CHAPTER I

THE PROBLEM AND ITS BACKGROUND

Introduction

Cementing is one of the vital processes in well completion in the oil and

gas industry. Drilling cement additives are mixed with the Portland cement to meet

the specifications required to meet the borehole conditions.

Increasing consumption and cost of Portland cement is one of the most

common problems encountered in well cementing operations. A partial

replacement for the Portland cement was considered and found that eggshells in

powder form can replace Portland cement as much as 10% of its original volume

to reduce consumption and cost.

Retarder additives are utilized to increase the set time, or setting time, of

cement slurries and also to increase pump time. Setting Time of the cement is

one of the most vital characteristics when utilizing cement in well operations.

Through the use of retarders as an additive it can control the time when a slurry

will set hard, keeping slurry viscous and pump-able in expected wellbore

temperatures and for the amount of time required to place the slurry. Retarders

decrease the rate of cement hydration, acting in a manner opposite to that of

accelerators.

Due to the expensive cost of retarder additives in the market it is best to

determine an alternative source of retarder additives. This is because of economic

reasons and to search for better efficiency in terms of lost circulation. Utilization of

1
rice husk, sawdust, and sugarcane bagasse with lightweight cement material can

reduce the slurry density, which is makes it easier to pump in the wellbore.

Different raw materials from various sources have already been utilized and

compared to standard additives used in real time drilling, such as agricultural

wastes that are pulverized and calcinated like powedered eggshells, sawdust ash,

rice husk ash, and sugarcane ash. This is done to develop alternatives for additives

and enhance the properties of drilling cement. Their ash concentration would

greatly affect the produced results. Different raw materials may or may not have

the same properties thus it is ideal to evaluate these alternatives in different ratios.

Partial replacement for a specific amount of additive from agricultural

wastes for cement will greatly reduce economic cost and also help solve solid

waste management. Solid waste management is vital to maintain a healthy

environment and people, and to also reduce waste generated on a yearly basis.

Organic waste is one of the main problems of the economy because it takes time

before it can fully dissolve itself when in fact in can be still of use, especially in the

cementing industry as an alternative additive.

The researchers have evaluated the agricultural wastes as potential

retarder additives using sawdust ash, sugarcane bagasse ash, and rice husk ash.

Evaluation will be in terms of setting time and economic cost in drilling cement with

additives for well cementing.

2
Objectives of the Study

The main thrust of this study is to evaluate agricultural wastes as drilling

cement additive.

Specifically, the study will aim to response the following:

1. Prepare the raw materials for mixture considering the proportion of:

1.1 Portland cement, eggshells, and rice husk ash

1.2 Portland cement, eggshells, and sugarcane bagasse ash

1.3 Portland cement, eggshells, and different combinations of rice husk ash,

sugarcane bagasse ash, sawdust ash.

2. Conduct preliminary testing to determine the operating conditions of the

designed mixer in terms of:

2.1 Operating Capacity

2.2 Mixing Speed using Froude’s Equation

2.3 Best Proportion of Retarders

3. Evaluate the properties of the product cement and compare to ASTM standards

in terms of the:

3.1 Autoclave Expansion

3.2 Setting Time

3.3 Compressive Strength

3.4 Fineness

3
4. Present a mathematical model of setting time as a function of ash

concentration.

5. Provide an experimental manual for the preparation of cement using

agricultural wastes as retarder.

Significance of the Study

The utilization of powdered eggshells, sugarcane ash, sawdust ash, and

rice husk ash will lessen the waste produced and help reinforce cement in well

completions. These additives from agricultural waste will serve as retardants to

change the setting time of the cement slurries while also strengthening the cement.

The study may be beneficial to the following:

The Oil and Gas Industry, evaluation of the blended-cement with agricultural

waste ash will be of significant value to be cost-effective in the industry while

enhancing the properties, characteristics, and efficiency of well cementing.

For the Philippine Government Agencies such as Philippine National Oil

Company (PNOC), this will be a supplementary to their research on industrial

advancement.

The Department of Energy and the Philippine National Oil Company, a

supplementary research for the advancement of the oil and gas sector in this

country.

4
 The agricultural sectors, this study will make them aware of the applications

of powdered eggshells, sugarcane ash, sawdust ash, and rice husk ash in the

industry.

The local farmers, this will be an additional knowledge for the application of

powdered eggshells, sugarcane ash, sawdust ash, and rice husk ash in the

cementing industry.

For the Petroleum Engineering Department, the study will help in improving

the department’s aim for quality education specifically in making and developing

studies about the alternative drilling cement additives or retarders in relation with

the oil and gas industry.

For the researchers, the study will deepen and increase their skills and

knowledge in understanding the concepts and principles that are used in the study

which may be applied in their future career.

And to the future researchers, the study will serve as a useful reference and

guide in developing and conducting related studies for further advancements.

Scope and Delimitations of the Study

The study covered the evaluation of the effectiveness of powedered

eggshells, sugarcane ash, sawdust ash, and rice husk ash as drilling cement

additive with Portland cement at specified ratio and proportions: 10% and 20% for

the eggshells; 50%, 60%, 70%, and 80% for the Portland cement; and 10%, 20%,

and 30% for the agricultural wastes. The two existing studies from Goce, et al.,

(2018) entitle “Evaluation of Rice Husk as Drilling Cement Additive” and Pumatong,

5
et al., (2015) entitle “Development of Pulverizing and Mixing Machine for Drilling

Cement Additives” was the basis for this evaluation and produced results was

utilized in making a mathematical model of the experimental values obtained.

Mixing speed was determined by using the Froude’s Equation and mixing

time has been set to 10 minutes according to the powder mixing handbook (Perry’s

8th Edition, 2008).

The properties tested were Autoclave Expansion, Setting time,

Compressive Strength and Fineness. These properties undergo laboratory test to

indicate the best proportion of the Portland cement, eggshell, sugarcane bagasse

ash, rice hush ash and sawdust by comparing to ASTM Standards. The

proportions of the rice husk ash with eggshell and Portland cement were 80:10:10,

70:10:20, 60:10:30, 70:20:10, 60:20:20 and 50:20:30. In addition, the proportions

of sugarcane bagasse ash with eggshell and Portland cement were 80:10:10,

70:10:20, 60:10:30, 70:20:10, 60:20:20 and 50:20:30.

The study also only covered dry mixing of specified Portland cement Type

1, powder eggshells, and the ashes from agricultural wastes that will serve as the

alternative to chemicals used as a retarder in cement. It did not utilize water in the

mixing process.

However, the study did not cover the testing of drilling cement on actual well

completion.

6
Conceptual Framework

The paradigm below illustrates the flow system of the research that includes

the conceive, design, implement, and operate that were arranged systematically

to direct the course of the study.

In the development of a mixer and the evaluation of agricultural wastes as

retarder cement additives, the researchers considered the proper selection of

appropriate materials that was used in the system. Likewise, simple and

economical design was take into consideration, low material cost and maintenance

cost, the availability of materials, and the assurance of higher efficiency of the

machine.

In order to achieve the objectives of the study, a research paradigm was

developed and presented in Figure 1. Based on the figure, stages that followed

were conceive, design, implement, and operate. Under the conceive stage was the

knowledge requirement. It consisted of knowledge about well cementing, Froude’s

Equation, Properties of Portland Cement, ASTM Standard on Cement, Cement

Additive properties of the ashes.

The design stage included the design layout, system components, and

material specification of the pulverizing and mixing machine. The pulverizing and

mixing machine was designed using Sketchup.

The implementation covered the fabrication of the machine, preliminary

testing, and the evaluation of specified properties. Preliminary testing established

the operating capacity, mixing speed, and best proportion. The evaluation of the

7
properties of the raw materials with the Portland Cement was also included in this

stage. Properties evaluated were autoclave expansion, compressive strength,

setting time, and fineness.

Operation stage included the development of the mixer for best alternative

retarder cement additive and analysis of the best proportion of sawdust ash, rice

husk ash, sugarcane bagasse ash, and powdered eggshells as drilling cement

additive to Portland cement. Presentation of mathematical model of the results

were also included in this stage. Lastly, the operation stage included the operation

and maintenance manual of the prototype.

A better view of the research paradigm was shown in Figure 1.

8
9
Definition of Terms

The following terms are defined operationally and conceptually for the better

understanding of the study.

Agricultural Wastes. Wastes produced as a result of various agricultural

operations. To be specific, sugarcane bagasse, sawdust, rice husks, and eggshells

(Environmental Case Study, 2017).

ASTM International. American Society for Testing and Materials (ASTM,

2001).

Autoclave Expansion. This provides an index of potential delayed

expansion caused by the hydration of CaO or MgO or both (Continental cement

Company, n.d.).

Cementing. Performed when the cement slurry is deployed into the well via

pumps, displacing the drilling fluids still located within the well, and replacing them

with cement (Rigzone, n.d.).

Cement Additives. Chemicals and materials added to a cement slurry to

modify the characteristics of the slurry or set cement (Schlumberger Oilfield

Glossary, 2014).

Compressive Strength. Is the maximum compressive stress that, under a

gradually applied load, a given solid material can sustain without fracture

(Corrosionpedia).

10
 Egg shell. In this study, it is the raw material to be pulverized and will be

added to Portland cement.

Lignosulfonate. In this study, it is one of the chemical properties that affect

the setting time.

Loss on Ignition. This is used to determine the organic matter content

(%OM) of a soil sample (Robertson, 2011).

Portland Cement. It is the basic ingredient of concrete. Abbreviated as

OPC in this study (Portland Cement Association US, 1916).

Retarder. In this study, it is the classification of the cement additive, which

delays the time of setting.

Rice Husk. In this study, it is the raw material use. The coating on a grain

of rice. It is formed from lignin and silica and hard materials to protect the seed

throughout the growing season. Abbreviated as RHA in its ash form in this study.

Sawdust. In this study, it is the raw material use. It is a by-product or

waste product of wood working operations such as sawing, milling, planning,

routing, drilling and sanding. Abbreviated as SDA in its ash form in this study.

Setting Time. In this study, it is the time before or required for the cement

slurry to harden and turn into concrete.

Slurry. It is a mixture of suspended solids and liquids (Schlumberger Oilfield

Glossary, 2014).

