Central Institute of

Petrochemicals Engineering &

Technology, Lucknow

Plastic Material Testing Lab

Manual

B. Tech 3rd Year (PE)

(KPE551)

Department of Plastic Engineering

1
Subject Code: KPE 551 Plastic Material Testing Lab LTP: 002 Credits: 1

Course outcomes: The student will be able to Blooms

taxonomy

CO-1 Apply contour cutting technique to prepare a specimen as per given standard K3

CO-2 Determine basic properties of plastic materials related to nature and K3

composition

CO-3 Calculate thermal stability and melting temperature of polymers K3

CO-4 Measure various electrical properties of plastics K3

CO-5 Determine various mechanical properties of plastics K3

Syllabus: Study of the following techniques with analysis and interpretation of results
:(Minimum 08)
1. Specimen preparation using contour cutter.
2. Determination of Ash Content of a plastic sample.
3. Determination of Moisture Content of a plastic sample.
4. Determination of Filler content of a plastic sample.
5. Determination of Melt flow index of a plastic sample.
6. Determination of Opacity of a plastic sample.
7. Determination of HDT/VST & melting temperature of a plastic sample.
8. Determination of Dielectric strength/Tracking Index of a plastic sample.
9. Study of Weathering properties of plastic materials.
10. Determination of Density of a few plastics’ material samples and film samples.
11. Determination of Bulk density for powder materials.
12. Determination of Mechanical properties (Tensile strength/Modulus, Flexural Strength
/Modulus, Elongation at break, Young’ Modulus, creep resistance, compression
strength of Plastic Material.
13. Determination of abrasion resistance of a plastic sample.
14. Determination of Impact strength of a plastic sample.
15. Determination of Hardness of a plastic sample (Rockwell, Durometer)

2
 LIST OF EXPERIMENTS

S. No. List Of Experiments Page No.

1. Filler Content 5–6

2. Moisture Content 7–8

3. Hardness Test 9 – 11

4. Impact Strength Test 12 – 14

5. Vicat Softening Temperature 15 – 16

6. Heat Distortion Temperature 17 – 19

7. Melt Flow Index 20 – 21

8. Ash Content 22 – 24

3
 LAB REGULATIONS

 Before starting laboratory work follow all written and verbal instructions carefully.

 Keep silence in the lab.

 Bring calculator and other accessories when you come to lab.

 The performance of unauthorized experiments is strictly forbidden.

 In the absence of instructor, no student shall be allowed to work in the laboratory.

 Observe good housekeeping practices. Work areas should be kept clean and tidy all
times.

 Report all accidents to your teacher.

 Conduct yourself in a responsible manner at all times in the laboratory.

 Thoroughly clean your laboratory work space at the end of the laboratory session.

 Do not venture to other lab stations for any reason.

 Never chew plastic materials in the laboratory.

 Never weigh a hot object.

4
 EXPERIMENT – 1
FILLER CONTENT

Aim:
Determination of filler content of a plastic sample.
(ASTM D 2584)

Apparatus:
Crucible of silica or platinum of suitable accommodate test of 2-5gm.

 Analytical weighing balance: It is capable of weighing crucible and sample to

accuracy of 0.1 mg.
 Muffle furnace: It capable of maintaining temperature 0f 850 0C is used.
 Desiccators: Desiccators with CaCl2 as drying agent is used for cooling for the
crucible.
 Tongue: A steel tongue of sufficient length is used for handling crucible in hot
condition.

Definition:
It is defined as a % by mass of the residue left after ignition of specified quantity of material in
furnace under the specified conditions and time.

Principle & Significance:

 A specified quantity of materials is heat in the furnace at ignition temp (Ranging 500 to
800° C for various plastics) for a specified duration until constant mass is achieved.
The residue left after the ignition is calculated in percentage.
 The filler contents in the polymeric material determined and cont. of the various physic
mechanical, electrical, optical, Rheological and other properties of materials. They
influence the processing characteristics and performance of materials and products.
Certain fillers are low-cost materials and influence the performance of the material,
when added with polymers.
 This test is used for quality control of product.
 This is used for research and development (R&D) for evaluating qualitative and
quantitative effects.

