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CHAPTER 4
MATERIALS INVESTIGATION
4.1
INTRODUCTION
Samples of each and every constituent material are tested in
laboratory for their physical and chemical properties. This results of various
tests conducted are presented in this chapter.
4.2
concrete in this research. The total requirement was calculated and was
purchased from local dealers and stored in a dry place inside casting yard and
kept covered with tarpaulin sheets, to avoid clotting. RAMCO 43-grade
cement has been used throughout this investigation. The physical properties
of the cement obtained from the tests conducted as per relevant IS codes are
shown in Table 4.1.
Table 4.1 Physical properties of cement
Sl.
Physical property
No.
Tested
value
1. Specific gravity
3.10
2. Standard consistency
Setting time
3. Initial
Final
4. Soundness test
5. Compressive strength (28 days)
30%
Reference Code
Le-Chatelier flask
IS : 1727-1967
IS : 4031-1968 part 4
IS : 4031-1968 part 5
57 minutes
IS : 4031-1968 part 5
4 hours
0.95 mm Le-Chateliers apparatus
44.37MPa
-------
43
Chemical Compound
Average %
Permissible limits
Silica (SiO2)
20.99
------
Alumina (Al2O3)
6.05
6.01
62.74
---------
1.33
5% max (BIS)
1.82
1.14
Alkalies
0.8
1.5%, max(BIS)
Chlorides
0.015
------
0.88
0.66-1.02, max(BIS)
Lime saturation
factor(LSF)
44
4.3
FINE AGGREGATE
The fine aggregate used in this investigation was clean river sand
passing through 4.75 mm sieve with fineness modulus 3.0, the specific gravity
2.60 and the bulk density was 1.72 and 1000 gm of sample was taken for test.
The particle size distribution is given in Table 4.3. The tests on sand were
carried out as per IS: 2386-1963(III). The sand used belonged to Zone II. The
grading curve is given in Figure 4.1.
Table 4.3 Sieve analysis of fine aggregate
Sieve size
(mm)
Weight of
material
retained
(gm)
% Weight of
material
retained
Cumulative
% weight of
material
retained
% Weight of
material
passing
4.75
100
2.36
74
7.4
7.4
92.6
1.18
367
36.7
44.1
55.9
0.60
132
13.2
57.3
42.7
0.30
317
31.7
89
11
0.15
110
11
100
4.4
COARSE AGGREGATE
Locally available crushed blue granite metal aggregate of size 20
mm and below was used and various tests were carried out to ascertain the
physical properties of coarse aggregate which are listed in Table 4.4.
45
120
percentage passing (%)
100
80
60
40
20
0
0.1
1
Sieve size(mm)
Specific gravity
Fineness modulus
Tested
value
2.75
7.12
Percentage voids
Crushing value
39.02%
27.07%
Physical property
Reference code
FLY ASH
46
% by Weight**
% by Weight
Silica (SiO2)
50.20
63.53
Alumina (Al2O3)
26.30
27.40
2.27
1.26
14.40
3.67
0.58
0.85
1.48
0.35
0.36
0.19
1.57
----
0.32
0.01
0.58
0.9
Titanium Dioxide
** Australian fly ash (Typical)
------
1.84
47
WATER
Potable water was considered throughout this study for diluting
NaOH flakes, for manufacturing OPC concretes and for preparing aggressive
liquids. The amount of solids was below the permissible limits as specified by
48
IS: 456-2000. The result of quality control tests done on water is presented in
Table 4.6.
Table 4.6 Results of water quality analysis
Serial
No.
1.
2.
3.
4.
4.7
Description of test
pH value
Hardness (ppm)
Sulphate (ppm)
Chlorides(ppm)
Water
sample
8.9
403
100
137
Maximum
permissible limit
6.0-9.0
1000
400
500
ALKALINE LIQUIDS
A combination of sodium hydroxide and sodium silicate was used
in this study to prepare the alkaline solution. Both the chemicals are
commercially available in the local market.
