ML20080E139

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Rev 1 to Procedure 08-S-04-320, Chemistry Instruction: Development & Use of Calibr Curves for Boron Determinations Using Fluoroborate Electrode,Safety Related
ML20080E139
Person / Time
Site: Grand Gulf  Entergy icon.png
Issue date: 09/10/1982
From:
MISSISSIPPI POWER & LIGHT CO.
To:
Shared Package
ML20080E069 List:
References
08-S-04-320, 8-S-4-320, NUDOCS 8308300741
Download: ML20080E139 (8)
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Text

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b o *e PLANT OPERATIONS MANUAL Voltme 08 08-S-04-320

,_ Section 04 Revision: 1 .

Date: 9-10-82

_ CHEMISTRY INSTRUCTION DEVELOPMENT AND USE OF CALIBRATION CURVES FOR BORON DETERMINATIONS USING THE FLUOR 0 BORATE ELECTRODE l SAFETY RELATED l

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Development & Use of Calib. Cur. No.: 08-S-04-320 Revision: 1 Page: 1 for Baron Deter. Using the Fluoro. Elec.

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1.0 PURPOSE The purpose of this Chemistry Instruction is to provide directions for the development and use of calibration curves for boron determinations using the fluoroborate electrode. This instruction pertains to boron concentrations from 50 ppb to 1000 ppe.

2.0 REFERENCES

2.1 Orion Research, Instruction Manuals; Fluoroborate Ion Electrode, Model 93-05 and Reference Electrode, Model 900200 2.2 Chemistry Procedure 08-S-03-1, Qualification of Chemistry Program 2.3 Chemistry Instruction 08-S-04-109, Operation of Orion 701 Ion Analyzer 2.4 Chemistry Instruction 08-S-04-401, Baron Standard 2.5 Chemistry Instruction 08-S-04-443, Acetate Buffer Solution and Filling Solution used With the FSIE and Double Junction Reference Electrode 2.6 U.S. NRC Document Number 50-341, Suitability Evaluation of Post-Accident Chemistry Analysis Procedures I 3.0 DEFINITIONS None 4.0 PREREQUISITES 4.1 Apparatus Required 4.1.1 Fluoreborate electrode 4.1.2 Double junction reference electrode 4.1.3 p4/mV meter I -- .. .

GRAND GULF NUCLEAR STATION CliEMISTRY INSTRUCTION ' ,

l Tic 10: Devalopment & Uso of Calib. Cur. No.: 08-S-04-320 Revisica: 1 Prgs: 2 lfor Boron Deter. Using the Fluoro. Elec.

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4.1.4 Beakers, various sizes -)

4.1.5 Microsample dish 4.1.6 Magnetic stirrer 4.1.7 Stirring bars and/or wires 4.1.8 Pipettors, various sizes 4.1.9 Pipet tips, various sizes 4.2 Reagents Required 4.2.1 10, 100, 1000, and 10,000 ppe Boron standards 4.2.2 Acetate buff fer solution (0.05 N sodium hydroxide 0.10 M glacial acetic acid) 4.2.3 10.0N sulfuric acid (H SO4) 2 4.2.4 Sodium fluoride, saturated 4.2.5 Water, domineralized

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5.0 PRECAUTIONS When in continuous use, the outer solution (acetate buf fer solution) of the double junction electrode must be changed every four (4) hours and the verification card attached to the instrument must be initialed when done.

Daily change out is acceptable when not in continuous use.

6.0 INSTRUCTIONS 6.1 Determination of a Calibration Curve NOTE Two types of curves are presented, however, it is necessary to generate

[ only that curve which represents the method by which the sample will be analyzed.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION * ,

Titlo: Devalcpment & Uso of Calib. Cur. Na.: 08-S-04-320 Rsvisica: 1 Pcga: 2 for Boron Deter. Using the Fluoro. Elec.

