32

CHAPTER 4
MATERIALS AND PRILIMINARY LABORATORY
INVESTIGATIONS

4.0 INTRODUCTION
In this chapter the physical and chemical properties of Ingredients of biomass ash
geopolymer concrete are investigated and presented in detail.
4.1 PRELIMINARY TESTS: Preliminary tests are conducted on the various
ingredients with following objectives.
1. To know the physical properties of Aggregates (Coarse aggregate and Fine
aggregate).
2. To know the physical and chemical properties of Alkaline Activators (Sodium
Hydroxide NaOH and Sodium Silicate Na2SiO3).
3. To know the physical and chemical properties of Super plasticizer.
4. To know the physical properties of the three different biomass ashes (Sugarcane
Bagasse Ash, Groundnut shell ash and cattle dung ash).
5. To obtain the chemical composition of three different biomass ashes (Sugarcane
Bagasse Ash, Groundnut shell ash and cattle dung ash).
6.To study the chemical composition of three different biomass ashes (Sugarcane
Bagasse Ash, Groundnut shell ash and cattle dung ash) by comparing the chemical
composition of ordinary Portland Cement and Low calcium fly-ash ( ASTM Class -
F).
7. To know the physical and chemical properties of the fly ash used in this research
work.
4.2 FUNDAMENTAL LABORATORY INVESTIGATIONS
4.2.1 Aggregates
4.2.1.1. Coarse Aggregate
The coarse aggregate used in Geopolymer and OPC concrete was typically spherical
in shape, properly graded, and had a smaller maximum size than the coarse aggregate
used in conventional concrete [33]. The coarse aggregate utilized ranged in size from
10mm to 20mm. Graded aggregate is especially crucial for casting concrete in
severely congested reinforcement or small-diameter formwork [34]. In this study,
 33

crushed granite metal with diameters ranging from 20 mm to 10 mm was procured

from locally available quarries. IS 383-1970 [Methods of physical tests for hydraulic
cement] was used to test them. Table 4.1 lists physical parameters such as specific
gravity, bulk density, flakiness index, elongation index, and fineness modulus [35].
Table 4.1 Physical properties of Coarse aggregate
S.No. Property Method Coarse
Aggregate
1 Specific Gravity Pycnometer IS:2386 Part 3-1986 2.68
(Sg)
2 Flakiness Index (IS:2386 Part 2-1963) 6.65%
3 Elongation Index (IS:2386 Part 2-1963) 6.6
4 Bulk Density Loose IS:2386 Part 3-1986 1705kg/m3
Compacted
5 Fineness Modulus Sieve Analysis (IS:2386 Part 2- 7.32
1963)
4.2.1.2. Fine Aggregate
The fine aggregate used was local river sand free from organic impurities and
conforming to IS: 383–1970 [36]. The fine aggregate was tested for its physical
requirements such as density, fineness modulus and bulk density in accordance with
IS: 2386 - 1963 and the results were shown in Table 4.2.
Table 4.2 Physical properties of Fine aggregate
S.No. Property Method Fine Aggregate
1 Specific Gravity Pycnometer IS:2386 Part 3- 2.58
(Sg) 1986
2 Bulk Density Loose IS:2386 Part 3-1986 1586kg/m3
Compacted
3 Bulking IS:2386 Part 3-1986 6%
4 Fineness Modulus Sieve Analysis (IS:2386 Part 2.2%
2-1963)
 34

4.2.2. Alkaline Activators

4.2.2.1 Sodium Hydroxide (NaOH)
Sodium hydroxides are commonly accessible as pellets or flakes in the solid state. The
price of sodium hydroxide is mostly determined by the purity of the product [37]. In
this investigation, sodium hydroxide is used to activate a homogeneous substance
called Geopolymer concrete [38]. As a result, sodium hydroxide is recommended for
its cost-effectiveness and purity. The sodium hydroxide pellets were utilized in this
study, and their physical and chemical parameters are reported in Tables 4.3 and 4.4
by the manufacturer.
Table 4.3 Physical Properties of (NaOH)
Description Property

Appearance White
Molar mass soli 40 gr/mol
Density 2.1gr/cc
Boiling point 13900C
Melting point 3180C
Amount of heat liberated when dissolved in 266 cal/gr
water

Table 4.4 Chemical Properties of (NaOH)

