ULNRC-05710, Blind Specimen Test Results

Blind Specimen Test Results

ML101580080
Person / Time
Site:	Callaway
Issue date:	06/04/2010
From:	Sandbothe S AmerenUE, Union Electric Co
To:	Document Control Desk, Office of Nuclear Reactor Regulation
References
ULNRC-05710
Download: ML101580080 (10)

Text

AmerenUE PO Box 620 Callaway Plant Fulton, MO 65251 June 4, 2010 ULNRC-05710 u.s. Nuclear Regulatory Commission Attn: Document Control Desk Washington, DC 20555-0001 10CFR26.719(c)

Ladies and Gentlemen:

~~ DOCKET NUMBER 50-483 wAmeren CALLAWAY PLANT UNIT 1 UNION ELECTRIC CO.

UE FACILITY OPERATING LICENSE NPF-30 BLIND SPECIMEN TEST RESULTS On 5-5-2010, blind positive specimens were submitted to three lllIS certified laboratories who have contracts with Callaway Plant. On 5-6-2010, one laboratory returned unexpected results. On 5-7-2010, the other two laboratories returned the expected results. All three laboratories are Department of Health and Human Services (DlllIS) laboratories. Two of the three specimens were manufactured from the same lot with the third specimen manufactured from a different lot, however similar results were expected for all three specimens. This information was provided to Duo Research, Callaway's blind specimen provider, who is currently conducting their own investigation.

In accordance with 10CFR26.719(c), enclosed is the documentation of investigative findings and the corrective actions taken by Clinical Reference Laboratory. Duo Research has also submitted an interim report of findings. Please contact Anna Lee at 573/676-4435 if any additional action is needed as a result of this information.

This letter does not contain new commitments.

Sincerely,

~~;44 Scott Sandbothe Manager, Plant Support CSP/nls Enclosures a subsidiary of Ameren Corporation

ULNRC-05710 June 4,2010 Page 2 cc: Mr. Elmo E. Collins, Jr.

Regional Administrator U.S. Nuclear Regulatory Commission Region IV 612 E . Lamar Blvd., Suite 400 Arlington, TX 76011-4125 Senior Resident Inspector Callaway Resident Office U.S. Nuclear Regulatory Commission 8201 NRC Road Steedman, MO 65077 Mr. Mohan C. Thadani (2 copies)

Senior Project Manager, Callaway Plant Office of Nuclear Reactor Regulation .

U. S. Nuclear Regulatory Commission Mail Stop 0-8G 14 Washington, DC 20555-2738

ULNRC-05710 June 4, 2010 Page 3 Index and send hardcopy to QA File A160.0761 Hardcopy:

Certrec Corporation 4200 South Hulen, Suite 422 Fort Worth, TX 76109 (Certrec receives ALL attachments as long as they are non-safeguards and may be publicly disclosed. )

Electronic distribution for the following can be made via Other Situations ULNRC Distribution:

A. C. Heflin F. M. Diya L. S. Sandbothe C. O. Reasoner III S. A. Maglio S. L. Gallagher T. L. Woodward (NSRB)

T. B. Elwood Ms. Diane M. Hooper (WCNOC)

Mr. Dennis Buschbaum (Luminant Power)

Mr. Ron Barnes (APS)

Mr. Tom Baldwin (PG&E)

Mr. Wayne Harrison (STPNOC)

Mr. John O'Neill (Pillsbury Winthrop Shaw Pittman LLP)

Missouri Public Service Commission

Am8renUE PO Box 620 Callaway Plant Fulton, MO 65251 AAFFD 10-0022 June 2,2010 Mrs. Anna Lee Supervisor Access AuthorizationIFitness for Duty Ameren DE Callaway Plant P.O. Box 620

~~ Fulton, MO 65251 wAmeren U£ RE: Investigation of Blind perfonnance testing error I have received and reviewed the investigative reports submitted by Clinical Reference Laboratory and Duo Research. I am in agreement with the statements made and the corrective actions that are planned. As :MRO, I am satisfied that the appropriate actions have been taken to resolve the issue. If any further questions arise please do not hesitate to give me a call at 573-676-4301.

