LESSON 3 TESTS FOR IDENTIFICATION OF FIBRES

STRUCTURE

3.0 OBJECTIVES

3.1 INTRODUCTION

3.2 RANGE OF TESTS TO IDENTIFY A W IDE RANGE OF FIBRES

3.3 MICROSCOPIC TESTS

3.4 BURNING TESTS

3.5 SOLUBILITY TESTS

3.6 ELEMENT IDENTIFICATION TESTS

3.7 DENSITY MEASUREMENT

3.8 DETERMINATION OF MELTING POINT

3.9 FEELING TEST

3.10 ASSIGNMENTS
3.10.1 CLASS ASSIGNMENTS
3.10.2 HOME ASSIGNMENTS

3.11 SUMMING UP

3.12 POSSIBLE ANSWERS TO SELF-CHECK QUESTIONS

3.13 TERMINAL QUESTIONS

3.14 REFERENCES

3.15 SUGGESTED FURTHER READING

3.16 GLOSSARY
 3. TESTS FOR IDENTIFICATION OF FIBRES
After classifying textile fibres in the first lesson of this unit, their properties
were described in the second lesson. This third and final lesson of the unit tells
you how the fibres can be identified.

3.0 Objectives
After going through this lesson, you will be able to;

• Identify fibres using a wide range of techniques.

• Observe the longitudinal and cross sectional microscopic view of different

fibres with their respective unique features.

• Understand the different burning characteristics of fibres.

• Distinguish between the fibre types using the criterion of solubility in a

chemical.

• Distinguish fibres on the basis of density and melting temperatures on the

basis of data.

3.1 Introduction
In recounting the history of textiles, it is generally not appreciated that till
about 100 years ago, it used to be an age of natural fibres dominated by cotton,
linen, jute, wool and silk fibres. As shown later in Table 3.1, because of some
unique features (like peanut like cross section of cotton, scaly structure of wool
fibre, triangular cross section of silk, etc.) these fibres could be identified by
examining their longitudinal and cross sections on a low-magnification
microscope. The first man-made fibre, viscose rayon, dates back to the end of
the 19th Century and it also had a distinctly different cross-sectional geometry
compared to the natural fibres of that time. However, as synthetic fibres were
discovered and commercially produced - the first being nylon 66 in 1938 followed
by nylon 6 in 1939, acrylic fibre in 1949, polyester fibre in 1943, polypropylene in
1957 – fibre identification became more complex because most of these synthetic
fibres were smooth with circular cross sections and a rather featureless
geometry. It therefore became necessary to extend the range of tests so that
given an unknown fibre, its exact identity should be specified.

A number of interesting developments that have taken place in the textile

industry have made the process of identification more complex. Only two of these
will be pointed out here. Large quantities of fabrics are now made from blended
yarns, e.g. the blend of cotton with polyester fibre represents a very popular
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product in which cotton confers comfort mainly due to its high moisture absorbing
capacity and polyester fibre gives the fabric a number of other desirable
characteristics, e.g. the requisite mechanical properties like strength and
durability. Also because of the ability of polyester fibre to dry quickly (drip-dry)
and its resistance to creasing, the fabric containing polyester fibre acquires the
well-known wash and wear characteristic. Yarns taken out from these fabrics will
thus contain both cotton and polyester fibres and the tests must be able to
identify both of them. The second development worth mentioning is that of
bicomponent fibres in which a single filament may contain two different fibre-
forming polymers - a core of polypropylene encased in a sheath of polyester.
Both there will be revealed during the test. These and other developments have
thus added a degree of complexity in the attempts made to identify the fibres and
one must take note of this.

