ML20154N630

Forwards Catawba Nuclear Station 316(a) Demonstration: Chemical & Biological Characteristics of Lake Wylie,Sc, During First Yr of Operation of Units 1 & 2 of Catawba Station & Correspondence Re NPDES Permit Mod

ML20154N630
Person / Time
Site:	Catawba
Issue date:	09/20/1988
From:	Tucker H DUKE POWER CO.
To:	NRC OFFICE OF ADMINISTRATION & RESOURCES MANAGEMENT (ARM)
Shared Package
ML20154N636	List: ML20154N630 ML20154N671
References
NUDOCS 8809290363
Download: ML20154N630 (19)

Text

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1 11 l e Duke 1%cer Company llu B hse

' PO Bat 31199 nce hesident Charlotte. N C 28242 Nac' rat hvJaaron (iV4)3?.1 till DUKEPOWER September 20, 1988 Document Cc,ntrol Desk U. S. Nuclear Regulatory Commission Washington, D.C. 20555

Subject:

Catawba Nuclear Station Docket Nos. 50-413 and 50-414 Environmentil Protection Plan NPDES Permit Pursuant to the Catawba Nuclear Station Environmental Protection Plan and NPDES perait, please finds attached the Catawba 316(a) Demonstration. Additionally, please find attached correspondence between Duke Power Company and the South Carolina Department of Health and Environmental Control regarding a modification to the facility NPDES permit.

Very truly yours, fbtl0 W /pl H. B. Tucker Qiru JGT06.Dl/lcs Attachments xct (with attachment)

Dr. J. Nelson Grace Regional Administrator, Region II U. S. Nuclear Regulatory Commission 101 Marietta Street, NW, Suite 2900 Atlanta, Georgia 30323 W. T. Orders NRC Resident Inspector Catawba Nuclear Station 8809290 POR ADO 880920

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,e DUKE Powen COMPANY t PO BOX 33189  !

WILLI AM A. H ALLEA mean g

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July IS, 1968 ,

Ms. Nancy Weatherup Gauth Carolina Department of Health and Environmental Control Industrial and Agricultural Wastewate't Division l 2600 Bali Street

Ce,1umbia, South Carolina 29201 i

SUBJECT:

Catawba Nuclear Station NPDES Permit Modificaticn File: CN-702.13

. Itegarding your letter dated May 31, 1998, we concur with your reconnendation l

to modify Catawba Nuclear Station's existing NPDES Permit to include

effluent limits for Hydrazine and Ethylene Glycol. We have reviewed the

! draft modifications along with the suppcrting rationale which you provided.

4 f.isted below, please find our concents and suggestions as they pertain to

the proposed modification. The changes we have suggested are aimed at structvring the permit language to, (1) assure that our discharge is effectively monitored so as not to 1.'gact receiving waters, and (2) provide

!, additional clarification for the requirements in the permit.

RATIONA.E l

Section 4.B.5. - There is a mistake in the calculation of the l

Daily Average Limit for Ethylene Glycol (outfall 002). The l correct vajue should be 11.9 mg/1.

ouTFALL 002

\

l A. Hydrazine l

We recorrend that the monitoring frequency for hydrazine be reduced to once/ occurrence.

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Ms. Nancy Weatherup July 13, 1999 Fage Two B. Ethylene Glycol We recommend that the menitoring f requency for ethylene glycol to reduced to once/ occurrence.

Note: Justification for changing the monitoring f requency of this Outfsli to "once/ occurrence" is because the waste treatrent system is released on a catch oasis and is homogeneous prior to release. Once/ occurrence monitoring will te representative of the entire discharge, ouTTALL 004 A. Hydrazine We recommend that the nonitoring frequency for hydrazine be reduced to once/ occurrence.

B. Ethylene Clycol The presence of Ethylene Glycol in this system is expected to be very infrequent. We therefore recommend that there be no cpecific effluent limitations assigned to ethylene glycol for Outfall 004.