Procedure:
Test Specimen: Cut pipe in small pieces with help of knife/saw in sufficient amount (approx.
10-15 gm).

Samples: No of sample to be tested :02

Conditioning: Unless otherwise specified no condition is required.

5
  Switch "ON" the muffle furnace and set the test temperature as 550 0C±500C.
 Take the crucible clean it properly.
 Now weigh the empty crucible and record as W1.
 Take 2-3 gm material in crucible and weigh it again and record as W2.
 After reaching set temp of 550°C, keep the material inside muffle furnace and allow it
to heat for one hour.
 After one hour of heat treatment, remove the crucible from furnace using steel tong
and keep inside desecrator.
 Allow to cool to the room temp.
 After cooling take the weight of the crucible containing residue and record as W3.

Factors affecting test results:

 Test temperature and duration of heating material and furnace affect the ignition of the
polymeric material and hence the result affected.
 Moisture content in the material may affect the test result and incorrect result may
obtained.

Observation, formula & calculation:

Record the following observations:

 Material ________________ gm
 Test Temperature ____________0C
 Mass of empty crucible = W 1
 Mass of crucible + Material = W 2
 Mass of crucible + Residue = W 3
 Test duration __________ hrs.
 Date _________

The quantity of filler is calculated by using following formula-

Filler content (%) = (W 3-W 1)/W 2-W 1) × 100
W 1 = weight of empty crucible.
W 2 = weight of crucible + Material.
W 3 = weight of crucible + Residue.

Result & conclusion:

The filler content of material is = _______%

Safety & precautions:

 Clean the crucible properly before starting experiment.
 Handle the glass desiccators carefully containing sample and residue.
 After removing the crucible from furnace, keep the crucible inside
 Desiccators as soon as possible.
 Use temperature resistance gloves & gas mask.

6
 EXPERIMENT – 2
MOISTURE CONTENT

Aim:
Determination of Moisture Content of a plastic sample.
(ASTM D 789)

 Air oven/Vacuum oven.

 Petri dish boro-silicate glass.
 Tongs/ twizer Safety Gloves Analytical weighing balance of 1000 capacity and to the
accuracy of the 1mg.
 Desiccator.

Definition:
 Moisture content in the Polymeric material may be defined as the quantitative amount
of moisture absorbed by material.
 The moisture content is expressed in %.

Principle & significance:

 The principle of moisture content is to determine the amount of moisture
present in the sample.
 This test is based on the principle of drying a standard quantity of sample in oven under
the specified condition & time. The moisture content in the sample material is the loss
of weight in the sample due to evaporation of moisture from the material. It is
determined by finding the difference in Light of sample before and after the heating.
 Many polymeric materials absorbed moisture from the air. Depending upon the nature
and confusion of the Polymeric material. The hygroscopic material absorbs high
percentage of moisture. The presence of moisture causes processing as well as
dimensional stability problem and affect the quality of product. It results the
performance of product and loss of impact strength and other properties.
 This test is used for quality control of material & product. This test ensures good
process ability of materials.

Procedure:
Test Specimen: Raw-material in the form of granule or powder about 50gms.
Conditioning: No conditioning is required.
Test Procedure:

 Take clean the empty Petri dish and dry in the air oven at 100° C for sufficient time for
it's completely dryness.
 Takeout from the oven and cool in the desiccator to room temp.
 Take the mass of empty Petri dish and record as W1.
 Take 2-5 gm. Sample in Petri dish and record the mass as W2.
 Set temperature 100°C In the vacuum/ air oven and allow to reach the said
temp.

7
  Place the Petri dish with sample in the vacuum/air oven.
 After one hour take out the sample along with Petri dish from the oven and
cool in the desiccator.
 Take weight of the sample and record mass as W3.