11
 Sugarcane Bagasse. It is the by-product of sugarcane stalks milled for

juice extraction (Feedpedia and Preston, 1995).

Sulfur Trioxide. In this study, it is one of the chemical properties that

affect the setting time of the cement (Schlumberger Oilfield Glossary, 2014).

12
 CHAPTER II

REVIEW OF RELATED LITERATURE

This chapter presents the conceptual literature, research literature and

synthesis which guided the researchers in the completion of the study.

Conceptual Literature

This segment presents the key concepts that explain the different principles

that serve as a guide for the study.

I. Well Cementing

Cementing the casing and liner strings in place in oil and gas wells

is integral to wellbore architecture, which in turn is integral to well

performance and total hydrocarbon recovery. Conventionally, cementing is

viewed as a one-time event, yet it serves as a foundation for ultimate

recovery if engineered to withstand pressure and temperature differentials

during life of the well events such as completion operations, fracture

stimulation, and production cycles. In other words, rather than simply being

the last step during drilling operations, it is economically more beneficial to

view cementing as the first step in completion operations. The cement

sheath can be subject to thousands of psi (pounds per square inch)

pressure changes and hundreds of degrees of temperature changes

throughout the life of the well. In spite of such dynamic fluctuations, the

cement sheath is expected to resiliently withstand immediate and

13
cumulative stresses, retaining seal integrity to securely isolate producing

zones and restrain unwanted fluid production.

(http://www.halliburton.com/en-US/ps/cementing/cementing-solutions/life-

of-the-well/default.page)

1.1 Well Parameters

Cement is designed to support the wellbore casing and isolate

zones to prevent each penetrated zones, and their formation fluids,

from interacting and contacting with each other, thus preventing case

buckling and contamination of freshwater zones, salt formations, and

drilling mud. In order to achieve these functions, well parameters

must first be determined to establish the necessary properties to

make the cement slurry in a specific zone or formation. These are:

1. Depth – Influenced by the volume of wellbore fluids, friction

pressures, hydrostatic pressures, temperatures, and

corrosive fluids that may hamper concrete lifespan.

2. Wellbore geometry – affects the amount of cement to be

used in the well caused by deviation angles and deformations,

rugosity and washouts.

3. Temperature – critical in designing the cement slurry as it

greatly affect, rheology, fluid loss, stability, and setting time.

Influenced by Bottomhole circulating temperature (BHCT),

14
 Bottomhole static temperature (BHST), and Temperature

Differential.

4. Formation pressures – creating wellbores disturbs the

natural balance for pressures in the penetrated formations,

thus various pressure changes will occur. Influenced by pore

pressure, fracture pressure, and rock characteristics.

5. Formation characteristics – various formation composition

greatly affects how the cement should be made. Water

sensitive formations, high-pH fluids and flowing fluids should

be taken into consideration.

(Stiles and David, 2012)

2. Drilling Cement

The basic raw material for cementing operations is Portland cement.

It is characterized by a certain percentage of clinker, which is obtained by

the appropriate selection of raw materials: limestone (or chalk) - providing

calcium oxide and clay particles (clay, shale) - introducing into the

composition of silica and alumina. Sometimes a marguer is also used as a

rock constituting a mixture of limestone and clay materials. The

technological process of cement production is quite complicated, which is

related to the high requirements of its properties (proper grinding, specific

surface area, etc.). Portland cement must comply with certain chemical and

physical standards, depending on their purpose. The principal

distinguishing feature of Portland cement in terms of chemistry is the

15
relative distribution of the main clinker phases, called the phase

composition.

Composition of Drilling Cement

2.1 Portland Cement

Portland cement also called "pure", because it contains no

mineral additives, consists entirely of Portland clinker; it is practically

inaccessible on the Polish market, manufacturers are inclined

towards mixed Portland cement. It is a hydraulic cement that, when

combined with water, hardens into a solid mass. Interspersed in an

aggregate matrix it forms PCC. As a material, Portland cement has

been used for well over 175 years and, form an empirical

perspective, its behavior is well-understood. Chemically, however,

Portland cement is a compel substance whose mechanism and

interactions have yet to be fully defined.

16
 Table 1
Chemical Composition of Portland Cement

Component Formula Trade Amount Function

name %
Tricalcium 3CaO.Si C3S 50% Fastest hydration
silicate O2 Overall and early
strength Protect
sulphate attack
Dicalcium 2Cao.Al2 C2S 25% Fastest hydration
Silicate O3 Overall and early
strength Protect
sulphate attack
Tricalcium 3CaO.Al2 C3A 10% Initial set and early
Aluminate O3 strength
Tetra calcium Initial set and early
Aluminum strength
Ferrite 4Cao.Al2 C4AF 10% Low heat of hydration
O3.Fe2O3
Other oxides 5%
such as gypsum,
sulphate
magnesia, free
lime

17
 (Source: Portland Cement, n.d.)

Table 1 shows the chemical composition of Portland cement which

Tricalcium Silicate, Dicalcium Silicate,Tricalcium Aluminate, Tetra calcium

Aluminum, Ferrite and other gypsum with accordance with their formula,

trade name, amount in percent and function.

2.1.1 Physical Properties

1. Fineness

Fineness of cement means the particle size of cement. At

affects the hydration process of cement. That means it affects the

rate of the strength gain of cement.

2. Soundness

Cement has a trend to shrink when it is hardened. This is

called soundness of cement. Good soundness cement doesn’t shrink

after hardening.

3. Consistency

Consistency means the required water to produce plastic

cement paste for particular cement. Thus, one can know the water

cement-ratio for better workability of mix.

4. Setting Time

18
 As soon as water is mixed with Portland cement, hydration

process starts and it begins to set. Cement has two setting time,

initial-setting time and final-setting time. In construction, initial-setting

time shouldn’t be too early and final-setting time shouldn’t be too late.

Normally, initial-setting time is 30 to 45 minutes and final-setting time

is below 10 hours.

5. Compressive Strength

Cement has three types of strengths, compressive strength,

tensile strength and flexural strength. However, compressive

strength is taken into consideration, the rest can be ignored. For

knowing compressive strength of cement, only cement paste can’t

be tested. For this purpose, either cement-sand mortar cubes or

”cement-concrete cubes” are made. The testing result of cubes can

be affected by several things such as water-cement ratio, curing and

dampness of cubes during testing. Minimum compressive strength

result for 3 days mortar cube should be 16 N/mm2 and for 7 days

cube should be 22 N/mm2.

6. Specific Gravity

Specific Gravity of cement is necessary for calculating the

mass for desired volume of cement. The Specific Gravity of normal

type of cement is 3.15.

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2.1.2 ASTM Standard of Portland Cement

2.1.2.1Types of Portland Cement (ASTM C150)

1. Type I (Normal)

Also called Ordinary Portland Cement (OPC), Type I is

a general-purpose cement, which is adequate for most uses,

except those which require the special properties of other

types. It has an adequate strength and a low heat of hydration.

Type I cement is not suitable for uses where the concrete can

face chemical attacks, or excessive temperature during

curing. It can be used in applications like precast concrete

products, reinforced buildings, floors, bridges, reservoirs,

tanks, culverts, sewers, pavements, sidewalks, pipes, etc.

2. Type II (Moderate Sulfate Resistance)

Type II has the same uses as Type I, along with a

moderate resistance to sulfates. It generates only a moderate

heat of hydration, and at a lesser rate. It is ideal for

applications where the concrete comes into contact with soils

or groundwater having some amount of sulfate ions, though

not excessively high. It's low concentration of C3A, which is

lesser than 8%, imparts this resistance to sulfate attack. It is

common in parts of western USA and Canada which have

20
such sulfate-rich conditions. It is ideal for heavy structures like

abutments, piers, and retaining walls.

3. Type III (High Early Strength)

Type III cement is chemically almost identical to Type

I, though it has a lesser curing time, which means it hardens

faster. It is also ground finer, and contains a higher amount of

C3S, both of which promote the rapid setting of concrete. This

type imparts strength faster than Type I, typically in less than

a weeks’ time, though its final 28-day strength may be equal,

if not lesser. It is ideal for applications which require quick

setting, so that structures can become operational faster, and

where formwork needs to be removed and reused. It is also

ideal for cold areas, where the quick curing of concrete

prevents damage due to frost.

4. Type V (High Sulfate Resistance)

This is almost similar to Type II, except that it is even

more tolerant to the attack of sulfate ions. This is achieved by

reducing the C3A percentage even lower to 5%. So, it is

suitable for buried concrete structures, where the soil or

groundwater is rich in sulfate ions. However, it gains strength

at a slow rate as compared to Type I (OPC). Like Type II, it is

more common in the western United States and Canada. It is

21
used for applications like canal linings, retaining walls, and

culverts, which may be exposed to a sulfate attack.

5. Type Ia, IIa, IIIa

These types are almost identical to the basic I, II, and

III types, respectively, except that they contain small amounts

of air-entrainment admixtures which are blended with the

cement during its manufacture. These mixtures form small air

bubbles inside the concrete block when it sets, which is ideal

for cold temperatures, where freeze-thaw cycles can produce

cracks in the concrete. The smaller water-cement ratio also

increases the workability of the cement.

6. White Portland Cement

It is similar to Type I Portland cement, except that it is

white in color. This is achieved by reducing the percentage of

iron (C4AF) and magnesium oxide, which impart a gray color

to ordinary Portland cement. Since it requires additional care

in the choice of ingredients, and to produce white color, this

type is complex and expensive to manufacture. It is ideal for

applications like precast curtain walls, facing panels, stucco,

terrazzo surface, cement paint, and white/colored concrete

and mortar. While these are the most common types of

Portland cement, certain hybrids like I/II or II/V are also used.

22
 These hybrids meet the requirements of both types and can

be used for the applications of either one.

2.1.2.2 ASTM C94

Portland Cement Concrete may be mixed at a central mixing plant or

in transit mixers. All mixing equipment and operations shall conform to the

requirements of ASTM C-94 Page 6 Standard Construction Specifications

Division 30 – Portland Cement Concrete Revised 11/08 (AASHTO M-157).

