ML20080E156

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Rev 0 to Procedure 08-S-04-905, Chemistry Instruction: Post-Accident Sampling/Analyses,Safety Related
ML20080E156
Person / Time
Site: Grand Gulf  Entergy icon.png
Issue date: 08/16/1982
From:
MISSISSIPPI POWER & LIGHT CO.
To:
Shared Package
ML20080E069 List:
References
08-S-04-905, 8-S-4-905, NUDOCS 8308300749
Download: ML20080E156 (28)


Text

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Volume 08 08-S-04-905 Section 04 Revision 0 Date: 8-16-82 l

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CHEMISTRY INSTRUCTION POST ACCIDENT SAMPLING / ANALYSES SAFE 3' RELATED Prepared: Ye #M m__ jM e Rsviewed: > [ /-  ; / _

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GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION T,itle:, Post Accident Sampling / No.: 08-S-04-905 Revision: 0 lPage: 1 Analyses J p

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1.0 PURPOSE This instruction is designed to be a guide to the Chemistry Section for collecting, analyzing, and monitoring parameters during a post accident situation where reactor water activities may approach 10 Ci/ml immediately following the accident.

2.0 REFERENCES

2.1 USNRC Regulatory Guide 1.97; December, 1980 2.2 Chemistry Instruction 08-S-04-14; Sample Preparation for Counting 2.3 Chemistry Instruction 08-S-04-104; Operation of Conductivity Bridge 2.4 Chemistry Instruction 08-S-04-107; Operation of pH Meter, and 08-S-04-109, Operation of Orion 701 Ion Analyzer 2.5 Chemistry Instruction 08-S-04-316; Development and Use of Calibration Curve for Chloride Determination using the Chloride Electrode 2.6 Chmnistry Instruction 08-s-04-303; Boron in Reactor Water, and 08-S-04-320; Development and use of Calibration Curve for Boron Determination using the Fluoroborate Electrode 2.7 Chemistry Instruction 08-S-04-133; Operation of Cas Chromotograph 2.8 USNRC Docket No 50-341; Suitability Evaluation of Post Accident Chemistry Analysis Procedures 3.0 DEFINITIONS 3.1 Post Accident Sample System - The system designed to draw high active samples following a post accident condition resulting in activities as high as 10 Ci/ml in the reactor water.

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!NFORMD0K ONil WORD PROCESSENG v

GRAND CUI.F NUCLEAR STATION CHEMISTRY INSTRUCTION * *.

Titlo: Post Accidont Saspling/~ No.: 08-S-04-905 Rsvision: O Pcgs: 2 Analyses ,

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4.0 PREREQUISITES 4.1 Prior to sampling in a condition that very high activities are suspected, all of the following should be done:

4.1.1 Determine which, if any, functions of the Post Accident monitoring System have failed and outline which samples are to be taken and the methods by which the samples will be analyzed, consistent with AIARA.

4.1.2 The Plant Chemist should brief all involved chemistry personnel to insure they are cognizant of their duties.

4.1.3 The Hot Lab should be set up and prepared for receiving and analyzing high radiation samples.

4.1.4 All instrumentation that will be used for performing analyses has been inventoried and confirmation made that calibration due for instruments are within the prescribed dates.

4.1.5 Ascertain that the required reagents, chemicals, standards and solution are available and that the shelf lives of each have not been exceeded.

4.1.6 Notified the Health Physics Section of sampling intentions and obtained dose extensions for the personnel who will be handling

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and/or analyzing samples, if required. An RWP will be required.

4.1.7 Obtained suitable anti-contamination clothing and dosimetry as deemed necessary by the Health Physics Section.

4.1.8 Sufficient monitoring equipment with up-to-date calibration has been made available as deemed necessary, by the Health Physics Sections.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION T.itle .. Post Accident Sampling / No.: 08-S-04-905 , Revision: 0 Page: 3 Analyses l l

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4.1.9 A coordinated time schedule is established with the Health Physics Section and tha Operations Section for exact time of sample and planned transfer routes in order to exclude unessential personnel.

4.1.10 The Plant Chemist's permission is received prior to drawing any high activity sample.

4.2 Attachments 4.2.1 Attachment I; Post Accident Pre-Sampling Work Sheet 4.2.2 Attachment II; Post Accident Apparatus and Reagent Monthly Inventory Check Off List 4.2.3 Attachment III; Gas Sample Analysis Work Sheet 4.2.4 Attachement IV; Liquid Sample Analysis Work Sheet 4.2.5 Attachment V; Time vs Dose Rate Graph '

, 4.2.6 Attachment VI; Shielding vs Dose Rate Graph

. 5.0 PRECAUTIONS 5.1 Each individual involved should verify that he/she.is properly badged and protected against the very high radiation dose rates, surface contamination and airborne contamination.

