Routine announced inspection of: 3(1) the chemistry program, g( including peccedures,s organization, and training; (2) qvimary and secondary (

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, Persons Contacted     j s  1G. Plim1,. Station Manager, CECO-Zion 1P M. Zwilling, lead Chemist    ]

1T. Rieck, Services Superintendent, Ceco-Zion l 1W.' Stone, Station QA Superintendent, CECO

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1J., Ballard, QC Supervisor, CECO 1A. Bless, Regulatory Assurance, CECO -l 1RL J..Budowle, Assistant Superintendent Technical Services, CECO 1 G. Trzyna, Rad / Chem Supervisor i V. Williams, Lead Health Physicist ' 2K.'.. Miedlar, Analytical Chemist 1

  ;C. Doi'l, Auxiliary Systems / Radiochemist   ;

L. L. Schaeve, Primary Systems Chemist i

 . D. P. Heminerle, Secondary Systems Chemist   ,

K. McEvoy, Rad / Chem Foreman  !

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M. Finney, Rad / Chem Foreman l

  .J. Etten, Laboratory Foreman .

J. Habcon,' Rad / Chem Technician (RCT) R. Russell, RCT

:P  .R. Schuster, RCT T. Ellsworth, RCT     j

f 2M. M. Holzmer, Senior Resident Inspector, NRC i Si The inspectors also interviewed other licensee personnel in various

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1 Denotes those present at the plant exit interview on October 9, 198 ! 2 Telephone conversation held on October 15, 198 l 4 Licensee Action on Previous Inspection Findings l

       ; (Closed) Open Items (50-295/86010-01; 50-304/86009-01): Licensee to develop improved procedures for control and reporting of chemistry l analytical result The inspectors reviewed the changes in the QA/QC program which has been upgraded and implemented. Control charts are j now used for most laboratory analyses, including high level baron by l auto titrator; chloride and sulfate by ion chromatography (IC);

fluoride by specific ion probe (SIP); silica, hydrazine, and ammonia ; by UV/ visible spectrophotometry; and chromate, copper, iron, magnesium, j sodiure, lithium and aluminum by atomic absorption spectrophotometry j

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  (AAS). This program is discussed further in Section l

The licensee modified the data reporting forms in response to findings ) in an INP0 evaluation.1 The secondary system data sheets in l Procedure No. ZCP-401, " Chemistry - Worksheets/ Data Forms / Logs," j Tables 34A-G dated from April 9,1986 to February 25, 1987, j

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1 Region III Inspection Reports No. (50-295/86010; 50-304/87009).  ;

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containing limiting valees for the analyses and now requiring a reviewer's signature, are set up for each system and day of the

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week. The tables for the primary system were similarly modifie _ These tables appear to be satisfactory, b .' (Closed) Open Items (50-295/86010-02; 50-304/86009-02): Licensee to increase the rate of. testing of RCTs to twice yearl The licensee % has increased the frequency of performance testing the RCTs to semiannually. Presently the tests are conducted with unknown samples made up by the Analytical Chemist and given to the RCTs by the  ! Laboratory Foreman. The present unknowns are for analyses required ! by the Technical Specification (T/S) chloride, fluoride and boron in primary matrice The program will be expanded in the next round to include other critical analyses, including lithium by AAS and chloride and sulfate for the secondary system by IC. This program appears to be progressing well, but is still under development; its progress will be examined in subsequent routine chemistry inspection I

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l (Closed) Open Items (50-295/86018-01; 50-304/86017-01): Verify the I Co-60 calibration calculations and analyze a spiked liquid sample supplied by the NR .The inspectors' reviewed licensee documenta- ~ tion on the calibration that indicated the Co-60 calibration was correct. Also, the results of the Co-60 in a spiked sample supplied by the NRC Reference Laboratory showed agreement (Table 1). It appears that the disagreement was due to counting a low-level sample (liquid radwaste) without subtracting the licensee's rather substantial Co-60 background from the relatively small Co-60 peak in the sample. This appeared to be a generic problem with the licensee I and was a finding in a recent INP0 evaluation. The licensee was L working on a procedure to make systematic corrections for background ' radiation. This will be followed under Open Items No. (50-295/87029-01; 50-304/87030-01) (Closed) Open Items No. (50-295/86018-02; 50-304/86017-02): Analyze a liquid discharge sample for gross beta, H-3, Sr-89 and Sr-90 and report results to the Region. As shown in Table 1, the licensee's results and those of the NRC Reference Laboratory are in agreement I for the gross beta and H-3 in the split sample. However, because of the low levels of the Sr-89 and Sr-90 activities, no comparison is possible. In the future, low-level split samples will be made from diluted reactor coolant with measurable Sr-89 and Sr-90 activities.