Instead, we suggest that similar language be used here as was use/

for the hydrazine (ies record results and if value is gre "

than 23.8 mg/1, then this permit may be modified to prc limitations on glycol). Furthermore, we suggest that monito frequency for ethylene glycol be reduced to once/ occurrence.

Scts: Justification for changing the monitoring for this Outf all to once/ occurrence is based on the f act tnat the Padwaste system discharge tank is homogeneous prior to discharge.

Once/ occurrence monitoring would be representative of the entAre discharge.

For convenience of understanding, we have attached copics of af fected pages of the NPCES permit incorporating our reco m.endations. Please note, for better clariflestion we have suggested that scee of the language f rem the Rationale be included in Part III (page 24 of 24) of the permit.

Attached also, for your review and approval, are the analytical procedures which we intend to use to comply with effluent Itmitations once they are finalized. The source from which these procedures were cetained, is referenced in Section 5.0 of each procedure.

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! Ms. Nancy Weatherup 2 July 18, 1988 ,

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We appreciat.e the opportunity to coment on this draft of the permit t

! nodification. Please review these corrents at your oorliest convenience. i Gnce you've had an opportunity to perform the review, we would like to meet l with you do diens the specifics of our coments in greater detail. In the k

) rean time, should you have any questions, please contact Mitch Griggs at

• 704-173-7080. Your attention to this matter is greatly apprec 4ted.

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il W. A. Italler, Manager l Nuclear Technical Services t 1

i NOG /28/rhm Attachment .,

4 4 xc; Al Williams, Catawba District I

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S. Biswas R.E. Baker R.T. Wardoll Staff M.L. Dirch CN-3000.02-01 R.W. Eaker CN-3000.02-02 R.W. cuellette '

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M00!flCAi!ON DAIE

. Sureau of Water Pollution Control

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A. ffittillT LIrlifATIOf15 Afl3 MONIIORin RifKilRinitlIS DRA -

During II.c period beginning on the ef fective date asui lasting through the expiration date ti.e gerwittee is aut,horized to discharge from outfall(s) serial nued>cr(s)D02, wastewater treatment system dischar< ped take Wylie (Low volume wastes. chemical metal c1 caning Such discharge shall be limited and monitored by the permittee as specified below: wiste(#005).

Disciurge Limitations ebnitoring Requirements Effluent Characteristics Other Units (Specify)

• Picasurement Sample Daily Avg. Daily mm. Frequency Type O

o flow-m3 / day (ED) - -

1/ week flow Indicator 15 mg/l 20 mg/l 2/ month Grab Oli and Grease 30 mg/l 100 mg/I 2/ month Grab Total Suspended solids

.43 e5/l al/t.ccurrence Grab Ilydrarine -

!!. % /3 23.8m9/l at/occurreisce Grab

{ fthylene Glycol

• Measurement frequency is on.e per occurrence, but need not be more than twice per month.

The radiological cosgenents of this discharge is regulated by the United States llucicar Regulatory Commitsion (NRC 10 CTR 50 Appendix I) and is monitored and reported to the NRC. .

Based on a design flow of 3.4 MCD.

.: =

'2';

,- , m.

7. Z Ihe pH shall not be less than 6.0 statutard units nor greater than 9.0 standard units and shall be g, *"

monitored: cace ger week by grab sample.

a3 i 5' There shall tie no discharge of floating solids or visitale foam in other than trace aocunts. q 3U Samples taken in compliance with the sumitoring requirements specified above shall be talien at the I'"*

gk d following location (s): dischar9e frue the wastewater treatment system prior to mining with any other waste streams.

