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Problem of controlling the gypsum setting time

Article  in  Russian Journal of Applied Chemistry · June 2013

DOI: 10.1134/S107042721306027X

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N. V. Pashchevskaya
Kuban Social Economic Institute, Krasnodar,Russia
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ISSN 1070-4272, Russian Journal of Applied Chemistry, 2013, Vol. 86, No. 6, pp. 942−944. © Pleiades Publishing, Ltd., 2013.
Original Russian Text © V.E. Akhrimenko, N.V. Pashchevskaya, 2013, published in Zhurnal Prikladnoi Khimii, 2013, Vol. 86, No. 6, pp. 1001−1003.

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Problem of Controlling the Gypsum Setting Time

V. E. Akhrimenkoa and N. V. Pashchevskayab

aKuban State Agricultural University, Krasnodar, Russia
bKuban Socio-Economic Institute, Krasnodar, Russia
e-mail: phv2@yandex.ru

Received February 7, 2013

Abstract—Effect of molasses, a waste formed in manufacture of sugar, on the gypsum setting time was studied.
It is shown that molasses solutions can be used to control the hardening time of the gypsum paste.

DOI: 10.1134/S107042721306027X

Gypsum plaster belongs to rapidly hardening air-
setting binders. The hardening of a gypsum paste begins
already in 3–5 min after its tempering with water. The
gypsum setting time (GST) largely depends on the start-
ing raw material, technology of its manufacture, storage
duration, and presence of additives. The rapid setting of
gypsum in numerous industrial processes is a positive
factor that enables fast extraction of articles from molds
and their higher turnover rate in assembly-line production
of articles.
However, the rapid setting of gypsum gives no way
of preparing its paste in substantial amounts. That is why
various additives are used to control the GST [1]. A search
for effective additives for controlling the GST and rais-
ing the mechanical strength of gypsum casts is a most
important practical task to whose solution the authors of
[2] have made a significant contribution. In [3], the influ-
ence exerted on the hardening of gypsum hemihydrate by
complexonates of Ba2+, Ca2+, and Cr3+, synthesized on
the basis of their salts with a doubly charged anion of eth-
ylenediaminetetraacetic acid, was considered.
The goal of this study was to seek for an effective
GST-controlling agent whose application would make it
possible to prepare substantial amounts of gypsum paste,
necessary in building and finishing procedures.
EXPERIMENTAL
As objects of study were chosen gypsum plaster
from Khabezskii gypsum plant [GOST (State Standard)
125–79, G-5, G-6] and additives: an organic electrolyte
(molasses), an inorganic electrolyte (hydrated lime), and
a neutral substance (beet sugar).
Molasses is a water-soluble waste formed in
manufacture of sugar, 80% composed of calcium
saccharates. The gypsum paste was prepared by vigorous
agitation of a gypsum powder with a tempering fluid
whose role was player by potable water and solutions
of the above additives in this water. The GST was
determined using the Vick’s instrument. For this purpose,
the gypsum paste was placed in the ring of this device
and its needle was dropped into the paste after a certain
interval of time. The depth to which the needle penetrated
into the paste after this interval of time was used to find
the beginning and end of its setting. To determine the
strength of the stone being formed, the gypsum paste
was placed in 20 × 20 × 100 mm dismountable metallic
molds and the gypsum beams obtained were subjected
to compressive strength tests.
The manner in which the setting time of the gypsum
under study varies with the water-to-gypsum ratio (W/G)
in the case when drinking water served as the tempering
fluid can be seen in Fig. 1, curve 1.With increasing W/G,
the gypsum setting process becomes slower. The process
is decelerated to an even greater extent in the presence
of molasses in the gypsum paste (curve 2). It follows
from Fig. 1 that, with the gypsum paste containing 2%

942
 PROBLEM OF CONTROLLING THE GYPSUM SETTING TIME 943

Effect of the percentage content of molasses on the saccharate anions are firmly retained by calcium atoms
compressive strength of stone and its adhesion to a metal in contained in gypsum. As a result of the adsorption of
two days (W/G = 0.6, T = 25°C) this kind, gypsum grains are coated with a protective
Molasses Compression Adhesion film blocking their active centers, which precludes
concentration, %
the agglomeration and coarsening of these grains and,
MPa
on the whole, hinders the gypsum hardening process.
0 1.67 0.72 Comparison of curves 1 and 2 in Fig. 1 shows that an
0.6 1.21 0.63 increase in W/G diminishes the GST to an even greater
extent because the concentration of dissolved gypsum
1.2 0.97 0.58 (CaSO4·2H2O) decreases upon dilution. The dissolved
1.8 0.86 0.51 gypsum is formed via hydration of gypsum hemihydrate
in the course of its hardening, which occurs by the
2.0 0.78 0.48 reaction

СаSО4·0.5Н2О + 1.5Н2О = СаSО4·2Н2О.