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< (Closed) Open Items No. (50-295/86018-04; 50-304/86017-04):

Recalibrates gas geometries within two weeks after receipt of standard. The inspectors reviewed the gas recalibrations completed as of August 13, 1986. The licensee had used the new calibration data to recalculate the activities in the intercomparison samples of . Inspection Reports No. (50-295/86018; 50-304/86017), which then gave good agreement with the NRC results. Further, in a crosscheck with a vendor (Analytics, Inc.), all valuas were in agreemen ,

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K (Closed) Open Items' No. (50-295/86018-05; 50-304/86017-05): Licensee to complete revisions to Procedures ZCP-530-13 and ZCP-531-7 by September 1,~1986. The inspectors reviewed the revisione.to the data logsheets for these procedures in Procedure ZCP-401, " Chemistry - Worksheets/ Data Forms / Logs," Tables 76 (Packard Tricarb Liquid Scintillation Counter Performance . Log, Revision 2, September 22, 1986) and Table 81 (Performance Test : Log for Eberline Model SAC-4 Scintillation Counter, Revision 2, September 22, 1986). The revisions, which require additional data on the' sheets, such.as mean and control limits, appeared to be . satisfactor .i Management Controls, Organization and Training - The Chemistry Group management structure is essentially unchanged since c the previous inspection in this area.2 . A new Laboratory Foreman has replaced the previous one, who is now a Health Physics Forema The' Rad / Chem Department lost one RCT and now has 3 RCTs continue to be rotated between health physics and chemistry which makes it more difficult to maintain laboratory continuity and RCT proficienc Licensee representatives recognize the problem and noted that the company is presently trying to resolve i The licensee's RCT training program has been reviewed by INP0 and certification is expected in the near futur No violations or deviations were identifie c Water Chemistry Control Program The inspectors reviewed the secondary water system based on A0P 5.2,

 '" Secondary Sys'am Chemistry Excursion," Revision 0, June 17, 1987 and ZCP 311-1, jecondary System Analysis Requirements," Revision 7, February 14, 1987. Steam Generator blowdown is monitored for pH, cation and specific conductivity, sodium, chloride, sulfate and silic Feedwater is tested for pH, dissolved oxygen, iron, copper and hydrazin Condensate is monitored inline for dissolved oxygen and sodium. A0P f delineates parameters monitored for each system, normal values, action
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levels and associated operational limit From a review of selected trend charts, chemical parameters are maintained well below Action Level j One and excursions beyond this level are very infrequent, for short j duration and are due to a change in plant operating status, such as j startup or a power increase. The trend charts suggest that the chemical ; parameters monitored are'well controlled and conform to the EPRI Owners l Group Guidelines (PWR Secondary Water Chemistry Guidelines, Revision 1, j June 1904) The plant recently installed new secondary system monitoring j panels obtained from the Marble Hill plant. All of the inline monitors ) in these panels were upgraded to state of the art instrumentation, j Feedwater, condensate, main steam and heater drains are connected to i these instrument l 2 Ibi l

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k}. In general, the various N rameters representing contamination are well controlled. The plant has not been out of Technical Specifications limits for chemistry and presently does not use the performance indicator of time out-of-specificatio The water quality control program appears to be satisfactory and is very : usefu ~ i '

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No violations or deviations were identifie ' Implementation of the Chemistry Program The inspectors reviewed the chemistry programs including physical facilities and laboratory operation Housekeeping was good and bench space was adequate for the analyses performe The hot lab was located !