All concrete shall be delivered to the work site thoroughly mixed to a uniform

color and show uniform distribution of aggregates and cement throughout

the mixture. Concrete shall be delivered to the Project site, discharged from

the truck completely and in the forms ready for vibration within one and one-

half (1-1/2) hours after introduction of the cement to the aggregates. At the

discretion of the Engineer, the above period may be extended one (1)

minute for every degree of temperature at which the concrete is delivered

below seventy degrees (70ᵒ) Fahrenheit to a maximum total time of two (2)

hours.

The use of non-agitating equipment for transporting concrete will not

be permitted. The mixing drums of transit-mix trucks shall be thoroughly

washed after discharging each load to prevent the accumulation of adherent

layers of concrete.

2.1.2.3 Autoclave Expansion (ASTM C151)

23
 Calculate the change in length of the test specimen by subtracting

the length comparator reading before autoclaving from that after

autoclaving, and report as percent of effective gage length to the nearest

0.01 %. Report the percentage of increase in length as the autoclave

expansion. Indicate a decrease in length by a minus sign prefixed to the

percent value.

2.1.2.4 Compressive Strength (ASTM C109)

This test method provides a means of determining the compressive

strength of hydraulic cement and other mortars and results may be used to

determine compliance with specifications. Further, this test method is

referenced by numerous other specifications and test methods. Caution

must be exercised in using the results of this test method to predict the

strength of concretes.

2.1.2.5 Time of Setting (ASTM C191)

Standard which defines procedure, minimum requirements for

testing equipment for determination of setting time according with Vicat

needle method, instructions related with sample preparation and the

calculations needed for reaching the appropriate results of VICAT test.

AUTOVICAT equipment is an automatic solution to perform in a

reliable, repetitive, accurate and easy way the VICAT test according to

ASTM C191 and EN 196-3.

24
3. Factors affecting the mixing of cement

1. Water Content

If the water-cement ratio is small, it indicates high amount

cement which is helpful for good strength. But the small water-

cement ratio is responsible for lower workability. If proper compaction

cannot be achieved, concrete will not be enough strong as desired.

2. Mix Proportions

Rich concrete mix (cement content is high) is more workable

because due to sufficient cement aggregates will have proper

lubrication for easy movement which means more workability.

3. Size of Aggregates

Finer particles require more water for a larger surface;

hence aggregate with finer particles need more water to make it

workable. Bigger particles give higher workability for fixed water

content. But maximum size of aggregate depends on some practical

considerations like handling-mixing and placing equipment, concrete

section, and spacing of reinforcement.

4. Shape of Aggregates

Irregular shape and rougher texture of angular aggregate

demand more water than the round shaped aggregate. For fixed

volume or weight, rounded or sub-rounded particles have less

25
surface area and less void and they have less friction resistance too.

Hence round shaped aggregates show higher workability than

angular, flaky or elongated aggregates.

5. Grading of Aggregates

Well-graded aggregates tend to fill up voids and easily get

workability. Less amount of water can make it workable. If grading is

better, there will be fewer voids and excess paste will be available to

give better lubricating effect. Due to excess paste, the mixture gets

cohesive and prevents segregation. It also makes it get compacted

easily i.e. increases the workability.

6. Surface Texture of Aggregates

Aggregates with smooth surfaces are more workable than

roughly textured aggregates. Roughly textured aggregates show

high friction and segregation tendency. Besides, non-absorbent

aggregates are more workable because porous and non-saturated

aggregates demand more water than aggregates which are non-

absorbent.

7. Use of Admixtures

There are some admixtures which can improve workability.

Some admixtures are mixed intentionally to increase workability and

some admixtures increase workability as a side effect of its main

purpose.

26
 8. Use of Additives

There are many supplementary materials used for improving

quality of fresh concrete. Some of these, like fly ash, improve

workability and some of these like steel or synthetic fibers decrease

workability.

9. Time

Mixing is a case where more is not necessarily better. There

is usually an optimal mix time, which must be determined

experimentally. By using Froude’s number which is a dimensionless

group equal to N2D/g, where N is rotational speed, D is a

characteristic dimension of the mixer such as diameter, and g is the

acceleration due to gravity, all in consistent units. The implication of

this approach is that as a mixer of the same geometric ratio, such as

length to diameter, gets larger the required rotational speed is

reduced to keep the Froude number constant. The resulting mix time

in a larger mixer might actually increase because the intention is to

keep the number of turnovers Nt, where t is the mix time, constant

(Valentas et al. 1991).

Rotation speed also matters and usually has an optimum

value. At too low a speed, there is inadequate agitation; but at low

speeds, avalanching flow can occur, which is efficient in mixing. At

27
 too high a speed, centrifugal force sends all the particles to the

perimeter. The Froude number is the relevant scaling parameter:

Fr = N2D/g

Where:

N is rotation speed, s–1

D is radius of cylinder, mg is acceleration of gravity, m/s2

Fr = 1 defines the beginning of centrifuging, so values

considerably less than 1 are needed for mixing

It is important to control mix times because excessive mixing

can promote segregation.

10. Temperature

High temperature reduces workability and increases slump

loss. Slump loss is less influenced by temperature in stiff mixes

because this type of mix is less affected by a change in water

content.

4. Cement Additives

Additives are available to mix with cement to improve cementation

efficiency and sealing efficiency of reservoir rocks. All possible additives for

cement or cement slurry are divided into the following:

1. Accelerators

28
 Accelerators speed up or shorten the reaction time required

for cement slurry to become a hardened mass. In the case of

oilfield cement slurries, this indicates a reduction in thickening time

and/or an increase in the rate of compressive-strength development

of the slurry.

2. Retarders

The commonly used cements in well applications are API

Class A, C, G, and H. These cements, as produced in accordance

with API Spec. 10A do not have a sufficiently long fluid life (thickening

time) for well applications above 38°C (100°F) Bottom Hole

Circulating Temperature (BHCT). To extend the thickening time

beyond that obtained with a neat (cement and water without additives

or minerals) API-class cement slurry, additives known as retarders

are required.

3. Extenders

In many parts of the world, severe lost circulation and weak

formations with low fracture gradients are common. These situations

require the use of low-density cement systems that reduce the

hydrostatic pressure of the fluid column during cement placement.

Consequently, lightweight additives (also known as extenders) are

used to reduce the weight of the slurry.

29
 4. Weighting Agents

Weighting agents or heavyweight additives are used to

increase slurry density for control of highly pressured wells.

5. Dispersants

Dispersant is known to be friction reducers that are used

extensively in cement slurries to improve the rheological properties

that relate to the flow behavior of the slurry.

6. Fluid loss control

Fluid-Loss-Control Additives (FLAs) are used to maintain a

consistent fluid volume within a cement slurry to ensure that the

slurry performance properties remain within an acceptable range.

7. Lost-Circulation Control Agents

Cement slurries can be lost to the formation and not circulated

back to the surface during completion of a wellbore. This is defined

as lost circulation. It should not be confused with the volume

decrease resulting from fluid-loss filtration.

8. Special Additives

There are number of additives that do not fit nearly into

functional groupings. Fibers are used for controlling lost circulation.

Special types of fibers also improve the impact resistance and tensile

strength of cement.

30
5. Properties and Materials used as Cement Additives

A. Wood

Figure 3 shows the appearance of wood. An organic material a

natural composite of cellulose fibers that is strong in tension and

embedded in a matrix of lignin that resist compression.

Figure 2. Wood
Source: (Nataliia K/Shutterstock, 2018)

All wood is composed of cellulose, lignin, hemicelluloses, and minor

amounts (5% to 10%) of extraneous materials contained in a cellular

structure. Variations in the characteristics and volume of these components

and differences in cellular structure make woods heavy or light, stiff or

flexible, and hard or soft. The properties of a single species are relatively

constant within limits; therefore, selection of wood by species alone may

sometimes be adequate. However, to use wood to its best advantage and

most effectively in engineering applications, specific characteristics or

physical properties must be considered.

31
 Composition of Wood

The main constituent of wood is cellulose, which accounts for up to

70 per cent by weight of dry wood substance. There are two types; one, the

alpha cellulose which is the constituent of major importance in the making

of paper. The main cementing action that bonds cells together and imparts

rigidity to the wood is provided by lignin, in amounts from 18 to 28 per cent.

There are, in addition, certain minerals present that can be recovered as

ash when wood is burned, in amounts up to 1 per cent. These three

constituents form the essential dry wood substance. Wood may contain, in

addition to substantial amounts of water, certain chemical compounds that

may be extracted from the wood by solvents of various kinds. These include

tannins, starch, oils, waxes and resins, which may contribute colour, taste

and odour as well as resistance to decay to the wood.

Table 2
Chemical and Physical Composition of Wood

Cellulose 40-50%
Lignin 18-25%
Hemicellulose 20-30%
Extractives 2-30%
Ash-forming minerals 2-30%
Moisture Content 5-15%
Typical size of wood dust/sawdust 6mm-10mm
(Source: B. Russell; AGB Technologies, Inc., Analysis of Stockpiled Wood
Residues, A report prepared for Saskatchewan forest center, 2003)

Table 2 show the chemical and physical composition of wood by

percentage mainly composed of cellulose, lignin, hemicellulose, extractives,

32
ash-forming minerals, moisture content and typical size of wood dust or

sawdust.

Wood Chemical Composition

A. Cellulose – Carbohydrate of long chain polymers organized

into microfibrils.

B. Lignin – Organic compound the binds the microfibrils

together in the secondary walls and middle lamella.

C. Hemicellulose – A cellulose-like material in the wood cell

wall that is easily decomposed by dilute acid to yield simple sugars

D. Extractives – Organic material deposited during heartwood

formation (gums, resins, oils, alkaloids)

Mahogany Wood

Figure 4 shows mahogany wood from the mahogany tree or

Swietenia Mahagoni which is a large tropical tree with a semievergreen

growth habit. Mahogany trees produce broad, spreading growth with foliage

that can span 50 feet in width and 75 feet in height at maturity. According

to Moreira (2015), the lignin content of Mahogany is nearly constant, around

25%, with localized regions presenting contents of 45% to 65% of lignin.

