ML20105B821

Forwards Results of Investigation of Unsatisfactory Performance Test Result Obtained by Medtox Labs on 920806. Urine Custody & Control Form,Part 7 Encl

ML20105B821
Person / Time
Site:	Duane Arnold
Issue date:	09/01/1992
From:	Denise Wilson IES UTILITIES INC., (FORMERLY IOWA ELECTRIC LIGHT
To:	NRC OFFICE OF INFORMATION RESOURCES MANAGEMENT (IRM)
References
DAEC-92-0303, DAEC-92-303, NUDOCS 9209210210
Download: ML20105B821 (17)

Text

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lowa Electric Light and Power Company September 1, 1992 DAEC-92-0303 U.S. Nuclear Regulatory Commission Attn:

Document Control Deak Washington, DC 20555

Subject:

Duane Arnold Energy Center Docket No. 50-331 Op. License DPR-49 10 CFR Part 26, Appendix A Unsat.isfactory Parformance Test Result File:

A-202 Gentlement In accordance with Section 2.8(e)(4) of Appendix A to 10 CFR Part 26 i

please find enclosed the results of the investigation of an ansatiafactory performance test result obtained by ModTox Laboratories on August 6, 1992.

P Appendix I, MedTox to St. Luke's letter dated August 13, 1992, transmitted the laboratory's initial notification, investigation and corrective actions, i

Appendix II, MedTox to St. Luke's letter dated August 21, 1992 provides additional detail regarding the conduct of the test and the l

corrective actions to prevent reoccurrence.

Please note that no document 3 exists in Appendix II, other documents as listed are attached.

If you have any questions regarding this submittal, please contact D.

Engelhardt at 319/851-7280.

Sincere y, dLL

/) W David L. Wilson y

Plant Superintendent - Nuclear t

DLW/DE/bj Enclosures As Stated I

cc L. Liu L. Root i

R. McGaughy J.

Franz K.

Young A.

Bert Davis (NRC Region III)

C. Shiraki (NRC-NRR) i NRC Resident Inspector 9209210210 920901 p

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m, 612 636-7466 l

402 Mst CounO'RoadD St. Paul, Minnesota 55112 i

l August 13, 1992 s

Ms. Kathy Epley St. Luke's Hospital l

1026 A. Avenue F E.

Cedar Rapids, IA 52402 t

Dear Ms. Epley:

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This letter is in respense to your inquiry concerning a specimen submitted to MEDToX under the identification of 461 0191.

This specimen was received on 8/1/92 and assigned the MEDTOX number of G469499.

The specimen tested positive for amphetamines by both Emit immunoassay and FPIA immunoassay and was then analyzed by gas chromatography / mass spectrometry (GC/MS) for confirmation.

I The confirmation results showed an amphetamine value of 16 ng/ml j

and a methamphetamine value of 1688 ng/ml.

In accordance with NIDA guidelines the specimen was called negative because 4 he amphetamine i

did not exceed 200 ng/ml.

The results were released on 8/3/92.

l Af ter your phone call of 8/4/92 indicating that the specimen should be posjtive for amphetamine and methamphetamine, all of the data 4

was gathered for review.

At this time a calculation error was i

discovered which corrected the amphetamine value to 1572 ng/ml.

The report was amended on 8/5/92.

l The protocol for reporting results requires that a second analyst check all of the work including the calculations generated by the original analyst.

The results are then reviewed by the certifying scientict before release.

All of these steps were documented as being followed for this specimen.

Obviously, there was a breakdown in this procedure.

l l

The corrective action initiated for this problem consisted of discussing the situation with those individuals involved and i

reemphasizing the need for detailed resiew.

This was also linked to a continuing education seminar for Lll of the technical staff dealing with the review and checking of results.

This incident has also been submitted to the QuTlity Control Committee.

r i

MED7DX l.aborrories, inc.

