Gypsum Phase Analysis

Geoenvironmental Engineering GSP 241 ASCE 2014 222
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Availability of Density Measuring Methods Estimating Gypsum Hemihydrate

Content in Reclaimed Gypsums
Shinya Inazumi1, Hiroaki Sano2, Mikio Yamada3 and Hsin Ming Shang4
1
Akashi National College of Technology, 679-3, Nishioka, Uozumi, Akashi, Hyogo
6748501, Japan; inazumi@akashi.ac.jp
2
Oita National College of Technology, 1666, Maki, Oita, Oita 8700152, Japan;
sano@oita-ct.ac.jp
3
Fukui National College of Technology, Geshi, Sabae, Fukui 9168507, Japan;
yamasan@fukui-nct.ac.jp
4
Jines Construction Co. Ltd., No.67, Lane 11, Kwang-Fu N.Road, Taipei City,
Taiwan; shm@jines.com.tw
ABSTRACT: In order to utilize reclaimed gypsums (gypsum board waste) derived

from waste plasterboards as geo-materials, thermal behaviors of the reclaimed
gypsums and reagent gypsum are investigated in this paper. As the results, it was
found that the dihydrate gypsum is changed into the hemihydrate gypsum under
thermal condition of 90C and the hemihydrate gypsum is changed into anhydrite
under that of 120C with heating of 24 hours. The followings were clarified in this
paper. The cement density measuring method was available in order to measure the
density of reclaimed gypsums; that density was depended on the drying conditions of
the reclaimed gypsums; and the density measuring method was appropriate to
estimate the gypsum hemihydrate content on reclaimed gypsums.
INTRODUCTION
As more gypsum boards are produced, gypsum board waste from construction sites,
and so on, is also increasing every year. According to the Gypsum Board Association
of Japan, it is estimated that the total annual waste volume of gypsum boards may
reach 2,969,000 tons in 2038 (Gypsum Board Association of Japan 2012): 159,000
tons from new construction sites and 2,810,000 tons from sites being demolished.
Under such circumstances, development of new treatment methods not to dispose
gypsum board waste (gypsum dihydrate) has become imperative in Japan. As one of
such methods, many researchers have studied the applicability of gypsum board waste
as foundation material in the civil engineering sector that consumes a high volume of
gypsum in each construction project (Kamei and Shuku 2007a and 2007b; Horai et al.
2008; Kamei et al. 2009). The authors have also studied the application of gypsum
Geoenvironmental Engineering
dihydrate, hemihydrate and anhydrate obtained by crushing, fracturing, separating

and burning the gypsum board waste as ground improvement materials. These studies
were to actively leverage the water absorption and solidification properties achieved
during the transformation of gypsum dihydrate from gypsum hemihydrate: when
gypsum dihydrate is burned, it transforms to gypsum hemihydrate, and further
transforms to gypsum dihydrate when it comes into contact with water (The Society
of Inorganic Materials, Japan 1996). According to past studies, it has been reported,
in relation to the application of gypsum board waste as ground improvement material,

cement partially replaced with gypsum hemihydrate is likely to be more effective in
engineering and economical aspects than the single use of cement.
When the application as geo-material as well as ground improvement material is
discussed, gypsum hemihydrate is mainly used. Therefore, the gypsum board waste
has to be crushed, fractured and separated before the gypsum powder (gypsum
dihydrate) is heated to be transformed into gypsum hemihydrate. Existing rotary
kilns, newly developed furnaces, and so on, are used as the heating devices for this
purpose.
While the engineering effectiveness of gypsum recycled from the gypsum board
waste has been reported, if such poor-quality half-burned gypsum manufactured by
some companies with poor technical ability is distributed in the market, it is predicted
that the reliability of the studies regarding the effective use of the gypsum recycled
from gypsum board waste would be undermined, and it may become a considerable
obstacle in the utilization of gypsum recycled from the gypsum board waste, while
increasing in volume of the gypsum board waste, and reduction of the available free
space in the management-oriented final disposal sites are anticipated. To avoid this
situation, development of not only effective use but also quality control technology of
the recycled gypsum should be actively developed.
This study reviews in detail the thermal behavior of recycled and reagent gypsum
from the viewpoint of recycled gypsum utilization as geo-material, and at the same
time, discusses the methods to determine the content of the gypsum hemihydrate from
the viewpoint of density as a simple quality judgment method of the recycled
gypsum. Here, the gypsum gained by crushing, fracturing and separating the gypsum
board waste shall be called gypsum derived from the gypsum boards (recycled
gypsum dihydrate).
BASIC PROPERTIES OF RECYCLED GYPSUM AND REAGENT GYPSUM
Thermal behavior of the recycled gypsum and reagent gypsum
A lot of literature describes gypsum dihydrate transforming to gypsum hemihydrate

