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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