ML20128N226

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Rev 0 to CP 807/2807/3807AA, Baron Analysis
ML20128N226
Person / Time
Site: Millstone  Dominion icon.png
Issue date: 09/13/1993
From: Dauria G
NORTHEAST NUCLEAR ENERGY CO.
To:
Shared Package
ML20128N126 List:
References
CP-807-2807-380, NUDOCS 9610160327
Download: ML20128N226 (15)
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Text

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l. MIL 1 STONE NUCLEAR POWER STATION
CHEMISTRY PROCEDURE
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i Boron Analysis

! CP 807/2807/3807AA

Rev.0 l

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i Approval: kk <w Vice President - Millstone Station

! SORC Mtg. No: 93-3/o Effective Date: 9'/3- 93 9

d Level of Use Subject Matter Expert:

General Greg D'Auria 9610160327 961004 PDR ADOCK 05000245 p PDR

Millstone All Units

. . Chemistry Procedure Boron Analysis .

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TABIF OF CONTENTS l I

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1. PURPO S E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2. PREREQUISITES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
3. PRECAUTION S . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 l
4. INSTRUCTIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 4.1 Sample Analysis by Autotitrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 l 4.2 Preparation and Standardization of 0.05 N NaOH Solution for Autotitrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
5. REVIEW AND SIGNOFF . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
6. REFERENCES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
7.

SUMMARY

OF CHANGES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

, ATTACHMENTS AND FORMS Chem Form 807/2807/3807AA-1,"Borou Analysis Log Sheet" Chem Form 807/2807/3807AA-2," Boron Control Chart" I

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CP 807/2807/3807AA I Level of Use Rev. O General 1 of 14 1

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1. PURPOSE 1.1 Objective This procedure provides a method for boron analysis, for all nuclear plant applications with boron concentrations above 1.0 mg/ liter (1.0 ppm).

1.2 Discussion ,

A sample containing boric acid or borate is weighed and results are transferred to the autotitrator. Demineralized water and mannitolis then added to sample. The mannitoboric acid formed is then titrated with a standard NaOH solution to a pH of 8.5. The milliliters of titrant used is proportional to the amount of boron present in the sample.

1.3 Frequency 1.3.1 A quality control check of the method is performed dailv by analyzing a 1000 ppm boron standard.

2. PREREOUISITES 2.1 General

' 2.1.1 N/A 2.2 Tools and Consumables 2.2.1 Autotitrator 2.2.2 Collapsible container ("cubitainer")

2.23 Demineralized water ,

l 2.2.4 Dropper bottles for hcl and NaOH 2.2.5 Electronic Balance 1 2.2.6 Magnetic stirrer and teflon bars 1

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CP 807/2807/3807AA Level of Use Rev. 0 General 2 of14

2.2.7 Solutions 1000 ppm Boron Standard - Certified, vendor supplied

  • Buffer solution pH 4.00
  • Buffer solution - pH 7.00
  • pH probe reference solution 2.2.8 pH-mV meter equipped with pH clectrode 2.2.9 Plastic beaker 2.2.10 Potassium Biphthalate (KHP) 2.2.11 Reagents
  • 0.025 E Sodium Hydroxide Solution
  • 0.05 N Sodium Hydroxide Solution 0.2 H HCL

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  • 0.001 H HCL
  • 50% W/W Analytical Reagent NaOH

+ Mannitol 2.3 De5mitions 2.3.1 Potassium Biphthalate - Other common chemical names, Potassium Hydrogen Biphthalate (KHP) or Potassium Acid Phthalate (KAP) i 2.3.2 W/W - Weight per Weight l

3. PRECAUTIONS I 3.1 The exposure of a specific ion electrode to acidic or alkaline gases, sugh as HCL or NH from 3 laboratory air, can cause meter drift and error in analysis.

CP 807/2807/3807AA Level of Use Rev. 0 General 3 of 14 l

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4 3.2 When preparing a gravimetric standard of boric acid, th5 boric acid should not be heated. When boric acid is heated, it gradually loses water, changing first to meta boric acid (HBO2 ) and finally dehydrating i completely to anhydrous oxide (B2 03).

3.3 The method stored in the autotitrator must not be altered without a Chemistry Supervisor's or designee's approval. -

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h CP 807/2807/3807AA Levolof Use Rev. 0 General 4of14 s

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4. INSTRUCTIONS 4.1 Sample Analysis by Autotitrator 4.1.1 START the e.utotitrator as follows:
a. IE pH probe is being placed in service, PERFORM the .

fol'owing:

1) REMOVE protective cap from pH probe filling port.
2) CHECK reference solution level.
3) IE reference solution level is below halfway point, FILL pH probe with reference solution.
b. ENERGIZE titrator and balance.
c. PERFORM pH probe calibration as follows:
1) REMOVE titrant dispensing tip from its holder.
2) RINSE pH probe.

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3) IMMERSE probe in approximately 50 mL pH 4.00 buffer solution.
4) PRESS "pH Calib" button

,. (" Buffer A" light will blink).

NOTE When "RUN" is pressed, stirrer will start and millivolts will be displayed.

