ML17341A687
| ML17341A687 | |
| Person / Time | |
|---|---|
| Site: | Turkey Point  |
| Issue date: | 10/03/1978 |
| From: | FLORIDA POWER & LIGHT CO. |
| To: | |
| Shared Package | |
| ML17341A684 | List: |
| References | |
| NC-82, NUDOCS 8112080212 | |
| Download: ML17341A687 (5) | |
Text
FLORIDA POWER
& LIGHT COMPANY TURKEY POINT UNITS 3 AVD 4'UCLEAR CHEMISTRY PROCEDURE NC-82 OCTOBER 3 1978
1.0 Title
DETERMINATXON OF CHLORIDE IN AQUEOUS SOLUTION'S
\\
2.0 A
royal and List of Effective Pa es:
MERCURHKTRXg TXTRA'ZXON 2.1 Review and A rov 1:
Consultant Consultant Radiochemist
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Tech Supv 'i '.
gr Plt Supt Nuc e gQ++ /~i o r,
Cgx Date Date Date Date Approved by P ant Nucle Safety Committee Date October 2.2 List of Effective Pa es:
~Pa e Date 10/3/78
~Pa e Date 2
10/3/78
~Pa e
Date 10/3/78 3.0
~3co e:
Technical Specifications Table 4.1-2 requires the monitoring of reactor-cool'ant samples for chloride (5/wk).
In addition, Cl is monitored in both primary and secondary systems and their auxiliarie's to insure a high degree of purity and to monitor the effects of transient conditions such as condenser inleakage, etc.
3.2
~Put oee:
The purpose of this procedure is to provide laboratory personnel with an approved standardized method for the determination of low level chloride ion concentration in aqueous solutions.
3.3 Acce tance Criteria:
The Cl limit in the reactor coolant system is 0.15 ppm.
The minimum sensitivity for this titration is 0.05 ppm Cl r<l
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4.0 Xns true tions:
NOTE:
Refer to the lab booklet on preparation of reagents for a listing of reagents used and their prepare'tions.
8ii20802i2 Bii202'I PDR ADDCK 05000250 P
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DETERMINATION NUCLEAR CHEMISTRY PROCEDURE NC 82 ~
PAGE 2
OF CHLORIDE IN A UEOUS SOLUTIONS - MERCURIMETRIC TITRATION 78
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4.1 Use of 4.1.1 the rea ent blank:
A reagent blank is utilized in this procedure to compensate for the effects and possible minor'impurities of the reagents used.
The reagent blank consists of a portion of Cl free water that is otherwise representative of the sample to be analyzed.
{i.e.,
demineralizer water is used as a, reagent blank for RCS, makeup water tanks, condensate, steam generators, etc.
For CCW, a Cl-free sample of water containing approximately the same concentra'tion of, potassium, chromate should by used.)
'4.1.2 A reagent blank should be titrpted just prior to the sample, by the same analyst titrating the'sample.
However, whenever numerous samples a>>qe analyzed for Cl during the day, it is only necessary to have the reagent blank analyzed once per day by each analyst performing the test.
Determine a new reagent blank whenever reagents are renewed or contamination of reagents is suspected.
4.2 Test Procedure Cl
{0-1.0 m):
4.2.1.Transfer 100 ml of colorless sample and 100 ml of colorless reagent blank into a container suitable for'titrating.
4.2.2 To each of the containers add 8-10 drops of. chloride indicator.
(Diphenylcarbazone br'omophenol blue) 4.2.3 Following addition of the indicator, the sample should be a shade of blue, violet, or red. If a yellow or orange color develops, refer to ASTM procedure D-512.
4.2. 4 4.2.5 4.2.6 4.2. 7
- To 'each container add 0
- .3% nitric acid dropwise while stirring until a pale yellow color develops, then add approximately 1 ml excess acid.
. Carefully, -titrate each sample with 0.0141N mercuric nitrate using a microburrette'graduated in.01 ml increments.
The end point is reached when a pale violet color persists. 'oth "the blank and sample should be titrated to an identical shade of violet.
'I;>>
Not'e the number of milliliters of mercuric nitrate used for each titration.
.If the final burrette level is between graduatio'nk,,
read to the nearest
.005 ml.
4.2.8
'Subtract the amount (ml) of mercuric.nitrate used to titrate the. blank from the amount
{ml) of mercuric nitrate used to titrate the sample.
Multiply the difference by 5 to obtain the concen-tration of Cl in ppm.
Report Cl 'concentration to a minimum sensitivity of.05 ppm. If less than.05, report as <0.05 ppm.
4.3 Test procedure Cl..(>1.0 m)
4.3.1 Follow the procedure; 4.2 above except that titration of the sample should be performed rapidly at first.
As the endpoint is neared, the titration rate should be slowed.
The endpoint is reached when a pale violet color persists.
a.
Use of"a larger" volume..burrette in place of the:microbuirette
(.01 ml graduations)" should be considered for obtaining more rapid. results..
I
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NUCLEAR CHEMISTRY PROCEDURE NC-82, PAGE 3
DETERMINATION OF CHLORIDE IN A UEOUS SOLUTIONS - MERCURIMETRIC TITRATION 10/3/78 4.3.2 For very high concentrations of chloride
(>50 ppm), volumetric dilution of the samples should be considered.
Multiply the results obtained in step 4.2.8 by the appropriate dilution factor to obtain the final results.
4.4 Removal of Interferences:
4;.4'.1 'urbid samples should be filtered to remove '.suspended materials prior to analysis.
4.4.2 Removal of chromium from systems such as component cooling water can be accomplished as follows:
a.
Transfer a quantity of sample and reagent blank into separate containers, such that 100 ml of, colorless sample will be available for analysis.
b.
Add two scoops of barium nitrate to each of the containers and mix well.
c.
The resulting barium chromate can now be separated by centrifuging or filtration.
J d.
Use the resulting colorless solutions for reagent blank and samples.
4.4.3 For removal of interferences other than those normally encountered, refer to ASTM procedure D-512.
4-5
.Cl Concentration in solutions containing concentrated boric acid (i.e.
BASTs):
4.5.1 Samples of solutions containing concentrated boric acid are diluted such that crystalization of boric acid will not occur at room temperature.
4.5.2 Immediately after sampling, transfer 25 ml of concentrated boric acid sample into a suitable container.
Dilute to 100 ml with demineralized water.
4.5. 3 Perform the titration and calculations in accordance with 4.2 or 4.3 above.
4.5.4 Multiply results obtained in 4.5.3 by 4 to account for. the dilution factor and to obtain Cl concentration.
The minimum sensitivity achievable is 0.2 ppm.