Application Note Gypsum

Purity Determination in Gypsum

Fast Analysis for Precise Process Control

Purity and free moisture content are important quality factors for both nat­
ural gypsum and synthetic gypsum produced by Flue Gas Desulphurisa­
tion (FGD). In the case of FGD gypsum, the purity level gives an indication
of the operational performance of the FGD plant. Continuous monitoring of
the purity level is therefore necessary to control the FGD process.

This application note describes how METTLER TOLEDO Halogen Moisture

Analyzers expedite the analysis of gypsum by delivering accurate data on
both free moisture content and crystal water content.

HR83-P
Halogen Moisture Analyzer
 Introduction
Gypsum is a versatile substance used in the exhaust gases. In this process,
in a wide range of applications such as sulfur dioxide (SO2) reacts with lime
Application Note Gypsum

medicine, agriculture, and the arts as (CaCO3) to produce high purity gyp­
well as in numerous building products sum. The correct functioning of the
e.g. plasterboards. desulfurization process can therefore
A quality parameter for gypsum is be monitored by testing the purity of
its purity. METTLER TOLEDO’s HR83 the obtained gypsum.
Halogen Moisture Analyzer offers a fast Quality criteria published by Euro­
solution for quality analysis of gypsum gypsum, the association of European
(CaSO4 • 2H2O) and the hemihydrate gypsum industries, states that, for
plaster (CaSO4 • ½H2O). synthetic (FGD) gypsum, free moisture
content should be below 10% and
Natural Gypsum gypsum content (CaSO4 • 2H2O) should
Gypsum is a mineral found in natural be higher than 95% 1.
rock. It is extracted either by quarry­
ing or mining. Pure gypsum contains Processing of Gypsum
79.1% calcium sulfate (CaSO4) and When gypsum is pulverized and
20.9% chemically bound water (H2O). heated at around 150 °C, 1½ crystal
However, since gypsum is a natural water is eliminated resulting in hemi­
material, pure gypsum is rarely found. hydrate plaster (CaSO4 • ½H2O). This
Natural gypsum typically contains up plaster can be mixed with water, to
to 15 to 20% impurities such as lime, allow molding into the desired shape
clay and sand 2,3. (e.g. plasterboards). The wet molded
Purity of gypsum is important to know, product then rehardens to gypsum
e.g. plasterboard typically requires a (dihydrate). The excess free water
minimum of 70% gypsum. evaporates or can be removed by
gentle drying at low temperatures
Synthetic/FGD Gypsum (see Figure 1).
An alternative source of gypsum is
synthetic gypsum derived as a side Purity Control with HR83
product from the flue gas desulfuriza­ The HR83 Halogen Moisture Analyzer
tion (FGD) process – the so-called quickly and easily provides two mois­
FGD-gypsum. ture values – free water and crystal
FGD plants are typically used at fossil water content. The purity of the gypsum
fuel power stations to reduce pollutants and the hemihydrate plaster can be
calculated using these values. Thanks
1
-1 /2 H2O
CaSO4 • nH2O
to its step drying program the values
heat (150°C) + H2 O gypsum can be determined in a single mea­
gypsum plaster + additives slurry surement and analysis time required
is significantly reduced compared to
1
CaSO4 • 2H2O CaSO4 • /2 H2O

shaping
-nH2O using a drying oven.
final rehardened wet The following example shows the
drying at low
product temperatures product product HR83 method used by FGD producers
CaSO4 • 2H2O CaSO4 • 2H2O
+
CaSO4 • nH2O for determining the purity of gypsum
nH2O
and thus for control of the flue gas
Figure 1: Burning, Mixing, Shaping and Rehardening of gypsum desulfurization process.