Factors affecting:

 Percentage absorption by the material depends upon the many some of them are listed
as below.
 factors Chemical nature of material. Hygroscopic material absorbs high moisture
absorbed Halogen group of polymers absorbed loss moisture.
 amount and types of additive present in the material: Moisture content is
increased by presence of additives.
 Percentage of moisture present in air and temp.
 Duration of exposure of polymer to the atmosphere.
 Hygroscopic materials absorb high percentage of moisture.

Observation, formula & calculation:

Record the following observations.

 Weight of blank Petri dish = W 1

 Weight of (Petri dish sample) before drying = W 2
 Weight of (Petri dish sample) after drying for 1 hour = W 3
Use the following formula to calculate moisture content. Moisture content (%) =
(W 2-W 3)/(W 2-W 1) x 100.

Result & conclusion:

The percentage of moisture content in the sample is = _____%.

Safety & Precautions:

 Use twizer and hand gloves handling of Petri dish and Mai-anvil and shall ensure that
cost and other contaminations do not adds to materials.
 The test quantity o. sample should be spreader in one in Petri dish layer to ensure
complete removal of moisture.
 Test temp. and time shall be adequate for a material.

8
 EXPERIMENT – 3
HARDNESS TEST

Aim:
Determination of Hardness of a plastic sample.
(ASTM D 785)

Apparatus:
 Rockwell Hardness tester with accessories.
 Indenters of various sizes (1/2n,1/4n,1/8n,1/16n, diamonds indenter) bn.
 Standard Hardness block of known hardness value.
 Micrometer capable of measuring thickness to the accuracy of 0.01mm.

Definition:
Hardness is defined as the resistance to indentation, penetration, scratching and deformation
particularly permanent deformation. For the plastic materials it is measured in the scales such
as R, L, M, E & K. Rockwell hardness is expressed in numbers.

Principle & significance:

 Under Rockwell Hardness test the surface of the material is subjected from miner load
of 10Kg. to major load through a specified size of spherical indenter and then return to
the minor load within 15 seconds. Rockwell Hardness measures the net increase in
the depth of impression after the major load is returned to the minor load.
 The hardness is an important surface property of material and represents the polymers
characteristics Rockwell hardness test results are useful for comparative evaluation
material and their grading. This is also used for quality control of the product.

Procedure:
 Test Specimen: Test specimen should be minimum 6mm thick and 25mm 2. The
minimum width should be 3mm.
 Conditioning: The test specimen shall be precondition (if specified) according to the
specified condition.
 Procedure:
 Calibrate the equipment by using the standard “Test Block” supplied with
machine and note down the difference (if any) in reading.
 Choose the test scale for measuring Rockwell hardness from the table given
below for the material.

TABLE
Rockwell Hardness Minor Load Major Load Indenter or
Scale Kg. Kg. Diameter
Mm/in
R 10 60 12.700±0.0025

9
 0.5000±0.0001
L 10 60 6.350±0.0025
0.2500±0.0001
M 10 100 6.350±0.0025
0.2500±0.0001
E 10 100 3.175±0.0025
0.1250±0.0001
K 10 100 3.175±0.0025
0.1250±0.0001

 Select the anvil according to shape of test specimen and place it in its position.
 Fit the test Indenter assembly into the housing chuck of the hardness tester. Tighten
the indenter with the help of Allen screw.
 Set the major load by turning the load adjusting wheel provided in the side of
equipment.
 Place the test specimen on the anvil.
 Apply, the minor load of 10Kg. by turning hand wheel in the clock wise direction so that
the specimen is pushes the indenter and shows the reading of the dial gauge at “3” on
the small pointer. A red spot is marked against the figure “3” to avoid any confusion.
 The long pointer automatically stops at "0" on Back scale, i.e., “B” on red scale. This
adjustment applies a minor load of 1Kg. which is in built in machine.
 After 10 second apply major load by releasing the trip lever.
 After 1 sec ±1 remove the major load and read the Rockwell hard on the scale to the
nearest full-scale division 15 sec after removing the major load.
 Use outer scale of dial in case of tests on "A" and "C" scale and inner scale for tests
on "B" scale only.

