33 Available online at www.irejestjournal.

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International Research Journal in Engineering, Science and Technology
IREJEST. June 2011, 8(1) 33-42. ISSN-1597-5258.


The Influence of Gypsum on Foundry Slag for Cement Making
O. O. Egunlae
Mineral Resources Engineering Dept. Federal Polytechnic, P.M.B 5351, Ado Ekiti
e-mail: olawaleegunlae@yahoo.com
Abstract
The right positioning of cement industry is important for the growth of any nation. Only one type
of cement is produced in the country. In the recent years the price of cement and cement
products are increasing on daily basis. Hence, there is need for diversification. The use of
locally available raw materials will lead to the production of other cement products (e.g slag
cement, High alumina cement and so on). This work focused on the investigation of influence of
gypsum on the mechanical properties of slag cement using local foundry slag as the main raw
material. The tests carried out include compressive strength test, setting time, moisture content
and linear shrinkage. Results show that the cement has low strength development which
increased with increasing curing time similar to the commercial Blast furnace slag cement and
Ordinary Portland Cement (OPC). The material retained moderate amount of water which
allowed adequate setting time of about 30 minutes with high thermal stability in terms of the
linear shrinkage at low temperature. Thus, this forms part of research works on the use of local
foundry slag available in country the as a prelude to recycling of waste Blast furnace slag BFS
products expected from Ajaokuta steel plant when it becomes fully operational.

Key words: gypsum, setting agent, local foundry slag, cement making

Introduction
One of the greatest challenges facing the
Nigeria industries generally is the issue of
research into the use of local raw materials
(Fayose, 1987; Agbazue 1988, 1990, 1992;
Ali,1997; Daggash, 1997; Onyemaobi
2001). Then, with the gradual progress in
the field of iron and steel in Nigeria, the
problems of machinery and machine spare
parts would begin to improve. In many
countries of the world, cement manufacture
sort locally and this is a challenge to Nigeria
to utilize the cement substance to produce
good quality cement. (Erdem and Olmes
(1993); Gillot and Wang (1993); Ichikawa
and Komukai 1993)

The importance of cement industry in the
Nigerian economy cannot be over
emphasized since cement plays a vital role
in building and construction sectors. From
time past, efforts are being made by the
Federal Government, the Nigerian society of
Engineers (NSE), cement manufactures
Association of Nigerian (CMAN) and other
related bodies to strengthen the cement
industry for the economic growth of Nigeria.
(Ali, 1997; Daggash, 1997)

The quest for diversification into different
types cements products and minimized cost
of production leads to the main focus of this
work. The research is made into the use of
local foundry slag for cement production as
alternative prior to production of blast
furnace slag in Nigeria. Moreover, the
cement companies production cannot meet
to the daily demand which resulted in price
skyrocketing of cement in Nigeria. (Egunlae
et al. 2002; Egunlae and Oloruntoba, 2002;
Egunlae 2009 and 2010)

34 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


The work assesses the influence of gypsum
on the mechanical properties (such as
compressive strength test, linear shrinkage
test, setting time and moisture content) using
local foundry slag as main raw material for
slag cement.
Cement may be defined as adhesive
substances capable of uniting fragments or
masses of solid matter to a compact whole.
Blast furnace slag is a by-product obtained
in the manufacture of pig-iron in the blast
furnace (The Crust, 2003), and is formed by
the combination of the earthly constituents
of the iron ore with the limestone flux. The
essential components of slag are the same
oxide, as are present in Portland cement
namely lime, silica and aluminium, but their
proportions differ. Therefore, slag has found
a considerable use in the road and building
industries and in the production of
cementing materials, as an aggregate in
concrete and in the manufacture of slag
wool for thermal insulation. Therefore, slag
cement contains a larger percentage of slag
with different component, gypsum and other
additives which is also capable of uniting
loose particles together.

