ML20080P452

Change 0 to Procedure CP/O/B/8100/52, Chemistry Procedure for Determination of Sodium - Furnace Aa

ML20080P452
Person / Time
Site:	Catawba
Issue date:	11/14/1983
From:	Cox J, Evans L, Painter R DUKE POWER CO.
To:
Shared Package
ML20080P419	List: ML20080P417 ML20080P421 ML20080P430 ML20080P443 ML20080P446 ML20080P449 ML20080P452 ML20080P460 ML20080P466 ML20080P469 ML20080P485 ML20080P488 ML20080P498 ML20080P505 ML20080P518 ML20080P526 ML20080P531 ML20080P535 ML20080P547 ML20080P549 ML20080P554 ML20080P561 ML20080P569 ML20080P575 ML20080P578 ML20080P586 ML20080P590 ML20080P598 ML20080P602 ML20080P605
References
CP-O-B-8100-52, NUDOCS 8402220549
Download: ML20080P452 (9)

Text

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Form 34731 (10-81)

(Formerly sod-1002-1)

DUKE POWER COMPANY (1) ID No:CP/0/B/8100/52 PROCEDURE PREPARATION Change (s) c> to PROCESS RECORD b Incorporated (2) STATION: Catawba (3) PROCEDURE TITLE: Cheristrv Procedure for the Deterrinntion of Sodium -

Furnace AA (4) PREPARED BY: ) DATE: //!/V![2 (5) REVIEWED BY: DATE: //-s )"-/.3 Cross-Disciplinary Review By:  : ,(

4 TEMPORARY APPROVAL (IF NECESSARY):

By: (SRO) Date:

By: . Date:

(7) APPROVED BY: W- Date: 1)!/ $3 (l

//

(8) MISCELLANEOUS:

Reviewed / Approved By: Date:

Reviewed / Approved By: Date:

MASTER FILE e

l

r-Form 34634 (4-81) SPD-10012 DUKE POWER COMPANY NUCLEAR SAFETY EVALUATION CHECK LIST (1) STATION: Catawba UNIT: 1 2 3 OTHER: Shared (2) CHECK LIST APPLICABLE TO: CP/0/B/8109/52 (3) SAFETY EVALUATION - PART A The ite:r to which this evaluation is applicable represents:

Yes No / A change to the station or procedures as described in the FSA or a test or experiment not described in the FSAR?

If the answer to the above is "Yes", attach a detailed description of the item being evaluated and an identification of the affected section(s) of the FSAR.

(4) SAFETY EVALUATION - PART B Yes No Will this item require a change to the station Technical Specifications?

If the answer to the above is "Yes," identify the specification (s) affected and/or attach the applicable pages(s) with the change (s) indicated.

(5) SAFETY EVALUATION - PART C As a result of the item to which this evaluation is applicable:

Yes No Will the probability of an accident previously evaluated in the FSAR be increased?

Yes No / Will the consequences of an accident previously evaluated i

in the FSAR be increased?

Yes No May the possibility of an accident which is different than any already evaluated in the FSAR be created?

Yes No Will the probability of a malfunction of equipment important to safety previously evaluated in the FSAR be increased?

Yes No /Willtheconsequencesofamalfunctionofequipment important to safety previously evaluated in the FSAR

!, be increased?

Yes , No f May the possibility of malfunction of equipment important to safety different than any already evaluated j / in the FSAR be created?

Yes No Will the margin of safety as defined in the bases to any Technical Specification be reduced?

If the answer to any of the preceding is "Yes", an unreviewed safety l question is involved. Justify the conclusion that an unreviewed safety question is or is not in olved.< Attach additional pages as necessary.

(6) PREPARED BY: A , -

DATE: h/ P_3 _

(7) REVIEWED BY: d ) C h" DATE: M-/ V /3 (8) Page 1 of /

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Form 18855 (3-80)

DUKE POWER COMPAhi ALARA EVALUATION CHECKLIST (1) Station Catawba Unit: 1 2 3 Other: Shared (2) Checklist Applicable to: CP/0/B/8100/52 (3) ALARA Evaluation Check those items below which were considered applicable during the preparation and review of this document.

Flushing and draining were used to minimize source - strength and con-tamination levels prior to performing an operation.

Permanent and/or movable shielding was specified for reduction of levels.

Use of permanent or temporary local exhaust ventilation systems was used for control of airborne contamination.

Operation was designed to be completed with the least practicable time spent in the radiation field.

Appropriate tools and equipment were specified for the operation to be performed.

The operation was designed considering the minimum number of people necessary for safe job completion.

Remote handling equipment and other special tools were specified to reduce external dose.

Contamination - control techniques were specified.

The operation was designed to be conducted in areas of as low an exposure as practicable.

Additional ALARA considerations were:

/ ALARA Principles were not considered since the procedure did not involve work in a radiation area.

