ML20245J243

Insp Repts 50-456/89-04 & 50-457/89-04 on 890110-13 & 18-20. No Violations Noted.Major Areas Inspected:Chemistry Program, Including Procedures,Organization & Training,Primary & Secondary Sys Water QC Programs & QA in Lab

ML20245J243
Person / Time
Site:	Braidwood
Issue date:	02/17/1989
From:	Holtzman R, House J, Schumacher M NRC OFFICE OF INSPECTION & ENFORCEMENT (IE REGION III)
To:
Shared Package
ML20245J228	List: ML20245J223 ML20245J243
References
50-456-89-04, 50-456-89-4, 50-457-89-04, 50-457-89-4, NUDOCS 8903060215
Download: ML20245J243 (14)

See also: IR 05000456/1989004

Text

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.. U.- S. NUCLEAR REGULATORY COMMISSION-

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REGION III-

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Reports No. 50-456/89004(DRSS); 50-457/89004(DRSS) .,[

' Docket Nos.. 50-456;.'50-457 Licenses No. NPF-72; NPF-77- -

Licensee: Commonwealth Edison Company

Post Office Box 767

Chicago,-IL 0690 g

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= Facility Name: Braidwood Nuclear Power. Station, Units 1 and 2 l

Inspection At: Braidwo;od:-Site,.Braceville, Illinois .

! Inspection Conducted: January 10-13 and 18-20, 1989.(Onsite)

Inspectors: R. B. Holtzman

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J. E. House .2- F1- ? i

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Approved By: M. Schumacher, Chief

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Radiological Controls and Date

Chemistry Section'.

Inspection Summary

Inspection on January 10-13 and 18-20, 1989 (Reports No. 50-456/89004(DRSS);  !

No. 50-457/89004(DRSS) 't

Areas Inspected: Routine announced inspection of: (1) the chemistry program,

including procedures, organization, and training (IP 84750); (2) primary and

secondary systems water quality control' programs (IP 84750); (3) quality

assurance / quality control program in the laboratory (IP 84750); and

(4) nonradiolgical confirmatory measurements '(IP 79701). .

Results: The licensee has an extensive water quality control program that ,

?- conforms to the EPRI Steam Generator Owners and Primary Systems Guidelines.

The' steam generator (S/G) blowdown showed moderate, but decreasing levels

of chloride and sulfate (but generally within the EPRI guidelines), apparently

due to. cleanup of the relatively new reactor systems. The nonradiological

confirmatory measurements results were good, but demonstrated some weaknesses

in the QA/QC program. The licensee identified weaknesses in the measurements

program and corrected them.

No violations or deviations were identified.

8903060215 890221 "

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DETAILS

1. Persons Co~ntacted

1R. Legner, Assistant Superintendent-Technical Services, Bwd

IR. E. Aker, Radiation-Chemistry Supervisor, Bwd

1J. R. Petro, Assistant Rad Chem Supervisor, Bwd

1J. B. Cronin, Station Chemist, Bwd

IW. E. Lloyd, Chemist, Bwd

1P. L. Barnes, Regulatory Assurance Supervisor, Bwd

1P.-Holland, Regulatory Assurance, Bwd

1E. W. Carroll, Regulatory Assurance, Bwd

1R. D. Kyrouac, QA Superintendent, CECO

1M. J. Harper, QA Inspector, CECO

1L. W. Raney, Nuclear Safety, CECO

G. Vickery, Chemist, Bwd

R. F. Rysner, Chemistry Engineering Assistant, Bwd

R. H. James, Chemistry Engineering Assistant, Bwd

J. McLenighan, Chemistry Technician (CT), Bwd

J. Price, CT, Bwd

D. Hildson, CT, Bwd

1T. M. Tongue, Senior Resident Inspector, NRC -

2Present at the Exit Meeting on January 20, 1989.

The inspectors also interviewed other licensee personnel in various

departments in the course of the inspection.