S.No. Specification Percentage
1 Carbonate (Na2CO3) 2.0%
2 Chloride (Cl) 0.01%
3 Sulphate (SO4) 0.01%
4 Silicate (SiO2) 0.02%
5 Phosphate (PO4) 0.001%
6 Arsenic(As) 0.0001%
7 Iron(Fe) 0.005%
8 Lead (Pb) 0.001%
9 Zinc(Zn) 0.02%
 35

4.2.2.2 Sodium Silicate solution (Na2SiO3)

Sodium silicate is also known as water glass or liquid glass, and it comes in a liquid
gel form [27]. Table 4.5 shows the physical and chemical parameters of the silicates
were provided by the manufacturer. Na2SiO3 resolution is commercially available in a
variety of grades, but it should be noted that powdered water glass performs worse
than liquid water glass [28]. Salt resolution with a SiO2 to Na2O magnitude relation
(by mass) of 2.0 combined with 8–18 M matter twenty four hours before use [29] is
recommended for optimal outcomes.
Table 4.5 Physical and Chemical Properties of Sodium Silicate
S.No. Chemical compound Percentage
1 Na2O 10%
2 H2O 62%
3 SiO2 28%
4 Appearance Liquid (Gel)
5 Color Light yellow
6 Boiling Point 1020 C for 30% aqueous
solution
7 Molecular Weight 183.03 g
8 Specific Gravity 1.39

4.2.3. Super plasticizer

Super plasticizers are a type of water-reducing additive that is used to improve the
workability of concrete at lower water-cement ratios without sacrificing compressive
strength [30]. These admixtures reduce the body of the paste by generating a thin
layer over the cement particles after they disperse in cement agglomerates. Water-
reducing admixture Conplast SP 430 according to IS 9103: 1999 was utilised in the
gift work [31]. M/s Fosroc Chemicals manufactured Conplast SP 430, a sulphonated
hydrocarbon-based mainly gas (SNF) super softener. Table 6 lists the features of the
super softener utilized.
 36

Table 4.6 Properties of Super plasticizer

S.No. Specification Description
1 Form / state Liquid (sulphonated naphthalene based
formaldehyde)
2 Color Brown
3 Specific gravity 1.220 at 30°C
4 Chloride content Nil
5 Air entrainment 1%
6 Dosage The rate of addition is in the range of 1-2.5% by
weight of binder content.

4.2.4 Biomass Ashes:

4.2.4.1 Sugarcane Bagasse Ash:
BAGASSE is a cellulose fiber that remains after the sugarcane juice has been
extracted. In tropical countries, biomass is a substantial source of energy [55].
Bagasse ash is a biomass source and a substantial byproduct in sugar processing
plants, which frequently use bagasse as a primary fuel source to meet all of the
furnace's energy requirements [71]. The ash is produced by using bagasse as an
energy source, which is considered a waste that has a difficult time being disposed of
[56]. The silica content of bagasse ash varies depending on the kind of soil and
collection [56], as well as the amount of time and temperature that the bagasse is
exposed to. The ash produced by the consumption of sugarcane bagasse is
approximately 7 to 8% of the total bagasse consumed [57]. The CO2 emissions from
bagasse are equal to the amount of CO2 ingested from the atmosphere by sugarcane
throughout its development, making the co-age ozone-harming chemical neutral [57].
The broad miniature scientific examination of sugarcane bagasse ash (SBA) provides
either actual technique, mechanical strategy, compound technique, or a combination
of these strategies to frame able size, shape, nature of molecule surface, surface space
of molecule, and so on of pozzolanic mineral, which is directly helpful for upgrading
the pozzolanic movement of sugarcane bagasse ash (SBA), with the goal of it being
used as a valuable cementitious material in concreting [70]. The cristobalite type of
silica, which is responsive and successfully consolidates with calcium and water to
 37

form calcium silicate hydrate, which will directly add to the cement strength sections
[56].
Biomass power plants, advancements, and sugarcane ventures should take use of the
specialized, business, and effective benefits of combining sugarcane bagasse ash
(SBA) in biomass ash based geopolymer cement [69]. Calcium silicate hydrates (C-S-
H) gel is the principle by which objects are shaped by the reaction of calcium
hydroxide and sugarcane bagasse ash (SBA) [57].
According to Singh et al. [58], an enormous number of C-S-H was shaped in the glue
in the presence of SBA, and the compressive strength increased. The pozzolan feature
of the SBA is due to its high silica content; however the presence of unburned
material and carbon may reduce its reactivity [60]. SBA would be ordered as a
pozzolanic material [60], and its reactivity would be based primarily on the smallest
molecular size and fineness.
The creation of pozzolanic ash from SBA necessitates the use of ultrafine pounding to
transform this agro-squander pile into a raw material for the creation of biomass ash-
based geopolymer concrete. Previous analysts [61] accounted for the effects of
misfortune on start (L.O.I.) and fineness of SBA on the energy of the pozzolanic
response and compressive strength on midway substitution of concrete in concrete
cement. Figure 4.1 displays a photo of sugar stick bagasse ash that has been kept for
drying and is used to assemble biomass ash geopolymer concrete after sieving.

