ML20058H619

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To Chemistry Instruction:Sample Preparation for Counting Safety-Related
ML20058H619
Person / Time
Site: Grand Gulf  Entergy icon.png
Issue date: 02/02/1982
From: Wedgeworth B
MISSISSIPPI POWER & LIGHT CO.
To:
Shared Package
ML20058H456 List:
References
RTR-NUREG-0737, RTR-NUREG-737, TASK-2.B.3, TASK-TM 08-S-04-14, 8-S-4-14, NUDOCS 8208030653
Download: ML20058H619 (12)
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Text

PLANT OPERATIONS MANUAL to AECM-82/339 Volume 08 08-S-04-14 Section 04 Revision 2 1

Date: 2-2-82 t

' CHEhISTRY It'STRUCTION SAMPLE PREPARATION FOR COUNTING SAFETY RELATED e

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Che7m stry/ Radiation Contre Superintendent Concurrence:

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' Assistant Plant Manager List of Ef fect ive Pages :

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GRANT) GULF NUCLEAR STATION CHEMISTRY INSTRUCTION JTitle:

Stmple Preparation

  • No.:

08-S-04-14 Revision:

1 Pcge:

I for Counting Y

1.0 PURPOSE The purpose of this instruction is to provide detailed ins t ructions for preparing samples for counting so that sample geometries will be reproducible.

2.0 RF.FERENCES 2.1 Standard !!ethods, 14 Edition, 560 2.2 Chemistry Procedure 08-S-03-1, Qualification of Chemistry Program 3.0 DEFINITIONS

d None 4.0 PREREQUISITES 4.1 Apparatus Recuired 4.1.1 1-Liter Marinelli be'aker 4.1.2 4-Liter Marinelli beaker 4.1.3 1-Liter poly bottle 4.1.4.14 el off gas vial

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4.1.5 1 dram vial 4.1.6 k'hatman filter paper, No. 542 4.1.7 Planchet

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4.1.8 Liquid scintillation vial 4.1.9 Charcoal Cartridge, 81.-705C-727 or equivalent b

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. GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Sceple Prepa.3stion No.:

08-S-04-14 Revision:

1

Pcge

2 for Counting 4.1.10' Filter paper, 47mm 4.1.11 Resin paper, 47mm 4.1.12 Saran Wrap 4.1.13 Millipore Petri Dish, PD 10-047-00 4.1.14 Millipore Petri-Slide, PD 15-047-00 4.1.15 Mounting card, 3 x 2 1/2 inches 4.1.16 ' Tie wrap labels 4

I 4.1.17 Mylar film 4.1.18 Electrical tape or equivalent 4.1.19 Two-sided tape 4.1.20 Bag sealer 4.2, Reagents Required 4.2.1 Insulin 4.2.2 Sodiun Hydroxide, IN 4.2.3 Sodium Sulfate, 100eg/ml 4.2.4 Gel-Guard or equivalent 4.2.5 Silicone grease 4.2.6 Scintillation solution i

4.2.7 Acetone, reagent grade l

o l

i

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Sample Preparation No.:

08-S-04-14 Revision:

1 Prge:

3 for Counting 5.0 PRECAUTIONS 5.1 Extreme care should be exercised to keep the external surfaces of samples free of radioactive contamination.

5.2 Handle radioactive samples in accordance with radiological safety procedures.

6.0 INSTRUCTIONS 6.1 1-Liter Marinelli Beaker 6.1.1 Transfer 1.0 liter of sample to a clean Marinelli beaker.

If the volume of sample is less than 1 liter, record the volume of sample I

and dilute to 1.0 liter with demineralized water.

6.1.2 If visible particles are present, the sample should be gelled with Gel-Guard or eauivalent.

Do not gel calibration standards or regulatory samples.

6.1.3 Label the Marinelli beaker lid appropriately.

6.1.4 Place cover on Mari'nelli beaker and secure with electrical tape or equivalent.

6.1.5 Clean the outside of the beaker

  • to remove' any contamination.

6.1.6 The sample is in the correct reometry for counting on a Germanium detector sys tem.

l 6.2 4-Liter Marinelli Beaker 6.2.1 Transfer.3.0 liters of sample to a clean Marinelli beaker.

If the volume of the sample is less than 3 liters, record the volume of the sample and dilute to 3.0 liters with demineralized water.

6.2.2 If visible particles are present, the sample should be gelled with Gel-Guard or equivalent.

Do not gel

  • calibration standards or regulatory samples.

6.2.3 L bel tb-Parinelli heal"tr 'id.:pr-ar iately.

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1

. GRAND GULT NUCLEAR STATION CHEMIST 3Y i.f i Titic:

Scmple Preparation No.:

OS-S-04-14 Revision:

1 l Para:

for Counting I

(

6.2.4 ' Place cover on Marinelli beaker and secure with s:tet- ' :: :

tape or ecuivalent.

