Department of Mechanical Engineering

College of Engineering and Design

Silliman University

ME 51PN- Engineering Project I

THE INFLUENCE OF BIO-FILLERS FROM WASTE GREEN MUSSEL

SHELLS (Perna viridis) TO THE FLAME RETARDANCY, THERMAL
STABILITY, AND FLEXURAL BEHAVIOR OF POLYESTER SHEETS

Submitted to:

ENGR. LOUIE PIERRE O. EQUIO

Submitted by:

ALFEREZ, VERN JASMINE M.

BAILON, JENNICA ANNE A.

GRANADEROS, KEN B.

TORRES, MA. COLEEN V.

Dumaguete City

October 2, 2019
 TABLE OF CONTENTS

I. INTRODUCTION ......................................................................................................................1

A. Background of the Study .......................................................................................................1

B. Statement of the Problem ......................................................................................................1

C. Hypotheses ............................................................................................................................2

D. Research Questions ...............................................................................................................3

E. Objectives of the Study .........................................................................................................3

F. Significance of the Study ......................................................................................................4

G. Scope and Limitations ...........................................................................................................5

H. Definition of Terms ...............................................................................................................6

II. REVIEW OF RELATED LITERATURE, THEORETICAL FRAMEWORK, AND

CONCEPTUAL FRAMEWORK .................................................................................................9

A. Related Works .......................................................................................................................9

B. Theoretical Framework ........................................................................................................14

C. Conceptual Framework .......................................................................................................32

III. METHODOLOGY ................................................................................................................34

A. Fabrication Procedure ..........................................................................................................34

B. Testing Procedure ................................................................................................................38

C. Post- Test Data Analysis .....................................................................................................39

 D. Ethical Consideration ..........................................................................................................43

IV. REFERENCES ......................................................................................................................45

V. APPENDIX ..............................................................................................................................48
 LIST OF TABLES

Table 1. Chemical Composition of Shellfish CaCO3. Characterization of Calcium. ...................12

Table 2. Effect of concentration (%) ..............................................................................................14

Table 3. Pure Unsaturated Polyester Properties.. ..........................................................................20

Table 4. Sample Data Table for ANSI/UL94. ...............................................................................41

Table 5. Example table results for 20mm- Vertical Burning Testing.. .........................................42

Table 6. Material Classification. ...................................................................................................43

Table 7. Materials used in the procedures. ....................................................................................48

Table 8. Equipment used in the procedures. .................................................................................50

 LIST OF FIGURES

Figure 1. The Philippine Green Mussels or Tahong. ......................................................................9

Figure 2. The chemical structure depiction of calcium carbonate. ...............................................11

Figure 3. Ground calcium carbonate. ............................................................................................11

Figure 4. Mineralogical composition of limestone and mussel ....................................................11

Figure 5. Unsaturated polyester resin chemical structure. ............................................................17

Figure 6. Styrene. ..........................................................................................................................18

Figure 7. Methyl ethyl ketone peroxide (MEKP). ........................................................................19

Figure 8. Horizontal Burning Test for HB Classification .............................................................25

Figure 9. Vertical burning test for V-0, V-1, V-2 classification. ..................................................25

Figure 10. Thermogravimetric analysis. ......................................................................................26

Figure 11. Flexural strength as highest stress, σ, experienced.. ....................................................28

Figure 12. Three-point flexural testing. ........................................................................................29

Figure 13. Load Deflection Curve.. ..............................................................................................29

Figure 14. Proportional limit in stress-strain curve. ......................................................................30

Figure 15. Stress-strain curve showing Young’s Modulus of elasticity.. .....................................30

Figure 16. The Conceptual Framework... .....................................................................................32

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Figure 17. Molder Design (Top view and Isometric view, respectively). ....................................35

Figure 18. Mixing set-up.. .............................................................................................................36

Figure 19. Horizontal Burning Test for HB Classification. ..........................................................39

Figure 20. Vertical Burning Test for V Classification.... ..............................................................40

Figure 21. Timetable. ....................................................................................................................52

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 I. INTRODUCTION

A. Background of the Study

In the constant search for innovations and enhancements of current technology,

reinforcements to improve the properties of materials are slowly getting the attention from the field

of engineering. Polymers has long been considered as the material mostly used as insulation

materials, appliances, furniture, construction materials, dinnerware and many more economical

uses of polymers. However, when subjected to different conditions, these polymeric composites

are susceptible to mechanical damage when loaded with different stresses and thermal degradation

when exposed to flame or heat. A lot of studies have been documented on the reinforcement of

different fibers into the polymers have successfully improved their mechanical capabilities. In this

study, the researchers are going to delve into improving the other major technological barrier when

it comes to polymers, its thermal capabilities. Enhancing the thermal stability, flame retardancy

and flexural strength of polymers using organic reinforcements from the green mussel shells

(Perna viridis) is an economical way of fully utilizing the wastes from human consumption.

B. Statement of the Problem

Despite dominating the market, polymers still possess qualities that make them

disadvantageous in some applications. One example of which is low thermal conductivity and

brittleness of thermosetting plastics. Although they exhibit high strength, these materials have

limited plasticity, and they undergo permanent deformation when subjected to stresses beyond

their capabilities. Moreover, according to a research on the organic and inorganic reinforcements

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of polymeric materials, a complete ban or restriction on the use of halogenated flame retardants

have challenged the plastics industry today due to the adverse health, safety and environmental

effects on the commonly used inorganic reinforcements like aluminum and magnesium hydroxides

(H. Abba et.al., 2015). In addition, another research stated that halogen retardants have been

shown to leach out of polymers into the natural environment where their presence is ubiquitous

and are endocrine disruptors. This problem has driven the search for alternative “halogen-free”

fire retardants which include metal hydroxide, carbonate fillers, phosphorus compounds, low melt

glasses, as well as a range of more esoteric materials (Hull, T. Richard et. al., 2011). Thus

nowadays, a lot of research are going towards enhancing the thermal and mechanical properties of

polymers by utilizing the organic products and wastes where calcium and ammonium salts are

abundant. Using reinforcements to enhance the property of polymers through bio-fillers from green

mussel shells (Perna verdis), thermal insulation, flame retardancy and flexural strength of

polymers will be improved.