By standards here are different types of
hydraulic, Portland and slag cements (ACI
1995; API, 1991; ASTM, 2001; Bensted,
1993; BSI, 1996 and 2002) among which the
most popular include;

Granulated blast furnace slag is the product
obtained by the rapid chilling of a basic
(high lime) blast furnace slag, a sit emerges
from the blast furnace; it is a high, friable
and porous product. Slag cement, or cold
process slag cement: Sometimes it is called
a mixtures of hydrated lime and granulated
blast furnace slag. Certain salts may be
added to accelerate the set. This type of
cement is known in Belgium as cement de
laitier. (Lea, 1970; Matusinovic and Curlin,
1993; Sehra et al, 1993)

Portland cement clinker and granulated blast
furnace slag in proportions, as defined in the
British standard, such that the content of
granulated slag does not exceed 65% of the
whole. Similar cements, but with various
permitted proportion of granulated slag, are
manufactured in other countries. (BSI, 1996
and 2002)

Super sulphated cement is composed
essentially of granulated blast furnace slag,
calcium sulphate and a small percentage of
Portland cement or lime.
Portland cement: This may be defined
according to British Standard as a product
obtained by intimately mixing together
calcareous and argillaceous or other silica,
alumina, and iron oxide bearing materials
burning them at a clinkering temperature
and grinding the resulting clinker.

i. Rapid hardening Portland cement is
similar to ordinary Portland cement, but
is normally ground finer and slightly
altered in composition. Its setting time is
similar, but it develops its strength more
rapidly.
ii. Quick setting Portland cement differs
only from a normal Portland cement in
that its setting time is less. Its rate of
hardening may be similar to that of
ordinary or rapid hardening Portland
cement.
iii. White Portland cement is an ordinary
Portland cement containing only a low
proportion of iron oxide, so that its
colour is white instead of grey.
iv. Mansory cements are cements that
consist of materials use in mortar. It
gives more plastic mortal than ordinary
Portland cement. They are also made by
inter-grinding mixtures of Portland
cement with hydrated lime, granulated
slag, or inert fillers with the addition of
35 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


calcium stearate or some other
waterproofing agents.
v. Natural cements are formed by calcining
a naturally occurring mixture of
calcareous and argillaceous substances at
below sintering point (Agbazue, 1989)
High alumina cements: These types of
cement are manufactured by fusing a
mixture of limestone and bauxite. The
ASTM specification places no limit to MgO
content but limits the SO
3
content to 3.0%
and the sulphide sulphur to 2.0%. The
German standard requires that slag should
conform to this formula.
(CaO + MgO + Al
2
O
3
) / S;O
2
. (1)

Materials and Equipment
The materials used and their sources are
shown below:
Samples 1, 2, 3, 4 and 5 were obtained from
different places.

Procedure
Each slag of samples, gypsum and clay were
crushed by Jaw crusher and pulverised using
the vibratory mill. The products of slag
samples and clay from the pulverizing
machine were further sieved by sieve shaker
into fine particles where the sieve sizes
ranged from 75mS ~ 120m.

Weighing and Mixing: The ratio 80:15:5
was first used for the blending of each slags
with clay and gypsum. That is the 80 percent
of each slays samples was mixed with 15%
clay and 5 % gypsum. Then about 10ml of
water was poured to the blended materials to
form a slag paste. Spatula was used to mix
the slag paste thoroughly on a flat iron plate
surface. After all these, the slag pastes
formed were poured into different plastic
cylindrical containers tagged with number of
days, that is 3, 7 and 28days. Another slag
paste was poured into shrinkage mould for
each slag samples to determine their
shrinkage tests and also the setting time was
observed. Finally the 100% slag water was
prepared for each samples and the
compressive strength test taken.

Effect of increasing percentage of gypsum
on the compressive strength, setting time
and linear shrinkage. The Five slag samples
were mixed together to form slag blend. The
slag blend was sieved to -75m size and the
percentage ratio (99% slag + 1% gypsum +
98% slag + 2% gypsum, 97% slag + 3%
gypsum, 96% slag + 4% gypsum and 95%
slag + 5% gypsum was used.

Setting time test - stop watch and clock
were used to time the slag paste (starting
from the initial time of mixing with water
till the time when the each slag paste
resisted the motion of a stirrer used to stir it.
The setting time was obtained as,

setting time = Final setting time initial
setting time .(2)

Linear shrinkage tests: The slag paste was
poured in to a shrinkage mould and it was
carefully spread on the mould. The linear
length of the slag paste in the mould was
measured at 3-days, 7-days and 28days.