William P. Cravens, M.D.

Callaway Plant Medical Review Officer cc: A160.0001 Attachment 1 to ULNRC-OS71 0 Review performed by Dr. William Cravens Page 1 of 1 a subsidiary of Ameren Corporation

CLINICAL REFERENCE LABQRATORY Aaron Enloe, FFD coordinator 6/2/10 Union Electric Company D/B/A Ameren UE Callaway Plant JCT HWY CC and HWY 0 Fulton, MO 65251 FAX: (573) 676-4615

Dear Mr. Enloe,

Clinical Reference Laboratory (CRL) issued a report of "negative" for urine specimen

1. 6402184841 identified by laboratory accessioning number 47340347. CRL was subsequently notified that this specimen was an external blind that was expected to test positive for THC.

This sample was received by the laboratory on 5/6/10. The sample screened negative for drugs.

SVT analysis yielded a creatinine value of 71.1 mg/dL. The sample did not meet the FFD requirements for testing at LOa because the creatinine was greater than 20.0 mg/dL. The sample was reported as negative in accordance with CRL SOP and FFD program guidelines.

On 5/07/10. the laboratory received notification that the sample was an external blind which had failed to meet the expected result of "positive for THeil. The stated target range for the blind sample was 65.0 ng/mL to 77.5 ng/mL. At your request, the specimen was moved to long term storage on 5/7/10.

At your request on 5/10/10, the screening data was submitted and at the same time an investigation was initiated by CRL. The initial screening data was reviewed. The initial (semi~

quantitative) THC screening value was 43 ng/mL. An aliquot of the sample was forwarded for confirmation testing. The result obtained by GCMS analysis was 36.1 ng/mL. This "confirmed" value is below the 50 nglmL screening cutoff.

The laboratory requested further information from you on 5/10/10. Along with a narrative of the process. you submitted a copy of the instructions for submitting a blind to CRL and a DTI for submitting blind specimens. The first document specifically states the sample should be mixed before submission. The second does not mention mixing. To rule out a sample that was not sufficiently mixed, the laboratory sent to confirmation an aliquot of bottle B. The value obtained was 40.0 ng/mL. The similarities in obtained values indicates the sample was mixed on submission. However, both values from bottle A and bottle B are clearly below the stated target value and below a level that would trigger a positive of 50 ng/mL or greater on screening.

W VA If we, c,' a", n be of further assistance in this mattlier" P, lease I r l ekno u s.

Sincerely, i' J r\ .

,,'~I"*Y" ,'" ,-' , [)

JOhn)tvn1g ../ ) David Kuntz Re~onsible P~n Responsible Person Clinical Reference Laboratory Clinical Reference Laboratory Lenexa, Kansas 66215 Lenexa, Kansas 66215 (913) 693-5405 (913) 693-5406 Attachment 2 to ULNRC-0571 0 Investigative Report provided by CRL Page 1 of 1

.,_, _ _ ......... ~_~ ___ .~_ ..._ ...... __ ...___,._.... _............................. ".............. "**.......... ,.,............ _.,... _........................_ ... ,...... __ .,._._."h ...'.. "" ... .. ,.,." ... ,."_ .................._,." ....."...*. ,,.......................... ..........*. "....... ,_, ... __ ._.... ,........................... _._ ... ,.............. _ ........

, .~ ~ _,~ ........... _ _ ............... _ ....... .*..*. ,... ,... "........... ,.... ,....... .

~~

JUN/02/2010IWED 06:24 AM FAX No. P.002 INTERIM INVEST,IGATION REPORT

,on Blind Performance Test Samples Objective:

~he l~ceneee ehal~ inveetigate any unsatisfactory perfor.mance testing result.

