SOP for Performance Checks of Karl Fischer Appara tus

Standard operating procedure to calibrate the karl fischer apparatus using disodium tartrate.

1. Objective

To calibrate the equipment far reliable and accurate results.

2. Scope

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

3. Responsibility

3.1. Doing TechnicalAssistant

3.2. Checking Executive/Asst. Manager

4. Accountability

Head of the Department

5. Procedure
Frequency Once in a month

5.1. Operate the instrument as per SOP

5.2. FOR BURETIE CALIBRATION
5.2.1. Place the burette outlet in 20 ml 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 formal.
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 Annex 1.
5.2.7. Frequency of calibration: Once in a month.
5.3. FOR INSTRUMENT PERFORMANCE
5.3.1. Add accurately weighed 50mg, 1OOmg, 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.

% Water (W/W) = Volume of KFR consumed in mi X 100 X Factor / - 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 Annex 1

5.3.5. Frequency of calibration: Once in a month.

6. ABBREVIATIONS

6.1. % = Percentage
6.2. mg = milligram
6.3. W/W = Weight by Weight
6.4. SO P = Standard operating procedure
6.5. ml= milliliter
6.6. KFR = Karl fischer reagent
ANNEX 1
Q. C. Department

PERFORMANCE CHECK REPORT OF KARL FISCHER APPARATUS

PERFORMANCE CHECK DDATE OF LAST NEXT DUE FOR

APERFORMANCE PERFORMANCE CHECK
TCHECK DONE
E

INSTRUMENT DETAILS

INSTRUMENT NAME INSTRUMENT MAKE INSTRUMENT ID No.

OBSERVATION

Sr.No. Wt. taken of di- Volume of KFR Factor %Water Tolerance

sodium tartrate required (ml) mg.H2O /ml obtained
(mg)

2 14.87% to 16.44%

Linearity : _____ (NLT99,00%) % RSD : (NMT 1.0 ºlo)

Calculation :

BURETTE CALIBRATION :

Actual temp of water: ___________

Factor: ___________
Wt. of beaker (A) : ___________

Sr.no. Displayed Wt. of beaker+ Wt. of water Actual volume Difference Tolerance ±
volume (ml) water (g) (g) (ml) F = (E B) 0,5% of
B C D = (C A) displayed
E= (Factor X volume
D)
1

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