Sei sulla pagina 1di 7

A G A L WA

110. PROCEDURE FOR CALIBRATION OF pH METERS.

C o n t r o l l e d C o p y No. 1

rsion

Amendments

Date

Page

Section

30 July
1997

Authorised B y : L O M

Details

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-

CI
LOM

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GAL WA Regional Procedure

Issue: I

C(Htf-.
~~&titiyl*U

Page: I of 6

fkle: Q10 Procedure For Calibration ofpH Meters


tthorised By: WA Laboratory Operations Manager

Issue Date :30 July 97

lURPOSE
p i s procedure provides instructions for t h e calibration a n d m a i n t e n a n c e of p H meters
Bed at A G A L W A . to report t h e p H in s a m p l e s .

1COPE
lis procedure is applicable t o t h e R a d i o m e t e r P H M 8 0 portable p H meter (asset number.
11/0175-LE) in u s e in t h e W A R e g i o n a l L a b o r a t o r y .

EFERENCES
I 3 9 0 1 . 1 9 8 7 Quality Systems for D e s i g n / D e v e l o p m e n t ,
rvicing
*\L

Production, Installation a n d

National Quality M a n u a l

|LTA General R e q u i r e m e n t s for Registration


2300.1.6-1989 M e t h o d s of c h e m i c a l a n d physical testing for the d a i r y i n g industry
thod 1.6: general m e t h o d s a n d principles - Determination of p H , A p p e n d i x B
\A 4 5 0 0 - H + B Electrometric M e t h o d
it Regional M e t h o d W L 120
6438:Part 2 : 1 9 8 4 . E l e c t r o c h e m i c a l
Krnance of p H value analysers

Analysers,

Part

2.

Method

for

["A t e c h n i c a l Note 2 1 , 1 9 9 4 , p H m e t e r s - Calibration a n d Electrode


:ks (see attached).

specifying

Performance

INITIONS
>ration

T h e c o m p a r i s o n of a m e a s u r e m e n t s t a n d a r d or instrument with
a n o t h e r s t a n d a r d or i n s t r u m e n t t o report, or eliminate by adjustment,
any variation (deviation) in t h e accuracy of t h e item being c o m p a r e d .

k:\quality\procedurNproq 10# 1 .doc

GAL WA Regional Procedure

Issue: I

Page: 2 of 6

title: Q10 Procedure For Calibration of pH Meters,


ithorised By: WA Laboratory Operations Manager

Issue Date :30 July 97

lOCEDURE
1. G e n e r a l
Calibrate t h e
requirements,
that is :-

pH

meter

according

to

schedule

which

complies

with

NATA

Calibrate o n use with at least t w o s t a n d a r d buffer solutions a p p r o p r i a t e t o t h e


participated p H of t h e s a m p l e ( s ) b e i n g t e s t e d (Note that w e prepare o u r buffers e v e r y
[three months^by m a k i n g n e w o n e s u p a n d c h e c k i n g against c o m m e r c i a l buffers).
[Check the reference e l e c t r o d e junction w e e k l y O R c h e c k t h e slope r e s p o n s e ( o n 3 r d
buffer) of t h e electrode s y s t e m w e e k l y .
Clean t h e p H probe six monthly (or a s required).
C h e c k each c o m m e r c i a l batch of p H buffers before initial use..
[Keep a record of t h e s e actions in t h e p H m e t e r log book.

C o n t r o l of T e s t E q u i p m e n t

E q u i p m e n t I d e n t i f i c a t i o n : All p H meters shall be identified by t h e A s s e t


Register N o . i n d i c a t e d o n their a t t a c h e d DAS A s s e t t a g .
*
S t o r a g e a n d H a n d l i n g : All p H buffers a n d reagents shall be stored at r o o m
t e m p e r a t u r e a n d o u t of direct sunlight.
"

N o n c o n f o r m i n g E q u i p m e n t : A n y p H meter that d o e s not satisfy t h e


r e q u i r e d c a l i b r a t i o n t o l e r a n c e will b e brought to t h e attention of b o t h t h e
Cost C e n t r e M a n a g e r a n d t h e Administration M a n a g e r w h o will a r r a n g e
appropriate servicing.

Note: N o n c o n f o r m i n g p H meters shall not be used until satisfactory repair a n d r e calibration h a s b e e n c o n d u c t e d .


N o n c o n f o r m i n g p H meters shall b e
r e m o v e d f r o m t h e servicing area or clearly labelled a s "Not to b e U s e d " w h i l e
awaiting repair.

k:Nqu al i ty\proced ur^proq 10# 1 .doc

AGAL WA Regional Procedure

Issue: I

Page: 3 of 6

Title: Q10 Procedure For Calibration ofpH Meters


Authorised By: WA Laboratory Operations Manager

Issue Date :30 July 97

Faulty E q u i p m e n t : A n y p H meter which has been i n v o l v e d in a n y e v e n t


which may affect its a c c u r a c y must be re-calibrated.