MEDIDX Bio Analytical MEDIDX Bio-Analytiini Saint Patd. Minnesc?a Oicago, Illinois ins Angeles, Gdsfornia e

612-636 7466 312 &7k6900 818-718Dil5

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l We thank you for the. confidence you have shown in HEDT0X to perform your testing.

Be assured that we are very concerned about i

i this incident and have taken steps to safeguard against its i

i recurrence.

If you need additional information or data, I cr.n be i

l reached at 1-800-832-3244.

i l

Sincerely yours, l

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Gary,Hemphill, Ph.D.

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Director of Occupational Toxicology j

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l August 21, 1992 4

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Ms. Kathy Epley j

St. Luke's Hospital i

1026 A. Avenue N.E.

Cedar Rapids, IA 52402 I

Dear Ms. Epley

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In response to your recent inquiry concerning specimen number l

G4e.,499 I am enclosing additional documentation that includes the j

custody and control form, raw data from the Emit immunoassay, raw l

data from the fluorescence polarization immunoassay (FPIA), data j

l from the gas chromatography-mass spectrometry assay, and an outline j

i of the seminar presented by Dr. Kings 1cy Labrosse, Director of j

l MEDTOX Laboratories.

1 i

As indicated in the first letter, the Emit immunoassay was positive for amphetamines as noted in document 1B (AMPH 61H).

The

[

l-FPIA immunoassay was also elevated ac noted in document 2.

The specimen was then tested by gas chromatography-mass specurometry I

i as seen in document 4A-G.

i Document 4A represents the data summary for the batch of l

. specimens that included G469499. _ This data represents the original

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l data and the amended data as noted by the cross out and initials

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l in data columns 7 and 9 for G469499.

Documents 4B and 4C represent the blank that was injected before specimen G469499-- to dor:ument i'

thLt no carryover occurred from previous sampins.

Documents 4D-j 4G represent-the documentation for specimen G469499.

Document 4D i

j and E represent the chromatograms -from the run.

The -data

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calculated by the GC/MS computer system -for the amphetamine is shown on 4E.

The instrument is programmed to choose the proper l

peak from the retention time (RT), integrate the peak height, and l

calculate the ion ratios for the analyte, in this case amphetamine.

l Occasionally due to the complexity of-the urine specimen with the many compounds residing in it, a second peak emerges close to-the peak of interest, and the instrument chooses the wrong one.

This l

Was the case with specimen G469499.

On 4E the retention times (RT) are very similar, ' but ion 118 has a retention. of 0.21 minutes different.

When-this occurs, the ion ratios must-be calculated manually from the data on 4F for those ratios involving-ion 118.

The correct integration number for ion 118 should have been 188970 i

f rom retention time - 5.103 rather than 3465 from retention tima 5.31.

This calculation changes ion ratio 117/118 to 0.18, 140/113 4

i i

l

..IEDTOX laboratories Inc.

MEDTOX Bio-Analytical MEDTOX Bio Analytical '

Lm Anecles, California Ciucago. fl.'inois Saint Paul, Minnesota e

e I-612 636-7 A 312-MU-6900 81&71%01!$

l to 1.24, and 118/123 (the ion ratio used to calculate the quantitation of amphetamine) to 2.76 (188970/68305). The first two ion ratios were changed and transferred to the data sheet (4A), but 1

the 118/123 was inadvertently not changed from 0.05 to 2.76.

This j

was also missed in subsequent checks of the dhta.

Since the 0.05 was used to calculate the amphetamine concentration instead of the l

1 2.76, a value of 16 ng/ml was calculated rather than 1572 ng/ml.

l The data for the methamphetamine was correctly calculated by the instrument and transferred to the data sheet correctly.

l The corrective action as indicated in my previous letter involved a discussion with the individuals running these tests, those checking the data, and the supervisory staff in the forensic laboratory. The importance of the correct handling of data and the accurate checking was emphasized.

It was also decided that the j

computer data that is wrong will be crossed out and initialed in r

j order to more graphically emphasize the manual correction needed.