C. Hypotheses

▪ There is a significant difference in the flame-retardant capability of green mussel shell

reinforced polyester sheets compared to the pure polyester sheets.

▪ There is a significant difference in the thermal stability of green mussel shell reinforced

polyester sheets compared to the pure polyester sheets.

▪ There is a significant difference between the flexural behavior of the green mussel shell

reinforced polyester sheets compared to the pure polyester sheets.

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D. Research Questions

▪ Is there a change in the surface burning rate and ignition of the green mussel shell reinforced

polyester sheets compared to the pure polyester sheets?

▪ Does the varying ratio give changes to the results of burning rate and ignition of the green

mussel shell reinforced polyester sheets?

▪ Is there a change in the thermal stability of green mussel shell reinforced polyester sheets

compared to the pure polyester sheets?

▪ Does the varying ratio give changes to the capability of green mussel shell reinforced polyester

sheets in terms of thermal stability?

▪ Is there a significant difference between the flexural strength of a pure polyester sheets green

mussel shell reinforced polyester sheets?

▪ Does the varying ratio give changes to the capability of green mussel shell reinforced polyester

sheets in terms of flexural strength?

E. Objectives of the Study

The general objectives of the study are to produce 12” by 12” by 1/2” polyester sheets

utilizing green mussel shell reinforcements to the polyester matrix and to test their thermal

stability, flame retardancy and flexural strength properties.

The specific objectives of the study are:

▪ To prepare the green mussel shell reinforcement in particulate form.

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 ▪ To fabricate 12” by 12” x 1/2” green mussel shell reinforced polyester sheets with varying

weight ratios of 50%, 60%, 70%, 80%.

▪ To test the thermal conductivity of the green mussel shell reinforced polyester sheets and

compare the obtained data it to that of the pure polyester sheet.

▪ To test the flame retardancy property of the green mussel shell reinforced polyester sheets

and compare the obtained data to that of the pure polyester sheet.

▪ To test the flexural strength of the green mussel shell reinforced polyester sheets and

compare the obtained data to that of the pure polyester sheet.

F. Significance of the Study

Polymers being strong, lightweight and moldable makes them convenient to the many

appliances and home equipment involved in people’s everyday lives. Based on a global scale,

human dependence on plastic is entirely high that over one hundred million tons of plastic is

produced annually. From high-rise buildings down to furniture, polymers are incorporated in so

many ways. Just like any material, these polymers also have weaknesses in terms of mechanical

properties and thermal capabilities. As future innovators of the society, improvements on these

properties must be done through reinforcements using organic products to further the capabilities

of the polymeric materials as one of our basic commodities while prioritizing the health, safety

and environmental effects to the growing population.

In addition, seashell or marine mollusk abundance in the Philippine shores provide an

important source of income to many coastal communities. According to a recent data gathered

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about the abundance of mussels, the output went up by 2.31% in 2017 and an even higher

increment of 36.93% on the succeeding year (Fisheries Situation Report, 2018). This wide shellfish

cultivation is continuously expanding due to its demand in seafood consumption which in turn

resulted in the large volume of shell waste which eventually would become a health hazard and

environmental problem. According to a research on shells from aquaculture, one regularly

overlooked the aspect of mollusk aquaculture is waste generation: namely the production of

calcareous shell which when decomposed, produce harmful gases with significant odor and

toxicity which are hazardous to human. Shells from the aquaculture industry are widely regarded

as a nuisance waste product, yet at the same time calcium carbonate is mined and viewed as

valuable commodity (James P. Morris et.al., 2018) This lead to this study’s use of the wastes from

the consumption of these mussel shells or better known as “tahong” in the Philippines as bio-filler

to polyester sheets. This is a sustainable way of fully utilizing the wastes from the human

consumption of these mussel shells or better known as “tahong” in the Philippines.

G. Scope and Limitations

The study will be focusing on the influence of green mussel shell to the thermal stability,

flame retarding and flexural capabilities of polyester sheets. This study is also limited to the use

of polyester resin available locally. The specimens for testing should be in the established

dimensions of 12” x 12” x 0.5’. Testing Only four volume ratios will be explored in the fabrication

and testing: 50%, 60%, 70%, 80%.Testing for each polystyrene plate is limited to 10 trials each

testing apparatus and will be conducted using a UL 94-HB for horizontal burning test, UL 94-V

20mm for vertical burning test and a Universal Testing Machine (UTM) for testing its flexural

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strength . The parameters to be measured, calculated and compared for this research are limited to

burning rate, thermal conductivity, deflection, strain, flexural strength. The only statistical test to

be employed in this research is a Spearman’s Correlation Statistical Test.

H. Definition of Terms

▪ Calcium Carbonate- Its most common natural forms are chalk, limestone, and marble,

produced by the sedimentation of the shells of small fossilized snails, shellfish, and coral over

millions of years. Although all three forms are identical in chemical terms, they differ in many

other respects, including purity, whiteness, thickness and homogeneity.

▪ Cutting- is the separation or opening of a physical object, into two or more portions, through

the application of an acutely directed force.

▪ Cure- The process in which the liquid resin becomes a solid and bonds to the fibres. This is a

chemical reaction between with different components of the resin or between the resin and a

hardener.

▪ Filler- are particles added to resin or binders (plastics, composites, concrete) that can improve

specific properties, make the product cheaper or a mixture of both. The two largest segments

for filler material use is elastomers and plastics.

▪ Flame retardants- refer to a variety of substances that are added to combustible materials to

prevent fires from starting or to slow the spread of fire and provide additional escape time.

▪ Flame spread – it can be the upward direction over a vertical wall surface or in the downward

direction is against the entrained airflow.

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▪ Green mussel (Perna viridis) - are described with shell tapers to a sharp, downturned beak

and has a smooth covered surface (periostracum) with straight or weakly concave ventral

margin and finely pitted ridge.

▪ Grinding- is an abrasive machining process that uses a grinding wheel as the cutting tool.

▪ Hardener- Hardener is a component of certain types of mixtures. In some mixtures a hardener

is used simply to increase the resilience of the mixture once it sets.

