DEPARTMENT OF POLYMER & PROCESS

ENGINEERING
University of Engineering & Technology, Lahore-Pakistan

FUNDAMENTALS OF
POLYMER ENGINEERING
PPE-102L
Laboratory Manual
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

Contents

1. INTRODUCTION ...................................................................................................... 2
1.1: LABORATORY ORGANIZATION ........................................................................ 2
1.2: CONDUCT OF STUDENTS IN LABORATORY ................................................... 2
1.3: LAB LOCATIONS ................................................................................................ 2
2. LABORATORY REPORTS ......................................................................................... 3
2.1: DATES FOR SUBMISSION ................................................................................. 3
2.2: SUBMITTING LABORATORY REPORTS ........................................................... 3
2.3: STRUCTURE OF LABORATORY REPORT ........................................................ 3
2.4: DATA PRESENTATION ....................................................................................... 4
2.4.1: GRAPHS ........................................................................................................ 4
2.4.2: TABLES ......................................................................................................... 4
3. OVERALL OBJECTIVES ........................................................................................... 5
4. COURSE LEARNING OUTCOMES (CLOs) ............................................................... 5
5. LIST OF EXPERIMENTS ............................................................................................ 6
6. WEEKLY SCHEDULE ................................................................................................ 7
7. REFRENCES ............................................................................................................ 10
8. EXPERIMENTS……………………………………………………………………………..11
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

1. INTRODUCTION

1.1: LABORATORY ORGANIZATION

You will perform 09 laboratory exercises for this course. All of these experiments will be
written up as a report according to the questionnaires and guidelines provided. This
booklet contains the scripts for all of the lab exercises. You need to have read the
relevant script before beginning a laboratory exercise.
You can improve your chance of receiving high marks for a lab exercise by planning
ahead. This will allow you to:
• Prepare tables to record data.
• Plan graphs that need drawing.
• Prepare questions to ask during laboratory session.

1.2: CONDUCT OF STUDENTS IN LABORATORY

• No smoking, eating or drinking in the laboratory for reasons of health and safety.
• Students are responsible for leaving the apparatus in good condition and the bench
should be clean and tidy. At the end of the practical work one student from each
experimental group will report to the Laboratory Technician, who will check and record
that this has been done.
• Appropriate clothing, including laboratory coat, should be worn at all times.

1.3: LAB LOCATIONS

The various laboratory exercises for this semester take place in a range of locations.
Make sure that you know where to go in plenty of time before the labs. The location of
each laboratory exercise is indicated on the top of their scripts.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

2. LABORATORY REPORTS

2.1: DATES FOR SUBMISSION

Laboratory reports must be submitted within 2 weeks of completing a lab class. After
submission time had passed the reports can only be entertained with prior permission
from Departmental Chairman.

2.2: SUBMITTING LABORATORY REPORTS

All laboratory reports are to be submitted in printed copy.

Both Reports and Questionnaires: 2 weeks after lab session.
Digital copies of the lab reports are to be submitted at the end of semester before final
viva voce.

2.3: STRUCTURE OF LABORATORY REPORT

The laboratory report must use a consistent template and formatting. A typical structure
of laboratory report is given below:
1) Abstract (75-120 words – summary of work done and the main findings).
2) Introduction
3) Experimental – refer to the Lab Sheet for experimental and do not reproduce this in
the text
4) Results and discussion – full presentation of data derived (tables or graphs).
Attempt to assess errors and statistical significance, whenever possible.
Discussion of results and interpretation. As a rule you should make sure that the points
covered in the questionnaire are covered in the full report
5) Conclusions
6) References
The laboratory report must contain table and figure captions with proper formatting.
Examples of calculations should be put into an appendix that appears at the end of
report. The appendix will be used to check the calculations.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

2.4: DATA PRESENTATION

2.4.1: GRAPHS

To gain full marks a graph must meet the following criteria:

 The axes range covers data set without leaving large regions with no data
 The axes are correctly chosen between Linear/log axes
 The label step size is suitable (e.g. in steps of 10 for a range from 0 to 50).
 Correct SI prefixes are used so that the numbers are in a sensible range.
 The varied parameter is on the xaxis and the measured/calculated quantity is on
the yaxis.
 The axes are labelled correctly with suitable name and correct units.
 The data points (and accompanying error bars where appropriate) are clear.
 Any trend line or fit to the data is physically meaningful—e.g. no trend lines
(unless a request has been made for one in the questionnaire).
 All the data sets requested have been plotted.
 No unnecessary decorations such as gridlines have been included.
 A suitably descriptive caption is provided—this is compulsory in reports and may
be requested in questionnaires.

2.4.2: TABLES

• To gain full marks a table must meet the following criteria:

• Headings are clear.
• The units are included.
• SI multipliers are used so that the numbers are in a sensible range.
• The errors associated with average values are presented.
• The data are presented in columns not rows.
• Where appropriate the data have been calculated correctly.
• In a report a suitable descriptive caption is included.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

3. OVERALL OBJECTIVES

There are 09 practical’s in the laboratory rotation covering the testing techniques of
Melt flow indexer, Hardness meter/durometer, Rheometer, Melting point apparatus,
Falling ball impact tester, Density meter, Flowmeter and tensile testing. On completion
of the practical sessions the student should be able to (for each technique):
• Describe the operation of the instrumentation.
• Discuss the underlying principles.
• Understand the data that can be obtained and how it is analyzed.