1 This will call additional attention to the problem so that the data handler and checker can insure that the calculation was correct and j

accurately transferred to the summary J,heet.

j I have enclosed a summary of our technical staff seminar presented by Dr. Labronse that dealt directly with the proper method of calculating results and the obligation of the technologist checking the results to review and recalculate all l

results.

If you need additional documentation or interpretation, I can be reached at 1-800-832-3244.

Sincerely yours, f

hb Gary-ifemphill, Ph.D.

Director of occupational Toxicology GH:ch I

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2QQQ-g fI 4.D G.' O G.G 89'.9 T.m.

c m i e,

)

Ion 887.00 amu.

1. eam DATA QGQ2A23A.D t

O00 jC h

8 GOO-4Dr 3

2 08.

O O

T 4.O G [O G [Q 1 e '. e Teme fmim. 1 I

Ion 142.Ga amu.

1. eom DATAeQGe2A22A.D

~

s ggg

}

400-e, 3

200-

,' O G.' O G.' O 17.e 4

T,m.

<m,-

Ian 119.00 amw.

1. eom D AT A s OO Q2 A2 3 A. D h

E00]

6' g

3 4004 100-3 c-

'i 4.O G [Q G [O t m' g Time f m o e.

3 g

Zon 12 3. O ks amw.

1. eom DATAsQGQ2A22A.D i!

"aaj WW@@eM C

3 202-

$3 2

a Ttma (min. 3 Ian 144.00 amu.

1. eom DATAeQGO2A22A.D g

f GCO-Y 1

ill 400-200-

,3 o.

[G G[O G[G t e '. a 4

Ttme Cmtn. 3 p.

.._m_.

._.m.--

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f hs i

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)

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F (de tyr.es GC / T1S D AT A f,!LE i

Sernp !e Narae C469499 X2 Mice Info I

j Operator D A S/r1S D #4 i

Date 2 Aug 92 11 : 2 3 prn I n s t r urnen t s r1S_5 970 l

Inlet

CC i

Sequence index i 1

Als bottle num i 24 Repiteate num i

1 TIC a# DATA: OGO2A24A.D t.OC4e-l

} 1 t,

o k, + 5 -

I L

u-

- w

[

l T

'o G.' O a.' c

c' o Teme t c.. s e.

1 i

Zon i17. 30 mmu.

from DATA: OG02A24A.D

[

g i :

. a a o s -l I

i e

t I

i

• O000H a

?

2 G G 0 0 ~.

i 6

1 t0300-F aj MNs-

- k

{

4

• %.O E.O 6.O t0.0 Tt me Cmin. )

Ian 140.00 mmu.

1. eom D A T.7 s O G Q 2 A 2 4 A. D 0

OU*S' l

J i

e e

4,QC+5-N

=

, 3

! J k,0C+S-

! 3 e

I

,j c,QC+a-r 4

O C.Q G.O 10.0 Time t en i r.

1

.s 1 iG.QQ amu.

e m DATA +QQQ2A24A.D f

6 i

j 2.OC+5 g

..=C.

3 s

t 0 ;.

l'

i oc + s 4 5. O C + 4 ](

a j g, g g, g.)

d s-4.0 G.O G,0 10.0 Time t m i r.

)

,= w Ion 123.QO mmu.

1. eom DATA: t3G22A24A,D e

'l i

w*

GuuCO-40033-Q P

r 4 ',

2O200-a 4

-- l e

g 4.0 G,O G.O 10.0 T i me tmtn

)

I Ion 144 QQ

amu,

1. emm DATAsOQQ2A24A.D r

C g

3.QC+51 V

e

. o C.,j 3

=

c

0. 08

+O-i

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}

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_L

'a g g 4.' O G.O Q.Q 1 O '. a

}

Tt mm (mtn Zon 154 20 mmu.

from DATAsQQQ2A24A.D I,y_ Go. C C + 5 4

t g

l 4.OC.s-'

a

[ 2. O C' + 5 -

5 2

f0 (B. O C + O t

li i

4.Q G.O G.O 1Q.O

((

Tome tmtn. ?