A reco~d sha~l be made of ~e investigative ,findings and the corrective action taken by the laborato~. 'Ihe licensee shall send the document to the NRC a.s a

~eport of the unsatisfactory performance testing incident within 30 days.

Referenoes:

10 CFR 26 Subpart G, §26.168(g) (3)

Observation:

Ameren submitted blind quality controL samp1es meeting the requiremQnts of 526.168(g) (2) and (3) I i.e.; positive samples and false negative challenge samples; conta~ning XHC-9-acid, to two laboratories. Only one of thQ laboratories reported the posit~ve sample as positive and the other laboratory repoite4 the sample as neqative.

Findings (1):

1_ The THC-9-ao~d po~it~ve samplea we~e eent frozen to Amersn UE Callaway Plant by Ouo Reaearoh Inc. on April 6; 2010. The samples were packaged in individual Nalgene bottle$, which had ~emained frozen f~om the time of production. ~eference analyeie was conducted on october 13; 2009, by Medrox Laboratories, which obtained a concentration o£ 95 ng/mL. ~he acceptable range for the THCA Positive 8amp~e ~ is 75 to 100 ~g/mL. It is the usual proceQ~re for Ameren etaff to thaw the samp~e bottles, transfer the samples into the specimen vials p=ov:ided by the 1aboratories, and submit the samplQs appearing as real apec;i.mens to th~' t;hree labo',ratories. The samples were subm~ tted to the two labo~ator:i..es May' 5,' '2010.

2. A negative ~eBult was reported by one of the laboratories and a positive result by the other laboratory. The results and reviaw of the infor.mation provided by each laboratory are :F;>rssented separately. A general. comment about the screening reagents and how the results are presented: HRS certified laboratories are required to ,inc1ude a number of ~a1ity control samples in each screening batch. Amongst thesQ are two that are at 25% above and 25%

below the cutoff concentration. This is thQ acceptab2e range permi~~ed for samples at the cu'toff concentration to fall. between. The labora~ories may use different instrument settings to express the results compa~ed to the instrument reading for the cutoff calibrator.

Attachment 3 to ULNRC-0571 0 Investigative Report provided by Duo Research Page 1 Page 1 of 5

JUNI02/2010/WED 06:24 AM FAX No, p, 003 Investigation Report Page 2

3. Cl~nical Reference Laboratory

~his laboratory reported the sample as negat~vQ. The laboratory provided Ameren with printouts from the screen~ng results, which had a reading of 42, which indicates i t was negative. Ameren did not request the laborat.ory t.o conduct the quantitative test.

4. Quest Diagnostics, Lenexa, KS This laboratory repor~ed ~e. sample ae pO$~tive. The labor~to~ conducted the GC/MS analys~s wi~ a result of 49 n~/mL.

Observation:

Ameren ~ubmitted blind quality control samples maat~ng the requirements of

§26.168(g) (2) and (3), i.e., positive samples and false negative challenge samples, containing THC-9-acid, to two laborator~es. Only one of the laboratories reported the positive sample as pos~tive and the other laboratory reported the sample as negative.

Fi.ndings (2);

1. The THC-9-acid false nega~ive challenge samp1aa were sent frozen ~o Amere.n UE Callaway Plant by Duo Research Ina. on May' 10, 2010. Tha samples were packaged in individual Nalgene bottles, ~h~eh had rema~ned fro~en from the time of production. Reference analys~s was eondueted on Oetober ~3, 2009; by MedTox Laboratories, wh~ch obtained a eo~cen~at~on of 74 ng/mL. The aoceptab1e range for the THCA Positive aamp1e type is 65 to 77.5 ng/~. It is the usual procedure for Ameren staff to thaw the samp1e bottles, tranafer the samples into the' specimen via1s prov1ded by the laboratories, and eubmit the samples appearing as rea1 speoimens to the three laboratoriee. The sampleB were submitted to the two 1aboratories May 12, 2010.

2. A positive result was reported by both of the labo~ato~ieB. The resultB and review of Che infor.mation provided by eaeh laboratory are presented separately.

