ML20128N167

From kanterella
Jump to navigation Jump to search
Rev 0 to CP 807/2807/3807AP, Hydrazine Colorimetric
ML20128N167
Person / Time
Site: Millstone  Dominion icon.png
Issue date: 08/02/1995
From: Peiffer D
NORTHEAST NUCLEAR ENERGY CO.
To:
Shared Package
ML20128N126 List:
References
CP-807-2807-380, NUDOCS 9610160312
Download: ML20128N167 (8)
v • d • e


Text

_ ___ _ _ _ - _ _ _ _ . _ _ _ _ . _ _ . _ , _ . . _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . _

i , STATION PROCEDURE COVER SHEET A. IDENTIFICATION I

Number: CP 807/2807/3807AP Rev. O  !

Title:

HYDRA 7TNE COLORIMETRIC i i

1 Prepared By: DAVE PEIFFER l

B. REVIEW j I have reviewed the above procedure and have found it to be satisfactory.

IIILE SIGNATURE /DATE TITLE SIGNATURE /DATE DEPARTMENT HEAD /b /

% . F, 4qerCsi /

6-p.r,p C. SPECIFIC UNRE WFn OUESTION EVALUATION REQUIRFn:

1 Modifies intent of procedure and changes operation

of systems as desenbed in design documents. YES [ ] NO hQ (If yes, perform written USQ determination and Safety i Evaluation, and contact Manager, Safety Analysis Branch to dete2mine need for Integrated Safety Evaluation.)

ENVIRONMENTAL REVIEW REQUIRFD (Adverse environmentalimpact) YES [ ] NO %

I D. SPECIFIC SAFETY EVALUATION REQUIRFD

, Affects response of safety systems, performance of systems which may have been credited in the safety analysis or non-credited systems which may indirectly affect safety system response. YES [ ] NO[4 (If yes, coordinate Safety Evaluations and contact Manager, Safety Analysis Branch to determine need for Integrated Safety Evaluation.)

E. INTEGRATED SAFETY EVALUATION REQUIRFn YES [ ] NO %

E BIENNIAL REVIEW ,

1 This revision satisfies biennial review requirements. YES pq NO[]  :

G. PROFFnURE REQUIRES PORC/SORC REVIEW (In addition to review, items with a YES response j must be documented in the PORC/SORC meeting minutes.) YES [ ] NO)(1 H. PORC/SORC APPROVAL PORC/SORC Meeting Number Dom 4.1 be04t4 i

I. APPROVAL AND IMPT FMENTATION

[f-D-95.)

l The procedure is hereby approved, and effective on the date below:

W_ l1-I'+ Cr3 EFFECTIVE DATE

.l h p VICE P ESIDENT/ SERVICES / UNIT DIRECTOR 9610160312 961004 PDR ADOCK 05000245 P PDR

~

STATION PROCEDURE COVER SHEET A. IDENTIFICATION Number: CP 807/2807/3807AP Rev.D

Title:

IJYDRAZINE COLORIAETRIC Prepared By: DAVE PEIFFER B. REVIEW I have reviewed the above procedure and have found it to be satisfactory.

TITLE SIGNATURE /DATE TELE SIGNATURE /DATE DEPARTMENT HE AR /fo M '72 b _m. d - LLd 1 r , b f. D-41 y i o-

/ _

/

C. SPECIFIC UNREVIEWED SAFETY OUESTION EVALUATION REQUIRED:

Modifies intent of procedure and changes operation of systems as described in design doctiments. YES[ ] NO ((

(If yes, perform written USO determination and Safety Evaluation, and contact Manacer, Safety Analysis Branch to determine need for Integrated' Safety Evaluation.)

ENVIRONNENTAL REVIEW REQUIRED (Adverse environmental impact) YES[ ] NO ((

D. SPECIFIC SAFETY EVALUATION REQUIRFD Affects response of safety systems, performance of systems which may have been credited in the safety analysis or non-credited systems which may indirectly affect safety NO ((

system response. YES [ ]

(If yes, coordinate Safety Evaluations and contact Manager, Safety Analysis Branch to determine need for Integrated Safety Evaluation.)