▪ Ignition- initiation of flaming combustion.

▪ Mineral Fillers- A finely pulverized inert mineral or rock that is included in a manufactured

product--e.g., paper, rubber, and plastics--to impart certain useful properties, such as hardness,

smoothness, or strength. Common mineral fillers include asbestos, kaolin, and talc.

▪ Mollusk- also spelled mollusc, any soft-bodied invertebrate of the phylum Mollusca, usually

wholly or partly enclosed in a calcium carbonate shell secreted by a soft mantle covering the

body.

▪ Opposed flow flame spread- occurs when flames spread in the opposite direction of the

surrounding airflow.

▪ Polymer- substance that has a molecular structure consisting chiefly or entirely of a large

number of similar units bonded together, e.g., many synthetic organic materials used as

plastics and resins.

▪ Premix- Premix refers to a substance or object which is mixed in an early stage in the

manufacturing and distribution process.

▪ Resin- In polymer chemistry and materials science, resin is a solid or highly viscous substance

of plant or synthetic origin that is typically convertible into polymers.Resins are usually

mixtures of organic compounds.

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▪ Retardant- is a substance that makes the progress or growth of something slower.

▪ Reinforcement material- is added to the matrix material to enhance the physical properties

of the final composite material.

▪ Thermal Stability- Thermal stability of polymer is defined as the ability of the polymeric

material to resist the action of heat and to maintain its properties, such as strength, toughness,

or elasticity at given temperature.

▪ Thermal conductivity- is a measure of a material’s ability to conduct heat.

▪ Thermal insulation - is the reduction of heat transfer between objects in thermal contact or

in range of radiative influence.

▪ Wind-aided flame spread- mode, flames spread in the same direction as the surrounding

airflow.

▪ UL 94- HB-The horizontal burning test is used to determine the HB flammability rating of a

material.The flammability rating is calculated for a test specimen as a function of the burning

rate and taking account of the material thickness.

▪ UL 94V- This test measures the self-extinguishing time of the vertically oriented polymer

specimen. The top of the test specimen is clamped to a stand and the burner is placed directly

below the specimen. The test evaluates both the burning and afterglow times and dripping of

the burning test specimen.

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 II. REVIEW OF RELATED LITERATURE, THEORETICAL FRAMEWORK AND

CONCEPTUAL FRAMEWORK

A. Related Works

1. Philippine Green Mussels

The Philippine Green Mussels (Perna viridis), also known as the Asian Green

Mussels, is a bivalve mollusk that belongs to the family Mytilidae. Locally known as

tahong, the green mussel is one of the species commercially farmed in the marine areas

of the Philippines due to its least cost in production and its ability to grow fast. According

to the Fisheries Situation Report, the expected volume of mussel production in the

Philippines in 2018 increased by 36.93% from the 2017 production level. A continuous

growth was observed on the mussel production for the previous years (Fisheries Situation

Report, 2018).

Figure 1. The Philippine Green Mussels or Tahong.

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 With the increasing production and consumption of tahong, a corresponding

increase in shell wastes can be observed. The tahong shells are non-biodegradable in

nature and are usually regarded as nuisance waste product. Shell accumulation is common

around the world, but the disposal procedure is unregulated and is often overlooked

(Mohamed et al. 2012). According to the World Organization for Animal Health, aquatic

animal shell wastes are among the common wastes that can possibly be used for green

technology and may just be the solution to the problem on disposal (World Organization

for Animal Health, 2010).

Preparation of the Bio-Filler from Mussel Shells. It is crucial that the fillers be

free from impurities. In the experiment by Fernandes, L (2014), to remove the impurities,

the mussel shells are washed and then soaked in 4% sodium hydroxide (NaOH) for 48

hours. It is then washed with deionized water and then dried. It is then grinded and sorted

by using a sieve shaker (Fernandez, 2014).

2. Calcium Carbonate in Mussel Shells

The bivalve shell of mussels is made of calcium carbonate that is embedded in the

organic matrix. Calcium carbonate, CaCO3, is the carbonic salt of calcium. The

appearance of this salt is a white, odorless powder or colorless crystal (National Center

for Biotechnology Information, n.d.).

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Figure 2. The chemical structure depiction of calcium carbonate.

Figure 3. Ground calcium carbonate.

Figure 4. Mineralogical composition of limestone and mussel.

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 Table 1.

Chemical Composition of Shellfish CaCO3. Characterization of Calcium.

Source: Carbonate Obtained from Oyster and Mussel Shells and Incorporation in

Polypropylene (2012).

It has long been accepted by science the attributes of mussel shell; made from 95 to

99.9% calcium carbonate, with a small amount of organic matrix (Currey 1999; Harper

2000). Reflected in Figure 4, a pie graph from the research on the “Waste Mussel Shells

to Treat Acid Mine Drainage” conducted in New Zealand, mussel shells have a calcium

carbonate content of 96% weight (Uster, B., et.al., 2014). Moreover, in a materials

research on the Characterization of Calcium Carbonate Obtained from Oyster and Mussel

Shells and Incorporation in Polypropylene, Hamester, Balzer and Becker identified the

oxides present in mussel and oyster shells. Shown in Table 1, mussel shells contain 95.7%

calcium oxide, and a significant 0.7% Fe2O3 content. This high quantity can influence

polymer oxidation when the shells are utilized as fillers in polymer matrix (Hamester, M.,

et.al., 2012). As obtained from the Materials Thermal Properties Database, CaCO3 has a

thermal conductivity of 2.259 W/mK, and a density of 2710 kg/m3.

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 As mineral fillers. Calcium carbonate is one of the commonly used minerals as

fillers in plastic molding compounds (Mraz, S., 2015). Mineral fillers are introduced into

polymers for the purpose of enhancing performance and reducing cost. Carefully selected

mineral filler could enhance tensile strength, impact resistance, flame retardancy and

many other properties (Shrivastava, A., 2018).