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N)DirICATION DME:

Bureau of W ter Pollution Control b

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l~'. s, A. EfftDfHI tittlIATI0ftS Alto I:DillI0 RING Rti)tilRitifMIS During tiee peritw1 tscolonin9 on the effective date amt f asting thrteiil the capiration date ll.e pensittee is authorized to discharge from outfall(s) serial send.cr(s))D4: Rachsaste System Discharge Such discharge shall be limited and monitored by the permittee as siccified below:

Discharge Limitations Monitoring Requirements, Effluent Characteristics O other Units (Specify]

• Itasurement Sample Monthly Aves. Daily Max. Irequency lype U

I 15 mg/l 20 swj/1 t/ year Crab Oli and Grease Total Suspended Solids 30 mg/l 100 mg/l ./ year Grab

• 1/ quarter 30 Day Composite Boron

• Grab

• **1/ occurrence laydrazine Grab

' *

• a*1/occurrence y Ethylene Glycol 4 _ _ .

E 1his disciurge is regulated by the United $tates MucIcar Regulatory Commission (NRC 10 CFR 50 Appendix I)

• - and is monitored and reported to the NRC. Ifowever, in the event that chmical metals cicaning wastes as defined a in 40 CfR Part 423 are discharged through this serial ammber, treatment shall be,provided to assure -

7 ttat discharges are in compilance with requirements of Part 423.13.

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' Based on a Design of .140 MGD.

-- Q Samples taken in compilance with the monitoring requirements specified above shall be taken }7U at the following location (s): Wastewater treatment system prior to mixing with any other waste 'g#

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" stream. Boron shall be sangled from the radiological sample location. ~

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• Record results.

• • Measurement frequency is onc.- per occurrence. t>ut need not be more than twice per month.

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. Page 24 of 24 Pemit No. SC000:273 y

JRAt U. A menitoring pregram will be imolemented to determine downstrean concentratiens of boren. A downstrean sarole shall be collected at the radiolcgical samole location and analyzed f or boren 'once per quarter. If there is no significant impact on water quality af ter 5 years of dsta collection, the menitorina requirement will be eliminated. ..

V. Monitoring of the rad waste discharge for oil and grease and total suspended solids will be implemented for one year. If shown that the above parameters are not in significant amounts in the rad wastewster tne monitoring requirement will be eliminated.

Duke will perfom a 316(a) study to assess any measurable therm.al effects on the biota of Lake Wylie. ine first year pre-operational W.

data was collected by a censultant, Industrial Biotest, Inc. Duke implemented the second yeaa of pre-ocerational data Collection in The operational impact. .

May, 1933 and will continue through May, 1984 assessment phase of the study will be similar to the secend year pre-operational phase with only minor changes made if the results indicate modificatiens are necessary. The plan and any significant change must be approved by CeDartrent of Health and Environmental Control. The o;erational phase will co rence when Unit I reaches Another second year of 50% power and will continue for one year.

data collection will be initiated when Unit 2 reaches 50% power.

A report will be subcitted to DHEC upon Co Dietion of each one-year operaticnal phase study.

X. The rad waste discharge vill be required to be monitored and1resultsPage 7 reported of the discharge concentration for Hydrazine (Part of 24). If values are greater than 15 mg/1, this permit may be modified to provide Hydrazine ilmitations and/or biological monitoring.

to Section 402 of the Clean Vater Reporting requirements, pursuantSection 102 of CERC1.A (Regulation 40 CTR Act (Regulation 40 CTR 117), for an 302), end Section 302 of SARA Title !!! (Regulation 40 CTR 355),

exceedence of the applicable reportable quantity for Hydrazine, will be initiated if the discharge concentration of Hydrazine exceeds 15.0 mg/1, and the reportable quantity has been exceeded.

Y. The radwaste discharge vill be required to be monitored and results!

reported of the discharge concentration for Ethylene Clycol (Part Page 7 of 24). If values are greater than 23.3 mg/1, this permit may be nodified to provide Ethylene Clycol limitations.