'i Ian 110.20 mmu.

4' c o m DATA:OQQ2A24A.D

I,

(

y 2.5C+59

'C C.DC+$'

8 1.5C+5-3 1.OE+59 i

,,g e 3 5.QC+4-

' i

(

Q.OC+Q-

~

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4.0 G.O Q.%

10.0 Y$me (min

)

Ton 11J.CO amw.

4 m DAT A

• OQ Q2 A2 4 A. O

!! C

'li 5{e 1.0L+5-a I

a S

S C

5.OC+4-5

s 1 (^

"lT'.U Q.OC+O 4.Q G.Q G.O 10.O Ttmm (min. )

Ion 150.00 mmu.

team DATA: QQQ2A24A.D l1 g 4.OC+59 f

3.QC+5i ig I,OC+5-l jf's.

1.OC+5-i

.; ;l; Q. O C -e Q

• . kJ G.O W.O 1 (1 $. O j-*

T e m e.

fmtn. )

a ri r H E F 4 M iliE CCHFIRMATION 10rt RATIOS :

i I U: % i10 117/118 = 10. 3 2 C l

[ Ori RATIO 14 M110 =67.69s IDH RH110 123/144 =0.4/

'h ION RAT:0.A8/123 =0.05 HMFHETHnir4EON PLAK' HEIGHTS :

' FEAR HEIGHT FOR ION 117 35759

=

R.T.

5.10

=

F E R Vs HEIGHT FOR IUN 140 234550

>=

R.T.

5.10

=

3465 E

i'E AK HEIGHT FOR ION 118

=

/.

R.T.

5.31

=

J i'E AK HEIGH T FOR ION 123 68305 R.T.

5.07

=

.'LHK HEIGHT FOR 10N 144 146130 o r

= v n>

= ---,--~-.,-_.__

't THhr4PHETAMINE CONFIRMATION ION RATIOS i s

ION RATIO 118/110 =0.86

9M RATIO 154/110 =2.70 4

ION RATIO 113/158 =0.36 ION RATIO 110/113 =1.74 4

i METHAMPHETAMINE ION PEAK HEIGHTS 8 1

229101 I

PEAK HEIGHT FOR ION 118

=

n.T.

- 6.40 r-PEAK HEIGHT FOR ION 154 - 719339 4

R.T.

- 6.40 PEAX HEIGHT FOR ION 110 266487

=

R.T.

= 6.39 L

PEAK HEIGHT FOR ION 113 = 153305 R.T.

6.35

=

PFAK "EIGHT FOR ION 150 = 124055 l

R.T.