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4.1.4 Beakers, various sizes 4.1.5 Microsaeple dish 4.1.6 Magnetic stirrer 4.1.7 Stirring bars and/or wires 4.1.8 Pipettors, various sizes 4.1.9 Pipet tips, various sizen 4.2 Reagents Required 4.2.1 10, 100, 1000, and 10,000 ppe Boron standards 4.2.2 Acetate bufffer solution (0.05 M sodium hydroxide 0.10 M glacial acetic acid) 4.2.3 10.ON sulfuric acid (H SO4) 2 4.2.4 Sodium fluoride, saturated 4.2.5 Water, domineralized

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5.0 PRECAUTIONS When in continuous use, the outer solution (acetate buffer solution) of the dcuble junction electrode must be changed every four (4) hours and the verification card attached to the instrument must be initialed when done.

Daily change out is acceptable when not in continuous use.

6.0 INSTRUCTIONS 6.1 Determination of a Calibration Curve NCfrE j Two types of curves are presented, however, it is necessary to generate only that curve which represents the method by which the sample will be analyzed.

GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

.Iitle: Development & Use of Calib. Cur. No.: 05-5-04-320 Revision: 1 Page: 3 Ifor Boron Deter. Using the Fluoro. Elec.

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1 *b 6.1.1 Assure that the rubber washer is in place on the threaded insert of the fluoroborate sensing module, the sensing module is finger tight and the electrode has been shaken down in the manner of a clinical thermometer to ensure electrical continuity.

6.1.2 Verify that the outer solution (acetate buffer solution) of the double junction reference electrode has been changed and the inner

. solution is at the required level (at least 1 inch above the level +

of the outer chamber filling solution).

6.1.3 Ensure that start-up of the Orion 701-A Ion analyzer was done in accordance with Reference 2.3.

( 6.1.4 Verify that a functional check was performed within the proper i time frame as stated in the Calibration Functional Check Log Book.

l 6.1.5 If the Orion 605 electrode switch is used, select the channel j corresponding to the electrode to be used and ensure electrode switch is energized.

6.1.6 Lower the selective ion and reference electrode into a beaker '

( containing domineralized water.

6.1.7 Macro-volume calibration curve.

NOTE Calibration curves using other volumes may be generated simply by adjusting, porportionately, the volumes of saturated sodium fluoride, and the 10 N sulfuric acid.

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a. Pipet 10 ml of the desired boron standard into a 50 mi beaker containing a stirring bar or wire.
b. Place the beaker on a magnetic stirer and start the stirrer.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION ,

Titlo: Devolopment & Uso of Calib. Cur. No.: 08-S-04-320 Revisicn: 1 Pcgs: 4 l for Baron Deter. Using the Fluoro. Elec. I e

c. For each 10 al of solution use:

(1) 2 al of saturated sodium fluoride in step 6.1.7d.

(2) 1 at of 10 N sulfuric acid in step 6.1.7e.

d. Add the sodium fluoride.
e. Start a timer or note the time while addint the sulfuric acid, and allow the solution to stir for 15 minutes after the sulfuric acid is added.
f. Into another 50 mi beaker containing a stirring bar or wire, pipet 10 ml of acecate buf fer solution.

NOTE Larger volumes of acetate buffer solution may be used, but calibration curves using larger volumes must be generated separately.

g. Rinse the fluoroborate and reference electrodes with domineralized water, lower the electrodes into the buffer solution, and start the stirrer.

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Do not change the stirring speed of the buffer solution during the generation of the calibration curve or during analyses.

h. At 15 minutes from step 6.1.7e. , stop stirring the boron standard.
i. Set the pH/mV meter to mV.
j. Pipet 0.05 al of the boron stanadard into the acetate buffer solution,
k. Allow the mV readings to stabilize, then record the reading.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION

Title:

Developement & Use of Calib. Cur. No.: 08-S-04-320 Revision: 1 Page: 5 fdr Boron Deter. Using the Fluoro. Elec.