6.2.5 Clean the outside of the beaker to remove any on t enin.

6.2.6 The sample is in the correct geometry for coim e ir.2 m-detector system.

6.3 1-Liter Poly Bottle 6.3.1 Transfer 1.0 liter of sample to a clea61-liter poly bot- '4

.f

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~

the volume of the sample is less than 1 liter, record

-bs-

'of the sample and dilute to 1.0 liter with de.~inerc:'.:ad ~ :e.

I 6.3.2 If visible particles are present, the sample shoul. -

.I'.ed wi-h

~

Gel-Guard or equivalent.

Do not gel calibration =:nai: ris or regulatory samples.

6.3.3 Cap the bottle securely and label appropriately.

6.3.4 Clean the outside of'the bottle to remove any contamin-tion.

6.3.5 Place the bottle in a plastic bag and seal with bar

..>.11 e r e r tape.

6.3.6 The sample is in the correct pecmetry for corntinn 6: rer anium detector system.

6.4 14 n1 Of f-Gas Vial' 6.4.1 The volume of individual off gas vials are measured prior to use.

l The of f gas sample panel normally allows the vials to be completely filled, but when not completely filled with of f. gas, L..._..,

the effective' volume can be calculated from the following l

formula.

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p..Lg.y I.g.f o.s

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t.m C tie:

.:nple Preparation lNo.:

0*-E-9 -l-

. -vision:

1 iPage:

5 for Counting l

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V2 vip

=

V Where:

V2 - The effective

.-?,

"I = Vol;pe of the of

,=., ~1 I

P = Pressure in fil".er: ; f !- :: =

.01,

-- "2 6.4.2 Use an adhesive label en ':Sei :Se o#f-:

'.*. vith appre ri?.te data.

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6.4.3 Wrap the vial in Saran Wrc;, twist an.d.' secure with tape.

Trim the excess wrap.

6.4.4 The _ vial may also be labeled with'a tie vrap' label.

6.4.5 The sample is in the correct ceonetry for counting on a "erennium detector system or well counter.

,6. 5 ' charcoal cartridge 6.5.1 Fission gases are reneved fre:- Ihe char:ani c tr:ridee by sleving clean dry air through the carr-idee for 0 ci'n ::es in an aperating hood.

6.5.2 Wrap the charcoal cartridge in Saran Wrap such thr.t Se excess..

wrap is on the side of the cartridge so that the cartridge wil'1 lay flat on both the inlet and outlet sid e s.

6.5.3 Secure the Saran wrap with te-e and trim the excesn' rap.

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6.5.4-The cartridge may be labeled with a tie wrap label.

6.5.5 The sample is in the correct geometr$. for count ing

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.t ' Germanium detector system or well enunter.

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~ 2 T.*l.T NUC1 AR STATION CHEMISTRY INSTRUCTION 7itie:

Sample Preparetion No.:

08-S-04-14 Revision:

1 lPoge:

6 3

i for Counting l

(

i.6 1-Dram Vial 6.6.1 Transfer 2 ml of sample to a' clean 1 dram vial, secure the cap and clean the outside of the vial.

6.6.2 ' Use an adhesive label to Icbel the vial with the appropriate data.

6.6.3 Wrap the vial in Saran Wrap, twist and secure with tape.

Trim the excess wrap.

6.6.4 The vial may also be labeled with a tis wrap label.

6.6.5 The sample is in the correct geometry for counting on a well counter or Germanium detector sys tem.

i 6.7 Planchet 6.7.1 Beta Counting a.

Clean the planchet with reagent grade acetone.

After cleaning, handle' the planchet with forceps or tongs.

b.

Sparingly apply silicone grease to 'the edge of the planchet to prevent migration of the sample during evaporatien.

c.

Transfer' approximately 2 =1 cf sample to the planchet.

d.

Add 3 to 4 drops cf insulin or NaOH (IN) to reduce the sur f a c,e tension.

e.

Place the planchet in an infrared drying oven.

f.

As the sample evaporates, additional sample may be added to the planchet until all of the required sample has been trans ferred to the. planchet.

Record the total volume of liouid that is evaporated as the sample volume.

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GRAND CULF NUCLEAR STATION CHEMISTRY INSTRUCTION Iitle:

Steple Preperation No.:

08-S-04-14 Revision:

1 lPage:

7 for Counting g.

Add the appropriate volume of Na7 SO4 (100mg/ml) to the planchet to bring the total solid on the planchet to approximately 100 mg.

The Na2 SO4 is added to give each sample a uniform self absorption.

h.

Evaporate to complete dryness exercising care not to overheat and splatter the sample.

i.

Remove the sample from the infrared even and allow to cool to room temperature.

