1.0 PURPOSE:
2.0 SCOPE:
This procedure covers the operation, cleaning and calibration of KF Coulometer which is used in Quality Control department of (Company name).
3.0 DEFINITIONS:
Nil.
4.0 RESPONSIBILITY:
4.1 Quality control chemist shall be responsible to Operation, cleaning and calibration of KF Coulometer and maintains the record.
4.2 Head – Quality Control or his designee to ensure compliance.
5.0 PROCEDURE:
5.1 Switch ON the main power supply.
5.2 Switch ON the KF Coulometer to start the instrument and use the button to start the stirrer.
5.3 Operate the KF Coulometer by using a keyboard which is provided with the instrument.
5.4 Selection of existing Method:
5.4.1 Press “USER METH” button on keyboard.
5.4.2 Select “Recall” by pressing “ENTER” button.
5.4.3 Select the required method using navigation keys and press “ENTER” button to confirm the method.
5.5 Press “START” on keyboard for conditioning of Coulometer Solution.
5.6 It displays as ‘wait’ till the conditioning reaches. After conditioning is reached it displays as ‘Ready’.
5.7 Press the “SAMPLE DATA” button on the keyboard and give the sample details.
5.8 Result units shall be ppm, mg, pg or %.
5.9 Never insert the magnetic stirring rotor in the vessel when it is kept on the machine. The pull of the powerful magnet inside the machine will break the vessel.
5.10 Changing of KF reagent after each determination is not necessary since individual determinations can be carried out in succession in the same reagent solution. Change the reagent solution in reaction vessel when delay in conditioning is observed.
5.11 Molecular sieves should be changed whenever necessary.
5.12 Pour the coulometer solution in titration vessel minimum of 100 ml.
5.13 Operation procedure for Thrmoprep:
5.13.1 Switch on the instrument of thrmoprep.
5.13.2 Operate the 860 thrmoprep by using a keyboard which is provide the Instrument.
5.13.3 Press ‘FLOW’ Button for the passage of filtered air.
5.13.4 Select one of the preset temperatures using the ‘TEMP’ Key.
Note: The carrier gas should emerge from the tip of the heating tube in the working medium as tiny bubbles and be spun there forcefully. Alter the stirring rate if necessary. The tip of the Syringe should be immersed into the vial.
5.14 Determination of water content in sample:
5.14.1 Direct addition method:
5.14.1.1 Press the ‘START’ button for conditioning of Coulometer Solution.
5.14.1.2 After conditioning is reached, Enter the sample details.
5.14.1.3 Press ‘START’ and add the specified sample quantity as per STP in the titration vessel through the lid.
5.14.1.4 Give the sample weight and press the button ‘ENTER’.
5.14.1.5 After completion of analysis the result will be printed automatically.
5.14.2 Using the Thermoprep:
5.14.2.1 Place vial/sample in vial, in a suitable vial holder into the Thermoprep.
5.14.2.2 Heat the sample as per temperature given in STP.
5.14.2.3 Press ‘START’ and Pierce the syringe into the vial and ensure that the bubbles are evolving in titration vessel.
5.14.2.4 Allow the moisture completely transfer into titration vessel as per the time mentioned in STP.
5.14.2.5 Enter the sample weight and press ‘START’.
5.14.2.6 After completion of analysis the result will be printed automatically.
5.15 Monthly performance verification procedure:
5.15.1 Weigh 50mg Di Sodium Tartrate into clean dried 10 ml vial, seal it securely and heat the DST at 1500C. Keep the sample heating time as 300 sec.
5.15.2 Following the procedure described in step no. 5.14.2.3 to 5.14.2.6 determine the water content.
5.15.3 Perform the above analysis in five replicates.
5.15.4 Enter the details in performance verification record as per Annexure-I.
5.15.5 Acceptance criteria:
5.15.5.1 The moisture content should be 15.66% ± 0.3.
5.15.5.2 The relative standard deviation for 5 trials shall not be more than 2.0%.
5.15.6 Calibration Schedule: Once in 30 days and after any major Maintenance job.
6.0 ABBREVIATIONS:
SOP : Standard Operating Procedure
KF : Karl Fischer
% : Percentage
Mg : Milligram
Pg : Microgram
Ppm : Parts per Million
ml : Milli liter
7.0 REFERENCES:
Nil.
8.0 LIST OF ANNEXURES:
Annexure-I: Monthly performance verification record for KF Coulometer.