4. COURSE LEARNING OUTCOMES (CLOs)

 The students should be able to demonstrate the theoretical knowledge and

technical skills in the performance of polymer testing of Melt flow indexer,
Hardness meter/durometer, Rheometer, Melting point apparatus, Falling ball
impact tester, Density meter, Flowmeter and tensile testing. (Specialized
Knowledge/Applied Learning)
 The students should be able to demonstrate mathematical, statistical and error
analysis and develop ability to interpret and report analytical data and establish a
valid route for solving problems. (Critical Thinking)
 The student should be able to communicate the knowledge gained during the lab
sessions effectively with fellow students, laboratory personnel, research staff,
and the class tutor. (Communication Fluency)
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

5. LIST OF EXPERIMENTS

1. To determine the hardness of the given polymer (LDPE and HDPE) and rubber
specimens (NBR, NR and SBR) using hardness meter / durometer
2. To determine the melt flow rate of PP and ABS using melt flow indexer
3. To determine the melting point of the given polymeric materials (PP, ABS, PS
and HDPE) using melting point apparatus
4. To determine the impact strength of different plastic sheets (PET,LDPE, PP and
HDPE) through falling ball impact tester
5. To determine the viscosity of gelatin suspensions as a function of temperature
and RPM on a rheometer
6. To determine the moisture content in ABS, PMMA, Nylon 6 and PS using
brabender AQUATRAC moisture meter
7. To determine the mechanical behavior of common thermoplastics in terms of
their modulus, strength and elongation through tensile testing
8. To determine the flow characteristics of given polymeric materials (PS, Nylon 6,
ABS, TPU, PP and HDPE) using fluometer
9. To determine the density of HDPE, PPVC, UPVC, PPRC, LDPE and PET
specimens by displacement method
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

6. WEEKLY SCHEDULE

Week Plan
Week Activity CLO
1  Introduction to Fundamental of Polymer Engineering CLO2
Laboratory
 Brief description of Laboratory Equipment
 Rules and regulations for laboratory conduct
 Safety instructions
 Laboratory organization
 Laboratory report writing
 Preparation of lab layout

2  Data presentation for laboratory report CLO2,

 Introduction to American Standard for testing Materials
(ASTMs)
 Assignment 1: Collect American standard for testing
materials (ASTM) for each of the equipment included in this
lab. Each group should have a copy of all ASTMs with them
during laboratory session.

3 
Importance of Fundamental of Polymer Engineering CLO1,
Laboratory
CLO2
 Utilization of Laboratory Equipments in the industry
 Overview of American standard for testing materials (ASTM)
for each of the equipment included in this lab
 Assignment 2: Collect and submit material safety data
sheets/property sheets and manufacturer name for each of
the polymeric specimens used in experimentation.
4-7 Experimentation and report submission CLO1,
1. To determine the hardness of the given polymer (LDPE and
CLO2,
HDPE) and rubber specimens (NBR, NR and SBR) using
hardness meter / durometer CLO3
2. To determine the melt flow rate of PP and ABS using melt
flow indexer
3. To determine the melting point of the given polymeric
materials (PP, ABS, PS and HDPE) using melting point
apparatus
4. To determine the impact strength of different plastic sheets
(PET,LDPE, PP and HDPE) through falling ball impact tester
5. To determine the viscosity of gelatin suspensions as a
function of temperature and RPM on a rheometer
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

6. To determine the moisture content in ABS, PMMA, Nylon 6

and PS using brabender AQUATRAC moisture meter
7. To determine the mechanical behavior of common
thermoplastics in terms of their modulus, strength and
elongation through tensile testing
8. To determine the flow characteristics of given polymeric
materials (PS, Nylon 6, ABS, TPU, PP and HDPE) using
fluometer
9. To determine the density of HDPE, PPVC, UPVC, PPRC,
LDPE and PET specimens by displacement method
Assignment 3:
(a) Prepare and submit in electronic form a detailed report on
measurement of electrical properties of polymers such as
Dielectric strength, dielectric constant and dissipation factor
(b) Prepare and submit in electronic form a detailed report on
weathering properties of polymers and also describe the
accelerated weathering and out-door weathering testing of
polymers
8 Examination Week CLO1,
CLO3
9-13 Experimentation and report submission CLO1,
1. To determine the hardness of the given polymer (LDPE and
CLO2,
HDPE) and rubber specimens (NBR, NR and SBR) using
hardness meter / durometer CLO3
2. To determine the melt flow rate of PP and ABS using melt
flow indexer
3. To determine the melting point of the given polymeric
materials (PP, ABS, PS and HDPE) using melting point
apparatus
4. To determine the impact strength of different plastic sheets
(PET,LDPE, PP and HDPE) through falling ball impact tester
5. To determine the viscosity of gelatin suspensions as a
function of temperature and RPM on a rheometer
6. To determine the moisture content in ABS, PMMA, Nylon 6
and PS using brabender AQUATRAC moisture meter
7. To determine the mechanical behavior of common
thermoplastics in terms of their modulus, strength and
elongation through tensile testing
8. To determine the flow characteristics of given polymeric
materials (PS, Nylon 6, ABS, TPU, PP and HDPE) using
fluometer
9. To determine the density of HDPE, PPVC, UPVC, PPRC,
LDPE and PET specimens by displacement method
Assignment 4:
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

(a) Prepare and submit in electronic form a detailed report on

measurement of Optical properties such as Refractive index,
luminous transmittance, haze and gloss
(b) Prepare and submit in electronic form a detailed report on
measurement of Chemical properties of polymers by Immersion
tests and describe solvent stress-cracking resistance and
environmental stress-cracking resistance of polymers