5.2 Shielding and distance principles should be utilized to minimize radiation doses to personnel.

5.3 Each individual should closely monitor their accrued radiaton dose by pocket dcaimeter and estimate their stay time by using the Time vs Dose Rate grs.ph, Attachment V.

5.4 No sample under these conditions should be taken unless absolutely necessary.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTI0th

Title:

Post Accidsnt Sampling / No.: 08-S-04-905 Rsvision: O Pcge: 4 Analyses ,

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5.5 As much time as possible between shut down and sample time should elapse i to allow for as much radioactive decay of the short-lived nuclides as pos sible .

5.6 After a sample is taken, as much time as possible should be taken before opening the sample flasks to allow for decay before handling, consistent with the time requirement of Reference 2.1.

5.7 Prior to sampling, quick disconnect fittings should be bagged or sleeved to contain all drops.

6.0 INSTRUCTIONS

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6.1 Time Requirements 6.1.1 After the decision is made to sample, the combined sampling and analysis times should not exceed 3 hours3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br />, with the exception of the chloride analysis, for which up to 24 hours2.777778e-4 days <br />0.00667 hours <br />3.968254e-5 weeks <br />9.132e-6 months <br /> is allowed.

6.1.2 For in-line parameters, back-up equipment will be capable of performing analysis once per day for seven days following the onset of the accident, then one sample per week until the accident condition no longer exists.

6.1.3 All required times are subject to plant conditions.

are severe enough, no samples will be taken and these time require-If conditions )

ments will not apply until the decision to draw the first sample is made.

NOTE If in-line pH and conductivity measurements using the In-Line Sampling and Analysis Apparatus (ISAA) are to be done while doing step 6.2, do steps 6.6.2.d(3)(a) through 6.6.2.d(3)(u) where applicable.

6.2 Obtain a desired grab sample and/or perform an on-line chemical analysis or other desired functions according to the following sections of Chemistry Instruction 08-S-04-904, Post Accident Monitoring System (PAMS)

Operations :

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GRAND GULF NUCLEAR STATION CPEMISTRY INSTRUCTION

Title:

Post Accident Sampling / No.: 08-S-04-905 Revision: O Page: 5 Analyses s -

6.2.1 Sample Cask Attachment, 6.2.1 6.2.2 Containment or Drywell Atmosphere Grab Sample, 6.2.8 6.2.3 Off-Gas Sample, 6.2.10 6.2.4 High Pressure Un-diluted Liquid Grab Sample, 6.2.11 6.2,5 Diluted (1000:1) Grab Sample, 6.2.12 6.2.6 Decontamination of the PAMS, 6.2.9 6 . 2 .~ 7 Sample Cask Removal, 6.2.9 6.3 Movement of Sample cask NOTE If determined by Health Physics that the person drawing the sample l

is approaching his exposure limit, another person may perform actual movement of the sample / cask.

6.3.1 When control has concurrence from Health Physics that the sample

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transport route is cleared of unnecessary personnel, move the cask to the designated area using the cleared transport route as directed by control. i NOTE It is recommended that the sample cask be taken from the 93' i

elevation Turbine Building through the access hatch into the 93' radwaste elevation, moved to the 118' elevation Radwaste Building via the freight elevator, and delivered to the Hot Laboratory via the shortest route from the elevator.

6.3.2 Place the sample cask as near as possible to the last cubicle area adjacent to the Radwaste Control Room.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION- -

Title:

Post Accidcnt Sampling / No.: 08-S-04-905 Rsvis ion: O Pcge: 6 Analyses ,

6.4 Sample Transfer )i NOTE Sample removal steps may be done in the Turbine Building.

6.4.1 For each cask from which sample is to be transferred, place rubber septas on two 120 cc vials, evacuate them to about 20 inches Hg, label one of the vials as radwaste and the other with sample name, Seal each vial in a clean plastic bag.

sampledate,andtime.Yb:d*4 cTfil57dl N. In Wa

  • 6.4.2 For gas samples, obtain another 120 cc9 o h vial, or greater)  % .'.fifill N MitSJ y .

with water and seal it with a rubber septa.