Factors affecting test results:

 Temperature and humidity: Material tested with increased temperature and humidity.
 Surface condition of specimen: Surface finish have significant effects on hardness
test result. A smooth moulded surface specimen yields higher hardness.
 Filler content: Hardness value very depends upon the type and amount of filler added
in the resin.

Observation, formula & calculation:

 Material___________
 Test equipment___________
 Test method__________
 Type of test specimen & dimension__________
 Specimen preparation___________
 Test conditions___________

TABLE
S.No. Indenter Load Dial Scale Rockwell Remarks
Dia. Kg. Reading
1.
2.
3.

10
  Count the number of times the needle passes through zero on the red scale on the
application at the major load and calculate the Rockwell hardness is as below.
 Subtract from this the number of time the needle passes through zero upon the
removal of this load.
 If this difference is zero, record the value as the reading plus 100.
 If the difference is 1, record the reading without change, if the difference is 2, record
the reading as the sale reading minus 100.

Result & conclusion:

Rockwell Hardness of material in scale …….. is………

Safety precautions:
 Apply the minor load slowly by turning the wheel without any shock.
 Release the shift lever slowly to apply the measure load without any shock.
 Read the hardness value on the dial within the prescribed the time limit.

11
 EXPERIMENT – 4
IMPACT STRENGTH TEST

Aim:
Determination of Impact strength of a plastic sample.
(ASTM D 256)

Apparatus:
 Impacto meter with accessories for determination of the Izod impact resistance.
 Notch cutter for notching of test specimens.
 Test jigs for Izod and Charpy test.
 Micrometer for measuring thickness and width of the specimen.

Definition:
 It is defined as the ability of material to withstand sudden shock load at the time of
failure.
 It may also be defined as the ability to resist the fracture under the applied stress. Most
commonly the impact strengths is measured by two method Izod and Charpy.

Principal:
 When a material is subjected to a sudden load it undergoes to the deformation under
the influence of impact force. Depending upon the intermolecular flexibility and
intermolecular force of the polymer molecules, material ma absorb energy. In this
process of deformation material absorb the energy at the time failure and fracture
process.
 Impact strength of the material is related to the toughness of the material. Therefore,
the impact strengths gives the toughness of the material.
 Toughness is the ability of material to absorb the energy at the time of failure It
indicates the relative toughness and brittleness characteristics of the material.
 The impact strength of the material is used for inspection, quality control and grading
the materials.
 The area under stress is-strain curve of tensile test is directly proportional to the
toughness of a material.
 Impact test shows the notch sensitivity of the material.

Procedure:
Test Specimen :

 For Izod impact-Molded specimen of 61.5mm * 12.7nm * 3.2mm in used.

 For Charpy impact-Molded specimen 12.7mm X 12.7mm X 6.4mm is used.
 The specimen from sheet should be cut. It should be equal to the thickness of the
sheet, except that it should not exceed 12.7mm sheet material thicker it an 12.7mm
should be machined down to 12.7mm
 Specimen less than 3.2cm in thickness should be laminated together with al suitable

12
 adhesive to prevent buckling or twisting during impact.
 At least five no.s, of good test specimen shall be tested.

Notching:

 Test specimen shall be notched with the help of notch cutter in the centre of the test
specimens Izod and Charpy.
 The angle of notch shall be 45 0 ± 10 with a radius of 0.25mm. The depth of notch shall
be 2.54mm.
 The linear speed of notching cutting tool shall be between 90 to 165 mtr./min
Conditioning: Pre-condition the test specimen in the environmental chamber at
standard atmospheric condition as specified by standard. In a number of cases, it is
taken as 27±2 0C and 65±5% RH.

Procedure:
 Calibrate the equipment as per the operating instructions of equipment. Take the
pendulum to its release position and release. The energy loss friction (if any) is
recorded.
 Measure the width and thickness of the specimens with the micrometer to the accuracy
of 0.05mm.
 Clamp the test specimen in position of rigidly in the vice in such a way that half of
notched portion is above vice.
 The specimen should be positioned in such a way that notched end of the specimen
facing the striking edge of pendulum.
 Set the reading of the equipment in zero position and take the pendulum to release
position.
 Release the pendulum by depressing release lever and allow to strike the specimen
and cause breaking
 Arrest the pendulum and return to its release position.
 Record the energy absorbed in breaking the specimen in joule.
 Repeat this test on all five test samples and record the observations.