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1. Using increasing volumes of the boron standard, repeat steps 6.1.7j. and k over the range desired.

Example:

PFM BORON STANDARD 10 100 1000 10,000 ist addition of 0.05 a1 = 0.05 ppe 0.5 ppe 5.0 ppe 50 ppm 2nd addition of 0.10 ml = 0.15 ppm 1.5 ppa 15.0 ppm 150 ppe 3rd addition of 0.10 ml = 0.25 ppm 2.5 ppm 25.0 ppm 250 ppm 4th addition of 0.25 a1 = 0.50 ppe. 5.0 ppe 50.0 ppm 500 ppe '

m. Using standard 3 cycle seuilogarithmic graph paper, plot the a7 readings along the K-axis and the concentrations along the Y-axis.

6.1.8 Micro-Volume Calibration Curve

a. Prepare dilutions of the boron standard encompassing the expected concentrations of the sample (s) to be analyzed.
b. Starting with the lowest concentracions, pipet 0.25 al of the boron standard into a microsample dish.

( c. Add 0.05 al of saturated sodium fluoride and agitate.

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d. Add 0.025 al of 10 N sulfuric acid and agitate. i
e. Note time and allow 15 minutes reaction time.
f. After 15 minutes have passed, pipet 0.5 al of the acetate buffer solution into the micro dish and mix carefully.
g. Rinse the fluoroborate and reference electrodes in damineralized water.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION Titlot Devalcpment & Us3 of Celib. Cur. Ns.: 08-S-04-320 RGvisien: 1 Pcg3: 6l Ifor Borou Deter. Using the Fluoro. Elec. ,.

h. Lower the fluoroborate and reference electrodes into the solution,
i. Allow the reading to stabilize, then record the mV value.
j. Repeat steps 6.1.8b. through 6.1.81. until all standards are processed.
k. Do step 6.1.7m.

6.2 Sample Analysis 6.2.1 Based on the expteted boron concentration of the sample, select the method by which the analysis will be performed according to step 6.1.7 or 6.1.8 of this procedure.

6.2.2 Select a standard with a boron concentration approximating the expected concentration of the diluted or undiluted sample.

6.2.3 Process the sample along with the standard, but after adding the sulfuric acid to the standard, allow 1 to 2 minutes to elapse before adding the sulfuric acid to the sample.

6.2.4 Proceed as follows:

a. If step 6.1.7 was selected, treat the standard and sample according to steps 6.1.7 through 6.1.7i. , then pipet the

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desired aliquot into the acetate buf fsc solution and lower the electrodes into the solution.

b. If step 6.1.8 was selected, pipet 0 25 al of standard and sample into microsample dishes, then treat the standard and saeple according to steps 6.1.8c. through 6.1.8h.

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GRAND GULF NUCLEAR STATION CHEMISTRY INSTRUCTION tTitle: Development & Use of Calib. Cur. No.: 05-S-04-320 Revision: 1 Page: 7

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Boron Deter. Using the Fluoro. Elec.

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NdrE The following step (6.2.5) is used only for measuring the '

Boron standard and adjusting the mV reading to the standard's value.

6.2.5 Allow the mV reading to stabilize, then adjust the mV reading to J the specific value of the standard's known concentration, as taken from the most recent calibration curve.'

j 6.2.6 Remove the electrodes from the standard, rinse them with domineralized water, then at exactly 10 minutes af ter adding the sulfuric acid to the sample, lower the electrodes into the sample solution and allow the reading to stabilize.

6.2.7 Record the mV reading.

6.2.8 Convert mV to ppe boron, using the calibration curve.

7.0 DOCUMENTATION / CORRECTIVE ACTION Document results on appropriate reporting forms as per Chemistry Procedure 08-S-03-10. Process completed forms in accordance with Chemistry Procedure g- 08-S-03-3.

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