G., NOTE n>

Sealing of water vialVis not necessary, if radiation levels of the samples permit. If the water vial is not sealed, the hypodermic needle in Step 6.4.3 will not be required.

6.4.3 Deliver a hypodermic needle for venting the water vial and the prepared sample and radwaste vials to the decant location, and place the evacuated sample vial into a portable cask.

NOTE )

If a liquid sample is to be transferred, proceed to step 6.8.5.

6.4.4 Evacuate ' % bypass tubing of the gas sample cask as foll'ows:

a. Attach a syringe assembly, with a hypodermic needle in each, to the top and bottom " quick disconnect" of the sanipling cask.
b. Insert the needle of the lower syringe assembly through the septa of the vial containing water and the upper syringe needle through the septa of the vial marked " bypass radwaste."

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GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

, Post Accident Sampling / No.: 08-S-04-905 Revision: 0 Page: 7 Analyses l A

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c. Insert a hypodermic needle through the septa of the water vial to provide a vent.
d. Open the bypa.s valve (middle valve) and allow the bypass line to fill wi h water.
e. When water is being delivered into the waste vial at an even flow, close the bypass valve.

6.4.5 Transfer the gas sample as follows:

a. Remove the upper syringe assembly from the radwsste vial and insert it through the septa of the 120 cc sample vial in the portable cask.

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b. Open the upper sampling cask isolation valve, then slowly open l the lower isolation valve, and allow the gas sample to flow into the evacuated sample vial.
c. When a steady stream of water begins to flow after the gas tranfer, close the lower isolation valve, then the upper isolation valve.
d. Measuce and record the radiation dose rate of the gas sample.
e. Remove the hypodermic needle from the septa of the sample vial and insert the needle into a rubber stopper.
f. Transfer the sample to the fume hood which has been prepared for receiving the sample.
g. Using a liquid manometer, return the sample vial to atmospheric pressure. 74 A w%fw m e8er b be m@

wmF  %. v: .t a.m a, a w A 4 wrw 144. ace. . 2%f e, weach %JL NOTE Woo A +- 6 46It bp. A wA w~MI  % l. LII;q d. p s .

The gas volume in the sample cask is approximately 30 cc and if the water is extracted from the sample vial, I cc of the gas in the 120 cc sample vial is equal to approximately 0.25 cc of the original sample.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlo: Post Accident Sampling / No.: 08-S-04-905 Rsvision: 0 Page: 8 Analyses i I ,

h. When finished with the sample, seal all hypodermic needle penetrations with a dab of silicone grease.

6.4.6 Evacuate the bypass tubing of the liquid sample cask as follows:

a. Attach the " vent assembly" to the upper " quick disconnect."
b. Attach the " syringe assembly" to the lower " quick disconnect."
c. Push the needle of the syringe through the plastic bag and through the septa c.f the radwaste vial.
d. Open the bypass valve (middle valve) and the vent valve to allow the flush water to flow into the radvaste vial.
e. Close the bypass and vent valve.

6.4.7 Transfer the liquid sample as follows:

a. Remove -he hypodermic needle from the septa of the radwaste vial and insert it through the septa of the sample vial in the portable cask.

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b. Open the topjMbottom _n/did "-- valves to allow the sample to

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flow into the sample vial.

c. Check the area radiation dose rate.
d. Obtain and record the contact dose rate of the sample.
e. Close the inlet, outlet and vent valves.
f. Dc steps 6.4.5.e, 6.4.5.f and 6.4.5.h.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

, Post Accident Sampling / No.: 08-S-04-905 . Revision: O Page: 9 Analyses O

C 6.5 Grab Sample Analysis NOTE 1 Baeed on levels of redioactivity, radioactive contamination and the nature of the contamination, the Senior Radiochemist will determine which approved Chemistry Procedure, what instrumentation and apparatus, and what volumes of sample will be used, consistent with the principles of ALARA. j NOTE 2 Prior to and during sampling, the required instrumentation shall be checked for up-to-date calibration and placed into operation, all reagents and apparatus shall be inventoried for each procedure and bench and/or calibration standards shall be analyzed at the discretion of the Senior Radiochemist. Systems and instrumentation are as follows:

1. Germanium Lithium Detector System I
2. Gas Chromatograph
3. Fluoroborate Selective Ion Electrode, double junction reference l electrode and the pH/mV that will be used with it. (if required)
4. Chloride Specific Ion Electode, double junction reference electrode and the pH/mV meter that will be used with these electrodes
5. pH and conductivity instrumentation used routinely
6. pH and conductivity using the "In-line Sampling and Analysis Assembly." (If this method is used, start up, check out, etc.,

must precede sampling and analysis, since sampling and analysis are concurrent.)

