SOP for Performance Check of Karl Fischer

1.0 OBJECTIVE

To calibrate the equipment for reliable and accurate results.

2.0 SCOPE

This procedure is applicable for Karl Fischer apparatus installed in the quality control department.

3.0 RESPONSIBILITY

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

4.0 ACCOUNTABILITY

Head of the Department

5.0 PROCEDURE

5.1 For Linearity and accuracy:

5.1.1 Frequency of the calibration: Monthly
5.1.2 Weigh accurately about 50, 100, 150, 200, 250 mg of Disodium Tartarate.
5.1.3 Perform the titration using the KF reagent as per the S.O.P.
5.1.4 Note the Burette reading and the water content.
5.1.5 Report the results in the given format as per Annexure-I
5.1.6 Check the linearity and correlation coefficient.
5.1.1 Linearity should not be less than 99.0%
5.1.2 Correlation coefficient should not be less than 0.9900%.
5.1.3 The performance of the instrument is satisfactory if the obtained Linearity and Correlation coefficient is within the given limit.

Related: Water Content Determination by Karl Fischer

5.2 Burette calibration:

5.2.1 Frequency of the calibration: Once in 3 Months
5.2.2 Use water for calibration.
5.2.3 Mount the burette tip firmly on the stand rod, it must not be moved during the test.
5.2.4 Set dispensing and filling rate of the burette to ‘max’
5.2.5 Take a dried beaker and tare the beaker.
5.2.6 Discharge the volume into the beaker and note volume dispensed.
5.2.7 Press <FILL> Key.
5.2.8 Weigh the dispensed volume.
5.2.9 Repeat 5 discharges of different volume.
5.2.10 Calculate the actual volume
5.2.11 Note down the reading in the provided format Annexure – I
5.2.12 Maximum relative error of the 10 ml exchange unit should NMT 0.5%.
5.2.13 The performance of the burette is satisfactory if the obtained relative error is within the limit.
5.3 If the performance is not satisfactory then follow S.O.P.

6.0 ABBREVIATION

6.1 % = Percentage
6.2 ml = Millilitre
6.3 mg = Milligram

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 IDENTIFICATION NO.

OBSERVATION

  

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

Limit : Linearity : NLT 99.00%

Correlation coefficient : NLT 0.99

Burette calibration :

Actual temp of water  : ___________

Factor                         : ___________

Weight of beaker        : ___________ (A)

Sr. no.	Displayed volume (ml) B	Wt. of beaker + water (gm) C	Wt. of water (gm) D= (C-A)	Actual volume (ml) E= (Factor xD)	Difference F= (E-B)	Tolerance + 0.5 % of displayed volume
1
2
3
4
5

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