Application
Water determination
according to Karl Fischer in
organic liquids
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Application
Use
This method is a general description how to determine the water content in organic liquids such as methanol,
isopropyl alcohol, glycol and other similar liquids.
Appliances
• Titrator: TL 7500 KF (TL 7500 KF 05/10/20) or TL 7750 with KF accessories
• µl syringe or one-way insulin syringe with needle (> 0.8 mm)
• 4 digit balance
Electrodes
• KF 1100 with fixed cable
Reagents
• Titration agent: 1 component titrant or 2 component Titrant with 2 or 5 mg/ml concentration
• Solvent: dry methanol, combi solvent or a two component solvent/solvent E
Description
The setup of the instrument is described in the operating manual.
Determination of the titrant concentration
The determination of the titrant concentration (titer determination, standardization) is necessary before the
sample titration and we recommend a weekly titer determination.
Fill the titrant in the exchange unit and the solvent in the titration vessel as described in the manual. Do not
forget to enter the concentration of the titrant (e.g. 2 or 5) into the WA unit. Otherwise the drift determination
is wrong. Load the standard method (default method) Titer 1-Comp. (liq. std.) or Titer 2-Comp. (liq. std.) as
user method and start the method.
The KF titrator starts automatically the conditioning routine. The solvent and also the titration vessel contents
also water which has to be titrated before. When the conditioning is ready you see “Conditioning ready” on
the screen.
The conditioning remains active until the actual titration is started by pressing <F1/START>.
• Open the glass ampoule with the water standard (10 mg/g) and rinse the 10 ml syringe 1-2 times
with 0.5 - 1 ml of the standard.
• Fill the complete content of the liquid standard then into the syringe and wipe then the needle with a
tissue.
• Place the syringe with needle on a 4 digit balance. Maybe use a beaker, place this beaker on the
balance and put the syringe then into the beaker during the weighing process.
• Press the tara button.
• Press Start/F1 to interrupt the conditioning. You are prompted immediately to add the sample.
• Please add between 0.5 and 1 g standard for a 2 mg/ml titrant and 1.5 – 2 g for a 5 mg/ml titrant
through the septum,
• Place the syringe again on the balance and read the absolute weight form the balance (ignore the
minus)
• Enter the sample ID (optional)
• Enter the sample weight and confirm with ENTER/F1
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Application
The titrator starts then automatically the titration. The result will appear on the screen at the end of the
titration. Repeat the titer determination two times (total 3 times). The average value of the titrant
concentration in mg/ml will be stored automatically in the exchange unit and used for the calculation of the
sample water concentration.
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Application
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Application
Sample Titration
The procedure for organic liquid samples is the sample as for the liquid standard. The only difference is the
used method. Please load the default method “Sample 1 Comp.” or “Sample 2 Comp.” for the sample
titration. Use also a suitable syringe (1, 2, 5 or 10 ml) with needle for the liquid sample.
• Rinse syringe 1-2 times with 0.5 - 1 ml of the sample. Use between 0.2 – 10 g of the sample
depending on the expected water concentration (Please refer to the enclosed table)
• Place the syringe with needle on a 4 digit balance. Maybe use a beaker, place this beaker on the
balance and put the syringe then into the beaker during the weighing process.
• Press the tara button.
• Press Start/F1 to interrupt the conditioning. You are prompted immediately to add the sample.
• Add the sample trough the septum
• Place the syringe again on the balance and read the absolute weight form the balance (ignore the
minus)
• Enter the sample ID (optional)
• Enter the sample weight and confirm with ENTER/F1
The titrator starts then automatically the titration. The result will appear on the screen at the end of the
titration.
Recommended sample amounts:
expected water amount Titre 2 mg/ml Titre 5 mg/ml
10 ppm – 100 ppm > 10 g -----
100 – 500 ppm 2- 10 g -----
500 ppm – 1000 ppm (0.1 %) 1- 5g 5 – 10 g
0.1 % - 10 % 0.5 – 1 g 1–2g
1 % - 10 % ----- 0.1 – 2 g
10 % - 100 % ----- max. 0.1 g
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Application
Methods
Sample titration (page 1)
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Application
sample titration (page 2):
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Application
Hints
If you have any questions concerning the application, you are welcome to contact us.
Literature
SI Analytics GmbH Phone: +49 (0) 6131 / 66 – 5062
Hattenbergstr. 10 +49 (0) 6131 / 66 – 5118
55122 Mainz Fax: +49 (0) 6131 / 66 – 5001
Germany E-Mail:
[email protected] Homepage: www.si-analytics.com
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