at 130-150C, and to gypsum anhydrate at 200C. However, the authors undertook
burning for 24 hours at certain temperatures and found the gypsum formation changes
at a much lower temperature than the temperature described in the literature, and
reported the formation change cannot be confirmed only by the temperatures.
This indicates that the recycled gypsum dihydrate needs to be burned at a certain
temperature and for a certain length of time so that the recycled gypsum hemihydrate
can be used as a main ground improvement material, although different cases apply to
the recycled gypsum dihydrate.
Also, various burning treatments are required to test the application of the recycled
gypsum as a geo-material. Particularly, Test method for water content of soils (JIS A
1203: 2009) (Japanese Geotechnical Society 2009a) and Test method for density of
soil particles (JIS A 1202: 2009) (Japanese Geotechnical Society 2009b) are
commonly implemented in all the geo-material tests and these tests require oven-
drying at (1105)C to gain samples with a specified mass, and it usually takes about
18-24 hours. As mentioned above, the formation of gypsum is significantly
influenced by heating temperature and time. Therefore, to use the recycled gypsum as
a geo-material, the behavior under heating at 110C should be identified.
Therefore, to review the thermal behavior of gypsum in detail, changes in mass of
different masses of gypsum during oven-drying, i.e., changes in the water content,
were measured, and the formation change of gypsum was discussed based on the
masses calculated considering the chemical Equations of the gypsum.
In order to implement the tests, the gypsum board waste was transported to the
intermediate treatment site for industrial waste in Oita City and a pile of the boards in
a warehouse were crushed, fractured and separated from the original board paper
using a crushing machine to obtain recycled gypsum dihydrate. Because there was no
facility to thermally dehydrate gypsum dihydrate in such intermediate treatment site
in Oita City, the heating unit installed in Isahaya City, Nagasaki Prefecture, was used
to obtain gypsum hemihydrate from the above-mentioned recycled gypsum dihydrate.
The gypsum sampled in April 2008 and July 2011 was used for this test.
Because the recycled gypsum dihydrate forms particles of up to 2.5mm due to the
performance of the crusher of the intermediate treatment site, the original particles
were sieved and sorted by 2000m, 850m and 425m sizes to use for the test to
study the influence of the difference in particle diameter.
The method for the heating test was as follows: samples were accurately weighed to
10g each at room temperature, and put into stainless containers of diameter 6 cm and
height 3 cm. At that time, the surface of the samples were flattened as much as
possible to help with the drying. Here, with 10g of sample, the thickness was about
6mm and the bulk density was 0.59g/cm3.
Next, the containers were placed in a constant-temperature drying oven (DX601
manufactured by Yamato Scientific Co., Ltd., interior capacity: 153L, temperature
control range: +5 to 280C, temperature control accuracy: 1C, temperature
distribution accuracy: 10C (setting temperature at 280C, exhaust vent 1/3 open)),
which controlled the temperature by units of 10C between 40-160C, and was heated
for 24 hours at specified temperatures. Further, a condition with a temperature setting
of 45C was added as prescribed in the method for quantifying the water content of
gypsum included in Methods for chemical analysis of gypsum (JIS R 9101:1995)
(Japanese Sandards Association 1995).
After heating, the samples were cooled down in a desiccator for 30 minutes until the
temperature became room temperature and then the mass was measured. The heating
tests were implemented on 6 samples at different temperatures and the average value
was used, considering variations in the data.
This time, because of the performance of the constant-temperature drying oven
(temperature distribution accuracy: 10C), the influence of the temperature
difference due to location in the oven was unavoidable. Taking this into
consideration, 6 samples were prepared and placed in the same place in the drying
oven, and measured and the temperature in the drying oven was adjusted as needed.
The authors believe the reliability of the results was secured in this way.
Here, when gypsum dihydrate and gypsum hemihydrate were heated, it is believed
that a formation change occurs in a certain temperature range as shown as the
chemical equations below(The Society of Inorganic Materials, Japan 1996).
(1) From gypsum dihydrate to gypsum hemihydrate
1 3
CaSO4 2 H 2O CaSO4 H 2O H 2O (1)
2 2
(2) From gypsum dihydrate to gypsum anhydrate
CaSO4 2H 2O CaSO4 2H 2O (2)
(3) From gypsum hemihydrate to gypsum anhydrate

