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inatech@skynet.be 07 / 2003
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The determination of water in plaster (gypsum)

(CaSO4 * ½ H2O) – comparison to analysis of CaSO4 * 2
H2O
The water content of various plaster samples (CaSO4 * ½ H2O) was determined using the
Karl-Fischer-Titration coupled with complete cure technology. In doing so, one can differ
between adsorbed surface water and chemically bonded crystallization water. The plaster’s
degree of purity can be determined from the portion of crystallization water.

The main principle

The sample is weighed in the sample container (weighted sample approx. 30-40 mg). After
starting analysis, the sample container is placed into the complete cure chamber of the
AQUA 40.00. The complete cure takes place in a continuous flowing inert gas stream (i.e.,
N2, Ar, or air). The gas regulation is done by using the stream controller of the inert gas
module. The gas velocity should be adjusted to 4-6 l/h. Dehumidification (drying gas) results
from two drying cartridges that are filled with molecular sieve.
A temperature program allows complete curing. The released water is transported into the
measuring cell of the AQUA 40.00 by means of the inert gas stream and then immediately
titrated.

Complete cure with a temperature gradient of 2°/min

The following Figure shows a complete cure done with a temperature gradient. The left
diagram displays total amount of water converted (water in %). The right diagram shows the
amount of water currently titrated in µg/min.
The water existing in the samples is desorbed differently. After measuring has started, the
adsorbed surface moisture is almost immediately separated. The first distinct peak at 30-40°
C in the right diagram makes this clear.
One can see a gradual increase in released water by further heating. In the range of 60° C
an upwards, a further increase in released water is noticeable. The maximum amount is
released at 120-140° C. The release of water stops at 160-180° C.
Besides the complete cure of CaSO4 * ½ H2O, the diagram also shows the complete cure of
the converted dihydrate. Here it is shown, that higher temperatures are necessary for the
desorption of crystallization water in the dihydrate. Thus, the water is more tightly bonded.

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Developed by: ECH Elektrochemie Halle GmbH, Weinbergweg 23, D-06120 Halle/S.
Telefon: 0345/5583-711, Telefax: 0345/5583-710, Internet: http://www.ech.de, E-mail: info@ech.de
 07 / 2003
KF_18_03_e

The complete cure of an original sample of a plaster blend and of its set dihydrate.
Temperature gradient 2°/min (40-280° C with an increase of 2°/min)
red graph – original sample: analysis of CaSO4 * ½ H2O
black graph – after treatment with water and drying at 105°C: analysis of CaSO4 * 2 H2O

Complete cure using a time-controlled temperature program

A two-stage complete cure is used in order to analyse the different water bonding types in
one measurement. During the first partial measurement, the released water is desorbed at
40° C. When the water release is completed, the complete cure temperature is raised to 200°
C and the remaining crystallization water in the material is determined.
The following Figure shows a two-stage complete cure of sample 6. The desorption of the
released water takes 10-15 min at 40° C. Afterwards, the sample remains in the furnace
chamber and is heated to 200° C. The crystallization water is desorbed with a certain time-
delay due to the fact, that crystallization water only starts to separate significantly at 100° C
and upwards.

2/4
Developed by: ECH Elektrochemie Halle GmbH, Weinbergweg 23, D-06120 Halle/S.
Telefon: 0345/5583-711, Telefax: 0345/5583-710, Internet: http://www.ech.de, E-mail: info@ech.de
 07 / 2003
KF_18_03_e

Two-stage complete cure (sample 6):

1. 40° C isothermal (black curve) – Determination of the surface moisture
2. 200° C isothermal (red curve) – Determination of the crystallization water

Results

The following Table shows a summarization of the results.

Sample Surface Crystallization Grade of purity

Moisture water (calculated)
1 0.92 % 5.05 % 81.4 %
2 1.19 % 5.32 % 85.7 %
3 0.31 % 5.61 % 90.4 %
4 0.57 % 5.53 % 89.1 %
5 0.51 % 5.59 % 90.0 %
6 0.58 % 5.83 % 93.9 %
7 0.67 % 6.20 % 99.9%
8 1.12 % 6.20 % 99.9%

The results show that the complete cure technology of the AQUA 40.00 can be used in order
to selectively determine surface moisture as well as crystallization water.
The determined crystallization water content can be used to easily calculate the products
grade of purity.

3/4
Developed by: ECH Elektrochemie Halle GmbH, Weinbergweg 23, D-06120 Halle/S.
Telefon: 0345/5583-711, Telefax: 0345/5583-710, Internet: http://www.ech.de, E-mail: info@ech.de
 07 / 2003
KF_18_03_e

Using the software’s integrated formula editor is especially advantageous. With it’s help, it is
possible to directly convert the water content into any desired unit of measurement. The
products determined grade of purity can thus be displayed during the measurement process.
All measurement parameters are stored, including the chosen conversion formulas and
measurement related factors. Thus, the data resulting from analysing can be compared and
completely tracked.

Conclusion

The water content of plaster mixtures can be determined absolutely reliable and exact using
the Karl-Fischer-Titrator AQUA 40.00. It is possible to distinguish among different types of
bonds. In addition, the product’s grade of purity can be determined from the crystallization
water.
The AQUA 40.00`s comfortable computer control-software gives you various possibilities for
comparing results and furthermore, for their interpretation.
The unit is very compact and easy to handle, due to the used complete cure principle. It can
easily be used for routine-analysis.

Measurement technology

• Karl-Fischer-Titrator AQUA 40.00 equipped with a complete cure chamber for solids and
an inert gas module
• Head-Space-Module including Autosampler

4/4
Developed by: ECH Elektrochemie Halle GmbH, Weinbergweg 23, D-06120 Halle/S.
Telefon: 0345/5583-711, Telefax: 0345/5583-710, Internet: http://www.ech.de, E-mail: info@ech.de