When millivolts reading is stabilized, " Buffer B" light will blink.

5) PRESS "RUN."
6) WHEN " Buffer B" light blinks, REMOVE probe from pH 4.00 buffer and RINSE probe.
7) IMA1ERSE probe in approximately 50 mL of pH 7.06 be.ffer solution.

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( CP 807p727AA Level of Use General 5 14

NOTE When "RUN" is pressed, stirrer will start. When reading stabilizes the unit will beep and the calibration will display.

8) PRESS "RUN."
9) WHEN " Buffer B" light goes out AND 3 beeps are heard, REMOVE probe from pH 7.00 buffer.
10) RINSE pH probe.
11) INSTALL titrator tip in holder.

4.1.2 CHECK pH as follows:

a. IMMERSE probe in approximately 50 mL of sample.
b. PRESS "3."
c. PRESS "pH Calib."

,. d. WHEN sample pH has stablized, PRESS " reset."

e. REMOVE sample and RINSE pH probe.

4.1.3 CONDUCT a quality control check as follows:

a. TARE a clean, dry, plastic beaker.
b. PRESS "RUN" and WAIT for weight ligP slink.
c. ADD 8 to 12 grams of 1000 ppm Bc .ndard to a clean, dry plastic beaker.
d. WHEN weight has stabilized, PERFORM the following:
1) PRESS "RUN" to enter sample weight into the autotitrator.
2) WAIT for " BUSY" light to blink.
3) RECORD sample weight on Chem Form 807/2807S97AA-1.

807/2807S807AA Levol cf Use Rev.0 General 6 of 14 s

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l e. REMOVE beaker from balance.

f' f. ADD 6 to 7 grams mannitol.

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{ g. FILL to 50 mL with demineralized water.

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h. RINSE probe. ,
i. ATTACH sample cup to autotitrator collar.
j. PRESS "RUN" to start titration.
k. ADJUST stirring rate to between 4 and 5.
1. WHEN unit beeps AHR displays boron ppm value, RECORD value and initials on Chem Form 807/2807/3807AAr-1.
m. PLOT boron ppm value on Chem Form 807/2807/3807AA-2.
n. IE Boron Control Chart on Chem Form 807/2807/3807AA-2 is new, ENTER start date.
o. IE Boron Control Chart on Chem Form 807/2807/3807AA-2 is complete, PERFORM the following:
1) ENTER end date.
2) SUBMIT Chem Form to Chemistry Supervisor or designee.
3) REVIEW data on Chem Form.

Chemisdt supav or 39"** 4) SIGN " Reviewed By."

5) RECORD title.

l Technician l" P. RECORD the following data on Chem Form 807/2807/3807AA-1.

. Sample date

  • Sample time
  • Sample type l CP 807/2807/3807AA Level of Use General $14 )

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  • Normality of titrant
  • Dilution factor
q. E the concentration of the controlis less than 990 ppm .QR

, greater than 1010 ppm, CONSULT Chemistry Supervisor to j outline corrective action.

r. REMOVE sample and RINSE pH probe.

1 4.1.4 CONDUCT a sample analysis with the autotitrator as follows:

a. RECORD the following data on i

Chem Form 807/2807/3807AA-1.

  • Sample date
  • Sample time
  • Sample type
  • Normalityof titrant
  • Dilution factor
b. MEASURE sample pH.
c. E pH is less than 4.0, ADJUST pH to approximately 5.5 using 0.025 N NaOH.
d. E pH is greater than 8.0, ADJUST pH to approximately 5.5 using one of the following:

0.001 N hcl 02SHQ .

e. TARE a clean, dry, plastic beaker.
f. PRESS "RUN" and WAIT for weight light to blink.

f CP 807/2807/3807AA Level of Use Rev.0 General 8 of14

'f NOTE i For dilute a l of solution.queous solutions,1 gram of solution is equivalent to 1 milliliter 1

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g. Refer To Table 1," Sample Size for Anticipated Boron  !

Concentrations" and ADD an appropriate volume of sample )

to beaker.

Table 1 - Sample Size for Anticipated Boron Concentrations i Anticipated Sample Sample Size Concentration, ppm grams

> 3000 0.1 - 1 1500 - 3000 4 500 - 1500 5 - 15 100 - 500 15 - 20 10 - 100 20 - 40

< 10 100

h. WHEN weight has stabilized, PERFORM the following:
1) PRESS "RUN" to enter sample weight into the autotitrator.
2) WAIT for" BUSY" light to blink.
3) RECORD sample weight on Chem Form 807/2807/3807AA-1.
i. REMOVE beaker from balance.  :

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j. ADD 6 to 7 grams mannitol.

NOTE Samples containing less than 10 ppm boron do not require addition of ,

demmeralized water.

"~! k. IE anticipated sample concentration is greater than 10 ppm, FILL to 50 mL with demineralized water.

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CP 807/2807/3807AA Level of Use J Re 0 General 1,

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1. RINSE probe.
m. ATTACH sample cup to autodtrator collar.
n. PRESS "RUN" to start titration.