14 Viva and Assignment Submission CLO1,

CLO3
15 Quiz 2 CLO1,
CLO3
16 Final Laboratory Marks Distribution and discussion with students on CLO3
their grades
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

7. REFRENCES

Textbooks:
1. Christopher S. Brazel, Stephen L. Rosen, Fundamental Principles of Polymeric
Materials, Third Edition, John Wiley & Sons, Inc., 2012 (ISBN-13: 978-0470505427)

2. Alberto Naranjo et. al., Plastic Testing and Characterization: Industrial Applications,
Carl Hanser Verlag, Munich, 2008 (ISBN-13: 978-1569904251)

Reference book:
3. Vishu Shah, Handbook of Plastics Testing and Failure Analysis, Third Edition, John
Wiley & Sons, Inc., 2007 (ISBN-13: 978-0471671893)
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the hardness of the given

polymer (LDPE and HDPE) and rubber
specimens (NBR, NR and Neoprene
Rubber) using hardness meter/durometer

Fig.1: Hardness Meter

INTRODUCTION
The term hardness has been applied to scratch resistance and to rebound resilience, but
for polymers it is taken to refer to a measure of resistance to indentation. The mode of
deformation under an indenter is a mixture of tension, shear, and compression, and
hardness is by no means a fundamental property. The result depends on the indenter
geometry and the degree of indentation as well as the time of indentation after which the
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

measurement is made. Regardless of the arbitrary nature of the test, it is attractive

because of its cheapness and apparent simplicity.

Although hardness tests are applied to most classes of polymer materials, they are far
more common or important for some materials than for others. Hardness is almost
inevitably included in properties of rubbers, fairly often for plastics, and only rarely for
composites. With cellular materials a test more equivalent to compression stiffness is
termed hardness, while the indentation of fabrics is not practical. Because of the range of
stiffness involved across these materials, the methods applied vary considerably.

ARRAY OF HARDNESS TEST METHODS

The Rockwell Hardness Test and Superficial Rockwell are performed on castings,
forgings and other relatively large metal products and samples because the tests produce
a large visible indentation.

The Brinell Hardness Test can be applied to almost any metallic material and is the
method most commonly used to test castings and forgings that have a grain structure too
coarse for other hardness testing methods.

Microhardness testing by Knoop and Vickers Hardness Test methods measure

small samples or small regions in a sample. They are often used to measure surface or
coating hardness on carburized or case-hardened parts, as well as surface conditions
such as grinding burns or decarburization. (Vickers is also available on the macro scale
to 50 kg.)

The Shore Durometer Test measures the hardness of polymeric materials. Hardness
testing of polymeric materials, including plastics and rubbers, is performed by the Shore
Durometer Test according to ASTM D2240. Like the hardness tests for metal, this method
determines a material’s hardness value or resistance to indentation by penetration of an
indenter into the test sample. Hardness can be defined as a material’s resistance to
permanent indentation and Durometer is one of several scales used to measure
hardness. The most common instrument for measuring rubber hardness is called a Shore
durometer. A spring is used to push a metal indenter into the surface of the material,
measuring how far it penetrates. The instrument measures the depth penetration from
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

zero to 0.100 inches. A zero reading on the scale means the indenter is at the maximum
depth and a reading of 100 indicates that no penetration was detected. Shore durometers
come in a variety of hardness ranges. The Shore A scale uses a blunt indenter with a
moderate spring force. Shore A instruments are not as accurate when readings are above
90, so for harder materials, the Shore D durometer is used, as it has a sharp indenter and
a stronger spring to penetrate to a greater depth.

Fig. 2: A typical shore hardness scale for polymeric and rubber specimens

SPECIMENS
Molded articles of LDPE, HDPE, Natural Rubber, Nitrile Butadiene Rubber and Neoprene
Rubber

ASTM
D2240-10: Standard Test Method for Rubber Property—Durometer Hardness

PROCEDURE

Shore D Measurements
Measure the thickness of LDPE and HDPE molded specimens using thickness gauge.
Switch on the electronic console. Select the test code, measurement time and type of
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

hardness. Place the sample to be tested on the plain surface. Put the testing unit on the
sample in a vertical position. Wait until the sound of the console that the test time has
been passed and the hardness value has been stored. Record the reading on the display
and take eight readings to calculate the standard deviation.

Shore A Measurements
Measure the thickness of Natural Rubber, Nitrile Butadiene Rubber and Neoprene
Rubber molded specimens using thickness gauge. Place the sample to be tested on the
plain surface. Put the testing unit on the sample in a vertical position. Wait until the dial
of the console is stable. Record the reading on the display and take eight readings to
calculate the standard deviation.

QUESTIONARE
1: Tabulate the thickness of the given polymeric and rubber specimens along with their
average values and standard deviations

2: Tabulate the measured hardness values of the given polymeric and rubber specimens
along with their average values and standard deviations

3: Plot the thickness against the measured hardness for rubber specimens.

4: During testing, which specimen exhibited the highest hardness values? Explain?

5: Explain the relationship between hardness and tensile strength values for polymers.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the Melting Point of the

given polymeric materials (PP, ABS,PS and
HDPE) using Melting Point Apparatus.

