SOP for Calibration 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 /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 10ml standard calibrated measuring cylinder
5.2.2 Press the START key and then press ENTER key. Then again press START key.
5.2.3 When the display show 3ml, immediately press STOP key.
5.2.4 Note down the observed volume of Karl Fischer reagent in the measuring cylinder.
5.2.5 Now repeat step No 5.2.2 to 5.2.4 for 6ml and 9ml.
5.2.6 Record the obtained volume and displayed volume in the enclosed format.
5.2.7 The volume displayed on the instrument and the volume collected in cylinder should not vary by more than ± 0.1 ml, otherwise, follow the S.O.P.
5.2.8 Record the results in Annexure.
5.2.9 Frequency of calibration: Once in a month.

Related: Water Content Determination by Karl Fischer

5.3 FOR INSTRUMENT PERFORMANCE

5.3.1 Add accurately weighed 100mg 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, otherwise follow the S.O.P.
5.3.4 Repeat the step 5.3.1 & 5.3.2 and take total five reading.
5.3.5 Record the results in Annexure-I.
5.3.6 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 number
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 DETAIL
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	Tolerance
1					14.87 % to 16.44 %
2
3
4
5
			% RSD :		(NMT 1.0 %)

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