4.7.1
in viscous translucent liquid form, was purchased from the local suppliers. Its
reactivity with sodium hydroxide depends upon the Na2O/SiO2 ratio which
was maintained as 2.2. The mass of soluble silicate (SiO2) and sodium oxide
(Na2O) present in sodium silicate liquid is 33% and 15% respectively. The
picture of sodium silicate is shown in figure 4.4.
4.7.2
49
Handling the flakes with bare hands gave a sense of irritation, and it
necessitated the use of gloves. Initially, the solution was prepared and kept in
metal containers. Due to the exothermic heat developed during dissolution,
the metal containers started to melt. So, the solution was mixed and kept in
plastic containers. The picture of NaOH flakes is shown in Figure 4.5 and the
composition of sodium hydroxide flakes is presented in Table 4.7.
Table 4.7 Composition of sodium hydroxide flakes
Chemical compound
Composition
99 % by weight, min.
Iron (Fe2O3)
Heavy metals
20 ppm, max.
50
4.8
CHEMICAL ADMIXTURES
In order to improve the workability of stiff and fresh concrete to
GLENIUM B233. It was purchased from BASF, India which is a high range
water reducing Superplasticiser based on modified polycarboxylic ether
formulation. The product has been primarily developed for applications in
high performance concrete where the highest durability and performance is
required. GLENIUM B233 is free of chloride (< 0.2%) and low alkali. It is a
light brown colour liquid with relative density 1.09 and pH value greater than
6. The specific gravity of this GLENIUM B233 is 1.09 and solid contents not
less than 30% by weight. The product has complied with ASTM C494 Type F
and shall be free of lignosulphonates, naphthalene salts and melamine
formaldehyde when subjected to IR Spectra.
4.8.2
trade name Conplast 320 was purchased from ROFF chemicals private
limited, Chennai.
51
4.9
MIXTURE PROPORTIONS
4.10.1
tests and all the OPC concretes produced were taken as reference concrete.
The mixture was designed according to IS Code method of design. The target
strength of the OPC concrete control mix was 30 MPa for normal strength
concrete and 50 MPa for high strength concrete. The same amount of
superplasticizer was added in the mixtures to match with Geopolymer
concretes. A detail of mix design calculation is presented in Appendix 1. The
mixture proportion of the control mix for normal strength concrete and the
mix proportion of the high strength concrete are presented in Table 4.8. The
nomenclature of concrete giving 30MPa compressive strength will be
henceforth addressed as M 30 and the same for concrete of strength 50MPa
will be addressed as M50 concrete in this report. The OPC control concretes
M30 grade and M50 grade were prepared using the mix ratios 1:1.84: 3.6
1and 1:0.94:3.07 with water cement ratio 0.38 and 0.34 respectively. The
52
water cement ratio was effectively maintained and concrete was mixed in a
pan mixer for accurate results.
Table 4.8 Mix proportions of M30 and M50 grade concretes
20
M30
in kg / m3
380
M50
in kg / m3
--
12
502
809
380
540
River sand
642
425
Cement
350
450
7.5
--
---
125
145
Constituent Materials
Coarse aggregate
in mm
Lignosulphonated based
Superplasticizer
Carboxylic based
Water
4.10.2
referring GCI report (Hardjito et al 2005) and assuming some parameters such
as aggregate content, alkaline/fly ash ratio and sodium silicate/sodium
hydroxide ratio. The calculation was used to obtain the quantity of fly ash,
aggregate, solid sodium hydroxide, sodium silicate, and water.
The primary difference between Geopolymer concrete and Portland
cement concrete is the binder. The silicon and aluminium oxides in the lowcalcium fly ash react with the alkaline liquids to form the Geopolymer paste
that binds the loose coarse aggregates, the fine aggregates and other unreacted
53
G50
in kg / m3
in kg / m3
20
388
--
12
543
841
363
360
River sand
554
647
Fly ash
378
408
Sodium Hydroxide
50
63
Sodium Silicate
124
138
7.5
--
---
---
---
Constituent Materials
Coarse aggregate
in mm
Lignosulpho-
Super
Plasticiser
nated based
Carboxylic based
Water
54
from that of the proportion adopted by Vijaya Rangan to suit the properties of
Indian fly ash.