33
 Figure 3. Mahogany Wood
Source: (Bell Forrest, 2017)
B. Sawdust or wood dust

Figure 5 show the sawdust or wood dust is a by-product or waste

product of woodworking operations such as sawing, milling, planning,

routing, drilling and sanding. It is composed of fine particles of wood. These

operations can be performed by woodworking machinery, portable power

tools or by use of hand tools. Wood dust is also the by-product of certain

animals, birds and insects which live in wood, such as

the woodpecker and carpenter ant. In some manufacturing industries it can

be a significant fire hazard and source of occupational dust exposure.

Figure 4. Sawdust
Source: (Indiamart, 2015)

34
 Two waste products, dust and chips, form at the working surface

during woodworking operations such as sawing, milling and sanding. These

operations both shatter lignified wood cells and break out whole cells and

groups of cells. Shattering of wood cells creates dust, while breaking

out of whole groups of wood cells creates chips. The more cell-shattering

occurs, the finer the dust particles that are produced. For example, sawing

and milling are mixed cell shattering and chip forming processes, whereas

sanding is almost exclusively cell shattering.

C. Sawdust ash

Figure 6 illustrates a sawdust ash. The biomass is heated to within a

critical temperature band but with a restricted supply of air so that it does

not ignite. Various processes options are available including simple earth

kilns to more complex retorts that make use of the volatile compounds in

heating the process. (KMEE Engineering, 2016)

Figure 5. Sawdust Ash

Source: (Antileak Industrial, 2016)
According to Michael Thomas, Ph.D., sawdust ash can used as a

supplementary cementitious material (SCM) in the production of portland

35
cement concrete. A supplementary cementitious material, when used in

conjunction with portland cement, contributes to the properties of the

hardened concrete through hydraulic or pozzolanic activity, or both. As

such, SCM's include both pozzolans and hydraulic materials.

Table 3
Chemical Composition of Sawdust Ash

Chemical Components Weight Fraction (%)

SiO2 76.3%
Al2O3 5.8%
CaO 4.7%
Fe2O3 2.9%
SO3 1.6%
MgO 1.2%
Other Oxides 2.5%
Loss in ignition 3.9%
(Source: Stabilization of soft clayey soils with sawdust ashes, Karim,
research gate, 2018)

The table 3 shows the chemical composition of Saw Dust Ash which

contains silicon dioxide, ferrous oxide, calcium oxide, other oxides and etc

with their respective weight fraction percentage.

D. Rice Husk

Figure 7shows the rice husk which is the coating on a seed or grain

of rice. It is formed from hard materials, including silica and lignin, to protect

the seed during the growing season. Each kg of milled white rice results in

roughly 0.28 kg of rice husk as a by-product of rice production during milling.

36
 Figure 6. Rice Husk
Source: (NorthernBrewer,2018)

Around 20% of paddy weight is husk and rice production in Asia

produces about 770 millions of husk annually. In 2008 the world paddy

production was 661 million tons and consequently 132 millions of rice husk

were also produced. While there are some uses for rice just it is still often

considered a waste product in the rice mill and therefore often either burned

in the open or dump on wasteland. Husk has high calorific value and

therefore can be used as a renewable fuel. Rice husk is produced in the

first step in the milling process when the husk is removed from the grain in

the husking stage mill.

Characteristics of Rice Husk:

1. Rice husk is difficult to ignite and it does not burn easily with open

flame unless air is brown though the husk. It is highly resistant to

moisture penetration and fungal decomposition. Husk therefore

makes a good insulation material.

37
2. Rice husk gas high silica (SiO2) content which means that it

decomposes slowly when brought back to the field.

3. Handling of rice husk is difficult because it is bulky and dusty. Its

angle of repose is about 40-45C which means that its flow ability,

e.g. in feed hoppers is very poor.

4. Rice husk has low bulk density of only 70-110 kg/m3, 145 kg/m3

when vibrated or 180 kg/m3 in form of brackets or pellets. It thus

requires large volumes for storage and transport, which makes

transport over long distance un-economical.

5. Rice husk has a high average calorific value of a 3410 kcal/kg

and therefore is a good, renewable energy source.

6. Because of the high silica content rice husk is very abrasive and

wears conveying elects very quickly.

7. Rice husk is not an easy fuel. One concern in rice husk firing is

the behavior of the ash, i.e., its slagging and fouling tendency

caused by a low melting point of the rice husk ash.

Table 4
Chemical and Physical composition of Rice husk

Chemical and Physical composition of Rice husk

Cellulose 50%
Lignin 25-30%
Silica 15-20%
Carbon 39.8 – 41.1%

38
 Hydrogen 5.7 – 6.1%
Oxygen 0.5 – 0.6%
Nitrogen 37.4 – 36.6%
Moisture Content 8.68 – 10.44%
Typical Size (length) 7mm

(Source: ARPN Journal of Engineering and Applied Sciences2006-2015,

oriental journal of chemistry n.d., tandfonline, ricehuskfaq.com)

The table 4 illustrates the Chemical and Physical Composition of

Rice Husk that have cellulose with 50% content, lignin with 25-30%, silica

with 15-20%, carbon 39.8-41.1%, hydrogen with 5.7-6.1%, oxygen with 0.5-

0.6%, moisture content with 8.68-10.4% and typical size in length is 7mm.

These are good component for better cement additive.

E. Rice Husk Ash (RHA)

The figure 8 shows the appearance of rice husk. It is heated

and burnt within a critical temperature.

Figure 7. Rice Husk Ash

Source: (Indiamart, 2017)

RHA (Rice Husks Ash) produced after burning of Rice Husks has

high reactivity and pozzolanic property. Chemical compositions of RHA are

39
affected due to burning process and temperature. Silica content in the ash

increases with higher the burning temperature. The effect of partial

replacement of cement with different percentages of ground RHA on the

compressive strength and durability of concrete is examined.

Table 5
Physical Properties of Rice Husks Ash

PARTICULARS PROPERTIES

Color Gray
Particle size <45 micron
Specific gravity 2.3

(Source: S.D Nagrate et. al., 2012, page 1-2)

Table 5 shows the physical properties of Rice Husks Ash with color

of gray, <45 micron particle size and 2.3 specific gravity. The properties

identified the rice husks accordingly.

Table 6
Chemical Properties of RHA

Chemical Properties Constitutes (weight,%)

Fe2O3 0.54

K2O 0.1-2.54

SiO2 62.5-97.6

CaO 0.1-1.31

MgO 0.01-1.96

40
 Na2O 0.01-1.58

P2O5 0.01-2.69

SiO3 0.1-1.23

Carbon 2.71-6.42

(Source: S.D. Nagrale et. al., 2012, page 1-2)

Table 6 shows the composition of Rice husk ash with a range. It is

composed of ferrous oxide, potassium oxide, silicon dioxide, calcium oxide,

magnesium oxide, sodium oxide, phosphorus, silicate and carbon.

F. Sugarcane Bagasse

Figure 9 shows the appearance of sugarcane bagasse which is an

agricultural waste and constituted by cellulose, hemicellulose and lignin.

Figure 8. Sugarcane Bagasse

Source: (Indiamart, 2011)

These three components amount to more than 90% of the dry weight

of the fiber. The ash content is, in general, low. In turn, the non-fiber

compounds, commonly referred as extractives, may represent a significant

41
portion of the dry weight in the raw material. In the present study, samples

of raw bagasse were extracted with water, ethanol and water followed by

ethanol. Then, the extracted bagasses had their chemical compositions

determined by a series of analyses based on the methods proposed by

Browning (1967), with modifications. As can be seen in Table 1, the water

extraction removed 5.8% of extraneous materials from the bagasse fibers.

The ethanol extraction led to a similar content of extractives (5.6%). On the

other hand, the sequential extraction with both solvents reduced the dry

weight of the raw material in 9.4%, thus showing that these two solvents

dissolved structurally different compounds. This assumption was further

confirmed by the relative absorption spectra of the extracts.

Table 7
Chemical and Physical Composition of Sugarcane Bagasse

Chemical and Physical Composition of Sugarcane Bagasse

Cellulose 41.8%

Hemicellulose 28%

Lignin 21.8%

Carbon 45.5%

Hydrogen 5.6%

Oxygen 45.2%

Nitrogen 0.3 %

42
 Other elements like aluminum, calcium,
magnesium, sodium, and silicon
3.4%
Moisture Content 40-50%
Typical Size (length) 10mm – 30mm
(Source: H. Hajiha, M. Sain, 2015)

The chemical and physical composition of Sugarcane Bagasse

contains cellulose with 41.8% content, hemicellulose with 28%, lignin with

21.8%, carbon with 45.5%, hydrogen with 5.6%, oxygen with 45.2%,

nitrogen with 0.3% and other elements. This includes also the moisture

content with 40-50% and has typical size of 10mm-30mm.

G. Sugarcane Bagasse Ash

The figure 10 shows the appearance of a burnt sugarcane bagasse

within a critical temperature.

Figure 9. Sugarcane Bagasse Ash

Source: (Sciencedirect, 2016)

Bagasse is a by-product from sugar industries which is burnt to

generate power required for different activities in the factory. The

burning of bagasse leaves bagasse ash as a waste, which has a

43
 pozzolanic property that would potentially be used as a cement

replacement material. It has been known that the worldwide total

production of sugarcane is over 1500 million tons. Sugarcane consists

about 30% bagasse whereas the sugar recovered is about 10%, and the

bagasse leaves about 8% bagasse ash (this figure depend on the quality

and type of the boiler, modern boiler release lower amount of bagasse

ash) as a waste, this disposal of bagasse ash will be of serious concern.

Sugarcane bagasse ash has recently been tested in some parts of the

world for its use as a cement replacement material.

Table 8
Chemical Composition of Sugarcane Bagasse Ash (SCBA)

Chemical Components Weight fraction (%)

SiO2 78.34
Al2O3 8.55
Fe2O3 3.61
Cao 2.15
Na2O 0.12
K2O 3.46
MnO 0.13
TiO2 0.5
MgO 1.65
BaO <0.16
P2O5 1.07
Loss on ignition 0.42

(Source: Cordeiro et al., 2004)

44
 Table 8 shows the chemical composition of Sugarcane Bagasse Ash

that contains silicon dioxide (SiO2) with 78.34% weight fraction, aluminum

oxide with 8.55%, ferric oxide with 3.61%, calcium oxide with 2.15%, sodium

oxide with 0.12%, potassium oxide with 3.46%, manganese oxide with

1.65%, barium oxide with <0.16%, phosphorus pentoxide with 1.07% and

loss on ignition with 0.42%. These components made sugarcane bagasse

ash a good cement additive which is needed in this study.