Linear Change % = Final length-original length x 100 (3)
Original length 1

Compressive strength test: The each
samples of the slag paste after the each
specified days, (3,7, and 28 days) was taken
for compressive strength. Firstly, the
diameter of the plastic cylindrical container
was measured to be 2.8cm, then the machine
readings were noted. The results are shown
in Tables 3, 4, 5 and 6

Compressive strength =
Compressive force /Cross-sectional Area
(4)


36 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


Discussion
The result of chemical composition of slag
samples [using the Atomic Absorption
spectrometer (AAS)] is shown in Table 1
and clay, gypsum, clinker and Portland
cement are shown in Table 2.

Table 1 shows that the major components
and minor components that constitute
cement such as (Al
2
O
3
, SiO
2
, CaO and
Fe
2
O
3
, ZnO, Na
2
O, K
2
O and CuO
respectively) are present in slag samples.
Thus, it can be deduced that the slags have
some cement constituent characteristics but
in lower proportions. Also, it is discovered
that the minor component have larger
quantities than the major components, hence
this might have resulted from the various
compositions of metal scraps used for
smelting from which the slag were obtained.
The compositions of ordinary Portland
cement and blast-furnace slag are monitored
right from the raw materials used as shown
in Table 2. (Erdem et al 1993; The Crust,
2003). Therefore the samples in Table 1
were not monitored from point of
production, so undesired result was
obtained.

The result of compressive strength tests in
Table 3 shows that samples 1, 2 and 3
possess cementitious characteristics than
samples 4 and 5 in terms of compressive
strength development with time. The
behaviour of sample 4 and 5 could be traced
to Table 1, since they are both ferrous slag
and have lower quantities of major raw
materials.

Also from Table 4, the compressive strength
values of samples 4 and 5 are zero while that
of sample 1, 2 and 3 increased with increase
in time. The behaviour of samples 4 and 5
might be due to the low quantity of major
components like CaO, SiO
2
and Al
2
O
3
.
Therefore the samples need the addition of
cementing agents. (Lea, 1970).

Table 5 shows the compressive strength
values obtained from blend samples for both
100% slag and the ratio of three additives.
The blend 2 (80% blend slag + 15% clay +
5% gypsum) has a better compressive
strength with increase in time than Blend 1
of 100% blend slag. Lea, 1970; Erdem and
Olmes 1993 explained that cementing agents
such as clay, gypsum, air entrainer (Taylor
1964) and so on have positive effect on the
compressive strength of the material and
also reduce the porosity.

Table 6 shows the compressive strength of
increasing % of gypsum made from slag
blend. It is observed that the compressive
strength values of day three were very low.
This might be due to the presence of much
moisture content. Lavoisier in 1765 showed
that the setting of gypsum was due to the
recombination of the calcium sulphate with
the water of crystallization of which it had
been deprived by heat. Therefore, the
compressive strength is increased with the
increase in percentage of gypsum and
increase in time. Le chatelier ascribed the
development of cementing strength to the
precipitation of hydration products in the
setting of gypsum. Then the increasing % of
gypsum and precipitation bring cohesion but
much gypsum acts as retarders or
accelerators.

Tables 7, 8 and 9 show the result shrinkage
tests carried out on various slag samples. It
is observed that the values recorded were
zero. This shows that the samples have good
cement characteristics since the samples did
not shrink. Yet it can be seen that they
behaved contrary to Hooks law that shows
relationship between the expansion as water
is absorbed and the two dimensional
pressure exerted by the absorbed water film.
37 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


It can be concluded that the swelling
pressure and concentration due to vapour
pressure are zero. Egunlae 2009 and 2010
explained that the amount of gypsum
required for minimum shrinkage increases
with the content of 3C
a
O. Al
2
O
3
and of
alkalis in the cement. Relating Table 9 to
this, it can be deduced that the slag
composition has affected the non shrinkage
behaviour.

