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OPERATION AND CALIBRATION OF KARL FISCHER APPARATUS

SOP NO.: EffectiveDate: Review Date: QC00X-01 DD/MM/YYYY DD/MM/YYYY

Supersedes Page No.: Department: NA 01 of end Quality Control

I           OBJECTIVE 

            To describe the Operation and Calibration Procedure for the Karl Fischer Apparatus.

II          SCOPE

            This Procedure applies to the operation and calibration of the Karl Fischer Apparatus in the QC Department of ABC Ltd, Location.

III        RESPONSIBILITY 

            1. The analyst, who operates the instrument, is responsible for following the procedure.

            2. The QC Manager / Designee is responsible for implementing the procedure.

IV        DOCUMENT REFERENCE(s)

   SOPs:   a) Policy on calibration (Current version of QA 0XX)

                 b) Operation and calibration of Analytical Balance (Current version of QC00X)

                 c) Maintenance of desiccants (Current version of QC0XX)

Forms

S.No Detail Format No 1 KF Standardization Calibration Record QC00X/F01

V        SCHEDULE:

1.0      External Calibration shall be carried out once every 3 months.

2.0      Internal calibration:   Daily  

VI        PROCEDURE  

1.0       Precautions:

1.1       Keep the lid of the KF vessel tightly closed to protect against atmospheric moisture.

1.2       Care should be taken while transferring the test sample to the KF vessel so that the test sample does not fall on the wall of the KF vessel.  

1.3       Ensure that the KF tube is free from any air bubbles.

1.4       Ensure that the Silica gel is good in condition.

2.0       Operating Procedure:

2.1       Transfer about 50 to 60 ml of fresh methanol into the clean and dried titration vessel Fill the 25 ml burette with KF Reagent up to the mark.

2.2       Switch on the instrument and observe the END LED glow.

2.3       Press the start button to start the addition of KF reagent to the titration vessel.             Observe ADDLED glows.

2.4       Wait until methanol is neutralized and fill the burette to the mark.

2.5       Now add a small quantity of sample into the titration vessel.

2.6       Again press the start button to start the KF reagent addition.

2.7       Wait until the END LED glows and note down the KF consumed.

2.8       Finally calculate the moisture content of the sample using the formula given below and document the details in the equipment log.                                      Volume of KFR consumed X KFR factor X 100           Calculaton      =  ______________________________________                                   (Volume /weight) of the sample X 1000                                                                                                

3.0       Calibration Procedure    :

3.1       Fill the KF reagent in the reagent bottle.

3.2       Switch on the instrument.

3.3       Remove the mixture of KF reagent and sample solution from the titration vessel.

3.4       Wash the titration vessel with 10 ml of methanol.

3.5       Place about 50 to 60 ml of methanol into the titration vessel.

3.6       Neutralize with KF reagent to an electronic endpoint.

3.7       Weigh accurately about 0.1 to 0.15 gm of Disodium tartrate (DST) and transfer it to the titration vessel.

3.8       Stir to dissolve and titrate with KF reagent.

3.9       After completion of titration, note down the burette reading (TV) and calculate as follows:

                                             Weight of DST X 15.66 X 100              Calculaton      =  ________________________________                                                               T.V X 100                                                                       

3.10    Repeat the same from step No. 3.7 to 3.9 and take the average value of the KF factor.     

3.11    The tolerance limit for two trials should not be more than 0.15. If doesn’t comply repeat the same.

3.12     If the Karl Fischer Reagent factor is less than 4.8 mg of H2O/mL discard the Karl Fischer Reagent solution and take fresh reagent.

3.13     Ensure the details are documented in the calibration log.

3.14     Enter the breakdown details & spares utilized in the Equipment History Card.

 REFERENCE:

*  Instrument Manual of KFR Auto Titrator.  

REVISION HISTORY Version Effective Summary of Revision

0.0 DD/MM/YYYY New SOP

END O F THE DOCUMENT                                   

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