1 1
CaSO4 H 2O CaSO4 H 2O (3)
2 2
Based on the molecular masses of above (1)-(3) chemical equations, the mass of
gypsum hemihydrate generated from 10g of gypsum dihydrate is calculated as 8.43g.
In similar ways, 7.91g of gypsum anhydrate is generated, and 9.38g of gypsum
anhydrate is generated from 10g of gypsum hemihydrate.
The mass of the recycled gypsum hemihydrate () decreases at 110C, but does
not decrease along with a temperature rise at 120C and higher.
When the above phenomena are reviewed with the formation change of the gypsum
related to the masses calculated from the Equations (1)-(3), it is implied that the
recycled gypsum dihydrate transforms to the recycled gypsum hemihydrate through
thermal dehydration for 24 hours at 90C and the recycled gypsum hemihydrate
transforms to the recycled gypsum anhydrate through the thermal dehydration for 24
hours at 120C.
The reagents were calcium sulfate dihydrate (reagent manufactured by Kanto
Chemical Co., Ltd., Cica 1 Class, content: 98.0% or more) and calcined gypsum
(reagent manufactured by Kanto Chemical Co., Ltd., Cica 1 Class, content: 99.0% or
more). Hereafter, calcium sulfate dihydrate shall be called reagent gypsum
dihydrate and calcined gypsum shall be called reagent gypsum hemihydrate
corresponding to the representation of the recycled gypsum.
For the masses of the samples in the test, by referring to the description in Test
method for water content of soils (JIS A 1203: 2009) (Japanese Geotechnical
Society 2009a), If the maximum particle diameter of the sample is 2mm, the
minimum mass required to measure is 10-30g, the masses of the samples were
varied in 4 categories within the range of 5-30g to review the influence of the sample
volume on the mass change at heating.
The heating test was implemented using 6 samples at each temperature and the
average value was used, considering dispersion of the data, which was the same as
when the recycled gypsum was tested.
Figure 1 shows the relationship between heating temperature and mass of the
reagent gypsum dihydrate and gypsum hemihydrate when the masses at the beginning
of the test were 5g, 10g, 20g and 30g. Also, the masses calculated from above
Equations (1)-(3) are shown as one chain line in the figure. When 5g, 20g and 30g of
samples were used, the results were converted to 10g for indication purposes.
The figure shows that although the reduction trend of the gypsum mass at heating,
i.e., the thermal dehydration trend, depends on the gypsum mass at the beginning of
the test, the mass of the reagent gypsum dihydrate (marked as ) starts
sharply decreasing at 80C (First Phase) when heated, there is no major change at 90-
100C, it decreases further at 110C (Second Phase), and there is no major change at
120C and more.
Here, when inferred from the chemical Equations (1)-(3), the First Phase
corresponds to the process in which 10g of gypsum dihydrate produces 8.43g of
gypsum hemihydrate and the Second Phase corresponds to the process in which 10g
of gypsum dihydrate produces 7.91g of gypsum anhydrate. These results imply the
reagent gypsum dihydrate transforms to gypsum hemihydrate through thermal
dehydration for 24 hours at 90C and gypsum anhydrate through thermal
dehydration for 24 hours at 120C.
Then, the mass of the reagent gypsum hemihydrate ( ) decreases by
heating at 40C. Further, the mass starts decreasing at 110C, there is no major mass
11
Reagent dihydrate Weight of gypsum
Weight of gypsum m
Reagent hemihydrate 5
10
10 20
30
9.38g
9 Gypsum hemihydrateGypsum anhydrate
8.43g Gypsum dihydrate