Table 9
Physical Properties of Sugarcane Bagasse Ash (SCBA)

Properties Sugarcane Bagasse Ash

(SCBA)

Color gray-black

Specific gravity 2.20 - 2.40

Median particle size, d50(μm) <50 µm

Mass passing through 50- μm sieve (%) 8.4

Specific surface area (m2/kg) 308 – 514

Density (g/cm3) 2.16-2.52

Particle shape Spherical

(Source: modified Cordeiro et al., 2004; Madurwar et al., 2014; Tijore et al.,
2013; Sivakumar et al., 2014)

Table 9 illustrates the Physical Properties of Sugarcane Bagasse

Ash with color of gray-black, 2.20-2.40 specific gravity, 28.9-45 μm median

particle size, 8.4% mass passing through 45- μm sieve, 308-514 m2/kg

45
specific surface area, 2.16-2.52 g/cm3 density and spherical particle shape.

These properties of sugarcane bagasse ash showed that it qualifies as a

good cement additive based on the previous studies.

H. Eggshells

Figure 11 shows the appearance of eggshell which is the outer

covering of a hard-shelled egg and of some forms of eggs with soft outer

coats.

Figure 10. Eggshells

Source: (thebetterindia, 2018)

According to Thapon and Bourgeois, eggshell is approximately 11%

of the total weight of the egg and it presents contents of: calcium carbonate

(94%), calcium phosphate (1%), magnesium carbonate (1%) and organic

substances (4%). So, eggshell is a rich source of mineral salts, mainly

calcium carbonate.

Table 10
Chemical Composition of Eggshell

Content Amount (%)

Calcium Carbonate 94-97

46
 Magnesium 0.2
Phosphorus 0.3
Organic Matter 2
Sodium, Potassium, Iron, Copper, Less than 1%
Manganese

(Source: Compound chemistry, 2016)

Calcium carbonate or calcite is the number one mineral found in

limestone Table 10 shows the chemical composition of eggshell, with

calcium carbonate as the main component and this is the same chemical

which makes up limestone present in Portland cement.

Uses of Eggshell

1. Pest Control

Crush eggshells around vegetables and flowers to keep away

snails, slugs, and cutworms. These pests don’t like crawling over

the chalky sharpness of ground eggshells. Sprinkle the eggshell

on the stems of your plants to keep the destructive critters away.

2. Treat Skin Irritations

Relieve those skin irritations naturally by mixing crushed

eggshells with apple cider vinegar and dabbing it on your skin.

3. Eco-friendly Household Abrasive

Shake crushed eggshells and a little soapy water to scour

hard-to-clean items like thermoses and vases. Crushed eggshells

can also be used as a nontoxic abrasive on pots and pans.

47
 4. Compost for Naturally Fertilized Soil

Eggshells quickly decompose in the compost pile and add

valuable calcium and other minerals to the soil in the process.

Operating Principle of Mixer

1. Benford Concrete Mixer

Figure 12 shows a Benford Concrete Mixer The barrel of the machine is

made of high-quality stainless steel and stainless steel. It will not rust if it is

washed with water. With a drum capacity of 120L and a mix capacity of 102L,

it is easy to use and highly portable with two wheels.

Figure 11. Benford Concrete Mixer

Source: (bruceatfield, 2018)
2. Ratio and Proportion of Cement Additive
The reaction of cement additives with the cement and the

interaction between them is not well defined chemically. What is

actually known are the physical effects of these additives on the slurry

performance properties. Different proportion of additives have different

48
 effects on the properties of the cement therefore, the proportion of

additives with respect to amount of cement must be balanced based

on requirements.

RESEARCH LITERATURE

LOCAL STUDIES

This section presents previous studies relevant to the evaluation of

the drilling cement additive.

In the study “Application of sugarcane bagasse ash as a partial

cement replacement material” by Dinku, et al., (2012), test results indicated

that partial replacement of cement by using bagasse ash results in better or

similar concrete properties and further environmental and economic

advantages can also be exploited by using bagasse ash as a partial cement

replacement material.

In the study “Development of Pulverizing and Mixing Machine for

Drilling Cement Additives,” by Goce, et al., (2017), it was concluded that

partial replacement of up to 20% eggshell powder in cement mixture was

proven effective through several laboratory testing parameters.

In the study of Bagsit, et al., (215), entitled “Evaluation of Rice Husk

Ash as Drilling Cement Additive “, the raw material used was rice husk ash

mixed in different proportions with Portland cement. The results were

subjected to various tests to verify the affectivity of the additive. However,

49
in the present study, the researchers will be utilized pulverized eggshell as

partial replacement for Portland cement Type 1 and ground rice husk, saw

dust and sugarcane bagasse that will be carbonized to be ashes according

to the maximum temperature of each that will serve as retarders that

delayed the setting time of cement. The carbonizing temperature for rice

husk will be based on this study.

In the study “Study on Properties of Rice Husk Ash and Its Use as

Cement Replacement Material” by Habeeb, et al., (2010), it was concluded

that RHA concrete gave excellent improvement in strength for 10%

replacement (30.8% increment compared to the control mix), and up to 20%

of cement could be valuably replaced with RHA without adversely affecting

the strength. Increasing RHA fineness enhanced the strength of blended

concrete compared to coarser RHA and control OPC mixtures.

In the study “Influence of Sawdust Ash (SDA) as Admixture in

Cement Paste and Concrete” by Ayuba, et al., (2014), The addition of SDA

in cement decreased drying shrinkage but increased consistency, initial and

final setting times and could be used as a retarder. The addition of SDA in

concrete showed a decrease in slump, but increase in compressive

strength, with an optimum of 2% SDA.

According to Elinwa (2007) in the study, “Effect of addition of sawdust

ash to concrete bricks”, sawdust ash was burned to temperatures of 200

°C, 600 °C and 1200 °C and cured with concrete to allow the limestone

(CaCO3) component to be converted into quick lime during firing and

50
hydrate without expansion in the volume of the bricks. Measurements taken

on the comprehensive strength, water absorption and linear shrinkage show

that the compressive strength of the bricks decreased as sawdust ash was

increased and maximum compressive strength was achieved at a burning

temperature of 600 °C at 10% sawdust ash replacement.

In the study, “Modelling of Cement Thickening Time at High

Temperatures With Different Retarder Concentrations” by Umeokafor, et

al., (2010), a mathematical model which predicts thickening time at the

specified retarder concentrations and temperatures was developed. The

model showed good agreement with experimental values with less than

10% deviation.

Synthesis

Presented here are the studies related to the proponents’ target of

evaluating different agricultural wastes as drilling cement additive and for

the development of a mixer.

A study made by Varma, (2016), entitled “Effect of Change in Mixing

Time of mixer on Wet Density, Dry Density, Workability and Compressive

Strength of Concrete”, the study was carried out on concrete properties by

changing its mixing time. Ten concrete samples were prepared and tested

with mixing time of maximum 10 minutes.

In the present study, 14 samples composed of Rice husk ash,

Sugarcane Bagasse Ash, Sawdust ash and Eggshells were prepared and

51
tested with the standard mixing time of 10 minutes. No adjustments have

been done.

As per the result of the research conducted by Goce, et al., (2018)

entitled “Development of Pulverizing and Mixing Machine for Drilling

Cement Additives”, the mixing speed used was 60 rpm and yielded positive

results. The present study used the 60 rpm mixing speed but with the helical

ribbon blade impeller type.

In the study “The maximum percentage of fly ash to replace part of

original Portland cement (OPC) in producing high strength concrete” by

Mallisa, et al., (2014), concluded that the maximum percentage of fly ash to

replace a part of cement in the high-strength concrete mix to obtain the

strength, which is equivalent to the strength of concrete with OPC only is

25%. The strength of concrete with 25% fly ash (86.62 MPa) at age 28-days

is slightly higher than that of strength of OPC only (84.09 MPa). The use of

fly ash of 30% as the replacement of cement gives a strength (78.93 MPa)

lower than that of OPC only strength.

In the present study, the researchers had undergone adjustments

with the percentage of ash replacement. They used up to 30% of ash

replacement in order to test the capability of the raw materials being used

as retarder.

The above-mentioned related literatures were based on the previous

studies for better understanding for this research. Moreover, this research

52
doesn’t duplicate any literature but serves as supplementary information for

producing partial replacement of Portland cement and different retarders for

drilling cement.

Mathematical Model

Mathematical modelling is the process of using various mathematical

structures - graphs, equations, diagrams, scatterplots, tree diagrams, and

so forth - to represent real world situations. The model provides an

abstraction that reduces a problem to its essential characteristics.

53
 CHAPTER III

RESEARCH METHODS AND PROCEDURE

This chapter presents the detailed experimental methods and procedures

that was used by the researchers for the completion of this study

Research Design

This study is limited to the evaluation of the mixed proportion of the

produced mixture and the mathematical modelling of the experimental values

obtained.

Preparation of the raw materials for

mixture considering ratio and
proportion

Determination of the operating

conditions of the mixer in terms of
operating capacity, time, and speed

Evaluation of the properties of the

product cement in terms of autoclave
expansion, setting time, compressive
strength, and fineness

Mathematical modelling of setting

time as a function of ash
concentration.

Figure 12. Workflow for the Study

54
Methods of Testing

1. Preparation of the cement slurry considering ratio and proportion

As per the result of the research conducted by Goce, et al., (2018)

entitled “Development of Pulverizing and Mixing Machine for Drilling

Cement Additives”, the partial replacement of up to 20% eggshell powder

in cement mixture is proven effective through application of standard

laboratory testing process mandated by the ASTM.

A study made by Mallisa, et al., (2017) entitled “The Maximum

Percentage of Fly Ash to Replace Part of Original Portland Cement (OPC)

in Producing High Strength Concrete”, shows that the maximum percentage

of fly ash to replace a part of Portland cement is 25%.

