PSCC STANDARD OPERATING PRECEDURE

TITLE: OPERATING KARL FISHER TITRATION INSTRUMENT

EFFECTIVE DATE: NOVEMBER 1, 2018 SOP NO.: LAB-0001
REVISON: 0 TOTAL PAGES: 2

PSCC STANDARD OPERATING PRECEDURE

TITLE: OPERATING KARL FISHER TITRATION INSTRUMENT

EFFECTIVE DATE: NOVEMBER 1, 2018 SOP NO.: LAB-0001
REVISON: 0 PAGE: 2

CREATED BY APPROVED BY APPROVED BY APPROVED BY

NAME
TITLE
DATE
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1.0. PURPOSE :
To provide a procedure for the operation of Karl Fisher titrator, MANUFACTURER
& MODEL : Lasco, KFTA.

2.0. SCOPE :
Applicable for Karl Fisher titrator instrument in the quality control laboratory.
MANUFACTURER & MODEL : Lasco, KFTA

3.0. RESPONSIBILITY:
All QA/QC students.

4.0 DEFINITION:
Karl Fisher titrator instrument used to determine the water content of a sample.
A Macro Karl Fischer Instrument uses standardized volumetric solution to
determine the amount of moisture in samples, and is used when the expected
result is between 1 mg to 100 mg of water. A Micro Karl Fischer Instrument uses
an electrical current (coulometry) for determination of moisture in samples, and
is used when the expected result is between 10 μg to10 mg of water.

5.0. PROCEDURE: Commented [RA1]: Include spaces between paragraphs

Formatted: Space After: 12 pt

5.1. Ensure the calibration status is valid.
Commented [RA2]: Fix the alignment among all
5.2. Ensure the instrument is clean and free from dust. paragraphs, like:
5.0 Procedure:
5.3. Switch on the instrument by using switch provided on rear side of left. 5.1 Ensure …
When the instrument is ON, the Green LED ‘O’ will glow. 5.2 Ensure …

Formatted: Space After: 12 pt

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PSCC STANDARD OPERATING PRECEDURE

TITLE: OPERATING KARL FISHER TITRATION INSTRUMENT

EFFECTIVE DATE: NOVEMBER 1, 2018 SOP NO.: LAB-0001
REVISON: 0 TOTAL PAGES: 2

5.4. Fix Karl Fischer Reagent (KFR) bottle by screwing on the plastic cap, Commented [RA3]: When we want to use abbreviation
operate bellow, holding instead of the full name, the first time we mentioned the
vertically and closing the “T” joint connection tube. full name with the abbreviation.
5.5. Air pressure in KFR Formatted: Indent: Left: 0", Hanging: 0.49"
bottle increases and lifts KFR to fill burette., w When level crosses ‘0’ mark,
Formatted: Indent: Left: 0", Hanging: 0.49"
remove finger, Zero level gets automatically.
Commented [RA4]: Automatic? No pushing sth? You
5.5. Place the magnetic stirring paddle slowly by sliding in to the reaction
mention later to remove finger but no mentioning of
vessel
pushing/putting finger somewhere, then to remove it!
and fix the burette by lifting the burette by lifting the burette assembly.
Better to make it a separate step.
5.6. Pour about 20ml of methanol into the reaction vessel.
5.7. Connect jack wire to reaction vessel and electrode terminals marked ‘e’ Formatted: Indent: Left: 0", Hanging: 0.59"
rear side on the instrument.
5.8. Switch on stirrer, set required speed by using regulator, wait for 10 to
15 seconds for uniform stirring.
5.9. Add KFR by drops into reaction vessel by operating burette valve. Until
pre end point. Yellow LED glows ‘P’ is nearing end point indication.
5.10. ANow add KFR by drops slowly giving 10-20 seconds between additions Commented [RA5]: Don’t use NOW or any terms used
until Red LED ‘E’ glows continuously for 30 seconds which it indicates in books/stories
the end Formatted: Indent: Left: 0.33", Hanging: 0.36"
point of the titration . ( Neutralisation of methanol).
5.11. Fill the burette with wh?,
5.12. wWeigh a 1ml syringe with needle with a small quantity
of distilled water
5.13. and aAdd 25-100mg into the reaction vessel and close
the stopper. Start magnetic stirrer, titrate up to end point .(ie. REDRED Formatted: Indent: Left: 0", Hanging: 0.69"
LED
glows for 30 seconds.).
5.14. Note the burette reading and calculate the water Formatted: Indent: Left: 0.2", Hanging: 0.49"
equivalent of KFR by using the following calculation.
F = M/A
Where, M - mg in water;
A - Volume of KFR consumed.
Repeat the same and take mean.
5.12.Weigh the sample in the plastic spoon then add it to the reaction vessel.
5. 13., fFill the
burette and start the stirrer,.
5.14. wWait until samples dissolves, then . Aadd KFR up to Formatted: Indent: Left: 0", Hanging: 0.59"
the end point.
5.15. and nNote the burette reading.
5.16. , and cCalculate the water content Formatted: Indent: Left: 0", Hanging: 0.59"

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PSCC STANDARD OPERATING PRECEDURE

TITLE: OPERATING KARL FISHER TITRATION INSTRUMENT

EFFECTIVE DATE: NOVEMBER 1, 2018 SOP NO.: LAB-0001
REVISON: 0 TOTAL PAGES: 2

by using the following formula:. Commented [RA6]: Break down into single easy to
% of water content = B X F X 100 / W follow steps
Where, B - Volume of KFR consumed.
F - Factor
W - Weight of sample in mg.
5.13. After completion of analysis remove the KFR bottle from the plastic cap
and fix the methanol bottle. Drain KFR from the burette and fill
methanol and wash the reaction vessel.
5.14. Switch OFF the instrument and clean the place.

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