Fig. Melting point apparatus

INTRODUCTION
Melting point apparatus is used for melting point determination of different materials. The
melting point value can be used to identify a substance and to get an indication of its
purity. The melting point of a solid is the temperature at which the solid exists in
equilibrium with its liquid state under an external pressure of one atmosphere. Both the
melting point range (the interval between the beginning of liquefaction and complete
liquefaction) and the temperature of complete liquefaction are valuable indicators of the
purity of the solid compound. A pure crystalline organic compound usually possesses a
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

sharp melting point and it melts completely over a narrow temperature range. The
presence of even small amounts of impurities usually produces a depression of the
temperature at which melting is complete and usually produces a marked increase in the
width of the melting point range. A wide melting point range usually indicates that a
substance is impure.

Two basic methods are used for melting point determination. For the first method, a
Fisher–Johns melting point apparatus is most commonly used. The apparatus consists
of a rheostatically controlled heated block, a thermometer, and a viewing magnifier. A
small pellet or a sliver of the plastic material to be tested is placed on the electrically
heated block along with a few drops of silicone oil. A cover glass is placed over the
material and the heat is gradually increased until the sample material melts or softens
enough to deform. The meniscus formed by the oil is viewed through the magnifier. The
temperature at which the meniscus moves is considered the melting point. The expected
accuracy of the test is within ±5°F of the published literature value. This method can be
used for both crystalline and amorphous plastics. All crystalline plastics have a sharp
melting point and the transition is much easier to detect. In contrast, amorphous plastics
melt over a wide range and an exact melting point is difficult to determine.

The second method, known as the Kofler method, is used only for semi-crystalline
polymers. It consists of heating the sample by hot-stage unit mounted under a microscope
and viewing it between crossed polarizers. When crystalline material melts, the
characteristic double refraction from the crystalline aggregates disappears.

The point at which the double refraction or birefringence (typically a rainbow color)
completely disappears is taken as the melting point of the polymer. The use of a control
sample for comparison is particularly helpful in both methods.

SPECIMENS
Pellets of PP, ABS and HDPE
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

PROCEDURE
Switch on the apparatus. Find out the heating rate of plate. Take a reference temperature
i.e. 80oC or 90oC.Place the sample on hot plate of apparatus. Continuously monitor the
sample through lens. When the sample starts to diffuse, note the softening temperature.
When the color of sample starts to change, note the temperature. When the sample is
completely melted, note the temperature. This will indicate the melting point of sample.
Pick up the molten sample with pin. After removal of molten sample, wait until the
temperature reaches the reference value then place the second sample. Repeat the same
procedure for each provided sample.

PRECAUTIONS
Make sure that lid is properly cleaned before starting the test. Use a very small sample if
solid then 2-3 grains. Note the temperature carefully. Do not touch the lid with your hand
during test.

QUESTIONNARE

1) Find out the heating rate of melting point apparatus heating plate.

2) Tabulate the melting point of materials.

3) Report the state of the material’s corresponding temperatures for given materials;
three states are softening, color change and molten state.

4) Explain the significance of melting point apparatus in polymer process industry.

5) In a polymer process industry explain the main drawbacks of using the melting
point apparatus.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the density of HDPE, UPVC,

PPVC, LDPE, PPRC and PET specimens by
displacement method

Fig. Density Meter

INTRODUCTION
The density of plastic materials is defined as the weight per unit volume and is expressed
in grams per cubic centimeter or pounds per cubic foot. Specific gravity is defined as the
ratio of the weight of the given volume of a material to that of an equal volume of water at
a stated temperature. The temperatures elected for determining the specific gravity of
plastic parts is 23°C.

Specific gravity values represent the main advantage of plastics over other materials,
namely, light weight. All plastics are sold today on a cost per pound basis and not on a
cost per unit volume basis. Such a practice increases the significance of the specific
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

gravity considerably in both purchasing and production control. Two basic methods have
been developed to determine specifi c gravity of plastics depending upon the form of
plastic material. Method A is used for a specimen in forms such as sheet, rods, tubes, or
molded articles. Method B is developed mainly for material in the form of molding powder,
flakes, or pellets.

Method A

This method requires the use of a precision analytical balance equipped with a stationary
support for an immersion vessel above or below the balance pan. A corrosion-resistant
wire for suspending the specimen and a sinker for lighter specimens with a specific gravity
of less than 1.00 are employed. A beaker is used as an immersion vessel.

The test specimen of any convenient size is weighted in air. Next, the specimen is
suspended from a fine wire attached to the balance and immersed completely in distilled
water. The weight of a specimen in water (and sinker, if used) is determined.

SPECIMENS
Molded articles of HDPE, UPVC, PPVC, LDPE, PPRC and PET

ASTM
ASTM D792 -13 -Standard Test Methods for Density and Specific Gravity (Relative
Density) of Plastics by Displacement

PROCEDURE
1: Collect the specimens given in the form of small molded articles.

2: Identify the specimens according to the color and opacity, specify the color and
opacity in your report.

3: Turn on the balance.

4: Press REF to enter density mode.

5: Measure the weight of specimen in air and then measure the weight of specimens in
liquid.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

USE WATER FOR PS AND PVC AND TOULENE FOR HDPE MOLDED ARTICLES

6: The specific gravity of the plastic materials can be calculated by using formula;
𝑎
𝑆𝑝. 𝑔𝑟. 23/23°𝐶 =
(𝑎+𝑤−𝑏)
Where,

a = apparent mass of specimen in air.

b = apparent mass of specimen in liquid.

w = apparent mass of totally immersed sinker (if used) and of partially immersed wire.