2. Licensee Action on Previous Inspection Findings

a. (Closed) Open Item (50-456/81999-01): NRC to collect water samples

from Braidwood city wells and wells from a farm in Wilmington,

Illinois after the Braidvood Station is in operation. Samples were

collected from the city wells and the farm. Gamma scans and

analyses for H-3, Sr-89 and Sr-90 were done by the NRC Reference

Laboratory, RESL, Idaho. No appreciable levels of reactor produced i

activities were found, as shown in Table 1. Further, gamma scans

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with longer counting times done in the Region III laboratory showed l

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the Minimum Detectable Activities (MDA) of the Cs-137 and Co-60 to

be at about 11 pCi/ litre. No activity from Cs-137, Co-60, H-3,

Sr-89, or Sr-90 was identified. Letters from the Region III Office

will be sent to the Mayor of Braidwood and to the owners of the farm j

to inform them of the findings.

b. (Closed) Open Item (50-456/87008-01; 50-457/87007-01): Licensee

to analyze a spiked sample from RESL for Fe-55 and reported the 1

results to Region III. The licensee's analyses performed by its

contractor (SAIC) was 30% greater than that of the NRC reference

laboratory (RESL). This disagreement, may have been caused by the

, contractor's use of an x-ray analysis. The licensee subsequently

analyzed a split radwaste sample and a spiked sample from RESL. 1

These are discussed in the following section (2.c).  !

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c. (Closed) Open Item (50-456/88017-03; 50-457/88817-03): The licensee

to split and analyze a radwaste liquid sample for gross beta, H-3,

Sr-89, Sr-90 and Fe-55 and report the results to the Region III

office for comparison to those from RESL. The results of the analyses

are given in Table 2 (" Split Radwaste"). The gross beta and H-3

results are in agreement based on the acceptance criteria in

Attachment 1, while the Sr-89 and Sr-90 results were not compared

due to poor statistics; the Fe-55 value is a disagreement. The

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problem appeared to be due to the low concentrations of the nuclides

in the sample which was exacerbated by the submission of too little

sample to the contractor laboratory. Subsequently, the NRC submitted

a spiked sample to the licensee for analysis. The results in the

third' group in Table 2, resulted in agreements in the Sr-89

and Sr-90, but still a disagreement for the Fe-55 value. However,

the licensee vendor reanalyzed the Fe-55 in the radwaste split

sample and obtained an agreement (Liquid Radwaste rerun) shown as

the last item of Table 2.

3. ManagementControls, Organization,andTraining(IP84750]

The management structure of the Chemistry Group was substantially modified

since the previous inspection in this area,1 and is still in a state of.

flux. The most significant recent event has been the dropping of the

rotation of the Rad-Chem Technicians (RCT) between health physics and

chemistry and the permanent assignment of 21 of them as Chemistry >

Technicians (CT) to the chemistry laboratory. Currently 13 are

qualified as technicians under ANSI N18.1, 1971. Further, the Chemistry

Department staff is also being reorganized. At present the Station

Chemist position has been replaced by the newly-appointed Assistant

Rad-Chem Supervisor who reports to the Rad-Chem Supervisor and is

supported by four Chemists, four Engineering Assistants (EA) and

three chemistry foremen. They are planning a division into two groups,

Operations and Analytical under the Chemistry Supervisor.

The inspectors looked into the qualifications of the new supervisor for

Chemistry. He has a Bachelors degree in biology with a minor in

chemistry, and has been with the company in various capacities

since 1974 in environmental affairs and the last three years as the

Radwaste Planner (Coordinator). He has good supervisory experience in t

the related field of radwaste, and will have the support of experienced

Chemists and EAs, including that of the former Station Chemist. He noted

that until he has had more experience with chemistry (for about a year),

he will not make any decisions without help from the staff. Most of the

signoffs on data and decisions are riade by the staff members, in any case. .

It appears that he should be able to supervise the department

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satisfactorily. The separation of the technicians should result in

improved technician proficiency, laboratory continuity and a reduction

in the burden on the laboratory supervisors to continually train and

track the proficiencies of a large number of technicians.