(5) Prepared by: / / Date ///#![7 (6) Reviewed by: Date // ~/M3

CP/0/B/8100/52 DUKE POWER COMPANY CATAWBA NUCLEAR STATION CHEMISTRY PROCEDURE FOR THE DETERMINATION OF SODIUM - FURNACE AA .

1.0 DISCUSSION 1.1 Scope This procedure describes the determination of sodium by furnace atomic absorption spectroscopy.

1.2 Principle Refer to CP/0/B/8100/41.

1.3 Precision and Interferences 1.3.1 The precision and accuracy of this procedure will be determined by Quality Control Chart, data.

1.3.2 This procedure is applicable for sodium concentrations in the range of approximately 0.5 ppb to 8 ppb. Samples of higher concentration should be diluted into this range with cation polished water or Super-Q water.

1.4 Limits and Precautions 1.4.1 The limits and precautions given in CP/0/B/8100/41 should be followed.

1.4.2 Every effort should be made to minimize contamination when analyzing metals in the ppb range.

1.4.3 All volumetric flasks, pipet tips, and sample cups should be stored in - 10% HNO 3 and rinsed thoroughly with cation-l polished water or Super-Q water immediately prior to use.

2.0 APPARATUS l 2.1 Perkin-Elmer Model 4000 Atomic Absorption Spectrophotometer with HGA 500 Furnace and AS-40 Autosampler 2.2 Sodium hollow cathode lamp 2.3 Nalgene volumetric flasks 2.4 Eppendorf pipets

CP/0/3/8100/52 Paga 2 of 6

. 2.5 Sample cups for autosampler 2.6 Argon -

3.0 REAGENTS 3.1 Sodium Stock Solution (1000 ppm Na) _

3.1.1 1000 ppm Sodium Reference Standard Solution (e.g. Fisher Atomic Absorption Reference Standard Solution)

Alternately, a 1000 ppm sodium stock solution can be prepared by adding 2.5419 1 0.0010 grams of oven dried

(~ 1 hr. @ ~ 105'C) sodium chloride (Nacl) to a 1000 ml volumetric flask and diluting to volume with cation-polished water or Super-Q water.

3.2 Sodium Standard Solution 3.2.1 1 ppm Sodium Pipet 100 microliters of the 1000 ppm Na stock solution (Section 3.1) into,a 100,m1, acid washed, nalgene volumetric flask. Dilute to volume with cation-polished

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water or Super-Q water. This standard should be prepared

, weekly.

3.2.2 8 ppb Sodium Pipet 800 microliters of 1 ppm Na standard solution into a 100 m1, acid washed, nalgene volumetric flask and dilute to volume with cation-polished water or Super-Q water.

This sample should be prepared daily.

3.2.3 5 ppb Sodium Pipet 500 microliters of 1 ppm Na standard solution into a 100 m1, acid washed, nalgene volumetric flash and dilute to volume with cation polished water or Super-Q water.

This standard should be prepared daily.

3.3 Cation-Polished Water and Super-Q Water Cation polished water and Super-Q water should have a resistance in excess of 13 megohms.

4.0 PROCEDURE 4.1 Sample Collection 4.1.1 Samples should be collected in nalgene bottles which have been stored filled with - 10% HNO . The sample bottles must be rinsed thoroughly with cation polished water or Super-Q water prior to sampling.

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'CP/0/B/8100/52 Page 3 of 6

. 4.1.2 The sample should be analyzed as soon as possible after collection but within 6 hours6.944444e-5 days <br />0.00167 hours <br />9.920635e-6 weeks <br />2.283e-6 months <br />.

4.1.3 The sample should be shaken well immediately prior to pouring it into the sample cup. I 4.2 Insnur.:ent Setup ,

4.2.1 Spectrophotometer Turn on instrument and optomize lamp alignment per Section 4.1 of CP/0/B/8100/41. The correct wavelength for sodium is 589.5 nm and the correct slit setting is 0.7 nm. .

4.2.2 Autosampler 4.2.2.1 Press " STANDBY" to take the autosampler out of the standby mode.

4.2.3 Furnace 4.2.3.1 Press " STANDBY" to take,the furnace out of standby.

4.2.3.2 Press "130" and " TEMP".

4.2.3.3 Press "6" and " RAMP TIME".

4.2.3.4 Press "20" and " HOLD TIE".

4.2.3.5 Press " STEP" to advance to Step 2.

4.2.3.6 Press "900" and " TEMP".

4.2.3.7 Press "S" and " RAMP TIE".

4.2.3.8 Press "20" and " HOLD TIME".

4.2.3.9 Press " STEP" to advance to Step 3.

4.2.3.10 Press "2000" and " TEMP".

4.2.3.11 Press "0" and " RAMP TIE".

4.2.3.12 Press "5" and " HOLD TIE".

4.2.3.13 Press "-5" and " REC".

4.2.3.14 Press "-1" and " READ".

4.2.3.15 Press "50" and " INT FLOW".

4.2.3.16 Press " STEP" to advance to Step 4.

CP/0/B/8100/52 Page 4 of 6 4.2.3.17 Press "2500" and " TEMP".

