Text

Public Version of Rev 1 to Emergency Plan Procedure LZP-1330-20, Post-Accident Analysis of Boron (Backup Procedure),Safety Evaluation Format Procedure History & Receipt Form
	ML20076G637
Person / Time
Site:	LaSalle
Issue date:	07/26/1983
From:	Knoll R; COMMONWEALTH EDISON CO.
To:	;
Shared Package
ML20076G630	List: ML20076G637;
References
	LZP-1330-20, NUDOCS 8308310478
	Download: ML20076G637 (100)
	v • d • e

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' LAP 020-2 ATTACHMENT F evision 20 (Page 1 of 2) January 11, 1083

~~

,. 10CF350.59 FORMAT FOR SAFETY EVALUATION 20 l

b bD "C UN17 O STATICN Re J. /

_ SYSTEM N TEST / PROCEDURE NO. LE f t330-4 O TEST / PROCEDURE TITLE fbst Accabear A44wsn ec %Re a ECUIPMENT No. Al*

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DESCRIPTION OF TEST / PROCEDURE

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1%kkaa. f fs.AsdN

%m % c. .h ~~il"u *S k0 f SAFhT/ EVALUATICN: Answer the following questions with o l'yes or "no*, and provide specific reasons justifying the decision:

1. Is the probability of an occurrence or the consecuence of en accident, er malfunction of eauipment important to safety as previously evaluated in the Final Sciety Analysis Report

'-- increased? Yes v No, Because:

Alo 9 4 es de & a-Qu v'o ~ d 2e f ,, Q p

2. Is the possibility for en accident or malfuncticn of a different type than any previously evaluated in the Final Sciety Ana!ysis Report created? Yes X No, Because:

A o

N Y h 4 u- a a-WM[m a [.

3. Is the margin of safety, os defined in the basis for any Technical Specification, reduced?

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Yes Y No, Because:

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065 j/f 8308310478 830825 Performed 3v /" Cafe PDR ADOCK 05000373 Approved By NC Care ' '

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. 4 LAF-320-2 AWAC.ME.lT H

F kvisien *3 Janura ry. 11, !?

(Page 2 of 2) 21 (Final)

PRCCEDURE HISTORY AND SAFETY EVALUAT:CN (10 CFR 50.39)

Oces ma crecscureirevision censue.ite a enange :o me procedure as desenbec in me Final Safsty Anaivsis Recert?

Yes ( ) v No ( '

4 is a enange in tne Tecnnical Scecificauens involved?

No ( )

h v SAFETY EVALUATION: Answer me felicwing quescons witts a "yes" or "no", and provide specific reasons jusufying the cecisien:

1. Is me procacility of an occurrence, the censecuence of,sn accident, er me malfunction of safety.retated ecuicment, as grevicusly evaluated in me Final Safety Analysis Report, increasec?

Yes No, because:

- 2. Is the possibilir/ for an accident or the rnalfunction of i different a

type men any previously evaluated irphe Final Safety Analysis Report Yes V No, because:

createe?

$ /'

3. Is the margin of safety, as defined in the basis fpr any Technical Yes No, because: . . - . . . . .

Scecification, reducac?

Anv Answer

Yes ( ) All Answare No (p )

/

v Request and receive Nuclear Regulatory Commission aumortzation for change.

Authorization Received ( )

y ananate Precsours

NOTE: imolementation Any answer checked "yes a

//

should be reported in me Performed by / 4 annual recort to me NRC.

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l LZP INDEX PAGE 7/08/83 4

-ROC. NO. TITLE RE4. REV OATE CISAETT

.P 1200-4 CLASSIFICATION CF A LICUIC RELEASE Cl 5/82 01 f I

1. P 121C-1 HAZAR00US MATERIAL INCICENTS REPORTING C2 3/63 01 l uP 122C-1 EMERGENCY TELEPHONE NU'4BER C1 5/81 01 P 1220-4 DELETED Cl 7/81 01 CONTAINMENT ATMOSPHERE FOR RACICICINES DETERMINATION AND PARTICULATES ALTERNATE MEANS

.P 131C-1 NOTIFICATIONS CXt 7/83 C2

.P L320-1 AUGMENTATION CF PLANT STAFFING C5 1/83 02

P 133C-1 OELETED C2 7/82 02

.P 1330-2 DELETED C2 7/82 G3

P 1330-3 OELETED C3 7/82 03

.P 1330-4 CELETED C2 7/82 C3

P

. 1330-5 POST-ACCIDENT NO3LE GAS RELEASE RATE CO 11/SC 03 DETERMINATION

P 1330-6 DELETED C1 7/81 03

.P 1330-7 OELETED C2 7/82 02

'. P 1330-8 SAMPLING LIQUID PROCESS MCNITCRS Cl 8/82 G3 CURIriG LIQUID MCNITOR HIGH RACIATION ALARM CCNDITIONS P 133C-10 DELETED Cl 1/82 03 P 133C-11 OILUTION AND TRANSFER OF GAS SAMPLES CC 11/81 03 P 1330-20 POST-ACCIDENT ANALYSIS OF BARCN CO 3/81 03 (BACKUP PROCECURE)

P 1330-21 POST-ACCICENT ANALYSIS OF CHLORIDE C3 6/82 03 P 1330-22 CALIBRATICN OF THE MODEL 10 OIONEX C2 +/82 03 ION C:!n0"ATCGRAPH P 133C-23 DETERMINATICN OF REACTOR COOLANT PH, C2 6/82 03 CCNOUCTIVITY AND DISSCLVED OXYGEN CGNCENTRATION AT THE HIGH-RADIATION SAMPLE SYSTEM P 133C-24 OETERMINATICN OF REACTJR COOLANT C2 1/d3 03 nYJRCGEN ANO CFF-GAS CJWCENTRATIONS AT THE HIGH RADIATION SAMoLING-SYSTE.*

LZP-1330-20 Aevision 1 July 2o, 19d3 1

POST-ACCICENT ANALYSIS OF SORON (Sackup Procedure)

A. PURDOSE The purpose of this procedure is te celineate an alternate metnod for determining Doron following a Regulatory Guide 1 3 or 1.4 release of fission procucts. The metnod described by this procedure is referenced to as the Curcumin Spectrophotometric Metnoa.

8. REFERENCES

1. Final Report, Analyses for Dissolved Hycrogen, Di ssol ved Oxygen, Boron, Cnloride, pH, ano conductivity under normal Post-Acciaent Conditions, NUS Corporation, Octooer, 1980.

2. LCP 110-2, "Preparati'on of Reagents".

3. LCP 210-6, " Operation of the Klett-Summerson Colorimeter".

C. PRj3]CUISITES

1. Equipment:

a. Klett-Summer son Col or i meter .

o. Filter No. 54.,

c. 20 mm X 40 mm cell s.

c. Gracuated cylinders, 10 or 25 ml anc SCO ml.

1

e. Volumetric flasks. 25 m1, 100 ml ana 1000 ml.

f. Evaporating dishes. 10C to 150 ml capacity.

Vycor glass (Corning gl ass), or equivalent (usea for boron cetermination coly).

g. Oxford pipettes with disposable plastic tips, 1 m1, 4 m1, 5 m1, 15 m1, 20 m1, ana 5 ml .Mohr pipatta. nr aqu i vei en e. .

n. Beakers 250 ml or 400 ml, wide forr.

LZP-1330-20 Revision 1 July 26. 1933 2

i. Tongs, long reacn.

j. Pol yethyl ene sti rri ng roos, 7.

k. Medicine droppers, 7.

1. Filter paper, knatman No. 3C, or equi val ent.

m. Glass cr plastic funnel.

n. Semi-legarithmic paper, cual cycle.

o. Water bath, set at 55 + 2 C, in an operating fume nooa.

2. Reagents:

a. 95% Isopropyl al cohol .

D. Curcumin re6 gent.

c. Boron stock stancaro solution, 100C ppm coron.

d. Doron stancaro solutions, 0.5 ppm, 1.0 ppm, 1.5 ppm, and 2.0 ppin.

C. PRECAUTIONS

1. A Regulatory Guioe 1.3 or 1.4 release of fission products implies extremely nign levels cf radioactivity. Oose rates may De nigh enougn to prevent entry into many areas of tne plant tnat are normall y haoi taol e. Rad /Cnem Supervisicn snoulc ce contacted prior'to entry into any area wnen sucn a release of fission products is suspectec.

2. wear raciation dosimetry as recommended by Rad /Cnem Supervision.

3. Wear protective clothing and respiratory protection as recommenced Dy Rad / Chem Supervision.

4. Handle the sample container witn long reacn tongs.

Ooss ratss from a 5 mi sampla could ranga up to 50 R/nr.

5. Appropriate survey instruments snould os availaole for monitoring ouring ens processing anc analysis of this sample.

LLP-1330-;C Revision 1 July 26, 1983 3

6. Carry out all analytical operations cenino acequate shielding in an operating fume nood.

7. Se certain any spills are uipsa up immeciately ano properly disposed of.

8. The same geometry evaporating oisnes must ce usea for all standards and samples to assure that evaporative rates are equivalent.

9. The temperature of the Dath must be controlled so that all samples dry at the same rate.

10. The curcumin reagent must ce stored uncer refrigeration after preparation and not ce more tnan tnree days old.

11. Tests show tnat many variaoles can af f ect the color development in this procecure. To minimize these effects, the procedure includes processing stancard boron solutions along with the samples.

E. LIMITATIONS AND ACTIONS

1. The diluted reactor water sample should contain between 0.5 and 2 ppm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This proceaure may also oe usea for boren analysis unaer-normal conoitions. If so, treat tne sample in accordance witn practices for routine reactor water.

F. PROEjpyEj

1. Clean the immediate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical sur f aces, tne fil ter, ano tne cell s. The outaice l surface of tne cells must De free of dirt, fingerprints, ano scratenes.

LZP-1330-20 Revision 1 July 2.o . 1933 4 1 4 Pipette 1.0 ml of ODI water (bl ank ) and 1 0 ml or the 0.5, l.C, 1.5 and 2.0 ppm coron standaros into separate lacelea evaporating disnes.

5. Pipette 1.0 ml of the ailuted sample solution into two separate evaporating aishes for cuplicate analyses.

CAUTIO1 Carry out all anal yt i cal operations oenino acequate shieloing in an operating fume noco.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl the contents gentiy to mix, using icng tongs to nandl e the two radicactive samples.

7. Place each evaporating dish cn the cottcm of tne 250 or 400 m1 wice-form Deakers, using long tengs to hancle the radioactive samgles. Float the DeaKers in a water Datn set at 55 1 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness anc note the time of dryness for each sample.

9. Remove tne evaporating oisnes from tne catn at 15 minutes after the contents appear cry and allow them to cool to room temperature.

10. Acc approximately 10 ml of 95 percent isopropyl alcohol to eacn evaporating cisn. Use a pol yetnylene stirring rod to aic in dissolution of the rea-coloreo reaction product and oxalic acid.

11. Using a medicine arcpper, transfer the contents of the evaporating dishes to i r.d i v i dua l 25 mi volonetric flasks which have osen previousi y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent alcohol and add the contents to tne flasxs. Cilute the enntents of each Flask to 25 0 ml using 95 percent isooropyl alcohol.

13. Zero tne Klett-Summerson Colorimeter witn deionizea

.ater in accorcance witn Reference 3.

I l

LZP-1330-20 Ravision i July 20, 19d3

14. witnin one hour of aissolution of the dried procuct (step F.d.), pour the "olanka into tne cell ana measure the absorbance. Recora the reacing on LRC From 1088 (Attachment 4).

CAUTIGM The waste from steps F.15.-F.17. contains radionuclidesi dispose of this waste in accorcance with guidances provided oy Rad / Chem Sapervision.

2915 If cose levels warrant, tne Klatt-Summerscn shoulo ce put in the fume hood oenino the snieloing witn appropriate precautions caden to prevent contamination of this instrument. i

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour che sample into tne cell and measure the aosoroance. Recora tne reading on LRC Form 1088 (Attacnuent A).

h2If If a solution appears turoic, filter enrough a cry filter paper airectly inte a clean dry cell.

16. Empty and rinse the cell witn a small pcrtion of tne duplicate sample, tnen pour that sample into tha cell and measure tne aosoroance. Recora sne reacing on LRC From IC38 (Attachment A).

17. Empty and rinse the cell witn a small pcrtion of the 0.5 ppm boron standara, then pour the stancara into tne cell and measure the aosoroance. Record the reading on LRC Form 1C88 (Attachment A). Repeat for each of the remaining standarcs; 1.C. 1.5 and 2.0 ppm coron.

18. Subtract the "blanx" from each of the measured samples and stancards aosorcances. Reccro tne dif ference on LRC From 1088 (AttaCnment A).

19. Plot the corrected absoroance for the standards on the log axis of dual cycl e semilogarithric graph paper against concentration (linear axis), refer to attachment 8. Draw the oest fit straight line l

thrcugh the cata points.

l

f e-L2P-1330-2C ~~ !

davision 1 I July 26e 19 ti 3 o

20. Determine tne ppm coron in eacn sampic from the calioration curve. Record the val ue en LRC Form 1088 (Attachment A).

21. Calculate the average ooron concentraticn for the duplicate samples in accordance with LRC Form 10dd (Attacnment A). ,

22. Mul t i pl y tne average boron concentration by the sample ailution f actor to determine the sample coron concentration. Refer'co LRC Form 1088 (Attachment A).

23. Clean and decentaminate tna Klett-Sumcerscn Col or imeter and cell s as necessary. .

24. Einsure tne sampling containers and liquid samples have been properly disoosed of in.accorcance witn instructions providea oy Rad / Chem ' S'upe r v i~s i on. .

25. Survey the work area for radioactive. contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessiry. s G. CHECKLISTS

1. None.

H. Tg nNICAL SPE E Q TION REF6R Q g s

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' LZP 1330-20 l .

Revision 1

( .

ATTACHMENT A Ju1y 26, 1983 )

IASALLE COUNTT STATION Post-Accident Analysis of Boren Date:

. Absorbance Concentration frota Measurement Absorb ance-B i rmte Calibratien curse

'l 97.AM1r Satople 1 Sample 2 0.5 com Standard .,

1.0 outs Standard I ,

- 1.5 paa Standard 2.0 orm standard

_ Ave. boron conc., ppm = Conc. sample #1 + Conc. semple #2 2

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Sample boren cone., p;-' = (Ave. boron conc., ppm) x Dilution Factor (DF) e g

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O LZP INDEx PAGE 7/06/83 .