1 Region III Inspection Report Nos. (50-456/87046; 50-457/87047).

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L , The' Chemistry Technician training program was accredited by the National

H . Nuclear Accrediting Board of_INP0 on October 21, 1988.

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No violations or deviations were identified.

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'.4. Water Chemistry Control Program (IP 84750)'

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The inspectors reviewed t'he water chemistry control program based on

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the~ corporate directive NO Directive N0D-CY.1, "PWR' Secondary Water

Chemistry Control Program," Revision 0,. March 22, 1988 (revision of i;

,the previous NSD Directive NSDD-S01) and, implemented in BwCP PD-4,

"Braidwood Station Secondary Water Chemistry Program,"' Revision _4,

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August 22,.1988. :This document commits the. licensee to and is

consistent with the EPRI.0wners Group Guidelines. Approval to waive _ _

the: guidelines must come from the Vice President-PWR Operations or the,

General Manager-PWR Operations.

-In-line monitor's: provide' data for secondary wat'er systems including

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condensate, feedwater and main steam. Chemistry parameters tracked

include pH, conductivity, dissolved oxygen, hydrazine and sodium. The

steam generator blowdown (S/G BD) sample panel is located in the

chemistry laboratory. The panel's in-line monitors provide data on

conductivity, pH, sodium and dissolved oxygen levels. The in-line

instrumentation data from the secondary and S/G BD panels are transmitted-

to Autograph 800 Dataloggers located in the laboratory area; the data are

sampled and processed by computer. Water _ chemistry parameters are

monitored daily by Chemistry.and Operations.

Trend charts for secondary water quality lare maintained by the licensee.

A review of selected data for the previous year indicated that plant-

water quality is. fair. Sulfate, chloride, conductivity and silica

levels have been high (near the Action Level 1 values) and sulfate has

risen significantly above the guideline levels on.several occasions.

Other parameters, such as sodium and chloride, have remained generally

within the guidelines. As this is a new plant and systems are undergoing

a general cleanup, secondary water. quality should improve with time. The

levels parallel those of other plants in the same time frame relative

to startup. Feedwater metals are not presently analyzed awaiting

installation of the filtration system for dissolved and suspended

metals. This is to be accomplished during the next refueling outage.

This will be reviewed in subsequent inspections.

Various levels of management review the chemistry parameters and their

trends. Chemistry prepares a status sheet for the plant morning meeting

with a copy to Operations and the Plant Manager. Chemistry trends are

also submitted to corporate management in a monthly report.

The water quality control programs appear to be satisfactory and

well run.

No violations or deviations were identified.

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5. Implementation of the Chemistry Program (IP 84750)

The inspectors reviewed the chemistry programs, including physical

facilities and laboratory operations. . Housekeeping was good and

bench space was adequate for the analyses performed. The laboratories

were well equipped. The hot laboratory has acquired three PC

computer-controlled Dionex AI 400 Ion Chromatography used for anion

and cation analyses. One system uses tetraborate gradient eluant for

anion analyses. The licensee also uses an inline IC system for anion

and cation analyses on the S/G BD.

The inspector observed several cts analyze several of the confirmatory

measurements samples on the ion chromatography, and the boron autotitrator.

They appeared to be generally knowledgeable about the work and followed

the procedures. They appeared to do well in the analyses.

Overall, the laboratory appeared to be adequate for the proper operation

of the plant and to be operating satisfactorily.

No violations or deviations were identified.

6. Nonradiological Confirmatory Measurements (IP 79701)

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 requirements. These samples had been prepared,

standardized, and periodically reanalyzed (to check for stability)

for the NRC by the Safety and Environmental Protection Division of

Brookhaven National Laboratory (BNL). The samples were analyzed by the

licensee using routine methods and equipment.