Table 10 shows the setting time of the
various samples, it is observed that the
increasing percentage of gypsum reduces the
setting time, it can be deduced that the
addition of gypsum rendered it more plastic
and affected the setting time being a
retarded. It is known that di-calcium silicate
() exhibits no definite setting time and the
gauged mass of slag sets only slowly over a
period of some days. Thus relating this to
mixture of ratio 80:15:5, it can be deduced
that the slag composition with higher
content of lime (CaO) set quickly compare
with samples 4 and 5 with lower content of
lime (CaO). Also, Lea F Arnold 1970
explained that the solubility of gypsum is
decreased by the presence of lime, therefore
samples 1 and 2 behaved normally.

Tables 10 - 12 show setting time (min)
values obtained from slag and gypsum
mixtures. In Table 10, the setting time (min)
values obtained from slag blend gypsum
mixture is about 65 mins. For each of pure
slag sample in Table 11 the setting time
(min) values varied as 45 mins and 40 mins
for samples 1 and 2, while sample 5 set after
90 mins. The results of increasing content of
gypsum from 1% to 5% in Table 12 shows
that setting time (min) values increased with
increase in %gypsum addition

Table 13-15 show the moisture content (%)
characteristics obtained from slag samples
after 3, 7 and 28 days. Increased percentage
gypsum samples have greater moisture
content than others. Therefore the
combination of slag, clay and gypsum
display better moisture content than the
increasingly % gypsum samples. The water
loss was low in 80:15:5 ratio sample,
therefore possess sufficient stability to
withstand cracking.

Conclusion
From the results obtained from all the tests
carried out on the mechanical properties of
local foundry slag, it can be deduced that the
major components of the slag used
determined their behaviour as compare to
Ordinary Portland Cement. That is the
ferrous slag behaved irrationally while the
non-ferrous showed better cementing
properties.

Also the setting and hardening of foundry
slag cement could not be fully understood
due to the variation of slag components
used. Nevertheless, the addition of gypsum
to local foundry slag cement not only
controls the set but also influence the
properties. Therefore the setting time is
affected by the addition of gypsum in a
manner similar to that of Portland cement,
that is the gypsum added acted as a retarder
in this experiment. Moreover, the high
porosity and expansive nature of some of the
slag can be reduced by finding out
appropriate additives like air entrainer,
accelerators such as NaCl, CaCl
2
, and CaC
2

and so on. The addition of gypsum to the
sample mass rendered it more plastic and
has some effect (positive) on the setting
time. Therefore the increasing percentage of
gypsum on foundry slag cement gave some
positive results that are comparable with that
of influence of gypsum on other standard
cements.
As part of the research works into the use of
foundry slag in slag cement production on
38 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


commercial quantity, these are
recommended.
i. There should be further investigation on
the suitable percentage of gypsum that
will give best result based on the slag
composition.
ii. The need for Government to
collaborate with cement manufacturers
Association of Nigerian to create a
serious research centre that will test for a
cheapest cost of producing quality slag
cement using local available material
such as (foundry slag clay, gypsum and
so on)
iii. The need for creating another means of
utilizing the waste products from
Ajaokuta steel plant when it would be
fully operated. This can lead to the idea
of recycling the industrial waste to
produce Blastfurnace slag cement of
various type.
iv. Government should set the ball rolling
by reviewing the cement standard
specification to bring it in line with local
run materials available, economic needs
and the world wide trend for
manufacturing multiple type of cements.

References
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in productivity improvement in the cement
works. National seminal on cement. NSE
June 28-30, 1988, Lagos.

Agbazue V. E. (1990): Manual on Basic
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nd
Edition) F.
D. Press Ltd, Nigeria.
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Ali H.K. (1997): Policies of federal
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Pp 1-11.

America Concrete Institute ACI 1995
ground granulated blast furnace slag as a
cementitious constituent in concrete
Farmington Hills Michigan.

American Petroleum Institute (1991).
Specification for well cements, API
specification 10A, 21
st
Ed. 1991.
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ASTM (2001) standard specification for
ground granulated blast furnace slag for use
in concrete and mortals, West Conshocken
P.A.