As a result, the researchers have come up with a matrix to obtain the

best proportion of Portland Cement Type I and Pulverized Eggshell mixture

and sugarcane bagasse ash, sawdust ash, and rice husk ash given by the

table below:

Mixing components were prepared by carbonizing the raw materials

from agricultural wastes up to 750 degrees Celsius. Produced ashes

where weighted and mixed together with Original Portland Cement,

powder eggshells, and other ashes in specified ratio and proportions.

55
 Table 11. Matrix for OPC, Eggshells, and Rice Husk Ash

(10 mins. Mixing Time)

Mixture Ordinary Portland

Eggshells % Rice Husk Ash %
Name Cement %

Rice Husk Ash 1 10 80 10

Rice Husk Ash 2 10 70 20

Rice Husk Ash 3 10 60 30

Rice Husk Ash 4 20 70 10

Rice Husk Ash 5 20 60 20

Rice Husk Ash 6 20 50 30

Table 12. Matrix for OPC, Eggshells, and Sugarcane Bagasse Ash

(10 mins. Mixing Time)

Ordinary Portland Sugarcane

Mixture Name Eggshell %
Cement % Bagasse %

Sugarcane Bagasse 1 10 80 10

Sugarcane Bagasse 2 10 70 20

Sugarcane Bagasse 3 10 60 30

Sugarcane Bagasse 4 20 70 10

Sugarcane Bagasse 5 20 60 20

Sugarcane Bagasse 6 20 50 30

56
 The table 11 and 12 was used in determining the best proportion for

the Portland Cement Type 1 and the said additives. In the RHA table and

SCB table; composition of eggshells in mixtures 1, 2, and 3 only have 10%,

while mixtures 4, 5, and 6, have 20% of composition; composition of

Portland cement in mixtures 1, 2, and 3, are 80%, 70%, and 60%, while

mixtures 4, 5, and 6 have 70%, 60%, and 50%, respectively; and

composition of ashes in mixtures 1 and 4 are 10%, mixtures 2 and 5 are

20%, and mixtures 3 and 6 are 30% Mixing time is set at 10 minutes in

accordance to the specified mixing time for ribbon-type blenders.

2. Determination of the operating conditions of the mixer

a.) Method of Determining Operating Capacity

The operating capacity of the mixer will depend on the operating

capacity of the pulverizing and the carbonizing machine. This was done

through trial and error. Based on the calculations conducted considering

the requirement of the laboratory testing center, it is determined that

10kg should be the capacity of the mixer.

ASTM C94, “Specification for Ready Mix Concrete”, indicated

that the volume of concrete in a mixer shall not exceed 80% of the total

volume of the drum or container.

b.) Method of Determining Mixing Time

The mixing time was determined by using the standard given for

ribbon blender by the powder mixing handbook which is 10 minutes.

57
 c.) Method of Determining Mixing Speed

The mixing speed was determined by using Froude’s

Equation for stirred tanks given by:

𝐹𝑟𝑜𝑢𝑑𝑒 ′ 𝑠 𝑁𝑢𝑚𝑏𝑒𝑟 × 𝑔𝑟𝑎𝑣𝑖𝑡𝑎𝑡𝑖𝑜𝑛𝑎𝑙 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡, 𝑚/𝑠2

𝑚𝑖𝑥𝑖𝑛𝑔 𝑠𝑝𝑒𝑒𝑑, 𝑟𝑝𝑚 = √
𝑟𝑎𝑑𝑖𝑢𝑠 𝑜𝑓 𝑚𝑖𝑥𝑖𝑛𝑔 𝑡𝑜𝑜𝑙, 𝑚

Where:

Froude’s Number = 0.9, designated value for ribbon mixers

Gravitational constant = 6.67408 × 10-11 m3 kg-1 s-2

Radius of mixing tool = 0.285m

(Perry’s Chemical Engineers’ Handbook, 2007)

3. Evaluation of the properties of the product cement

a.) Autoclave Expansion (ASTM C151)

ASTM C151 or “Standard Test Method for Autoclave Expansion

of Hydraulic Cement” delivers an index of the potential delayed

expansion. This is caused by the hydration of CaO, or MgO, or both.

At a high pressure, a small sample of the paste was put into a

vessel. The autoclave is slowly brought to 2.03 MPa. Afterwards, for 3

hours, it was kept at that pressure. The change in the length of the

specimen due to its time in the autoclave was measured and was

recorded in percentage.

58
b.) Compressive Strength (ASTM C109)

A mortar was used in this method. It consists of first the cement and

second, the sand proportioned by mass. At specified water or cement

ratios, the air-entraining Portland cements was mixed.

By tamping in two layers, a two-inch test cubes was compressed.

Together with the mold, these was cured for three to seven days. It was

stripped. Afterwards, it was immersed in water which is lime until tested.

(ASTM International, 2005)

c.) Time of Setting (ASTM C191)

The sample was molded in the laboratory. According to research,

usually it is placed or run in a cabinet which is moist and is allowed to

start setting. Penetration tests was performed periodically. A 1-mm Vicat

needle is allowed to settle into the sample paste. The initial time of

setting of Vicat was calculated. This was possible as the time elapsed is

at 25 mm between the penetration time and the initial contact of water

and cement. As the time when the needle does not sink visibly into the

paste sample, the Vicat final time of setting was calculated. (ASTM

International, 2005)

The presence and capability of lignin, an effective retarding agent

in the sawdust ash was tested through the determination of the setting

time of cement with the cement additives. The retarder will delay the

time of setting or hardening time of cement without decreasing its

strength. The longer the time it takes for the cement to set or harden,

59
 the more ideal it is to be used in deep, hot wells since the cement was

able to reach deeper in the wellbore.

d.) Fineness (ASTM C430)

This test covered fineness of the cement. It used sieve in testing.

The frame of the sieve was made of a metal which was shaped in circle

with dimensions that were specified. Either a nickel sieve sheet which is

electroformed or a woven-wire which is stainless steel is fitted. (ASTM

International, 2003) 75 microns as the size of particle was the standard

of the Portland cement.

4. Methods for Mathematical Modelling

a) Data Evaluation and Preparation

Setting time plots from for the cement slurry from the experiments

was used together with the temperature range investigated.

b) Data Correlation using Excel Spreadsheet

Excel spreadsheet is a platform developed by Microsoft for

windows that has calculation, graphing tools, data analysis and a

macro programming language called visual basic for application

which allows the user to make use of varieties of numerical method.

Excel has functions that can solve engineering and statistical

problems.

Additional features that are readily available using add-ins such

as analysis toolpak which provides statistical and engineering

60
 analysis tools. In this work, regression analysis under data analysis

was used to develop correlations for each parameter that are

candidates for wax appearance temperature prediction

c) Comparison of results of the model prediction with

experimental results

The results will then be tabulated and compared to the

experimental results. Percentage errors was calculated from the

predicted time of setting with the experimental time of setting.

61
 CHAPTER IV

DEVELOPMENT OF THE PROTOTYPE, EXPERIMENTAL RESULTS AND

DISCUSSION

This chapter presents the schematic diagram, the components and

functions of each part and the mixer's final setup. It also includes the presentation

and discussion the preliminary and final performance testing experimental results.

Development of the Prototype

The design of the mixer was made through Google’s SketchUp.

Calculations for the mixer’s design are made using various literatures such as

handbooks, standards, and peer-reviewed research papers.

Schematic Diagram of the Machine

The mixer shown in Figure 14 is integrated in the prototype study entitled

“Design and Development of Agricultural Wastes Processing Machine for Drilling

Cement Retarder“ by Beltran,.et al. The mixer is a helical ribbon mixer type. Ribbon

blenders are convective mixers. The mixture movement is forced by the rotation of

the ribbon which is circulating the product in 2 directions. By mixing enough time,

those 2 axial movement, coupled with some radial movement (blades "cutting" the

material when rotating), will allow to reach the required degree of homogeneity.

62
Mixing Time

The mixing time is defined as the time required reaching a desired

homogeneity.

The mixing time is set to 10 minutes based on Powder Mixing Handbook (2018),

Varma (2016), and Goce et al., (2018), and Lamotte (2018). The following

elements will influence the mixing time:

a. Mixing Volume

Mixing volume should be 70% of mixer total volume. Visually, the top

of the blades must be slightly above the level of product, and some head

space to the top cover must always be available. It is a very common

problem to find ribbon blenders overloaded which is strongly decreasing

their performance. To be noted that it is not advised to under-fill a ribbon

blender, since the level of powder must reach inner ribbon in order to be

moved and thus mixed.

b. Mixing Speed

The optimum mixing speed is of course dependent on the design of

the mixer. Mixing speed is then dependent on the Froude number,

mixing volume, and impeller type and diameter.

c. Froude Number

Froude number is a dimensionless quantity used to indicate the

influence of gravity on fluid motion.

63
System Components and Functions

1. Controller

It facilitates the speed at which the rotation of the mixer’s impeller is

done. The controller ranges from 0 rpm to 60 rpm.

Figure 13. Mixer Controller

2. Impeller

It is used to mix the amounts of Portland cement, eggshell powder,

and different types of ash prior to laboratory testing. Double helical impeller

is used in the design because of its effectivity and efficiency in mixing

powders.

Figure 14. Impeller

64
 3. Motor

It is used to rotate the impeller in order to agitate the powder.

Figure 15. Motor

4. Pillow Block

A pillow block (or plummer block) is a pedestal used with compatible

bearings and multiple accessories to support a rotating shaft.

Figure 16. Pillow Block

5. Shaft

The shaft is a rotating machine element that transmits energy to spin

and begin the pulverizing of the belt and pulley assembly. 1-in diameter

stainless steel shaft is used to support the weight and the torque of the

mixer.

65
 Figure 17. Shaft

6. Body

The body is used to contain the powder being mixed in the mixer. It

is made of stainless steel and has a height of 0.3 meter and a diameter of

0.23 meter.

Figure 18. Body

Determining the Best Proportion of the Drilling Cement Mixture

After obtaining the laboratory results, samples RH1, RH2, RH3, RH6,

SCB2, and SCB3 failed to form in a mold and will therefore not be further be

pursued. On the other hand, samples RH4, RH5, SCB1, SCB4, SCB5, SCB6, M1,

and M2 will be further be evaluated using the standard type 1 (Normal) cement or

Ordinary Portland cement specified by ASTM C150 .