CHARPY IMPACT:

 Charpy impact test is carried out using same equipment in similar manner using
Charpy test specimen and fixtures.
 Fix the charpy impact fixture, specimen support and striking hammer.
 Measure width and thickness of specimen with micrometer to the accuracy of 0.01mm.
 Mount the specimen horizontally on the specimen supported at both end Notched side
of specimen should be faces opposite side of specimen the sticking hammer.
 Take the pendulum to its release position.
 Release the pendulum by depressing release lever and allow to strike the specimen in
midway between support and break in single blow. Arrest the pendulum and return to
its release position.
 Arrest the pendulum and return to its release position.
 Record the energy absorbed in breaking the specimen in joule.
 Repeat the test on remaining sample and record the energy reading.

Factors affecting test results:

13
  Following factors affect the impact strength of material.
 Rate of loading: At low rate of impact strength is higher than high rate of impact
testing.
 Notch Dimensions: Notch radius and its depth have an effect on impact strength. Large
radius will yield high impact & vice versa. Lower notch depth will procedure high
impact.
 Test Temperature: At lower temperature impact strength is reduced where as at
higher temp. it is significantly improved.
 Orientation: Higher the orientation of polymer molecules during moulding will have
higher impact strength in direction flow of material.
 Processing condition: Inadequate processing conditions such as voids preset
component. High processing temp. may degrade material, weak weld line procedure
during moulding will reduce impact strength. Compression moulded specimen
generally show lower impact strength compared to injection moulded specimens.
 Degree of crystallinity & molecular: Higher percentage of crystallinity decrease the
impact strength.

Observation, Formula & Calculation:

Record the following observation-

 Date………
 Material……
 Specimen preparation………….
 Izod impact/ Charpy impact…………
 Distance between support………...
Specimen NO.

 Width in (mm)_____
 Thickness(mm)_____
 Impact meter reading Izod/Charpy (Joule)______
 Impact strength Izod/Charpy (J/mm2) _______
 Remarks_________
 Calculate the compressive properties using the following formula,
Impact strength = (impact energy) / (cross section area of the specimen)

Result & conclusion:

 Izod impact strength of material is =………… J/mm2
 Charpy Impact is = .......J /mm²

Safety & precautions:

 Check that pendulum is free from friction between the moving part.
 Select the correct hammer for the test.

14
 EXPERIMENT – 5
VICAT SOFTENING TEMPERATURE
Aim:
Determination of VSTof a plastic sample.
(ASTM D 1525)

Apparatus & equipments:

Heat distortion and vicat softening apparatus consisting; 'immersion bath Heat transfer liquid
(such as silicon oils, glycerine ethylene glycol etc.) Support or stand for specimen and dial
gauge, Dial gauge (0-25mm) for measuring of 1 mm depth of penetration to accuracy of
0.01mm; Temperature indication device. (Such as thermometer); Weight: (1.0 kg. or 5.0 kg.)
depending on test method; Flat-ended needle of 1 mm² circular cross section.

Definition:
Vicat softening temperature is the temperature at which a flat-ended needle of 1 mm² circular
section will penetrate a thermoplastic specimen to a depth of 2 mm under a specified load
using a selected uniform rate of temperature rise. The two standard permissible rate of rise of
temperature are 50 ± 50°C/hr and 120±12°C/hrs.

Principle & significance:

 Determination of temperature at which a standard indenter penetrates 1mm in to the
surface of plastic test specimen under one of the load as given above. During the test
temperature is raised at uniform rate either at 50 ± 5°c / hrs. or 120°C ± 12°C/hrs. The
temperature at 1 mm penetration is quoted as Vicat softening temperature (VST) in
°C.
 This test is useful for quality control of development and characterization of material.
Vicat softening data obtained from this test is used for comparing heat softening
qualities of thermoplastic materials.