 -in the radiologically controlled area of the plan The laboratories were'well equipped including Dionex Ion chromatography equipment, uv/ visible spectrophotometers, an atomic absorption spectrophotometer, gas chromatography and automatic titration equipment. The licensee recently acquired a Waters liquid / ion chromatography' system that is j capable of performing a variety of analyses. Development work is j underway on boron analysis utilizing the Waters Model 410 differential l refractometer as the detector. This system has considerable potential j for the analysis of.both anions and cations,   j
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A computer generated instrument calibration schedule has been develope ; An instrument log book is used to track both in house as well as vendor maintenanc Calibration stickers are used to certify that instruments have been calibrated and indicate the .next calibration date. Reagents were properly labeled with expiration dates listed and no outdated reagents were observe The inspectors observed several RCTs analyze routine samples on various instruments. They appeared to be generally knowledgeable about the work i and followed the procedure . Overall, the laboratory appeared to be adequate for the proper operation of the plant and to be functioning satisfactoril No violations or deviations were identifie j Nonradiological Confirmatory Measurements

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The inspectors submitted chemistry samples to the licensee for analysis as part of a program to evaluate the laboratory's capabilities to monitor ) ' nonradiological chemistry parameters in various plant systems with respect to various Technical Specification and other regulatory and administrative 1 requirement These samples had been prepared, standardize.d, and j periodically reanalyzed (to check for stability) for the NRC by the Safety 1 and Environmental Protection Division of Brookhaven National Laboratory (

 (BNL). The samples were analyzed by the licensee using routine methods and j equipmen ]

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The samples were di'uted by licensee perscnnel as necessary to bring the concentrations within the ranges' normally analyzed by the laboratory, and '

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runlin' trip ~licate in a manner similar to that of routine samples. The results are. presented in Table 2 and the criteria for agreement in

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Attachment 2. These criteria for agreement are based on comparisons of the'mean values and estimates of the standard deviations (s.d.) of the measurements. Consideration was given to the fact that the uncertainties ' ..

 :(s.d.)'of the licensee's results were not necessarily representative of f the laboratory's because they were obtained by one analyst over a short period of tim Consequently, when the licensee s.dc was less than that of BNL, and a disagreement resulted, the BNL value was substituted for that of the licensee in calculating the s.d. of the ratio Z (S i Attachment 2). {
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The licensee also prepared two samples to be split with BNL. To these were-added analytes supplied by the inspectors. Reactor water was spiked with the anions chloride and sulfate, and a sample of feedwater was spiked with copper, iron, and chromium ions. The licensee will determine the concentrations of the analytes in each and the results will be sent to Region,III for' comparison with the values determined by BNL. This will be followed under Open Items No. (50-295/87029-02; 50-304/87030-02). 1

 .The licensee analyzed eleven materials at three concentration each. Of the initiai 33 analyses, 28 were in agreement (85%) and five were in .

disagreement with the BNL data. The disagreements included all three copper concentrations, the low fluoride and the middle hydrazine. The licensee was experiencing difficulties with the atomic absorption spectrophotometer (iron and copper) and decided to wait until the vendor i serviced the instrument before completing those analyses. After repairs, the three copper reanalyses were in agreement. Reanalysis of the intermediate hydrazine concentration also showed agreement. The low ' fluoride concentration was prepared at a higher dilution for reassay and

 .this concentration was read from a different portion of the calibration curve (100 ppb instead of 200 ppb). At the lower concentration, the low fluoride sample was in agreement, suggesting that the licensee's ,
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calibration curve might be inaccurate in the higher range (200 ppb).

The inspectors were concerned that the LLD of the fluoride was too hig Procedure ZCP 120-1, " Fluoride Determination by Ion Specific Probe," Revision 3, April 19, 1985 states that the LLD for fluoride is 50 ppb, although the curve is calibrated to 33 ppb and could be calibrated to j approximately 20 ppb. The calibration range is given as 50-320 ppb which ! is much higher than necessary and does not cover the range in which 5 fluorf Je would be expected to be found (<50 ppb). In addition, plotting the curve on linear graph paper instead of semi-log could improve the 1 H readability of the graph and the accuracy of the analysis. Licensee i representatives agreed to look into these concern The silica analyses, although in agreement, exhibits a low bias at the ! low and medium concentrations that indicates a problem may exist with the l assay. Using independent controls along with a new calibration curve prepared from fresh standards could improve this assa l s j g j L_-______ __ _ \

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The~ low'leve'l iron analysis, although in agreement, had considerable I imprecision (4.67 ppb i 2.4) which represents a coefficient of variation I of-(51%) suggesting that some difficulties still exist with this assa ] A'different' standard for chromium is needed. The. licensee uses a j dichromate material that is the same 'as is added to cooling wate ! The licensee agreed to consider obtaining chromate (or chromium) from another' source, e.g., a vendor supplied atomic absorption standar The licensee utilizes multiple point calibration curves where possible, maintains control charts, uses st;ttistical parameters to control assays and is ' investigating the use of independent controls in place of. controls prepared from calibration material. These controls would be used along with the calibration checks to ensure that the calibrator solutions have not detectorated. The licensee's precision was equal to or better than that for BNL and most of the analyses had a bias of <15%. The licensee's performance following reanalysis of those analyses that were in disagreement'.was 33 of 33 or 100%. Progress in the fluoride analysis and the acquisition of chromate and {

 ' independent' controls standards will be followed under Open Items i No. (50-295/87029-03; 50-304/87030-03).

