STANDARD OPERATING PROCEDURE OPERATION AND MAINTENANCE OF KARL FISCHER TITRATOR


STANDARD OPERATING PROCEDURE

SUBJECT :                    
OPERATION AND MAINTENANCE OF KARL FISCHER TITRATOR
DEPARTMENT           : QA
SOP NO.                      :
Page No                       :
Effective Date             :
Next Review                :
Version No                  :

1.0       OBJECTIVE:

To provide guidelines for the operation and maintenance of the Karl Fischer titrator.

2.0       SCOPE : 

To ensure establish a procedure for handling of Karl Fischer Titrator.

3.0       PROCEDURE:

3.1       Switch on the power supply and allow the instrument to run for 5 minutes.

3.2       Fill the burette with Karl Fischer reagent.

3.3       Place few ml of dehydrated methanol to dip platinum electrodes in titration vessel and neutralize with KF reagent.

3.4       Titrate to the electrometric end point with the Karl Fischer reagent.

3.5       Add quickly 150 to 350 mg of Sodium tartrate, accurately weighed, stir for 1 minute, and titrate to the end point with Karl Fischer reagent

3.6       Calculate the water equivalence factor F in mg of water per ml of the reagent by the expression
= 0.1566 x W/V, where
           
W is the weight, in mg, of the Sodium Tartarate.

V is the volume in ml, of the reagent required.

3.7       Transfer quickly the prescribed amount of the substance being examined, accurately weighed, to the titration vessel. Stir for 1 minute and titrate again to the electrometric end point using the Karl Fischer reagent Note the reading in the burette.
3.8       Calculate the water content of the sample, in mg, by the expression

            =F x 100 x V/W1, where

            F is the water equivalence factor

            V is the volume in ml, of the reagent consumed

            W1 is the weight, in mg, of the sample.

3.9       Air in the entire system should be kept dry during the titration.

3.10     After completion of the titration, switch off the power system and clean the titration vessel with dehydrated methanol.

3.11     Enter the KF factor Log book.

4.0       FREQUENCY: As and when required.

5.0       RESPONSIBILITY: Executive (Q.A)

6.0       REVIEW GUIDE:  KF Log book.

7.0       ANNEXURE: -------

8.0       SOPs DISTRIBUTION:

            This SOP shall be distributed to following Departments:

Name of the Department
Master Copy
Circulatory Copy
QA/QC
Production
x
x
Warehouse
x
x
General
x
x
Maintenance
x
x

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