6.36

=

e Height Percent

=

Report by Signal i

a

~

~~~~~~'~~~~~~'~ ~ "~~~~~~~~~~ ~~~~~~~~~'~ "

hSEat$rIbA5"MSbk4 2 AIsg 92 51I33 pr5 }

! Method File Name : AMPH.M l Sample Info a C469499 X2 1

Misc Infas

Integration File Name DATAs0802A249,I Method i. d i 1

Batt le Number i 24 a

l r

4 Mars 117.00 emu

)

Ret Time Type Area Height Ht. %

Ratio 4

...o.a.........................m..........

2.....................n..,........n..

i 5.103 SU 1425146.6047 35759.206357 '

44.315 100.00 6.394 BB 1297132.5561 44733.655461 55.686 125.66 3

' Mass ~ 140.00 amu

~

Ret Time Type Area Height Ht. %

Ratio %

...o.o.............

5.103 BU 10390807.633 234550.23338' 27.167 100.00 5.561 BU 1476794.0358 39370.185319 4.560 16.79 6.994 BU 395957.57995 11217.997697 1.299 4.78 7.502 BB 4952772,9416 578222.63521 66.973 246.52 i

Mass 118.00 amu Ret Time Type Area Height Ht. %

Ratio %

,....o................................................................,.........

1 5.103 BV 7982053.2994 188970.13542 '

44.820 100.00 i

]c 5.313 VV S3184.641665 3465.2123416 0.822 1.83 6.394 RU 4743340 "M 7 4 790 on EXQ*^

EA 2"o

L-qj vo s.esm...a o -..s,a

~.

.v.

6 Ma t. s 123.00 amu le t f itne. lype Area Height Ht. %

Ratio %

i 5. 0,' T _BV 2650735.3870 68.'05.058074' 100.000 100.00 Mass 14 4. 00 amu Height Ht. %

Ratio %

et T i tue Type-Area

+

3..................

j

~

s 5.071 BV 5644136.7872 146129.91336 95.233 100.00 5.872 BB 184738.69757 7315.4953708 4.767 5.01.

Mass 118.00 amu et Time Type Area Height Ht. %

Ratio %

l

........................................................n......................

t 5.103 BV 7982053.2994 188970.13542 44.820 100.00 l

5.313 VU 53184,661665 3465.2123416 0.822 1.83 6.594 DU 6243340.5376 229180.53834 54.358 121.28 Mass 154.00 amu

et Time Type Area Height Ht. %

Ratio %

j................................................................................

6.193 PV-11955.120027 499.93268759 0.069 0.07 i

6.3YS BV 18562449.999 719338.92992 99.931 100.00 i

Mass 110.00 amu

',et lime Type Area Height Ht. %

Ratio %

........u.......

6.390 BV 7101707.2959 26.487.42779 100.000 100.00 i

F f

I 1

Mase 113.00 amu

et time lype Area Height Ht. %

Ratio :.

...................u........

j 5,103 BV 271809.75341 7916.4763851 4.608 5.16 6.350 80 4215569.1558 15J304.51025 89.243 100.00 7.502 BB 107330.20568 10562.069740 6.148 6.89 1_____________________________________________.___.______________________________

Mass 150.00 amu

Het.ime lype Arne Height Ht. %

Ratio %

_...................=.....................................................u.....

6 355 BV 11806598.969 424055.32004-100.000 100.00 t

JilD OF REPORT for file

DATA 080iH24A.1 11:44 pm 2 Aug 92

?

a

7 y.z. i p' a.a b -e

% M MS W/7

• }

A y,

• D r. L a b r o ss <.

CONFTRMATION VERIFICATION a

i i

4 1.

Check 20 % ion rat -uge of threshold standard.

1

~

2 2.

Check lines with linear regression calculator (Excludes TARGET). Ensure

' standard quants within limits.

3.

Check that ion ratios are within the 20 % ion range for standards,

, controls, and positive patient specimens.

t 4

s s

4.

Check that controls are within range.

I

[

l

-5.

Check chain of custody and worksheet initials.

s 6.

Check chromatogram ida.ntification numbers witli specimen number on worksheet.

l j

l 7.

Re-calculate the quant ion ratio and verify quantitation in the linear regression line.

4 8.

Check chromatography; i.e., peak shape, interfering peak, baseline and abundances.

f i

1 9.

Check retention times of the drug (

0.04 min from inte.rnal std retention l

time).

l 1

10.

Verify that all positive specimens have quant values greater than the threshold cut-off limit.

i E

i 11.

Verify that all quant confirmation drug levels are above the LOQ.

[

12.

Verify that all " retests" are quantitated to LOD. Report as "presenc'e of drug is confirmed".

i s

?

l 13.

Check and initial requisition confumation forms.

i 14.

Initial verifier spot on worksheet (both pages).

15.

For opiate confirmation verify the presence or absence of 6 MAM.

i

. 16.

For d, & L. methamphetamine - report quantitations.

17.

For THC confirmations on clinical mother and baby specimens report to LOQ.

[

4 e

- + - - - -,

~

f

=y

,yy-,ry.,

y

--y, j,, g y