3.2 Range of Tests to Identify a Wide Range of Fibres

There are around twenty fibres that must be considered whenever an
identification exercise for an unknown fibre is on. These include the natural
fibres, viz. cotton, wool, silk, linen, and jute (it may be mentioned that jute is being
blended in small amounts with other firbes for some textile fabric production).
Pineapple fibre is not included in this list as only very small amount of this fibre is
used. The second category comprises man-made fibres based on natural
feedstock, the major fibre in this category being viscose rayon. As noted earlier,
this is made by regenerating pure cellulose fibre from cellulose xanthate. A direct
route has now been found and Tencel and Lyocell are the trade names for man-
made cellulose fibres through the direct route. The two important chemically-
modified cellulose fibres that are made in small quantities are cellulose diacetate
and cellulose triacetate fibres. The third important category is that of synthetic
fibres and includes polyamides (nylon 66 and nylon 6), polyester (mainly
Polyethylene terephthalate or PET and small quantities of polybutylene
terephthalate), acrylic (polyacrylonitrile) and modified acrylic (modacrylic),
polyolefin (polypropylene and polyethylene) and polyurethane (Lycra, Spandex).
Amongst inorganic fibres asbestos, glass, metallic and carbon fibres are worth
mentioning. So given these twenty or so fibes, it is unlikely that a single test will
lead to its identification – there is a need to have a range of tests and the
following have been found to be particularly useful:

i) Microscopic examination of the longitudinal and cross sections of the

fibre,

ii) Burning test in a flame, and

iii) Solubility tests in chemical reagents.

In addition to these three tests, the following four tests also provide useful
information:

iv) Element identification

v) Density measurement

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 vi) Determination of melting point, and

vii) Feeling test.

In practice, identification tests are used in combination. The various tests

listed above will now be briefly described.

3.3 Microscopic Tests

The microscopic test reveals the macroscopic features of the fibre. When
observed along the length (longitudinal section), the surface features are
revealed. When a fibre is cut in the perpendicular direction and a thin cross-
section examined on the microscope, the shape of the cross-section and the
macroscopic features in the cross-section can help identifying some fibres.

An optical microscope with a magnification of at least 100 is generally

used. A projection microscope is however, preferred since it gives an enlarged
view on the screen, which can be traced on a tracing paper. If the microscopes
are of the polarizing type, the contrast is sharper and more information can be
collected. Thus polarizing projection microscopes allow greater amount of detail
and are therefore generally used.

To examine the fibre in the longitudinal direction, a few fibres (or a few
short lengths of cut filaments) are straightened and parallelized and placed on a
glass slide. They may be secured with the help of cellotape on both ends. To
reduce scattering of light, the fibre is immersed in a drop of inert liquid having a
refractive index close to the refractive Index of the fibre and covered with a cover
glass. The sample is then mounted on the microscope stage and its focussed
image observed on the screen. The longitudinal texture may then be traced on
tracing paper.

The cross-section can be made as follows: A bundle of straight and

parallel fibres is embedded in a cork with the help of a needle in which the yarn or
filaments are threaded. A thin section of the cork is then carefully cut using a new
blade and this thin section is then placed on a glass slide and secured with
cellotape. The assembly is mounted on a microscope. The cross sectional view,
when combined with the corresponding longitudinal view, may then assist in
identifying the fibre. The cross-sectional (top) and longitudinal sectional (bottom)
views of cotton, wool and silk fibres taken on a scanning electron microscope are
shown in Fig. 3.1 and it is interesting to observe that the characteristic features of
these fibres are quite different and thus can assist in their identification.

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The characteristic features shown by some other fibres are shown schematically
in Fig. 3.2.

Fig. 3.1 Cross section (top) and longitudinal section (bottom) of cotton (left), wool (middle) and silk
(right) fibres.

Fig. 3.2 Cross- section (top) and longitudinal section (bottom) of some common fibres.

It may be added that important synthetic fibres like polyester and nylon are
generally made with circular cross section and their longitudinal and cross
sectional views are featureless and are not of great assistance in identifying
them. However, it is worth pointing out that fibres with non-circular cross-sections
(trilobal, triangular, octagonal, etc.) are also made in small quantities.

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 The common observations that may be made from an examination of the
longitudinal and cross sectional views of a number of fibres are summarized in
Table 3.1.