1 E. INTEGRATED SAFETY EVALUATION REQUIRED YES[ ] NO (( I l;

F. BIENNIAL REVIEW This revision satisfies biennial review requirements. YES ((NO [ ]

G. PROCEDURE REQUIRES enc VIEW (In addition to review, items with a sponse must be documented in the PODF meeting minutes.) YES[ NO [ ] '

H. %R APPROVAL MRhMeeting Number N~d I. APPROVAL AND IMPLEMENTATION edure is hereby elow-The attabchedk 'bproved, w and effective on the date// nb78 VICE7 RESIDENT /SElt/ ICES /lfNTT DIRECTOR EFtECTIVE DATE SF301/13/s/SES/92-31/lof1

t )

$~N J. '%

. n. r

. I \D  %

. FORM'APFROVED BY DIRECTOR. MILLSTONE STATION EFFECTIVE DATE SORC MTG NO.

PROCEDURE LEVEL-OF-USE PROCEDURE TITLE: VdM iN o f ien (J FC I PROCEDURE NUMBER AND REVISION: M N2 bV [

t LEVEL.OF.USE CONTINUOUR USE QENERAL USE INFORMATION USE sieo.ov. i.e u r er.i ersor w,no p.,to n.ne. ri e.c r.. .

rm.i.e.c in.n.no r ,ir.ain-e o i not roeuer.e ~' te recuer.c to cerform

.et.. t . o. oro au r.

EPARTMENT HEAD APPROVAL DEPARTMENT HEAD SIGNATURE. k DATE: N 2 V

PMOCEDURE USER RESPONSIBILITIES

  • PWOCEDURE COMPLI AVCE . Inieni and direction provided in the procedure snail ne tellow ed regard 6ess ei ine ses el es use Deviations. encept allowed Delow. are not permittes s tihout an approsec change
  • PkOCEDLRE Review - Siers. noies caytions .warningr.. sequences and esoecied responses shoulu ce andersione e personnel prior to starting worn. or clarsfied e; appropriate suce vision
  • DATA RECORDING 110N-OFF5 . Record data or sign where indicaied wnen the step activit> has even compleien. usuess dire.:..

otherwise by the procedute

  • NIULTIPLE USERS . Each individual should hase a copy to sol.ow is practicat Sergie m.sier copy assilable f or s;;is.o'n Sign-otts in manier copy compitied when activity is comp.eted
  • IN ADEOL ATE L% EXPECTED RE5tLT5 . Stop the task Place equipment in stable or safe condition Centact hrst ime supersisor ior resc.u.cn Process prucedure changes, af needed
  • SEOVENCE OF STLPS . Perterm sieps in seevence unless otherwise direcied within reocedure Firs: hne suretusar m s = an e this requirement il Ine intent will col de meditied er tampromised e LSE OF N A- - Liv or N A hmned to those siepi clearb not srrassapie sur a task ce u nen hmard rei:i....

precedure art authorized to et compieted

  • PAkflAL PEli>ORM ANCE . Sociions portions serms.ot.siers performa.ce is alloweo it approved by firsi kne superme:
  • JOB EXPEkiENCE . Detailed procedure er change is not reevired se task within a pro.edure is semple snd cuni.usrid wnhin the sails el she trade Ths cepartment hsad shall determine whi h tashi ma3 he rtri * *vd b) has personnel withoui a procedure
  • CONruCTS . Contact firsi hne supermon to evaluate conHiet and inniate changes, il necessar> Choses art m .it per ACP.04 3 0:
  • ACP CONFUCT5 . Ben.lution of conllect by department head. Submu recommended changes for rester and errem.at D.coment resolutaen and autmit to appropriate Director and ACP Procedures group
  • EMERGENCY EVENT 5 . Emergency or ett. normal events not specifically covered in pari or teial by an appreved cr tdute should be addressed by plant .peraisons personnel.
  • ON E.TNE CH ANGr.1 . Openihse shanses see alsweil penweileit the intens er specitisans and sicars. siana sad ih. .hanes o prosessed as inisnt or non.ineeni per ACP.OA.) U*