' ROC . NO . TITLE RE/. REv OATE CISKETT

.P L2CO-4 CLASSIFICATION CF A LI'JUIC R ELE ASE C1 5/82 01

'. P 121C-1 HAZAR0005 MATERIAL INCICENTS REPORTING C2 3/o3 01 49 1220-1 EMERGENCY TELEPHCHE NU'4SER Cl 5/81 01

.P 1220-4 DELETED C1 7/81 01

. CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATION AND PARTICULATES ALTERNATE MEANS sP L3LC-1 NOTIFICATIONS CXt 7/83 C2 1

P L320-1 AUGMENTATION CF PLANT STAFFING CS 1/83 02 l CP 133C-1 DELETED C2 7/82 02

'P 1330-2 DELETED C2 7/82 03 iP 1330-3 0ELETED C3 7/82 03

P

. 1330-4 CELETED C2 7/d2 03

!P 1330-5 POST-ACCIDENT NO3LE GAS RELEASE RATE CO 11/SC 03 DETERMINATION

'. P 1330-6 DELETED C1 7/81 03

'P

. 1330-7 DELETED C2 7/82 02

'. P 1330-8 SAMPLING LIOU10 PROC,ESS MONITCRS C1 8/82 03 CURIt.G LIQUID MCNITOR HIGH RACIATION ALARM CCNDITIONS

.P L33C-10 DELETED CL L/82 03

.P 133L-11 OILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 P 1330-20 POST-ACCIDENT ANALYSIS OF dARCN CO 3/81 03 (BACKUP PROCECURE)

P 1330-21 POST-ACCICENT ANALYSIS OF CHLORIDE 03 6/82 03 P 1330-22 CALIBRATICN OF THE MODEL 10 OIONEX C2 +/82 03 ICN CHRCMATCCRAPH 3 .133C-23 DETERMINATICN OF REACTOR COOLANT PH, C2 6/82 03 CCNOUCTIVITY AND DISSCLVED GXYGEN CCNCENTRATICN AT THE HIGH RAOIATICN SAMPLE SYSTEM P 133C-2* CETERMINATICN OF RIACTJR C'JOLANT C2 1/d3 03 NYJRCGEN AND CFF-GAS CJi4CE77 RATIONS AT THE HIGH RADI4TICN SAMoLING SYSTEM

LZP-1330-20 Avvision 1 July 20, 1903 1

1 POST-ACCICENT ANALYSIS OF SORCN (dackup Procedure)

A. fyfE01]

The purpose of this procedure i s to delineate an alternate metnod for cetermining ooron following a Regulatory Guice 1 3 or 1.4 release of fission prooucts. The inetnod described by this procecure is referenced to as the Curcumin Spectropnotometric Metnoo.

8. REELRENQg1

1. Final Report, Anal yses f or Di ssolved Hycrogen, Dissolved Oxygen, acron, Cnlorice, pH, and conductivity under normal Post-Accioent Conditions, huS Corporation, Octooer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Summerson Colorimeter".

C. P R FR EQU E SJJT_Ej

1. Eoulpment:

a. Klett-Summerson Color imeter.

o. Filter No. 54.

c. 20 mm X 40 mm cell s.

. c. Graduated cylinders, 10 or 25 ml and 500 ml.

e. Volumetric flasks. 25 m1, 100 mi ano 1000 mi.

f. Evaporating dishes. 10C to 150 mi capacity, Vycor glass (Corning glass), or equivalent (useo f or coron catermination cnl y).

g. Oxford pipettes witn disposable plastic tips, j

1 m1, 4 al, 5 m), 15 m1, 20 m1, ano 5 ml Mohr pipet +e. nr equivoient.

l

h. Beakers 250 ml or 400 m1, wide fort.

I i

LZP-1330-2C Revision 1 July 2o, 1983 2

1. Tongs, long reacn.

j. Pol yethyl ene sti rr ing roos, 7.

k. Medicine droppers, 7.

1. F11 ter paper, Wnatman No. 30. or equivalent.

m. Glass cr plastic funnel.

n. Semi-Icgarithmic paper, cual cycle.

o. Water Dath, set at 55 1 2 C, in an operating fume nood.

2. Reagents:

a. 95% Isopropyl al cohol .

c. Curcumin resgent.

c. Boron stock stancaro solution, 100C ppm coron.

d. Boron stancara solutions, 0.5 ppm, 1 0 ppm, 1.5 ppm, and 2.0 ppin.

C. PREC AtJTIONS

1. A Regulatory Guide 1.3 or 1 4 release of fission products implies extremely hign levels cf radioactivity. Oose rates may oe nigh enougn to prevent entry into many areas of tne plant tnat are normally haoitaole. Rad /Cnem Supervisicn snoulc ce contacted prior to entry into any area unen sucn a release of fission products is suspectec.

2. Wear raciation cosimetry as recommended by Rad /Cnem Supervision.

3. Wear protective clothing and raspiratory protection as recommenced Dy Rad / Chem Supervision.

4. Handle the sample container witn long reacn tongs.

Oose ratas from a 5 .r.1 sample could range up to 50 R/nr.

5. Appropriate survey instruments snould oe availaule for monitoring during ena processing anc analysis of tni s sainpl e.

~

LZP-133C-ZC Avvision 1 July 26,-19d3 2

6. Carry out all analytical operations cenino acequate shielding in an operating rume nooo.

7. Se certain any so;ils are niped up immeolately and properly dis: su of.

8. The same geometry evaporating aisnes must oe usuo for all standards and so.nples to assure that evaporative rates are egalvalent.

9. The temperature of the Dath must be controlled so that all samples cry at the same rata.

10. The curcumin reagent must ce stored under ref ri geration after preparation and not ce more tnan tnree days old.

11 Tests show that many variaoles can af f ect the color development in this procecure. To minimize these effects, the procedure includss procassing stanuaro boron solutions along witn the samples.

e. mnartoNs ano agnQM

1. The diluted reactor water sample snoula centain between 0.5 and 2 ppm coron.

2. The total anal ysi s time for this proceaure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This proceaure may also oe used for ooren analysis unoer normal concisions. If so, treat tne sampla in accordance witn practicos for routine reactor nater.

F. PRQQgQURS

1. Clean the immealate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfeces, the filter, ano ene cell s. The outsice surface of tne cells must De free of dirt, fingerprints, anc scratenes.

l i

l

LZP-133G-20 Revision 1 July 2o,.1983 4

4. Pipette 1.0 ml of 001 dater (bl ank ) and 1.0 ml or the 0.5, 1.0, 1 5 and 2.0 ppm coron stancaros inte separate laoeleo evaporating cisnes.

5. Pipette 1 0 ml of the diluted sample solution into two separate evaporating alsnes for auplicate analysos.

CAUTIO!

Carry out all anal yt i cal operations oenina acequate shielaing in an operating fume nooa.

b. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl tne contents gentiy to mix, using icnq tongs to nandl e the two radicactive samples.

7. Pl ace each evaporating dish on the cottom of tne 250 or 400 m1 wice-form osakers, using long tongs to nanale the radioactive samgles. Float the oedkers in a water catn set at 55 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness anc note the time of dryness for each sample.

9. Remove tne evaporating cisnes from tna Catn at 15 minutes after the contents appear dry and allow tnam to cool to room temperatara.

10. Aca approximately 10 ml of 95 percent isopropyl alcohol tc eacn evaporating cisn. Use a polyetnviene stirring rod to ala in Jissolution of tPe reo-Colored reaction procuct and oxalic acid.

11. Using a medicine orcpper, transfer the contents of l

the evaporating dishes to individual 25 mi volunetric flasks which have Deen prsviousiy rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent al cohol and aad the contents to tne flasks. Cilute the contents of each flask to 25.0 ml using 95 percent f isopropyl alconol.

l i

l 13. Zero the Klett-Summerson Colorimeter witn oeionizeo l water in accordance aitn Reference 3.

4

LZP-1330-20 Revision 1 July 2o, L9d3 3

14. witnin one hour of cissolution of the dried procuct (step F.d.), pour the "olank" into tne cell anc measure the absorbance. Record the reacing on LRC From 1088 (Attacnment A).

C_AUTID'd The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accorcance with guidances provided oy Rad / Chem Supervision.

!!EIE If cose levels warrant, tne Alatt-Summerscn shoulc ce put in the fume hood oenina the snielaing witn appropriate precautions tanen to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour tne sample into tne cell and measure the aosoroance. Recore tne reading on LRC Form 1088 (Attacnuent A).

h211 If a solution appears turoic, filter enrough a cry tilter paper airectly inte a clean cry cell.

16. Empty and rinse the cell witn a small ocreion of the duplicate sample, tnen pour that sanple into the cell and measure tne aosoroance. Reccro tne reacing on LRC From IC48 (Attachment A).

17. Ematy and rinse the cell witn a small pcrtion of the 0.5 ppm Doron standard, then pour tre stancara into tne cell ano measure the acsoroance. Record the reading on LRC Form IC88 (Attachment A). Repeat for each of the remaining standaras; 1.C, 1.5 ano 2.0 ppm coron.

18. Suotract the " blank" from each of the measuraa samples and stancaras aosorcances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoraance for tne standards on the log axis of dual cycle semilogarithnic graan paper against concentration (linear axis), refer to attacnment 8. Draw the oest fit straignt line througn the cata points.

LLP-1330-2C Revision 1 July 25, 1983 o

20. Determine the ppm coron in each sample from tne calloration curve. Record tne value on LRC Form 10a8 (Attachment A).

21. Calculate the average ooron concentraticn for the duplicate samples in accordance with LRC Form 1Gda (Attachment A).

22. Multiply tne average boron concentration Oy the sample ailution factor to cetermine the sample coron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontami nate the Alett-Sumre rsen Col or imeter and cells as necessary.

24. Ensure tne sampling containers and liquid samples have been properly aisposed of in accorcance witn instructions provided oy Rad / Chem Supervision.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. {HECKLTSTS

1. None.

H. Jg HNICAL SPE @ QJJON REFg g g i

1. None.

i i

I

j LZP 1330-20

,. Revision 1 ATIACILMENT A July 26, 1983 I

IASALLE COUNTT STATION Post-Accident Analysis of Boron Date:

Absorbance Concentration from Absorbance-31 mte Calibratien cu me Measuremene 97ANY Sample 1 Sample 2

~

0.5 ope Standard

/

1.0 com Standard 1.5 ppa Standard 2.0 nom standard Ave. boron conc., ppa = Conc. sample #1 + Conc. sample #2 2

Sample boron conc., ppa = (Ave. borou conc., ppm) x Dilution Factor (DF)

.. . - - , n . - -

4 LZP-1330-20 ATTACErr 3 I I

& I I I g i

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< *g_____.__=.r..=_-_z Fq ,*- _ M ?--T M a=- 4WM _n=. . _'1_E=-tg&W - -- - . - n_a u___sg e_=i=iMJ#= 2iminha-Pi=d _ _l;M -:h insNMJ 7_ _-=_ _r =__._ __ ___- =__e==.__ _ _ .g_a 5 _ __1_ __ __

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a

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0.5 0.75 1.0 1.25 1.5 1.75 Borer Concentration, ppm I

i

- , , , - , - _ ,l

l LZP INDEX PAGE 7/06/83 8 ROC. NO. TITLE RE/. REV OATE CISKETT P L2CC-4 CLASSIFICATION CF A LIQUIC RELEASE C1 3/82 01 HAZAR00US MATERIAL INCICENTS REPORTING C2 3/b3 01 (P 121C-1 LP 122C-1 EMERGENCY TELEPHONE NU 4BER Cl 5/81 Cl DELETED Cl 7/81 01 iP 1220-4 CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATICN AND PARTICULATES ALTERNATE MEANS LP 131C-1 NOTIFICATIONS CXt 7/83 C2 AUGMENTATION CF PLANT STAFFING CS 7/83 02 (P L320-1 ZP L33C-1 DELETED C2 7/82 02 iP 1330-2 DELETED C2 7/d2 03 LP- 133C-3 OELETED C3 7/82 03 (P 1330-4 OELETED C2 7/82 C3 SP 1330-5 PCST-ACCIDENT NOSLE GAS RELEASE RATE CO 11/SC 03 DETERMINATION IP 1330-6 OELETED Cl 7/81 03 iP 1330-7 OELETED C2 7/82 02 (P 1330-8 SAMPLING LIQUID PROCESS 10NITCRS C1 3/62 03 CURING LIQUID MCNITOR HIGH RACIATION ALARM CCNDITIONS IP 1330-10 DELETED C1 1/82 03 iP L33C-11 OILUTION AND TRANSFER OF GAS SAMPLES CC 11/81 03

P L330-20 POST-ACCIDENT ANALYSIS OF dARCN C0 3/S1 03 (BACKUP PROCECURE)

P

. 1330-21 POST-ACCICENT ANALYSIS OF CHLCRIDE 03 o/82 03

~

P L330-22 CALI6RATICN OF THE MODEL 10 OIONEX C2 4/82 03 ICM CHRCMATCORAPH

? 133C-23 DETERMINATICN OF REACTOR COOLANT PH, 02 6/82 03 L CCNOUCTIVITY ANO DISSCLVED OXYGEN CCNCENTRATICN AT THE HIGH RAOIATION SAMPLE SYSTEM i

CETERMINATICN OF REACTJR COCLANT C2 l/$3 G3

P 1330-2*

NYORCGEN AND CFF-GAS CJuCENTRATION5 AT THE HIGH PACIATION SAMDLING SYSTEM

L2P-1330-20 Aevisian 1 July 20, 19d3 i

POST-ACCICENT ANALYSIS OF SORON (Backup Procedure )

A. Py3P0}j The purpose of this procedure is to celineate an alternate metnod for cetermining Doron following a Regulatory Guide 1 3 or 1.4 release of fission proaucts. The inetnod described by this procecure is referenced to as the Curcumin Spectrophotometric Metnoa.

8. EffEElhC11

1. Final Report, Analyses for Dissolved hycrogen, Dissolved Oxygen, Boron, Cnloride, pH, anc conductivity under normal Post-Accident Conditions, huS Corporation, Octooer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Sum.nerson Colorimeter".

C. PREREQUISTTES

1. Ecolpment:

a. Klett-Summerson Color imeter.

o. Filter No. 54.

c. 20 mm X 40 mm cells.

c. Gracuated cylinders, 10 or 25 ml and 500 ml.

e. Volumetric flasks, 25 m), 100 mi anc 1000 mi.

f. Evaporating disnes. 10C to 150 ml capacity, Vycor glass (Corning gl ass), or equi val ent (usea for boron catermination cnly).

g. Oxford pipettes witn disposable plastic tips, 1 ml, 4 ml. 5 ml, 15 ml, 20 ml, ana 5 ml Mohr pipette, or equivelent.

n. Beakers 250 ml or 400 m1, wide ferr.

I

LZP-1330-20 Revision 1 July 26, 1983 2

.i. Tongs, long reacn.

j. Polyethylene stirring roos, 7.

k. Medicine droppers, 7.

1. Fil ter paper, knatman tao. 30, cr equi val ent.

m. Glass cr plastic funnel.

n. Semi-logarithmic paper, cual cycle.

o. Water oath, set at 55 1 2 C, in an operating fume nooc.

2. Reagents:

a. 95% Isopropyl alconol.

o. Curcumin reagent.

c. Boron stock stancaro solution, 100C ppm Doron.

d. Boron stancara solutions, 0.5 ppm, 1 0 ppm, 1.5 ppm, and 2.0 ppin.

C. P3gqAUIloys

1. A Regulatory Guide 1 3 or 1 4 release of fission products implies extremely hign levels cf radioactivity. Oose rates may oe nigh enougn to prevent entry into many areas of tne plant that are normally haoitaole. Rad /Cnem Supervisicn snoulc ce contacted prior to entry into any area wnen sucn a release of fission products is suspectac.