7. Any apparatus, instrumentation, reagents and standards associated with approved Chemistry Procedures which may be used to replace any of the above I

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION -

Title:

Post Accidsnt Sampling / No.: 08-S-04-905 Revision 0 Pege 10 Analyses . .

6.5.1 Gas Analysis

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a. Record sample source, date, time and initials of the person who drew the sample in the spaces provided on the worksheet.
b. Record the initials of the person who transferred the sample to the 120 ce flask and the contact dose rate (mR/Hr) of the sample in the 120 ce flask at time of transfer.

NOTE In most, but not all cases, the person performing the analysis is not the person who drew the sample or made transfers and prepared dilutions of samples.

c. Gamma Spectral Analysis (1) If the dose rate of the sample is within limits acceptable to the Senior Radiochemist, seal a clean, new 14.7 cc gas vial with a clean, new rubber septa and using the same gas tight syringe that will be used for pipetting the gas sample, evacuate 4 cc of air from the 14.7 ce gas vial.

(2) Eject the air from the syringe and quickly transfer (pipet) 4 cc of the gas sample from the 120 mi flask to

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the evacuated 14.7 cc gas vial.

NOTE The 14.7 cc vial now contain 1 cc of the original sample.

(3) Place the 14.7 cc vial with gas sample outside of the energy field generated by the sample in the 120 mi flask, measure the dose rate of the vial at contact and record the dose rate on the worksheet.

(4) If the dose rate is less than 0.5 mR/Hr dab the needle penetrations with silicone grease, change gloves, wrap the vial in clean plastic film (ex. Saran Wrap), twist, secure with tape, crim the excess film, place in a clean plastic bag and deliver to the detector cave that will be used for counting the sample, then proceed to step 6.5.1.c (12).

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

, Post' Accident Sampling / No.: 08-S-04-905 Revision: O Page: 11 Analyses O

-1 (5) If the dose rate is greater than 0.5 mR/Hr using the table below, determine the number of dilutions which will provide a gas vial contact dose rate of less than 0.5 mR/Hr when using other sealed 14.7 cc gas vials with I cc of air evacuated from each vial and replace with I cc of gas sample in successive order, beginning with the gas sample measured in step 6.5.1.c (3).

GAS DILUTION TABLE

_ Sample Sp1 Vial Dose Dilutions Reg'd ml orig. Sp1 Multiplication From Rate (mR/Hr) I cc to 14.7 al in vial Factor 6.5.1.c (3) <0.5 count as is 1 1 6,5.1.c (3) 0.5-8 1 .068 14.7 l

prev, dil. 8-120 2 .0046 217 prev. dil. 120-1900 3 .0003 3333 prev. dit. 1900-30,000 4 2.04E-5 4.9E4 prev. dil. 30,000-50,000 5 1.39E-6 7.19E5 (6) Based on the number of dilutions required, remove 1 cc of

' air from new, labeled (adhesive label) vials using the gas tight syringe that will be used for pipetting.

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GRAND GULF NUCLEAR STATION CHE'MSTRY INSHbCTIdN

Title:

Post Accidsnt Sampling / No.: 08-S-04-905 I}svision: 0 ;Pege: 12 Analyses ,

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(7) Maka successive dilutions by tranferring I cc aliquots 9 from the previous dilution to the partially (lec) evacuated gas vials.

(8) Using an HP dose rate instrument, measure the dose este (mR/Hr) of each dilution.

(9) On the work sheet, record the dose rate (mR/Hr) of each dilution and indicate which dilution will be counted by checking the appropriate blank.

(10) Seal all needle penetrations in the septas of all dilutions with a ses11 dab of silicone grease.

(11) Change gloves and wrap the dilution selected for counting in a clean sheet of plastic film (Saran Wrap), twist and secure with tape, crim the excess film, place in a plastic bag and deliver to the detector cave that will be used for counting the sample. .

(12) Perform a quantitative isotopic analysis of the sample according to Chamistry Instruction 08-S-04-200 and 08-S-04-212 using the GSMCA program to collect the spectrum and the GSRAP program to analyze the spectrue.

(13) Record count date and time, geometry, name of person performing the analysis and the attivity of those isotopes listed on the work sheet.