I

CP/0/3/0500/09 Revision 1 OLTI PobtR CCMPANY CATAh1A NYC!.ZAR STATION CXEM!STRY PROCEDull TOR TXE DETEMINAT!CN OF m RA2!NI IN VASTI WATER 1.0 DISCUSSION 1.1 Scope ,

This procedure desertbes the colorimetric method for the deterwination of hydratine in vaste water.

1.2 Principle Para dimethylasinobenzaldehyde produces a specif tc yellow reaction with hydrastaa se cheval 0

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3 C33 para dimethylaminobenzaldehyde azine (yellow)

Thr' intensity of the yellow color is proportional to the amount of hydrazine in the sample within the specified concentration range.

1.3 !.isits Sample concentration should be between 0.005 and 0.25 pre hydrazine. Higher concentrations suit be proportionally diluted prior to analysts. The lover liatt of detectable hydrazine is 0.005 ppe.

CP/0/3/4500/cg

, Page 2 of 5 Revision 1 1.4 Precision and Accuracy 1.4.1 The precision and accuracy of this method will be determined by Q Sua data.

1.4.2 A new calibration curve should be generated at least once a year.

1.5 Interferences 1.5.1 Hydraatne content say be dtaintshed by oxidizing agents.

1.5.2 Turbadity say cause high results. Ifturbidityisaprobles, filter the sample through a .45pe sembrane filter prior to analyzing.

1.5.3 Coloration in a sample say interfere with the quantitative determination of hydrazine.

1.6 Precautions 1.6.1 Labcoat, eye and hand protection shall be worn when .

worktes with para disethylaminobenzaldehyde or hydrochloric acid (HCL).

1.6.2 Hydrazine is a skin irritant and a potential skin sensitizer; therefore, precautions must be taken to avoid skin contact. Lab coat, hand and eye protection will be worn when working with hydrazine dihydrochloride and hydrazine containing solutions and samples. If skin contact occurs, wash the af fected area immediately with

. soap and water.

1.6.3 The light path surf aces of cuvettes should be buf fed with a lint free tissue such as "Xiavipes" prtor to being placed into the spectrophotometer.

1.6.4 If matched cuvettes are not available, correct the sample absorbance by subtracting the absorbance caused by the cuvette.

2.0 AFPARATUS. .

2.1 Spectrophotometer, with wavelength set at 458 na. Allow spectrophoto-seter to warm up for 30 minutes before use.

2.2 Erler.meyer flanks 2.3 Oraduated cylinder 2.4 Eppendorf pipets with required tips 2.5 Pipet dispenser 2.6 Balance 2.7 Two matched 1.0 ca cuvettes

CP/0/8/8500/09

. Page 3 of 5 Revision 1 3.0 RIACENTS 3.1 Hydrazine Stock Solution (100 pre)  !

Dissolve 0.3280 2 0.0005 grass of hydrazine dihydrochloride (N H 2HC1) in a 1000 al volumetric flask with desineralized waker, . Add to 10.5 si of concentrated MC1, then dilute this solutton to volume with destneralized water and six. Shelf life is 6 sooths.

3.2 Hydrazine Reagent (PAB) i J Otssolve 16.0 1 0.1 grams para dimethylantacbenzaldehyde in 800 t to al of methyl alcohol and 80 1 0.5 el of concentrated MC1.

Store in an amber bottle. This solution is stable indefinitely.

3.3 Hydrochloric Acid Solution (1% V/V)

, In a volumetric flask, dilute 1010.5 al concentrated hcl to 1 liter u th desineralized water. This solution is stable indefinitely.

4 4.0 PROCEDt.'RE .

4.1 Generation of Calibration Curve 1 NOTE: Generation of a new calibration curve ts not required if I this procedure is in current use; however, a new l calibration curve should be generated at least once a year, ,

1 Two (2) .050 ppa Q sua standards should be run datly when  !

ustog this procedure.