The samples were diluted by licensee personnel as necessary to bring the

concentrations within the ranges normally analyzed by the laboratory, and

run in triplicate in a manner similar to that of routine samples. The

results are presented in Table 3 and the criteria for agreement in

Attachment 2. These criteria for agreement are based on comparisons of

the mean values and estimates of the standard deviations (SD) of the

measurements. Consideration was given to the fact that the uncertainties

(SD) of the licensee's results were not necessarily representative of the

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laboratory's because they were obtained by one analyst over a short

period of time. Consequently, when the licensee SD was less than that of

BNL, and a disagreement resulted, the BNL value was substituted for that

of the licensee in calculating the SD of the ratio Z (S in Attachment 1).

Additionally,arelativestandarddeviation(SD)of3%isconsidered

acceptable for all analyses except boron.

l The licensee will also prepare a sample of secondary system water spiked

with fluoride, chloride and sulfate to be split with BNL. The licensee  ;

will determine the concentrations of the analytes and the results will be  !

sent to Region III for comparison with the values determined by BNL. This

will be followed under the Open Item Nos. (50-456/89004-01;

50-457/89004-01).

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L The licensee determined 11 analytes at three concentrations each. Of the

l initial 33 analyses 24 were in agreement (73%). The chloride results

showed an decreasing bias with increasing concentration, which indicated

contamination of the dilution water. The licensee confirmed this

indication by showing the blank to contain over 2 ppb; the blank also

showed the presence of fluoride, consistent with the high biases in the

lower-level samples, even though in agreement. The blank correction

improved but did not fully compensate for the low-level chloride bias.

The silica results showed substantial negative biases. This effect

appears to have been due to inaccuracies caused by the low absorbances

when using a 1-cm path length sample cell. Repetition of the analyses

using a 5-cm cell resulted in agreements with very small biases.

There are possible problems with the calibration techniques. The

low-level lithium disagreement may have been caused by sample

concentrations below the calibration range or by the licensee's use of a

linear calibration curve when the instrument is actually nonlinear.

Reruns in the range of calibration showed agreement. The low-level

sodium was in disagreement, but appears to have been resolved on rerun.

The cause of the ammonia disagreement was not ascertained, but

two results with low biases suggests that the standard is high.

The boron analyses of the two lower-level samples showed a nega+.ive

bias of about 4%. This is substantial in view of the inherently high

precision of the analytical method. In this analysis the licensee used

a dead-stop endpoint of pH 8.6 which is consistent with the inflection

point on the titration curve. Similar negative biases were observed at

other licensees in Region III. The source of the bias has not yet been

ascertained; but BNL is investigating the problem.

The licensee will modify the silica procedure to use the 5-cm cell for

low-level measurements and to check the water blanks on the IC daily, and

examine the chloride biases. These will be followed in subsequent

inspections under Open Item Nos. (50-456/89004-02; 50-457/89004-02).

Overall, the results of the analyses were fairly good. Laboratory

personnel demonstrated a willingness and good ability in determining the

causes of the disagreements,

llo violations or deviations were identified.

7. pplementationoftheOA/QCProgramintheLaboratory(IP84750)

The inspectors reviewed the chemistry laboratory quality assurance program

as specified by Nuclear Operations Chemistry Quality Control Program,

Revision 2, March 15, 1988. The licensee maintains statistically based

cortrol charts on which the mean i 2 standard deviations (SD) are plotted.

Independent controls are in use and this data is used in preparing control

charts. The inspectors noted to the licensee that several charts ,

currently in use lacked a mean value line although this value was on the t

accompanying data sheet. The licensee agreed to review and correct the

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. charts. Multiple point calibration curves are in use for'a11' assays.

Curves for UV/VIS spectrophotometric assays (Beckman DU 30

Spectrophotometer) are calculated by a linear least squares reg'ression

, analysis from'4 points not including zero. The inspectors noted'that the

zero point should be included in the analysis and the licensee. agreed to

investigate incorporation of.this point into the curve fitting procedure.

Atomic absorption (AA) analyses use a-4 point least squares curve derived

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l from a computer' external to the AA instrument. The ion chromatograph

L (Dionex Auto Ion 400) uses a three point curve but a least squares fit is.

not performed. Instrument calibration procedures' appear.to be adequate.