No' violations or deviations were identifie . Implementation of the QA/QC Program in the Chemistry Laboratory The inspectors reviewed the nonradiological QA/QC program in the laboratory, as noted in Section 2a. The program is required by the Corporate directive, Nuclear Stations Chemistry Quality Control Program, NSDD-25, January 1987, and implemented in procedures for the various analyses. The inspectors discussed the following concerns with licensee representatives:

 (1) Control charts do not identify the bases for obtaining the control parameters (x bar,s) used and the licensee does not clearly specify criteria for renormalization of the chart For some analyses the licensee does not maintain a table of the data used to calculate the actual parameter. (2) For the boron analysis the control charts are not statistically based but are arbitrarily set at 10 ppm, a method that provides no information on the statistical variability of the measurement -
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process. (3) Data used to prepare calibration curves are not always maintained but are discarded after the curve is diawn. The inspectors - also noted that control charts were illegible and difficult to rea The inspectors reviewed the station's interlaboratoring comparison program which is managed by the licensee's corporate Technical Support Cente Unknowns are run on a quarterly basis. A review of data covering March 1986 through June 1987, indicetes that the licensee's analytical )

. performance is improving but several analyses still have a high relative error. This program appears to be well managed and should assist the station in improving the precision and accuracy of routine chemical analyses. Performance in this program will be followed in the routine chemistry inspection ,
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   , Thelinspectors reviewed the licensee's RCT_ performance program ,ZCP:1021-3, !
   ." Radiation Chemistry Technician; Proficiency Check Program,": Revision 0, .;

1 - Mayc5,~ 1987. Selected unknownsLfrom the list.of T/S analyses are prepared a, -

   ' in-house and distributed to the RCT's for analysis on a semiannual V

   -basis. Results of the program indicate that most RCT's,have little
 ,  , idifficulty in, passing. Acceptance criteria'is arbitrarily establish'ed at t 10.%,; except for' boron which.is i 5%. Statistically based ' acceptance
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criteria'would provide more accurate: assessment'of.the RCT's capabilitie ,

  ,', This program.will be examined in subsequent; routine chemistry inspection >
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The licensee's.QA/QC program has progressed utisfactorily.since the '

   ' previous. inspection and it appears that'it will be.a good-progra .
   .No-v'folations or deviations were. identifie >

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  ' 8. . Audits and Appraisal .The inspectors reviewed the latest available corporate audit relating to
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Chemistry 22-86 II conducted.during September 23-26, 1986. One finding-

   .concerning balance. calibration was made and resolved-in a timely manne '
   . The audit : report . indicates that the' licensee's mechanisms for. responding ;
   ,to audit findings are adequat '
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No violations or deviations were identifie I y Environmental Mon'itoring: TLD Collocations

   'The inspector's reviewed the data on the locations of the four collocated NRC TL0s'and confirmed that they were' located on the same structures as
   .theslicensee's. A few minor discrepancies in described azimuth were n'oted and will be resolve t    ..No. violations or deviations were identifle H
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  -1 Open Item n
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Open items are matters which have been discussed with the licensee, which

 '  will be reviewed further by the inspector, and which involve some action
   . on the part of. the NRC or licensee, or both. Open items disclosed during the-inspection?are discussed in Sections 2 and I
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1 Exit Interview-The scope and findings of:the inspection were reviewed with licensee '

   ; representatives (Section llet the conclusion of the inspection on
   ,.0ctober 9, 1987. The' inspectors discussed the Open Items in Section 2  !

Dand observations on quality control measurements program and confirmatory j

   . measurements. Licensee' representatives. agreed to improve the QC chart 1 quality and to consider other modifications of the program, as discussed I in' Section 7. The inspectors acknowledged considerable improvement in the j i

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chemistry program since the previous inspection, but again noted their concern over the rotation of laboratory personnel between chemistry and Health Physics (Section 3).