2. Wear raciation dosimetry as recommended by Rad /Cnem Supervision.

3. Wear protective clothing and raspiratory protection as recommenced by Rad / Chem Supervision.

4. Handle the sample container with long reach tongs.

Ooss ratas from a 5 m1 sampla cculd ranga up to SC R/nr.

l

5. Appropriata survey instruments snould os availaole for monitoring curing ena processing anc analysis of this sample.

l

LZP-133C-IC Aevision 1 Jul / 26,'19d3 3

6. Carry out all analytical operations ceninc aceauate shielding in an operating fume noco.

7. Se certain any spills are wipsa up imreciataly and properly disposed of.

8. The same geometry evaporating oisnes must ce useo for all stancards and so.nples to assure enat evaporative rates are equivalent.

9. The temperature of tne bath must be controlled so that all samples cry at the same rata.

10. The curcumin reagent must ce stored under refrigeration after preparation and not ce more tnan tnree days old.

11. Tests show tnat many variables can af f ect tne color development in snis procecure. To mininize enese effects, the procecurs includes processing stanuard boron solutions along witn the samples.

E. (13tTATIONS AND ACTICNS

1. The diluted reactor water sample snould cen ta in between 0.5 and 2 ppm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procedure may also De used for boren analysis unoer normal conaitions. If so, treat tne samp1=

in accordance witn practices for routine reactor nater.

F. PROCj0URE

1. Clean the immediate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfaces, une fil ter , ano tne cells. Tre outsice surface of the cells must De free of airt, fingerprints, and scraccnes.

i LZP-1330-2C Revision 1 July 20, 1983 s

4. Pipette 1.0 ml of 001 water (bl ank ) ano 1 0 ml or the 0.5, 1.C, 1 5 and 2.0 ppm coron stancaras into separate laoelea evaporating cisnes.

S. Pipette 1.0 ml of the ailuted sample solution inte two separate evaporating aishes for cuplicate analyses.

CAUT!OJ Carry out all anal yt i cal operations oehina acequate shielcing in an operating fume nood.

6. Pipette 4.0 ml of curcumi n reagent into eacn evaporating dish. Swirl the contents gentiy to mix, using icng tongs to nandl e the two racicactive samples.

7. Place each evaporating di sh on the Dottom of tne 250 or 400 ml wice-form oeakers, using long tcngs to nanale the radioactive samgles. Float the Deaners in a water batn set at 55 1 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness ano note the time of dryness ror each sample.

9. Remove tne evaporating cisnes from tne catn at 15 minutes after the contents appear dry ano allow them to cool to room temperatare.

10. Acc approximately 10 ml of 95 oercent isopropyl alcohol to eacn evaporating cisn. Use a polyetnylene stirring rod to ala in dissolution of the rea-colored reaction proauct and oxalic acid.

11. Using a medicine arcoper, transfer tne contents of the evaporating cishes to individual 25 mi volunetric flasks mnich hava cean previousl y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent al cohol and add the contents to tne flasas. Cilute the contents of eacn Flasw to 25.C ml using 45 percent isopropyl alconol.

13. Zero tne Klett-Summerson Colorimeter witn ceionizac water in accordance .i tn Ref erance 3.

i

LZP-1330-20 Ravision 1 Jui f 20, 19d3

14. Within one hour of oissolution of the dried proouct (step F.d.), pour the aolanK" into the cell ano measure the absorbance. Record the reacing on LRC From 1088 (Attachment A).

fr.*!11E The waste from steps F.15.-F.17. contains radionuclidos; dispose of this waste in accoraance with guidances proviced oy Rad / Chem Supervision.

U.915 If cose levels warrant, tne Klett-Summersen shoul a ce put in the fume hood oenino the shieloing witn appropriate precautions taxen to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour the sample into tne cell and measure the aosoroance. Recorc tne reading on LRC Form 1C88 (Attacnaent A).

k915 If a solution appears turoic, filter enrough a cry tilter paper airectly inte a clean cry cell.

16. Empty and rinse the cell witn a small pcrtion of the duplicate sample, enen pour that sarple into tha cell and measure tne 60soroance. Recoro tne reacing on LRC From 1C38 (Attacnnent A).

17. Empty and rinse the cell with a small pcrtion of tne 0 5 ppm boron standara, then pour the standara into tne cell and measare the aosoroance. Record the reading on LRC Form 1088 (Attachment A). Repeat for each of the remaining standards; 1.C. 1.5 ano 2.0 ppm coron.

18. Sootract the "olank" from each of the measured samples and standards aosoroances. Recera tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for the standards on the log axis of dual cycle semilogarithnic graan paper against concentration (linear axis), refer to attachment 8. Oran tha oest fit straight line thrcugh the cata points.

LZP-1330-2C Revision 1 July 26. 1983 e

20. Determine the ppm coron in each sample from the calloration curve. Record tne value on LRC Form 1088 (Attacnment A).

21. Calculate the average ooron concentraticn for the duplicate Samples in accordance with LRC Form 1Gda (Attachment A).

22. Mul t i pl y tne average boron concentration by the sample oilution factor to determine the sample coron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontaminate tne Klett-Sumrerson Colorimeter and cells as necessary.

24. Ensure the sampling containers and liquid sampl es have been properly disposed of in accordance witn instructions provided Dy Rad / Chem Supervision.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. {HECKLISTS

1. None.

H. J,152 ICAL SPE M QJ,J,0N RQFgR,g g 1

1. None.

I t

LZP 1330-20 Revision 1 ATTACIDENT A July 26, 1933 IASALLE COUNTY STATION Post-Accident Analysis of Boron Date:

Concentration from j

, Absorbance Measu m...nr Absorbance-B % k Calibratf en cur ,

Mf _ A MY Sample I Sample 2 0.5 pos Standard 1.0 com Standard 1.5 pem Standard 2.0 oom standard Ave. boron conc., ppa = Conc. sample #1 + Conc sample #2 2

Sample boron conc,, ppa = (Ave borou conc., ppm) x Dilucion Factor (DF) l 1

l

.. - - - . _ - . _ _ . - _ - - - ~ - .. . .. - . - . . . -- . .. .-..-- . _ . . _ . -_

i L2P-1330-20 ATTACIMENT 3

.W ;

i s

1 4 t s .

1 ,

a . i ,

i m 1 1

1 aa

i. r i i , ,i i i -

. .. .. i i

& , i i , e i I i , , t 4 . t , L . . - -* . - . . .

. . . + . > . . +4 .

as ,,, . . . , , . . . . , . , i . , , , . . .

Of 3 u.

ze ai 3

ee g -

o

,1 .

j . - .

g

' . . l N , ,

, 2, m

e m

as e

4

.a e 4

i 4&

5Z

. - 7 c

jut one -

a

.Z-3 .r. C

. J2.

5

t s:

0 a 310.

~

a$2 ln 4

- d

., G 3

i

, 6 i

I I l

, i i . . i - i. . ,

, , , , . . , .ii , , ,

I . i t i . . 3 , I i e i , , , i 6

,,, . . . . . , i . . . , . . . . . . .

l

, i ii .

1, . . . , . ,

t 0.3 0.75 1.0 1.25 1.5 1.75 2.0 Boron Concentration, pos l

l l- , - - . - , . . . . , , . . - , - , - - - , - - , _ .- - . - . - - - . - . . - - - ...- . .- - .. . - - , - . - .

LZP INDEx JAGE f 7/06/83 8R OC . .40 . TITLE red. AEV OATE CISAETT CLASSIFICATION CF A LIOUIC REL2ASE C1 3/82 01

P 120C-4 HAZARDCUS MATERIAL INCICENTS REPORTI'4G C2 3/63 01 (P 121C-1 C1 5/81 01 LP 122C-1 EMERGEf4CY TELEPHONE NUMBER DELETED C1 7/81 01 P 1220-4 CONTAINNENT ATMOSPHERE FOR RACICIDINES DETERMINATION AND PARTICULATES ALTERNATE MEANS (P 131C-1 f40TIFICATIONS OL{- 7/83 C2 AUGMENTATION CF PLANT STAFFING CE 1/83 02 EP 1320-1 C2 7/82 02 (P 133C-1 OELETED iP 1330-2 DELETED C2 7/82 C3 DELETED C3 7/82 03

P 1330-3

P 1330-4 DELETED C2 7/82 03 1330-5 PCST-ACCIDENT NO3LE GAS RELEASE RATE CO 11/ dC 03

P DETERMINATION

P

. 1330-6 OELETED 01 7/81 03

.P 1330-7 OELETED CZ 7/82 02 SAMoLING LIQUID PROCESS MONITCRS C1 8/82 03

.P 1330-8 CURIt.G LIQUID MCNITOR HIGH RADIATION ALARM CCNDITIONS P 1330-10 DELETED 01 1/82 03 P 133L-11 DILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 P 1330-20 PCST-ACCIDENT ANALYSIS OF dARCN CO 3/81 03 (BACKUP PROCECURE)

P 1330-21 POST-ACCICENT ANALYSIS OF CHLCRIDE 03 6/82 03 P 1330-22 CALI8RATICN OF THE MODEL 10 OIONEX C2 */82 03 ION C:tROM ATCGR A,"tt DETERMINATICN OF REACTOR COOLANT PH, C2 6/82 03 P 1330-23 CCNOUCTIVITY AND DISSCLVED OXYGEN CCNCENTRATION AT THE HIGH RADIATICN SAMPLE SYSTEM CETERMINATION OF REACTJR CJCLANT C2 1/d3 33 P 133C-24 HYJACGEN AND CFF-GAS CJdCENTRATIONS AT THE HIGH RA0!ATION SAMoLI'4G SYSTEM

LZP-1330-20 Awvision 1 July 20, 19d3 L

POST-ACCICENT ANALYSIS OF 30RCN (dackup Procedure)

A. Py3PO}j The purpose of this procedure is to delineate an alternate metnod for cetermining Doron following a Regulatory Guioe 1 3 or 1 4 release of fission proaucts. The netnod described by this procedure is referenced to as tne Curcumin Spectropnotometric Motnoo.

8. RjfgR{NCjS

1. Final Report, Analyses for Dissolved hycrogen, D i s sol ved Oxygen, Boron, Chloride, pH, anc conductivity under normal Post-Accident Conditions, huS Corporation, Octooer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of tne Klett-Summerson Colorimeter".

C. 23fdg00!STTES

1. Equipment:

a. Klett-Summerson Color imeter.

o. F il ter No. 54.

c. 20 mm x 40 mm cell s.

c. Gracuated cylinders, 10 or 25 ml ana 500 ml.

e. Volumetric flasks, 25 m1, 100 ml ano 1000 ml.

f. Evaporating disnes. 10C to 150 ml capacity, Vycor glass (Corning gl ass), or equivalent (usec f or boron catermination cnl y).

g. Oxford pipettes witn disposable plastic tips, 1 m1, 4 al, 5 m1, 15 ml, 20 ml, ana 5 ml Mohr ni,natte. nr equ i val ent .

h. Beakers 250 ml or 400 m1, wide fors.

. l l

l 1

l LZP-1330-20 Revision 1 July Joe 1983 2

i. Tongs, long reacn.

J. Pol yethyl ene sti rri ng rods, 7.

k. Medicine droppers, 7.

1. Fi l ter paper, knatman No. 30, cr equi val ent.

m. Glass cr plastic funnel.

n. Semi-1cgarithmic paper, cual cycle.

o. Water oath, set at 5512 C, in an operating fume hood.

2. Reagents:

a. 95% Isopropyl alcohol.

o. Curcumin reagent.

c. Boron stock stancaro solution, 100C ppm coron.

d. Boron stancara solutions, 0.5 ppm, 1.0 ppm, 1.5 ppm, and 2.0 ppin.

c. paggaurrons

1. A Regulatory Guice 1.3 or 1.4 release of fission products implies extremely hign levels cf radioactivity. Oose rates may os nigh enough to prevent entry into many areas of tne plant that are normally haoitaole. Rad /Cnem Supervisicn snoulc oc contacted prior to entry into any area unen such a release of fission products is suspectec.

2. wear raciation dosimetry as recommendec oy Rad / Chem Supervision.

3. Wear protective clothing and respiratory protection as recommenced oy Rad / Chem Supervision.

4. Handle the sample container witn long reacn tongs.

Oosa ratas frca a 5 mi sample could ranga up to 50 R/hr.

5. Appropriata survey instruments snould oe availaole for monitoring during tna processing anc analysis of this sample.

LZP-133C-2C Revision 1 Jul / 26,'19d3 3

6. Carry out all anal yt i cal operations ceninc acequate shielding in an operating fume hooa.

7. Se certain any spill s ara nipea up immeciatel y and properly disposed of.

8. The same geometry evaporating aisnes must ce used for all standards ano so,nples to assure that evaporative rates are agaivalent.

5 The temperature of the cath must be controlled so that all samples dry at the same rata.

10. The curcumin reagent must ce stored under refrigeration after preparation and not ce more tnan :nree days old.

11. Tests show tnat many variaoles can af f ect the color development in this procecure. To minimize enese effects, the procedure includes processing stancara boron solutions along with the samples.

E. W ITATIONS AND Aglog g

1. The diluted reactor water sample snoul d ccntain Detween 0.5 and 2 ppm coron.

2. The total analysis time fo r this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procedure may also oe used for Dorcn analysis unoer normal conoitions. If so, treat tne sampla in accordance witn practicas for routine reactor water.

F. PROCjouRf

1. Clean the immediata work area.

2. Inspect the laoware and clean if necessary using-approved cleaning techniauss.

3. Clean tne Klett-$ummerson Colorimeter optical surfaces, the filter, ano tne cells. The outsio=

surface of tne cells must De free of dirt, l . fingerprints, and scratenes.

l l

l

LZP-143C-2C Revision L July lo, 1983 s

4. Pipette 1.0 ml of ODI sater (bl ank ) anc 1.C ml or tha 0.5, 1.0, 1 5 and 2.0 ppm coron stancaras inte separate laoeled evaporating cisnes.

5. Pipette 1.0 ml of the ciluted sample solution into two separate evaporating aishes for cuplicate analyses.

2 1119.!

Carry out all anal yt i cal operations oenino adequate shieloing in an operating fume noca.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl the contents gently to mix, using lcng tongs to nandl e the two racicactive samples.

7. Pl ace each evaporating di sn on the cottcm of tne 250 or 400 ml wide-form oealers, using long tongs to nanole the radioactive samgles. Float tne Deaners in a water Datn set at 55 1 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness and note the time of dryness for each sample.

9. Remove tne evaporating oisnes from tne catn at 15 minutes after the contents appear cry ano allon enem to Cool to room tempera Jre.

10. Acd approximately 10 ml of 95 oercent isopropyl l

alcohol to eacn evaporating cisn. Use a polyetnf lene stirring rod to aio in aissolution of the reo-coloreo reaction product and oxalic acid.

11. Using a medicine oropper, transfer the contents of the evaporating cishes to individual 25 mi volumetric l

flasks wnich have ceen previously rinsec witn 95 percent alconol.

12. Rinse the evaporating oisnes witn 95 percent al cohol and add the Contents to tne flasks. Cilute the contents of eacn Flasw to 25.C m1 using Q5 percent isopropyl alcohol.