3. Calibration of pH Meters
3.1 P r e p a r a t i o n of Buffer S o l u t i o n s
3.1.1 Phthalate Buffer S o l u t i o n , pH 4.0
Dissolve 5.069g of p o t a s s i u m h y d r o g e n phthalate in grade 1 w a t e r a n d m a k e u p to
5 0 0 m L in a volumetric flask at 2 0 C . Note : See table for the variation in p H units
of this buffer solution in t h e t e m p e r a t u r e range 2 0 C to 2 5 C . R e p l a c e buffer
solution every six m o n t h s . R e c o r d preparation details in the pH meter log b o o k .
3.1.2 P h o s p h a t e Buffer S o l u t i o n , pH 6.88
Dissolve 1.77g N a 2 H P 0 (dried at 1 2 0 C for 2 hours) and 1.695g of K H 2 P O 4
(dried at 1 2 0 C for 2 hours) in grade 1 water and make up to 500ml_ in a v o l u m e t r i c
flask at 2 0 C . N o t e : See table for the variation in p H units of this buffer s o l u t i o n in
the temperature range 2 0 C t o 2 5 C . Replace buffer solution every six m o n t h s .
R e c o r d preparation details in the p H meter log book.
4

3.1.3 B o r a x Buffer S o l u t i o n , p H 9.18


'
Dissolve 1.90g N a 2 B 4 O 7 . 1 0 H 2 O in g r a d e 1 water a n d make up to 5 0 0 m L in a
volumetric flask at 2 0 C . N o t e : See table for the variation in p H units of this buffer
solution in the t e m p e r a t u r e range 2 0 C to 2 5 C . Replace buffer solution e v e r y six
m o n t h s . Record p r e p a r a t i o n details in the p H meter log book.
Temperature C

Phthalate Buffer pH

20
21
22

4.0001
4.0002

6.88
6.87

4.0002

6.87

9.225
(9.216)
(9.207)

23
24
25

4.0003
4:0004
4.0005

6.87
6.86
6.86

(9.198)
(9.189)
9.18

Phosphate Buffer pH

Borax Buffer p H

le values in brackets are interpolated from the 20C and 25C values given in the British

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AL WA Regional Procedure

Issue: I

Page: 4 of 6

e: QIO Procedure For Calibration of pH Meters


'horised By: WA Laboratory Operations Manager

Issue Date :30 July 97

3.2 Calibrate o n U s e
Calibrate t h e p H m e t e r s a s per A G A L R e g i o n a l M e t h o d W L 120 with p H 7 a n d p H 4
buffer solutions e a c h d a y before u s e . Calibrate t h e p H meter with p H 7 a n d p H 9.2
buffer solutions if it is e x p e c t e d that t h e s a m p l e p H value will b e g r e a t e r t h a n p H 7.
Record the calibration details in t h e p H m e t e r log book.
3.3 C h e c k R e f e r e n c e J u n c t i o n E l e c t r o d e
Measure t h e p H of t h e phosphate buffer solution a n d c o m p a r e w i t h t h e p H of t h e
s a m e buffer solution diluted 1:10 with w a t e r (i.e. diluted with 9 p a r t s of w a t e r ) . T h e
p H of t h e diluted buffer should be 0.15 - 0.25 p H units higher t h a n t h e o r i g i n a l
buffer. Record t h e a p p r o p r i a t e details in t h e p H meter log book.
3.4 C h e c k S l o p e R e s p o n s e of the E l e c t r o d e S y s t e m
T h e slope r e s p o n s e of t h e electrode s y s t e m shall be 95_percent t o 102 p e r c e n t of
t h e theoretical v a l u e (S) for t h e glass electrode at t h e t e m p e r a t u r e of m e a s u r e m e n t ,
i.e.
58.167 m V / p H unit at 2 0 C 59.157 m V / p H unit at 2 5 C ^ Measure t h e p H a n d electrode potential (mV) of t h e phthalate buffer a n d t h e
phosphate buffer (taking note of the sign w h e n m e a s u r i n g the p o t e n t i a l ) .
Calculate the p e r c e n t a g e slope from t h e following e q u a t i o n :
Percent slope

(mVy - mV4)
ApH

where
mV7 =
mV4 ApH
=
S

100

e l e c t r o d e potential in p H 6.88 buffer s o l u t i o n , in millivolts . . .


e l e c t r o d e potential in p H 4 buffer solution, in millivolts
n o m i n a l p H of t h e buffer p H 6.88 solution minus n o m i n a l p H of t h e p H
4 buffer solution (e.g.. 6.88 - 4.0 = 2.88)
t h e o r e t i c a l slope response at t h e t e m p e r a t u r e of m e a s u r e m e n t ( s e e
above)

Record t h e a p p r o p r i a t e details in t h e p H meter log book.