Density of samples (whose individual values are less than 1 g/cm3) can be measured by
using formula

𝐷23𝑐 , 𝑔/𝑐𝑚3 = 𝑠𝑝 𝑔𝑟 23/23°𝐶 × 0.866

QUESTIONNARE
1) Tabulate the density of the three specimens and compare the values with those
given in literature.
2) Explain other methods used for the measurement of density of polymers and
metals.
3) How density variation in a molded article can affect their performance, explain.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the mechanical behavior of

common thermoplastics in terms of their
modulus, strength and elongation through
tensile testing

Fig. Universal Testing Machine (UTM)

INTRODUCTION
Tensile tests of polymers are generally carried out to measure the force required to break
a specimen and the extent to which the specimen elongates before that breaking point.
All tensile tests produce a force displacement diagram, which can be used to produce a
stress-strain curve from which various properties such as Young’s modulus, yield
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

strength, ultimate tensile strength can be calculated for design and research. These data
points are often used to specify a material, to design parts to withstand application force
and as a quality control check of materials.

SAMPLE PREPARATION
Cut the testing sample according to the supplied cutting mold of dumbbell shape

ASTM
D638-08-Standard Test Method for Tensile Properties of Plastics

PROCEDURE
1. Check safety parameters for the load cell on the vertical sported column.
2. Check safety button.
3. Switch on the computer and machine power supply.
4. Start the software from the desktop’s icon TIRA.
5. Get the sizes of the testing sample (Dumbbell Shape) manually with vernier calliper
& thickness measuring gauge.
6. Thickness = a (in mm)
7. Width = b (in mm)
8. Gauge length = l (in mm)
9. Press the setting button on the main tool bar. A “Test Setting” dialog box with
different tabs.
10. Insert sample data by selecting “TEST DATA” tab. i.e. Material, Batch Number.,
Order Number etc.
11. Insert sample dimensions by selecting “DIMENSIONS” tab. i.e. Thickness, Width,
and gauge length in given boxes “a”, “b” and “l” respectively.
12. Insert rate of the test sample by selecting “TEST RATE” tab.
13. Similarly check the other tabs to insert the specific data concerning machine
operation.
14. Load the sample in jaws as follows:-
15. Press down the jaw clamping leaver and insert the sample from clamping area.
16. Move down the upper jaw to clamp the other side of the sample into the lower jaw
by using manual controls from panel.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

17. On software window screen, ZERO the Cross head Position, Force, and length by
pressing the button on main tool bar.
18. Select the Axis Parameters by pressing the button of “DIAGRAM AXIS” on the
main tool bar. Also change the diagram name from Manu Bar i.e. Diagram-Setting.
19. Start the test by pressing “START” button on main tool bar.
20. After completion of test, save the test result by pressing “SAVE” Button on the main
tool bar, with the desired file name or path.
21. Get off the test sample pieces from the clamping jaws. Exit from the software
properly and shut down the computer as well.
22. Power off the whole system from electric supply properly in the end.

QUESTIONARE
1) Tabulate the ultimate tensile strength, elongation at break, yield strength and
modulus of specimens along with the respective standard deviation values.
2) Draw the stress vs elongation curve for each of the specimens.
3) Explain the difference between the mechanical behavior of ductile, brittle and
elastomeric polymer materials.
4) Explain the effect of temperature change on the mechanical behavior of polymers.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the melt flow rate of PP and

ABS specimens by using MELT FLOW
INDEXER.

Fig.1: Melt flow indexer

INTRODUCTION
A familiar form of tube flow testing is the melt index test (MI, MFI, and MFR), which
measures the rate of extrusion of a molten material through an orifice of specified length
and diameter under a prescribed temperature and load.

The melt index generally correlates inversely to the molecular weight of a material. High
molecular weight materials have a low MI and low molecular weight materials have a high
MI. Extrusion, thermoforming, and blow molding grades normally have low MI’s. Injection
molding and fiber grades have high MI’s. Melt Flow extrusion plastometer can be used to
determine the melt mass flow rate (MFR) and melt volume flow rate (MVR). Flow Rate
measures the rate of extrusion of thermoplastics through an orifice at a prescribed
temperature and load. It provides a means of measuring flow of a melted material which
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

can be used to differentiate grades of polymers, or determine the extent of degradation

of the plastic as a result of molding. Degraded materials would generally flow more as a
result of reduced molecular weight, and could exhibit reduced physical properties. Melt
flow quantities are used to designate grades of materials. Data are reported in grams of
extrudate per 10 minutes or in decagrams per minute.

ASTM D1238 lists specific loads and temperatures for a given material. For example,
polypropylene requires 230 °C and 2.16 kg load, while polycarbonate requires 300 °C
and 1.2 kg load. The conditions are chosen to generate a relatively low shear rate. The
shear rate should be reasonably low enough to be strongly influenced by molecular
weight and less influenced by molecular weight distribution. Consequently, the melt flow
index is routinely used to classify commercial materials according to their molecular
weight.

