Determination of Water Content in Glycerine monostearate Using Karl Fischer Titration

Product Group

Alcohols, Esters of carboxylic acids

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%).

Esters of carboxylic acids

Esters of carboxylic acid can be analysed analogously to the hydrocarbons according to standard Karl Fischer methods. Long-chain compounds require the addition of solubilisers, e.g. long-chain alcohols or chloroform. Unsaturated compounds can usually be titrated in the same way. Recommended methods are both the volumetric titration with one or two component reagents, as well as the coulometric analysis. The latter is predominantly applied for low water concentrations (< 0.1 %).

Special Information concerning the sample and the methods

At room temperature glycerine monostearate dissolves only slowly in alcoholic media. Volumetric titration is recommended at 50 °C

Titration one component system

Reagents:

Titrant
188005 Aquastar™ - CombiTitrant 5 - One component reagent for volumetric Karl Fischer titration, 1 mL = approx. 5 mg water
or
188002 Aquastar™ - CombiTitrant 2 - One component reagent for volumetric Karl Fischer titration, 1 mL = approx. 2 mg water

Solvent
50 mL 188008 Aquastar™ - CombiSolvent - Methanol-free solvent for volumetric Karl Fischer titration with one component reagents
or
50 mL 188021 Aquastar™ - CombiSolvent fats - Solvent for volumetric Karl Fischer titration with one component reagents for fats

Titration Parameters:
Stirring time: 3 - 5 min.
Titration temperature 50 °C
Default titration settings, e.g.:
I(pol) = 20 - 50 µA, U(EP) = 100 - 250 mV
Stop criterion: drift < 20 µL/min

Sample size:
1 g

Procedure:
The titration medium is first placed into the cell, heated to titration temperature and titrated dry by means of the titrant. Then the sample is added from a weighing boat (exact sample weight determination by weighing of weighing boat before and after addition) and the titration is started. For complete dissolution of the sample a stirring time of 3 to 5 minutes is recommended.

Titration two component system

Reagents:

Titrant
188010 Aquastar™ - Titrant 5 - Titrant for volumetric titration with two component reagents, 1 mL = approx. 5 mg water
or
188011 Aquastar™ - Titrant 2 - Titrant for volumetric titration with two component reagents, 1 mL = approx. 2 mg water

Solvent
50 mL 188016 Aquastar™ - Solvent oils & fats - Solvent for volumetric Karl Fischer titration with two component reagents for oils & fats

Titration Parameters:
Stirring time: 3 - 5 min.
Titration temperature 50 °C
Default titration settings, e.g.:
I(pol) = 20 - 50 µA, U(EP) = 100 - 250 mV
Stop criterion: drift < 20 µL/min

Sample size:
1 g

Procedure:
The titration medium is first placed into the cell, heated to titration temperature and titrated dry by means of the titrant. Then the sample is added from a weighing boat (exact sample weight determination by weighing of weighing boat before and after addition) and the titration is started. For complete dissolution of the sample a stirring time of 3 to 5 minutes is recommended.

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:
Stirring time: 120 sec.
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:
0.3 - 0.5 g

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 added from a weighing boat (exact sample weight determination by weighing of weighing boat before and after addition) and the titration is started. For complete solution of the sample a stirring time of 120 seconds is recommended.

Coulometry without diaphragm

Reagents:

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

Titration Parameters:
Stirring time: 120 sec.
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:
0.3 - 0.5 g

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 added from a weighing boat (exact sample weight determination by weighing of weighing boat before and after addition) and the titration is started. For complete dissolution of the sample a stirring time of 120 seconds is recommended.

Materials

     
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