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AGAL WA Regional Procedure

Issue: I

Page: 5 of 6

Title: Q10 Procedure For Calibration of pH Meters


Authorised By: WA Laboratory Operations Manager

Issue Date :30 July 97

3.5 C h e c k C o m m e r c i a l pH B u f f e r s
Calibrate t h e p H meter with either previously verified c o m m e r c i a l p H buffers o r
make the p h o s p h a t e buffer solution a n d t h e phthalate buffer s o l u t i o n as s h o w n
above. M e a s u r e t h e p H of t h e n e w commercial pH buffer (before initial u s e ) . T h e
new buffer is a c c e p t a b l e if it is within + 0.02 pH units of t h e notional value. R e c o r d
the appropriate details in t h e p H meter log book.
3.6 E x t e r n a l C a l i b r a t i o n of pH Meters
Not applicable.

Acceptability Criteria
W h e n t h e p H meter d o e s not meet t h e a c c e p t a b l y criteria as s p e c i f i e d below t h e n
the test should be r e p e a t e d . If t h e p H meter does not c o m p l y o n t h e s e c o n d test t h e n
it should be r e g a r d e d a s n o n c o n f o r m i n g equipment a n d treated a s specified i n
section 2.
4.1 R e f e r e n c e J u n c t i o n E l e c t r o d e
T h e pH of t h e d i l u t e d buffer s h o u l d be 0.15
buffer.

0.25 pH units higher t h a n the o r i g i n a l

4.2 S l o p e R e s p o n s e
*
/
T h e slope r e s p o n s e of t h e e l e c t r o d e system shall be 9 5 percent t o 1 0 2 percent o f
the t h e o r e t i c a l v a l u e (S) for t h e glass electrode at t h e t e m p e r a t u r e o f
measurement.
4.3 C o m m e r c i a l p H B u f f e r s
T h e n e w c o m m e r c i a l buffer is a c c e p t a b l e if it is within + 0.02 p H units of its n o t i o n a l
value.

j5. Maintenance of t h e pH Meters


5.1 pH P r o b e S t o r a g e S o l u t i o n
W h i l e the p H p r o b e is not in u s e leave it soaking in the p H probe s t o r a g e s o l u t i o n .
W e i g h approx 0.71 g Na2HPC>4 (or approx 0.88g N a H P 0 . 2 H 2 0 ) , approx 0 . 6 8 g
K H 2 P O 4 a n d a p p r o x 1.0g K C I in 200ml_ of water.
2

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AL WA Regional Procedure

Page: 6 of 0

Issue: I

: QIO Procedure For Calibration ofpH Meters


horised By: WA Laboratory Operations Manager

Issue Date :30 July 97

5.2 C l e a n i n g the p H P r o b e
The pH probe s h o u l d b e cleaned at least every 6 m o n t h s .
Dip the p r o b e in :
1 % pepsin in 0.1 M H C I for 30 m i n s , (to r e m o v e protein materials),
0.1 M E D T A solution f o r 3 0 mins (to r e m o v e inorganic coatings),
a mild d e t e r g e n t s o l u t i o n (or a solvent) for 2 hours (to remove oils a n d g r e a s e s ) ,
then
drain a n d refill t h e reference c h a m b e r with s a t u r a t e d KCI s o l u t i o n a n d a d d s o m e
KCI granules a n d s o a k t h e probe in t h e p H 7 storage solution o v e r n i g h t .
Recalibrate t h e p H p r o b e as specified in section 3.
Record t h e a p p r o p r i a t e details in t h e p H m e t e r log book.
5.3 Maintenance D e t a i l s
Record any c h a n g e s t o t h e p H meter, e . g . battery replacement, n e w p r o b e i n s t a l l e d
etc in t h e p H meter log book.

PONSIBILITY
O

S e c t i o n L e a d e r : T h e Section L e a d e r is to e n s u r e that t h e a p p r o p r i a t e staff c a r r y


out the calibration a n d maintainance p r o c e e d u r e s as specified a b o v e .
Laboratory Staff: Responsible for c o n d u c t i n g calibration a n d m a i n t e n a n c e
procedures a s d i r e c t e d by Cost C e n t r e M a n a g e r s .

ATED P R O C E D U R E S
edure for I n s p e c t i o n , M e a s u r i n g , & T e s t E q u i p m e n t

"

ERENCE DOCUMENTS
applicable.

WCHARTS
e.

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kiV^ualityVproceduiNproqlOS 1 .doc