Fig.2: Schematic Diagram of Melt flow indexer

SPECIMENS
Pellets of ABS and PP
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

ASTM
D1238 – 13: Standard Test Method for Melt Flow Rates of Thermoplastics by Extrusion
Plastometer

PROCEDURE
Note the temperature and load conditions for the given sample from the literature. Set the
temperature of the barrel at a required value, inset the plunger into the barrel and give 15
-20 minutes to achieve the set temperature. Close the knob at the discharge so that there
will be minimum heat loss. Remove the plunger and introduce 4-5 g of material into the
hot chamber. Replace the plunger and load then wait until the temperature display shows
the constant set value. Open the knob at bottom and note the time taken by the material
to flow between the two specific marks on the plunger. Measure the weight of the material
that flow out of die when plunger plus weight move between the specific marks. Convert
the weight into g/10 mints to get the MFR of the material.
The melt flow rate (MFR) is calculated by using the following equation:

𝒕𝒓𝒆𝒇 × 𝒎
𝑴𝑭𝑹 =
𝒕

Where:
m = the average mass of the cut-offs in g
tref = the factor used to convert grams per second into grams per 10 min. which is 600s
t = cut off time interval in seconds

PRECAUTIONS
Properly clean the barrel before each test .Give sufficient time to plunger inserted into the
chamber to attain the required temperature. Keep the material under load into the
chamber until the temperature display shows a constant reading.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

QUESTIONARE
1) Tabulate the results along with the conditions for PP and ABS.
2) Using standard deviation calculations, illustrate the variations in the experimental
data.
3) Using mathematical derivation, illustrate how the values of given load can be
transformed into their corresponding pressure values?
4) Illustrate using examples how the MFI values are used for quality control or
material supply chain management in industry?
5) Explain using examples the significance and uses of MFI values in polymer
processing industry?
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

Appendix 1

Reference marks on the piston

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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the Water contents in ABS,

Nylon 6, PMMA and PS using brabender
AQUATRAC moisture meter

Fig. 1: AQUATRAC brabender Moisture Meter

INTRODUCTION
The AQUATRAC brabender Moisture Meter is used to measure the water contents in
polymers. The measurement of water content of plastics should take place fast and be
simple to accomplish. The AQUATRAC measures the humidity content in granular
materials and is readily deployed in the plastic processing industry. It is durably and
compactly designed and can be easily transported thus it can be used directly at the
production place. As an absolute measurement it does not require calibrations for
different substances. The sample weight is high so repetitive experimentations are not
required.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

THEORY
In the AQUATRAC the moisture from the sample under test reacts with a reagent,
generating hydrogen in addition to other products. The gas pressure is the original
indication of this ‘manometric’ method. The reagent is calcium hydride in granules of
0.5….5 mm, the reaction with water being according to the formula

CaH2 + 2 H2O Ca(OH)2 + 2H2

The generated product calcium hydroxide Ca(OH)2 can be seen as pale grey powder on
the surface of the reagent. At medium temperatures hydrogen is not very reactive, in
consequence interfering reactions with the substance under test should not be expected.

Calcium hydride as well as calcium hydroxide are not toxic, but avoid contact with open
flames, ingestion and contact with mucous membranes.

In the AQUATRAC 40 mg of water are necessary to obtain full scale, as this corresponds
to a pressure of appox. 450 mbar in the system. The sample weight is fed into the
instrument via switches, the result in % water content being calculated.

The water will be evaporated from the substance under test by means of temperature and
vacuum. The water vapour penetrates the granular reagent, which is situated in a mesh-
based insert above the sample. There the reaction takes place and generates the gas.
The partial pressure of the water vapour in the system is finally zero, hence also
hygroscopic substances will release their moisture completely.

TYPES OF PRODUCT
The water content in granulated plastics shall be determined. The reason for this limitation
to granules is, that large sample volumes of mainly 40 g are used. The air between the
particles permits the water vapor from the lower part of the sample to reach the reagent.

The limitation is not necessary when there are only small samples ( max. 10 cm 3).
Therefore it is possible to test powder with a density of 1 in a sample of 10 g. The height
of the sample will be so small, that the released vapour will come into contact with the
reagent.
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

For the same reason moldings can be measured when the wall thickness is sufficiently
small, that the release of water does not take too long a time. This means that the
AQUATRAC can be used to test parts in Polyamide after conditioning, but because of the
rather high water content, the sample weight will be small.

Table 1: Material Temperature Data for AQUATRAC moisture meter

MATERIAL ABBREVIATION TEMPERATURE
Acrylonitrile-butadiene-styrene ABS 130o
Ethylene-vinyl-acetate EVA 105
0

Ethylene-vinyl-acetate Cross linked EVA 130

0

Polyamide 6 PA6 130/160

0

Polyamide 6 GF 30 PA6GF30 160

0

Polyamide 6.6 PA 6.6 160

0

Polyamide 12 PA 12 130
0

Polyacryletherketone PAEK 160

0

Polybutene-terephtalate PBTP 160

0

Polycarbonate PC 160
0

Polyester PET 160

0

Polyester-elastomer TPE 160

0

Co-polyester PETG 105

0

Polyether-block amid PEBA 130

0

Polyehterimide PEI 160

0

Polyethylene HDPE 130

0

Polyethylene LDPE 105

0

Polyethylene-terphtalate PETP 160/190

0

Polymerblends PC/PET 160

0

Polymethyl-methacrylat PMMA 160

0

Polyoxymethylene POM 130

0

Polyphenylenether PPE 160

0

Polyphenyleoxide .polyamide PPO/PA 160

0

Polypropylene PP 130
0

Polystyrene PS 105
0

Polysulphone PSU 160

0

Polyurethane TPU 130/160

0

Talcum 160
0

Titandioxide TiO2 105

0

Aluminiumhydroxyde AlOH3 105

0
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

SPECIMENS
Granules of ABS and PS

Fig.2: Schematic diagram of AQUATRAC brabender Moisture Meter

PROCEDURE
Connect AQUATRAC with power supply and press button. Ensure the audible alarm is
switched on. If not done before, perform preliminary run, but without sample material.
After this preliminary run the instrument is ready for first test, when it has cooled down.
This is indicated by the intermittent light above the temperature keys, which shows the
action on the temperature controller, provided the green 500C key is actuated. Aerate the
measuring system by depressing the red button. Open the reaction container by
untwisting the locking handle and sweep back the bracket of the cover. Take out the
sample container by hand or by means of tongs and place it on the table. Take out the
mesh based insert and empty the old reagent of the preliminary run into a suitable
container. Fill the insert with new reagent. The required quantity obtained by using the
33
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

measuring scoop, filled to the brim. The bottle with the reagent has to be closed
immediately to avoid carryover of moisture by ambient air. Put the weighed sample into
the sample container. Put the insert on top of the sample container. Insert the prepared
container into the reaction chamber.