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l The licensee's Interlaboratory comparison program is managed by the .

I corporate Technical Center for all stations. Data for the first

three quarters of 1988 indicate an improvement in licensee's performance.

First quarter agreements were 32%, second quarter 68% and the

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third quarter results showed 100% agreement. .The intralaboratory

. comparison program is defined by BwCP PD-8, Braidwood Station Chemistry .

Performance Evaluation Program, Revision 4, August 22, 1988. Technicians

are required to be tested annually on a variety of analyses including

, those required by Technical Specifications. A statistically derived

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', acceptance criterion is used (mean +.2 SD). Technicians whose results

fall outside of these limits are refrained and retested. A' review of

. selected data suggests that technicians.are' undergoing the required

testing.

No violations or deviations were identified.

8. Audits and Appraisals (IP 84750)

The inspectors reviewed the most recent off-site audit of the chemistry

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laboratory conducted from August 15-19, 1988 and the laboratory's

subsequent response. No findings, one observation and one open item were

made. The auditors appeared to address in adequate detail the

nonradiological chemistry quality assurance program. Items identified in

the audit appear to have been addressed in a timely manner.

No violations or deviations were identified.

! 9. Open Items

Open items are matters which have been discussed with the licensee, which 4

will be reviewed further by the inspectors, and which involve some action

on the part'of the NRC or licensee, or both. Open items disclosed during

the inspection are discussed in Section 6.

10. Exit Interview I

The scope and findings of the inspection were reviewed with licensee

representatives (Section 1) at the conclusion of the inspection on

January 20, 1989. The inspectors discussed the Open Items in Section 2 ,

and observations on_the quality control program and the confirmatory

measurements. Licensee representatives noted modifications to be made

to the chemistry proc 9dures, as discussed in Section 6.

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DuringtheexitLinterview,theinspectorsdiscussedthelikely

informational 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

} proprietary.

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Attachments:

1. Table 1, Radioactivity Levels in Well Waters,

Braidwood, Collected April 4, 1988

2. Table 2, Radiological Interlaboratory -

Test Results, 2nd Quarter 1988.

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3. Table 3,- Nonradiological Interlaboratory

I Test Results,, January 10-20, 1989.

4. Attachment 1, Criteria for Comparing

Radiological Measurements

, 5. Attachment 2, Criteria for Comparing

Analytical Measurements (Nonradiological)

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- Table 1 i

Radioactivity Levels in Well Waters

Braidwood Area

Collected April 6, 1988

Determined by RESL

Depth, Nuclide,

Sample ft pCi/ Litre i SD

Co-60 O b

Cs-137 H-3 Sr-89 Sr-90

Braidwood City

Wells

1. 1 1000 <11 -60 i 40 -100 1 300 1i1 -2 1 2

1. 2 1000 <11 16 1 26 -100 1 300 011 -212

1. 3 -2200 <11 0 1 30 -200 1 300 111 -012

Farm Wells

1. 1 (household) 285 <11 -40-1-30 -160 1 310 1i1 -3 1 2  ;.

1. 2 (Drinking)- 12 <11 0 1 30 -200 1 300 111 -2 1 2

1. 3 (Livestock) 12 <11 40130 -170 1 310 1i1 0i2

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a. Determined in the Region III laboratory, only.

b. In the Region III laboratory,where the t iting times were much

longer than at RESL, the minimum detectable activities (MDA)

for Co-60 and Cs-137 were each determined to be about 11 pCi/L

(<11),each.

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t U. S. Nuclear Regulatory Commission

L E0ffice 'of. Nuclear.. Reactor Regulation

Confirmatory Measurements Program

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Facility: Braidwood' , v.