Fig.4.1 Sugar Cane Bagasse Ash

The sugarcane bagasse ash sample was collected from Sugar factory, near Chithoor,
Chithoor district, Andhra Pradesh, India. Samples were collected while the cleaning
process of the boilers in the factory. In the factory, the sugarcane bagasse is burnt at a
temperature varying from 2000C to 5000C. Samples were collected during the
maintenance work factory. In the factory, basing on the moisture content and feed of
 38

the bagasse, the sugarcane bagasse is burnt at a temperature varying from 200 0 C to
0 C
500 . The sugarcane bagasse ash thus obtained is used for making geopolymer
concrete.
Table 4.7 Type of Biomass used for the study
Material Source
Sugar Cane Bagasse Ash Sugar factory - near Chithoor, Chithoor
district, Andhra Pradesh, India.

Table 4.8 Physical characteristics

Specific Gravity Mean particle size D60(µm)
2.36 48.0

Table 4.9 XRF Chemical analysis

S.No. Compound Percentage %
1 SiO2 42.62
2 Al2O3 5.51
3 Fe2O3 3.78
4 CaO 14.12
5 MgO 2.35
6 Na2O 0.75
7 K2O 2.01
8 LOI 8.43

4.2.4.2 Groundnut Shell Ash

The composition percentage of the chemical compounds in the GNSA is compared to
that of typical ordinary Portland cement (OPC) and to that of Low calcium fly-ash
(ASTM Class -F) (LCFA) [62]. The investigations show that GNSA consists most of
the chemical compounds prone to have binding characteristics required for concrete
work [63]. The composition percentage of CaO found in the GNSA was found to be
less than that in the OPC [64]. The complete level of iron oxide (Fe2O3),silicon
dioxide (SiO2) and aluminum oxide (Al2O3) is seen as not exactly the base of 70%
 39

determined for pozzolans by ASTM C618 (American Society for Testing and
Material) [65].
The ash produced by burning Ground Nut Shells is assumed to be pozzolanas since it
has chemical constituent of certain elements found in good pozzolanas and ordinary
Portland cement (OPC) [66]. The Ground Nut Shell Ash (GNSA) used in this work is
well grained into fine particles. The ash obtained by heating groundnut shells in a
furnace for 4.5 hours at 2000c to 4000c [68]. The Ground Nut Shell Ash thus obtained
is used for making geopolymer concrete.
Table 4.10 Type of Biomass used for the study
Material Source
Groundnut Shell Ash Local rice kilns in Kurnool district, Andhrapradesh state
,India

Table 4.11 Physical characteristics

Specific Gravity Mean particle size D60(µm)
2.76 49.0
Table 4.12 XRF Chemical analysis
S.No. Compound Percentage %
1 SiO2 36.04
2 Al2O3 6.23
3 Fe2O3 1.88
4 TiO2 8.53
5 P2O5 6.51
6 CaO 8.95
7 MgO 15.64
8 Na2O 4.3

Figure 4.2 shows the image of Ground Nut Shell ash kept for drying and which is
used for manufacturing of biomass ash geopolymer concrete after sieving is
completed.
 40

Fig.4.2 Ground Nut Shell Ash

4.2.4.3 Cattle Dung cake Ash

The ash produced by burning Cattle Dung cake is assumed to be pozzolanas since it
has chemical constituent of certain elements found in good pozzolanas and ordinary
Portland cement (OPC) [80]. The Cattle Dung cake ash used in this work is well
grained into fine particles [72]. The ash obtained by heating Cattle Dung cake in a
furnace for 4 hours at 2000c to 4000c. The Cattle Dung cake Ash thus obtained is used
for making geopolymer concrete [81].
Materials, for example, Cattle Dung cake Ash, Cattle manure powder, Fly Ash, Slag,
and Silica Fume, can be utilized as halfway substitution for cementing material [82].
In any event, the accumulation of mismanaged waste, particularly in developing
countries, has exacerbated the environmental problem [73]. However, since the use of
environmentally friendly, light weight construction materials has grown in popularity
in the construction industry, it has become necessary to investigate how this might be
accomplished while still meeting the materials requirements stipulated in the
standards [74].
When combined in solid constructions, cattle dung cake ash functions as a typical
inhibitor for microorganisms, acting as a creepy crawly repellant and also preventing
the entrance of brilliant radiation [83]. It possesses typical germicidal properties and
enhances degradation resistance. Houses that are covered in bovine waste mortar, for
example, are protected from atomic radiation [75]. Green solid constructions can help
to mitigate the detrimental effects of the bond market [84]. As a result, we should try
to reduce the quantity of bond used in construction, and concrete can be replaced with
valuable cementitious materials [85].
 41

