ML20058H497

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to Chemistry Instruction:Development & Use of Calibr Curves for Boron Determinations Using Fluoroborate Electrode Safety-Related
ML20058H497
Person / Time
Site: Grand Gulf  Entergy icon.png
Issue date: 06/26/1982
From:
MISSISSIPPI POWER & LIGHT CO.
To:
Shared Package
ML20058H456 List:
References
RTR-NUREG-0737, RTR-NUREG-737, TASK-2.B.3, TASK-TM 08-S-04-320, 8-S-4-320, NUDOCS 8208030596
Download: ML20058H497 (8)
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Attachmnt 1 to AECM-82/339

  • PLANT OPERATIONS MANUAL r .

Volu:ne OS 05-s-04-320 .;

Section 04 Revision: 0 Date: 6-26-82 CHEMISTRY INSTRUCTION DEVELOPMENT AND USE OF CALIBRATION CURVES FOR BORON DETERMINATIONS USING THE FLUORDEORATE ELECTRODI p SAFETY RELATED Prepared: a u , ' /~~) _

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Chemistry [RadTafion Contrcl Superintendent ,

Liit of Effectiv'e Page:

Page ,

1-7 .. _ ,, . . .

List of TC5's Incorperated:

l Revision TCH-No. ,

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8208030596 B20730 PDR ADOCK 05000416 P PDR

  • CRAND CULF NUCLEAR STATION CEEMIS~hY INSTRUCTION l71tle: Development anc use of lNo.: Ob-5-UL-320l Revision: 0lPaEe: 1l l Calibration Curves for Boron l [ l l

' Deter =inations Using the l l , l l [ .

-l Fluoroborate Electrode  ! I I l 1.0 FUEPOSE Ihe purpose of this Chemistry Instruction is to provide directions fer the Develop =ent and Use of Calibration Curves f or Soron Deter =inations Using the Fluoroborate Electrode.

2.0 REFERENCES

i 2.1 Orion Research, instruction Manuals; Fluoroborate lon Ilectrode, Model 93-05 and Reference Electrode, Model 900200 I . 2.2 Chc=istry Procedure 06-5-03-1; Qualification of Chemistry Program 2.3 Che=istry Instruction 08-S-04-109; Operation o'f Orion 701 Ion Analyzer 2.4 Che=is try Ins truc tion 05-S-04-401; boric ' Acid S tandard 2.5 che=istry Instruction 08-S-04-443; Ammonium Sulfate, Ionic Strength Adjuster (ISA) f 2.6 U.S. NRC Docu=ent No. 50-341; Suitability Evaluation of Post-Accident Che:istry Analysis Procedure .

.~.0 DEFINITIONS None.

re 4.0 PREEEQUISITES 4.1 Apparatus Required <

4 .1 :'l Tluorobcrate' electrode 4.1.2 Double junction reference electrode ~

i 4.1.3 pH/mV meter O

GRAND CULT EUCLEAR SIAT10N CHEM 197RY 1NSIRUCTAON l

Title:

Development anc Use of lNo.: Ob-S-04-320l Revision: 0lPage: 2l l Calibration Curves for Boron l ) l l

(" l Determi' nations Using the l [ .

Fluoroborate Electrode

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j' 1 l 4.1.4 Beakers, various sizes 4.1.5 Microsa=ple dish 4.1.6 Magnetic stirrer 4.1.7 Stirring bar'and/or wire i .

4.1.5 Pipettors, various sizes 4.1.9 Pipet tips, various sizes .

4.2 Rea' gents Required ,

4.2.1 100 ppm Boron Standard

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4.2.2 2.0M a=monium sulf ate, [(NH4 )2 SO4 ]

4.2:3 0.04M ammonium sulfate [NH4 )2 S04) ,

g 4.2.4 10.ON sulfuric acid (H 2SO 4) ,

4.2.5 Sod ium fluori'de, saturatec .'

L.2.6 Water, deicnized 5.0 FRICAUTIONS ,,

When in use, the outer solution [0.04N (NH4)2 SO 4 ) of the double junction electrode must be changed daily and the verification card attached

_ _ . . . to the instrument must be initialed when done. .

