Determination of Water Content in Miglyol, Neutral oil Using Karl Fischer Titration

Product Group

Cosmetics, Pharmaceuticals

General Information concerning the product group

Cosmetics

Cosmetics on an aqueous and alcoholic basis can be titrated without problems according to the Karl Fischer (KF) method. Due to the often high water concentration of the emulsions small samples are required. The accuracy of analysis is determined through exact sampling, weighing and adding. The coulometric method is unsuitable for most emulsions. Fatty and oily preparations are insoluble in methanolic KF solvents and require the addition of a solubiliser, or respectively titration with specific KF solvents for oils and fats.

Pharmaceuticals

Pharmaceutical products are often characterized by complex formulations. Difficulties observed during Karl Fischer determination are often caused by the limited solubility. In some cases side reactions have to be considered. In dependance of composition and properties of the formulations, various measures are necessary for an undisturbed Karl Fischer determination. In pharmaceutical guidelines (USP, Ph Eur, DAB) the Karl Fischer titration is described as common method for water determination. For some substances special procedures can be found. The determination of mass loss as method for water determination is not recommended.

Special Information concerning the sample and the methods

Neutral oil dissolves inadequately in methanolic KF solvents. The addition of solubilisers or use of specific KF solvents for oils & fats is necessary. Water determination can be carried out volumetrically or coulometrically. Due to the low water content of the sample, the volumetric method requires the use of a titrant with low factor.

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 188021 Aquastar™ - CombiSolvent fats - Solvent for volumetric Karl Fischer titration with one component reagents for fats

Titration Parameters:
Stirring time: 60 sec.
Default titration settings, e.g.:
I(pol) = 20 - 50 µA, U(EP) = 100 - 250 mV
Stop criterion: drift < 20 µL/min

Sample size:
5 - 10 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) or volumetric pipette and the titration is started. For complete dissolution of the sample a stirring time of 60 seconds is recommended. It is possible to analyse approx. 10 g oil before the KF solvent must be changed.

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

Sample size:
5 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) or volumetric pipette and the titration is started. For complete dissolution of the sample a stirring time of 60 seconds is recommended. It is possible to analyse approx. 10 g oil before the KF solvent must be changed.

Coulometry with diaphragm

Reagents:

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

Anolyte
80 mL 109255 Aquastar™ - CombiCoulomat frit - Coulometric Karl Fischer reagent for cells with diaphragm
and
20 mL 803463 Decanol - as solubiliser

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:
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
80 mL 109257 Aquastar™ - CombiCoulomat fritless - Coulometric Karl Fischer reagent for cells with or without diaphragm
and
20 mL 803463 Decanol - as solubiliser

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:
1 mL

Procedure:
The Karl-Fischer reagent and decanol are 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.

Materials

     
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