4.1.1 Prepare a series of hydrazine standards by diluting suitable volumes of hydrazine stock solution (Section 3.1) with 1% V/V hcl (Section 3.3) in 100 al volumetric flasks  ;

! to produce solutions of the desired concentrations as  !

! follows:

I i

j pl of 100 pro stock solution diluted to 100 s1 a pre N,H.

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10 pl 0.010 pre l 25 pl 0.025 ppe l 50 pl 0.050 ppe r 100 pl 0.100 ppe l 250 pl 0.250 ppe

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4.1.2 Transfer 50 al of each standard and a desineralized water .

blank into separate Erler.neyer flasks.

4.1.3 Ad!. 5.010.5 al of para disethylaminobenzaldehyde solution (

(Section 3.2) to each flash. MLa by swirling the flasks. f I.Jt the sixture stand 10 minutes, but not more than 100 minutes.

4.1.4 Adjust the spectrophotometer to the 458 na wavelength. l 4.1.5 Place the reagent blank in the spectrophotometer in a clean 1.0 ca cuvette. ,

CP/0/3/8500/09 Page 4 of 5

.- Revistoa 1 4.1.6 Set zero absorbance, s

4.1.7 Transfer the standards into the 1.0 ce cuvette la appropriate order and read the absorbance on the spectrophotometer checking the zero with the reagent blank before each seasurement. Standard concentration sessurements are to be made in order of increasing concentration. Rinse the cuvette with the subsequent sasple before each seasurement.

4.1.8 Prepare a calibration curve by plotting the absorbance vs -

concentration on a piece of graph p,qper. Indicate on the graph the date generated, analysts name, procedure number and spectrophotometer instrument number. This graph to particular to the instrument it was generated on.

4.2 Deterstaation of tlminown Concentrations cal TION: If the analysis is of a sample with turbidity and/or coloratton that might interfere with the analysis (RI., VC, and etc.), analyze a second portton of the saeple with no PAR added. Subtract ;he absorbance valve obtained from this sample with no PAR from the absorbance valve obtat'ned free the sample with PAB added.

4.2.1 Prepare two (2) .050 ppe standards for Q Sus by diluting 50 pl of the 100 pra hydrazine standard (Section 3.1) to 100 al with 1% hcl (Section 3.3) in a volumetric flask.

Measure 50 al of the .050 pps hydrazine standard into two (2) separate Erlenmeyer flasks. (To be done once per day when procedure is tn use.)

4.2.2 Transfer 50 si of each unknown sample and a desineralized water blant into separate Erlenmeyer flasks.

a.2.3 Add 5.0 g 0.5 al of para disethylasinobenzaldehyde solution (Section 3.2) to each flask. Mix by swirling the i

' flasks. 14t the etsture stand for 10 minutes, but not more than 100 minutes.

4.2.4 Adjust the spectrophotoneter to 458 nm. vavelength.

4.2*5 Place the reagent blank in the spectrophotometer in a 1.0 ca cuvette.

l 4.2.6 Set zero absorbance.

4.2.7 Transfer the unknown sample or standard into a 1.0 es cuvette. Read the absorbance.

4.2.8 Deterzine the hydrazine concentration of the sasple by comparing the sample absorbance to the calibration curve, l

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CP/0/8/4500/09 Page 5 of 5 l 4

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I 5.1 American Society for Testing and Materials,1987 Annual look of j ASTM Standards, D 1385 86. Page 514 517.

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! ) CATAW3A NUCLEAR STATION

'v CHIMISTRY PROCEDURE TOR THE DETERMINATION OF ETHYLENE GLYCOL CP/0/B/8500/29 1.0 DI S CL'S S ICN 1.1 Scope This procedure descrtbes the colorimetric determination of Ethylene Glycol in small concentrations. **

1.2 Principle Ethylene Glycol is reacted with Sodium meta Periedate to yield fo rmaldehyde :

H0CH 2 CH 0H + NaI0s

• 2CH 0 + Na!0 3+H 0 The formaldehyde is than determined colorimetrically.