Date: January 25, 1989

Sample Nuclide. NRC NRC- -Lic. Lic. Ratio Resol.: Result'  ;

'value SD value SD'

Li uid . H-3.~ 5.26E-3 8.00E-5 5.21Ev3' '2.50E-4' O.99 ~ ' 65.8- A^

rahwaste Sr-89 1.20E-8- 1.30E-8- <4.90E-7 0.00 0.9 N:

t- Sr-90 2. 00E- 9 3.00E-9 <1.1E-7 - 0.00 .0.7 N

Fe-55 :1.52E-5 2.00E-7. '<2.5E-6: 0.00 -76.0: .D- .

Gross B 2.89E-6 1.20E-7' '2.30E-6 0.80 24.1 A'

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-(rerun).FE-55 1.52E-5 2.00E-7 1.51E-6 0.99 '76.0 'A

. Liquid Sr-89 .5/17E-4' 1.50E-5- 5.18E-4 5.20E-5 1.00 34.5 A ,

. Spike b.Sr-90- 3.11E-5 1.20E-6 2.39E-5 2.39E-6 0.77' 25.9 .A-

.RESL #2 Fe-55 - 6 ~. 74 E-5 - 1.30E-6 1.66E-5 1. 66E-6 0.25 51.8 D

Liquid 1Fe-55 1.52E-5 2.00E-7. 1.51E-6 .0.99 76.0 A

radwaste '

(rerun)

a. . See Open~ Item Nos.-.(50-456/87008-01; 50-457/87007-01), Section 2.b.

This report.

b. See Open Item Nos. (50-456/88018-03; 50-457/88017-03), Section 2.c.

This rep' ort.

c. Comparison

A'= Agreement

D = Disagreement

N.= No Comparison

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'Nonradiological.Interlaboratory Test Resultsl. .

,Braidwood Nuclear Generating Station, Units' 1: and 2

l January 10-20, 1989~

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[ Analyte; . Analytical. NRC" ' Licensee Ratio Comparison

Method :

b Y i SD X i SD: Z.i SD i 2 SD

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Concentration, ppb

Fluoride- IC- 5.63 1 0.50 5.96 1 0.04 1.060 1 0.094' A

10.6 i.0.2 11.4 0.4 1.075 1 0.043 A

20.7 1 0.4 21 i 0.3 1.014 1 0.024- A-

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5.63 i 0.50 5.23 i 0.2 .0.930 i 0.090 A

10.6 i 0.2 10.4 si 0.3 0.983 i 0.034 A- .

Choride- .IC '4.63,1 0.03 7.49 i 0.40 1.619 1 0.087- D

9.33 1 0.15 11.73i 0.2~ 1.255 i~O 029 .. D'

-19.1 1 0.3' '20 i 0.1' 1.046 i 0.023 * -A*

-(rerun) 4.63 1 0.03 5.44 i 0.20 1.176 1 0.044 0

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9.33 i 0.15 9.95 i;0.20 '1.067 1 0.027; ,

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Sulfate IC 4.88 i.0.35 5.09 1 0.18. 1.044 1 0.084 A

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9.58 i 0.68 9.39 i 0.13 0.981 1 0.070 A

19.5 i 0.58 18.4 i 1.3 0.944 i 0.072 A-

(rerun) 4.88'i 0.35 5.14 i 0.60. 1.054'i 0.144' A

9.42 i 0.20 0.984 i O.072

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9.58 i 0.68 A

Silica- Spec /1 26.4 1.1. 4 17.3 i 1.2' O.655 1 0.049 D*-

43.5 1 1.8- 0.837 i 0.046 D*'

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', 8. 5 i1 69.4 1 2.2 0.884 i 0.'030- '

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. .(rerun) Spec /5 26i4 1 1.4 ,26 i 0.9 0.985 1 0.062 A

F "

52 12 51 2.5 0.981 1 0.061 A

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78.5 i1 80.7 11 1.028 i 0.018 A

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Fe AA/FL 372 10 392 1 0 1.054 1 0.028 A