13. Zero tne Klett-Summerson Colorimeter witn deionizeu water in accordance itn Reference 3.

l

.. . . . . . __.__._______ _ ___ _ _ _ _J

4 LZP-1330-20 Revision 1 Jul f 2o, 19d3 3

14. within one hour of oissolution of the dried proouct (step F.d.), pour the "olanka into tne ceII anc measure the absorbance. Racord the reacing on LRC From 1088 (Attacnment 4).

CAUTION The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accoroance with guidances provided oy Rad / Chem Supervision.

M.3 If dose levels warrant, tne Klatt-Summerscn snoula De put in the fume hood oeninc the snielding nitn appropriate precautions taken to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion or one of tne samples, then pour the sample into tne cell and measure the aosoroance. Recorc tne reading on LRC Form 1C88 (Attacnment A).

M3 If a solution appears toroic, filter enrougn a cry fil ter paper di rectl y inte a clean dry cell.

16. Empty and rinse the cell witn a small pcrtion of the duplicate sample, tnen pour tnat sarple into the cell and measure tne aosoroance. Recora ne reaoing on LRC From 1C38 (Attachment A).

17. Empty and rinse the cell witn a small pcrtico of the 0 5 ppm coron stancara, then pour tre stancara into the cell and measare the aosoroance. Record the reading on LRC Form 1088 (Attachment A). Repeat for each of the remaining stancards; 1.C. 1.5 ano 2.0 ppm coron.

18. Suotract the " blank" from each of the measured samples and stancards aosorcances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for the standards on the log axis of dual cycle semilogarithric graan paper against concentration (linear axis), refer to Attachment 8. Draw the oest fit straignt line through the data points.

1 1

LLP-1330-2C Revision 1 July 26. l963 o

20. Determine tne opm coron in each sample frcm the calloration curve. Record the value on LHC Form 1088 (Attachment A).

.. 21. Calculate the average ocron concentraticn for tha duplicate samples in accordance with LRC Form ICdd (Attachment A).

22. Multipl y tne average boron concentration by tne

' sample allution f actor to determine the sample coron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontaminate tna Klett-Sumrerscn Colorimeter and cells as necessary.

24. Ensure the sampling containers and liquid samples have been properly disposed of in accorcance witn

( instruations provided oy Rad / Chem Supervision.

l l 25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. (HECKLISTS

1. None.

l H. J,jf(MNICAL_SPE M M U CN REFg ggjl

1. None.

l

- LZP 1330-20 ,

Revision 1 l' ATIACHMENT A July 26,1933 LASALLE COMITY STATION Post-Accident Analysis of Baron Date:

Absorbance Concentration from

~

Measurement Absorb anc e-B i mte Calibratim cur-re MY AMir Sample 1 Sample 2 0.5 paa Standard 1.0 opa Standard /

1.5 ppe Standard N

2.0 nom standard Ave. boron cone., ppa = Conc. sample #1 + Coac, sample #2 2

l l

Sample boron conc., ppa = (Ave. borou conc., ppm) x Dilution Factor (DF) '

I

-1 v- ,

,_,as" e

E s

w y $ ,

._ m

4

'\

q ,

i .

4 ATTAC1DiENT 3 LZP-1330-20 1 ==ri

. - July 26, 196)ill

, 3 (Final) 1

s e ,

1 7

1

- \

[

, e t

,.-.= t i

1 1

i I

1 s

i gp .

ii

- 1 , i j i 6 , ! i

j Y m: 4, i - ' ' ' '

, G . . i 6 1 , , , 5

se , . i . . . , , i , ..i i , i *

.i.ii. ' ' 4 , - - - i' ' ' ' - ' ' '

si , ,' i . ,~ , , , , . i,, . . . . . !

4 S.

gT 3 I

1 e

r 5 m -s

'I : ,

{. ' ' - ' i ' f

, .. ; ,: - .j i , 1 i ' ,

1

'I 4 - ! ' ' I I i ' ' ' t j g2 i ,i6 6 i . i : . I I i .li i

j i ! t i I ' : ,

!i lii.; .

. .l ! ' j . ' '. '. '.i..i. . .i .

' i . , i i ; . . . . . . - i lei

> i- - 4

' i -

-i, . . . i . ..

m

r.

4 e

i us e

. : 4 C: -

1 !E

- v -

-e w i' I,as 4

i 2i! *= _.

l

t. 2 0, f

! 3

. <2- -> .

25 i;a ___

' i m

e= 4 i

4 t

d> 2

. u .

I. n I

.)

i

. s 1

l 1

1 _

I I

', +>

' ,, , , . . . , i 4-

, , . i + ' '

, , . . - - ' t i

,, . . i .. . . 4 . 4 ' + ' i ' '

, , , . , , , , ii # i !

s 4

1 I

3

, . i

. , . . . 6 4

' O.5 0.75 1.0 1.25 1.5 1.75 2.0 Boron Concentration, ppm s ,

. . . ~ . _ + . . . . - . . . - . . . . . _ . .--. - - . - - . . . . . . - . - . . , . - . . - . - . - . . - - . , _ . - - - . - , - - , - . - . -

l l

LZP INDEX PAGE .

7/06/83 9

> ROC. NO. TITLE AE/. AEs DATE GISKETT_

CL ASS If (C ATION CF A LIJUIC RELEASE C1 3/82 01 iP' 1200-4 HAZARCCUS MATERIAL INCICENTS REPORTING C2 3/e3 01

!? 121C-1 C1 5/81 01 49 1220-k' EMERGENCY TELEPHONE NUMBER 1220-4, DELETED C1 7/31 01 LP .

CONTAINMENT ATMC5PHERE FOR RACIOIDINES

. 0ETERMINATION AND PARTICULATES ALTER 4 ATE MEAN5 IP 131C-1 NOTIFICATIONS 04 7/83 C2

~

AUGMENTATION CF PLANT STAFFI,NG C5 1/83 02 CP 1320-1 ,

OELETED__ ' C2 7/82 02 EP 133C-1 C2 7/82 03

P 1330-2 DELETED P 1330-3 _

OELETED _

C3 7/82 03 P 1330-4 OEL ETED .C2 7/82 03 1330-5 POST-ACCICENT NO3LE GAS RELEASE RATE CO 11/SC 03

P ~~~

DETERMINATION

P 1330-6 .OELETED C1 7/81 03

.P -1330-7 OELETED C2 7/82 02 SAMPLING LIQUID PROCESS MONITCRS C1 8/82 03

.P 1330-8 CURING LIQUID MCNITOR HIGH RACIATION ALARM CCNDITICNS P 1330-10 DELETED C1 1/82 03 133C-11 OILUTION AND TRANSFER'OF GAS SAFPLES CO 11/81 03 P

P 1330-20 POST-ACCIDENT ANA' LYSIS OF dARCN CO 3/81 03 (SACKUP PROCECURE)

P 1330-21 POST-ACCICENT ANALYSI'S OF CHLCRIDE C3 o/82 03 P 133C-22 CALIBRATICN OF THE MODEL 10 DIONEX C2 4/82 03 ICM CHRCMATECRAPH DETERMINATICN OF REACTOR COOLANT PH, C2 6/82 03 2 1330-23 CONOUCTIVITY AND CISSOLVED OAYGEN f CGNCENT,RATIGN AT THE HIGH RADIATION ,,

'7 <

SAMPLE SYSTEM P if30-24 ,

OETERMINATICN OF REACTJR CJCLANT C2 1/d3 G3

- NYJRCGEN AND CFF-GAS CJnCENTRATIONS AT

<THE HIGH RAOIATION SAMDLING SYSTE.*

,q c ;-

' f u

' - ,, 3

?, \ ?

- s . :. , .

e LZP-i330-20 Aevision 1 July 20. 19d3 1

POST-ACCICENT ANALYSIS OF 3GRCN (Backup P roce dur a )

A. Pg3POjj The purpose of this procedure is to delineate an alterr. ate metnod for cetermining coron following a Regulatury Guide 1 3 or 1 4 release of fission proaucts. The metnod described by this procedure is referencsd to as the Curcumin Spectropnotometric Metnoa.

B. SEf!SibEs1

1. Final Report, Analyses for Dissolved Hycrogen, Di ssol ved Ox ygen, Boron, Cnl oride, pH, anc conductivity under normal Post-Accident Conditions, huS Corporation, October, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Summersen Colorimeter".

C. PREREQUISITES

1. Equipment:

a. Klett-Summerson Color imeter.

o. F il ter No. 54.

c. 20 mm X 40 mm cells.

c. Gracuateo cylinders, 10 or 25 ml ana 500 ml.

e. Volumetric flasks. 25 m1, 100 ml anc 1000 ml.

f. Evaporating disnes. 10C to 150 ml capacity, Vycor glass (Corning gl ass), or equivalent (usec f or boron aetermination col y).

g. Oxford pipettes witn disposable plastic tips, 1 m1,

m1, 5 m1, 15 ml, 20 mi, anc 5 ml Mohr pipette, or aquivalent.

h. Beakers 250 ml or 400 m1, wide (crs.

LZP-1330-20 Ravision 1 July 26, 1983 2

i. Tongs, Icng reacn.

J. Pol yethylene sti rr i ng rods, 7.

k. Medicine droppers, 7.

1. Fil ter paper, knatman t4o. 30, cr equivalent.

m. Glass cr plastic funnel.

n. Semi-logarithmic paper, cual cycle.

o. Water oath, set at 55 +2C. in an operating fume hood.

2. Reagents:

a. 95% Isopropyl alcohol.

D. Curcumin reagent.

c. Baron stock stancaro solution, 100C ppm coron.

d. Boron stancaro solutions, 0.5 ppm, 1.0 ppm, 1.5 ppm, and 2 0 ppin.

c. pagq3uIrons

l. A Regulatory Guide 1.3 or 1 4 release of fission products implies extremely hign levels cr radioactivity. Oose rates may oc nigh enougn to prevent entry into many areas of tne plant tnat are normally haoitaole. Rad /Cnem Supervisicn shoulc ce contacted prior to entry into any area unen sucn a release of fission products is sospectec.

2. wear raciation cosimetry as recommended oy Rad / Chem Supervision.

3. Wear protective clothing and respirstory protection as recommenced oy Rad / Chem Supervision.

f

4. Handle the sample container with long reach tongs.

Oose ratss frcm a 5 mi sample coulc ranga up tc 50 l

R/nr.

l

5. Appropriata survey instruments snould oe availaole for monitoring'during tne processing anc analysis of this sample..

LZP-133C-iC Revision 1 Jul / 26, 19d3 3

6. Carry out all analytical operations cenino acequate shielding in an operating fume hood.

7. Se certain any spills ara alpea up imreciately anc properly disposed of.

8. The same geometry evaporating aisnes must ce usea for all standards ano so,nples to assure tnat evaporative rates are equivalent.

9. The temperature of the bath must be controlled so that all samples dry at the same rata.

10. The curcumin reagent must ce stored under refrigeration after preparation and not ce more tnan tnree days old.

11. Tests show that many variaoles can af f ect the color development in this procecure. To minimize these ef fects, the procedure includes processing stanGard Doron solutions along with the samples.

E. (DJ,,,Idligb,,1.,,,A N D AE,Ilgu2

1. The diluted reactor water sample should centain Detween 0.5 and 2 apm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This proceoure may also oe used for boren anal ysis under normal conoitions. If so, treat tne sample in accordance witn practices for routine reactor water.

F. PROCj00Rj

1. Clean the immediate worn area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfaces, une fil ter , ano tne cells. The outsiae surface of tne cells must De free of cirt, fingerprints, ano scratenes.

LZP-1330-2C Revision 1 July 2o, 1983 r

4. Pipette L.0 il of DOI dater (bl ank ) and 1.0 n1 or the 0 5, 1.0, L.5 and 2.C ppm ooron standaros inte separate laoeled evaporating cisnes.

5. Pipette 1.0 ml of the ailuted sample solution intc two separate evaporating cisnes for cuplicate analyses.

I CAUT_D4 Carry out all anal yt i ca l operations cenino acequate shielaing in an operating fume nood.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl the contents gentiy to ;n i x e using leng tongs to nandl e tne two radicactive samples.

7. Pl ace each evaporating dish on the cottom of tne 250 or 400 m1 wice-form oeakers, using long tcngs to nanole the radioactive samgles. Float the Deaners in a water batn set at 55 1 2 C.

a. Evaporate the contents of each evaporating disn to complete dryness and note the time of dryness tor each sample.

9. Remove tne evaporating cisnes from the Datn at 15

.ai nu tes af ter the contents appear dry and allow them to cool to room teaperatare.

10. Aaa approximately 10 ml of 95 percent isoprcpyl alcohol to eacn evaporating aisn. Use a pol yetnylene stirring rod to aic in Jissolution of the rea-colored reaction procuct and oxalic acid.

11. Using a medicine arcpper, transfer the contents of the evaporating cishes to individual 25 mi volunetric flasks wnich have oesn previous 1 y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent alcohol anc aad the contents to tne flasks. Cilute thw enntents of asen Flasw to 25.C ml using 95 percent isooropyl alconol.

13. Zero tne Klett-Summerson Colorimeter witn ceionizeo water in accordance witn Referance 3.

l l

LZP-1330-20 Ravesion 1 July 20. 19d3 14, within one hour of aissolution of the dried procuct (step F.d.), pour the "olanx" intc tne cell ana measure the absorbance. Record the reacing on LRC From 1088 (Attachment A).

~.

M19.3 The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accorcance with guidances provided of Rad / Chem Supervision.

U21s If dose levels warrant, tne Klatt-Summerscn should oe put in the fume hood oenino the snielaing witn appropriate precautions taxen to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion or one of tne samples, then pour une sample into tne cell and measure the aosoroance. Record tne reading on LRC Form LC88 (AttaCnment A).

h91s If a solution appears turoic, filter enrough a cry t il ter paper ai rectl y intc a clean cry cell.

16. Empty and rinse the cell witn a small pcrtion of the duplicate sample, enen pour that sample into the cell and measur'e tne aosoroance. Recora tne reacing on LRC From 1C88 (Attachment A).

17. Empty and rinse the cell witn a small pcrtion of the 0 5 ppm Doron standard, then pour the stancara into tne cell and measare the aosornance. Record l

the reading on LRC Form 1C88 (Attachment A). Repeat for each of the remaining standarcs; 1.C, 1.5 ano 2.0 ppm coron.

18. Subtract the " blank" from each of the measured samples and stancards aosorcances. Reccrd tne l difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for the standards on the log axis of dual cycle semilogarithnic graan paper against concentration (linear axis), refer to Attachment 8. Draw the oes fit straight line thrcugh the data points.

l LZP-1330-2C Revision 1 July 26. 1983 0

20. Determine the ppm Doron in each sample from tne calloration curve. Record tne value cn LRC Form 1088 (Attacnment A).

21. Calculate the average coron concentraticn for the duplicate samples in accordance witn LRC Form lOdd (Attachment A).

22. Multiply tne average boron concentration oy the sample cilution factor to determine the sample coron concentration. Refer to LRC Form 1088 (Attachment A).