As flame retardant. According to Dr. Alexander B. Morgan of University of

Dayton Research Institute, calcium carbonate is often used as a mineral filler flame

retardant. It is often used as a bulk filler and since the compound is non-flammable, it

dilutes the total amount of fuel to be consumed (Morgan, A., 2009). In a study conducted

in Ahmadu Bello University in Nigeria, the calcium carbonate fillers contributed in the

enhanced burn ratings of the GPPS films (Abba, H., et.al., 2015).

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 Table 2.

Effect of concentration (%) of CaCO3 and (NH4)PO4 (singly and in combination) on the

UL 94 vertical burn rating of the GPPS films.

Source: Effect of Calcium Carbonate and Ammonium Phosphate on the Flammability and

Mechanical Properties of General-Purpose Polystyrene (2015).

The table above shows that there is an improvement in the burn rating of the GPPS

films when reinforced with CaCO3. A V-1 burn rating is achieved when there are calcium

carbonate fillers present, and V-0 (the best) burn rating when a combination of ammonium

phosphate and calcium carbonate fillers are present. These are better when compared to

the pure polystyrene films which only get a burn rating of V-2 (Abba, H., 2015).

B. Theoretical Framework

1. Particulate Fillers in Polymers

Bio-Fillers. Fillers are particles utilized as additives to polymers to lower the

consumption of more expensive polymer material improve or to enhance some properties

17
of the matrix material. Bio-fillers are natural, renewable resources-based and compostable

materials utilized as fillers to address rising ecological concerns (Mousa, A., 2014).

Reasons for Particulate Fillers. Particulate fillers have the ability to modify many

properties of a material. They are used for many purposes today. According to Professor

R.N. Rothon (n.d.), some of the main reasons for utilizing particulate fillers in polymers

are:

• Cost reduction

• Improved processing

• Density control

• Optical effects, such as translucency

• Thermal conductivity

• Control of thermal expansion

• Electrical properties, e.g., antistatic

• Magnetic properties

• Flame retardancy

• Improved mechanical properties, notably hardness, stiffness, abrasion and tear

resistance.

Calcium Carbonate as Particulate Filler. Calcium carbonate occurs widely in

nature and is used abundantly as a filter for having many suitable properties. There are

three crystal forms of calcium carbonate and the most commonly used is calcite. Calcite

has a specific gravity of 2.7, Moh hardness of 3 and is birefringent, with refractive indices

18
 of 1.65 and 1.48. Calcitic fillers can be produced from three different mineral sources;

chalk, limestone and marbles (Rothon, R. N., n.d.). Typical application of calcium

carbonates as filler are synthetic marble, SMC, BMC, matched die molding, building

panels, autobody putty, mine bolt grouts (Kandelbauer, A., et.al., 2014).

Morphology. Particle size and shape are important factors in determining the

performance of particulate fillers in all polymer types. Although these seem to be simple

concepts, their adequate measurement and description provides significant challenges.

Anisotropy, or aspect ratio, is particularly important, being valuable in improving factors

such as stiffness and heat distortion temperature (Rothon, R. N., n.d.). Particulate fillers

which are usually powdered substances, are particles usually less than 100 μm in size

(DeArmitt, C. & Rothon, R., 2015).

2. Polyester

Polymers. Polymers are substances whose molecules consist of units of a few types:

the units themselves, consisting of several atoms, are usually referred to as the segments

of the polymer. In the polymerization of a mixture of two monomers, the structure of each

macromolecule contains units of both monomers. Such mixture of monomers is called

copolymer and the process of its synthesis is called copolymerization (Dholakiya, B.,

2012).

Polyester. Polyesters are one of the synthetic copolymers with impressive

versatility. Several of polyester structures have found use in industry today which exhibits

19
a wide variety of properties and applications (Dholakiya, B., 2012). Still according

Dholakiya (2012), polyesters are classified into 4 categories: 1) vinyl ester resin; 2) alkyd

resin; 3) saturated polyester resin; and 4) unsaturated polyester resin.

Figure 5. Unsaturated polyester resin chemical structure.

Unsaturated Polyester Resin. The locally available polyester resin can be

categorized as an unsaturated polyester resin. Such resin type consists of two polymers:

a short-chain polyester containing polymerizable double bonds and a vinyl monomer. The

curing reaction consists of the synthesis of the vinyl monomer with the double bonds of

the polyester. Unsaturated polyester resins are classified as thermoset plastics (Fink,

2013).

Applications. The largest market for reinforced polyester resin (composite

materials) is the building and sanitary ware market; here the material finds usage as

structural parts cladding panels, sheeting (e.g. for pre-fabricated buildings), roofing tiles,

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 pipes and also for applications such as bathroom furniture (British Plastics Federation,

n.d.).

3. Polyester Resin Casting

Polyester resins are unsaturated synthetic resins that combine excellent mechanical,

electrical and thermal properties with very good chemical resistance and dimensional

stability. Polyesters also offer low moisture absorption and have good flow properties. It

has a tensile strength of 2.5 N/mm², a thermal coefficient of expansion 70 x 10-6, a

maximum continuous use temperature of 70 ᵒC and a density of 1.37 g/cm3 (British

Plastics Federation, n.d.).

Polyester Resin System. The polyester resin system to be employed in this research

will be involving the mixing of three components: 1) pre-polymer; 2) styrene, which acts

as the vinyl monomer; and 3) methyl ethyl ketone peroxide (MEKP), which acts as the

catalyst for the polymerization.

Figure 6. Styrene.

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 Styrene as the Vinyl Monomer. The vinyl monomer serves as solvent for the

polyester and reduces its viscosity. Moreover, it is the copolymerization agent in the

course of curing. Styrene is the most commonly used vinyl monomer for unsaturated

polyesters (Fink, 2013). It is a colorless liquid with a sweet smell. The chemical formula

for styrene is C8H8, and it has a molecular weight of 104.16 g/mol. (US Department of

Health and Human Services, 1992). Moreover, the dependence of the glass transition

temperature of polyester on the concentration of styrene has also been reported. The

increase of styrene concentration increases the glass transition temperature of different

phases (Sanchez, et.al., 2000). The physical properties of the product reach the optimum

when the amount of styrene ranges from 30% to 45% (Fradet & Arlaud, 1989).

Figure 7. Methyl ethyl ketone peroxide (MEKP).