During the exit interview,.the inspectors discussed the likely informa-tional content of the inspection report with regard to documents or processes reviewed by the inspectors during the inspection. Licensee representatives did not identify any such documents or processes as proprietar Attachments: 1. Table 1, Confirmatory Measurements Program Results, 3rd Quarter 1986 2. Attachment 1, Criteria for Comparing Analytical Measurements (Radiological) Table 2, Nonradiological Interlaboratcry Test Results, October 5-9, 1987 4. Attachment 2, Criteria for Comparing Analytical Measurements (Nonradiological) l

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TABLE 1

:;-     U.S NUCLEAR REGIILATORY COMMISGIOM- ' OFFICE'OF INSPECTION AND ENFORCEMENT
    ' CONFIRMATORY MEASUREMENTS PROGRAM FACILITY: ZION
     .FOR-THE 3 QUARTER OF 1986
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    -- - - -- N P C ---- --- - ----LICENSEE -
        ---L'ICENSEE NRC----

, $ AMPL ISOTOPE' RESULT 'EPROP RESU ERROR RATIO RES- T L SPIVED.CO-60 7.3E-05 i,4E-06 7.3E-05 O.OE-01 1.OE 00 5.2E 01 A L WASTE . BETA l'.2E-05 5.0E-07 9. 4 E-06 0.0E-01 7.9E-01 2,4E 01 lH-3 4.7E-02- 7.OE-04 4.SE-O'2 0.OE-01 1.OE 00 6.BE 01 A SR-09 -5.-0E-09- 6.OE-09 (6.6E-09 0.OE-01 0.OE-01 -8.3E-01 N SR-90 3.OE-09 3.OE-09 <3.2E-09 0.OE-01 1.1E 00 1.OE 00 N T TESr,RESULTS

- A= AGREEMENT D= DISAGREEMENT . .

t= CRITERIA' RELAXED N=NO COMPARISON

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ATTACHMENT l'

   ' CRITERIA FOR COMPARING ANALYTICAL MEASUREMENTS
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 ;This attachment provides criteria for comparing results of capability tests-and verification measurements. The criteria are based on an empirical'

relationship which combines prior. experience and the accuracy needs of this progra .

 -In these criteria, the judgment limits are variable'in relation to the comparison of the NRC's'value.to its associated one sigma uncertainty. As that ratio,
 . referred to.in this: program as " Resolution", increases, the acceptability of a licensee's measurement should be more selective. Conversely,; poorer agreement should be considered acceptable as the' resolution decreases. The values in.the ratio criteria may be rounded to fewer significant figures reported by the NRC
 : Reference Laboratory, unless such rounding will result in a narrowed category of  i acceptanc i RESOLUTION  RATIO = LICENSEE-VALUE/NRC REFERENCE VALUE Agreement

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4- 7 0. 5 - ; 8- 15 0.6 - 1.66 0.75 - 1.33 'I

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.i 51 - 200   0.80 - 1.25 200 -   0.85 - 1.18 Some discrepancies may result from the use of different equipment, techniques, and for some specific nuclides. These may be factored into the acceptance criteria and identified on the data sheet.

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TABLE 2 1 Nonradiological Interlaboratory Test Results i Nuclear Generating Station, Units 1 and 2 j October 5-9, 1987

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Analyte AnalyQs- Dilu- NRC Licensee Ratio Comparisons; Method tion, 1:x Y i s.d.(n) X i s.d.(n) Z i s.d. i 2 Concentration, ppb

 ~

F SIP 100 231 1 (7) 106.3 i 1. 2 0.806 1 0.028 D ~! 1000 4 .9 (7) 39.0 1 2. 0 0.897 1 0.060 A 1000 83.5 1 2.8 (8) 78.0 1 3. 0 0.934 1 0.048 A (repeat) 100 231 i 5 192 1 .831 1 0.028 D*

  (repeat 2) 200 115 .957 i 0.033 A Cf IC' 2000 12.0 1 1.6 (7) 9.90 1.39 0.825 1 0.160 A ,