Gypsum hemihydrate
8 7.91g
Gypsum dihydrateGypsum anhydrate
45 :by JIS R 9101
110 :by JIS A 1203
7
20 40 60 80 100 120 140 160 180 200 220
(Room temperature) Heating temperature T
Fig. 1 Relationship between heating temperature and mass of reagent

gypsum dihydrate
change at 120C and a mass change along with a temperature rise does not occur. The
stage at 120C corresponds to the process in which 10g of gypsum hemihydrate
transforms to 9.38g of gypsum anhydrate. Also, this temperature corresponds to the
temperature at which gypsum hemihydrate transforms to gypsum anhydrate after
reagent gypsum dihydrate transforms to the gypsum hemihydrate, which was shown
above.
When judged comprehensively from the result of the heating tests of the recycled
gypsum and the reagent gypsum above, it was empirically proved that gypsum
dihydrate transforms to gypsum hemihydrate through thermal dehydration for 24
hours at 90C and gypsum hemihydrate transforms to gypsum anhydrate through
thermal dehydration for 24 hours at 120C.
Density of recycled gypsum and reagent gypsum
The analysis method of gypsum is prescribed in Methods for chemical analysis of

gypsum (JIS R 9101:1995) (Japanese Sandards Association 1995) and it is different
from the method for soil analysis. The reasons are that the state of gypsum varies
depending on the volume of the contained bound water, that the properties vary
depending on heating temperatures, and that gypsum hemihydrate transforms to
gypsum dihydrate to be solidified when water is added, and so on.
To understand the basic properties of gypsum as a geo-material, both of Methods
for chemical analysis of gypsum (JIS R 9101:1995) (Japanese Sandards Association
1995) and Geo-material test should be considered. Especially, the items to be
focused on are water, pH and density. The density is discussed below.
When the density of soil particles for geo-material is measured, a pycnometer is
typically used as a testing instrument, complying with the Test method for density of
soil particles (JIS A 1202: 2009) (Japanese Geotechnical Society 2009b). However,
this method cannot be applied to gypsum hemihydrate, because this method requires
the immersion of the samples in distilled water to determine the volume of the soil
particles, but the gypsum hemihydrate is solidified after reacting to water. Therefore,
the test was implemented complying with the density test prescribed in Physical
testing method for cement (JIS R 5201: 1997) (Japanese Sandards Association
1997), in which mineral oil is used instead of water to determine the volume.
Under the density test of soil particles, oven drying is implemented at 110C to
determine the mass of the soil particle. However, as mentioned in the gypsum heating
test section, because the specified drying temperature for determining the gypsum
water content in this method was 45C, the test was implemented under the following
3 conditions: natural state, dried at 45C and dried at 110C.
The test procedures were as follows: filled Le Chatelier flasks with mineral oil and
placed them in a constant temperature room at a room temperature of 20C until the
temperature of the mineral oil become stable. Then, 3 types of recycled gypsums in 3
conditions were loaded into the Le Chatelier flasks and the air was removed.
However, because it was difficult to remove air from gypsum, the test took a long
time and it was inefficient to repeat the steps to remove the air and then place the
flasks in the water tank until the surface of the mineral oil become flat. Therefore, the
authors decided to implement the following procedure: after removing the air, the
flasks were placed and left in the water tank, the scale of the mineral oil surface was
read one day after that, then the flasks were shaken again to remove the air for
another day. This procedure was repeated until the mineral oil surface became stable
and then the values read at that time were taken as the measured values. A standing
still period of 3-4 days was required.
Also, although the specified cement volume for the test is 100g (Japanese Sandards
Association 1997) under the method complying with the cement density test, the
sample volume was adjusted to 85-90g, because the gypsum densities (reagent
gypsum dihydrate: 2.326g/cm3, reagent gypsum hemihydrate: 2.681g/cm3) are
generally smaller than that of Portland Cement (3.15g/cm3).
ESTIMATION ON CONTENT OF GYPSUM HEMIHYDRATE USING THE

DENSITY METHOD
First, the density of gypsum dihydrate is referred to as GD (GD: abbreviation of