molasses relative to the mass of gypsum, the hardening
time substantially increases for each W/G. For example,
the hardening time for gypsum with W/G = 0.6 (straight
line 1) is 13 min, whereas for the gypsum paste with
2% molasses and the same W/G, this time is as long as
97 min. These data indicate that molasses is an active
decelerating agent for the gypsum hardening process. A
study of the effect of the molasses concentration on the
setting time of the gypsum paste demonstrated (Fig. 2)
demonstrated that the hardening time of the gypsum
paste becomes longer as the content of molasses in the
paste is raised.
The decelerating effect of molasses on the gypsum
hardening process can be understood as follows.
Molasses contains a large amount of well-soluble calcium
saccharates of general formula C12H22O11·CaO·2H2O.
Being electrolytes in an aqueous medium, calcium
saccharates form large anions chemisorbed on gypsum
grains bearing an electric charge. The chemisorbed
τ, min
The decrease in the concentration of the soluble
substance, associated with the number of gypsum grains
in unit volume, violates one of the conditions for the
hydration hardening at a certain, rather close, distance,
which provides formation of a 3D skeleton structure
via coalescence of crystals of the solid phase [4]. To
verify the supposed mechanism of the decelerating
effect of molasses on the GST, we performed tests
with a gypsum paste in which sugar solutions with
different concentrations served as the tempering fluid.
The experiments demonstrated (within the measurement
error) that pure beet sugar taken in an amount of 10%
relative to the mass of gypsum has no effect on the GST
and only slightly raises the flowability of gypsum.
Saccharose molecules are species bearing no
electric charge, which makes them inert toward the
poorly soluble gypsum. The existing electric charges of
gypsum do not possess the sufficient energy (because
τ, min

ω, %
W/G
Fig. 1. Effect of W/G on the gypsum setting time. (τ) Gypsum Fig. 2. Gypsum setting time τ vs. the molasses concentration
setting time. Tempering fluid: (1) water and (2) molasses ω. W/G = 0.5, T = 25°C.
solution.

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 86 No. 6 2013

944 AKHRIMENKO, PASHCHEVSKAYA
of its poor solubility) for neutral saccharose molecules
to be adsorbed on their surface to give screening films
that could preclude agglomeration of gypsum particles.
In addition, sugar solutions possess no ionic strength
and have no effect on the solubility of gypsum and
thereby cannot affect the process of its hydration and,
consequently, change the setting time, too.
Another type of behavior is exhibited b gypsum
tempered with substances having an ionic structure, e.g.,
Ca(OH)2. Being a strong base, Ca(OH)2 is present in
solution as Ca2+ and OH– ions. Calcium and hydroxy ions
affect by their electric field the crystal lattice of gypsum
hemihydrate, weaken its bonds, and make gypsum more
soluble. The increase in the solubility of gypsum is
also due to the presence of likely charged ions, which
accelerates the saturation process of the unit volume of
the solution and is accompanied by further hardening of
gypsum. In the case under study, the gypsum paste with
W/G = 0.6 and 0.5% Ca(OH)2 sets in 2.5 min.
Inorganic electrolytes form on the surface of gypsum
grains ionic sheaths whose thickness and charge are
determined by the concentration of ions in the liquid
phase and by their properties. With increasing content of
electrolytes in the gypsum paste, the potential difference
between the diffusion and adsorption layers becomes
lower and particles coagulate, which leads, n the whole,
to a faster setting of gypsum and its shorter setting time.
An important technological parameter of the gypsum
stone is its adhesion to metallic, wooden, and cardboard
surfaces. The effect of the W/G ratio and molasses
concentration on the adhesion of the gypsum stone to
the metallic surface was determined by the procedure
described in [5]. The study demonstrated that, at the
concentrations under study, the adhesion of the two-
days-old gypsum tone to the metallic surface slightly
decreases with increasing molasses concentration,
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 86 No. 6 2013
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which is apparently due to its decelerating effect (see
table). As for the strength of the gypsum stone containing
the additive under study, this parameter grows with
increasing stone hardening time (ωmolasses = 2%, T =
25°C, W/G = 0.6):
Hardening time, h 1 2 3 4 7
Strength, MPa 0.89 1.67 1.93 2.78 4.57
CONCLUSIONS
(1) The molasses solution can be successfully used to
widely control the gypsum setting time.
(2) In the concentration range under study, the
gypsum setting time linearly grows with increasing
mass fraction of molasses.
REFERENCES
1. Pashchenko, A.A., Serbin, V.P., and Starchevskaya,
E.A., Vyazhushchie materialy: Uchebnik dlya vyssghikh
uchebnykh zavedenii po spetsial’nosti “Khimicheskaya
tekhnologiya vyazhushchikh materialov” (Binders:
Textbook for Higher School Institutions for the Specialty
“Chemical Technology of Binders”), Kiev: Vishcha shkola,
1985.
2. Ratinov, V.B. and Rozenberg, T.I., Dobavki v beton
(Additives to Concrete), Moscow: Stroiizdat, 1989.
3. Akhrimenko, V.E. and Akhrimenko, Z.M., Izv. Vyssh.
Uchebn. Zaved., Severo-Kavkaz. Region, Estestv. Nauki,
2000, no. 1, pp. 76–78.
4. Izgotovlenie i primenenie gipsovykh stroitel’nykh
materialov (Gypsum: Production and Applcation of
Gypsum Building Materials), Brückner, H.P. et al.,
Мoscow: Stroiizdat., 1981.
5. Akhrimenko, V.E., Str–vo Neft. Gaz. Skvazhin Sushe More,
2006, no. 5, pp. 34–36.