2000 1 .6 (7) 19.0 t 0.46 1.016 1 0.041 A+ ! 2000 40.3 1 1.1 (8) 37.0 1 1. 6 0.918 1 0.047 A Sulfate IC 2000 10.0 1 0.45(7) 10.7 1 1. 2 1.070 0.129 A 2000 20.5 i 1.2 (8) 20.0 1 0.35 0.976 0.060 A 2000 40.4 1 1.5 (7) 37.7 1 .933 1 0.053 A Silica Spec 500 108.6 1 11.2 (7) 89.0. i 4.8(6) 0.820 1 0.095 A+ 500 218 14 (7) 191.2 1 9.7(6) 0.876 1 0.072 A+ ' 500 320 1 10 (7) 295. i 5.1(6) 0.922 i 0.043 A* Cu AAS 1000 4.68 1 0.24(12) 5.23 1 0.06 1.118 1 0.077 A* 1000 9.66 1 0.49(14) 10.1 i 0.15 1.042 0.055 A i 1000 14.5 1 0.6 (12) 15.6 i .076 1 0.056 A Fe AAS 1000 4.89 1 0.35(13) 4.67 1 .955 i 0.496 A 1000 9.55 1 0.34(14) 10.3 1 0.67 1.075 1 0.080 A 1000 14.7 1 0.42(13) 14.8 1 1.65 1.007 1 0.116 A i Na AAS 500 9.16 i 1.0 (6) 9.0 i .983 1 0.110 A l 500 18.5 i 1.6 (6) 1 i .029 0.089 A ! 500 28.8 1 1.6 (6) 28.7 1 .997 i 0.092 A Cr AAS 100 51 1 (7) 44.2 i 1. 8 0.867 1 0.078 A* ! 100 94.1 1 (7) 100.6 1 7. 0 1.069 i 0.082 A ! 100 143 1 (7) 152 1 13 1.063 1 0.060 A {

\     2 , 3 0.937 1 0.060 A Hyd- Spec 1000 22.3 1 1.4 (7)

razine 1000 56.9 1 0.7 (7) 50.2 1 .882 1 0.024 0 i

        '

1000 104 i (7) 105.8 1 .017 1 0.015 A (repeat) 1000 56.9 i 0.7 (7) 5 .0 0.967 1 0.037 A l NH Spec 100 876 1 5 (7) 941 1 6 .074 1 0.098 A 1

100 3140 1 260 (7) 2816 1 143 0.897 1 0.087 A 100 9380 t 850 (7) 9030 1 380 0.963 i 0.096 A l

- _ _ _ _ -

-- - _ _ _ - - - - - - . _ _ - - - - . - - - .

      - _ _ - _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ ,
'
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TABLE 2 Nonradiological Interlaboratory Test Results Nuclear Generating Station, Units 1 and 2 October. 5-9, 1987 Concentration, ppm-B' Titr 1 1000 1 1 (7) 1006 1 1. 0 1.006 1 0.010 A 1 3024 i 4 (7) 3003.7 1 1. 2 0.993 1 0.015 A 1 4947 1 6 (7) 495 .001 1 0.018 A Value'i standard deviation (s.d.); n is number of BNL analyse The number of licensee analyses is 3 unless otherwise noted, Analytical methods: Titr - titration IC - Ion chromatography Spec - Spectrophotometric SIP - Specific ion probe AAS - Atomic absorption Spectroscopy (furnace) A = Agreement D = Disagreement j A+ = Borderline Agreement

* Substituted the BNL uncertainty for licensee's uncertaint l
           !

d

_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ -

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_ - _ _ z--., - - _ q p.; -

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ATTACHMENT 2-  ! i \ , Criteria for Comparing Analytical Measurements : .l

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       .
        -

This attachment provides criteria for' comparing results of the ca'pabilit iThe acceptance, limits are based on the uncertainty.(standard deviation)ofy the- test ratio of the licensee's'mean value (X) to the'NRC mean.value (Y),'where

     .
  (1)' Z:='X/Y is the ratio, and
  .(2) S -is the uncertainty.of the ratio determined from the -

pfopagationoftheuncertaintiesoflicensee'smeanvalue,

  '
.

Sx , and of the'NRC's mean'value, S .1 Thus, y S2 32- 32: 1 z _ - -x p- pr , y2v,' so that 'l S2 a  ! S'=.2 *X2:[1 +'32D'

2-- ' Y2) The results are considered to be in agreement when the bias in the ratio l

  .(absolute value of difference between unity and the-ratio) is less than or equal to twice the uncertainty in the ratio, l.1-Z.I 5 2*S z' National Council on Radiation Protection and Measurements, A Handbook of Radioactivity Measurements Procedures, NCRP
  ' Report No. 58, Second Edition, 1985, Pages 322-326 (see  y Page 324).

. 4/6/87

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