Procedure:
Test Specimen: Specimen of minimum 12 mm wide and 3.0 to 6 mm thick shall be used. It is
surfaces shall be flat parallel and free form flash.

 Place the specimen in specimen support.

 Position the flat needle in such a way that needle rest in the sample in Centre.
 Immerge the specimen support assembly with sample in immersion bath. Set the
micrometer to zero.
 Place the weight to load carrying plate on the spindle, which is fitted with flat needle
so that total load on test specimen is 1.0 kg. for method A of and 5.0 kg. for method
B.
 Increase temperature of oil bath at the rate of 50° ± 5°C/hr (Rat A) or 120° ± 12°C/hr
(Rat B).
 Observe the dial gauge for penetration of needle in the specimen.
 Note the temperature of oil bath at which indenting tip has penetrated into test
specimen by 1.0 mm and record it as vicat softening temperature (VST).

15
Observation & calculation:
Record the following information-

 Material………...
 Test load............kg.
 Rate of heating……... deg/hrs
 Vicat softening temp......... deg Celsius.

Result & conclusion:

Vicat softening temperature of given material is……… at……….kg. load & concession and at
rate of 50 ± 5 or 120°C ± 12°C/hr.

Safety precautions:
 Safety gloves should be used.
 Check the oil level in oil bath.
 Place the test assembly in oil bath carefully.
 Cool the oil to room temperature before starting the next test.
 Use correct grade of heating oil to achieve derived test range."
 Check the calibration of the equipment is data of Vicat softening temperature of
plastics.

16
 EXPERIMENT – 6
HEAT DISTORTION TEMPERATURE
Aim:
Determination of HDT of a plastic sample.
(ASTM D 648)

Apparatus:
 HDT-VSP tester fitted with deflection measuring device (Dial gauge range 0 to 25mm,
accuracy 0.01mm)
 Immersion bath
 Heat transfer liquid (silicon oil)
 Weights
 Micrometre (0 to 25mm)
 Thermometer (up to 350 0C)
 Test fixtures

Definition:
It is defined as the temperature at which a standard test bar of 127 x 12.7 x. 6.4 mm deflects
0.01 in (25 mm) under stated fibre stress of either 66 PSI (4.6 kg. /Cm²) or 264 PSI (18.5 kg.
/Cm²).

Principle & significance:

 Determination of temperature when a rectangular test bar is subjected under specified
load at its centre like simple beam and heated underload in heat transfer medium. The
temperature of heat transfer medium is raised at the rate of 2°C/min. The temp of oil
is measured when test bar deflects 0.25 mm. Two test methods are uses. Method A
uses fibres stress of 12.7 mm to 3 kg. /Cm² and method is 4.6 kg. /Cm².
 This test predicts the behaviour of plastics under short-term heat and used for quality
control, screening and ranking of material.
 From the HDT data a good comparison can be made from one material to another
material. HDT test value can be a good guide for selecting best performing material for
specific application.
 This test is useful for quality control of material and to check the batch uniformly.

Procedure:
 Test specimen: Take two Test specimens of 127 mm long 13 mm wide and 3 to 13
mm thick.
 Measure width and thickness: Of specimen with suitable micrometre.
 Calculate testing load to be applied by using following formula.
 F = 2sbd2 / 3L
 Place the test specimen in fixture of apparatus with its depth (in vertical position 13
mm dimension).
 Ensure that testing force applied on compression moulded and sample Cut from sheet
is in perpendicular to direction of moulding pressure.
 Place thermometer or temperature measuring device close to test specimen (within

17
 3.2 mm) but does not touch the specimen.
 Prepare the calculated test load and apply if on the test rod. The total test load shall
include the weight of rod.
 Allow the load to act for 5 minutes. Then make the zero reading of dial gauge i.e.,
deflection-measuring device.
 Raise the temperature of both at an average rate of 2º C/ min with heat control device
and observe the deflection of the dial gauge.
 Not down the temperature of heating medium by thermometer when sample has
deflected 0.25mm.
 When using method B, the applied fibre stress on the test sample is 4.6 kg/cm²
 Repeat the same procedure on another test sample.