QUESTIONNARE
1. Tabulate the moisture content of the specimens along with standard deviation
values.
2. Explain the significance of using a moisture meter in a polymer process industry.
3. What are the drawbacks of using Brabender Aquatrac moisture meter?
4. What are the other ways of finding the moisture content of polymer materials?
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the impact strength of

different plastic sheets (PET, LDPE, PP and
HDPE) through falling ball impact tester

Fig. 1: Falling Ball Impact Tester

INTRODUCTION
The impact properties of the polymeric materials are directly related to the overall
toughness of the material. Toughness is defined as the ability of the polymer to absorb
applied energy. The area under the stress–strain curve is directly proportional to the
toughness of a material. Impact energy is a measure of toughness. The higher the impact
energy of a material, the higher the toughness and vice versa. Impact resistance is the
35
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

ability of a material to resist breaking under a shock loading or the ability to resist the
fracture under stress applied at high speed.

The falling dart, drop impact, or Gardner impact test employs a free falling weight that
strikes a plastic sample at rest.

Fig. 2: Falling dart, drop impact, or Gardner impact test

The energy required to rupture the sample is determined from the weight of the impacting
device and the height from which it was dropped. The impact energy is calculated by
multiplying the weight by the drop height. It is usually expressed in Joules (in.-lbf).

The test is normally conducted by raising a weight to a desired height and allowing it to
free-fall on a striker that is resting on a flat sample. The striker transfers the energy to the
sample. The kinetic energy transferred by the falling weight at the instant of impact is
equal to the energy used to raise the weight to the drop height. This is equivalent to the
potential energy possessed by the weight as it is dropped. The mean failure height is
determined from a statistically significant number of drops that will result in failing of 50%
36
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

of the specimens. From this the mean failure height, the impact energy, is calculated
(mass × gravity × height). This technique for determining the mean impact energy is called
the Bruceton Staircase Method or Up-and-Down Method.

Falling weight impact results are dependent on the geometry of the falling weight, striker,
and support. In addition, it is dependent on the sample configuration and the preparation
methods. As a result, impact testing should be used only to compare and rank materials.
Impact values from this technique cannot be considered as absolute.

The desired approach is to use equipment and test specimens that conform to the
intended end use of the material. Data obtained from different geometries cannot be
compared directly to each other.

SPECIMENS
Molded sheets of PET, PP, LDPE and HDPE

PROCEDURE
Prepare the sample of PET according to the conditions given in ASTM D5420. There
should be no air bubbles or molding defects in your prepared specimen as it will affect
the value of impact testing. Now raise the ball in the column to a certain height. Place the
specimen at the impact spot. Drop the ball carefully on the specimen. Examine the
specimen to check whether a crack appears on this height or not. If a crack appears
calculate the potential energy of ball at this height. If no crack appears, then increase your
height and again examine the sheet. Make various readings at different heights and find
the point at which crack appears on material surface or it ruptures completely. Note the
number of cracks and crack length and calculate their average value along with their
respective standard deviations. Similarly, prepare the sheet samples for LDPE and HDPE
according to the ASTM and perform the experiment as described above. Calculate the
failure energy by using formula,

Potential Energy = mgh

Where
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FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

m = mass of the dropped weight

h = height from which weight is dropped

g = Gravitational acceleration

PRECAUTIONS
Never place your fingers at impact point. To find out the impact strength of a polymer,
prepare at least five samples and then note down their status at different heights and find
the maximum height up to which it can resist impact load. Always find out the impact
strength at narrow height range. Never place your fingers at impact point

QUESTIONNARE
1: Tabulate the failure energy of the specimens at various height, along with the status of
the material

2: For each indentation, tabulate the number of cracks and crack length at various heights.
Also indicate the standard deviation for each crack length value

3: Based on the test results identify the factors that have effects on the toughness of
polymers. In what way is the toughness changed by each of these factors?

4: Explain in detail, the working principles of charpy and izod impact testing of plastics.

5: One of the technique used for the testing of impact energy of plastics is Instrumental
falling weight impact testing machine, explain the difference between the falling ball
impact tester and Instrumental falling weight impact testing machine.

6: PET sheets used during experimentation are transparent, while LDPE and HDPE
sheets were opaque, explain this difference of opacity for the three materials.
38
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the flow characteristics of

given polymeric materials (PS, Nylon 6,
ABS, PP, TPU and HDPE) using fluometer

Fig. 1: Fluometer

INTRODUCTION
Pourability is defined as a measure of the time required for a standard quantity of material
to flow through a funnel of specified dimensions. Pourability characterizes the handling
properties of finely divided plastic material. The procedure simply calls for pouring the
material through a specified size funnel and measuring the time required for material to
completely pass through the funnel.