Table 4.13 Type of Biomass used for the study

Material Source
Cattle Dung cake Ash Milk processing boiler, Thadekenapalli village,
Kurnool district, Andhra Pradesh state, India.
Table 4.14 Physical characteristics
Specific Gravity Mean particle size D60(µm)
2.33 48.5
Table 4.15 XRF Chemical analysis
S.No. Compound Percentage %
1 SiO2 64.35
2 Al2O3 4.64
3 Fe2O3 5.53
4 TiO2 16.18
5 P2O5 3.07
6 CaO 1.21
7 MgO 5.07
8 Na2O 3.84

Figure 4.3 shows the image of Cattle Dung Cake Ash kept for drying and which is
used for manufacturing of biomass ash geopolymer concrete after sieving is
completed.

Fig.4.3 Cattle Dung Cake Ash

 42

4.2.5. Fly Ash

Fly ash is a fine powder that is recovered from the gases produced when coal is
burned to generate electricity [76]. Silica, alumina, and iron make up the majority of
these micron-sized earth elements. Because fly ash particles are virtually completely
spherical, they can flow and blend readily in mixes. Fly ash enhances the bonding
activity between aggregate and reinforcement and improves the performance of binder
paste [77]. The qualities of fly ash can vary significantly depending on a number of
factors, including the source coal's geographical origin, combustion conditions, and
sample location within the power plant. Si, Al, Fe, Ca, C, Mg, K, Na, S, Ti, P, and Mn
are the principal elemental elements of fly ash. Fly ash contains trace amounts of
nearly every naturally occurring element [42]. Particle surfaces are the primary source
of some trace elements such as As, Mo, Se, Cd, and Zn. Inorganic ions, such as Ca,
Na, Mg, K, Fe, S, and C, are the most prevalent species in fly ash extracts [43].
For more than half a century, fly ash has been regularly utilized as a partial
replacement for cement in concrete [44]. Saving cement and minimizing the heat of
hydration in mass concrete are two of the advantages [48]. Fly ash in concrete is cost-
effective and improves workability, strength, abrasion, heat evolution, shrinkage, and
reduces water additive demands in both fresh and hardened concrete [46].
Furthermore, the use of fly ash in concrete solves the storage and disposal problem of
fly ash, which is an industrial waste or by-product; otherwise, the fly ash must be
disposed of in landfills at a high expense. It inhibits autogenous and plastic shrinkage
cracking [47].
In this research work the fly ash is procured from Sri Rayaseema High Strength Hypo
Pvt limited, Kurnool District, and Andhra Pradesh, India. The class of the fly ash used
is F class fly ash. Tables 17 and 18 represent the physical and chemical analysis of fly
ash obtained from the basic laboratory investigations. The values shown in the tables
signify that the fly ash samples conform to IS 3812:1981 [100] codal provisions.
 43

Table 4.16 Type of Biomass used for the study

Material Source
F class Fly Sri Rayaseema High Strength Hypo Pvt limited, Kurnool District,
Ash Andhra Pradesh, India.

Table 4.17 Physical characteristics

Specific Gravity Mean particle size D60(µm)
2.5 47.6

Table 4.18 XRF Chemical analysis

S.No. Compound Percentage %
1 SiO2 36.02
2 Al2O3 16.58
3 Fe2O3 10.91
4 TiO2 14.75
5 P2O5 2.4
6 CaO 0.45
7 MgO 0.88
8 Na2O 0.17
Table19 shows that the Comparison among the chemical composition of Ordinary
Portland Cement (OPC), Low calcium fly-ash (ASTM Class -F), Sugar cane bagasse
ash, Groundnut shell ash and Cattle Dung Cake ash.