Observation & calculation:

 Material-- Test sample preparation
 Method……….
 Method used (A/B: Fibre stress applied.……… kg/cm².
 Rate of rise of temperature………... °C/min

Table
Date of test Heat deflection Length, Width Immersion Remarks
temperature & Thickness of Medium
specimen

 Calculation the testing load to be applied using formula = 2sbd 2 / 3L,

Where;
S = fibre stress
b = length. of the specimen
d = thickness of specimen
L = span length distance between supports (100 mm)

Result & conclusion:

 Heat Deflection temperature …………...0C
 Results are found to be close to the literature value.

Safety & precautions:

 Check equipments having valid calibration and are not manufacturing.
 Use safety gloves.
 Check the oil level in the oil bath.

18
 Place the test assembly in the oil bath carefully.
 Cool the oil to room temperature before starting the next test.
 Use correct grade of heating oil to achieve desired test range.

19
 EXPERIMENT – 7
MELT FLOW INDEX
Aim:
Determination of Melt flow index of a plastic sample.
(ASTM D 1238)

Apparatus:
 MFI tester capable of maintaining temperature from ambient to 350°C.
 Die: Internal die 2.096 mm, cutting tool, changing tool, loading piston, Die existing tool
etc. standard without as given in table.
 Stop Watch.
 Weighing Balance.

Definition:
Melt flow index is defined as the rate of extrusion of molten resin under specified temperature
and pressure through a specified size of die in 10 minutes. It is expressed in g/10 min.

Principle & significance:

This characteristic is primarily useful for measuring uniformity of flow rate of materials. This
is used for grading of thermoplastic material and their quality control i.e., in determining lot-
to-lot consistency of resin. A material having high molecular weight has more resistance flow
than the low molecular weight polymer.

Procedure:
 Clean the barrel and die using cleaning tool.
 Select the test condition such as temperature and load to use for test.
 Place the die into the barrel.
 Set the specified temperature and allow to reach.
 Change the required amount of material (about 8-10g) into barrel and compress the
material by hand pressure through changing tool so that there is no air bubble In this
process place vit for few minutes (3 - 4 min.) temperature has returned to set temp.
Place the piston in barrel.
 Apply selected test load over the piston so that it defends up to lower materials under
gravity.
 Discard the extrudate of this position.
 Select cut-off time in second (=)
 Collect about 06 extrudate each cut-off time interval.
 Discord the extrudates if anyone is containing air bubbles.
 Take weight of each extrudate on weighing balance to the accuracy of 0.000 g.

Observation, formula & calculation:

20
Record the following observation-

 Date of Test______
 Material________
 Test Method______
 Test Temp._________0C
 Weight of extrudate sample_______
 Avg. wt. of extrudate_______ in gm.
 Melt flow index
 Calculate the result using following formula
Melt flow index: (600 X M)/t g/min.
Where;
t: cut-off time in second
M: Average mass (gm.)

Result & conclusion:

 Melt flow index of given materials is _____g/10min, at_____kg/°C.
 Test result is within/ out of time specified the given material. Identification of result.
Melt flow index can be interpreted in different way.
 Level, the equipment properly.

Safety precautions:
 A significantly different MFI value may indicate different grade, of material.
Hygroscopic material should be pre-dried before test.
 Data of melt flow and index of various materials.
 Use Asbestos gloves.
 See the equipment is in proper level with the help of split level and alignment of piston
in barrel is correct.