Gypsum Dihydrate), and the density of gypsum hemihydrate is referred to as GH
(GH: abbreviation of Gypsum Hemihydrate). Assuming that mass (mGD+mGH) and
volume (VGD+VGH) of gypsum dihydrate and gypsum hemihydrate are mixed in
recycled gypsum derived from a wasted gypsum board, the density of the sample
(GD+GH) can be calculated by the following Eq. (4):
m GD m GH
GD GH (4)
V GD V GH
Where, m represents mass of gypsum and V represents volume of gypsum and the
subscripts represent forms of gypsum. Then, the density of gypsum dihydrate GD
and the density of gypsum hemihydrate GH can be represented as the following Eq.
(5) by its definitional equations:
m GD m GH
VGD , VGH (5)
GD GH
From Eq. (5)

m GD m
GD , GH GH (6)
V GD V GH
By substituting Eq. (6) for Eq. (4)

m GD
1
m m GH m GH
GD GH GD (7)
m GD m GH 1 m GD 1

GD GH GD m GH GH
On the other hand, the content gypsum hemihydrate in the recycled gypsum CGH
(abbreviation of Gypsum Hemihydrate Content) can be defined as the following Eq.
(8):
m GH
C GH 100
m GD m GH (8)
The following Eq. (9) can be obtained by transforming Eq. (8):

mGD 100 C GH
(9)
mGH C GH
Finally, Eq. (10), which the authors propose, can be obtained by substituting Eq. (9)
for Eq. (7):
100
GD GH (10)
100 C GH C GH

GD GH
In this calculation, first calculate the density of gypsum dihydrate GD (reagent

gypsum dihydrate: 2.326g/cm3) and the density of gypsum hemihydrate GH (reagent
gypsum hemihydrate: 2.681g/cm3), next, calculate the density of the recycled gypsum
(GD+GH) in which gypsum hemihydrate content CGH is unknown, and then Eq.
(10) can be used to calculate the gypsum hemihydrate content CGH and the gypsum
dihydrate content (100-CGH). This way, the volumes of gypsum hemihydrate and
gypsum dihydrate in the recycled gypsum can be estimated with the simple quality.
Although the equations were established assuming the recycled gypsum contains
only gypsum dihydrate and gypsum hemihydrate, there might be gypsum anhydrate
depending on the heating temperature. However, as mentioned above, type 3 gypsum
anhydrate is prone to return to gypsum hemihydrate by absorbing water and very
easily and instantly transforms to gypsum hemihydrate on making contact with water
or moisture in the atmosphere (The Society of Inorganic Materials, Japan 1996).
Therefore, the authors didn't consider gypsum anhydrate to establish the above
equations.
As the next step, the authors empirically validated the above proposed Eq. (10) with
the reagent gypsum.
Specifically, to adjust gypsum so that the gypsum hemihydrate content was between 0
and 100%, gypsum dihydrate and gypsum hemihydrate with natural water content
were weighed so that the mixture ratio of reagent gypsum dihydrate and hemihydrate
became between 10:0 and 0:10, put them into a 500m polyethylene container with a
lid, and shook the container for 2 minutes so the content mixed evenly. After shaking,
the content of the container (sample) was taken out, accurately weighed to a specified
amount from 3 points, and a cement density test was performed. The sample amount
was adjusted to 85-90g.
Considering dispersion of the data, 3 samples were used for the test.
Figure 2 shows the relationship between the set gypsum hemihydrate content and
the density. The result (solid line) calculated by the proposed Eq. (10) is also shown
in the figure.
The figure shows the density values (marked with ) determined by the
experiment are nearly equation to the density values calculated using the proposed
equations. Therefore, it is believed that estimation of the gypsum hemihydrate content
CGH is possible by using the above-proposed Eq. (10).
When an approximate expression (broken line in Fig. 1) was calculated using the
minimum square method, the following Eq. (11) was obtained:
2.323 0.003591CGH r 0.999

<GD:Gypsum Dihydrate GH:Gypsum Hemihydrate>
2.8
3
Reagent gypsum hemihydrate =2.681g/cm
2.7
Experimental Eq.: =2.323+0.003591CGH r=0.999
Density g/cm
3
2.6
2.5
Proposed Eq.
2.4
3
Reagent gypsum dihydrate =2.326g/cm
2.3
Experimental value
2.2
0 20 40 60 80 100
Set gypsum hemihydrate content
CGH=mGH/(mGD+mGH) 100 %
Fig. 2 Relationship between set gypsum hemihydrate content and density
(11)
As the correlation of the empirical Eq. (11) was very high, again the validity of Eq.
(10) was confirmed.
The result of the density test of the recycled gypsum made in Oita Prefecture was
shown in Chapter 2. To validate the quality of the recycled gypsum as well as the
validity of the proposed Eq. (10) and the empirical Eq. (11), the density values
determined from the experiment were substituted for Eqs. (10) and (11) to calculate
the gypsum hemihydrate content CGH and the gypsum dihydrate content (100-CGH).
CONCLUSIONS
The main findings from this study are as follows:

(1) If heated for 24 hours, gypsum dihydrate transforms to gypsum hemihydrate at
90C and to gypsum anhydrate at 120C.
(2) To determine the density of gypsum, the cement density test is effective, and the
result depends on how much the sample is dried.
(3) The validity of the estimation method of gypsum hemihydrate content using the
density was empirically confirmed. Moreover, by calculating the gypsum
hemihydrate content from the measurement result of the recycled gypsum density,
the effectiveness of the quality control method based on the density was proven.
REFERENCES
Gypsum Board Association of Japan (2012). Gypsum board handbook.

Horai, H., Kamei, T., Ogawa, Y. and Shibi, T. (2008). Development of bassanite
production system and its geotechnical engineering significance: Recycling of
waste plasterboard. Journal of Japanese Geotechnical Society, 3(2), 133-142.
Japanese Geotechnical Society (2009a). Japanese Standards and Explanations of
Laboratory Tests of Geomaterials. 1/2, 104-114.

Japanese Geotechnical Society (2009b). Japanese Standards and Explanations of
Laboratory Tests of Geomaterials. 1/2, 97-103.
Japanese Sandards Association (1995). Methods for Chemical Analysis of Gypsum.
JIS R 9101:1995, 1-38.
Japanese Sandards Association (1997). Methods for Chemical Analysis of Gypsum.
JIS R 5201:1997, 1-38.
Kamei, T. and Shuku, T. (2007a). Unconfined compressive strength of cement-
stabilized soils containing bassanite produced from waste plasterboard. Journal
of Japanese Geotechnical Society, 2(3), 237-244.
Kamei, T., Kato, T. and Shuku, T. (2007b). Effective use for bassanite as soil
Improvement materials: Recycling of waste plasterboard. Journal of Japanese
Geotechnical Society, 2(3), 245-252.
Kamei, T., Ogawa, Y. and Shibi, T. (2009). Effect of curing periods on unconfined
compressive characteristics of cement-stabilized soils utilizing bassanite:
Beneficial use of waste plasterboard. Journal of Geotechnical Engineering
Society, 4(1), 99-105.
The Society of Inorganic Materials, Japan (1996). Semento-Sekkou-Sekkai
Handbook. Gihodo Shuppan.

Gypsum Phase Analysis

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Geoenvironmental Engineering GSP 241 ASCE 2014 222

Availability of Density Measuring Methods Estimating Gypsum Hemihydrate

ABSTRACT: In order to utilize reclaimed gypsums (gypsum board waste) derived

dihydrate, hemihydrate and anhydrate obtained by crushing, fracturing, separating

in relation to the application of gypsum board waste as ground improvement material,

BASIC PROPERTIES OF RECYCLED GYPSUM AND REAGENT GYPSUM

Thermal behavior of the recycled gypsum and reagent gypsum

A lot of literature describes gypsum dihydrate transforming to gypsum hemihydrate

(2) From gypsum dihydrate to gypsum anhydrate

CaSO4 2H 2O CaSO4 2H 2O (2)

(3) From gypsum hemihydrate to gypsum anhydrate

9 Gypsum hemihydrateGypsum anhydrate

8.43g Gypsum dihydrate

Fig. 1 Relationship between heating temperature and mass of reagent

Density of recycled gypsum and reagent gypsum

The analysis method of gypsum is prescribed in Methods for chemical analysis of

ESTIMATION ON CONTENT OF GYPSUM HEMIHYDRATE USING THE

First, the density of gypsum dihydrate is referred to as GD (GD: abbreviation of

From Eq. (5)

By substituting Eq. (6) for Eq. (4)

The following Eq. (9) can be obtained by transforming Eq. (8):

In this calculation, first calculate the density of gypsum dihydrate GD (reagent

2.323 0.003591CGH r 0.999

Fig. 2 Relationship between set gypsum hemihydrate content and density

The main findings from this study are as follows:

Gypsum Board Association of Japan (2012). Gypsum board handbook.

Laboratory Tests of Geomaterials. 1/2, 104-114.

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