SOP for Performance Checks of Karl Fischer Apparatus

1.0 Objective

To calibrate the equipment for reliable and accurate results.

2.0 Scope

This procedure is applicable to calibrate the Karl Fischer apparatus, installed in the quality control department.

3.0 Responsibility

3.1 Doing: Technical Assistant
3.2 Checking: Executive/Asst. Manager

4.0 Accountability

Head of the Department

5.0 Procedure

Frequency: Once in a month
5.1 Operate the instrument as per SOP.

5.2 FOR BURETTE CALIBRATION

5.2.1 Place the burette outlet in 20ml standard calibrated measuring cylinder.
5.2.2 Dispense 2,4,6,8,10,12,14,16,18 & 20 ml water into previously weighed & conditioned beaker and note the water weight of water for the dispensed.
5.2.3 Note down the observed volume of water in the measuring cylinder.
5.2.4 Record the obtained volume and displayed volume in the enclosed format.
5.2.5 The volume displayed on the instrument and the volume collected in cylinder should not vary by more than 0.5 %, otherwise, follow the S.O.P.
5.2.6 Record the results in Annexure.
5.2.7 Frequency of calibration: Once in a month.

5.3 FOR INSTRUMENT PERFORMANCE

5.3.1 Add accurately weighed 50mg, 100mg, 150mg, 200mg, 250mg of Disodium tartrate into the titration vessel containing neutralized methanol and test for water content.
5.3.2 Calculate the % water by using the formula given below.

                                Volume of KFR consumed in ml X 100 X Factor

% Water (W/W) = --------------------------------------------------------------

                                             Weight of disodium tartrate in mg

5.3.3 The performance of the instrument is satisfactory if the difference between the obtained values is within the tolerance limit of 15.66 ± 5% i.e. 14.87% -16.44.
5.3.4 Record the results in Annexure-I.
5.3.5 Frequency of calibration: Once in a month.

6.0 ABBREVIATIONS

6.1 % = Percentage
6.2 mg = milligram
6.3 W/W = Weight by Weight
6.4 S.O.P. = Standard operating procedure
6.5 ml = milliliter
6.6 KFR = Karl fischer reagent

ANNEXURE-I

Q. C. Department

PERFORMANCE CHECK REPORT OF KARL FISCHER APPARATUS

PERFORMANCE CHECK  DATE	DATE OF LAST PERFORMANCE CHECK DONE	NEXT DUE FOR PERFORMANCE CHECK

INSTRUMENT DETAILS
INSTRUMENT NAME	INSTRUMENT MAKE	INSTRUMENT ID No.

OBSERVATION

Sr. No.	Wt. taken of di-sodium   tartrate (mg)	Volume of KFR required (ml)	Factor mg. H2O/ml	% Water obtained	Tolerance
1					14.87 % to 16.44 %
2
3
4
5
	Linearity : ____(NLT 99.00%)		% RSD :		(NMT 1.0 %)

Calculation :

BURETTE CALIBRATION :

Actual temp of water   : ________

Factor                          : ________

Wt. of beaker (A)        : _________

Sr. no.	Displayed volume (ml) B	Wt. of beaker + water (gm) C	Wt. of water (gm) D=(C-A) gm	Actual volume (ml) E= (Factor X D)	difference F=(E-B)	Tolerance + 0.5 % of displayed volume
1
2
3
4
5
6
7
8
9
10

Calculation :

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