3. Cl1n~oal ~eferenoe Laboratory This laboratory reported the sample as pos~tive with a quantitative value of 42 ng/mL. The laboratory was contacted to obtain additional data; i.e., the aor~ening resu1ts to ola~ify what the. values of the control samples were relati~e to the cutoff. ~.the~ information has not yet been received.

5. Quest Diagnostics, Lenexa, KS This laboratory reported the sample as positivQ. The laboratory oonducted the CC/MS analys'is with a result of 48 ~q/mL.

Attachment 3 to ULNRC-0571 0 Investigative Report provided by Duo Research

. Page 2 of 5

JUNI02/2010/WED 06:24 AM FAX No. P. 004 Investigation Report Page 3 Discussion:

The intent of the NRC requirement in §26.168(g) (3) to eubm~t blind quality control samples in the range of 130% to 155% above the cutoff ie to challen ge the testing laboratories ability to detect the presence of drugs aCove the

+25% control limit required under HHS certification. ~o. cla.~f~cation, fo~

the THC-9-acid metabolite, a sample at exactly 50 ng/mL should screen p06~tive 50% of the time and negative 50% of the time on repeated testing. Over a range of increasing concentrations, a greater percentage of the samples should be positive. The NRC regulation has set 30% above the cutoff as the point that all samples should be positive. The assumption is that a sample of THC~g-acid at 66 ng/mL should be positive.

The qua~~~ con~rol samples submitted to the reference 1aboratory, MedTox, and by Ameren to -ehe t.wo labora~or~es, were subjected to somewhat different handling a~d sh1pp~ng. The refarenae sample was sen~ frozen to MedTox, which had to thaw the sample and oonduot the analyg~s. Th~s occurred w~th~n a day of

~ts reee~pt. The samples were also sent frozen to Ameren and stored frozen until they were thawed and prepared for Shipment as b11nds ~o the laboratories.

Because all of the t~e intervals are 5i~~arl w~th no obvious d~fferenQe$

in the handling and processing of the samples, i t is cone~uded that the laboratories obtained compa~able and ve~ 5im~lar results th~t ~ust be considered co~rect. Until additional information is obtainea i t is not possible to determine what the cause of the diacrepancy in values between the laboratories and the reference values.

A table with a summary of the results ia attached.

Recommenda.tion:

Duo Research is continu~ng to obtain ad~tiona1 information from thQ two laborator~es and will submit a final report as soon as the investigation is considered complete.

Prepared for: Ameren UE Callaway Plant by: ~fdf:(M/hk

/.

Date:. ~ ~2r2(O Duo Researoh Inc.

Attachment 3 to ULNRC-05710 Investigative Report provided by Duo Research Page 3 of 5

JUN/02/2010IWED 06:24 AM FAX No. P. 005 Investigation Report Page 4 Addendum:

As noted in the March 4, 2010, Inyestigation report( a study wae cond~cted to determine i f the transfer of the" THC-9-acid '\Fa~sQ Negat:i..ve Challenge" (FNe) sample to a l.aboratory speci.mc::m bottle and shipped overnight to the two laboratories contr~uted to their ~itial negativQ screening result. ~t was noted ~a~ an ~dentica1 sampl.e sent to the local. laboratory screened positive the day '\::he sample was prepared and was su,bsequEiln tly confirmQd.

The other ~aaue was whether a concentration c10se to the min~um 130% ~~mit eet by NR.c for auc::h samples poses a chal).ce t:.hat. qua.li. ty control samplGs conta.in.ing the THC-9-acid may have an incr"eased risk of failing the initial sc~een. ~his .ie baaed on an e~tansive literature descr1bing the stability and potential ~ources of loes of this anal.yte.

The study ~nvolved the p.o~~ction of a new batoh of the THC-9-aoid ENe samp~es. The target concentration was to be close to the uppar 1B5% 1QVQl for these samples, 77.5 ng/mL.