21
 EXPERIMENT – 8
ASH CONTENT
Aim:
Determination of Ash Content of a plastic sample.
(ASTM D 2584)

Apparatus & reagent:

 Crucible: Silica or platinum crucible having upper diameter b. t. 45-75 m and height
equal to diameter of crucible is sufficient so the crucible is not filled more har half by
size test portion.
 Analytical Weighting balance: Analytical weighting balance capable of weighing
crucible and sample to an accuracy of 0.1mg.
 Bunsen Burner: Bunsen Burner with silica & tripod or other suitable heating device.
Muffle Furnace: Muffle Furnace capable of maintaining Temp. of 850±10°c is used.
 Pipette: The glass pipette of appropriate capacity is used.
 Desiccators: Desiccators with CaCl2, as drying agent is used for cooling the crucible.
 Tongue: A steel tongue of sufficient length is used for handling crucible in hot
condition. Concentrated Sulphuric Acid (Density 1840 Kg/M³).

Definition:
It is defined as the % by mass of the residue left after ignition of specified quantity of the
material in furnace under the specified conditions and time.

Principle & significance:

Calcinations with Sulphuric acid after combustion, that is by burning the substance and
transforming the residue into sulphates using Conc. Sulphuric Acid & finally, heating the
residue at 850°c until constant mass is reached.

Procedure:
Sample Preparation: Cut pipe in small pieces with help of knife/ saw in sufficient amount (10-
15 gm).
Samples: No. of samples to be tested:02
Test procedure:

 Wash and clean the crucible so that there is no contamination and foreign material in
it.
 Place the crucible in muffle furnace maintained at 850+10°c until constant mass of
crucible is reached.
 Take out crucible from muffle furnace & place in a desiccator. Allow to cool to room
temp. for 1 hr.
 Take the weight of crucible nearest 0.1 mg & record it as M₁.
 Cut in small pieces from the pipe sample.

22
  Take 2 to 5 gm of cut sample in crucible and weight nearest to 0.1 mg & record it as
M2.
 Continue heating until evolving of smoke from sample is stopped.
 Remove crucible with sample content from Bunsen burner & allow it to cool.
 Add Sulphuric acid in residue drop wise by means of pipette until residue is soaked.
 Place the crucible with residue completely soaked in Sulphuric acid on Bunsen burner
& heat again until evolution of smoke ceases.
 Remove crucible from Bunsen burner and allow it to cool.
 Add 1 to 5 drops of Sulphuric acid if carbon is evident in crucible & reheat in Bunsen
burner.
 Continue heating till evolution of white smoke is stopped.
 Remove crucible with content from Bunsen burner with the help of tongue.
 Place crucible at mouth of muffle furnace maintained at 850 ± 10°C and advance
crucible into furnace slowly.
 Heat for 30 mins at 850 ± 10°C.
 Remove the crucible from the furnance with the help of tongue and place it in the
desiccators.
 Allow to cool room temp. for about 1 hr.
 Calcin again & again at 850°c ± 10°c until the constant mass is reached i.e., until the
weight of two consecutive weighing doesn’t differ by more than 0.5 mg.
 In case constant mass is not reached as above but totally heating time in furnace
exceeded 3 hrs. then stop further heating.
 Allow to cool the desiccators to room temp. & take the weight the crucible with residue
& record it as M3.
 Take the weight of crucible with content nearest to 0.1 mg and record it as M3.

Factors affecting:

 Ignition temp. and duration of the ignition.

 Amount of filler added in material.

Observation & calculation:

 Date of test ______
 Material_______
 Test temp. ______
 Mass of sample _______ gm
 Mass of Empty crucible_______ gm.
 Mass of residue (Ash)________ gm.
 Calculate the Sulphated Ash content as follows.
 % Sulphated Ash content = (M3 – M1)/ (M2 – M1) * 100
 (By Mass) Where;
M1 = Mass of crucible,
M₂ = Mass f crucible & test portion Sample,
M3 = Mass of crucible & Residue.

 Take the average of two measurements.

 If the test results differ from each other by more than 10% of their mean, then repeat
the test until two successive results don't differ from each other by more than 10% of
their mean.

23
Result & conclusion:
 The Sulphated ash content is _____ %
 The average Sulphated Ash content of two measurements shouldn't exceed 11% to
treat the sample for passing the test.

Safety & precautions:

 Use temperature resistance gloves & gas mask.
 Handle the glass desiccator carefully containing sample and residue.

24