Determination of Water Content in Glycerine, Glycerol, 1,2,3-Propantriol Using Karl Fischer Titration

Product Group

Alcohols

General Information concerning the product group

Alcohols

Water determination after Karl Fischer poses no problems for most alcohols. Alcohols are easily soluble in the common Karl Fischer working media. Only alcohols with very long chains require the addition of solubilisers. Side reactions are not to be expected. Suitable methods are both the volumetric titration with one or two component reagents as well as the coulometric determination. The latter method is predominantly applied for low water concentrations (< 0.1%).

Special Information concerning the sample and the methods

Glycerine is easily soluble in methanol and alcoholic Karl Fischer solvents. The chemical structure does not lead to expectation of any interferences. Thus titration can be carried out according to standard methods, although volumetry is preferred. Due to its hygroscopic properties, however, glycerine requires careful sample handling.

Titration one component system

Reagents:

Titrant
188005 Aquastar^® - CombiTitrant 5 - One component reagent for volumetric Karl Fischer titration, 1 mL = approx. 5 mg water

Solvent
50 mL 188008 Aquastar^® - CombiSolvent - Methanol-free solvent for volumetric Karl Fischer titration with one component reagents
or
50 mL 188009 Aquastar^® - CombiMethanol - Solvent for volumetric Karl Fischer titration with one component reagents, max. 0.01 % water

Titration Parameters:
Default titration settings, e.g.:
I(pol) = 20 - 50 µA, U(EP) = 100 - 250 mV
Stop criterion: drift < 20 µL/min

Sample size:
0.5 - 2 mL

Procedure:
The titration medium is first placed into the cell and titrated dry by means of the titrant. Then the sample is added with a syringe (exact sample weight determination by weighing of syringe before and after injection) and the titration is started.

Titration two component system

Reagents:

Titrant
188010 Aquastar^® - Titrant 5 - Titrant for volumetric titration with two component reagents, 1 mL = approx. 5 mg water

Solvent
50 mL 188015 Aquastar^® - Solvent - Solvent for volumetric titration with two component reagents

Titration Parameters:
Default titration settings, e.g.:
I(pol) = 20 - 50 µA, U(EP) = 100 - 250 mV
Stop criterion: drift < 20 µL/min

Sample size:
0.5 - 2 mL

Procedure:
The titration medium is first placed into the cell and titrated dry by means of the titrant. Then the sample is added with a syringe (exact sample weight determination by weighing of syringe before and after injection) and the titration is started.

Coulometry with diaphragm

Reagents:

Catholyte
5 mL 109255 Aquastar^® - CombiCoulomat frit - Coulometric Karl Fischer reagent for cells with diaphragm

Anolyte
100 mL 109255 Aquastar^® - CombiCoulomat frit - Coulometric Karl Fischer reagent for cells with diaphragm

Titration Parameters:
Default coulometer settings for cell with diaphragm:
For end point indication, e.g.:
I(pol) = 5 - 10 µA, U(EP) = 50 - 100 mV
Stop criterion: drift < 10 µg/min

Sample size:
0.1 mL

Procedure:
The Karl-Fischer reagent is placed into the cathode and anode compartment of the titration cell with diaphragm. The coulometer is started and the solvent is titrated dry. After preliminary titration and stabilisation of drift the sample is injected into the titration cell with a syringe (exact sample weight determination by weighing of syringe before and after injection) and the water determination is started.

Coulometry without diaphragm

Reagents:

Working medium
100 mL 109257 Aquastar^® - CombiCoulomat fritless - Coulometric Karl Fischer reagent for cells with or without diaphragm

Titration Parameters:
Default coulometer settings for cell without diaphragm:
For end point indication, e.g.:
I(pol) = 5 - 10 µA, U(EP) = 50 - 100 mV
Stop criterion: drift < 10 µg/min

Sample size:
0.1 mL

Procedure:
The Karl-Fischer reagent is placed into the titration cell without diaphragm. The coulometer is started and the solvent is titrated dry. After preliminary titration and stabilisation of drift the sample is injected into the titration cell with a syringe (exact sample weight determination by weighing of syringe before and after injection) and the water determination is started.