66
Evaluation of Laboratory Test Results

Samples RH4, RH5, SCB1, SCB4, SCB5, SCB6, M1, and M2 will then be

evaluated for Autoclave Expansion, 3 and 7-day Compressive Test, and Initial and

Final Setting Time.

a. Autoclave Expansion

Table 13 shows the results for ASTM C151 or Standard Test Method for

Autoclave Expansion of Hydraulic Cement.

Table 13
Test Result for Autoclave Expansion
Sample No. Paramater Specification Results (%)
Limit
Rice Husk 4 0.03
RH5 0.04
SCB1 0.1
Soundness: (%)
SCB4 0.17
Resistance to
SCB5 0.18
Autoclave 0.80% max
SCB6 0.2
expansion or
M1 0.19
Contraction
M2 0.12
SD1 0.43
Pure Portland -0.01

A maximum expansion of 0.80% is set with accordance to ASTM

C151. All samples passed the standard and exhibit a low expansion

67
 percentage which means that the produced samples are promisingly sound

and are not prone to excessive expansion.

Sample RH4 exhibits the lowest expansion percentage which is

explained by its low CaO and MgO content which greatly influence the

gradual expansion of the cement. The higher the CaO and MgO content,

the more likely the cement will expand during hydration.

b. Fineness

Table 14 shows the results for ASTM C430 or Standard Test Method

for Fineness of Hydraulic Cement.

Table 14
Test Result for Fineness of Hydraulic Cement

Sample No. Paramater Specification Limit Results

(%)
RH4 94.6
RH5 94.3
SCB1 95.8
SCB4 95.1
SCB5 96.3
Fineness 90% min
SCB6 94.7
M1 93.1
M2 94
SD1 95.19
Pure Portland 98.3

68
 A minimum fineness of 90% is set with accordance to ASTM C430.

All samples passed the test specified by the standard.

c. Compressive Strength

Table 15 shows the results for ASTM C109 or Standard Test Method

for Compressive Strength of Hydraulic Cement for 3-day compressive

strength.

Table 15
Test Result for 3-day Compressive Strength
Sample No. Paramater Specification Limit Results
(%)
RH4 14
RH5 13.5
SCB1 15
SCB4 14.32
SCB5 15.39
3-day
SCB6 14.63
Compression 12 MPa min
M1 12.72
Test
M2 10.76
SD1 12.5
Pure Portland 21

A minimum 3-day compressive strength of 12 MPa is set with accordance

to ASTM C109. All samples passed the standard except for sample M2.

Most of the sample exceeded the standard specification limit.

69
 Most of the samples passed the 3-day compression test except for

the sample M2. As seen in the graph, SCB samples shows higher

compressive strength than RH and M samples. This is because the

compressive strength is greatly influenced by the fineness of the sample.

Table 16 shows the results for ASTM C109 or Standard Test Method

for Compressive Strength of Hydraulic Cement for 7-day compressive

strength.

Table 16
Test Result for 7-day Compressive Strength
Sample No. Paramater Specification Results (%)
Limit
RH4 16.6
RH5 19.2
SCB1 19.02
SCB4 19.12
SCB5 19.05
7-day ≥19 MPa
SCB6 19
Compression
M1 17
Test
M2 17
SD1 19.6
Pure Portland 29

A minimum compressive strength of 17 MPa is set in accordance

with ASTM C109. Samples RH4, M1, and M2 did not pass the requirement

70
 of 19 MPa set by the standard. Samples RH5, SCB1, SCB5, and SCB6 on

the other hand, passed the test.

Samples RH5, SCB1, SCB5, and SCB6 passed the compressive test

and are closely linked to their particle fineness which greatly affect its

strength.

d. Setting Time

Table 17 shows the results of ASTM C191 or Standard Test Methods

for Time of Setting of Hydraulic Cement by Vicat Needle for Initial Setting

Time.

Table 17
Test Result for Initial Setting Time using Vicat Needle
Sample No. Paramater Specification Limit Results (%)
RH4 171
RH5 202
SCB1 211
SCB4 219
Initial >210 minutes
SCB5 237
Setting
SCB6 281
Time
M1 178
M2 218
SD1 216
Pure Portland 147

A specification limit of 210 minutes has been established in accordance

with ASTM C191 or Standard Test Methods for Time of Setting of Hydraulic

71
Cement by Vicat Needle. Samples RH4, RH5, and M1 failed the test, while

samples SCB1, SCB4, SCB5, SCB6, and M2 on the other hand passed the

specification set by the standard.

As shown, five samples namely SCB1, SCB4, SCB5, SCB6, and M2 passed

the test. It is also worth noticing that SCB samples exhibit a much higher initial

setting time than other samples. Although not all samples passed the test, the

setting time nevertheless increased as compared to standard OPC with the

exemption of SD1.

Table 18 shows the results of ASTM C191 or Standard Test Methods for

Time of Setting of Hydraulic Cement by Vicat Needle for Final Setting Time.

Table 18
Test Result for Final Setting Time using Vicat Needle
Sample No. Paramater Specification Limit Results (%)
RH4 295
RH5 480
SCB1 330
SCB4 365
Final Setting <420 minutes
SCB5 403
Time
SCB6 417
M1 550
M2 505
SD1 315
Pure Portland 210

72
 A specification limit of 420 minutes has been established in

accordance with ASTM C191 or Standard Test Methods for Time of Setting

of Hydraulic Cement by Vicat Needle. Samples RH4, SCB1, and SCB4

failed to pass the standard specification for final setting time while samples

RH5, SCB5, SCB6, M1, M2, and SD1 on the other hand, passed the test.

As shown in table 18, RH4, SCB1, SCB4, and SD1 passed the test.

Sample SCB6 exhibits the highest final setting time, exceeding the

specification limit. All samples show an increase in setting time relative to

OPC.

Table 19 shows the summary of the laboratory results for Autoclave

Expansion, 3-day Compressive Strength, 7-day Compressive Strength,

Initial Setting Time, and Final Setting Time.

Table 19
Summary of the Results

Autoclave Fineness, 3-day 7-day Initial Final

Expansion, % Compressive Compressive Setting Setting
% Strength, Strength, Time, Time,
MPa MPa min min
RH4 0.03 94.6 14 16.6* 171* 295
RH5 0.04 94.3 13.5 19.2 202* 480*
SCB1 0.1 95.8 15 19.02 211 330
SCB4 0.17 95.1 14.32 19.12 219 365
SCB5 0.18 96.3 15.39 19.05 237 403
SCB6 0.2 94.7 14.63 19 281 417
M1 0.19 93.1 12.72 17* 178* 550*

73
 M2 0.12 94 10.76* 17* 218 505*
SD1 0.43 95.19 12.5 19.6 216 315
OPC -0.01 98.3 21 29 147 210
(* Denotes failed results.)

Table 19 shows the summary of the results. All the samples are

compared to the existing OPC available commercially. Samples SCB1,

SCB4, SCB5, and SCB6 are the only samples that passed all the test

required by ASTM C150.

As per the Autoclave Expansion, all samples show an interestingly

low expansion and compression during hydration. SCB1, SCB4, SCB5, and

SCB6 recorded an autoclave expansion of: 0.1%, 0.17%, 0.18%, and 0.2%

respectively.

For fineness, all samples have passed the test. Samples SCB1,

SCB4, SCB5, and SCB6 recorded a fineness of 95.8%, 95.1%, 96.3%, and

94.7% which is relatively low compared to OPC.

For 3-day compressive strength, all samples passed the test except

for sample M2. Samples SCB1, SCB4, SCB5, and SCB6 recorded a 3-day

strength of 15 MPa, 14.32 MPa, 15.39 MPa, and 14.63 MPa respectively.

Samples have noticeably lower compressive strength than pure OPC.

For 7-day compressive strength, fewer samples have passed the

test. Samples SCB1, SCB4, SCB5, and SCB6 exhibits a compressive

strength of: 19.02 MPa, 19.02 MPa, 19.12 MPa, 19.05 MPa, and 19 MPa.

74
 For initial setting time, samples SCB1, SCB4, SCB5, and SCB6

recorded initial setting times of: 211 min, 219 min, 237 min, and 281 min

respectively.

For final setting time, the graph at some extent, resembles the initial

setting time graph. Samples SCB1, SCB4, SCB5, and SCB6 recorded final

setting times of: 330 min, 365 min, 403 min, and 407 min.

Mathematical Modelling

A mathematical model is used to describe how various cement constituents

affected the setting time of the produced cement retarder. By performing various

chemical test on the produced samples, the amount of each chemical component

is determined. Table 20 shows each sample’s chemical components.

Table 20. Chemical Components of the Produced Samples

SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2O K2O

SCB1 17.2 3.95 2.4 53.7 0.9 2.27 0.15 0.61

SCB4 39 2.65 1.93 44.51 0.79 1.85 0.22 0.95

SCB5 34.66 2.38 1.81 46.11 0.8 1.79 0.23 0.87

SCB6 31.91 2.33 1.77 49.28 0.8 1.77 0.23 0.8

The chemical components only of the best samples will then be evaluated.

75
 a. Mathematical Modelling using Ash Content

The samples are then modelled using the ash or the retarder content.

This is to determine the effects of different quantities of retarder with respect

to the cement.

Table 21. Data used in Mathematical Modelling using Ash Content

Ash Initial Final Autoclave 3-day 7-day

Conten Settin Settin Expansion Compressiv Compressiv

t g g ,% e Strength, e Strength,

Time, Time, MPa MPa

min min

SCB
10% 211 330 0.1 15 19.02
1
SCB
10% 219 365 0.17 14.32 19.12
4
SCB
20% 237 403 0.18 15.39 19.05
5
SCB
30% 281 417 0.2 14.63 19
6

Table 21 shows the different values that are used in various

mathematical models using ash content.

Initial Setting Time vs. Ash Content

The initial setting time is modelled with ash content to determine the

effect of different quantities of ash in the initial setting time of the cement.

76
The four data points which have passed namely: SCB1, SCB4, SCB5, and

SCB6 will be used.