4.2.3.18 Press 1" and " RAMP TIME".

4.2.3.19 Press "2" and " HOLD TIME".

4.2.3.20 If you wish to check your eptries, press

" CHECK". Then press the appropriate ster number and " STEP". Then press the key for tha parameter you wish to check.

EXAMPLE: If you wish to check the entry you made for ramp time on Step 2, press

. " CHECK", "2", " STEP", and " RAMP TIME".

To exit the check mode, press " CHECK". Then press "1", "SIEP" to return to Step 1.

4.2.4 Ensure that a standard graphite tube is in the furnace.

, See CP/0/B/8100/41, Section 4.3, NOTE.

4.2.5 Optical Temperature Sensor Optomize the Optical Temperature Sensor per Section 4.5 of CP/0/B/8100/41. The atomization temperature is 2000 C.

This must be done for each element.

4.2.6 Graphite Tube .

i Ensure that the graphite tube is free cf any residual sodium by performing Section 4.4 of CP/0/B/8100/41.

4.3 Sensitivity Check 4.3.1 Fill an acid washed, thoroughly rinsed sample cup with cation polished or Super-Q water and place it in the AZ slot on the sample tray.

4.3.2 Pour a portion of 8 ppb Na standard solution into an acid washed, thoroughly rinsed, sample cup and place it in the number 1 slot on the tray.

4.3.3 On the Autosampler controller:

l 4.3.3.1 Press "20" and " SAMPLE VOLUME".

. 4.3.3.2 Press "1" and "LAST SAMPLE".

t 4.3.3.3 Press " RESET" and allow the tray to reset.

4.3.3.4 Press " START /STOP".

• CP/0/B/8100/52 Page 5 of 6 4.3.4 At the end of the atomization cycle, for the 8 ppb standard observe the strip chart recorder. If the absorbence is not at least 0.15'absorbence units (15 small chart divisions),

stop the analysis. Review Sections 4.2 and 4.3 and/or call the responsible Chemistry Supervisor.

4.4 Quality Control Chart Data and Sample Analysis ,

4.4.1 Load the sample tray as follows:

Position Standard /Samule AZ Water used to make standards S1 8 ppb Na standard solution 1 5 ppb Na standard solution 2 5 ppb Na standard solution 3+ Samples (3 cups for each sample) 4.4.2 Press " RESET" on the Autosampler controller.

4.4.3 Press "AZ" on the spettrophotometer.

4.4.4 Press " MANUAL" on the Autosampler controller and allow the Autosampler to sample the AZ position twice. Then press

" MANUAL" again to stop sampling.

4.4.5 On the spectrophotometer:

4.4.5.1 Press " CONC" and " PEAK HEIGHT".

i 4.4.5.2 Press "8.0" and "S1" 4.4.5.3 Press "5" and "t" 4.4.6 On the Autosampler Controller:

4.4.6.1 Press the number corresponding to the last

l. sample and press "LAST SAMPLE".

4.4.6.2 Press "1" and "# STDS".

4.4.7. Press "AZ" on the spectrophotometer.

l 4.4.8 If the recorder is being used, press " REC MAN", re-rero the recorder (to 10 chart divisions) and press " REC MAN" again.

4.4.9 On the Autosampler controller, press " START /STOP" to initiate the analyses.

I NOTE: If the analysis has to be repeated, press

!. " ABS", " CONT", and "AZ". Then repeat j , Steps 4.4.2, 4.4.5, 4.4.7, 4.4.8 and 4.4.9.

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'CP/0/B/8100/52 Page 6 of 6 4.4.10 Read and record the results from the display on the spectrophotometer. The results from samples 1 and 2 will be the Quality. Control Chart data. Two of the three results for each sample must agree with each other within the limits of the current Quality Control Charts.

4.4.11 If the results are higher than the upper limit of the linear range given in 1.3.2, dilute with cation polished or Super-Q water and multiply the results by the dilution factor. If the results are less than the lower limit in l

1.3.2, report the results as less than that number.

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4.4.12 This analysis is subject to environmental contamination within the lab. If the results of this analysis are l higher than expected, repeat the analysis using the same sample from the original sample bottle but loading it into

-a different sample cup.

5.0 REFERENCES

, 5.1 Perkin-Elmer Model 4000 Atomic Absorption Spectrophotometer Operator's Manual 5.2 Perkin-Elmer AS-40 Autosampler Operator's M'anual 5.3 Perkin-Elmer HGA-500 Graphite Fernace Operator's Manual 5.4 Perkin-Elmer Analytical Methods for Graphite Furnace A.A.S.

6.0 ENCLOSURES None l

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