Table 3.1
Microscopic Appearance of Some Common Fibres

Fibre Longitudinal Section: Appearance Cross-section: Appearance

Cotton Flat, irregular convoluted ribbons Peanut or bean shaped with
which change direction with the twist lumen* running through the *length.
(mercerised cotton is smoother and
less irregular)
Wool Rough surface with scales Nearly round, medulla present in
protruding out coarse fibres is concentric and
irregular in size.
Silk (degummed) Smooth with distinct lengthwise Mostly triangular, irregular.
striations.
Viscose Rayon Striated, smooth Irregular, serrated
Nylon, polyester, Smooth, rod-like Regular, round
polypropylene
Acrylic Flat, irregular striations Irregular, dog-bone shape

*Lumen is an irregular hole running through the middle. While cutting the cross-section, it
may sometimes get covered.

Self-check Questions
1. Answer the following questions in terms of Yes/No.

i) The cross sections of the following fibres show unique features:

a. Polyester Yes / No
b. Cotton Yes / No
c. Wool Yes / No
d. Nylon Yes / No
e. Jute Yes / No

ii) The longitudinal sections of the following fibres show unique

features.

a. Cotton Yes / No
b. Wool Yes / No
c. Polyester Yes / No
d. Polypropylene Yes / No
e. Silk Yes / No

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3.4 Burning Tests
The fibres being chemically different, they show different burning
characteristics which can be used to identify them. The burning test is a relatively
simple test as all that is needed is a flame and a keen observer who should
carefully watch and note down the observations made (a) when approaching the
flame, (b) on the burning behaviour inside the flame, (c) during removal from the
flame, (d) relating to the smell emitted, and (e) on the residue left behind after the
fibre has burnt out.

The observations made on the burning behaviour of some common fibres

are summarised in Table 3.2

Table 3.2
Burning Behaviour of Common Fibres

Fibre Approaching In Flame Behaviour Smell Residue

flame outside the
flame
Cellulose Do not shrink Burn readily Continue to Burning hair Small amount of
Fibres without burn, after- light gray ash
(Cotton, melting glow
viscose)
Wool, silk Curl away Burn slowly Self- Burning hair Easily crushable
sputter extinguishing black bead
Asbestos Does not Does not Retains None Same as original
shrink burn, glows shape
Polyester Shrinks away Melts, burns Burns, drips, Sweet smell Hard, tough,
from flame slowly, drips may of ester gray bead
extinguish
because of
dripping
Nylon -do- -do- -do- Pungent, Hard, tough, light
burning colour
beans
Polypropylene -do- -do- Continues to Burning Hard, tough, tan
burn plastic bead
Acrylic -do- Burns -do- Acrid Irregular, hard,
readily, black bead
sputters

Activity
1. Take a cotton fibre and a polyester fibre. Burn the two fibres separately
and write down your observations.

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3.5 Solubility Tests
The solubility of fibres in some specific chemical reagents (acid, alkali,
bleaching agent, solvent) provides a definite means of identification, if not for a
specific fibre, then for a generic group. When combined with the results of
microscopic and burning tests, the results of solubility test make it possible to
identify the fibres in most cases.

There are different schemes for making solubility tests-of course they must
be carried out in a prescribed order as they work on the principle of elimination.
The following represents one such scheme meant to identify an unknown fibre:

Step 1: Treat the fibre sample with 0.25-0.50% sodium hypochlorite solution. If
soluble, they may be wool or silk. (To distinguish between the two, treat
the fibre in cold 70% sulphuric acid- if soluble, it is silk, otherwise wool.
Alternately, test the fibre for sulphur, which is present in wool). If the
fibre is insoluble in sodium hypochlorite, go to Step 2.

Step 2: Treat the fibre with cold acetic or glacial acetic acid. If soluble, the fibre
could be cellulose diacetate or cellulose triacetate. (To distinguish
between the two, treat the fibre with methylene chloride. If soluble, it is
cellulose triacetate, if not cellulose diacetate). If the fibre is insoluble, go
to Step 3.

