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7.identification and Chemical Properties
7.identification and Chemical Properties
VISHAL VERMA
Technical Officer
IDENTIFICATION
When working with plastics there is often a need to identify
which particular plastic material has been used for a given
product. This is essential to get an idea of the cost and likely
properties of the product. The identification of plastics is
generally very difficult due to:
The wide range of basic polymers that is available for
use.
The wide range of additives that can be used to modify
CONTENTS
Introduction
Simple method
cutting test
flotation test
bending test
dropping test
Burning test
Pyrolysis test
Specific gravity test
Solubility test
Softening and Melting point
Elemental Analysis
Confirmation test
CUTTING TESTS
If a shaving can be pared off with knife, it may be a
thermoplastic.
Note: PMMA and Polystyrene are brittle and difficult to
pare
If the material is rigid and will not pare off instead flakes of
Results
Scuffs with fingernail - Urea formaldehyde resin.
resin.
FLOTATION TEST
This test will give the idea to distinguish the material
according to their density.
BENDING TESTS
Some plastics will exhibit particular characteristics in the manner
in which they respond to bending. The bending behaviour of some
plastics of almost same cross-section is given in Table
PLASTICS BENDING BEHAVIOUR
1. Polyethylene Bends, tends to remain
2. Polypropylene Unbends most of the way
3. Polystyrene Cracks but retains bend
4. ABS Bend tends to remain
5. PVC (Rigid) Bends easily and springs back quickly
6. Cellulose acetate Bend tends to remain
7. PMMA Cracks and splinters
8. Nylon Difficult to bend, springs back
9. Polycarbonate Tough to bend
DROPPING TEST
When a polymer moulded component is dropped on hard
surface, it creates sound, which shall be either metallic
sound or dull sound. On the basis of sound polymer is
distinguished in two categories, which is tabulated in
Table
BURNING TEST
A small sample is held in flame. If it ignites withdraw it
from the flame a distance of flame. Make observations
as listed below and record the observations, for
example:
PE Melt and bubbles fiercely Blue with yellow tip Waxy (Burning Candle)
around the edge, Drips
PS / SAN Melts and bubbles around Orange – Yellow, Heavy, Mari gold, Strong smell
the edge, spurting, burns Black, Sooty Smoke of Styrene and Burning
readily rubbe
High Impact poly Melts and bubbles around Orange – Yellow, Heavy, Slight burning rubber
styrene the edge, spurting, burns Black, Sooty Smoke smell
readily
ABS Becomes soft but not fluid Orange – Yellow, Heavy, Slight burning rubber
Black, Sooty smell
PVC Soften and forms a ball, Yellow with green bottom Chlorine smell, pungent
chars at bottom, self – edge, Some White Smoke
Extinguishing
CA Melts and emits white smoke boils Yellow, burns brown at Smell of Vinegar (Acetic
and chars base, Some light Smoke acid)
CAB Melts and Char at the edge, drips Dark yellow with light blue Rancid butter (an Odour
base, Some light black of butyric acid)
Smoke
PMMA Boils and Bubbles Blue and Yellow Flame, Fruity, Floral smell
Some light black Smoke
PC Melt but chars, Bubbles develops a Orange yellow flame with Phenolic smell ( ink
cellular structure before black smoke smell)
decomposing, self – Extinguishing
PPO Melt but chars, self – Extinguishing Orange yellow flame with Phenolic smell ( ink
black smoke smell)
Nylon Melts round edges and chars, Blue with Yellow tip Burning hair / wool /
Froth formation and drips vegetarian
PET/ PBT Melts, opacifies, blackens, Yellow, Slightly smoky Pleasant elusive odour
Molten Material drips
Polyvinyl Softens Dark Yellow, Spurts with black Vinyl acetate smell (Sweet
Acetate smoke odour)
Melamine Resin Yellow with light blue edge, self Fishy smell
extinguishing
Polyester Resin Burn with orange yellow flame, Black Ester smell
(Unsaturated) smoke
Butile rubber (IIR) Smoke free, candle like Hydrocarbon smell Melt does not char
readily, tacky
Polyisoprene (NR) Yellow sooty Pungent like burn rubber Chars & crack
Polychloroprene (CR) Self extinguishing Pungent smell Strongly acidic fumes,
Yellow & smoky of chlorine black residue dry
powdery
Silicone rubber Burns continuously, glow No odour Dry white powdery
with white smoke powdery
Ebonite Smoke free Sulphur odour Chars readily
PYROLYSIS TESTS
In this testing, heat few milligrams of the sample in an ignition tube and test
the pyrolytic vapour with a moistened indicator paper. The behaviour of
vapour to indicator paper is given as follows:
ACID: turns blue litmus to red
BASE: turns red litmus to blue.