. SF 371 Ref: ACP-OA-3.02E Rev.O Page 1 of 1

M i

CP 807/2807/3807AP Page 1 Rev.0 i

h HYDRA 71NE COIARIMETRIC i

? Page No. Eff. Rev.

i 1-5 0 4

l k

o i

4

?

i l

1 i

j

-l l

l 1

m. _ . . _ _ _ . _ _ _ . _ . . _ . _ . ._ ._. __ _ _ _ _ _ _. _ . _ . _

- CP 807/2807/3807AP Page 2 Rev.0

1. DBIECTIVE 1.1 To provide a procedure for the analysis of low hydrazine concentration in the range 5 ppb to 100 ppb.

I 2. REFERENCES l 2.1 ASTM Disignation: D1385-67, Hydrazine in Industrial Water.

2.2 CP 800/2800/3800G I. mast Square Fit.

3. PREREOUISITES 1-j 3.1 Power is available to spectrophotometer and the instrument has been i

properly installed, i.e., isolated from corrosive fumes, mechanical shock l

} and electrical interferences.

3.2 Equipment l

  • Volumetric Flasks 1000,100 mL l

i

  • Pipets 0.5, 2.5, 5.0, 7.5 10 mL I
  • Graduated Cylinder 100,10 mL
  • Erlenmeyer Flasksh50 mL Ch'1t )

I i

  • Cuvettes 4 cm
  • Spectrophotometer j 4. PRECAUTIONS 4.1 ANALYZE the sample as soon after collection as practicable.

j 4.2 Sample color and turbidity can interfere with the analysis.

5. PROCEDURE 5.1 PREPARE HCL Solution (1.2 Molar) i 5.1.1 ADD slowly 100 mL of concentrated HCL to approximately 500 s mL demineralized water in a 1000 mL volumetric flask.

5.1.2 DILUIE to the mark with demineralized water.

f i

5.2 PREPARE Hydrazine Indicator Solution.

5.2.1 DISSOLVE 4.0 grams of p-dimethylaminobenzaldehyde in a solution of 200 mL methyl alcohol and 20 mL of concentrated

) H1 4 5.2.2 STORE in a dark bottle.

5.2.3 1.ABEL with an expiration date two (2) weeks from the preparation date.

, (

1 4

4

l

, 1 CP 807/2807/3807AP Page 3

.' Rev.0

~

5.3 PREPARE Standard Hydrazine Solution (1 ppm).

NOTE The 1 ppm solution must be made in two steps:

5.3.1 DISSOLVE 0.328 grams of hydrazine dihydrochloride (N2 H4 . 2HC1) in 100 mL of demineralized water and 10 mL of concentrated HC1.

5.3.2 DILUTE with demineralized water to 1 liter in a volumetric flask.

5.~3.3 DILUTE 10 mL of Stock Solution to one liter with demineralized water in a clean volumetric flask.

5.3.4 LABEL as a 1 ppm Hydrazine Standard with an expiration date of 3 months from preparation date. i 5.3.5 DISCARD the remaining 100 ppm stock solution. l 5.4 PREPARE Calibration Standards i 5.4.1 DILUTE the following quantities of 1 ppm hydrazine standards and 1.2 mL hcl to 100 mL in volumetric flasks with demineralized  ;

water to produce the corresponding concentrations. l mL 1 PPM N2 H4 Std mL 19 HCI Sol Std Cone. enb 10.0 5.0 100 ,

7.5 5.0 75 5.0 5.0 50 2.5 5.0 25 0.5 5.0 5 5.4.2 LABEL the flasks with an expiration date 1 week from preparation.

5.5 PREPARE a Calibration Curve i w l.c 'cb d

TRANSFER the calibration standards into separate 250 mL *:L 5.5.1 Erlenmeyer flasks.

5.5.2 ADD 5 mL of HCL solution (1:9) plus 95 mL of demineralized d water into a,250 mL Erlenmeyer flask (zero blank for the '%

spectrophotoWfeTIt7."