(14) Attach the work sheet to the data priatout.

d. Hydrogen and Oxygen (1) Using a gas-tight syringe, inject an aliquot (0.5 cc) into the gas Chromatrograph, and record date and time of analysis, volume of aliquot and name of the person performing the analysis.

(2) Read, then record the gas concentrations (%) on the worksheet.

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GRAND GULF NUCLEAR STATION CHDfISTRY INSTRUCTION

Title:

. Post Accident Sampling / ;No.: 08-S-04-905 Revision 0 Page: 13 l Analysis 0

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(3) If no other analyses are to be done, seal all needle penetrations that have not been sealed thus far with a dab of silicone grease, and store in the lead brick cave in the hot labortory.

6.5.2 Liquid Analyses NOTE Based on the radiation level (s) of the sample (s) and the possibility of airborne contamination when a sample is opened in ,

the fume hood, the Senior Radiochemist will determine the apparatus and the method (s) by which, the sample (s) will be analyzed at all applicable steps in this procedure.

a. Do steps 6.5.1 AND 6.5.1.b.
b. Wearing required TLD's (whole body and finger rings),

_ dosimeters and gloves, and using tongs and an HP dose rate instrument, determine as near as possible, the contact dose rate of the sample in the 120 m1 flask, and place the sample in the space prepared for it behind the lead brick barricade.

c. Gamma Spectral Analysis (1) From the dose rate obtained and at the discretion of the Senior Radiochemist, determine what volume of sample diluted to 3 al or to 1000 ml will be required to provide a dilution with a contact dose rate in teh range of 0.05 to 0.5 mR/Hr.

(2) Prepared the 2 al dilution in a clean, new I dram vial using a clean, new rubber septa or the 1000 ml dilution in a clean, new polypropylene bottle according to Chemistry Instruction 08-S-04-14.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION TitLc: Post Accidsnt Sampling /'

No.: 08-S-04-905 Rsvision: O Pego: 14 Analyses I CAUTION At the discretion of the Senior Radiochemist, if there is concern about possible airborne contamination, the sample should not be opened to the atmosphere, and the 1 dram vial or the 1000 ml polypropylene bottle should be sealed after the diluent is placed in it and a volume of air equal to the volume of sample removed from the vial or the 1000 mi bottle before the sample is added.

NOTE If airborne contamination is a concern, dab all needle penecrations in the septas of the sample and dilutions with silicone grease when pipetting is complete.

(3) Perform a quantitative isotopic analysis of the dilution according to Chemistry Instruction 08-S-04-200 and 08-S-04-212 utilizing the GSMCA program to collect spectrum and the GSRAP program to analyze the spectrum.

(4) Record count time and date, geometry and activities of those isotopes listed on the work sheet and sign or 3 initial the space provided. J (5) If no oth'er analyses are to be performed at this time, store all samples and dilutions as directed by the Senior Radiochemist,

d. pH and conductivity NOTE If determined by the Senior Radiochemist that the radiation level of the sample is too high, or that airborne contamination is likely if the sample is analyzed by routine methods, proceed to step 6.5.2.d(3).

(1) Use the designated fume hood if necce. ary, and perform a pH measurement according to Chemistry Instruction 08-S-04-104.

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GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION

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, Post Accident Sampling / No.: 08-S-04-905 Revision: O Page: 15 Analyses x

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(2) Record initials, analysis data and the method (s) used on the worksheet.

(3) pH and conductivity using the pH and conductivity "In-line Sampling and Analysis Assembly" (ISAA).

(a) Turn the pH/mV meter and the conductivity bridge off, unplug the electrodes, drain the ISAA, fill it with buffer solution and tape adeqtia.te sleeving over both quick disconnects.

(b) Request that Operations open all root valves to permit sampling at the Post Accident Sample Panel.

NOTE A coordinated time schedule with Health Physics and Operations must exist in order to exclude nonessential personnel, and approval for sampling muet be granted by the Plant Chemist.

(c) According to the directives of HP supervision relative to the existing conditions, don protective clothing (if required), respiratory protection devices (if required), whole body and externity TLDs and self reading dosimeter (s) as required.

(d) Select an HP survey meter, check that the calibration due is within the prescribed date and perform an instrument check.

(e) Set the HP survey instrument to the highest range before departing the laboratory.

GRAND GULF NUCLEAR STATION CHEMISTRY INSTkUCTION*

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Title:

Post Accident Sampling / No.: 08-S-04-905 Rsvision: 0 Ptgs: 16 Analyses . .