4.11
concrete is the binding phase. This is the main constituent of concrete which
binds coarse aggregates together to make a strong concrete. This binder could
be prepared from silicates and hydroxides of sodium or potassium, but to
achieve the desirable strength and durability properties of concrete, it was
carefully chosen in such a way that all the combinations of sodium and
potassium salts were tried.
The mixture proportion for mortar was selected based on Table 3.4
in GC-1 report by Hardjito et al (2005). For this preliminary study, 70.6 mm
size mortar cubes of 1:1 ratio were produced. Four different types of mixtures
were tried.
The mortar cubes cast with silicates + hydroxides of sodium,
potassium silicate + sodium hydroxides, silicates + hydroxides of potassium
and sodium silicate + potassium hydroxide were designated as N1, N2, K1
and K2 respectively. Out of the four combinations, the best combination was
chosen for further study, keeping in mind not only strength but also
economical factors. The best combination was salts of sodium. Further,
Geopolymer mortar cubes of various molarity of sodium hydroxide were tried
for fixing the concentration of molarity. All the four combinations that were
tried out are tabulated in Table 4.10.
55
4.12
4.12.1
Mortar Cubes
All the Geopolymer mortar cubes for this research work was
1.
2.
3.
Designation
of cubes
Combination of
salts
N1
Sodium hydroxide
and Sodium
Silicate
N2
Sodium hydroxide
and Potassium
Silicate
K1
K2
Potassium
hydroxide and
Potassium Silicate
Potassium
hydroxide and
Sodium Silicate
Materials
Sand
Flyash
Sodium silicate
Sodium hydroxide
Super Plasticiser
Sand
Flyash
Potassium silicate
Sodium hydroxide
Super Plasticiser
Sand
Flyash
Potassium silicate
Potassium
hydroxide
Super Plasticiser
Sand
Flyash
Sodium Silicate
Potassium
hydroxide
Super Plasticiser
Mass
(kg/m3 )
1052
774
196
78
12
1052
774
196
78
12
1052
774
196
78
12
1052
774
196
78
12
56
4.12.2
Concrete Cubes
The size of both Geopolymer concrete cubes and OPC concrete
57
4.12.6
the study of flexural behaviour. Out of this, series-A and series-B were of real
sized beams with different percentage of steel reinforcement for studying
exclusively the flexural behaviour. The first series-A was designed as a
representation of GB II - 3 of Sumajaouw (2006) beams and the second
series-B was designed based on the results of GB II 3 beams. Six specimens
were cast for each series at the rate of three specimens per M30 and G30
concretes. Totally, 12 numbers of beams were cast. But series-C beams of
model size were cast to evaluate flexural behaviour and durability
characteristics.
4.12.6.1
Series-A beams
A
2 X 12Y
200mm
2 X 12Y
8Y @
100mm
100 mmC/C
c/c
300mm
3x20Y
3300 mm
SEC - AA
Scale = 1:50
3x20Y
LONGITUDINAL SECTION
LONGIDUDIANAL
SECTION
Scale = 1:50
58
2 X 10Y
150mm
8Y
mm Bars @ 75 mm c/c
2 X 10Y
200mm
8Y @
100
C/C
100 mm c/c
2 X 12Y +
1X 10 Y
2x12Y +1x10Y
8 8mm
Y Bars @ 100 mm c/c
400 mm
SEC - AA
Scale = 1:50
1200
mm
LONGITUDINAL SECTION
Scale = 1:50
59
flexure span of the beam. All the rods used were of Fe500 grade. The clear
cover to main reinforcement was 25 mm all around.
4.12.6.3 Series-C beams
The series-C concrete beams 100mm x 100mm in cross-section and
500mm long were cast in steel moulds, three for each M30 and G30. The
details of the specimen are presented in Figure 4.8. Two numbers 8mm
diameter rods for tensile reinforcement, 2 numbers 6mm diameter hanger rods
with 6mm diameter two legged stirrups at 50mm centers were fabricated. The
grade of rods for tensile reinforcement was Fe500 and for others were Fe250.