Two of the samples were sent frozen to~e o~iginal re~eren¢e 1aboratory, MedTox. One sample was thawed and transfe~.ed into two labo.atory via1s, the same ~e of sample bott1e used by the Callaway Plant. One of the vial.s was stored at room temperature overnight. After a two hour d8~ay the other eample wa.s screened under standard laboratory condition along with other 5alIlplee.

The screening result was positive with an instrument response of 95(

compared to the +25% control (62.5 ng/mL) response of 98. The confirmation resu1t, conducted the same day, was 75 "ng/mL.

On the next day, the sampl.e that was stored at laboratory temperature overnight was suhmi~ted to ~e screening assay. It gave a response of 79 c::ompared to the +25% control response of 90, a larger separation than that of the sample tested the day i t was thawed. The confirmation result for this sampl.e was 62 ng/mL.

It ~a apparent that the sample does suffer some loss when transferred to the laboratory bottl.es and stored for" about 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> before testing, si~ulatin9 ~~ "~me frame of"~e ~wo"samplQs that scre9ned negative, although the actual $~orage eonditions may differ to some extent.

In ~on¢l~$~on, for THC-9-aa~d, i t is apparent that to avoid possib1e losses due to ~ans£err~n9 the sample to l.aboratory bottl.QS and conditions of Bhipping, the eamp1e via eommerc~al courier overnight, the concentration of this ana~yte muet be at: the upper linUt of the 130% 1:0 ~55% range specified by the NRC regulat~one.

Att~chment 3 to ULNRC-05710 Investigative Report provided by Duo Research Page 4 of5

c.........

c::=:

z

~

~

c:::>

~

Lab Duo Number COC# Results Quant Value Ref. Values Type of Blind Date of >-3 q

tr:J Submittal l ~

Quest 9657-]25-88717 8126992 Negative 58 nglmL 74nglmL Fal se negative 02/23/2010 L.l..>

TIle CRL 9657-125-84733 6402068862 Negative 48.9 nglInI} 74 nglmL False Negative 02/~/2010 >-cI 55::

THe Toxicology 9657-125-43805 T110449 Positive 50nglmL 74nglmL False Negative 02/23/2010 1--1 THe

~  :.

.....:. ..... :. .... -- -.:-' :: *.: .~.:~:::.:.~..:.;-:-.:,:...-:".

.=.' .. ,,-, .. " ....

~

..... 4 Positive THe tf)

...... Quest 7418-190-17621 8126930 Positive 49 nglmL 95 ng/mL 0510512010

()'Q

~>

...... ~

Toxicology 9657-125-29471 T113970 Positive 68 nglmL 95 nglmL Positive THC 05/0512010

-< fl)

~ (';) CRL 7418-190-23981 6402184841 Negative N/Al 95 nglmL4 Positive THe 05105/2010

~s

'"0 ~

l-cJo::s Quesf 9657-125-00536 8126930 Positive 48nglmL 74ng/mL False Negative 05112/2010 fl) ~ .....

'"0 .w (lQ (D '""t ..... THe 0-. 0 0 CRL j

9657 -125-36483 6402184831 Positive 42ng/mL 74nglmL False Negative o :5.C 05/1212010

~p..l" Vl8..Z ~ - - -----

THe >-x:I

x>-

cr'~ ><

'-<!(J z tiC 1 Results were obtained during the investigation process after reana1yzing..

,::::: Vl o .....,J

~~

(D 0 2. Results from Investigation have not yet been returned.

tf)

~ - .

8

T 3 Replacement samples that ~ere submitted due to the failure of the 2-23-2010 samples.

4 Samples from this lot were also subnritted blind in two other workplace programs, prepared in the lab kits ready for testing, with results from one laboratory of 69 and 70 nglmL, and from another at 105 nglmL.

Note that the sample for lot 9657-125 were prepared exclusively for AmerenUE, whereas those from lot 7418-190 were prepared in a similar manner for DOT workplace programs.

>-cI

~

~

Ul