ACID VAPOURS: may come from carbohydrate polymers & their
derivatives. [e.g., cellulose acetate]
HIGH ACID VAPOURS: often indicates the presence of chlorine. e.g., PVC
or rubber neutral vapors] evolved from hydro carbon polymers,
silicones and some polyesters hydrochloride.
ALKALINE VAPOURS: indicate the presence of N2. e.g. polyamide,
proteins & amino formaldehyde resins.
Rubber Testing: This scheme is useful for identification of CR, NBR, SBR, NR / IR,
IIR type of rubbers
Test Procedure: Heat strongly 0.5gm of sample in a test tube until sample begins
to decompose and pass the fume in solution II and I and observe change in
colour initially and after heating. (Refer the following table)
Solution - I : Dissolve one gram of p - dimethyl amino benzaldehyde in
5ml of HCl and add 10ml of ethylene glycol. Adjust the density to 0.851
gm /cc. by addition of methanol.
Solution - II : Dissolve 2gm sodium citrate , 200mg of citric acid , 300mg
of bromo cresol green and 300mg of metanil yellow in 500ml of water.
RUBBER Solution - I Solution II
Initial After Heating
Blank Solution Pale Yellow Pale Yellow Green
SOLUBILITY TESTS
Solubility tests form a basis of some older identification schemes for
main types of plastic materials. However, in many cases solubility
varies considerably for different samples of the same resin and it is
difficult to interpret the results Solubility of plastics may vary
according to the grade or to the whether or not other constituents
are present in the sample. The data in Table refer in principle to pure
polymers, although even those polymers may exhibit differences in
solubility. The solubility test should be carried out directly in a test
tube. To about 100 mg of a powdered sample add 10ml of solvent,
mix occasionally shake the contents of the test tube and observe for
a few hours swelling may occur before complete dissolution of the
polymer.
ELEMENTAL ANALYSIS
The results of test for the elements other than carbon,
hydrogen and oxygen, namely nitrogen, sulphur, and
halogens serve to indicate the possible nature of the
unknown material
It should be noted that the compounding ingredients
may contain elements which will also be detected and
thus give rise to a positive result. They may interfere
with the identification of the polymer. So additives free
extracted purified polymer should be used for elemental
analysis in order to identify exactly the nature of
polymer.
CENTRAL INSTITUTE OF PLASTICS ENGINEERING AND TECHNOLOGY, CHENNAI Home
IDENTIFICATION AND CHEMICAL PROPERTIES
Carbon
Experiment: 0.05 gm of material is mixed with 0.2 gm of
potassium dichromate, 10 drops of phosphoric acid in a test tube.
Exclude air present by blowing with CO2 with N2 or O2. Heat the
solution in H2SO4 or glycerol bath at 200oC. Connect test tube to a
U – tube containing clear BaCl2 solution.
Observation: White precipitate of BaCo3
Inference: Carbon confirmed
Hydrogen
Experiment: Place little of the sample in a
micro test tube with few o-g- of pure sulphur
cover mouth strain with led-acetate paper.
Heat the solution in glycerol bath for 2 min.
Observation: Brown black strain
Inference: Hydrogen Confirmed
Oxygen
Experiment: Reagent preparation: Dissolve 1 gm of
ferric chloride and 1gm of potassium thiocyanate
separately in 10 ml of methanol. Mix the two solutions
and after standing for few hours filter of the KCl
precipitate. Dip strips of filter paper in methanol
solution. Dry it is air, Prepare fresh strips before test.