Step 3: Treat the fibre with cold (heat if necessary) formic acid. If soluble, the
fibre is nylon 66 or nylon 6. (To distinguish between the two, treat the
fibre with boiling dimethyl formamide (DMF). If soluble it is nylon 6,
otherwise nylon 66. Alternately determine their melting points. Nylon 6
melts at 218º C, nylon 66 at 265ºC). If the fibre is insoluble, go to Step 4.

Step 4: Treat the fibre in cold DMF. If soluble it is acrylic fibre, if insoluble, go to
Step 5.

Step 5: Boil the sample in chlorophenol. If soluble, it is poly (ethylene

terephthalate) (polyester) fibre. If insoluble, go to Step 6.

Step 6: Treat the fibre with 70% sulphuric acid. If soluble, it could be cotton or
viscose rayon (To distinguish between the two, treat them with sodium
Zincate. If soluble, it is viscose rayon). If insoluble in step 6, go to step 7.

Step 7: Put the sample in water. If it floats, it could be polypropylene (PP) or

polyethylene (PE). PP is soluble in boiling carbon tetrachloride, PP is
soluble in boiling xylol.

Some additional tests listed below may be performed for further

confirmation:

i) Nylon 66 and Nylon 6: Soluble in formic acid (85%) and m-cresol

ii) Cellulose triacetate: Soluble in chloroform and methylene dichloride
iii) Wool: soluble in 5% NaOH at room temperature
iv) Silk: Soluble in 5% NaOH (hot)
v) Viscose rayon: dissolves in sodium zincate solution
vi) PET: Dissolves in orthochlorophenol at room temperature.
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 vii) Asbestos, glass: do not dissolve in common organic or inorganic
solvents.

(Lately the use of asbestos fibre in any product has been banned in many
countries because of its suspected carcinogenic effect).

The other identification tests listed earlier will now be briefly considered:

Activity
2. Take some unknown fibres (both natural and synthetic). Perform burning
tests on them and note down the observation made. Try to identify them
on the basis of the observations made.

Self-check Questions
2. State whether the following statements are True / False.

i) Element nitrogen is present in cotton fibre. True/False

ii) Nylons are the lightest fibres. True/False
iii) Viscose rayon is a protein fibre. True/False
iv) The presence of oxygen element in a textile fibre raises its
density.
True/False
v) Out of the three major tests used to identify fibres, solubility test
gives the most definite information.
True/False
vi) Wool burns readily. True/False
vii) Asbestos is resistant to solvents. True/False
viii) It is safe to wash wool with ordinary washing soaps. True/False
ix) Acrylic fibre floats in water. True/False
x) Silk fibre melts and drips on burning. True/False

3.6 Element Identification Tests

Tests for nitrogen and chlorine are sometimes performed for identifying
nylon, Lycra, acrylic (nitrogen) and modacrylic (chlorine) fibres.

3.6.1 Test for detecting the presence of nitrogen (Soda lime test)

Cover a few fibres in a small ignition tube with soda lime, plugging the
mouth of the tube with glass wool to prevent spitting. When the tube in heated,
ammonia will be found in the vapour if the fibre contains nitrogen. The vapour
being strongly alkaline will turn litmus paper blue.

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3.6.2 Test for detecting the presence of chlorine

Heat a copper wire in a bunsen flame until the flame is no longer of green
colour. Then take this wire out of the flame and while still hot, touch the fibres
with the wire. Thermoplastic fibres will adhere to the wire. Place the wire with the
fibres attached in the flame - a green colour will indicate the presence of chlorine.