23. Cl ean and decontaminate tne Klett-Sumrerscn Col or imeter and cells as necessary.

24. ensure the sampling containers and liquid samples have been properly disposed of in accorcance witn instructions provided oy Rad / Chem Supervision.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. [HECKLISTS

1. None.

H. M g ICAL SPE @ Q UCN R EFggg1

1. None.

LZP 1330-20 Revision 1 ATTACmENT A JuIy 26, 1933 IASALLE COUhTT STATION Post-Accident Analysis of Baron Date:

Absorbance Concentration from Ab s orb an c e-B 1,nte Calibrarien cu m ,

Measurement RTANY Sample 1 Sample 2 0.5 ppm Standard 1.0 com Standard

_1.5 ppm Standard ,

2.0 com standard Ave, boron conc., ppa = Conc. sample #1 + Conc. sample #2 2

Sample boron conc. , ppa = (Ave. borou conc., ppm) z Dilution Factor (DF)

- . . - - - - . . _ . . - - . .- - .. - - . . .__ -. - - - .. _-- . . ~- -- -

l AITAcafENT 3 LZP-1330-20 i i i i

i i i l I I i g i i

i I I l 1

I i

s:

T .

1 r

i i 4 4

,8 I

i

H E

!, 3; ;

i z l

) o >

,i

, i s a i , . , i i

a ii , . i i i a i i 6 . , # 3 t I j O ii , , es i 6 i

, , - c ag . i , , ,. . . . -, .~ . . . , , , i . . .. . , , ... . ,

e

3 e 6 . i . .. . . e i 6 * . s .

e i

)ae a s i . . . . . i a ,

c1 u

a. .

i j Zf Wg b t

il, O.

E 1 % -

m. , ,

1 I e

h 1 1 I .

i i ! I I i i i i I i 8

I I t ,. I i !

I 1 I I

, , i , , i .

. i , , , , i r ,

ma i , . i 1 . , .

g

, , , i i i . . . . , . . ,

i , . , , , , i . , ,. , , . ,. . ,

, i -

i i, . . . . . . . . . . . . . i . . . . , , , , , . .

. . . , i . . . , i ,

, i i. : -' -

,' . 2 l3: = _ . . . ~ . . ' ^

::_ ;= 51 =.p-x 2

- - ^ . . .' ? ' _~ : l-5 l~ _-_ 5 ~= l - - -W4^hi= % = * - . - -

w '_ 3

, e ,=,_- 3w -

- + ; -. ; .. . - :. .-y7 -= m 1 pg_gg _

- " 3 ? =- - . . '= - -- c. - ~ NE -i=~ "$ ~id = # 5 -t l- #5- = 4'~= '= h= --- M =-iM3E J - h mic+ M arw2g-s:- -Es h_hsca- =J -se-as 4

z r7 ~ =d: -

- - i - ' - - - -

, . e C ah - --. . . _=~:=--~:==----:==--r,==-===-_-=_ -n- n- -- z n s s; -_ r:- - ==--=-==__m=---=--=_--m--_=----=

t ..-_a_-- =

4 3 s : v-g E

,u r a a:

si.a . -

v ::o 1

.-3 22 f

e4>

.o- s i .g 3 ivo -

. i.,z .a as 4 ins t

3 e4

e. a f >

, u M i g

t a i 6 A f

, I t f

4 i f f A

, . . , , ,,. . . , , . , , . . .,, , , i

. , , i . . , , ,

, . . , , , ,, . . . e

,,. ...i , i i i l

L I l 1

6

, i

.t

, i t t - -

t , b i , , , . . ,

. . l

, , . . . . , i 1

0.5 0. M 1.0 1.25 1. 5 . 1.75 2.0 t l

Boron Concentration, ppa i

- -~ . -__ _- - . ~ . , . . . _ _ , . _ , , _ _ . ._,_ _ ___ _ _

LZP INDEX PAbE 7/C6/83

) ROC. NO. TITLE RE/. REV OATE CISAETT CLASSIFICATION CF A LIQUIC RELEASE Cl 5/82 01 IP L200-4 HAZAR00US MATERIAL INCICENTS REPORTING C2 3/63 01 1P 121C -1 Cl 5/81 01 LP 1220-1 EMERGENCY TELEPHONE NU'4BER Cl 7/81 01 LP 122C-4 DELETED CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATICN AND PARTICULATES ALTERNATE MEANS EP 131C-I NOTIFICATIONS CXt 7/83 C2 CP 1320-1 AUGMENTATION CF PLANT STAFFING CS 7/83 02 OELETED C2 7/82 02 LP LJ3C-1 C2 7/82 C3 iP 1330-2 DELETED DELETED C3 7/82 03 P 1330-3 DELETED C2 7/d2 03

P

. L330-4

'. P L330-5 POST-ACCIDENT NOSLE GAS RELEASE RATE CO ll/SC 03 DETERMINATION DELETED Cl 7/81 03

P 1330-0 C2 7/82 02

.P 1330-7 DELETED

.P L330-8 SAMPLING LIQUID PROCESS MONITCRS Cl 8/82 G3 CURIr.G LIGul0 MCNITOR HIGH RADIATION ALARM CCNDITIONS C1 1/82 03 P 1330-10 DELETED P 1330-11 DILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 POST-ACCIDENT ANALYSIS OF dARCN CO 3/81 03 j

P L330-20 (BACKUP PROCECURE)

POST-ACCICENT ANALYSIS OF CHLORIDE 03 o/82 03 P 1330-21 CALIBRATICN OF THE MODEL IC OIONEX C2 4/82 03 P 1330-22 ICN CHPCMATCCRA."H DETERMINATICN OF REACTOR COCLANT PH, C2 e/82 03 3 133C-23 CONOUCTIVITY AND DISSCLVED OXYGEN CONCENTRATION AT THE HIGH RAOIATICN l SAMPLE SYSTEM l.

OETERMINATION OF REACTJR COOLANT C2 1/B3 03 P L33C-24 HYORCGEN AND CFF-GAS CJuCENTRATIONS AT l THd HIGH RA01ATION SAM 0 LING SYSTE.*

L

LZP-1330-20 Aevision 1 July Zo, 1963 1

POST-ACCICENT ANALYSIS OF 30 ROM (dackup Procedure )

A. PgRP01E Tne purpose of this procedure i s to celineate an alternate metnod for determining ooron following a Regulatury Guice 1 3 or 1.4 release of fission proaucts. The metnod described by this procedure is referenced to as the 1

- Curcumin Spectropnotometric Metnoo.

8. RjfgR{NCgS

1. Final Report, Analyses for Dissolvec Hycrogen, Dissolved Oxygen, doron, Cnloride, pH, anc conductivity !

under normal Post-Accicent Conditions, NUS Corporation, Octocer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-o, " Operation of the Klett-Summerson Colorimeter".

C. PREREQUISITES

1. Equipment:

a. Klett-Summerson Color imeter.

o. Filter No. 54.

c. 20 mm X 40 mm cells.

c. Gracuated cylinders, 10 or 25 ml ana 500 ml.

e. Volumetric flasks. 25 m1, 100 ml anc 1000 ml.

f. Evaporating disnes. 10C to 150 ml capacity, Vycor glass (Corning gl ass), or equivalent (used for beron aatermination cniy).

g. Oxford pipettes witn disposable plastic tips, 1 m1, 4 m1, 5 m1, 15 ml, 20 m1, ana 5 ml Mohr l pipette, or equ i val ent .

i l

h. Beakers 250 ml or 400 ml, wide fors.

LZP-1330-20 Revision 1 July 26, 1983 2

i. Tongs, long reacn.

j.

Pol yethylene sti rring rods, 7.

k. Medicine droppers, 7.

1. Fil ter paper, knatman 140. 30, cr equivalent.

m. Glass cr plastic funnel.

n. Semi-legarithmic paper, cual cycle.

o. Water oath, set at 55 + 2 C, in an operating fume nood.

2. Reagents:

a. 95% Isopropyl al cohol .

o. Curcumin reagent.

c. Boron stock stancaro solution, 100C ppm coron.

d. Boron stancaro solutions, 0.5 ppm, 1.0 ppm, 1.5 ppm, and 2.0 ppm.

C. P33 CAUTIONS

1. A Regulatory Guide 1.3 or 14 release of fission products implies extremely hign levels cf radioactivity. Oose rates may De nigh enougn to prevent entry into many areas of tne plant that are normally haoitaole. Rad /Cnem Supervisicn snoulc ce contacted prior to entry into any area unen such a release of fission products is suspectec.

2. wear radiation dosimetry as recommended oy Rad /Cnem Supervision.

3. Wear protective clothing and respiratory protection as recommenced oy Rad / Chem Supervision.

4. Handle the sample container with long reacn tongs.

Oose rates frcm a 5 mi sample could range up to 50 R/nr.

l

5. Appropriate survey instruments snould oe availaole for monitoring during tna processing anc analysis of this sample.

l

LZP-1330-ZC Revision 1 Jul f Zo, 19d3 3

6. Carry out all analytical operations cenino acequate shielding in an operating fume nood.

7. Se certain any spills are wiped up imreciately anc properly disposed of.

8. The same geometry evaporating oisnes must ce useo for all standards and so.nples to assure tnat evaporative rates are egaivalent.

9. T-he temperature of the oath must be controlled so that all samples dry at the same rata.

10. The curcumin reagent must ce stored under ref ri geration after preparation and not oa more tnan tnree days old.

11. Tests show that many variaoles can af fect the color development in this procacure. To minimize enese effects, the precedure includes processing stancara boron solutions along with the samples.

E. (1MITATIONS AND ACTIONS

1. The diluted reactor water sample shoul d centain between 0.5 and 2 ppm ooron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procedure may also De used for boren dnalysis unoer normal conaitions. If so, treat tne sample in accordance witn practicas for routine reactor water.

F. PigCjpuRj

1. Clean the immediate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfeces, the f il ter , and tne cells. Tre outsiae surface of the cells must ce free of dirt, fingerprints, and scratenes.

LLP-1330-20 Revision 1 July Zo, 1983 4

4. Pipette 1.0 ml of DOI water (bl ank ) and 1.0 al or the 0 5, 1.C. 1 5 and 2.0 ppm coron stancaros inte separate laoeled evaporating cisnes.

5. Pipette 1.0 ml of the alluted sample solution into two separate evaporating cisnes for duplicate analyses.

CAUTIO1 Carry out all anal yt i cal operations cenino acequate shielaing in an operating fume nooa.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl tne contents gently to mix, using Icng tongs to nandl e the two racicactive samples.

7. Place each evaporating dish on the cottom of tne 250 or 400 ml wice-form Deakers, using long tongs to hanole the radioactive samgles. Float the Deaners in a water catn set at 55 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness and note the time of dryness for each sample.

9. Remove tne evaporating oisnes from tne catn at 15 minutes after the contents appear cry and allow tnem to cool to room temperature.

f 10. Add approximately 10 ml of 95 percent isopropyl l

alconol to eacn evaporating disn. Use a polyetnylene i stirring rod to aia in aissolution of the rea-colored l

reaction procuct and oxalic acid.

l

11. Using a medicine orcpper, transfer the contents of the evaporating cishes to individual 25 mi v ol une t r ic flasks =nich have esen praviousl y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent al cohol and aad the contents to tne flasxs. Cilute the contents of eacn flask to 25,0 ml using 45 percent isopropyl alcohol.

13. Zero the Klett-Summerson Colorimeter witn deionized water in accordance with Reference 3.

. l

, 1 L4P-1330-20 l Revision 1 July Zo. 19d3

14. within one hour of cissolution of the dried procuct (stop F.d.), pour the "olanx" into tne cell and measure the absorbance. Record the reading on LRC From 1088 (Attachment A).

CAUTION The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accorcar.ca with guidances provided oy Rad / Chem Supervision.

U21.E If dose levels warrant, une Klett-Summerscn shoul o ce put in the fume hood oenino the snielding witn appropriate precautions taken to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion or one of tne samples, then pour the sample into tne cell and measure the aosoroance. Recora tne reading on LRC Form 1088 (Attachment A).

h2LE If a solution appears toroic, filter enrough a cry fil ter paper ai rectl y inte a clean ary cell.

16. Empty and rinse the cell with a small pcrtion of the duplicate sample, tnen pour that sarple into tha cell and measure tne aosoroance. Reccro tne reaaing on LRC From IC88 (Attachment A).

17. Empty and rinse the cell with a small pcrtion of the 0.5 ppm Doron standard, then pour tre stancara into the cell and measare the aosoroance. Record the reauing on LRC Form 1038 (Attachment A). Repeat for each of the remaining stancards; 1.C. 1.5 ano 2.0 ppm coron.

18. Subtract the " blank" from each of the measured samples and standards aDsoroances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for tne standards on the log axis of dual cycl e semilogaritnaic graan paper against concentration (linear axis), refer to Attachment 8. Draw the oest fit straight line thrcugh the cata points.

LLP-1330-20 Revision 1 July 26..i963 e

20. Determine the ppm coron in each sample from the callDration curve. Record tne value cn LRC Form 10B8 (Attacnment A).

21. Calculate the average ocron concentraticn for tha duplicate samples in accordance with LRC Form 10d8 (Attacnment A).

22. Multiply tne average boron concentration oy the sample dilution factor to determina the sample Doron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontami nate tne Klett-Sumrersen Col or imeter and cells as necessary.

24. Ensure tne sampling containers and liquid samples have been properly disposed of in accorcance witn instructions provided oy Rad /Che.n Supervi sion.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. [HECRLIGTS

1. None.

H. J,$ NNICAL SPE M Q UCN R EFggi

1. None.

LZP 1330-20 Revision 1 ATTACHMDC A July 26,1983 IASALLE COUNTY STATION Post-Accident Analysis of Boron Date:

Absorbance Concentration from Absorbance-Binnie Calibraei m curfe Measurement l

MT Antr Sample 1 Sample 2 0.5 pom Standard 1.0 one Standard 1.5 ppe Standard 2.0 com sesnaard Ave. boren conc., ppm = Conc. sample #1 + Conc. sample #2 2

.t l

t 1

i i

f Sample baron conc., ppa = (Ave. baron conc., ppm) x Dilution Factor (DF) l i

ATTACHMENT 3 L2P-1330-20

. . i

, . .* M i to July 26, 19BJt5 (Final) ,

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.: 0.5 0.75 1.0 1.25 1.5 1.75 2.0 Baron Concentration, ppa

<_ .. _. -.._ _ _ .._.. _ ____.__ _ _ .-_. _. ~. _ _. _ _ . _ . _ _ _.-.. _ _ _ _ _ _ . _ _ _ __ _ _ _ __ _ .