Several drops of liquid polymer or its solution are
placed on the paper prepared above (conduct a blank
also)
Observation: Deep wine red colour
Inference: Oxygen confirmed
Nitrogen
Experiment: 2 ml of the sodium fusion extract is
boiled with 3 drops of freshly prepared aqueous
ferrous sulphate (approx 5%) & then cooled,
after acidification with acid, a drop of 0.5N
aqueous ferric chloride is added
Observation: Blue precipitate
Inference: Nitrogen confirmed
Sulphur
Experiment: Three drops of freshly prepared
aqueous sodium nitroprusside (approx 5%) are
added to the test portion.
Observation: Violet colour
Inference: Sulphur confirmed
Fluorine
Experiment: An aqueous solution of Zirconium nitrate
(0.1%) and alizarin reds (0.1%) is prepared. Filter
paper is immersed in the solution and then allowed to
dry. When required, a small piece of the paper is
moisturened with aqueous acetic acid (50%). The
solution to be tested is neutralized with 5N HCL and a
drop placed on the moistened test paper.
Observation: Red spot turns Yellow
Inference: Fluorine Confirmed.
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Test for Polycarbonate
About 1.0 gm of sample is pyrolysed in an ignition tube,
which is plugged with cotton. The cotton is removed and
immersed in 1% methanolic solution of p-dimethylamino
benzaldehyde and then one drop of 5 N-Hydrochloric acid
is added.
A dark blue colour appears in the case of polycarbonates.
A red colour that does not change to blue is observed in
the case of polyamides.
The cotton floak in which the prolysed vapours of the
sample absorbed is treated with dilute (1:1) HCI. An
intense red colour which is unaffected by methanol
indicates the presence of polycarbonate.
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Test for Cellulose Ethers:
The important cellulose ethers are Methyl cellulose, Ethyl.
Cellulose and Benzyl cellulose.
Reaction to Heating and Burning:
Cellulose ethers melt and char after heating and continuously
burn after ignition. Nature of flame and smell of the cellulose
ethers are as follows:
Cont.
CONFIRMATION TEST - Thermoplastics
Cont.
CONFIRMATION TEST - Thermoplastics
Detection of Ethyl Cellulose:
The sample is treated with one drop of dichromate solution
(1.0 9 of potassium dichromate K2 Cr2 07 + 60 ml water +
7.5 ml of con. H2S04) and then heated to 100° C. The
mouth of the tube is covered with a filter paper moistened
with a mixture of equal volumes of 20% aqueous
morpholine solution and 5% aqueous sodium nitroprusside.
A blue colour indicates the presence of Ethyl Cellulose.
Cont.
CONFIRMATION TEST - Thermoplastics
Cellulose Nitrate
1 ml of water is added to a test tube containing about 1mg of
the sample & 2 ml of freshly prepared 0.2% solution of
enthrone in conc. H2S04 . A green colour changing to dark
blue is confirmed cellulose.
20ml of diphenylamine is dissolved in 1ml of conc H2S04.
Cont.
CONFIRMATION TEST - Thermoplastics
Acrylonitrile – butadiene Styrene
The polymer (about 1 g) is refluxed with concentrated nitric acid (20 ml)
for 1 hr using a long air condenser in a fume cupboard. The mixture is
poured into water (100ml) and extracted with ether (2 x 25 ml) and the
aqueous extracts rejected. The ethereal layer is extracted with in aqueous
NaOH (2x25ml). The ethereal layer is rejected. The alkaline extracts are
combined and just acidified with concentrated HCl & then excess of acid
(20 ml) is added. Granulated zinc (5g) is added & the mixture heated on a
steam, bath for 20 min. The mixture is cooled freshly prepared sodium
nitrate (approx. 0.1g in 2 ml) added. The resulting solution is poured into
freshly prepared alkaline - Napthol solution (approx.0.05g in 10 ml SN
aqueous NaOH). The formation of vivid scarlet colour confirms the
presence of styrene.
Cont.
CONFIRMATION TEST - Thermoplastics
Casein
A sample about (0.02g) is dissolved in concentrated HNO3
(2ml) by boiling for about 5mn. The solution is cooled and
excess 5N ammonium hydroxide added. The formation of
orange colour confirms the presence of casein.