Bensted J (1993): the value of ICPMS in
heavy element trace analysis of oil well
cements for environmental monitoring
purposes. Cement and concrete research.
Vol 23 No 1. pp994.

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Specification For High Slag Blastfurnace
Cement (London) BS 4246, Page 12

British Standard Institution (2002):
Specification for ground granulated blast
furnace slag for use with portland cement,
BS 6699, Page 18

Daggash M.M (1997), Problems and
prospects of sourcing raw materials for the
cement industry in a depressed economy,
Nigeria Mining Journal
Vol. 2, Pp 31-35

Egunlae O.O and Oloruntoba D.T. (2002)
possibility of slag cement production in
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Congress (NIMACON) EMDI, Akure. Nov
11-13, 2002. 1(1): 200-202,

Egunlae O.O. (2009). Assessment of
foundry slag for cement production in
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th
Engineering
Forum Nov. 9-12, 2008, SOE, FPA Ado
Ekiti. 5(1): 236-240.
39 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42



Egunlae O.O (2010) Effect of set
accelerators on cementing properties of
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containing phospho-gypsum cem con Res
vol 23 No1 pergamon press USA

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press USA.

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Cement and Concrete (3
rd
Edition) Edward
Arnold Published Ltd, London.
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mineral resources development. Proceedings
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port- Harcourt Nov. 5-9, 2001. pp21-25

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Rapid Setting Magnesium Phosphate
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Vol 23 Pp 254-266.

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and steel plant (The Crust; News letter of
NMGS March 2003 Vol26.1, Edited by A.A
Elueze, Fab)

Table 1: Chemical content of slag samples using the Atomic Absorption Spectrometer (AAS)
% composition of oxides in slag Oxides
Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 (slag-mix)
SiO
2
1.69 1.02 1.51 0.38 0.64 5.90
Al
2
O
3
1.60 1.71 1.67 0.92 0.01 2.97
CaO 22.47 23.81 17.6 14.56 16.20 5.30
MgO 10.06 8.69 12.75 16.12 11.71 18.70
Fe
2
O
3
10.26 9.43 5.49 3.67 7.92 4.33
Na
2
O 17.52 14.36 15.33 12.71 14.12 9.20
K
2
O 9.02 6.13 7.31 7.99 7.56 5.90
ZnO 7.17 6.44 7.87 6.07 10.80 14.20
PbO 2.43 2.51 1.52 2.14 1.48 1.90
CdO 0.85 0.62 0.64 0.94 1.08 1.30
CuO 14.36 10.93 6.10 5.97 8.67 22.40
MnO
2
1.86 1.72 1.51 1.69 2.07 1.50
NiO 0.94 0.81 0.40 0.49 0.92 1.60
AS
4
O
6
0.05 0.08 0.07 0.04 0.03 0.93
Cr
2
O
3
0.38 0.13 0.13 1.10 0.21 1.15
40 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42



Table 2: Chemical composition of clay, gypsum, clinker and Portland cement additives











(Source: WAPC PLC, Ewekoro)

Table 3: Compressive strength (N/mm
2
) values obtained from different samples of 100% slag-
water mixtures using slag samples 1 to 5 after 3, 7 and 28 days.
100% slag water mix 3 days (N/mm
2
) 7 days (N/mm
2
) 28 days (N/mm
2
)
Sample 1 0.018 0.035 0.035
Sample 2 0.000 0.018 0.062
Sample 3 0.009 0.035 0.035
Sample 4 0.000 0.000 0.000
Sample 5 0.000 0.000 0.000

Table 4: Compressive strength (N/mm
2
) values obtained from different samples of 80% slag+
15% clay + 5% gypsum mixtures slag samples 1 to 5 after 3, 7 and 28 days.
80:15:5 of slag:
Clay: Gypsum
3 days (N/mm
2
) 7 days (N/mm
2
) 28 days (N/mm
2
)
Sample 1 0.009 0.009 0.044
Sample 2 0.035 0.097 0.106
Sample 3 0.000 0.009 0.027
Sample 4 0.000 0.000 0.000
Sample 5 0.000 0.000 0.000

Table 5: Compressive strength values obtained from blend sample, made from samples 1 to 3
with additives after 3, 7, and 28 days.