Methyl Ethyl Ketone Peroxide as the Hardener. The presence of a catalyst

(hardener) will cause the resin to cure. The most widely used catalyst is methyl ethyl

ketone peroxide (Dholakiya, B., 2012). It is used 1%- 3% by resin weight (Polymer

Products, n.d.).

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4. Polymerization

Polymerization is the process in which monomer units are joined together by

chemical reaction to form long chains. These long chains set polymer materials apart from

others and give them their unique characteristic properties (Young, 1987).

Conditioning of Resin Mix. To achieve quality of product, the following is to be

observed before it is poured into the molders: 1) even distribution of the fillers by

continuous stirring; 2) elimination of air and moisture; and 3) elevated temperature held

constant to maintain low viscosity (Resin dispensing, n.d.).

Ceiling Temperature. Ceiling temperature is the temperature at which the net

polymerization rate is zero. At this condition, rates of polymerization and

depolymerization is equal (Cowie, J.M.G., 1991). This is the ideal temperature at which

the filler may be introduced into the resin mixture while it is subjected to constant stirring

Table 3.

Pure Unsaturated Polyester Properties.

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 Gelling Time. Shown in Table 3, the gelling time for UPR is about 7 minutes,

meaning that it takes about 7 minutes for the resin system to gel or become so highly

viscous meaning that it can no longer be considered workable (Yaman, K & Taga, O.,

2018). The span of time between mixing the resin and pouring into the molders should

not exceed the gelling time of 7 minutes.

Melt Blending. Melt blending is one of the most common methods for preparation

of biopolymer composites. This method is eco-friendly. In this approach, the polymer

resin is first maintained at high temperature and subsequently the filler is then added to

the polymer resin at high temperature (Deshmukh, K., et.al., 2017).

Gravity Casting. Gravity involves the pouring of molten metal from a container

into a mold under only the force of gravity, without the use of pressurized gases, vacuums,

or centrifugal force (Chamberlain, M., 1976).

Curing Conditions. The minimum curing period for polyester resin systems is 72

hours. For proper curing, ambient temperature must remain above 20ᵒC (Piling, J.,2006).

5. Filler Ratio

Volume Fractions. The volume of the composite material is equal to the sum of the

volume of the fibers and the volume of the matrix (Velmurugan, n.d.).

𝑉𝑐 = 𝑉𝑚 + 𝑉𝑓

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 Where:

Vc- volume of composite material

Vf - volume of fiber

Vm - volume of matrix

The fiber volume fraction 𝑉𝑓 and the matrix volume fraction 𝑉𝑚 be defined as;

𝑉 𝑉
𝑉𝑓 = 𝑉𝑓 and 𝑉𝑚 = 𝑉𝑚
𝑐 𝑐

such that the sum of volume fractions is,

𝑉𝑚 + 𝑉𝑓 = 1

Weight Fractions to Volume Fractions. Relation between weight fractions and

volume fractions:

𝑉𝑓𝑖𝑙𝑙𝑒𝑟 𝑊𝑓𝑖𝑙𝑙𝑒𝑟 ρ𝑓𝑖𝑙𝑙𝑒𝑟

= =
𝑉𝑟𝑒𝑠𝑖𝑛 𝑊𝑟𝑒𝑠𝑖𝑛 ρ𝑟𝑒𝑠𝑖𝑛

6. Flame Retardancy

Flame Retardants. A flame retardant is an inorganic or organic molecule proven to

be useful in inhibiting flame growth by one of three mechanisms. Plastic combustion can

25
be stopped by the following mechanism: 1) inhibit combustion at flame front; 2) remove

heat from polymer; 3) prevent polymer decomposition / fuel release (Morgan, A., 2009).

General Flame Retardant Classes. There are three general flame retardant classes:

1) Gas Phase Flame Retardants- the reduction of heat from combustion is done by the

inhibition of combustion caused by the scavenging of free reactive radicals; 2)

Endothermic Flame Retardants- the polymer is cooled by the dilution of the fuel caused

by the release of non-flammable gases; 3) Char Forming Flame Retardants- thermal

insulation is provided by preventing fuel release. Carbonates belong to the second class

which is the endothermic flame retardants (Morgan, A., 2009).

Mineral Filler Flame Retardant. Calcium carbonate (CaCO3) is recognized as a

mineral filler flame retardant. Mineral filler FR is effective in lowering heat and smoke

release and is a green additive. In addition, mineral fillers have three quantifiable fire-

retardant effects: 1) heat absorption through endothermic decomposition; 2) increased

heat capacity of the polymer residue; 3) increased heat capacity of the gas phase through

the presence of water or carbon dioxide. Mineral filler FR are required in large loadings

of 50%- 80% weight ratio to obtain good FR performance (Morgan, A., 2009).

Calcium Carbonate Flame Retardancy Mechanism. The compound is non-

flammable and so it dilutes the amount of fuel consumed (Morgan, A., 2009). The fire-

retardant effect of calcium carbonate is through the endothermic decomposition:

CaCO3 → CaO + CO2

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The endothermic decomposition of the filler will increase the amount of heat needed to

vaporise the same amount of fuel, while the presence of gas phase flame diluents (in this

case carbon dioxide) will also tend to swell the flame, and reduce its temperature,

reducing the proportion of heat transferred back to the polymer (Hull, R., et.al., 2011).

Flammability Testing. The flammability of a polymer material depends

significantly on the formulation. As these materials are being utilized, the characterization

of their flame resistance becomes critical to ensuring safety (Marek, J. & Cooper, J., n.d.).

Test for Flammability of Plastic Materials for Parts in Devices and Appliances (UL

94/ ANSI 94) is to be employed in this research. ANSI 94 involve standard size specimens

and are intended to be used solely to measure and describe the flammability properties of

materials, used in devices and appliances, in response to heat and flame under controlled

laboratory conditions. The actual response to heat and flame of materials depends upon

the size and form, and also on the end-use of the product using the material. Assessment

of other important characteristics in the end-use application includes, but is not limited

to, factors such as ease of ignition, burning rate, flame spread, fuel contribution, intensity

of burning, and products of combustion (UL 94, 2000).