796 i 10 803 1 0 1.009 i 0.013 A-

1170 1 30 1215 i 0 1.038 i 0.'027 A

Cu- AA/FL- 400 i6 403 1 0 1.007 i 0.015 A

806 i 30 793 1 10 0.984 i 0.039 A

a 1200 1 30 1185 i 10 0.988 i 0.026 A

Na AA/FL 30.2 i 3.5 21.1 1 0 0.698 i 0.114 D*

53 i3 52 1 6 0.985 1 0.130 A

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79 i4 75 1 4 0.949 1 0.074 A

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(rerun). 12.1 1 1.4 16.1 1 0.2 1.331 i 0.218 A*

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Li AA/FL 394 8 356 1- 5 0.904 1 0.026 D*

600 -1 14 591 1 5 0.985 1 0.024 A

826 1 20 800 1 10 0.969 i 0.026 A

(rerun) 788 1 16 756 1 2 0.959 1 0.028 A*

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1200 1 28 1211 1 0 1.009 i 0.024 A

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1652 1 40 1610 1 12 0.975 1 0.025 A

NH 3 IC 104 1 5 84 1 2 0,812 1 0.055 D*

300 1 3 296 1 3 0.987 i 0.014 A

492 1 23 437 i 6 0.888 1 0.059 A*

Hydrazine SPEC 39.8 1 0.6 41.1 1 1.1 1.033 1 0.032 A

!

100 i 1 104 1.2 1.042 1 0.023 A

'

'200 1 2 206 i3 1.030 1 0.018 A

,

Concentration, ppm

Doron Titr 1040 i 10 1000 12 0.962 1 0.013 D* l

3089 t 41 2957 i3 0.957 1 0.018 D*

t

5000 1 90 4981 16 0.996 1 0.018 A

'

a. Value i standard deviation (50); number of BNL analyses is 6 to 9.

The number of licensee analyses is 3.

b. Analyticai methods: Titr - titration

IC - Ion chromatography

Spec /1 - Spectrophotometric, 1-cm cell  ;

Spec /5 - Spectrophotometric, 5-cm cell

AA/FL - Atomic absorption Spectroscopy

(flame)

c. A = Agreement

D = Disagreement

• Substituted the BNL uncertainty for licensee's uncertainty.

• • Substituted 3% RSD for licensee's uncertainty.

2

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,,_ _ _ , . . . . .

.

. . . .

. .

. . .

>

k

i

! .

1

ATTACHMENT 1  ;

' CRITERIA FOR COMPARING ANALYTICAL MEASUREMENTS

'

.c 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

program.

.;

'

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 ,_j

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

acceptance.

!

'

RESOLUTION RATIO = LICENSEE VALUE/NRC REFERENCE VALUE

' Agreement

<4 0.4 - 2.5 ,

4- 7 0. 5 - 2.0

8- 15' O.6 - 1.66

16 - 50 0.75 - 1.33

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.

sn

e

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p

w n

.a. ,;

4.,

..

.

.

-

e (

'

ATTACHMENT 2 .

,

1

y i - Criteria for Comparing Analytical' Measurements

.i

1

This attachment provides criteria-for comparing results of the capability tests.

The acceptance limits are based on the uncertainty (standard deviation) of the

ratio of the. licensee's mean value (X) to the NRC mean value (Y), where

(1) Z = X/V'is the ratio, and

(2) S is'the uncertainty of the ratio determined from the

propagation of the uncertainties of licensee's mean value,

S , and of.the NRC's mean value, Sy.1 Thus,

.

x

S2 z _ x

32 < s .2

ZY ~ X Y + Vy7, so that-.

32D

S

Z

=Z* [S*2-+ 1-

(X2' y2)

The results are considered to be in agreement when the bias in the ratio

(absolute value of difference between unity and the ratio) is less than or

equal to twice the uncertainty in the ratio, 1.e.

l 'l 1-Z l 5 2*S z*

1. National Council on Radiation Protection and' Measurements,

A Handbook of Radioactivity Measurements Procedures, NCRP

.

Report No. 58, Second Edition,1985, Pages 322-326 (see

F Page324).

4/6/87

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