(f) Deliver the ISAA and other apparatus to the Post Accident Sample Panel, and while enroute, continuously monitor radiation levels and the status of GAMS and ARMS.

(g) Survey the area around the " Sampling Skid," if the dose rate is too high to work in, move the " Sampling Skiti" as far away from the source as possible, run the lead wires threugh the lead brick shielding and plug them into the appropriate jacks for each.

(h) Apply pwer to the instruments.

(i) Retreat, if necessary, to an area with a lower background dose rate, and allow the instrument to warm up for 5 to 10 minuter, (j) Upon returning, adjust the pH/mV meter to the value of the buffer solution, and affirm that the conductivity bridge is functioning properly.

(k) Set the instruments to " standby."

(1) Place the " Sampling Skid" close enough to the

" Sampling Panel" to attach the ISAA to the undiluted -)

grab sacple outlets, then, attach the ISAA to the outlets.

(m) Slip the sleeving over the " quick disconnects" of the sample outlets and seal the sleeving with tape.

(n) Position the shielded " Sampling Skid" as flush as possible against the sample panel wall to cinimize

" shine."

(o) Cover the ISAA cavity with lead bricks.

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GRAND GUTJ NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

, Post Accident Sampling / No.: 08-S-04-905 Revision: 0 Page: 17 ,

Analyses l (p) Initialize purging and sampling as per Chemistry Instruction 08-S-04-904, Section 6.2.11 and measure radiation dose rates around the shielded skid.

(q) Set the instruments to read pH and conductivity.

(r) Retreat, if necessary, to an area with a lower )

background dose rate to allow adequate flushing sampling, and instrument stabilization.

(s) When readings have stabilized, record sample time, temperature, pH and conductivity, method used, and set the ins truments to " Standby" or "Of f."

(t) If not directed to retreat, decontaminate and shutdown the sampling system per Chemistry Instruction 08-S-04-904, Section 6.2.2.

(u) If directed to do so, back the shielded skid away from the ISAA and remove the ISAA per Chemistry Instruction 08-S-04-904, Section 6.2.9.

(4) Retreat from the area with or without the ISAA and other

.j instrumentation as directed by the Senior Radiochemist.

e. Chloride (1) Based on the radiation level and the possibility of airborne contamination from the sample, select one of the two following alternatives:

If the radiation level of the sample is low and (a) airborne contamination is not likely, analyze the sample for chloride using the approved Chemistry Instruction selected by the Senior Radiochemist, and record the analysis data and the method used in the spaces provided on the worksheet.

(b) If the radiation level is too high and/or the potential for airborne contamination exists, proceed to step 6.5.2.e (2).

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTIdN '

Title:

Post Accidsnt Sampling / No.: 08-S-04-905 Rsvision: 0 Psga: 18 Analyses ,

-s (2) Don the necessary whole body and extremety TLDs, self- ~D reading dosimeter (s), anti-contamination clothing and respiratory protection devices specified by the Health Physics Department.

(3) Using lead shieldies in the fume hood prepared for this analysis, perform a chloride analysis according to Chemistry Instruction 08-S-04-316 using the Lazar Specific Ion Electrode and the Lazar double junction

. reference electrode.

NOTE The Senior Radiochemist may select either the Chloride Analysis Chamber or the microdishes for analysis.

(4) Record the analysis data and the method used

f. Boron (1) Based on the radiation level and the possibility of airborne contamination from the sample, select one of the two following alternatives:

(a) If the radiation level of the sample is low and )

airborne contamination is not likely, analyze the sample for boron using the approved Chemistry Instruction selected by the Senor Radiochemist, and

. record the analysis data and the method used in the spaces provided on the worksheet.

(b) If the radiation level is too high and/or the potential for airborne contamination exists, proceed to step 6.5.2.f(2).

(2) Don the necessary whole body and extremety TLDs, self-reading dosimeter (s), anti-contamination clothing and respiratory protection devices specified by the Health Physics Department.

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION T(tle: 1 Post Accident Sanpling/ No.: 08-S-04-905 Rt; vision: 0 Page: 19 Analyses 0'

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(3) Using lead shielding in the fume hood prepared for this analysis and as determined by the Senice Radiochemist, analyze a small volume or a large volume sample for boron using Chemistry Instruction 08-S-04-320 for the analysis of high radiation samples.

(4) Record the analysis data and the method used in the spaces provided on the worksheet.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-905 Rev. 0 Attachment 1 Page 1 of 4 (7) .

