ML17277A630

Rev 0 to Chemistry Procedure 12.10.5, Post-Accident Sampling & Analysis,Gas Sample Analysis.

ML17277A630
Person / Time
Site:	Columbia
Issue date:	06/21/1983
From:	Martin J WASHINGTON PUBLIC POWER SUPPLY SYSTEM
To:
Shared Package
ML17277A623	List: ML17277A622 ML17277A624 ML17277A625 ML17277A626 ML17277A628 ML17277A630 ML17277A631 ML17277A632
References
12.10.5, NUDOCS 8307050165
Download: ML17277A630 (10)

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<<12e10.5 06/21/83 VOLUME NAME 12 CHEMIS. RY PROCEDURES SECTION 12.10 POST ACCIDENT SAMPLING PROCEDURES TITLE "12.10.5 GAS SAMPLE ANALYSIS 12.10.5.1 P~ur oee This procedure determines gas concentrations and activity from a sample taken from the post accident sample station.

12.10.5.2 Precautions/Prere uisites A. Lab personnel shall be issued extremity dosimetry as per Health Physics policy.

B. Lead shielding must be setup prior to sample handling.

C. The gamma spectrometer system must be operable.

D. The gas chromatograph must be calibrated (see 12.10.5.5) prior to analysis.

E. The gas chromatograph must be operating 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> prior to analysis.

F. Carrier gas flow must be approximately 20cc/min (20 psi).

G. All sample handling must be carried out in a hood.

H. Appropriate dose rate meter must be available and in calibration.

Use continuously to assure exposure ALARA.

12.10.5.5 E~ui ment A. 1.0 ml and 0.1 ml gas tight syringes B. Oxygen, hydrogen and nitrogen gas standards C. 14 ml and 125 ml serum vials 8307080i68 830623 PROCEOURE NUMBER REVISION NUMBER PDR ADOCK 08000397 PAGE NUMBER h

PDR j 12.10.5 12.10.5-1 of 8 WP 597 R1

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, 12.10.5.4 Procedure A.. On HP3390 integrator enter scale setting:

l. OP ( ) 6

2. Scale setting B. Open valve on gas tight syringe.

C. Insert 1.0 ml syringe needle into sample part and withdraw syringe plunger to 1.0 ml.

D. Allow a few seconds for pressure to equalized across the needle.

E. Close valve on syringe and release plunger.

F. Note actual volume sampled and record on. Attachment I.

G. Withdraw syringe from sample.

H. Insert syringe into septum on the gas chromatograph.

Open valve on syringe and inject sample.

If not already depressed, press the AUTO button then press clear.

Read percent concentration from HP3390 integrator and calculate 1 .1 .5.

A.

~1 percent concentration in containment as per Attachment I.

From sample dose rate determine what dilutions are needed to reduce sample dose rate to less than 5 mrem at 2 inches. Record dilutions on Data sheet, Attachment III.

B. Place septums or appropriate number of serum vials and evacuate.

C. Place vials behind lead shielding.

D. .With an appropriate syringe inject a volume of H20 equal to the desired aliquot then withdraw an aliquot and transfer to a 14 ml or 125 ml serum vial.

E. Complete required dilutions behind the lead shield as planned.

Final dilution is into a 14 ml serum vial for counting.

RQCEDURE NUMBER REVISION NUMBER PAGE NUMBER W~QB

,12.10.5 0 12.10.5-2 of 8

Bag or wrap in plastic the .final dilution, smear and survey'then when less than 1000 dpm/100cm2 contamination, remove to counting room.

G. Adjust sample counting time to reflect its activity as .estimated by its dose rate.

12.10.5.6 Calibration A. Using a gas tight syringe obtain a 100 micro liter sample of standard hydrogen gas.

B. Inject into gas chromatograph.

C. If not already depressed, press AUTO.

D. Press CLEAR.

E. When chromatogram is complete enter the data into the HP3390 integrator:

1. Del CALIB

2. CALIB ESTD

3. Ref RTW = 5

4. RTW = 5

5. RT = (retension time for hydrogen)

6. AMT = 10.0 (10.0 vol percent)

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7. ENTER F. Repeat Steps 12.10.5.5.A through 12.10.5.5.D for oxygen gas standard.

G. Enter data into HP3390 integrator:

l. EDIT CA! IB

2. REF'RTW = 5

3. RTW =5

4. CAL8 = 2

5. RT = (retension time for oxygen)

ROCEDURE NUMBER REVISION NUMBER )PAGE NUMBER 12.10.5 0 I 12.10.5-3 of 8 W~90

6. AMT = 10. (volume percent) 7.. AMT/HT = (10.0 volume percent divided by peak height)

8. ENTER H. Repeat Steps 12.10.5.5.A through 12.10.5.5.D for nitrogen.

I. Enter data into HP3390 integrator:

l. EDIT Calib

2. REF RTW = 5 RTW = 5

4. CALO = 3

5. RT = (retension time for nitrogen)

6. AMT = 10.0 (volume percent nitrogen)

7. AMT/HT = (10.0 volume percent divided by peak height)

8. ENTER Steps 12.10.5.5.A through 12.10.5.5.D can be repeated for any additional gases.

If a calibration table already exists, the calibration table can be updated by injection of a standard as in Steps 12.10.5.5.A through 12.10.5.5.D then pressing RCAL. This process would have to be repeated for each gas unless a mixed gas standard is available.

12.10.5.7 Documents A. Attachment I, Calculation of Containment Gas Concentration B. Attachment II, Conversion Factors C. Attachment III, Dilution Data Attachment IV, Final Concentration Calculation PROCEDURE hlUM8KR REVISION IYUM8ER ~PaCa nUM88R W~Qa 12.10.5 0 l 12.10.5-4 of 8

0' Sample percent by volume t

Calculation of Containment Gas concentration of each gas:

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Concentration

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'A VS A = AT V

A Where:

AT = volum percent analyzed AS = volum percent in vial before analysis VA = volume of aliquot removed from standard VS = volume of vial Percent by volume of each gas in containment:

C

( s)( c)( v) pc (Containment Pressure) (Partial Pressure of Water)

TV Vial Temperature Vial Pressure mm Hg TC Containment Temp Containment concentration in percent by volume = X H2 Attachment I ROCEOURK NUM8KR [REVISION NUM8ER PAGE NUMBER W~94 12.10.5 ~

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12.10.5-5 of 8

L 0 Conversion Factors ounds/s uare inch to mm H d

11/'4.696 1b/in Fto C oF = 9/5 (oC + 32)

Cto K oK =oC+ 273 Attachment II PROCKQVRK NVMBKR iRKVtStON aVM8KR [PACK i>VM8KR W~94 12.10.5 0 I 12.10.5-6 of 8

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, Dilution 1 aliquot cc (a) final volume cc (b)

Dilution 2 aliquot cc (c) final volume cc (d)

Dilution 3 aliquot cc (e) final volume cc (f) b X

d f X = dilution factor (df) a c e (measured uCi/cc)(df) = AR, activity remaining in vial after gas chromotgraphy analysis i

A. =

VA + VS VS A

R Ai = initial uCi/cc in sample VA=l CC VS = volum of vial Attachment III RQCEDVRE NUMBER REVISION NVMBER iPAGE NVMBER whee 12.10.5 0 12.10.5-7 of 8

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'I Final Concentration I~ecto e. uCI/co 'A UC1/CC kr85 kr88 Xe-133 Xe-135 Attachment IV PROCEQURE NUMBER (REVISION NUMBER (PAGE NUMBER wanga 12 10 ~ 5 I 0 12.10.5-8 of 8