Karl Fisher

SOP For Karl Fisher Apparatus(Titroline)

QC Lab Equipment's

1. Purpose

To provide a procedure for the operation of Karl Fisher titrator.

2. Scope

It is applicable for the operation of Karl Fisher titrator.

3. Responsibility

Analyst

Quality Control Manager

4. Operating Instructions

4.1. Ensure the calibration status is valid.
4.2. Ensure the instrument is clean and free from dust.
4.3. Switch on the instrument by using the switch provided on the rear side of the left. Green LED ‘O’ will glow.
4.4. Fix the KFR bottle by screwing on the plastic cap, operating bellow, holding vertically, and closing the “T” joint connection tube. Air pressure in the KFR bottle increases and lifts KFR to fill the burette, when the level crosses the ‘0’ mark remove the finger, Zero level gets automatically.
4.5. Place magnetic stirring paddle slowly by sliding into the reaction vessel and fixing the burette by lifting the burette assembly.
4.6. Pour about 20ml of methanol into the reaction vessel.
4.7. Connect jack wire to the reaction vessel and electrode terminals marked ‘e’ rear
side on the instrument.
4.8. Switch on stirrer, set required speed by using regulator, and wait for 10 to 15seconds for uniform stirring.
4.9. Add KFR by drops into reaction vessel by operating burette valve. Until pre-end point. Yellow LED glows ‘P’ is nearing the endpoint indication.
4.10. Now add KFR by drops slowly giving 10-20 seconds between additions until
Red LED ‘E’ glows continuously for 30seconds it indicates the endpoint of the titration. (Neutralisation of methanol)
4.11. Fill the burette, weigh a 1ml syringe with a needle with a small quantity of
Distilled water and add 25-100mg into the reaction vessel and close the stopper. Start magnetic stirrer, titrate up to endpoint. (ie. RED LED glows for 30secs.). Note the burette reading and calculate the water equivalent of KFR by using the following calculation.
F = M/A
Where, M à mg in water,
An A Volume of KFR consumed.
Repeat the same and take mean.
4.12. Weigh the sample in the plastic spoon add to the reaction vessel, fill the burette and start the stirrer, wait until the samples dissolve. Add KFR up to the endpoint and note the burette reading, and calculate the water content by using the following formula.
% of water content = B X F X 100 / W
Where, B – Volume of KFR consumed.
F – Factor
W – Weight of sample in mg.
4.13. After completion of analysis remove the KFR bottle from the plastic cap and fix the methanol bottle. Drain KFR from the burette and fill methanol and wash the reaction vessel.
4.14. Switch OFF the instrument and clean the place.

4.15 SIZE OF THE SAMPLE

Select a samples size, which contains 5.00 to 10.00 mg of water.

The following table will serve as a guide for samples size.

Expected moisture content Range of sample size
Bellow 1.0% Above  500 MG
1.0% to 5.0% 300 to 500 MG
5.0% to 10.0% 200 to 300 MG
Above  10% 100 to 200 MG

 

5. Precautions

5.1 Ensure that the power supply to be moisture balance is switched off before cleaning.

5.2 When a liquid sample is to be added by a syringe, always take some more volume and then inject the desired volume

5.3 Clean syringes and needless the Use dry them

5.4 While testing various samples of which the moisture contents are roughly known, test the sample having the lowest moisture first and then go on to the next in order to avoid contamination

5.5 If the moisture content of samples is an unknown and very small sample to obtain pilot reading and then adjust the size of sample accordingly.  Keep the next sample ready and if some time lapses between two titrations. Press START, get to the endpoint then add sample immediately.  This will eliminate the   error due to a lapse of time

5.6 Rinse the syringes with the sample itself 2.3 times and then take the test sample. This will remove the moisture from the syringe if any

6. Cleaning and maintenance

6.1 The TitroLine KF  Titrator should be cleaned using a damp cloth and normal household.

6.2 The bottom and the rear panel have to be treated dry. In no case must liquid penetrate into the interior of the TitroLine KF  Titrator.

6.3If any disturbance, malfunction, or another defect becomes obvious, maintenance work is required immediately.

6.4 As a principle, all work has to be done at max. intervals of 3 months.

7. Calibration

7.1Neutralize the water in methanol by Karl Fischer titrator

7.2Weigh accurately 100 mg of sodium tartrate dihydrate as a standard. Add into the

titration flask and titrate.  Record the volume required for the sample

7.3Take three reading and record  obtained results  by Karl fisher titrator

7.4 Calculate the  average water equivalent factor of Karl Fischer reagents

7.5 Standard value of titer  factor is 6.0 limit: ± 0. 5

FREQUENCY:     Every month.

FAQ:

1: What is coulometric Karl fisher/

Ans: coulometric Karl fisher(Coulometry) determines the amount of matter transformed during an electrolysis reaction by measuring the amount of electricity consumed or produced.

2. what is Mettler toledo Karl fisher

Ans: To learn about Mettler toledo Karl fisher please visit

3. What is Karl fisher water?

Ans: Karl fisher water is a technique for the determination of moisture content in any liquid or powder sample

 

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