SOP FOR KARL FISHER APPARATUS | STANDARD OPERATING PROCEDURE FOR CLEANING, OPERATION & CALIBRATION OF KARL FISHER APPARATUS

 1.0              OBJECTIVE

To lay down the procedure for operation of Karl Fisher Titrator

2.0              SCOPE

This SOP shall be applicable to Karl Fisher Titrator used in QC Dept.

3.0              RESPONSIBILITY

3.1              Chemist QC and above shall be responsible for the preparation and execution of this SOP

3.2              Sr. Chemist QC & above and QA Head shall be responsible for the checking and approval of this SOP.

4.0              ACCOUNTABILITY

Head QC

5.0              PROCEDURE

5.1              Cleaning

5.1.1        Ensure that power supply to the Karl Fisher Titrator apparatus is switched ‘OFF’ before cleaning and plug shall be removed from the socket.

5.1.2        Karl Fisher Titrator apparatus shall be kept on a clean table/platform.

5.1.3        Platform of Karl Fisher Titrator shall be wiped with a dry lint the free cloth on a daily basis so that there will be no dust particles on the Karl Fisher Titrator.

5.2              Operation

5.2.1      Ensure that place the titration the vessel in the space provided on the instrument & shall be tightened using two screws fully, but not excessively.

5.2.2        Ensure that amount the calcium chloride/silica gel G crystal shall be filled in the bulb of the bottle.

 

5.2.3        Ensure that the KF reagent shall be filled in the bottle which connects to the instrument with a delivery tube.

5.2.4        Ensure that the magnetic bar shall be put in the moisture titration vessel.

 

5.2.5        Ensure that after clamping, the beaker shall touch the circular stirring table disc.

 

5.2.6        Ensure that the rubber cork shall be removed from the hole provided on the solenoid valve to pour sufficient K.F.  grade methanol into the beaker so that the platinum wire of the sensors shall be fully immersed (all additions into the beaker are to be done through the hole).

 

5.2.7        Ensure that the rubber cork shall be replaced.

 

5.2.8        Ensure that the instrument shall be connecting to the mains and switch ‘ON’.

 

5.2.9        Ensure that the motor stirrer shall be switch ‘ON’.

 

5.2.10    Ensure that the speed of the stirrer shall be adjust such that the wired ends of the sensors do not get exposed.

 

5.2.11    Ensure for the pressing of ‘STARTS’ key and the massage shall be appearing as ADD SAMPLE > TITRATION STARTED   >K F REAGENT READING with buzzer alarms.

 

5.3              TO FIND OUT TITRATION FACTOR

5.3.1        Ensure that the ‘CAL’ key shall be press and the massage shall be appearing as ADD 10 microliter distilled water.

5.3.2        Ensure that Add 10µl. distilled water in the titration vessel. ‘ENTER’ key shall be press, and the message appear as CAL IN PROGRESS > Display K F reagent reading with buzzer alarms.

5.3.3        Ensure that add 2nd time 10µl. distilled water in the titration vessel. ‘ENTER’ key shall be press, and the message shall be appearing as CAL IN PROGRESS > Display K F reagent reading with buzzer alarms.

5.3.4        Ensure that again add 3rd time 10µl. distilled water in the titration vessel. Press the ‘ENTER’ key, the message shall be appearing as CAL IN PROGRESS > Display K F reagent reading with buzzer alarms.

5.3.5        Ensure that the ‘ENTER’ key shall be press, and the massage shall be display as CONT END…..CLEAR.

5.3.6        Ensure for the select END by select key and ‘ENTER ‘key shall be press and the massage shall be appearing as CAL IN PROGRESS > Display WAIT CALCULATING FACTOR>FACTOR=0.000, K/FREADING = 0.00ml    TO TEST THE SAMPLE

A)     SOLID SAMPLE

B)     LIQUID SAMPLE

          Note 1) Grind the solid sample before use

                   2) If moisture is high, the sample quantity shall be less.

5.3.7         Ensure for the pressing of  ’START’ key, and the message shall be appear as ADD SAMPLE Add specified Sample qty. of Sample in the titration vessel > TITRATION STARTED >K F REAGENT READING with Buzzer alarms.

5.3.8        Ensure that pressing of  ’%/PPM’ key the massage shall appear WAIT CALCULATING %/PPM >%=   00.000, PPM=000000.00, mg of H2O

5.3.9        Ensure that the ENTER key shall be press to exit.

5.4              TO CLEAN THE INSTRUMENT

5.4.1        Ensure that the Methanol (washing reagent) filled bottle shall be connecting to an instrument with a delivery tube.

5.4.2        Ensure for pressing of ’CLEAN’ key and the message shall be appearing as   WAIT CALCULATING STARTED.

5.4.3        Ensure that the clean’ key shall be press TO STOP. Remove the titration vessel from the instrument and shall be replaced after Cleaning and tightened using two screws fully, but not excessively

5.4.4        Calibration Procedure

Calibration of Karl Fisher apparatus shall be done by Self-calibration by using Di- Sodium Tartrate three months’ frequency

6.0              REFERENCES

Not Applicable

7.0              ANNEXURE

Annexure No.

Title of the Annexure

Format No.

  Annexure I

 Calibration Record of Karl Fisher Titrator

 

 

8.0              ABBREVIATIONS

SOP         :           Standards Operating Procedure

QC           :           Quality Control

HOD        :           Head of the Department

QA           :           Quality Assurance

QCD        :           Quality Control Department

QAD        :           Quality Assurance Department

EQP         :            Equipment

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