LZP INDEx PAGE -

7/C6/83 8 ROC. NO. TITLE RE/. REV GATE CISKETT-CLASSIFICATION CF A LIOUIC RELEASE C1 3/32 01

P

. 1200-4 HAZAR0CUS MATERIAL INCIDENTS REPORTI'4G C2 3/63 01

P 121C-1 Cl 5/81 01

P 1220-1 EMERGENCY TELEPHONE NUMBER DELETED C1 7/81 01

'. P 1220-4 CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATION AND PARTICULATES ALTERNATE MEANS

.P 131C-1 F40TIFIC A TIONS Oc{- 7/83 C2

.P 1320-1 AUGMENTATION CF PLANT STAFFING CS g/83 02

.P 133C-1 DELETED C2 7/82 02 P 1330-2 DELETED

~

C2 7/82 03 P 133C-3 OELETED 03 7/82 03 P 1330-4 OELETED C2 7/d2 C3 P L330-5 PCST-ACCIDENT NO3LE GAS RELEASE RATE CO 11/SC 03 DETERMINATION P 1330-6 DELETED 01 7/81 03 P 1330-7 OELETED C2 7/82 02 P 1330-8 SAMPLING LIQUID PROCESS MONITCRS Cl 8/82 03 CURING LICUID MCNITOR HIGH RADIATION ALARM CCNDITIONS P 133C-10 DELETED 01 1/82 03 P 153C-11 DILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 3 1330-20 POST-ACCIDENT ANALYSIS OF dARCN CO 3/81 03

[ (BACKUP PROCECURE)

) 1330-21 POST-ACCICENT ANALYSIS OF CHLCRIDE 03 c/82 03 2 1330-22 CALIBRATIGN OF THE MODEL 10 OIONEX C2 4/82 03

! ICN C:!ROMATOGR apt!

133C-23 DETERMINATICN OF REACTOR COOLANT PH, 02 6/82 03 cot 40UCTIVITY AND DISSCLVED 0xYGEN CCNCENTRATICN AT THE HIGH RAOIATION SAMPLE SYSTEM 2

1330-2* OETERMINATICN OF REACTJR COOLANT C2 1/63 03 nYORCGEN ANO CFF-GAS CJs4CENTRATIONS AT l

THE HIGH PADIATION SAMoLING SYSTEM L

LZP-1330-20 Aevision 1 l July 2o, 19o3 i i

POST-ACCIDENT ANALYSIS OF SORON (Backup P roce du re )

A. PURP01E The purpose of this procedure i s to celineate an alternate metnod for cetermining Doron following a Regulatory Guice 1.3 or 1.4 release of fission procucts. The metnod described by this procedure is referenced to as tne Curcumin Spectropnotometric Metnoa.

8. REFERENCES

1. Final Report, Analyses for Dissolved Hycrogen, Dissolved Oxygen, Boron, Cnloride, pH, anc conductivity under normal Post-Accident Conditions, huS Corporation, OctoDer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Summerson Colorimeter".

C. PREREQUISITES

1. Equipment:

a. Klett-Summerson Color imeter.

o. Filter No. 54.

c. 20 mm X 40 mm cell s.

c. Graouatec cylinders, 10 or 25 ml and 500 ml.

e. Volumetric flasks, 25 ml, 100 ml ano 1000 ml.

i

f. Evaporating disnes, 10C to 150 ml capacity, Vycor glass (Corning gl ass), or equivalent (used f or boron aetermination cnl y) .

g. Oxford pipettes witn disposable plastic tips, 1 ml, 4 ml, 5 ml, 15 ml, 20 ml, ana 5 ml .Mohr pipatta. nr aqu i val ent .

h. Beakers 250 ml or 400 ml, wide form.

i I

LZP-1330-20 Ravision 1 Jul f 2o. 1983 2

i. Tongs, long reacn.

j. Pol yethyl ene st i rr i ng rods, 7.

k. Medicine droppers, 7.

1. Filter paper, knatman too. 30, or equivalent.

m. Glass cr plastic funnel.

n. Semi-legarithmic paper, cual cycle.

o. Water bath, set at 55 + 2 C, in an operating fume nood.

2. Reagents:

a. 95% Isopropyl alcohol.

D. Curcumin reagent.

c. Boron stock stancaro solution, 100C ppm coron.

d. Boron stancarc solutions, 0.5 ppm, 1 0 ppm,

. 1.5 ppe, and 2.0 ppin.

c. paggagI1gus

1. A R0gulatory Guice 1.3 or 14 release of fission products implies extremely hign levels ci radioactivity. Oose rates may be nigh enougn to prevent entry into many areas of sne plant tnat are normally haoitaole. Rac/Cnem Supervisicn snoulc ce contacted prior to entry into any area anen such a release of fission products is suspectec.

2. wear radiation cosimetry as recommended oy Rac/ Chem Supervision.

3. Wear protective clothing and respiratory protection as recommenced by Rad / Chem Supervision.

4. Handle the sample container with long reacn tongs.

Ocss ratas frc.. a 5 r.1 sampla could ranga up to 30 R/nr.

5. Appropriate survey instruments snould os availaole f or moni toring curing ena processing anc anal ysi s of this sample.

i

-- _ ____ ____ __d

l LZP-133C-ZC Aavision 1 aul f 26 1983 3

6. Carry out all analytical operations cenino acequate shielding in an operating fume hood.

7. Se certain any spills ara nipea up imeeciately anc properly disposed of.

8. The same geometry evaporating oisnes must ce usea for all stanaards ano so.nples to assure tnat evaporative rates are agalvalent.

9. The temperature of the cath must be controlled so that all samples dry at the same rata.

10. The curcumin reagent must ce stored under ref ri geration after preparation and not ce more unan tnree days old.

11. Tests show that many yariaol es can af f ect the color development in this procecure. To minimize enese effects, the precedure includes processing stancard boron solutions along with the samples.

E. W HA_TIONS AND ACTIONS

1. The diluted reactor watGr sampl e snoul d CCntain between 0.5 and 2 ppm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procedure may also oe used for Doren enalysis unoer normal conoitions. If so, treat tne sampla in accordance witn practicas for routine reactor nater.

F. PROCEDURE

1. Clean the immediate worn area.

2. Inspect the laoware and clean if necessary using approved cleaning techniaues.

3. Clean the Klett-Summerson Colorimeter optical surfaces, the fil ter , ano tne cells. The outsice surface of tne cells must be free of dirt, fingerprints, anc scratenes.

l l

i I

LZP-1430-2C Revision 1 July 2o, 1963 s

4. Pipette 1.0 ml of DDI sater (Diank) and 1.0 ml or the 0.5, 1.0, 1.5 and 2.0 ppm coron stancaras inte separate laoeled evaporating aisnes.

S. Pipette 1.0 ml of the diluted sample solution into two separate evaporating dishes for auplicate analyses.

CAUTIDI Carry out all anal yt i cal operations oenind adequate shieloing in an operating fume nood.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl the contents gentl y to mi x, using Icng tongs to nandl e tne two radicactive samples.

7. Pl ace each evaporating dish on tne cottom of tne 250 or 400 ml wide-form Deakers, using long tongs to nanole the racioactive samgles. Float tne oeaners in a water natn set at 55 1 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness and note tne time of dryness for each sample.

9. Remove tne evaporating oisnes from tne catn at 15 minutes after the contents appear dry and allow enem to, cool to room temperatare.

10. Aca approximately 10 ml of 95 percent isoprcpyl alcohol to eacn evaporating cisn. Use a polyetnylena stirring rod to aio in dissolution of the reo-colored reaction proauct and oxalic acid.

11. Using a medicine cropper, transfer the contents of the evaporating dishes to individual 25 ml v ol o ne t r ic '

j flasks wnich have been prsviousi y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent al cohol ano aad the contents to tne flasxs. Cilute tha contents of each flask to 25.C ml using 45 percent l

Isooropyl al cohol .

l

13. Zero tne Klett-Summerson Colorimeter witn deionizea water in accordance aitn Reference 3.

t

LZP-1330-20 Ravision i July 20, 19d3

14. within one hour of oissolution of the dried proouct (step F.8.), pour the "olank" into tne cell ana measure the absorbance. Recora tne reacing on LRC From 1088 (Attacnment A).

2!11123 The waste from steps F.15.-F.17. contains radionuclides; cispose of this waste in accorcance with guidances provided oy Rac/ Chem Supervision.

F.SI.E If cose levels warrant, tne Kl att-Summerscn shoula ce put in the fume hood oenino the snieloing witn appropriate precautions taxen to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour the sample into tne cell and measure the aosoroance. Recorc sne reading on LRC Form IC88 ( Attachiaent A).

h2If If a solution appears turoic, filtar enrough a cry fil ter paper ai rectl y intc a clean cry cell.

16. Empty and rinse the cell with a small ocrtion of the duplicate sample, tnen pour that sanple into tha cell ano measure tne aosoroance. Recorc tne reading on LRC From 1C38 (Attachment A).

17. Empty and rinse the cell with a small pcrtion of the 0.5 ppm Doron standaro, then pour the stancara into tne cell and measare the aosoroance. Record the reading on LRC Form 1088 (Attachment A). Repeat for each of the remaining stancarcs; 1.C. 1.5 ano 2.0 ppm coron.

18. Subtract the " blank" from each of the measured samples and stancards aosorbances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for the standards on the log axis of dual cycl e semilogari thnic graph paper against concentration (linear axis), rarer to Attachment 8. Draw the oest fit straight line through the cata points.

i LZP-1330-2C Revision 1 July 26. 1983 o

20. Determine the ppm coron in each sample from tne calioration curve. Record the value en LRC Form 1088 (Attachment A).

21. Calculate the average ooron concentraticn for the duplicate samples in accordance with LRC Form 10da (Attachment A).

22. Multiply tne average boron concentration by tne sample oilution f actor to determine the sample Doron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontami nate tna Klett-Sumra rsen Col or imeter and cells as necessary.

24. Ensure the sampling containers and liauld samples have been properly disposed of in accorcance witn instructions provideo oy Rad / Chem Supervision.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. CHECKLISTS

1. None.

H. M g ICAl S P EC IFIQLi,0N REFg g g }

1. None.

l

LZP 1330-20 Revision 1 ATTACHMENT A July 26,1933 IASALLE COUNTY STATION Post-Accident Analysis of Boron Date:

. Absorbance Concentration from .

Measuremane Absorbance-? T ,nte Calibration cume R7 AN1r Sample 1 Sample 2 0.5 pom Standard 1.0 com Standard l

L.5 ppm Standard 2.0 com standard Ave. boron conc. , ppa = Conc. sample #1 + Conc. sample #2 2

Sample boron conc., ppa = (Ave. borou conc., ppm) x Dilution Factor (DF) l

-.- . . , - - - . . - ..n.~.~ . . . - . _ . _ . , . .- . _ ~ . _ - ~ . . - .- - . _ , . - - . . . . _ - c.-- ~ , . - - .

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l ATTACIDfENT 3 LZP-1330-20

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l

l' LZP INDEX JaGe f 7/08/d3 1

[ ROC. No. TITLE RE/. AEv OATE CISKETT Pc 1200-4 CLASSIFICATION CF A LIQUIC RELEASE C1 3/82 01 HAZAROCUS MATERIAL INCICENTS R E P OR T I '4G C2 3/o3 01 P' 121C-1 EMERGENCY TELEPHONE NUMBER CL 5/81 01 9 1220-1 OELETED Cl 7/81 01 3

9 -1220-4 CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATION AND PARTICULATES ALTERNATE MEANS P L31C-1 NOTIFICATIONS C4 7/33 C2 9 L320-1 AUGMENTATION CF PLANT STAFFING CE 7 /83 02 1330-1 OELETED C2 7/82 02 P

P 1330-2 DELETED C2 7/82 C3 P 1330-3 DELETED C3 7/82 03 l 'P 1330 .4 OELETED C2 7/82 C3 P 1330-S POST-ACCIDENT NO3LE GAS RELEASE RATE CO Ll/SC 03 0F.rERMINATION 3 1330-e OELETED Cl 7/81 03

) 1330-7 OELETED C2 7/82 02 2 1330-8 SAMPLING LICUID PROCESS MONITCRS Cl 8/82 03 l

OURING LIQUID "CNITOR HIGH RACIATION

! ALARM CCNOITIONS 2 1330-10 DELETED G1 L/82 03 8- OILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 f _133C-11 8

L330-20 POST-ACCIDENT ANALYSIS OF BARCN CO 3/81 03 (BACKUP PROCECURE) 7

1330-21 POST-ACCICENT ANALYSIS OF CHLORIDE 03 6/82 03 1330-22 1CALIBRATICN OF THE MODEL 10 DIONEX C2 4/82 03-s ICM CHROMAT00RAPH i 1330-23 OETERMINATICN OF REACTOR COOLANT PH, 02 6/82 03

,.a s Coh0UCTIVITY ANO DISSOLVED CAYGEN CCNCENTRATION AT THE HIGH RADIATION SAMPLE SYSTEM C2 1/d3 03 1330-2[ ,

, CETERMINATICN OF REACTJR COOLANT HYJRCGEN AND CFF-GAS-CJi4CENTRATIONS AT THE HIGH RAOIATION SAM 3 LING SYSTE.*

s

=

l LZP-1330-20 Avvision 1 July 2o, 19d3 i

POST-ACCICCNT ANAlfSLS OF SORCN (dackup Procedure)

A. EMEE925 ,

The purpose of this procedure ;i s to delineate an alternate metnod for determining coron following a Regulatory Guide 1.3 or L.4 release of fission prooucts. The .netnod described by this procecure is referencsd to as the Curcumin Spectropnotometric Methoo.

8. R E_F E R E'NC E S

1. Final Report, Analyses for Dissolved Hycrogen, Dissolved Oxygen, Boren, Cnloride, pH, ano conductivity under normal Post-Accident Conditions, huS Corporation, Octonor, 1980.

Z. LCP.110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Suminerson Colorimeter".

C. 333350VISITES L. Ecolpment:

a. Kle tt-Summer son Color imeter.

o. Filtor No. 54. ,

c. 20 mm X 40 mm cells.

c. Graduated cylinders, 10 or 25 ml and 500 ml.

e. Volumetric flasks, 25 ml, 100 ml ano 1000 ml.

f. Evaporating disnes, 100 to 150 ml capacity, Vycor glass (Corning gl ass), or equivalent (used for boron catermination cnly).

g. Oxford pipettes witn disposable plastic tips, o s 1 mi, 4 m1, 5 m1, 15 m1, 20 m1, ano 5 ml Mohr

, pipatte. nr aqu i val ent.

, h. Beakers 250 ml or 400 m1, wide form.

/4

LLP-1330-20 Revision 1 July 26, 1983 2

i. Tongs, long reacn.

J. Pol yethyl ene sti rr i ng roos, 7.

k. Medicine droppers, 7.

1. Fil ter paper, Wnatman t4o. 30, cr equi val ent.

m. Glass cr plastic funnel.

n. Semi-1cgarithmic paper, cual cycle.

o. Water bath, set at 55 + 2 C, in an operating fume nood.

2. Reagents:

a. 95% Isopropyl al conol .

o. Curcumin reagent.

c. Boron stock stancaro solution, 100C ppm Doron.

d. Boron stancarc solutions, 0.5 ppm, 1 0 ppm, 1.5 ppm, and 2.0 ppia.

c. gagq3u;1ggs

1. A Regulatory Guide 1.3 or 1.4 release of fission products implies extre.nely hign levels ci radioactivity. Oose rates may be nign enougn to prevent entry into many areas of tne plant that are normally haoitable. Rad /Cnem Supervisicn snoulc ce contacted prior to entry into any araa wnen sucn a release of fission products is sospc # -

2. wear raciation dosimetry as recommende.. ay Rad /Cnem Supervision.

