Get the latest updates from us for free
Android App

SOP for Calibration of Karl Fischer Apparatus


Standard operating procedure to calibrate the Karl Fischer Apparatus with Disodium tartrate.

1.0  OBJECTIVE

       To calibrate the equipment for reliable and accurate results.

2.0  SCOPE

       This procedure is applicable to calibrate the karl fischer apparatus, installed in quality control department.

3.0  RESPONSIBILITY

3.1  Doing      : Technical Assistant
3.2  Checking : Executive /Manager

4.0  ACCOUNTABILITY

       Head of the Department

5.0  PROCEDURE

       Frequency : Once in a month
5.1  Operate the instrument as per SOP.

5.2  FOR BURETTE CALIBRATION

5.2.1  Place the burette outlet in 10ml standard calibrated measuring cylinder
5.2.2  Press the START key and then press ENTER key. Then again press START key.
5.2.3  When the display show 3ml, immediately press STOP key.
5.2.4  Note down the observed volume of karl fischer reagent in the measuring cylinder.
5.2.5  Now repeat step No 5.2.2 to 5.2.4 for 6ml and 9ml.
5.2.6  Record the obtained volume and displayed volume in the enclosed format.
5.2.7  The volume displayed on instrument and the volume collected in cylinder should not vary by more than ± 0.1 ml, otherwise follow the S.O.P.
5.2.8  Record the results in Annexure.
5.2.9  Frequency of calibration : Once in a month.

Related: Water Content Determination by Karl Fischer

5.3  FOR INSTRUMENT PERFORMANCE

5.3.1  Add accurately weighed 100mg of Disodium tartrate into the titration vessel containing neutralized methanol and test for water content.
5.3.2  Calculate the % water by using the formula given below.
                                Volume of KFR consumed in ml X 100 X Factor
% Water (W/W) = --------------------------------------------------------------
                                             Weight of disodium tartrate in mg
5.3.3  The performance of the instrument is satisfactory if the difference between the obtained values are within the tolerance limit of 15.66 ± 5% i.e. 14.87% -16.44, otherwise follow the S.O.P.
5.3.4  Repeat the step 5.3.1 & 5.3.2 and take total five reading.
5.3.5  Record the results in Annexure-I.
5.3.6  Frequency of calibration : Once in a month.

6.0  ABBREVIATIONS

6.1  % = Percentage
6.2  mg = milligram
6.3  W/W = Weight by Weight
6.4  S.O.P. = Standard operating procedure number
6.5  ml = mililiter
6.6  KFR = Karl fischer reagent



ANNEXURE-I
Q. C. DEPARTMENT
PERFORMANCE CHECK REPORT OF KARL FISCHER APPARATUS
  
PERFORMANCE CHECK  DATE
DATE OF LAST PERFORMANCE CHECK DONE
NEXT DUE FOR
PERFORMANCE CHECK

INSTRUMENT DETAIL
INSTRUMENT NAME
INSTRUMENT MAKE
INSTRUMENT
IDENTIFICATION NO.

OBSERVATION

Sr. No.
Wt. taken of di-sodium   tartrate
(mg)
Volume of KFR required
(ml)
Factor
mg. H2O/ml
% Water obtained
Tolerance
1
14.87 % to 16.44 %
2
3
4
5
% RSD :
(NMT 1.0 %)

Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
Email: .moc.enilediugamrahp@ofni Need Help: Ask Question


Be the first to comment!

Post a Comment