ML20080P531

Change 2 to Procedure CP/O/B/8100/08, Chemistry Procedure for Determination of Silica (Manual Method)

ML20080P531
Person / Time
Site:	Catawba
Issue date:	06/29/1982
From:	Bolin C, Chaust R, Tuckman M 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-8100-08, CP-O-B-8100-8, NUDOCS 8402220573
Download: ML20080P531 (3)

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DUKE POWER COMPANY t1) ID No: ro /n /R /pinn /na PROCEDURE MAJOR CHANGE Change No: s PROCESS RECORD Permanent /R=ffg?n % Tp (2) STATION: Catawba (3) PROCEDURE TITLE: Chemistry Procedure for the Determination of Silica (Manual Method)

. (4) SECTION(S) 0F PROCEDUPI AFFECTED: 3 g 1. 3. 7. 4.1. 4 3 (5) DESCRIPTION OF CHANGE: (Attach additional pages, if necessary.)

3.6.1 Change 100 ml. to 1000 ml.

3.7 Change 1000 4 1 (1.0 mi.) to 100 ml.

4.1.4.3 Change 1 ml. to 2 ml. .

(6) REASON FOR CHANGE:

Procedure accuracy (7) PREPARED BY: M > DATE: 6/24/ 1982 (8) SAFETY EVALUATION This change:

Yes No x Represer.ts a change to the station or procedures as describec in the FSAR, or a test or experiment not described in the FSi x

Yes No Requires a change to the station Technical Specifications?

Yes No x Involves an unreviewed safety question?

If the answer to any of the above is "Yes", attach a detailed explanation.

As appropriate attach a completed " Nuclear Safety Evaluation Check List" forr..

By: hM Date: 6/24/1982 (9) REVIEWED BY: M //C [M DATE: (- / 7- [ 2.

Cross-Disciplinary Review By:

[vJM 721 (10) TEMPORARY APPROVAL (IF NECESSARY):

By: (SRO) Date:

By: Date:

(11) APPROVED BT: , '

lA C A DATE:

4

( 2.h [

(12) MISCELLANEOUS:

Reviewed / Approved By: Date:

. Reviewed / Approved By: Date:

(13) Page 1 of /

B402220573 840215 PDR ADOCK 05000413 E ' PDR Rev 14 9/20/77

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s CP/0/B/8100/08 Page 3 of 7 3.0 PIAGENTS 3.1 " Silica Free" water for Preparation of Reagents The water used for reagent preparation is to be Super Q water.

3.2 Ammonium Molybdate, 10% W/V Dissolve 20.0 0.1 gm of ammonium molybdate, (NH )6 0 7024 '0, in 200 1 5 ml of " silica free" water. Discard after 24 weeks. "

3.3 Reducing Agent Dissolve 0.50 2 0.01 gm of 1-amino-2-napthol-4-sulfonic acid (NH,3C ygH 6(OH)S0 3 H) in 50 1 ml of " silica free" water containing 1.0~1 0.I gm of sodium sulfite (Na,,S03 ). After the sulfonic acid dissolves, add the solution very sIowIy and with constant stirring to a second solution containing 30.0 ! 0.1 gm sodium bisulfite (NaHS0 )

in 100 ml of " silica free" water. Dilute to 200 5 ml with " silica 3 I

free" water. If precipitation has occured, filter the solution, at this time, through qualitative filter paper. Discard af ter two weeks.

3.4~ Oxalic Acid Solution Dissolve 15.0 0.1 gm of oxalic acid (H,C,0 2H,30) in 200 ! 5 ml of 4

" silica free" water. This solution is stable inuefinitely.

3.5 Hydrochloric Acid, 50% V/V Dilute 100 ! I ml of concentrated hydrochloric acid (hcl) by addition of the acid to 100 1 1 ml of " silica free" water. This solution is stable indefinitely.

._ 16 Silica Standard Solution, 100 ppm i A ll . ,Mk 3.6.1 100o In a Jee al nalgene volumetric flask add 46.75 ml (measured g.g with a Class A 50 ml burette) of Fisher Certified Silicon Standard (1000 ppm Si) to about 700 ml of " silica free" water and dilute to volume. This solution is stable for six months.

o NOTE: If the Certified Silicon Standard is unavailable, the 100 ppm Silica Standard Solution nay be made as per section 3.6.2.

3.6.2 Dissolve 0.4777 1 .0001 g of reagent grade Sodium Silicate (Na.,SiO3 9H,30) in approximately 700 ml of " silica free" water in 3 1000 m1 r.algene volumetric flask. Dilute to volume.

This solution is stable for six months.

3.7 Silica Standard Solution, 10 ppm

,_ j. ., A I IO8 M-

,""" g g In a 1000 ml nalgene volumetric flask, dilute '?"2 c: I ' .  : of 100

,..,7-12-72

' ppm silica standard (Section 3.6) to 1000 ml with " silica free" water.

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• _. i NOTE: Use this standard when generating a standard curve.

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CP/0/B/8100/08 Page 5 of 7 4.1.3 Preparation of Color Blank #1 To the' beaker containing the color blank add 1 ml ! .5 ml of 50% V/V hydrochloric acid followed by the addition of 2 ml ! 0.5 ml of oxalic acid. Thoroughly stir and add 2 ml

! 0.5 ml of ammonium molybdate, stir, and finally add 2 ml

! 0.5 ml of reducing agent. Stir and allow to stand until needed.

NOTE:

The oxalic acid is added before the ammonium molybdate to prevent the formation of the molybdate-silicic acid complex.

4.1.4 Preparation of standards and reagent blank #3 4.1.4.1 To the beakers containing standards and reagent blank #3, add 1 ml 0.5 nl of 50% V/V hydrochloric acid, followed by 2.0 ml ! 0.5 ml of ammonium molybdate. Mix and allow to stand for 5 minutes.

4.1.4.2 At the end of 5 minutes, add 2 ml ! 0.5 ml of oxalic acid, stir, and allow to stand for 1 minute.

A n:e A g gj fK 4.1.4.3 Add / ml 0.5 ml of reducing at it , stir, and

" g q.32 allow to stand for 10 minutes.

• .1.5 Preparation of Reagent Blank #2 4.1.5.1 To the beaker containing 45 ml of water, add double the normal volumes of reagents except for the reducing agent. Add 2 ml of hydrochloric acid, 4 ml of oxalic acid, 4 ml of ammonium molybdate and 2 ml of reducing agent.

4.1.5.2 Allow the appropriate reaction times af ter each addition as specified in Section 4.1.4.

NOTE: Reagent Blank #2 may be prepared simultaneously with the standards and l reagent blank #3.

4.2 Instrument Calibration 4.2.1 Adjust spectrophotometer to a wavelength of 815 nm.

4.2.2 Pour Color Blank #1 into a 100 mm sample cell, place in spectrophotometer, and set zero absorbance. Care must be taken to clean all cell faces with tissue paper.

4.3 Determination of Standard Curve 4.3.1 Analyze Reagent Blank #2, Reagent Blank #3, and the standards, in order of increasing concentration, using a 100 mm sample cell The sample cell is to be rinsed between each analysis with the next sample to be analyzed. Recheck zero absorbance with glor Blank #1 before each sample.