1
www.eurogypsum.org
2
www.rigips.ch
3
www.meningiegypsum.com.au
 Material and Methods
• HR83-P Halogen Moisture Analyzer
• Gypsum from FGD process
Application Note Gypsum

Method for determining the purity of gypsum (CaSO4 • 2 H2O) with the HR83

1. Press “Method” to select

method for gypsum.
• Drying Program: Step Drying
– Step 1: 25 min at 50 °C (to remove free water)
– Step 2: 0 min at 50 °C (Step 2 not required)
– Final Step: 200 °C
• Switch-off criterion 5 (1 mg/140 s)

2. Weigh approx. 5 g of powdered

gypsum into tared sample pan.

3. Press "Start" button

to begin measurement.

4. The results of each step are recorded.

Wet weight: 5.570 g

DW1 = Result from
Step 1 (50 °C): 5.113 g = 8.19% free water
DWF = Result from
Final Step (200 °C): 4.085 g

5. Crystal water content (CW) and

purity are then calculated.

Molecular weight CaSO4: 136.14 g/mol

Molecular weight 2 H2O: 36.03 g/mol
Molecular weight CaSO4 • 2 H2O: 172.17 g/mol

MW2 H2 O 36.03
Theoretical CW of pure gypsum: 100 % • = 100 % • = 20.9272 %
MWCaSO4 • 2 H2O 172.17

− DWF
DW−1 DW g −g 4−.085
5.113 4.085
g g = 20.106 %
Measured CW of pure gypsum: 100
100%%
DW
DW − DW
∗ • 1 F
= =100
100
%% 5.113 g − 4.085g
5.113
∗• = 20.106%
100% ∗ 1DW
DW1 1
F
= 100% ∗ 5.113
5.113 gg = 20.106%
DW 1
measuredCW
5. 113
20.106%
g
Purity [%]: 100 % • = 100 % • = 96. 07 %
theoretica lCW 20.9272%
 Alternative Method for determining free and crystal water

The HR83 offers the option to add two methods. In the first method the free
water content is determined at 50 °C, followed by the second method in which
Application Note Gypsum

the crystal water is determined at 200 °C. The dry weight of the first method is
used as the starting weight for the second method. The final result displayed is
the crystal water content.

Method 1: 50 °C for 25 min (add method “2”), standard drying

Method 2: 200 °C with switch-off criterion 5 (1 mg / 140 s), standard drying

Results
To monitor the performance of the FGD drying method with the HR83 Moisture
process a sample is taken from the Analyzer as illustrated above. In the
vacuum belt filters where the freshly example, the FGD gypsum has a free
produced FGD gypsum is washed moisture content of 8.19% and a crys­
and dewatered. Purity below 95% is tal water content of 20.106% which
an indication that the FGD process is correlates to a purity of 96.07%. This
not working optimally and must be indicates the flue gas desulfurization
checked for possible errors. and the dewatering processes are run­
The crystal water content of the ning smoothly yielding the best quality
sample is determined via the two step gypsum.

Conclusion
The Application Note demonstrates water – required for the calculation of
the determination of purity of gypsum purity of both gypsum and plaster.
(dihydrate). Determining the purity of The halogen technology provides
hemihydrate plaster is achieved using precise temperature control and fast,
the same method, but the purity cal­ homogenous drying, and the robust
culation is based on the theoretical construction is ideal for use in tough
crystal water content of 6.207% (com­ production environments. The HR83
pared to 20.9272% of the dihydrate). significantly reduces the time and
The correct purity level is important handling required for analysis com­
for both quality control and in-process pared to the drying oven method and
control of synthetic gypsum produc­ therefore contributes considerably to
tion. The HR83 Halogen Moisture Ana­ the operational efficiency of flue gas
lyzer ­rapidly and easily provides the desulfurization plants and gypsum
two moisture values – free and crystal processors.

Mettler-Toledo AG
www.mt.com/moisture
PO Box VI-400, CH-8606 Greifensee For more information
Tel. +41-44-944 22 11
Fax. +41-44-944 31 70

Subject to technical changes

© 03/2010 Mettler-Toledo AG
Printed in Switzerland 30004091
Global MarCom Switzerland