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GRAhDGULFHUCLEARSTATIbH CHEMIS7RY 1HSTRUCT10N l71tle: Development and Use of lNo.: 06-5-04-320l Revision: 0lPage: 3l l Calibration Curves for Boron l l r l, Determinations Using the ,

l Fluoroborate Electrode 6.0 INSTRUCTIONS 6.1 Deter =ination of a Calibration Curve NOTE Three types of curves are presented, however,3 it is neces'sary to generate only that curve which represents the method by which the sample vill be analyzed.

p 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 insure electrical continuity.

6.1.2 Verify that the outer solution [0.04M. (NH4)2 SO 4 ] of the double junct' ion reference electrode has been changee and the inner solution is at"the required level.

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 Qas pertermed within the proper

. t ime frcme as stated in the Calibratier. Functional Check Log Sook.

6.1.5 If the Orion 605 electroce switch is used, select the channel corresponding to the electrode to be used and ensure electroce

  • switch is energized.

6.1.6 Lower the selective ion and reference electrode into a beaker

. . . containing water.

6.1.7 Macro-Volume Calibration Curve (1-100 pp=)

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GRAND GULF UUCLEAR STATION CHEMISTRY INSTRUCTION l11tle: Development and Use of No.: 06-5-04-320l Revision: 0lFage: 4 l l Calibration Curves for Boron l l r' l Deternibations Using the l .

l' Fluoroborate Electrode l NOTE Calibration curves, using ether volu=es may be generated si= ply by adjusting, porportienately, the volu=es of saturated sodium fluorid., 10 N sulfuric acid and the Ionic Strength Adjuster

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(ISA). .

a. Using the 100 pp= boron standard, . pr'epare a minimum of 3 dilutions ranging from 1 to 100 ppo boron and pipet 5 ml of each dilution into appropriate sized beakers.

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b' . Place the beaker containinE the lowest concentration of boren on a magnetic stirer and start the stirrer.

c. For each 5 ml of dilution use:

(1) I'ml of satu, rated sodium fluoride in step 6.1.7(d)

(2) 0.5 ml of 10 N sulfuric acid in step 6.1.7(e)

(3) 0.1 ml of 2.0 M c==eniu= sulfate (ISA) in step 6.1.7( f)

d. Add the s'odiu= fluorice. ,
e. Start a timer or note the tice while adding the sulfuric acid.
f. At C.5 cinutes free Step 6.1.7(e), add 0.1 ml of 15A. ,,
g. At exactly 10 minutes f ro= step 6.1.7(e), stop the stirrer, lower the electrodes into the solution, read and record ,the

. . . . . mV. _ . _ . . _..

h. Repeat steps 6.1.7(b) through 6.1.7(g), until all dilutiens are processed, o

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GRARO GULT NUCLEAR STATION CHEMIS~EY INSTRUCTION lT2tle: Development enc Use of .No.: Ob-5-04-320; Aevision: 0lPage: 5 l l Calibration Curves for Boron , l Determinations Using the

(~ l i , l l ..

l- Fluoroborate Electrode i I l l

'i. Using standard 4 cycle se=ilogarithmic graph paper, plot the cV readings along X-axis and the concentrations along the Y-axis.

6.1.8 Micro-Volume Calibration curve (0.01 to-l.0 ppm)

a. Prepare a low level ISA [0.2 M (NE4)2 SO4 ) by diluting 10 ml of ISA [2.0 M INH4)2 S04 } to 100 ml' ,

of decineralized water. -

b. Dilute 10 ml of both the saturated sodium fluoride and the 10 I' ' .

N sulfuric acid .to 100 ml in demineralized water.

Using the 100 ppe boron solution an'd demincralized water, c.

prepare 100 ml of a 1 ppe boron solution.

d. Using the l ' ppm s,olution, prepare a minimum' of three 100 ml dilutions ranging from 0.01 to 1.0 ppm boren.