27
 Figure 8. Horizontal Burning Test for HB Classification.

Figure 9. Vertical burning test for V-0, V-1, V-2 classification.

According to the Standard Test Method ASTM D635 as referenced by ANSI 94,

the linear burning rate (V), in millimetres per minute, for each specimen where the flame

front reaches the 100 mm reference mark is calculated using the equation:

V=60L/t

where:

L = the burned length, in millimetres,

28
 t = the time, in seconds

7. Thermal Stability

Thermal Analysis. Thermal analysis is the analysis of a change in a property of a

sample, which is related to an imposed change in the temperature. The sample is usually

in the solid state and the changes that occur on heating include melting, phase transition,

sublimation, and decomposition (Shriver & Atkins, 2006).

Figure 10. Thermogravimetric analysis.

Thermogravimetric Analysis (ASTM E1131). The analysis of the change in the

mass of a sample on heating is known as Thermogravimetric analysis (TG). TG measures

mass changes in a material as a function of temperature (or time) under a controlled

atmosphere. Its principal uses include measurement of a material's thermal stability and

composition (Shriver & Atkins, 2006).

29
 Thermal Degradation. Thermal degradation of polymers is ‘molecular

deterioration as a result of overheating’. At high temperatures the components of the long

chain backbone of the polymer can begin to separate (molecular scission) and react with

one another to change the properties of the polymer (Zeus Industrial Products, 2005).

Differential Thermal Analysis. The most widely used thermal method of analysis

is differential thermal analysis (DTA). In DTA, the temperature of a sample is compared

with that of an inert reference material during a programmed change of temperature. The

temperature should be the same until thermal event occurs, such as melting,

decomposition or change in the crystal structure. In an endothermic event takes place

within the sample, the temperature of the sample will lag behind that of the reference and

a minimum will be observed on the curve. On the contrary, if an exothermal event takes

place, then the temperature of the sample will exceed that of the reference and a maximum

will be observed on the curve. The area under the endotherm or exotherm is related to the

enthalpy of the thermal event, ΔH.

8. Flexural Behavior

Flexural Strength. Flexural strength also known as modulus of rupture, or bend

strength, or transverse rupture strength. The flexural strength represents the highest stress

experienced within the material at its moment of yield. It is measured in terms of stress,

σ (Figure 2.4) (Hodgkinson, 2000). The formula for flexural strength is shown in the

figure below.

30
 Figure 11. Flexural strength as highest stress, σ, experienced.

Bending Stress. When a member is being loaded, bending stress (or flexure stress)

will result. Bending stress is a more specific type of normal stress. When a beam

experiences load, the top fibers of the beam undergo a normal compressive stress. The

stress at the horizontal plane of the neutral is zero. The bottom fibers of the beam undergo

a normal tensile stress. It can be concluded therefore that the value of the bending stress

will vary linearly with distance from the neutral axis.

Three-point Flexural Test. ASTM D-790- Flexural Properties of Unreinforced and

Reinforced Plastics and Electrical Insulating Materials. Flexural test (Figure 11) by

which a continuing increasing load is applied in the center of the sample until there is a

break or permanent bend in the material (Sciencing, 2018).

31
 Figure 12. Three-point flexural testing.

Load Deflection Curve. A graph (Figure 12) in which increasing flexural loads on a

beam are plotted along the vertical axis, and deflections resulting from these loads are

plotted along the horizontal axis.

Figure 13. Load Deflection Curve.

Proportional Limit. Highest stress at which stress is directly proportional to strain.

From the origin O to the point called proportional limit (Figure 13), the stress-strain curve

is a straight line.

32
 Figure 14. Proportional limit in stress-strain curve.

Modulus of Elasticity. Modulus of elasticity or Young’s modulus (Figure 2.9), E,

is a material property, that describes its stiffness and is therefore one of the most important

properties of solid materials. A stiff material has a high Young's modulus and changes its

shape only slightly under elastic loads (e.g. diamond). A flexible material has a low

Young's modulus and changes its shape considerably (e.g. rubbers). From the Hook’s law

the modulus of elasticity is defined as the ratio of the stress to the strain:

Figure 15. Stress-strain curve showing Young’s Modulus of elasticity.

33
9. Statistical Analysis

Independent T-test. The t-test assesses whether the means of two groups, or

conditions, are statistically different from one other. They are reasonably powerful tests

used on data that is parametric and normally distributed.

The independent t-test is used when you have two separate groups of individuals or

cases in a between-participants design (SAGE, 2017).

34
C. Conceptual Framework

Cleaning of Shells

Drying of Shells

Pre-Polymer Styrene Hardener Grinding of Shells

Polyester Resin Bio-Fillers from Tahong Shells

Mixing

Pouring into Molders

Curing of Sheets

Cutting into Specimens

Testing for Flame Testing for Thermal Testing for Flexural

Retardancy Stability Strength
UL 94 ASTM E1131 ASTM D790

Data Analysis

Figure 16. The Conceptual Framework.

35
 The material that will be utilized as bio-fillers in polyester matrix will be the green

mussel seashell particulates. For specimen to be produced, a designed molder will be

fabricated. After all the materials will be successfully gathered, the particulates will be mixed

with the Polyester using the high-speed mixer that will be assembled: 100% pure polyester

sheets; 80% bio-filled per weight polyester resin composite; 70% bio-filled per weight

polyester resin composite; and 60% bio-filled per weight polyester resin composite and 50%

bio-filled per weight polyester resin composite. Five specimens will be produced for each

set-up, five of which will be subjected to UL94 (Horizontal and Vertical), ASTM E1530 and

ASTM 790. The burning rate from UL 94 and temperature will be analyzed and interpreted

by spearman’s statistical test and the flexural strength will be compared with the set-ups.

calculations and conclusions will be then drawn.

36
 III. METHODOLOGY

A. Fabrication Procedures

Preparation of Green Mussel Shells Particulate Bio-Filler

1. The waste Green Mussel Shells will be washed with 4% sodium hydroxide solution for

48 hours (Fernandez, 2014).