3 j.

The planchet should be stored ~ in a ' labeled plastic Petri Dish.

I k.

For counting in a beta detector, the planchet should be removed from the Petri Dish with forceps or tongs.

1.

For counting on a Germanium detector system or well counter, the planchet should be.left in the plastic Petri Dish.

6.7.2 Alpha Counting a.

Clean the planchet with reagent grade acetone.

After cleaning, handle the planchet with forceps or tongs.

b.

Transfer approximately 2 ml of clear sample (e.g., reactor water, demineralized water) to the planchet, c.

Place the. planchet in, an infrared drying oven.

d.

As the sample evaporates, additional sample may be added to the planchet until all of the required sample has been transferred to the planchet.

Record the total volume of liauid that is evaporated as the sample volume.

e.

Evaporate to complete dryness, exercising care not to overheat the sample.

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' GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Semple Preparation No.:

08-S-04-14 Rcvision:

1 lPege:

8 for Counting I

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f.

Remove the sample from the inf rared oven and allow to cool to room temperature.

g.

The planchet should be stored in a plastic Petri Dish.

h.

For counting on an alpha detector, the planchet should be removed from the Petri Dish with forceps or tongs.

6.8 Filter Papers - 47 mm Diameter 6.8.1 Using fo r cep s, transfer the 47mm filte'r paper (e.g. Millipore, anion paper, cation paper, particulate filter) to a plastic Petri-

' Slide.

I 6.8.2 se an adhesive Imbel to label the Petri-Slide with the appropriate information.

6.8.3 The sample is in the correct geanatry for counting on a Germanium detector system or well counter.

6.8.4 For counting in a beta detector, the filter mus t - be removed from the Petri-Slide and placed on a clean filter to prevent the beta counter from becoming contaminated.

6.c. Whatman 542 Filter 6.9.1 Ga==a Counting

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a.

Draw diaFonal lines on the mounting ' card to facilitate centering of sample.

b.

Label the mounting card with the appropriate information.

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c.

Place the Whatman 542 filter at the intersection of the l

diagonal lines.

t d.

Cover the filter with 2 inch transparent tape.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Sc=ple Preparation-No.:

08-S-04-14 Rsvision:

1 Psge:

9 for Counting I

(

r e.

The sample is in the correct geometry for counting on a Germanium detector system.

f.

If counting is required on the well counter, the sample card must be trimmed, rolled and placed in a 1 dram vial.

Exercise care to keep the sample sealed while trimming the sample card.

6.9.2 Beta Counting a.

Label the underside of the mounting card with the appropriate information.

b.

Af fix a piece of two-sided tape,to the mounting card.

I c.

If the sample is to undergo further chemical treatment at a later time, (i.e., SR-90 analysis) place a piece of paper on the two-sided tape.

d.

Place the Whatman 542 paper on the center of the mounting card with the precipitate side up.

Cover the sample with Mylar film and seal to the two-sided e.

tape.

See Figure I for an illustration.

NOTE Back the Mylar film with a damp tissue to eliminate static charge on the film.

f.

Trim the mounting card to fit into a plastic Petri Dish.

Do not cut into the optional paper backing if used.

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Label the Petri Dish with the appropriate information t

h.

The sample is in the correct geometry for counting on the Germanium detector system or well counter.

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GRAND ClfLF NUCLEAR STATION CHEMISTTsY INSTRUCTION

Title:

Scmple Preparation No.:

08-S-04-14 Rcvisien:

2 lPcge:

10 l

l for Counting

[

i.

For counting in a beta detector, the sample must be removed from the Petri Dish and placed in the detector, sample side up.

6.10 Liquid.Scintillationyial 6.10.1 Add 10 n1 of scintillation solution to a clean vial.

6.10.2 Transfer 1.0 ml of the sample for all isotopes, other than Fe 55, to the vial containing the scintillation solution.

For Fe 55, transfer the organic layer from the sample (

5 ml) to the vial.

6.10.3 Secure the cap and clean the outside of the vial.

I 6.10.4 Label the cap with the appropriate information.

6.10.5 The sample is' in the correct geometry "for counting in the liquid scintillation counter.

6.11 Gas Marinelli Beakers 6.11.1 Label the Marinelli beaker lid appropriately.

6.11.2 The sample is in the correct geometry for counting on a Germanium detector sys tem.

7.0 DOCL' MENTATION / CORRECTIVE ACTION Document results on proper reporting forms as per Chemistry Procedure 08-s-03-3, Document Control.

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CRAND C'JLF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Scmple Preparation No.:

08-S-04-14 Revis ion:

1 Page:

11 for Counting

(

FILTER PAPER - MOUNTING ILLUSTRATIONS Figure 1 TOP VIEW Paper cr Cartboard Eac?.inc

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