Initial Setting Time vs. Ash Content

300
SCB6
Initial Setting Time, minutes
SCB5
250
SCB4
200 SCB1 y = 1100x2 - 110x + 215
R² = 0.9891
150

100

50

0
0% 5% 10% 15% 20% 25% 30% 35%
Ash Content, %

Figure 19. Scatter Plot for Initial Setting Time vs. Ash Content

Polynomial trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.9891 suggests a great positive correlation between the two

variables. Substituting the y in the equation y= 1100x2 - 110x + 215 with 210

which is the minimum specification limit for a retarder, the model shows a

9.06 or 9% minimum ash content.

Final Setting Time

The final setting time is modelled with ash content to determine the

effect of different quantities of ash in the initial setting time of the cement.

The four data points which have passed namely: SCB1, SCB4, SCB5, and

SCB6 will be used.

77
 Final Setting Time vs. Ash Content
450
400 SCB6

Final Setting Time, minutes

SCB4 SCB5
350 y = -2075x2 + 1177.5x + 250.5
SCB1 R² = 0.8673
300
250
200
150
100
50
0
0% 5% 10% 15% 20% 25% 30% 35%
Ash Content, %

Figure 20. Scatter Plot for Final Setting Time vs. Ash Content

Polynomial trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.8673 suggests a great positive correlation between the two

variables. Substituting the y in the equation -2075x2 + 1177.5x + 250.5 with

420 which is the maximum specification limit for a retarder, the model shows

a 33.37 or 33% maximum ash content.

Autoclave Expansion vs. Ash Content

The autoclave expansion is modelled with ash content to determine

the effect of different quantities of ash in the autoclave expansion of the

cement. The four data points which have passed namely: SCB1, SCB4,

SCB5, and SCB6 will be used.

78
 Autoclave Expansion vs. Ash Content
0.25

Autoclave Expansion, %
0.2 SCB6
SCB4 SCB5
0.15

y = -1.25x2 + 0.825x + 0.065

0.1 SCB1 R² = 0.5683

0.05

0
0% 5% 10% 15% 20% 25% 30% 35%
Ash Content, %

Figure 21. Scatter Plot Autoclave Expansion vs. Ash Content

Polynomial trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.5683 suggests a weak positive correlation between the two

variables. Therefore, ash content is not a good predictor of autoclave

expansion of the cement as suggested by the model.

By substituting y with 0.8 which is the maximum specification limit for

expansion, the model shows a maximum of 207% ash content which means

that any amount of ash will not exceed the standard limit for autoclave

expansion. Even so, this result is not conclusive because of the weak

correlation.

3-day Compressive Strength vs. Ash Content

The 3-day compressive strength is modelled with ash content to

determine the effect of different quantities of ash in the 3-day compressive

79
strength of the cement. The four data points which have passed namely:

SCB1, SCB4, SCB5, and SCB6 will be used.

3-day Compressive Strength vs. Ash Content

15.6

3-day Compressive Strength, MPa

15.4 SCB5

15.2
SCB4
15

14.8
y = -74.5x2 + 29.65x + 12.44
14.6 SCB6
R² = 0.6402
14.4
SCB1
14.2
0% 5% 10% 15% 20% 25% 30% 35%
Ash Content, %

Figure 22. Scatter Plot for 3-day Compressive Strength vs. Ash

Content

Polynomial trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.6402 suggests a weak positive correlation between the two

variables. Therefore, ash content is not a good predictor of 3-day

compressive strength of the cement as suggested by the model.

By substituting y with 12 which is the minimum specification limit for

expansion, the model shows a maximum of 41% ash. Even so, this result is

not conclusive because of the weak correlation.

80
7-day Compressive Strength vs. Ash Content

The 7-day compressive strength is modelled with ash content to

determine the effect of different quantities of ash in the 7-day compressive

strength of the cement. The four data points which have passed namely:

SCB1, SCB4, SCB5, and SCB6 will be used.

7-day Compressive Strength vs. Ash Content

19.14
7-day Compressive Strength, MPa

19.12 SCB4
19.1
19.08
19.06
SCB5
19.04
19.02 SCB1
y = -1.5x2 + 0.25x + 19.06
19 SCB6
R² = 0.3958
18.98
0% 5% 10% 15% 20% 25% 30% 35%
Ash Content, %

Figure 23. Scatter Plot for 7-day Compressive Strength vs. Ash Content

Polynomial trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.3952 suggests a weak positive correlation between the two

variables. Therefore, ash content is not a good predictor of 7-day

compressive strength of the cement as suggested by the model.

By substituting y with 19 which is the minimum specification limit for

expansion, the model shows a maximum of 30% ash content. Even so, this

result is not conclusive because of the weak correlation.

81
b. Additional Mathematical Models

Additional mathematical models were made to further describe the

effects of fineness, and sulfur trioxide content in compressive strength and

autoclave expansion respectively.

Table 22. Data used in Additional Mathematical Models

Ash Fineness, 3-day 7-day Sulfur Autoclave

Content, % Compressive Compressive Trioxide Expansion,

% Strength Strength Content, %

SCB1 10% 95.8 15 19.02 2.27 0.1

SCB4 10% 95.1 14.32 19.12 1.85 0.17

SCB5 20% 96.3 15.39 19.05 1.79 0.18

SCB6 30% 94.7 14.63 19 1.77 0.2

Table 22 shows the different values that are used in additional

mathematical models using Fineness and Sulfur Trioxide content in relation

with Compressive Strength and Autoclave Expansion respectively.

Fineness vs. 3-day Compressive Strength

The 3-day compressive strength is modelled with fineness to

determine the effect of different quantities of ash in the 7-day compressive

strength of the cement. The four data points which have passed namely:

SCB1, SCB4, SCB5, and SCB6 will be used.

82
 Fineness vs. 3-day Compressive Strength
15.6

3-day Compressive Strength,

y = -1.092x3 + 313.46x2 - 29992x + 956526
15.4
R² = 1
15.2 SCB5
15 SCB1
14.8

MPa
14.6 SCB6
14.4
SCB4
14.2
94.6 94.8 95 95.2 95.4 95.6 95.8 96 96.2 96.4
Fineness, %

Figure 24. Scatter Plot for Fineness vs. 3-day Compressive Strength

A third degree polynomial trend line is used in the curve fitting as it

shows the highest R square value compared to other types of trend line. An

R square value of 1 suggests a perfect correlation between the two

variables. Therefore, fineness greatly affects and is a good predictor of 3-

day compressive strength of the cement as suggested by the model.

Fineness vs. 7-day Compressive Strength

Fineness will then be modelled with Compressive Strength. The four

data points which have passed namely: SCB1, SCB4, SCB5, and SCB6 will

be used.

83
 Fineness vs. 7-day Compressive Strength
19.14

7-day Compressive Strength, MPa

SCB4
19.12
19.1
19.08
19.06 y = 0.3573x3 - 102.44x2 + 9790.7x - 311885
19.04 R² = 1
SCB5
19.02 SCB1
19 SCB6
18.98
94.6 94.8 95 95.2 95.4 95.6 95.8 96 96.2 96.4
Fineness, %

Figure 25. Scatter Plot for Fineness vs. 7-day Compressive Strength

A third degree polynomial trend line is used in the curve fitting as it

shows the highest R square value compared to other types of trend line. An

R square value of 1 suggests a perfect correlation between the two

variables. Therefore, fineness greatly affects and is a good predictor of 7-

day compressive strength of the cement as suggested by the model.

Sulfur Trioxide Content vs. Autoclave Expansion

Sulfur Trioxide content will then be modelled with Autoclave

Expansion. The four data points which have passed namely: SCB1, SCB4,

SCB5, and SCB6 will be used.

84
 Sulfur Trioxide Content vs. Autoclave Expansion
0.25

SCB6

Autoclave Expansion, %
0.2
SCB5
SCB4
0.15

y = 0.8668x-2.638 SCB1
0.1
R² = 0.9898

0.05

0
0 0.5 1 1.5 2 2.5
SO3 Content, %

Figure 26. Scatter Plot for Fineness vs. 7-day Compressive Strength

Exponential trend line is used in the curve fitting as it shows the

highest R square value compared to other types of trend line. An R square

value of 0.9898 suggests a nearly perfect correlation between the two

variables. Therefore, sulfur trioxide content greatly affects and is a good

predictor of autoclave expansion of the cement as suggested by the model.

85
 CHAPTER V

SUMMARY OF FINDINGS, CONCLUSIONS AND RECOMMENDATIONS

This chapter includes the summary of findings, derived conclusions, and

recommendations for the future researchers.

Summary of Findings

The following are the summary of findings from different calculations and

laboratory tests.

1.) Mixing capacity of 7 kg has been established considering the amount

requirement by the cement testing laboratories.

2.) Mixing speed of 9 rpm has been established considering the density, and

dimensions of the mixer using Froude’s Equation.

3.) Upon laboratory testing, only samples SCB1, SCB2, SCB3, and SCB4

passed all the requirements namely: Autoclave Expansion, Fineness, 3-day

Compressive Strength, 7-day Compressive Strength, and Initial and Final

Setting Time.

4.) A minimum of 9% and a maximum of 33% sugarcane bagasse ash

content are established as demonstrated by different mathematical

models.

86
Conclusions

The following are the results of the evaluation and interpretation of all the

data acquired.

1.) The amount of cement to be fed in the mixer should be 70% of the total

capacity of the mixer which is 7 kg for a suitable mixing.

2.) Mixing speed is affected by various factors such as mixture’s density,

radius of the impeller, and the Froude’s number of the mixer.

3.) Partial replacement of up to 20% powdered eggshell in Portland cement is

proven effective by the laboratory results.

4.) Sugarcane bagasse ash is proven the most effective as additive than rice

husk and sawdust especially in increasing the setting time of the cement.

5.) Further addition of ash on cement leads to a higher setting time as

described by the mathematical model.

6.) Further addition of ash on cement leads to lower 3 and 7-day compressive

strength as described by the mathematical model.

7.) Further addition of ash on cement leads to higher autoclave expansion as

described by the mathematical model.

8.) Fineness is proven to be a great indicator of compressive strength with its

perfect correlation as described by the mathematical model.

Sulfur trioxide greatly affects the expansion of the cement as proven by its

perfect correlation in the mathematical model.

87