Table4.19 chemical composition of OPC, FA, SCBA, GNSA and CDCA

S.No. Compound Ordinary Low calcium Sugar Ground Nut Cattle
Portland fly-ash Cane Shell ash Dung
Cement (ASTM Bagasse (GNSA) % cake Ash
(OPC) % Class -F) ash (CDCA)
(FA) % (SCBA) % %
1 SiO2 17 to 25 36.02 42.62 36.04 64.35
2 Al2O3 3 to 8 16.58 5.51 6.23 4.64
3 Fe2O3 0.5 to 6 10.91 3.78 1.88 5.53
4 TiO2 6.4 to 8.6 14.75 14.12 8.53 16.18
5 P2O5 0.2 to 0.3 2.4 2.35 6.51 3.07
6 CaO 60 to 67 0.45 0.75 8.95 1.21
7 MgO 0.1 to 4 0.88 2.01 15.64 5.07
8 Na2O 0.2 to 1.3 0.17 8.43 4.3 3.84
 44

4.3 Making of Biomass ash Based Geopolymer concrete

4.3.1 Making of Alkaline Liquids
Sodium Hydroxide
Sodium Hydroxide pellets (NaOH) taken and dissolved in water at the concentration
of 8, 10,12,14,16 and 18 molar concentrations [49]. Davidovits (2002) has urged that
the preparation of hydroxide resolution should be done twenty four hours before use
and conjointly if it exceeds thirty six hours it terminates to semi- solid liquid state. So
the ready resolution ought to be used among this point.
Molarity Calculation for Sodium Hydroxide solution
The Sodium Hydroxide pellets must be dissolved in water to make a solution with the
required concentration [50]. The concentration of Sodium hydroxide solution can vary
in different Molar. The mass of Sodium Hydroxide pellets in a solution varies
depending on the concentration of the solution. For example, Sodium Hydroxide
(NaOH) solution with a concentration of 8 Molar consists of 320 grams of Sodium
Hydroxide (NaOH) pellets per liter of water, where 40 is the molecular weight of
NaOH.
Mixing procedure of all ingredients of biomass ash geopolymer concrete
Davidovits also recommended that the preference of a mixture of sodium silicate
solution and sodium hydroxide solution together at least one day before adding the
liquid to the solid constituents. The biomass ash and the aggregates are first dry mixed
together in a mixing pan for about 3 to 5 minutes manually as shown in Figure 5.1 and
5.2. After the dry mix is made, the alkaline solution which is prepared 24 hrs before is
thoroughly mixed with the dry mix for another 3 to 5 minutes to make fresh biomass
ash geopolymer concrete [52]. The fresh biomass ash geopolymer concrete was filled
in the mould. The specimens were compacted with three – layer filling and tamping
using a stainless steel tamping rod [53]. This was followed by an additional vibration
of 10 seconds using a vibrating table. Specimens such as cubes, cylinders and beams
were cast and tested. After casting the concrete mix was allowed to settle down in the
moulds for 30 minutes [54].
Figure 4.4 shows the image of all ingredients used in manufacturing of biomass ash
based geopolymer concrete.
 45

Fig.4.4 Ingredients of biomass based geopolymer concrete

Figure 4.5 shows the image of initial process of mixing of all ingredients in
manufacturing of biomass ash based geopolymer concrete.

Fig.4.5 Initial mixing process of ingredients

Figure 4.6 shows the image of measuring NaOH pallets in order to prepare the sodium
hydroxide solution 24 hours before the making of biomass ash based geopolymer
concrete.

Fig.4.6 weighing of NaOH pallets

Figure 4.7 shows the image of dry mixing of coarse aggregate, fine aggregate and
sugar cane bagasse ash for making biomass ash based geopolymer concretes.
 46

Fig.4.7 dry mix of biomass based geopolymer concrete

Figure 4.8 shows the images of label of sodium hydroxide pallets (NaOH) with
specifications given by manufacturer which is used in the production of biomass ash
based geopolymer concrete. Figure 4.9 shows the images of sodium silicate solution
(Na2SiO3) with specifications given by manufacturer.
Figure 4.10 and 4.11 shows the images of total chemicals utilized in this experimental
work.

Fig.4.10 & Fig.4.11 Na2SiO3 solution

 47

Fig.4.11 NaOH pallets

4.4 SUMMARY:
This chapter provides the basic composition and properties of all the ingredients used
in the experimental work; also this chapter gave the making process of the solutions
utilized in the work. In this module the comparison statement of all three biomass
ashes, fly ash and Ordinary Portland cement was presented.