2. Then, it will be further washed with distilled water.

3. After, it will be sun-dried for 12 hours.

4. Following the sun-drying, it will be crushed by hammering and will be grinded

thoroughly to achieve fine powdered particulates about ≤ 100 μm.

5. Finally, the fine powdered particulates will be dried in a laboratory oven.

6. The fine powdered particulates will be weighed (50%,60%,70%, 80% of resin weight)

as bio-fillers.

Preparation of Molder

1. Five (5) square molds with the dimensions 12” x 12” x 1/2” will be made from

aluminum steel sheets (Figure 17).

2. For ease of removal of the sheets, the molder will be designed in a way that the floor

plate is separated from the wall plates.

3. A locking mechanism will be attached to one side of the wall plates to ensure no leaking

of the mix. This spring form square pan will be a help in the removal of the specimen

without being subjected to stress.

37
 Figure 17. Molder Design (Top view and Isometric view, respectively).

Assembly of Mixer Set-up

1. The paddle agitator will be fabricated with a length of 80% of inside diameter and

width of 1/10 of length.

2. To achieve good mixing, a baffle will be added in the design of paddle agitator.

3. Standard shank size will be machined on the other end of the paddle agitator to be

attached directly to kitchen mixer.

4. Devised mixing container will be in a non-stick deep casserole.

5. Set-up (Figure18) will be comprised of a burner, non-stick deep casserole and the

paddle agitator powered by kitchen mixer.

38
 Figure 18. Mixing set-up.

Preparation of Sheets

1. The ratio of 20:10:1 for the pre-polymer, styrene and hardener, the resin mixture will

be prepared.

2. The fine powdered bio-fillers will be added to the mixture.

3. The mixture will be mixed by high-speed mixer until it will be homogeneous and will

be formed as Polyester.

4. The mixture will then be poured into the sheet molder measuring 12” by 12” by ½”.

5. A 10-kg block cement weight will be placed on top of the cover of the molder for 6

hours to ensure compactness of the sheets.

6. After 6 hours, the weight will be removed.

7. The sheets will then be removed from the molders and will be cured for 72 hours and

stored in a room above 20 degrees Celsius.

39
Preparation of Specimens

Specimen for UL 94 (Horizontal and Vertical Burning Test)

1. After curing, representative test specimen will be cut into (5” x 0.5” x 0.5”) in size,

from the 12” by 12” by ½” sheet.

2. For UL standard testing, ten (10) specimen each will be prepared for Horizontal

burning test and 20mm-Vertical burning test in four (4) varying set-ups and one (1)

controlled set-up.

3. Ten (10) spare specimens will be prepared incase additional trial will be needed if one

(1) condition in the UL standard conditions will not be met.

Specimen for ASTM E1131 (Thermogravametric Analysis)

1. For ASTM E1131, ten (10) representative test specimen will be cut (5” x 0.5” x 0.5”

in) in size.

2.. After cutting operation, specimens will be fine sanded and dusted to have a smooth

finish.

Specimen for ASTM D790 (Flexural Strength Testing)

Ten (10) representative test specimen will be cut in (125 x 25 x 6) mm in size.

40
B. Testing Procedure

For Flame Retardancy Testing

UL 94-HB Horizontal Burning Test

1. The specimen will be measured and marked with two lines perpendicular to the

longitudinal axis of the bar 25mm and 100mm referenced from the end that is to be

ignited (Figure 3.1).

2. Next, the specimen will be clamped at the end farthest from 25 mm reference in a

flexible specimen support fixture.

3. The Set-up will be enclosed in a laboratory hood.

4. The wire gauze will be clamped horizontally beneath the specimen with distance of

10mm from the lowest edge of specimen.

5. Away from the specimen, the Burner tube will be ignited and adjusted to stabilize a

20 mm- high blue flame until it reaches equilibrium.

6. The burner will be placed on the free end of the test specimen to a depth

approximately 6mm with an inclination approximately 45 degrees to the horizontal.

7. The flame will be applied and positioned steadily for 30s to the specimen.

8. The flame will be withdrawn when 30s or when 25mm reference mark is reached.

9. The time (s) will be recorded when the specimen continues to burn with flame or

glowing combustion even after flame is withdrawn, starting from the 25mm reference

mark to where the flame stopped.

10. The burned length (mm) will be recorded.

41
11. The procedure will be repeated until all five (5) specimens will be tested. An

additional set of five (5) specimen will be tested if one (1) specimen does not comply

the requirement.

Figure 19. Horizontal Burning Test for HB Classification.

UL 94-V 20mm Vertical Burning Test

1. The specimen will be clamped from the top, with the longitudinal axis vertical, so that

the lower end of the specimen is 300 mm above a horizontal (Figure 3.2).

2. The burner will be adjusted to produce a blue flame 20 mm high with a gas flow rate

of 105ml/min.

3. The flame will be applied centrally to the middle point of the bottom edge of the

specimen so that the top of the burner is 10 mm below that point of the lower end of

the specimen for 10 seconds.

4. After 10 seconds, burner will be immediately withdrawn at a rate of approximately

300 mm/sec, to a distance at least 150 mm away from the specimen.

5. Simultaneously to step 4, the flame time will be recorded t1 in seconds.

6. Procedure 4 will be repeated for the second flame application and third flame

application respectively. Then, the flame time will be recorded t2 and t3, respectively.
42
 Figure 20. Vertical Burning Test for V Classification.

For Flexural Strength Testing

Standard Test Methods for Flexural Properties of Unreinforced and Reinforced Plastics and

Electrical Insulating Materials D 790 – 03

1. Five (5) specimens for each set-up will be subjected to a Three-Point Flexural Test

with the use of a Universal Testing Machine.

2. In conducting the flexural test, it will be made sure that the specimen will be loaded

at the center of span with the load applied to the finished face.

3. A constant loading speed of 10 mm/s will be applied.

4. The load at proportional limit will be recorded every trial.

5. The stress at proportional limit for each trial will then be calculated and

summarized into an average value.

43
C. Post-Test Data Analysis

1. Horizontal Burning Test

Table 4.

Sample Data Table for ANSI/UL94.