1.3 Limits

/x This method is applicable to samples having a concentration of 1 to

('- j 7500 ppe. Samples containing hister concentrations must be diluted accordingly.

1.4 Precision and Accuracy Precision and Accuracy will be determined by Q-Sua data.

1.5 Interferences 1.5.1 Some waters purified by too exchange techniques cannot be used because of the presence of minute particles of resin that might react to form f ormaldehyde. Demineralized water has not been found to cause this problem and should be used for this analysis.

1.5.2 Turbid saeples will interfere. All samples shall be

.- filtered before analysis.

1.6 Precautions 1.6.1 Eye protection, gloves and labcoat should be worn when performing analysis.

1.6.2 Concentrated Sulfuric Acid is very corrosive. Extreme care should be exercised when working wtth this chemical.

Tollow precautions given in CP/0/B/8300/09.

}

. CP/0/3/8500/29 Page 2 of 5 2.0 6[l&R.AR

\ 2.1 Spectrophotometer 2.2 1.0 ce cuvettes 2.3 Ippendorfs - 200, 400, 600, 800 and 1000 pt 2.4 Pipets - 10 al disposable 2.5 Automatic dispensers - 2a1 .

2.6 Glass stoppered graduated cylinders 50 and 100 al 2.7 Volumetric flasks 50, 200 and 1000 31 2.8 Clamp or holder for Nitrogen cylinder 2.9 Bubbling Apparatus 2.10 ...trogen Regulator 2.11 Analytical Balance 3.0 REAGENTS O 3.1 Sodius Chronotropate (Sodium 1. 8 dihydrory - napthalene disulfonate) CgeH 70 S

• Na Reagent Grade.

3, 6 -

3,2 Concentrated Sulfuric Acid (N:$0e) 3.3 Sodium sulfite (Na 50 3) 5.5%

Dissolve 11.0 1 .5 grams of Sodius Sulfite (Na:Sos ) into a 200 al volumetric flask, dilute to volume with dominera11:ed water and mix. Shelf life is one week.

3.4 Sodium meta Periodate (Na!0.) 0.1:t Dissolve 21.0 2.5 grams of sodium meta-Periodate (Na!0.) into a 1000 al volursetric flask, dilute to volume with desineralized water and six. Shelf life is six sonths.

3.5 Ethylene Glycol (HOC 1:rCH 0li) Stock Solution (100 pra)

Dissolve $00 2 .005 g of Ethylene Glycol into a 50 al volumetric flask, dilute to volume with desineralized water and six. Pipet 10 als of this solution and transfer it to a 1000 mi volumetric flask, dilute to volume with desineralized water and six. This solution should be made daily.

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- CP/0/3/8500/29 Page 3 of 5 3.5 Desineralized Water 3.7 Nitrogen 4.0 Procedure 4.1 Generation of Standard Curve Generation of a standard curve is not requireal if method is currently in use; however, a new standard curve should be generated at least once a yeat. Two (2) 1.0 ppa Q Sua standards should be run daily . (

when procedure is in use. -

l 4.1.1 Prepare a series of standards by diluting suitable volumes of Ethylene Clycol solu'. ton to 20 als with desineralized water in a 100 ml glass stoppered graduated cylinder.

Include a graduated cylinder with 20 als of desineralized water to be used as a blank, Mis of Ethylene Glycol Solution Concentration

.2 1.0 ppe 1

.4 2.0 ppe

.8 4.0 ppe 1.2 6.0 ppa O 1.6 2.0 8.0 ppa 10.0 ppa 4.1.2 Dispense 2.0 1 .1 al of Sodium meta Periodate solution into each 100 al glass stoppered graduate, stopper and six.

Allow to react for 15 minutes at room temperature. l 4.1.3 Dispense 2.0 t .1 al of Sodium Sulfite solution to each graduate, dilute to volume, stopper and mix.