POST ACCIDENT PRE-SAMPLING WORKSHEET Enter N/A in all spaces that are not applicable.

I Post Accident Monitoring System The monitoring capability of the following has/have failed:

Gross Activity Isotopic Analysis Hydrogen Dissolved Oxygen i

Chloride l PH Conductivity All of the above Analyses of Grab Sample (s) required:

Gcs Samples from:

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Analyses (of gases) required Gross Act. Gamma Spectral

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-905 Rev. O Attachment I Page 2 of 4 b --

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Chemistry personnel reporting for work on any later shift will be briefed before boing allowed to enter their assigned work areas and these briefings will remain in effect until such time, because of conditions, the briefings are deemed unnecessa ry.

Plant Chemist Date Radiation dose extensions have been requested.

Plant Chemist or Senior Radiochemist Date {

Ehsn completed and initialed, the following verifies that calibration due is within the prescribed date for each instrument or system:

Ins t rument/Sys t em MP&L No. Calib. Due Date Initial Ganuna Spectral System Gas Chromatograph pH/mV meter pH/mV meter Conductivity Bridge Conductivity Bridge Whan entered and initialed, the following verifies that startup, function checks, l calibration curves and bench standard analyses were performed / generated in accordance with the appropriate Chemistry Instruction for each instrument and is documented in the respective Calibration Functional Check Log Book for each Instrument / System (including electrodes, lead wires, connectors, filling solutions in use, etc.):

Instrument / System Chem. Instr. Date Done Enter By Br Gamma Spectral System 08-S-04-200 08-S-04-212 Cas Chromatograph 08-S-04-133 pH/mV meter 08-S-04-109 pH/mV meter 08-S-04-109 Conductivity Bridge 08-S-04-104 Conductivity Bridge 08-S-04-104 Flouroborate and reference _

electrode with pH/mV meter above 08-S-04-320 Spectrophotometer for 08-S-04-303 Boron Chloride and reference electrode (routine) with PH/mV meter above 08-S-04-316 V

CRAND' GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-905 Rev. 0 Attachment 1 Page 3 of 4

.)

Instrument / System Ch em. Instr. Date Done Bjr Enter By Chloride and reference electroda (Lazar) with pH/mV meter above 08-S-04-316 ISAA, pH 08-S-04-109 ,

ISAA, cond. 08-S-04-104 The Senior Radiochemist confirms the following:

Applicable reagents and other solutions listed in Section 4.0 have been inventoried and replaced as required, in accordance with the applicable, approved Chemistry Instructions for reagent preparation, confirming that the shelf life for each raagent to be used, has not been exceeded.

Tha hot laboratory (or assigned laboratory) has been set up to receive and analyze l high radiation samples according to Section 4.0.

l Adaquate anti-contamination clothing and respiratory protection devices have been i

provided.

7s Proper personal dosimetry and dose rate measuring instruments deemed 'necessary by I

Haalth Physics Supervision have been provided.

Senior Radiochemist Date Dose extensions for the following personnel have been granted by the Health Physics t Dspartment:

l NAME S. S. NO. NAME S. S. NO.

i 1

l S nior Health Physics or Senior Radiochemist Date y

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

, , [ 08-S-04-905 Rev. 0 l Attachcient I Page 4 of 4'

, -)

Parmission is granted to sample:

Time /Date Plant Chemist Plant Chemist Plant Chemist Plant Chemist Plant Chemist Plant Chemist Plant Chemist Plant Chinist Plant Chemist Plant Chemist Notified the Health Physics Section and the Operations Section of the intent to sample and set a time schedule for sampling and transferring samples in order to exclude unessential personnel.

Ssnior Radiochemist Time /Date 1

T 24 -.

\

, j s- 's

. g a  : -

.i- x s

a  %'

)

= - .

GRAND ' GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

, , 08-S-04-905 Rev. O Attachment 11 Page 1 of 2 l

_ f')

./

POST ACCIDENT APPARTUS AND REAGENT HONTHLY INVENTORY t

CHECK-OFF LIST Enter N/A in all spaces that are not applicable.