The clear cover of the main reinforcement was 10mm all around the cross
section. These beams were cast in order to evaluate the residual flexural
strength after immersion in sulfuric acid of 10% concentration, 5% sulfuric
acid + 5% hydrochloric acid, 10% magnesium sulphate and 10% sodium
sulphates solution. The molarity of sodium hydroxide was fixed as 8M. For
8Y
100mm
6 mm Bars @ 50 mm c/c
2 X 6R Hanger Bars
100mm
6R @ 50
50mm
mmc/cC/C
2 X 8Y Main Bars
SEC - AA
Scale = 1:50
LONGITUDINAL SECTION
Scale = 1:50
60
4.13
61
prepared which appeared like crystal clear water Figure 4.9 and Figure 4.10
show the sodium silicate and sodium hydroxide solutions.
Geopolymer mortar with coarse aggregates. Coarse and fine aggregates were
in oven dried condition under direct sun heat. To make better binding, all the
surfaces were made wet uniformly, to make fly ash-based Geopolymer
62
concrete. The saturated surface dried fine aggregate looked damp and
appeared to be free flowing. For mixing, a rotating pan mixer of 150 kg
capacity with two rotating wheels, as shown in Figure 4.11, was used.
Because of the adequate capacity of the pan mixer, two batches of concrete
were prepared to cast three beam specimens. The fly ash and sand were first
mixed in the laboratory pan mixer for about three minutes. At the end, the
alkaline liquid was added to this mixture and the mixing continued for another
four minutes to initiate polymerization. After all the ingredients were mixed
up thoroughly, the resultant was Geopolymer mortar. To this mortar, coarse
63
64
Table Compaction
As strength and density are closely related to the degree of
compactness, a table vibrator was used instead of a needle vibrator for better
compaction. The sides and bottom of steel moulds were coated with crude oil
to prevent the mix sticking to the mould and for easy demoulding. The
moulds were filled with fresh concrete to one-third height and kept over the
table vibrator. The vibration was done for 12-15 seconds until the concrete
was leveled. Again concrete was put into the mould, layer by layer, up to the
top of mould and got vibrated for a few seconds. For better and uniform
65
compaction, each layer was vibrated for 12 to 15 seconds and the specimens
being vibrated is shown in Figure 4.14.
66
Figure 4.16
67
could be altered to suit the profile of the elements. The cast specimens are
kept inside this chamber at 70oC for duration of 8 hours to 24 hours. Dry
cured specimens were left in the moulds for at least six hours in order to avoid
a drastic change in the environmental conditions. After demoulding, the
specimens were air dried in the room until the day of the test. The heat curing
chamber in operation mode is exhibited in Figure 4.15 and the Geopolymer
concrete cubes kept inside the curing chamber is shown in Figure 4.16.
4.14
68
MANUFACTURING
PROCESS
OF
SERIES
AND
SERIES C BEAMS
The manufacturing process of these two beams namely, series-B
and series-C, was the same as that of the other manufacturing process
mentioned in clause 4.12. In these two series, the beams were compacted by a
table vibrator instead of a needle vibrator. The reinforcement cage was placed
inside the steel moulds, and all the sides and bottom were applied with oil
before the concreting was done. To maintain the cover on the reinforcements,
cement briquettes were placed below the reinforcement cage prior to
concreting. Extra care was taken to avoid the displacement of the cage while
concreting, thus maintaining the cover.
4.16
69
stage, coarse aggregate was added to the mortar and the uniformity of the
mixing of concrete was checked. The measured quantity of superplasticiser
was added to get workability. The workability was measured by a slump test
on the fresh OPC concrete. The fresh mix was poured into the moulds that
had been coated with crude oil. Compaction was done with the aid of a table
vibrator and the specimens were manufactured. The specimens were left in
the mould overnight before demoulding. Demoulding of the OPC concrete
specimens was done on the following day. The cube and cylinder specimens
were kept in the water pond for curing. Because of the space constraint of the
water pond, large sized beam specimens were cured by covering with jute
gunny bags and cured by spraying water. This is shown in Figure 4.19. The
dampness of the jute bags was ensured throughout the 28 days curing period.
On the 28th day, the elements were removed from the water pond and placed
in an open area to get air cured until the day of the test.
70
4.17
Figure 4.20
Figure 4.21
71