, 4.1.4 Pipet 10.0 mis of each of the above dilutions into 50 31

, glass stoppered graduates.

6 4.1.5 Add approximately 0.06 aus of Sodium Chronotropate to each graduate and dissolve.

4.1.6 CAtTTIONt Extreme care should be taken when handling acids.

Add 10 als of concentrated Sulfuric Acid by riesas of a pipet and allow the normal heat rise to occur.

4.1.7 By means of the bubbling apparatus immersed in the solution, bubble vigorously with Nitrogen for 10 minutes. Allow the contents of each graduate to cool to room temperature.

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- CP/0/B/8500/39 Pa8e 4 of 5 1.8 Adjust the spectrophotometer to a wavelength of 570 na.

. 4.1.9 Place the blank in the spectrophotometer in a cleas 1.0 ce cuvette.

I 4.1.10 Set the "zero" absorbance.

i 4.1.11 Read the absorbance of the standards, in order of increasing concentration. Rinse the cuvette with each

. subsequent standard before each measurement. Recheck "zero" absorbance with the blank before each standard.

4.1.12 Prepare a standard curve by plotting absorbance vj ppa Ethylene Glycol.

4.2 Detertnination of Unknown Concentrations 4.2.1 Prepare two (2) 1.0 ppe standards for Q-Sua by diluting

.2 mis of Ethylene Glycol solution to 20 mis with deminer-alized water in a 100 ml glass stoppered graduated cylinder.

(To be done once per day when procedure is in use).

4.2.2 Into a glass stoppered graduated cylinder introduce the amount of sample indicated in the table below, diluting to 20 mis with desineralized water, if necessary.

Concentration, ppm Sample Size, mis 1-35 20.0 35-75 10.0 75-150 5.0 150-750 1.0 750-7500 0.1 Fc,r f.orcentrations of Ethylene Glycol greater than 7500 ppa

(.757) use a ruitable dilution of the sample in demineralized water. Include one graduated cylinder containing 20 ml of demineralized water for a blank.

4.2.3 Dispense 2.0 t 1 al of 0.1 M Sodium meta-Periodate solution 1 each graduate, stopper and mix, allow to react

... for 15 a.u ttes room temperature.

4.2.4 Dispense 2.0 t .1 mis of Sodium Sulfite solution to each graduate, dilute to the 100 ml mark with demineralized

! water, stopper and mix.

l 4.2.5 Pipet 10 mis of each unknown sample or standard into a 50 31 glass stoppered graduated cylinder.

l 4.2.6 Add approximately .06 gas of Sodium Chromotropate to each i graduate and dissolve.

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l CP/0/B/8500/29  !

Page 5 of 5 I l

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4.2.7 CaJTION

Extreme care should be taken when handling acid. l C',] Add 10 mis of concentrated Sulfuric Acid by means of a pipet and allow the normal heat rise to occur.

4.2.8 By means of the bubbling apparatus immersed in the solution, bubble vigorously with Nitrogen for 10 minutes. Allow the contents of each graduata to cool to room temperature.

4.2.9 Adjust spectrophotometer to a wavelength of $70 nm.

4.2.10 Placetheblankinaclean1.0cmcuveIte.

4.2.11 Set the "zero" absorbance.

4.2.12 Read the absorbance of the standards, in order of increasing concentration. Rinse the cuvette with each subsequent sample before each measurement . Recheck "zero" absorbance with the blank before each sample, 4.2.13 Determine the Ethylene Glycol concentration by comparing '

the sample absorbance to the standard curve. -

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5.0 REFERENCES

g- 5.1 Union Carbide, Technical S wice Bulletin - Ethylene Glycol, Colorimetric Determination cf Low '.oncentrations by the Sodium Periodate Procedure.

6.0 ENCLOSURES 1 .

6.1 Bubbling Apparatus 4

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