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SOP for Performance Check of Karl Fischer


Standard operating procedure to check the performance of Karl Fischer apparatus using Disodium Tartarate.

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 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 are 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 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






Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
Email: .moc.enilediugamrahp@ofni Need Help: Ask Question


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