NOTE

'l Fresh standards cust be prepared daily.

e. Measure 5 =1 of each standaEd as per steps 6.1.7(b) through 6.1.7(h) using the dilutiens prepared in steps 6.1.6(a) anc 6.1.6(b).

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f. Do step 6.1.7(i), r 6.1.9 Micro-volume Calibration Curve .

I a. Prepare dilutions of the boron standard bracketing the expected concentrations of the sa=ple(s) to be. analyzed where 0.3 or 0.5 c1 of sa ple or sa=ple/ dilution will be analyzed.

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GRAND GULT NUCLEAR STATION CHEMISTRY INSTRUCTION lIltle: Development anc Use of [No.: Ob-S-04-320 Revision: 0lPage: 6l Calibration Curves for Boron l l l l l

( l Determinations Using the l ..

l' Fluoroborate Electrode

b. Starting with the lowest concentrations, pipet 0.3 =1 or 0.5 el of the boron standard into a cierosa=ple disk.

NOTE If 0.5 c1 of standard or standard / dilution was used, proceed to step 6'.l.9(g). ,

c. If 0.3 ml of standard was used, add 0.06 ml'of saturated sodium fluoride and 0.03 el of 10 N sulfuric acid. Start

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the timer and mix. .

Y d.

.eL At exactly 10 minutes , lowertheelectrodesintogstandard, ,

read and record the mV reading, ,

e. Repeat steps 6.1.8(c) and 6.1.S(d) until all standards are processed.' ,
f. Do step 6.1.7(i)
g. If 0.5 c1 of sample or sample / dilution was, used, do steps 6.1.8(c) through 6.1.E(f) using 0.1 21 of saturatec soolu:

fluoride and 0.5 el cf 10 N ,' sulfuric acid.

6.2 Sa:ple Anal'ysis 6.2.1 Lased on the expectec boron concentation of the sa:ple, select,;the method by which the analysis will be performed according to 611.7, 6.1.8, or 6.1.9 of this procedure.

. . 6.2,2 Select a standard with a boron concentration-approximating the expected concentration of the sample.  ;.y h

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s GF.AND GULF UUCLEAR STATlON CHEMl!7RY 1NSTRUCT10N l71tle: Development anc use ot No.: 06-5-04-320 Revision: 0lPage: 7l l Calibration Curves for Boron l l

' Determinations Using the l l l l l .,

l Ilucroborate Electrode l I I l 6.2.3 Process the. sample along with the standard, but af ter adding the sulfuric acid to the standard, allow I to 2 =inutes to elapse before addinE the sulfuric acid to the sample.

6.2.4 Proceed as follows:

a. If eithe r' 6.1.7 or 6.1.6 were selec t.ed , pipet 5 c'l of the standard into a beaker and do steps.6.1.7(b) through 6.1.7(f) using the appropriate reagents prepared for 6.1.7 or 6.1.8.
b. If 6.1.9 was selected, pipet 0.3 ml or 0.5 ml of the boron p ,

- stardard into a microsample dish and do step 6.1.9(c), if 0.3 al of standard was used, or 6.1.9(g), if 0.5 ml of standard was used.

6.2.5 At exactly.10 mi.nutes after adding'the sulfuric acid to the standard, lower the e.lectrodes into the st andard solution and adjust the mV reading to the specific value of the standard's known concentration, as taken from the most recent calibration ,

curve.

6.2.6 At exactly 10 tinutes af ter accing the sulfuric acid te the sc ple, lower the electroces ir.t.c the sa:ple solutier. anc recere the =V reacing.

.6.2.7 Convert mV te ppm boron, using the calibrstion curve.

7.0 DOCU. MENTATION / CORRECTIVE ACTION Document results on appropriate reporting forms as per Chemistry Procedure

. 06-S-03-10. Process completed forms in accordance with Chemistry Procedure 06-S-03-3.

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