A. Sampling Apparatus and Reagent

1. Bag, plastic, various sizes
2. Buffer, solution (PH7 or 10) 3.

~

Cert, olectric pallet

4. Clothing, anti-contamination Ceseralls (cloth) (paper) Skull Cap (cloth)

Moods (cloth) Gloves (cloths) (plastic) (rubber)

Wet-Suit Shoe covers (cloth) (plastic) (rubber)

., Lab Coat (coat) (pape r) Tape

5. Conductivity Bridge (ISAA) i 6. . Dosimeters, self-reading high range low range
7. Electrode (s) (ISAA) comb. PH/ref. cond. cell (ISAA)

-8. In-line sampling and analysis assembly (ISAA) housing

~

9. Mirror
10. PH/mV meter 6 11. Radiation dose rate instrument
12. Sampling cask and skid: gas sp1 un-dil Spl dil spi
13. Sampling and analysis shield for ISAA
14. Scissors

. 15. ,pleeving (plastic) 3- '16. Stopwatch _

.17. Valva extension for the ISAA

-- 18. ISAA filling apparatus (inlet) (outlet) h -

.w B. Sample Transfer Apparatus

1. Bags (plastt,c)

Cask (s) portable 2.

3. Labels (cape) _,

4 Needles, hypodermic w

s M

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-905 Rev. O Attachment II Page 2 of 2 w- .

O B. ' Saaple Transfer Appratus'(Continued)

5. Silicona greeae

., 6. Scop pe rs , rubber

7. Syringe Assembly (2)
8. Tape
9. Vacuum gun with hypodermic needle
10. .'. Venting assembly ___

11~. Vials,';120 cc or larger with rubber septas (12 or more)

12. A.4 and A.il e

C. Analysis Apparatus and Reagents

1. Apparatus sad Reagents as per Chemistry Instruction:

08-S-04-104 08-S-04-109

, 08-S-04-133 =08-S-04-200 -

08-S-04-212 08-S-04-303 08-S-04-316 ~ 08-S-04-320

/ / .

r 1> .. 2. Chloride Analysis ' Chamber (l , ' r. 3. Gas tight syringe: Micro Macrc 47

/ Hypqdermic needles: Micro Macro 5 '. Lazar (or equivalent) chloride specific ton electrode

6. , Lazar (ce equivalent) reference electrode
7. Plastic bags ___

,8 . / Lead brick

, Rubber septas

l19.

10. ' Rubber stoppers
11. Shielded sample holders

-- 12 . A.4~and A.11 e

}

l Inventory Performed By:

Sampling Inv. Spl. Transfer Inv. Analysis Inv.

I e

+

9

+

m* __

t P

w q e_

,,.- . w 4sd

  • \ --'g

> M g _ _ _ _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ - _ _ - _ - - - - . - - - - - - - --

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

.

  • 08-S-04-905 Rev. 0 Attachment III Page 1 of 1 O_ O' GAS SAMPLE ANALYSIS WORK SHEET Enter N/A in all spaces that are not applicable.

Sample Source ,

Sample: Date Time Sampled By Trensfer to 120 mi flask by Dcca Rate at contact of sample in 120 ml flask mR/Hr.

G:mma Analysis original l Dil. 1 Dil. 2 Dil. 3 Dil. 4 Dil. 5 Dil. 6 ,

Dil. Used cc orig. spi 1 0.068 0.0046 0.003 2.004E-5 1.39E-6 9.46E-8 Mult. Factor 1 14.7 217 3333 4.9E4 7.19E5 1.06E7 l l \

mR/Hr. l i l j Count Date Time Geometry By Analysis Data i -

Isotope uCi/cc at Spl Time i Isotope I uCi/cc at Spl Time i Kr-85 Xe-133 i

Kr-85m Xe-135 Kr-87 Kr-88 Hydrogen and Oxygen Date Time, ml Sample By:

Q H2  % 02% N _ _ _

Ssnior Radiochemist Date I

i

( .

,CRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

  • 08-S-04-905 Rev. O I*

. (R

,- Attachment IV Page 1 of 1 l .

LIQUID SAMPLE ANALYSIS WORK SHEET

  • Enter N/A in'all spaces that are not applicable.

Sample Source -

Sample: .Date Time Sample By.

.i. Tecasfer to 120 ml Flask by Dose Rate R/He Couiit Date _ Tim; Geometry -

By

.;{- .

Isotope 'uCi/ml at Sample Time Isotope uCi/ml at Sample Time 1-

'I-131 Cs-137

. Water Analysis PH Cond. Cl- B Date Time

Analyst g . . . _ _ .

l Temp. *C al Sc.mple N/A N/A N/A - N/A Diluted To N/A N/A '

MV N/A N/A

\ ,~ -

~ '

Mathod Used Concentration /Value ppa ppe

> GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION 08-S-04-905 Rsv. 0 a * -

Attachment V Page 1 of 1 0v .

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