3. Wear protective clothing and respiratory protection as recommenced oy Rad / Chem Supervision.

4. Handle the sample container witn long reacn tongs.

Oose rates frcm a 5 mi sa ple could rangs up to 5C R/nr.

5. Appropriate survey instruments snould oe availaole l

for monitoring during sna processing anc anal ysi s i of this sample.

l

i L4P-133C-ZC Revision 1 Jui f 2o, 1963 3

6. Carry out all analytical operations cenino acequate shielding in an operating fume hood.

7. Se certain any spills are nipsa up imrediately ano properly disposed of.

8. The same geometry evaporating alsnes must ce used for all standards and sa.nples to assure that evaporative rates are agalvalent.

9. The temperature of the Dath must be controlled so that all samples dry at tne same rate.

10. The curcumin reagent must ce stored under ref ri geration after preparation and not ce more tnan tnree days old.

11. Tests show that many vari aol es can af f ect the color development in this procecure. To minimize snese effects, tne precedure includes processing stanuara Doron solutions along wi tn the samples.

E. g g 4 TION $ _AND Ag g 1 The diluted reactor water sample shoula contain bet een 0.5 and 2 ppm coron.

2. The total analysis time for this procedure i s aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. Th'is procedure may also oe usea for boren analysis unoer normal conaitions. If so, creat the sample in accordance witn practices for routine reactor nacer.

F. PQ0(g0yRj

1. Clean the immediate werk area.

2. Inspect the laoware and clean if necessary usin_

approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfaces, tne filter, ano tne cells. The outsioe surface of the cells must De free of dirt,

' fingerprints, and scratenes.

t l

I i

I l

l L2P-1330-2C Revision 1 Jul y Zoe 1963 4

4. Pipette 1.0 ml of 001 water (clank) and 1 0 ml or the 0.5, 1.C. 1 5 and 2.0 ppm coron stanaards inte separate laoeled evaporating aisnes.

5. Pipette 1.0 ml of the alluted sample solution into two separate evaporating alsnes for cuplicate analyses.

CAUTIOJ Carry out all anal yt i cal operations oenind adequate shieloing in an operating fume noco.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl the contents gently to .n i x ,

using 1cng tongs to handl e the two radicactive samples. -

7. Place each evaporating dish on the cottom of tne 250 or 400 m1 wide-form oeakers, using long tongs to nanole the rad'ioactive samples. Float the osaxers in a water catn set at 55 1 2 C. -

8. Evaporate the contents of eacn evaporating disn to complete dryness and note the time of dryness for each sample.

9. Remove tne evaporating oisnes from tne batn at 15 minutes after the contents appear cry and allo tnam to cool to room temperature.

10. Acc approximately 10 ml of 95 oercent isoprcpyl alcohol to eacn evaporating aisn. Use a polyennylene stirring rod to aic in aissolution of the rea-colored reaction proauct and oxalic acid.

11. Using a medicine arcoper, transfer tne contents of the evaporating cishes to individual 25 ml volonetric flasks which have Dean previousi y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent al cohol and add the contents to tne flasxs. Ci;ste the c.nntants of aach flask to 25.C ml using 9.' percent isopropyl alcohol.

13. Zero tne Klett-Summerson Colorimeter witn deionizeo water in accordance witn Reference 3.

I

LZP-1330-20 Ravision 1 July 2e, 19d3

14. within one hour of dissolution of the dried proouct (step F.8.), pour the "olank" into tne cell and measure the absorbance. Record the reaoing on LRC From 1088 (Attachment A).

C AtJT T01 The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accorcance with guidances provided oy Rad / Chem Supervision.

Nplj If cose levels warrant, the Klatt-Summerscn shoulc ne put in the fume hood oeninc the shieloing witn appropriate precautions ta<en to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour the sample into tne cell and measure the aosorbance. Racora tne reading on LRC Form ICB8 (Attachment A).

h215 If a solution appears turoic, filter enrough a cry filter paper airectly inte a clean cry cell.

16. Empty and rinse the cell witn a small pcrtion of the duplicate sample, tnen pour that sarple into the cell and measure tne aosoroance. Recora tne reaoing on LRC From IC88 (Attachment A).

17. Empty and rinse the cell witn a small pcrtion of the 0.5 ppm coron standard, then pour tre standaro into the cell and measure the aosoroance. Record the reading on LRC Form 1C88 (Attachment A). Repeat for each of the remaining stancards; 1.C, 1.5 ano 2.0 ppm coron.

18. Subtract the " blank" from each of ne measured I samples and stancards aosorbances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoraance for the standards on the log axis of dual cycl e semilogarithric graph paper against concentration (linear axis), r e f e 'r to Attachment 8. Draw the oest fit straignt line enrough the cata points.

1 LZP-1330-2C Revision 1 July 26. 19e3 l o

20. Determine the ppm Doron in each sample frcm tha calloration curve. Record tne value on LRC Form 1088 (Attacnment A).

21. Calculate the average ooron concentraticn for the duplicate samples in accordance with LRC Form lOdd (Attacnment A).

22. Mul t i pl y tne average coron concentration by tne sample dilution factor to determine the sample coron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontaminate tha Alett-Sumnarson Col or imeter and cells as necessary.

24. Ensure the sampling containers and liquid samples have been properly disposed of in accorcance witn instructions provided oy Rad / Chem Supervision.

25. Survey the work area for radioactive contaminacion and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. {HECKt.ISTS

1. None.

H. H{ DICAL SPE M Q ]CN Rgggg}

L. Hone.

i

LZP 1330-20 Revision 1 ATTACHMENT A July 26, 1983 LASALLE COUNTY STATION Post-Accident Analysis of Boron Date:

Absorbance Concentration from

~

Measuremane Absorb anc e-B hnle Calibraelen cu- re .

MTAMF Sample 1 Sample 2

~

0.5 ppa Standard 1.0 paa Standard -

1.5 ppe Standard N

2.0 nom semnamed Ave, baron conc. , ppe = Conc. sample fil + Conc. sample #2 2

Sample baron conc., ppa = (Ave. borou conc., ppm) x Dilution Factor (DF) l l

l l

i w-

, ._ _ . _ _ - . _ _ . ~ . - - - - . - - _ _ _ . . - - . . - _ . . - - - - .-_ _ _ - - - - . . . _. - . - . - . . . . -.--

1 i

f . . _ . . . _ .

l ATTAC11 MENT 3 L2P-1330-2,0 .

,. .- m 4

July 26,198)in j (Final)

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= i:-1 e w - - - - . - - :==:

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t 0.3 0.75 1.0 1.25 1.5 1.75 2.0 Boron Concentration, ppa

LZP INDEX 0466 7/C6/d3 840C. NO. TITLE RE/. REV 0 ATE CISKETT'

.P 120C-4 CLASSIFICATION CF A LI'JUIC RELE ASE C1 5/82 01

.P 121C-1 HAZAR00US MATERIAL INCIDENTS REPORTI1G C2 3/o3 01 9 1220-1 EMERGENCY TELEPHONE NUMBER C1 5/81 01 P 1220-4 DELETED Cl 7/81 01 CONTAINMENT ATMOSPHERE FOR RACI0t0INES DETERMINATICN AND PARTICULATES ALTERNATE MEANS P 131C-1 NOTIFICATIONS CFt 7/93 C2 P 1320-1 AUGMENTATION CF PLANT STAFFING CS 7/83 02 P 1330-1 DELETED C2 7/82 02 P 1330-2 OELETEG C2 7/82 G3 P 1330-3 OELETED C3 7/82 03

? 1330-4 DELETED C2 7/d2 C3 P 1330-5 POST-ACCIDENT NO3LE GAS RELEASE RATE CO 11/SC 03 DETERMINATION 2 1330-6 DELETED 01 7/81 03 2 1330-7 OELETED C2 7/82 02

) 1330-8 SAMPLING LICUID PROCESS MONITCRS C1 S/82 03 OURING LIQUID MCNITOR HIGH RADIATION ALARM CCNDITIONS 1330-10 DELETED C1 1/82 03 8

133C-11 OILUTION AND TRANSFER OF GAS SAMPLES CC 11/81 03 8

1330-20 POST-ACCIDENT ANALYSIS OF BARCN CO 3/S1 03 (BACKUP PROCECURE) 1330-21 POST-ACCICENT ANALYSIS OF CHLORIDE C3 o/82 03 1330-22 CALIBRATICN OF THE MCOEL 10 OIONEX C2 4/82 03 ICM CHRCMATCCRAPH 133C-23 DETERMINATICN OF REACTOR COOLANT PH, C2 $/d2 03 CONOUCTIVITY AND DISSCLVED OXYGEN CCNCENTR ATION AT THE HIGH RADIATION SAMPLE SYSTEM 1330-2* DETERMINATICN OF R2 ACTJR C'JCL ANT C2 1/d3 03 nYORCGEN AND CFF-GAS CJHCENTRATIONS AT THE HIGH RADIATION SAMoLING SYSTE.*

LZP-1330-20 Avvision 1 July 2o, 1963 1

POST-ACCICENT ANALYSIS OF SCRCN (dackup P roce dure )

A. Eggg013

~.

The purpose of this procedure is to delineate an alternate metnod for cetermining coron following a Regulatory Guide 1,3 or 1.4 release of fission proaucts. The .nethod described by this procedure is referenced to as tne Curcumin Spectropnotometric Motnoo.

8. RjfgR5_N SS

1. Final Report, Analyses for OisSolved Hycrogen, Di ssol veo Ox ygen, Boron, Cnlorice, pH, ano conductivity under normal Post-Accident Conditions, huS Corporation, Octooer, 1980.

2. LCP 110-2, "Preparatidn of Reagents".

3. LCP 210-6, " Operation of the Klett-Summerson Colorimeter".

C. PREREGUISTTES

1. Equipment:

a. Klett-Summerson Color imeter.

o. Filter No. 54.,

c. 20 mm X 40 mm cell s.

c. Graouatec cylinders, 10 or 25 ml anc S00 ml.

e. Volumetric flasks. 25 m1, 100 ml ana 1000 ml.

f. Evaporating disnes, LOC to 150 mi capacity, i

Vycor glass (Corning gl ass), or equival ent (used f or boron oetermination cnl y).

g. Oxford pipettes witn disposable plastic tips, 1 ml, 4 ml, 5 ml, 15 ml, 20 m1, ana 5 ml Mohr pipette, or equivelent.

n. Beakers 250 ml or 400 m1, wide form.

l l

[

t l

L2P-1330-20 Revision 1 Jul< 25. 1983 Z

i. Tongs, long reacn.

j. Polyethylene stirring rocs, 7.

k. Medicine droppers, 7.

1. Fliter paper, knatman No. 30, cr equivalent.

m. Glass cr plastic funno1.

n. Semi-logarithmic paper, cual cycle.

o. Water oath, set at 55 + 2 C, in an operating e fume hood.

2. Reagents:

a. 95% Isopropyl al conol .

o. Curcumin re6 gent.

c. Baron stock stancaro solution, 100C ppm coron.

d. Boron stancara solutions, 0.5 ppm, 1 0 ppm, 1.5 ppm, and 2.0 ppia.

O. PRECAUTIONS

1. A Regulatory Guide 1.3 or 1.4 release of fission products implies extremely hign levels cf ra'dioactivity. Oose rates may be nigh enougn to prevent entry into many areas of tne plant tnat are normally haoitaole. Rac/Cnem Suoervisicn snoulc ce contacted prior to entry into any area wnen sucn a release of fission products is suspectec.

2. Wear ractation cosimetry as recommended oy Rad /Cnem Supervision.

l 3. Wear protective clothing and respiratory protection as recommenced oy Rad / Chem Supervision.

4. Handle tne sample container witn long reacn tongs.

l Ooss ratas from a 5 mi sample could ranga up to 50

? R/nr.

l l S. Appropriata survey instruments snould os availaule

! for monitoring during tna processing anc analysis of this sample.

i l

l LZP-133C-ZC Aevision 1 J Jul / Zo, 19d3 3

6. Carry out all analytical operations oenino aceauate shielding in an operating fumo nood.

7. Se certain any spills ara nipsa up imreciately ano properly disposed of.

8. The same geometry etaporating aisnes must ce usea for all standards ano senples to assure that evaporative rates are equivalent.

9. The temperature of the Dath must be controlled so that all samples dry at tne same rate.

10. The curcumin reagent must oe stored under ref ri geration after preparation and not ce more enan tnree days ol d.

11. Tests show that many variaoles can af f ect the color development in this procacure. To mininize tnese effects, the procedure includes processing stancara boron solutions along with the samples.

E. g tTATIONS AND ACTgfj!S

1. The diluted reactor water sample snouid ccntain bet een 0.5 and 2 ppm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procedure may also oe used for coren analysis unaer normal conoitions. If so, treat tne sample in accordance witn practicas for routine reactor water.

F. PROCj0URg

1. Clean the immediate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfocus, the filter, and tne cells. Tne outssae surface of tne cells must De free of dirt, fingerprints, and scratenes.

LZP-1330-20 Revision 1 July 2oe 1983 4

4. Pipette 1.0 ml of 00I water (bl ank ) and 1.0 ml or the 0.5, 1.0, 1 5 and 2.0 ppm coron stancaras inte separate laoelea evaporating cisnes.

d. Pipette 1.0 ml of the ciluted sample solutisn into two separate evaporating cishes for duplicate analyses.

CAUTIO1 Carry out all anal yt i cal operations oenind adequate shieloing in an operating fume nood.

6. Pipette 4.0 ml of curcumi n reagent into each evaporating dish. Swirl the contents gently to mix, using long tongs to nandl e the two radicactive samples.

7. Place each evaporating dish dn the cottom of tne 250 or 400 ml wice-form oeakers, using long tongs to nanole the radioactive samgles. Fl oat tne osa'<ers in a water catn set at 55 + 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness and note the time of dryness for each sample.

9. Remove tne evaporating oisnes from the batn at 15 minutes after the contents appear dry and allow them to cool to room temperature.

10. Acc approximately 10 ml of 95 percent isoprcpyl alcohol to eacn evaporating cisn. Use a pol yetnyl ene stirring rod to aio in dissolution of the rec-colored reaction procuct and oxalic acid.

11. Using a medicine arcpper, transfer tne contents of the evaporating a i shes to i r.di v idual 25 mi voluretric l

l flasks wnich have Deen previousl y rinsec witn 95 percent alccnol.

12. Rinse the evaporating oisnes witn 95 percent al conal l

and add the contents to tne flas<s. Cilute the I contents of each flasw to 25.C ml using 95 percent l isopropyl alcohol.

I 13. Zero the Klett-Sunmerson Colorimeter witn ceionizac l water in accordanct with Asference 3.

i l

L2P-1330-20 Revision 1 July 2o. 19d3 J

14. Within one hour of cissolution of the dried proouct (step F.8.), pour the "olank" intc tne cell ano measure the absorbance. Record the reacing on LRC From 1088 (Attachment A).

CAUTTOM The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accoraance with guidances provicea oy Rad / Chem Supervision.

!!.Q.IE If cose levels warrant, tne Klatt-Summerscn shoulo oe put in the fume hood oenina the shielaing witn appropriate precautions tanen to prevent contan. .ation of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of tne samples, then pour the sample into tne cell and measure the aosoroance. Recorc tne reading on LRC Form 1088 (Attacnuent A).