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o. ADJUST stirring rate to between 4 and 5.
p. WHEN unit beeps MB2 displays boron ppm value, RECORD value and initials on Chem Form 807/2807/3807AA-1.
q. IE boron needs to be reported in different units, PERFORM the following:
1) Refer To Chem Form 807/2807/3807AA-1, page 2, and CALCULATE boron concentration in units desired.
2) RECORD boron concentration on Chem Form 807/2807/3807AA-1 in " Reported as" column. ,

4.2 Preparation and Standardization of 0.05 N NaOH Solution for Autotitrator t

4.2.1 PREPARE the 0.05 N NaOH titrating solution as follows:

a. PIPETTE 5.25 mL of 50% W/W Analytical Reagent NaOH l into 2 liter volumetric Gask.

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b. DILUTE 50% W/W Analytical Reagent NaOH to 2 liters  !

with demineralized water.

c. STORE solution in collapsible container ("cubitainer").

4.2.2 STANDARDIZE the 0.05 N NaOH titrating solution as follows:

NOTE When drying KHP i ~>en, do not exceed 6 hours6.944444e-5 days <br />0.00167 hours <br />9.920635e-6 weeks <br />2.283e-6 months <br /> of drying time. )

a. DRY KHP in oven for at least I hour.

I CP 807/2807/3807AA Level of Use Rw 0 General 9 ,1

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b. WHEN KHP has dries, 'EMOVE KHP from oven and i ALLOW to coolin desiccator, i
c. PRESS " MODE" key (The light above " CONC" will light).
d. ENSURE that 0.2042 is entered as "CONST REAG". I
e. TARE a clean, dry plastic beaker.
f. In the clean, dry, tared plastic beaker, WEIOH 0.2g of KHP.
g. To enter the mass of KHP, PRESS "RUN" key twice.
h. DISSOLVE KHP with 50 mL demineralized water. I
i. ENSURE the KHP is completely dissolved,
j. RINSE probe.
k. ATTACH sample cup to autotitrator collar.
1. To begin titration, PRESS "RUN".
m. REMOVE sample cup and RINSE probe.

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A new blank should be determined each time NaOH is standardized.

4.2.3 DETERMINE a blank as follows:

a. ADD 6 to 7 grams of Mannitol to a plastic sample beaker.
b. DILUTE to 50 mL J
c. ATTACH sample to sample attachment collar.
d. PRESS "2" and "RUN" to start stirrer.

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e. ADJUST stirring rate to between 4 and 5. ,

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f. WHEN Mannitol is completely dissolved, PRESS " RESET."
g. To light " BLANK" indicator, PRESS " MODE" key twice.

k CP 807/2807/3807AA Level of Use Rev.O j General 11 of 14 j I

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h. PRESS "RUN" key twice.
i. WHEN titration is finished, CHECK that blank is displayed.

i 4.2.4 IE NaOH has just been prepared OR difficulty is expenenced in the analysis of the control standard, PERFORM a control check )

of the normality of NaOH solution against 1000 ppm boron, standard as follows-

a. RECORD the following data and results on Chem Form 807/2807/3807AA-1. .

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  • Sample date
  • Sample time
  • Sample type

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  • Normality of titrant
  • Dilution factor
b. TARE a clean, dry, plastic beaker.

' c. PRESS "RUN" and WAIT for weight light to blink.

d. ADD 10 grams of 1000 ppm boron standard to beaker.

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e. .WHEN weight has stabilized, PERFORM the following:
1) PRESS "RUN" to enter sample weight into the autotitrator.
2) WAIT for " BUSY" light to blink.
3) RECORD sample weight on
Chem Form 807/2807/3807AA-1.
f. REMOVE be.aker from balance,
g. ADD 6 to 7 grams mannitol. ,

8 CP 807/2807/3807AA Level of Use General R2 '$'f M

NOTE Samples containing less than 10 ppm boron do not require addition of demmeralized water.

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h. IE anticipated sample concentration is greater than 10 ppm, FILL to 50 mL with demineralized water.
i. RINSE probe.
j. ATTACH sample cup to autotitrator collar,
k. PRESS "RUN" to start titration.
1. ADJUST stirring rate to between 4 and 5.
m. WHEN unit beeps and displays boron ppm value, RECORD value and initials on Chem Form 807/2807/3807AA-1.

4.2.5 COMPARE results with actual concentration of Boron standard.

4.2.6 IE the concentration of the control is less than 990 ppm OR

, greater than 1010 ppm, CONSULT Chemistry Supervisor to outline corrective action.

I f CP 807/2807/3807AA Level of Use R'

General 3fM

5. REVIEW AND SIGNOFF 5.1 The review and signoff for this procedure is located in Chem Form 807/2807/3807AA-1 and -2.
6. REFERENCES l 6.1 Baron In Water, Reactor Plant Chemistry Manual, CE NPD-28. -

6.2 Operating Instructions, Mettler DL 21 and DL 25 Titrator, Mettler Instruments AG, ME-703175.

l 6.3 CP 800/2800/3800, " Quality Control Program".

7.

SUMMARY

OF CHANGES 7.1 The content of this procedure was modified to incorporate new format criteria specified in Revision 0 of the " Millstone Procedure Writer's Guide."

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