SPECIMENS
Granules of PS, Nylon 6, ABS, PP, TPU and HDPE
39
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

PROCEDURE
For all the given polymeric materials record their shape and then weigh a specific amount
of this material say 150 g. Fit the bottom with different sized nozzle for same materials.
The size of nozzles used in experimentation are 10mm, 15mm and 25mm.

Fill the cup of fluometer with this material while bottom is closed with card board holder.
Then remove the card board holder and start the stop-watch while measuring the time of
flow. Repeat the experiment for different types of materials.

QUESTIONNARE
1: Tabulate the flow time of the polymeric materials along with the state of flow (no flow,
restricted flow and complete flow) observed for each nozzle.

2: Based on the test results identify the factors that have effects on the flow time of
polymers. In what way is the flow time changed by each of these factors.

3: Explain the importance of floumeter in polymer process industry.

40
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

To determine the viscosity of gelatin

suspensions as a function of temperature
and RPM on a rheometer

Fig. 1: Brookfield Rheometer

INTRODUCTION
Flow behavior of polymers is extremely important for the processor, material supplier, the
end user, and the polymer scientists. This property determines whether a material can be
used in a given manufacturing process; it establishes processing conditions; it determines
if there are undesirable residual stresses; it classifies materials and aids in material
development. As mentioned earlier, plastics are viscoelastic materials. That is, they have
both a viscous (flow) property and an elastic (solid) property simultaneously. In the liquid
state the viscous component is dominant.
41
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

Viscosity is a property of a material that involves resistance to continuous deformation.

Unlike elasticity, where the stress is proportional to the deformation, for viscosity the
stress is related to the rate of deformation or strain. Thus, it is related to liquid flow rather
than to solids. It is obvious that a great deal of information can be obtained by measuring
viscosity. These measurements have taken many different forms and used different
methodologies.

Those of significance in practical applications are the following:

Tube Flow (Fig. 2a) – This flow is the one most often used for viscosity measurements.

It occurs when the liquid is transported through a tube, pipe, or circular channel that is
smaller in diameter than the reservoir containing the liquid. The small channel is referred
to as a capillary.

Parallel Disk Flow (Fig. 2b) – This is a torsional flow generated when the liquid is
contained between two parallel plates and is sheared by the movement of one of the
plates relative to the other.

Cone and Plate Flow (Fig. 2c) – In this case, one plate is flat while the other has a cone
shape. Similar to the parallel plates, this flow is torsional. However, in this case the flow
field and stress fields are uniform. It represents a more precise measurement that is
favored by rheologists

Concentric Cylinder (Couette) Flow (Fig. 2d) – This is a drag flow generated by the
rotation of either the inner or the outer cylinder. Couette flow generates higher torque
compared to plates. Therefore, it is widely used for Newtonian and low viscosity fluids.
42
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

Fig. 2: Rheological test geometries: a) capillary, b) disk and plate, c)

cone and plate, d) couette

Concentric Cylinder – Couettes

Concentric Cylinder type measuring systems come in various forms such as coaxial
cylinder, double gap, Mooney cell, etc., as shown in Fig.2d. Standard coaxial cylinders
are referred to by the diameter of the inner cup.

Couette measuring systems require relatively large sample volumes and are more difficult
to clean. They usually have a large mass and large inertias and therefore can cause
problems when performing high frequency measurements.
43
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

Their advantage comes from being able to work with low viscosity materials and mobile
suspensions. Their large surface area gives them a greater sensitivity; therefore they will
provide good data at low shear rates and viscosities.

The double gap measuring system has the largest surface area and is therefore ideal for
low viscosity and low shear rate tests. It should be noted that the inertia of some double
gap systems may severely limit the top working frequency in oscillatory testing. To
calculate viscosity from coquette data use the following:

SPECIMEN PREPARATION
Prepare gelatin suspension by dissolving 10 gm of gelatin powder in 90 ml of distilled
water in a 250 ml beaker and then placing the resultant mixture in an oven at 120 oC for
40 minutes. Uniformly mix the contents of the beaker at regular intervals.
44
FUNDAMENTALS OF POLYMER ENGINEERING, PPE‐102L

PROCEDURE
Switch on the equipment. Set the desired temperature at thermo cell assembly. Pour the
sample in the metallic cylinder and place it into the thermo container. Give sufficient time
to the sample to acquire the chamber temperature. Remove the spindle from the
rheometer, level it and then auto zero by pressing on/off key. Lower the spindle into the
container until it is inserted into the liquid up to the specific mark. Adjust the desired RPM
onto the rheometer.

Note the torque value; if it is less than 10 % or greater than 100 %, then change spindle
or play with RPM to bring the torque value between the above limits. Once the required
torque value is achieved, reported the viscosity as a function of temperature, RPM,
spindle number and dimensions of the container.

PRECAUTIONS
Don’t shake the sample prior to testing. Give at least one hour to make viscous samples
to attain uniform temperature. Always use the right combination of temperature and RPM
the torque within allowable limits.

QUESTIONNARE
1: Tabulate the RPM, viscosity, shear stress and shear rate data for each of the spindle
used during experimentation.

2: Plot viscosity versus shear rate data for each of the spindle used during
experimentation.

3: Tabulate and plot the temperature, RPM, viscosity, shear stress and shear rate data
for each of the spindle used during experimentation.

4: Explain the effect of temperature and RPM on viscosity of polymer melts and solutions.

5: What are the basic sources of error in the rheological analysis of polymer melts and
solutions.