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SOP NO.: |
QC00X-01 |
EffectiveDate: |
DD/MM/YY |
Company Logo |
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Supersedes : |
NA |
Page No.: |
01 of end |
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Department: |
Quality Control |
Review Date: |
DD/MM/YY |
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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
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S.No |
Details |
Format No. (Current version) |
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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
3.1 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
Prepared By Checked By Approved By
Sign & Date
Name & Dept QA Executive QC Manage QA Manager
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