Determination of Water Content in Phenol urea formaldehyde resins Using Karl Fischer Titration

Product Group

Polymers, plastics

General Information concerning the product group

Polymers, plastics

Polymers are hardly or not at all soluble in the common Karl Fischer solvents. In order to extract the water trapped within the sample the plastic must be dissolved or swollen by means of an appropriate solvent to such an extent that the water can be released through diffusion. Which solvent is appropriate depends on the properties of the plastic. Some substances can be analysed through direct volumetry under addition of a solubiliser (e.g. polyvinyl acetate). Most substances require external extraction (e.g. polyamide), whereby an aliquot of the sample solution is analysed either volumetrically or coulometrically. Here too, the addition of a solubiliser is necessary in order to avoid renewed precipitation of the sample in the KF solution. For most plastics the KF oven technology is a suitable alternative. The water released through heating of the granulated or powdered sample in an oven is subsequently determined according to the Karl Fischer methodology. Due to the very low water concentration the combination with coulometry is preferred.

Special Information concerning the sample and the methods

These substances can directly be analysed volumetrically under addition of 30 % formamide to the solvent. Titration at 50 °C accelerates the release of water. The coulometric method is not recommended.

Titration one component system

Reagents:

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

Solvent
40 mL 188009 Aquastar™ - CombiMethanol - Solvent for volumetric Karl Fischer titration with one component reagents, max. 0.01 % water
and
20 mL 109684 Formamide - as solubiliser

Titration Parameters:
Stirring- / extraction time: 180 sec.
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:
0.5 g

Procedure:
The titration medium is first placed into the cell, heated up to about 50 °C 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 / extraction of the sample a stirring time of 180 seconds is recommended.

Titration two component system

Reagents:

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

Solvent
40 mL 188015 Aquastar™ - Solvent - Solvent for volumetric titration with two component reagents
and
20 mL 109684 Formamide - as solubiliser

Titration Parameters:
Stirring - / extraction time: 180 sec.
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 g

Procedure:
The titration medium is first placed into the cell, heated up to about 50 °C 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 / extraction of the sample a stirring time of 180 seconds is recommended.

Materials

     
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