Calibration of Karl Fischer Apparatus : Pharmaguideline

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Calibration of Karl Fischer Apparatus

Learn how to calibrate the Karl Fisher Apparatus using Disodium Tartrate (Standard value = 15.66 %).

CALIBRATION PROCEDURE

1. Switch on the main switch and switch on the instrument as per the operating procedure.
2. Reset the instrument and then press “MODE” key to the red light will glow on “CONC” position.
3. Press “RUN” key to neutralizing the methanol and the red light will glow on “READY” position. Once again press “RUN” key to the red light will glow on “WEIGHT” position.
4. Weigh accurately about 0.005 to 0.05 gm (5 to 50 mg) 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, the display will show the result in mg of H2O / 5 ml of KF reagent.

7. Repeat the same procedure by resetting the instrument to obtain 3 values for the factor of KF reagent which is not differing by 0.3 %.
8. Calculate the mean of all 3 values 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. 11. Press “RUN” key and enter stir time in seconds if required.
12. Again press “RUN” key to the red light will glow on “BUSY” mode and by pressing once again “RUN” key titration can be started.
13. At the end of the titration, the display will show the result in % of water content.
14. Repeat the same procedure by resetting the instrument to obtain 3 values of water content having not more than + 0.3 % deviation of the standard water content of Disodium tartrate (Standard value = 15.66 %) and record the result in calibration log.
15. Affix the calibration label on the instrument.
16. Drain off the titration vessel and dip the electrode in methanol, switch off the instrument switch off the mains.
Related: Water Content Determination by Karl Fischer

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 Di-Sodium 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 :





Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of pharmaguideline.com, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
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