Samples
Compressive Strength (N/mm
2
) in
3 days 7 days 28 days
Blend 1 (100% blend
slag-water)
0.000 0.027 0.044
Blend 2 (80% slag +
15% Clay, 5% gypsum
0.018 0.053 0.080


% Composition of Oxides in additive Oxides
Clay Gypsum Clinker Portland
Cement
S
i
O
2
39.76 2.03 21.27 20.00
Al
2
O
3
49.90 0.63 5.08 5.24
CaO 0.98 35.62 64.87 63.44
MgO 0.77 1.23 2.69 2.77
Fe
2
O
3
0.51 0.30 3.61 3.33
T
i
O 1.85 - - -
Na
2
O 0.60 - - -
41 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


Table 6: Effect of gypsum increase on Compressive strength (N/mm
2
) values obtained from
different samples of slag blend mix after 3, 7 and 28 days.
% Gypsum
increase
Compressive strength (N/mm
2
) in
3 days 7 days 28 days
1 0 0 0.017
2 0 0.017 0.027
3 0 0.017 0.073
4 0 0.037 0.105
5 0 0.037 0.105


Table 7: Result of shrinkage test obtained from blend samples made from samples 1 to 5 after 3,
7, and 28 days.
Shrinkage values in
3 days 7 days 28 days
Blend 1 (100% blend slag-
water)
0.00 0.00 0.00
Blend 2 (80% slag + 15% Clay,
5% gypsum
0.00 0.00 0.00


Table 8: Shrinkage values obtained from different samples of 80% slag+ 15% clay + 5%
gypsum mixtures slag samples after 3, 7 and 28 days.
80:15:5 of slag: Clay:
Gypsum
Shrinkage values in
3 days 7 days 28 days
Sample 1 0.000 0.000 0.000
Sample 2 0.000 0.000 0.000
Sample 3 0.000 0.000 0.000
Sample 4 0.000 0.000 0.000
Sample 5 0.000 0.000 0.000


Table 9: Shrinkage values obtained from slag blend gypsum mix after 3, 7 and 28 days.
% Gypsum increase 3 days 7 days 28 days
1 0.000 0.000 0.000
2 0.000 0.000 0.000
3 0.000 0.000 0.000
4 0.000 0.000 0.000
5 0.000 0.000 0.000

42 IREJEST Vol.8 No. 1 June, 2011 The Influence of Gypsum on Foundry Slag pp. 33-42


Table 10: Setting-time (min) values obtained from different samples of 80% slag+ 15% clay +
5% gypsum mixture
Sample Setting-time (min)
80:15:5 (slag blend: Clay: Gypsum) 65

Table 11: Setting-time (min) values obtained from different samples of 80% slag+ 15% clay +
5% gypsum mixtures
80:15:5 (each slag: Clay: Gypsum) Setting-time (min)
Sample 1 45
Sample 2 40
Sample 3 60
Sample 4 85
Sample 5 90

Table 12: Setting time (min) values obtained from slag blend gypsum mixture
% Gypsum increase Setting-time (min)
1 35
2 30
3 22
4 18
5 16

Table 13: Moisture content (%) obtained from slag bend samples after 3, 7 and 28 days.
Sample Moisture content
(%)
after 3 days
Moisture content
(%)
after 7 days
Moisture content
(%)
after 28 days
slag blend-water mix: 1.1 0.7 0.7
80:15:5 (slag blend:
Clay: Gypsum)
2.1 1.6 1.6

Table 14: Moisture content (%) obtained from different samples of 80% slag+ 15% clay + 5%
gypsum mixtures after 3, 7 and 28 days.
Sample Moisture content
(%)
after 3 days
Moisture content
(%)
after 7 days
Moisture content
(%)
after 28 days
Sample 1 1.413 1.527 1.510
Sample 2 1.412 1.507 1.520
Sample 3 1.410 1.542 1.602
Sample 4 1.644 1.601 1.865
Sample 5 1.744 1.750 1.876