Cont.
CONFIRMATION TEST - Thermoplastics
Polyisobutylene
Filter paper is immersed in freshly prepared mercuric
sulphate solution (prepared by dissolving yellow mercuric
oxide (1g) in boiling 5N H2SO4 (20ml) and cooling before
use and used without drying. The paper is inserted in the
mouth of an ignition tube containing the polymer (about
0.2g). The tube is gently heated. The formation of Bright
yellow colour confirms the presence of Polyisobutylene.
Cont.
CONFIRMATION TEST - Thermoplastics
Polymethyl Methacrylate
A sample (about 0.1) is heated in an ignition tube and the
pyrolysate collected in a test tube wrapped in a wet filter
paper. To the distillate is added conc. HNO3 ( 1 ml) and the
mixture is heated just to boiling and then cooled water ( 5ml)
and then Sodium nitrite ( 0.1g) are added. The formation of
Blue colour confirms the presence of PMMA.
Cont.
CONFIRMATION TEST - Thermoplastics
Polyvinyl Acatate
An iodine reagent is prepared by dissolving iodine (0.1g) &
potassiumiodide (1g) in a mixture of water (10 ml) &
ethanol (10ml) and making upto 100 ml with 2N HCL.
The polymer (about 0.05g) is covered with the iodine
reagent (1ml). The effect is enhanced if water (10ml) is
added. The formation of Stained deep red colour confirms
the presence of Polyvinylacetate.
Cont.
CONFIRMATION TEST - Thermoplastics
Polyvinyl Alcohol
A Sample (about 0.02g) is dissolved in water 5ml and
iodine reagent described above (5 drops) added. The
formation of Blue colour confirms the presence of Polyvinyl
alcohol.
Cont.
CONFIRMATION TEST - Thermoplastics
Shellac
A sample (0.05g) is dissolved in ethanol (1ml) with
warming. To the cooled solution is added water (about
1ml) to give an emulsion like precipitate. 5N aqueous
NaOH 2 drops is added to the mixture. The colour change
is reversed on acidification with 5N HCL. The formation of
Violet - red colour confirms the presence of Shellac.
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - THERMOSET PLASTICS
Cont.
CONFIRMATION TEST - RUBBERS
SBR- NR-IR
If 2 ml of chloroform show appreciable darkening
when shaken with 200 mg of sample of vulcanized
rubber product, and repeat pyrolysis test.
Cont.
CONFIRMATION TEST - RUBBERS
NR- IR
Extract a fresh portion of sample with acetone, and swell the
extracted sample in a little chloroform and add few drop of
bromine and wait for 2 min . add about 1 gm phenol and
warm on a stream bath to remove chloroform a blue to red
– violet colour indicate NR/IR.
Cont.
CONFIRMATION TEST - RUBBERS
SBR
Boil 2 gm of dried, acetone-extracted sample under reflux with 20 ml
HNO3 for 1 hr, and add 100 ml of water. Extract with 50, 25, 25 ml
portions of diethyl ether. Combine the ether extracts and wash twice with
15 ml of water and extract with 15 ml portion of NaOH solution and finally
extract with 20 ml of water.Discard the ether, combine the sodium
hydroxide extract and water washing, make just acid with HCl and add 20
ml in excess. Heat on a stream bath and reduce the nitro benzoic acid by
adding 5 gm on granulated zinc. Make ther solution alkaline with the
NaOH solutionto just dissolve the precipitate. Extract twice with ether
and discard the ether. Make the aqueous solution acid with HCl, cool to
room temperature and add 2 ml of NaNO2 solution. Pour this diazotized
solution into an excess of solution of B- Napthol in NaOH. A vivid scarlet
colour indicates SBR.
Cont.
CONFIRMATION TEST - RUBBERS
IIR
Place about 1 gm of dried, acetone extracted sample in a
tube and decompose it by heating and pass on the vapours
to seconds test tube placed in icxe, from these, the vapour
are transferred to another tube contains 0.5 gm of
mercuric acetate in 15 ml of methanol, evaporate the
methanol and boil the residue with 25 ml petroleum ether
and get petroleum ether extract and evaporate petroleum
ether to get mercuric derivate with melting point of 55
degree centigrade.
