Karl fisher apparatus calibration in pharmaceuticals
CALIBERATION PROCEDURE1. Switch on the main switch and instrument switch and proceed the step (1) to (6) as describe in operational procedure.
2. Reset the instrument and then press “MODE” key so the red light will glow on “CONC” position.
3. Press “RUN” key to neutralize the methanol and the red light will glow on “READY” position. Once again press “RUN” key so red light will glow on “WEIGHT” position.
4. Weigh accurately about 0.005 to 0.05 gm (5 to 50 ml) of water with the syringe and enter the weight in gram.
5. Press the “RUN” key so that red light will glow on “BUSY” position. Again press the “RUN” key so titration will starts.
6. At the end of the titration display will show result in mg of H2O / 5 ml of KF reagent.
7. Repeat the same procedure by resetting the instrument to obtain 3 value for the factor of KF reagent which is not differ by 0.3 %.
8. Calculate the mean of all 3 value and to enter it in memory, Press “RESET” key then “MODE” key once to glow red light on “CONC” position. Enter the value and again press “CONC”.
9. Reset the instrument and red light will glow on “WEIGH” position.
10. Weigh accurately about 0.05 gm to 0.15 gm of “Disodium tartrate” and enter the weigh in gm. Press “RUN” key and enter stir time in seconds if required.
11. Again press “RUN” key so red light will glow on “BUSY” mode and by pressing once again “RUN” key titration can be started.
12. At the end of the titration display will show result in % of water content.
13. Repeat the same procedure by resetting the instrument to obtain 3 values of water content having not more than + 0.3 % deviation of standard water content of Disodium tartrate (Standard value = 15.66 %) and record the result in calibration log.
14. Affix the calibration label on the instrument.
15. Drain off the titration vessel and dip the electrode in methanol, switch off the instrument switch off the mains.
CALIBRATION LOG
Instrument : ____________Code No. : ___________
Make : ____________
Model : ___________
Determination of Kf reagent factor.
Sr.No.Weight of Water (In gm)Factor of KF reagent (In mg H2O/5 ml)Mean factor of KF reagent (In mg H2O/5 ml)Remark
1.
2.
3.
Determination of water content of DiSodium Tartrate (15.66% ± 0.3 %)
Sr.No.Wt. of DiSod. Tartrate (In gm)Water of DiSod. Tartrate (In % )Mean Water of DiSod. Tartrate (In % )Remark
1.
2.
3.
Calibration Status : Satisfactory / Not Satisfactory
Next Calibration Due :
Calibrated By : Checked By :Date : Date :
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