U.97.E i

If a solution appears turoic, filter enrough a cry f il ter paper ai rectl y inte a clean cry cell.

16. Empty and rinse the cell witn a small ocrtion of the duplicate sample, tnen pour that sample into the cell and measure tne aosoroance. Recoro tne reading on LRC From 1088 (Attachment A).

17. Empty and rinse the cell witn a small pcrtion of the 0.5 ppm boron standard, then pour tre standara into the cell anc measdre the aosoroance. Record the reading on LRC Form 1C88 (Attachment A). Repeat for each of the remaining stancards; 1.C. 1.5 ano 2.0 ppm coron.

Id. Suotract the " blank" from each of the measured samples and stancaros aosoroances. Reccro tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoroance for tne standards on the log axis of dual cycle semilogarithnic graph paper against concentration (linear axis), refer to Attachment 8. Draw the oest fit straignt line through the cata points.

I i

LZP-1330-2C Revision 1 July 26. 1963 e

20. Determine the ppm coron in each sample from the calioration curve. Record the value on LRC Form 1088 (Attachment A).

21. Calculate the average ocron concentraticn for the duplicate samples in accordance with LRC Form 10d8 (Attacnment A).

22. Multipl y tne average boron concentration by the sample dilution factor to determine the sample Doron concentration. Refer to LRC Form 1088 (Attachment i

A).

23. Clean and decontaminate the Klett-Summersen Col or i mete r and cells as necessary.

24. Ensure the sampling containers and liquid samples have been properl y di sposed of in accorcance witn instructions provided oy Rad / Chem Supervi si on.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

]

26. Clean the work area and lauware as necessary.

J G. $HECKLTSTS

1. None.

l H. 13fC,nN IC A L S P EEL AIJ,0N REfdRQ M

^

1. None.

4

\

l

I l

i LZP 1330-20 Revision 1 ATTACHMENT A July 26, 1933 1ASALLE COUNTT STATION Post-Accident Analysis of Boron Date:

Absorbance Concentration from

^

Meesurement Absorbance-Bl ante Calibratien (%rve R1 AM1r Sample 1 Sample 2 0.5 993 Standard /

1.0 ppm Standard 1.5 ppm Standard 2.0 om standard Ave. boren conc., ppa = Conc sample #1 + Conc sample #2 2

Sample boron cone., ppa = (Ave. borou conc., ppm) x Dilution Factor (DF) l l

I l

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

i ATTACIDtENT B LZP-1330-20

' .1- ,

,, July 26, 19836 l

' 3 (Final) i e .__== _

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0.5 0.75 1.0 . 1.25 1.5 1.75 2.0 Boron Concentration, ppa

LZP INDEX PAGE 7/08/83 TITLE RE/. AEV QATE GISAETT

'_R OC . NO .

.P 1200-4 CLASSIFICATION CF A LIOUIG RELEASE C1 5/82 01 P 121C-1 HAZAROCUS MATERIAL INCIDENTS REPORTI4G C2 3/63 01 P 1220-1 EMERGENCY TELEPHONE NU'4BER C1 5/81 C1 C1 7/81 01 P 122C-4 DELETED CONTAINMENT ATMOSPHERE FOR RACICIDINES DETERMINATION AND PARTICULATES ALTERNATE MEANS P 13LC-1 NOTIFICATIONS Ott 7/83 C2 AUGMENTATION CF PLANT STAFFING CS 7 /83 02 P 1320-L C2 7/82 02 P 1330-1 OELETED P 1330-2 DELETED C2 7/82 C3 3 1330-3 OELETED C3 7/82 03

~

) 1330-4 DELETED C2 7/82 03 3 1330-5 POST-ACCICENT NO3LE GAS RELEASE RATE CO 11/SC 03 DETERMINATION 1330-6 DELETE 0 01 7/81 03

' 1330-7 OELETED C2 7/82 02 1330-8 SAMPLING LIQUID PROCESS MONITCRS C1 8/82 03 CURING LICul0 MCNITOR HIGH RACIATIdh ALARM CCNDITIONS 1330-1G DELETED C1 L/82 03 133C-ll DILUTION AND TRANSFER OF GAS SAMPLES CO 11/81 03 l

1330-20 POST-ACCIDENT AA-LYSIS OF dARCN CO 3/61 03 (b ACKUP PROCECUK:-)

1330-21 POST-ACCICENT ANALYSIS OF CHLORIDE 03 o/82 03 L330-22 CALIBRATICN OF THE MODEL 10 OIONEX C2 4/82 03

.. ... . .- . 0 G R A Ptt

.w.,

1330-23 DETERMINATICN OF REACTOR COOLANT PH, C2 6/82 03 CONOUCTIVITY AND DISSOLVE 0 OXYGEN CONCENTRATICN AT THE HIGH RADIATION.

SAMPLE SYSTEM 133C-2* OETERMINATICN OF REACTJR COOLANT C2 1/d3 03 HYORCGEN AND CFF-GAS CJi4CENTRATIONS AT THE HIGH RADIATION SAMDLING SYSTE.*

LZP-1330-20 Aevision 1 July 20, 19o3 1

POST-ACCIDENT ANALYSIS OF SORON (Sackup P roce dur e )

A* 3 MEES 15 The purpose of this procedure i s to delineats an alternate metnod for cetermining ooron following a Regulatory Guide 1 3 or 1.4 release of fission proaucts. The netnod described by this procecure is referenced to as the Curcumin Spectropnotometric Metnoo.

8. REFFRENCES

1. Final Report, Analyses for Olssolved Hycrogen, Dissolved Oxygen, Boron, Cnloride, pH, anc conductivit y under normal Pcst-Accident Conditions, NOS Corporation, Octooer, 1980.

2. LCP 110-2, " Preparation of Reagents".

3. LCP 210-6, " Operation of the Klett-Sum.nerson Colorimeter".

C. PRF4ECUISITES

1. Ecolpment:

a. Klett-Summerson Color imeter.

o. Filter No. 54

c. 20 mm X 40 mm cell s.

c. Graouated cylinders, 10 or 25 ml ara 500 ml.

e. Volumetric fl asks. 25 ml, 100 ml ano 1000 ml.

f. Evaporating disnes. 10C to 150 mi capacity, Vycor glass (Corning gl ass), or equivalent (used f or boron catermination cnl y) .

g. Oxford pipettes witn disposable plastic tips, 1 ml, 4 ml, 5 ml, 15 ml, 20 ml, ano 5 ml Mohr pipette, or aquivalent-

h. Beakers 250 ml or 400 m1, wide form.

_ o

__ _ =- . _. - . ...

4 l

LZP-1330-20 Revision 1 July 20.-1983 2

i. Tongs, long reacn.

J. Pol yethylene sti rring rods, 7.

k. Medicine droppers, 7.

1. Fil ter paper, wnatman r4o. 30, or equi val ent.

m. Glass cr plastic funnel.

n. Semi-legarithmic paper, dual cycle.

o. Water cath, set at 55 + 2 C, in an operating fume hood.

2. Reagents:

J

a. 95% Isopropyl alcohol.

o. Curcumin re6 gent.

c. Baron stock stancara solution, 100C ppm Doron.

d. Boron standard solutions, 0.5 ppm, 1 0 opm, 1.5 ppe, and 2.0 ppin.

c. g3,gepiteris

1. A Regulatory Guide 1.3 or 1 4 release of fission products implies extremely hign levels cf radioactivity. Ooss rates may be nigh enougn to prevent entry into ma6y areas of tne plant tna: are normally haoitaole. Rad /Cnem Supervisicn snoulc ce contacted prior to entry into any area mnen such a release of fission products is sospectec.

2. wear radiation dosimetry as recommended by Rad /Cnem Supervision.

3. Wear protective clothing and respiratory protection as recommenced oy Rad / Chem S.jpervision.

4. Handle the sample container with long reacn_ tongs.

Oose rates frcm a 5 mi sampla could ranga up tv 3G R/nr.

5. Appropriate survey i nstr uments snoul d oe availaule for monitoring during ena processing anc analysis of this sample.

LZP-1330-iC Aevision 1 Jul / Zo, 19d3 3

6. Carry out all analytical operations ceninc acecuate shielding in an operating fume nood.

7. Se certain any spills are nipea up imreciately anc properly disposed of.

8. The same geometry evaporating aisnes must ce usec for all standards and sa.nples to assure that evaporative rates aro equivalent.

9. The temperature of the Dath must be controlled so that all samples dry at the same rate.

10. The curcumin reagens must ce stored under refrigeration after preparation and not ce more than tnree days ol d.

11 Tests show that many variaoles can af f ect the color development in this procacure'. To minimize snese effects, the procedure includes processing stancara boron solutions along with the samples.

E. LIMITA_TIONS AND ACT1QNS

1. The diluted reactor water sample snould centain Det een 0.5 and 2 ppm coron.

2. The total analysis time for this procedure is aoout 120 minutes (2 hours2.314815e-5 days 5.555556e-4 hours 3.306878e-6 weeks 7.61e-7 months ).

3. This procecure may also oe used for ooren anal ysi s unoer normal conditions. If so, treat tne sample in accordance witn practicas for routine reactor water.

F. gggqjpyR3

1. Clean the immediate work area.

2. Inspect the laoware and clean if necessary using approved cleaning techniques.

3. Clean the Klett-Summerson Colorimeter optical surfaces, the fil ter , ano tne cell s. The outsiow surface of tne cells must De free of cirt, fingerprints, and scratenes.

LLP-133C-20 Revision 1 July 2e, 1983 4

4. Pipatte 1.0 ml of CDI water (blank) and 1 0 ml or the 0.5, 1.0. 1.5 ano 2.0 ppm ocron stancaras inte separate lacelea evaporating cisnes.

5. Pipette 1.0 ml of the alluted sample solution into two separate evaporating cisnes for cuplicate analyses.

CAUTIO1 Carry out all anal yt i cal operations oenino acequate shieloing in an operating fun.e noco.

6. Pipette 4.0 ml of curcumin reagent into each evaporating dish. Swirl tne contents gently to mix, using Icng tongs to nandl e the two radicactive samples.

7. Place each evaporating dish on the cottom of tne 250 or 400 ml wide-form oeakers, using long tongs to hancle the radioactive samgles. Float tne Deaners in a water Datn set at 55 1 2 C.

8. Evaporate the contents of each evaporating disn to complete dryness and note the time of dryness for each sample.

9. Remove t.ne evaporating aisnes from tne catn at 15 minutes after the contents appear dry and allow enem to cool to rocm temperature.

10. Acd approximately 10 ml of 95 percent isopropyl alcohol to eacn evaporating cisn. Use a polyetnylene stirring rod to ala in dissolution of tre rea-colored reaction product and oxalic acia.

11. Using a medicine arcpper, transfer the contents of tna evaporating dishes to individual 25 mi volonetric flasks which have Deen previousl y rinsec witn 95 percent alconol.

12. Rinse the evaporating cisnes witn 95 percent alcohol and add the contents to tne flasxs. Cilute the contents of eacn flasx to 25.C ml using 95 percent isopropyl alconol.

13. Zero the Klett-Sunmerson Col orimeter witn celoni zed water in accordance ith Reference 3.

-- -__-__-________-_______._________________.___.________J

LLP-1330-20 Revision 1 July 20, 19d3

14. within one hour of cissolution of the dried procuct (step F.8.), pour the aolank" into tne cell ana measure the absorbance. Record the reacing on LRC From 1088 (Attachment A).

EA!1110 The waste from steps F.15.-F.17. contains radionuclides; dispose of this waste in accorcance with guidances provided oy Rad / Chem Supervision.

M If dose levels warrant, tne Klett-Summerscn shoulo De put in the fume hoed oenino the snielding wi tn appropriate precautions taxen to prevent contamination of this instrument.

15. Empty and rinse the cell witn a small pcrtion of one of the samples, then pour the sample into tne cell and measure the aosoroance. Recorc tne reading on LRC Form 1C88 (Attachment A).

M If a solution appears turoid, filter tnrough a cry f il ter paper oi rectl y inte a clean ary cell.

10. Empty and rinse the cell witn a small pcrtion of the duplicate sample, tnen pour that sarple into the cell ano measure tne aosoroance. Recoro One reaaing on LRC From 1038 (AttaChnent A).

17. Empty and rinse ene cell witn a small acrtion of the 0.5 ppm Doron standard, then pour the standaro into the cell and measure the aosoroance. Record the reading on LRC Form 1088 (Attachment A). Repeat for each of the remaining stancaras; 1.C. 1.5 ano 2.0 ppm coron.

18. Subtract the " blank" from each of the measured samples and stancards aosorbances. Reccrd tne difference on LRC From 1088 (Attacnment A).

19. Plot the corrected aosoraance for tne standards on the log axis of dual cycl e semilogar i thn ic graph paper against concentration (linear axis), refer to Attachment 8. Draw the oest fit straignt line !

thrcugh the data points.

l l

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LLP-1330-2C Revision 1 July 26. 1983 l o

20. Determine the ppm coron in cach sample from the calloration curve. Record tne value cn LRC Form 1088 (Attachment A).

21. Calculate tne average acron concentraticn f or the cuplicate samples in accordance with LRC Form 1Gda (Attacnment A).

22. Multiply tne average baron concentration oy the sample cilution factor to cetermine the sample ooron concentration. Refer to LRC Form 1088 (Attachment A).

23. Clean and decontami nate the Klett-Sumre rscn Color imeter and cells as necessary.

24. Ensure tne sampling containers and liquid sampl e s have been properly oiscosed of in accoroance wi tn instructions provicea oy Rad / Chem Supervi sion.

25. Survey the work area for radioactive contamination and decontaminate as necessary.

26. Clean the work area and lauware as necessary.

G. $HECKLISTS

1. None.

H. TECnNICAL SPE @ Q UON R EFggy}

1. None.

e

LZP 1330-20 Revision 1 ATTACHMENT A July 26, 1933 IASALLE COUNTY STATION Post-Accident Analysis of Boron Date:

Absorbance Concentration from Measuremane Absorb ance-B i nnie Calibrstfen cur u MTAMT Sample 1 Sample 2 0.5 pos Standard k

/

1.0 pos Standard 1.5 ppm Standard 2.0 com sennaard Ave boron conc., ppa = Conc. sample #1 + Conc. sample #2 2

Sample boron conc., ppa = (Ave. boron conc., ppm) x Dilution Factor (DF)

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eAP 82C-3 Revision 22 augas: 25 1982 3 .

iNEC ATT AC.'-M E*47 C CFF-SITE DACCECURE *CCIFICAT:C.*4 .CAF M _(p - F, ec

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Pleasa AEMOVE 8 the following sagas f rom your ccarrellac coc y of sne LaSalla County 5:stion L 2F _@____ P r o c a cu r e s M an ua l .

na INSERT :ne ne. pages as incicatec anc IE*CVE anc CESTACY supersecea pages. SIGN :nis trans.ni:-41 form in :ne s;aca provicec for Manual ncicar c41c . RETURN :nis signac snee-sc:

Cffica Superviser ,

LaSalle County Station R. n. rclycax O. 5:a-ian Sucarie encen- -

LaSalle County.5:stien

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