CHEMICAL PROPERTIES
Chemical resistance is define in terms of stability of properties in contact
with chemicals like water, oxidizing agents, oils, lubricants, industrial
solvents and food stuffs.
The Interaction of chemicals with plastics can take place in different
ways, affecting adversely their useful properties at varying rates and to
varying degrees. The mechanisms involved can be chemical reaction,
solvation, absorption, plasticization and stress cracking. The strength of
the chemical bonds, the degree of crystallinity, branching, and polarity are
the deciding factors for the chemical resistance of polymers. Rise in
temperature increases the rate of chemical interaction.
IMMERSION TEST
Acetone immersion test
Significance This test method is applicable only for
distinguishing between inadequately fused and adequately
fused PVC.
Test Method
ASTMD 2152: Adequacy of fusion of extruded poly (vinyl
chloride) PVC pipe and moulded fittings by acetone
immersion.
Test Specimen
Specimen shall be a size that is convenient to immersion in
the test container but not less than 13 mm in height.
Conditioning
Specimen shall be kept in an oven for 24 h at 50 ± 30 C,
cooled in desiccators and immediately weigh to the nearest
0.001 g.
Equipment
•Weighing balance: up to 0.001 g precision
•Micrometer flat ended: up to 0.025 mm precision
Reagents
Acetone: maximum density of 0.7857 g /ml at 25 0 C.
Procedure
• Place sufficient dried acetone in to the container to
ensurte complete immersion of the specimen
• Place the test specimen in the acetone, seal the
container and do not agitate. Allow specimen to stand
immersed for 20 min.
• After 20 min remove the specimen from the container ad
subject for sign of attack.
• Attack is described as lifting, raising or removing of any
material outside surface inside surface or mid wall of the
specimen. Swelling surface of test specimen shall not be
considering attack.
Result
Results can be expressed in terms of lifting, raising or
removing of any material outside surface inside surface
or mid wall of the specimen.
Factors influencing
• Thickness of the specimen
• Test condition: Temperature, Time (with in
saturation)
• Concentration of chemical.
IMMERSION TEST
Acetic Acid immersion test
Significance: This test is applicable for distinguishing
between specimens that are highly stressed and specimen
that are not provided that other conditions are the same.
Test Method
ASTMD 1939: Determining residual stresses in extruded or
moulded Acrylonitrile- Butadiene- Styrene (ABS) parts by
immersion in Glacial Acetic Acid.
Test Specimen
Specimen shall be complete moulding or a cut piece of the
extrusion or moulding of sufficient size to not influencing the
stress being observed. .
Conditioning
Specimen shall be kept in an oven for 24 h at 50 ± 30 C,
cooled in desiccators and immediately weigh to the nearest
0.001 g.
Equipment
•Weighing balance: up to 0.001 g precision
•Micrometer flat ended: up to 0.025 mm precision
Reagents
Glacial Acetic Acid: 99.7% assay.
Procedure
• Place the acetic acid in container to ensure complete
immersion of the specimen.
• Place test specimen in to the acitic acid for 30 s.
• At the end of time, remove and rince the specimen at
once in running water, wipe dry.
• Then carefully observe the cracking.
• If no crack the keep another specimen and observe
cracking at interval of 90 s, 2 min with same way.
Result
Results can be expressed in terms of no cracking, slight
cracking, moderate cracking , extensive cracking.
Factors influencing
• Thickness of the specimen
• Test condition: Temperature, Time (with in
saturation)
• Concentration of chemical.
References:
Vishu shah, “Hand Book of Plastics Testing Technology”
second edition, John Willy & Sons, 1998.
Related Indian & International Standard.
Handbook of plastics test methods, R.P.Brown, George
Goodwin Publication
Testing and Evaluation of Plastics, A. B. Mathur, I. S.
Bhardwaj, Allied Publication, New Delhi.
Allen. W.S and Baker, P.N, “Hand Book of Plastics
Technology” Vol.2, CBS Publishers, New Delhi, 2004