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SOP for Operation and Calibration of Karl Fischer Apparatus

OBJECTIVE
To lay down the procedure for operation and calibration of the Karl Fischer Apparatus for better and error free use.

SCOPE
This procedure is applicable for Karl Fischer Apparatus installed in Quality Control Department at XYZ Limited.

RESPONSIBILITY
Execution : Chemist and above – QC department.
Checking : Asst. Manager and above – QC department

OPERATIONAL PROCEDURE
Karl Fischer titration shall be carried out in three stages.

To neutralize blank moisture from methanol
  • Neutralize the blank moisture from methanol and confirm the end point 3-4 times and observe the final reading, that should be about 0.1ml. This indicates that the instrument has stabilized and is ready for standardization of KF reagent.

Factor Determination
  • Factor of KF reagent shall be determined by using water.
  • KF Factor shall be determined three times and the average of the three values shall be obtained. KF factor shall be considered valid if % RSD for the three determinations is less than 1.0%.
  • KF factor shall be determined before use and the records maintained as per Annexure-1.
  • KF factor should be between 4.0mg/ml to 7.0mg/ml otherwise discard the KF reagent.
  • KF factor shall be determined as follows

Determination of Water content.
  • Select the sample size as per following table or otherwise mention in specific monograph.
  • Enter the sample quantity and calculate the moisture content by using following formula

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CALIBRATION PROCEDURE
Frequency: Once in 3 months
  • Operate the instrument as described above in operation procedure.
Accuracy of Instrument
  • Carry out titration as per 1st stage and neutralised the blank moisture from methanol
  • Add water and note down the KF reagent reading.
  • Repeat the procedure three times and record the results in Annexure-2
Accuracy of the Dispensing Pump
  • Fill the dispenser with the purified water and remove all the air bubbles.
  • Take the weight of empty 10ml volumetric flask (W1).
  • Connect the outlet of dispenser to 10ml empty volumetric flask
  • Press “CLEAR” key, instrument is now ready for validation of volume displacement. Press “ENTER” for Validation
  • Enter volume 10ml and press ENTER.
  • Take the weight of volumetric flask with water (W2) and calculate the dispensed volume as below
  • Repeat the procedure three time and record the results in Annexure-2.

REFERENCE(s)
Nil.

ABBREVIATION(s)
SOP : Standard Operating Procedure
Q.C Quality control
% Percentage
RSD Relative standard Deviation
ml Milliliter

ANNEXURE(s)
Annexure No. – 1 - Karl Fischer Factor Determination Record
Annexure No. – 2 - Calibration Record of Karl Fischer Apparatus

 
REVISION CARD
Nil

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