5.5.3 ADD 5 mL of Hydrazine Indicator solution to each flask.

5.5.4 MIX thoroughly.

5.5.5 WAIT 20 minutes for color 'evelopment.

f 5.5.6 Pl. ACE the spectrophotometer in the absorbance mode.

CP 807/2807/3807AP Page 4 Rev.0 ,

5.5.7 READ the absorbance of the standards with reference to the water blank at 458 nm.

5.5.8 RECORD the absorbance of each standard on Chem. Form 807/2807/3807 AP-1.

5.5.9 REPEAT 5.2.1-5.2.6 two additional times.

5.5.10 COMPUTE the average absorbance for each standard.

NOTE If directed by Chemistry Supervisor, Use the Least Squares procedure (CP 800/2800/3800 G) to prepare the calibration curve.

If the calibration curve is linear and the absorbance intercept is small, then samples may be measured in the concentration mode with a concentration factor set equal to 1/ slope from the linear fit.

A table listing absorbance vs concentration may be used in place of a calibration curve. The concentration values can be calculated by the linear equation y = mx + b (see procedure 800/2800/3800 G).

i 5.5.11 PLOT the average absorbance vs concentration on linear graph .

paper.

5.5.11.1 Plot concentration values on the x-axis and absorbance on the y - axis.

5.5.11.2 LABEL calibration curve  :

1

  • Title
  • Preparation Date
  • Expiration Date
  • Technician's Initials 5.5.12 CHECK the calibration curve with every set of analyses by the use I of a control standard.

5.5.13 PREPARE a new calibration curve yearly or if there is a significant change in the analytical system.

5.6 Sample Collection and Analysis I 5.6.1 Sample Collection 5.6.1.1 PLACE 5 mL of HCL solution 1.2 molar in a small '

bottle.

{

SEP-24-1996 11:26 MILLST0tE CFEMISTRY 203 444 4256 P.02

. CP 807/2807/3807AP Page 5 i

.- Rev.O l* 5.6.1.2 ADD 95 mL of sample to the sample boule.

a

5.6.1.3 MIX thoroughly l 5.6.2 Sample Analysis ,

. ,, 4 ,

! 5.6.2.1 PREPARE a control standard and transfer in to a'250

! mL Erlenmeyer flask.

l 5.6.2.2 PREPARE a spectrophotometer blank as per 5.1.2.

! 5.6.2.3 11tANSFER the collect semples into a separate,250 mL Chega l Ei'- i - flasks. taNL e e '

5.6.2.4 ADD a 5 mL of Hydrazine hwur=*w solution to each j flask.

i 5.6.2.5 WAIT 20 minutes for color devatap=*rt I

5.6.2.6 SET the spectrophotometer to read absorbance or

!, concentration. ..

i 5.6.2.7 -READ the absorbance or concentration of all solutions

! against the water blank at 458 nm.

l 5.6.2.8 TRANSFER the blank to a clean cuvette.

5.6.2.9 TRANSPER each sample to a clean cuvette.

  • 5.6.2.10 READ either absorbance or concentration on the

.W -/ -:-- - = r.

5.6.2.11 IP operating in the absorbance mode, THEN use the calibration curve to DEIERbENED the concentration for all samples.

5.6.2.12 RECORD the control standard concentration as read from the calibration cune, on the Control Chart.

5.6.2.13 RECORD data on Chem. Form 807/2807/38074=t-MP-1. ,

c y\ l

6. FIGURES 6.1 Nonci l
7. DISCUSSIOli .

7.1 Hydrazine is added to feedwater and closed cooling waters for corrosion control. Analyses are performed for control purposes. A surnple is acidired with HCL to prevent hydrazine consumption by oxygen. The reagent para-<limethylamino- benzaldhyde is added to produce a yellow

- colored complex, whers the intensity of the yeBow color is proportional to the amount of hydrazine in the water. The color intensity is read on a.

spew-p.w.wster at 458 nm wavelength. The upper and lower detection

_ limits are set at ido ' ppb and.5 ppb, based upon the high and low calibration points.

, . m .* SS .e *T Aa *# W

~

TOTAL P.02 1

,1

Retrieved from "https://kanterella.com/w/index.php?title=ML20128N167&oldid=2892628"