Standard Operating Procedure for the operation and calibration of Karl-Fischer Titrator.

 

1.       Title: Standard Operating Procedure for the operation and calibration of Karl-Fischer             Titrator.
2.             Purpose:
To lay down the standard operating procedure for the operation and calibration of Karl Fischer Titrator, which is used for the moisture content analysis of Raw material in process and Finished Product in the Lab.
3.             Scope:
This procedure shall be applicable for operation and calibration of Karl Fischer Titrator at Fermenta Biotech Limited. 
 
4.             Responsibility: Research Associate/Research Scientist.
5.             Operating Procedure :
5.1  Switch ‘ON’ the instrument.
5.2  Place a burette in bottle filled with Karl Fischer Reagent.
5.3  Place the platinum electrode in the glass beaker filled with moisture free methanol.
5.4 Click on the ‘Start’ button and burette will be filled by Karl Fischer reagent.
5.5 Start the stirrer. Neutralization of the methanol will start.
5.6 System will give Beep sound after the neutralization of the methanol get completed.
5.7 After that , add the sample and press ‘START’ to start the sample analysis.
5.8 after the completion of the analysis system will give beep sound again.
5.9 Click on the “SMPL mg/ ml” button and add the weight of the sample.
5.10 Click on the “PPM” button to get the moisture content value of the sample.
 
            Calculation:
                                                               V X   F   X 100
                                    Water content =      -------------------- =                 %w/w
                                                                     W X1000
             Where:  V         = Volume in ml of standard Karl- Fisher used.
                          W         = Weight of sample in gm.
                           F         = Karl Fisher water equivalent factor
 
6.0 Calibration of the Karl Fischer Titrator :
6.1 Fill the burette with Karl Fischer Reagent .
6.2  Take the moisture free methanol in the glass beaker where platinum electrodes are dipped in the
      Methanol.
6.3 Click on the “START” button to neutralize methanol.
6.4 After the neutralization of methanol system will give “BEEP” sound.
6.5 Add the water drop in the methanol and again press “START”
6.6 Wait till the moisture analysis get completed.
6.7  Note down the reading of the analysis and calculate the factor as per the following calculation.
6.8 Repeat the above procedure for six times and note down mean of the six readings.
 
Calculation:
                                                                           W
                               Water Equivalent Factor =   -----------     =               mg/ml                                                                                                          V
                    Where: V   = volume in ml. of standard Karl-Fisher used.
                     W   = weight of water in mg.
 
Determination of K-F water equivalent factor
 

Date	Weight of water drop  (in mg)	Volume of standard Karl Fischer used ( in ml)	K-F water equivalent factor = Weight of water drop Volume of standard Karl Fischer used (in ml)	Average K-F water equivalent factor	Signature

 
            Calculation:
                                                               V X   F   X 100
                                    Water content =      -------------------- =                 %w/w
                                                                     W X1000
             Where:  V         = Volume in ml of standard Karl- Fisher used.
                          W         = Weight of sample in gm.
                           F         = Karl Fisher water equivalent factor
7.0        Abbreviations:

mg	:	milli gram
w/w	:	weight / weight
ml	:	milli liter
gm	:	Gram
KF	:	Karl Fischer

8.0 RECORDS :
      Nil
                                                                
9.0 References: : Karl Fischer Titrator Manual and  ICH Guidelines Q7.