Time for Time for

Time to
flame front to flame front to Burnt
Specimen travel Burning Rate
reach 25mm reach 100mm distance, L
Number distance, L (mm/minute)
mark mark (mm)
(seconds)
(seconds) (seconds)
1
2
3
4
5

Appendix X1 of the UL 94 specifies that the behavior of the specimens shall be

classified as HB if:

(a) There are no visible signs of combustion after the ignition source is removed,

or

(b) The flame front does not pass the 25 mm reference mark, or

(c) The flame front passes the 25 mm reference mark but does not reach the 100

mm reference mark, or

(d) The flame front reaches the 100 mm reference mark and the linear burning rate

does not exceed 40 mm/min for specimens having a thickness between 3 and 13

mm or 75 mm/min for specimens having a thickness less than 3 mm.

44
 Important to note that (1) If only one specimen from the first set of specimens does

not comply with the criteria indicated, another set of specimens is to be tested. All

specimens from this second set shall comply with the criteria indicated in order for the

material, of that thickness, to be classified as HB. (2) If the linear burning rate does not

exceed 40 mm/min when tested in the 3.0 mm thickness, the HB category designation shall

be extended to a 1.5 mm minimum thickness.

2. Vertical Burning Test

Table 5.
Example table results for 20mm- Vertical Burning Testing.

Specimen T1 T2 T3 Total Time Cotton Class

Number (seconds) (seconds) (seconds) (seconds) Ignition Rating
1
2
3
4
5
The following are to be observed and recorded:

a) Afterflame time after first flame application, t1.

b) Afterflame time after second flame application, t2.

c) Afterglow time after second flame application, t3.

d) Whether or not specimens burn up to the holding clamp.

e) Whether or not specimens drip flaming particles that ignited the cotton

indicator

45
 Table 6.

Material Classification.

Materials shall be classified V-0, V-1, or V-2 on the basis of results obtained on

small bar specimens when tested as described in the table above.

D. Ethical Considerations

This study on the influence of bio-fillers from waste green mussel shells to the

flame retardancy, thermal stability, and flexural behavior of polyester sheets, both its

fabrication and testing methods, did not involve any procedures that may violate

International Standards. No human beings and animals were harmed in the research

process. The research conducted was only concerned on the effectivity of the green mussel

shells as bio-fillers to the polyester sheets. This study did not cause any harm, destruction

46
or disturbance to the environment even more, it helps eliminate wastes by incorporating

them into the most commonly used material of mankind, the polymers.

47
 IV. REFERENCES

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on the flammability and mechanical properties of general-purpose polystyrene.

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Agency for Toxic Substances and Disease Registry (ATSDR). Toxicological Profile for Styrene.

U.S. Public Health Service, U.S. Department of Health and Human Services, Atlanta,

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Ashby, M. (2011). Materials selection in mechanical design. Cambridge, MA: Butterworth-

Heinemann. p. 40

Balzer, P. S., Becker, D. & Hamester, M. R. (2012). Characterization of calcium carbonate

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Butcher, G. D. & Miles, R. (1990). Concepts of Eggshell Quality. Institute of Food and

Agricultural Sciences, 69 1-2. Retrieved from https://edis.ifas.ufl.edu/vm013.

Callister W. and Rethwisch D. (2000). Fundamentals of Materials Science and Engineering: An

Integrated Approach. New York, NY: John Wiley & Sons, Inc.

Cayla, A., Giraud, S., Guan, J., Mandlekar, N., Malucelli, G., Rault, F., et al. (2018). An overview

on the use of lignin and its derivatives in fire retardant polymer systems. Lignin –

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Cowie, J.M.G. (1991). Polymers: Chemistry & Physics of Modern Materials (2nd ed.). New York:

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Das, S. B., Kamat, S. Y. & Mittal, P. K. (1981). Bromine & iodine content in sponges & algae of

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Dhokaliya, B. (2000). Unsaturated polyester resin for specialty applications. Unsaturated

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Fanfarova, A. and Maris, L. (2016).The reaction to Fire test for fire retardant and for combustible

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Friedrich K. and Breuer U. (2015) Fire retardants. Multifunctionality of Polymer Composites.

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Gilbert, M. (2016). Brydson’s Plastic Material.Cambridge, MA: Butterworth-Heinemann.

Guerra P. and Eljarrat M & et al. (2011). Brominated Flame Retardants. New York, NY: Springer.

Hull, T Richard, Witkowski, Artur and Hollingbery, Luke (2011) Fire retardant action of mineral

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Roylance, D. (2008). Mechanical properties of materials. New York, NY: John Wiley & Sons,

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50
 V. APPENDIX

Table 7.

Materials used in the procedures.

Material Used

Asian green mussel, is an

Green Mussel economically important mussel, a
Shells bivalve belonging to the family
Mytilidae

A supply of absorbent 100

Cotton
percent cotton.

General-purpose polystyrene is
Pre-polymer
clear, hard, and rather brittle.

51
 It is colorless oily liquid that
evaporates easily and known as
Styrene
ethenylbenzene, vinylbenzene,
and phenylethenea.

It is used simply to increase the

Resin Hardener resilience of the mixture once it
sets

Sodium 4% solution used as an

Hydroxide industrial cleaning agent where it
Solution is often called "caustic"

52
 Table 8.

Equipment used in the procedures.

Equipment Used

Chamber with an inside volume

Test Chamber of at least 0.5 m3
or Hood to be used when testing the
specimens.

laboratory type burner having a

Laboratory tube with a length of 100±
Bunsen Burner 10 mm and an
inside diameter of 9.5
±0.3 mm.

A metal support fixture for

testing specimens that are not
Flexible
self-supporting. It is with clamps
Specimen
or the equivalent, for horizontal
Support
or vertical
Fixture
positioning of the specimen
and/or the wire gauze.

53
 A supply of technical grade
methane gas (min. 98 percent
Gas Supply
pure) with regulator and meter for
uniform gas flow.

Mesh with approximately 20

Wire Gauze, openings per 25 mm, made with
20-mesh 0.43 ±0.03 mm diameter iron
wire and cut to approximately
125 mm squares.

Timer with accuracy to 0.5

Timing Device
second.

Micrometer capable of being read

Micrometer
to 0.01 mm.

54
55