3.7 Density Measurement

The definition of density is derived from the relationship volume X density
= mass, i.e. density is the mass per unit volume of a substance and its units, are
gm/cm3. It can be accurately measured using a density gradient column
(described in suggested reading at no. 4). The density data on common fibres are
shown in

Table 3.3
Fibre Density Data
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Fibre Density (gm/cm )
Cotton 1.52-1.55
Viscose rayon 1.49-1.52
Linen 1.53-1.55
Jute 1.49-1.50
Polynosic 1.50-1.52
Cellulose diacetate/Triacetate 1.30-1.35
Wool 1.30-1.33
Silk 1.25-1.34
Nylon 6/Nylon 66 1.14
Polyester 1.38-1.40
Acrylic 1.16-1.19
Modacrylic 1.29-1.34
Spandex 1.20-1.25
Polyethylene (Low density) 0.92-0.94
Polyethylene (High density) 0.95-0.97
Polypropylene 0.91
Glass 2.50-2.54

3.8 Determination of Melting Point

The melting temperature of a fibre can be very accurately determined with
the help of a differential calorimeter (described in suggested reading no. 4). The
data on some common fibres is given in Table 3.4.

Table 3.4
Melting Temperature Data of Some Fibres

Fibre Melting temperature

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 Natural
Cotton Decomposes around 250ºC before softening/melting
Wool 220ºC
Silk Decomposes at 280ºC before it melts
Man-Made
Viscose rayon Decomposes before softening/melting
PET (Polyester) 265ºC
Nylon 6 218ºC
Nylon 66 265ºC
Acrylic 320ºC (May decompose before melting)
Polypropylene 165ºC
Polyethylene (Low den.) 115ºC
Polyethylene (High den.) 135ºC

3.9 Feeling Test

It is a subjective test and can only be performed by one with skill in this art
acquired after handling many different fabrics over a period of time-this refines
the individual’s perception, e.g. when he feels fabrics through his fingers, the
warmth in the finger is retained when the fibre is wool but is conducted away
when touching fibres like cotton, linen or rayon, the fabrics thus feel cold to touch.

Cotton is cool to touch and feels soft and inelastic. Linen is cold and
smooth and has a leathery feel. However, the feeling test has its limitations and
cannot always be relied upon.

Self-check Questions
3. Match the following.

i) Nylon 66 fibre a. Scaly surface

ii) Low density polyethylene b. Cellulosic fibre
iii) Polypropylene fibre c. Lowest melting temp
iv) Wool fibre d. High melting temp.
v) Silk fibre e. Triangular cross section
vi) Jute fibre f. The lightest fibre

3.10 Assignments
3.10.1 Class assignments

i) You may pick up a few numbered samples of fibres from out of those
available and try to identify them using facilities made available to you. A
report of the experiments performed and the conclusions reached should
be submitted.

3.10.2 Home assignments

i) On a chart paper, draw the longitudinal section and cross sectional view of
some common natural and synthetic fibres.

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3.11 Summing Up
In this lesson, the tests which are usually performed to identify fibres are
described. These include microscopic tests, burning tests, solubility tests, density
and melting point measurement, etc. On the basis of the information, an unknown
fibre can be identified using data obtained from these tests individually or in
combination. The investigation must be systematic and scientific.

3.12 Possible Answers to Self-check Questions

1. State whether the following statements are Yes / No.

i) a) no b) yes c) no d) no e) yes

ii) a) yes b) yes c) no d) no e) yes

2. State whether the following statements are True / False.

i) False
ii) False
iii) False
iv) True
v) False
vi) False
vii) True
viii) False
ix) True
x) False

3. Match the following

i) d
ii) c
iii) f
iv) a
v) e
vi) b

3.13 Terminal Questions

1. Explain the scientific basis of the following questions. If necessary, consult
relevant literature.

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 i) Though cotton burns readily, ladies are advised to wear cotton saris
while working in kitchen or during Deepavali and not saris of synthetic
material. Why?
ii) Why is wool warm to the touch and cotton cool?

3.14 References and

1. Gupta, V.B. and Kothari, V.K. (Eds.). 1997. Manufactured Fibre
Technology. (Gupta, A.K. Chapter 10 Characterization of Polymers and
Fibres. Pp. 203-247). Chapman & Hall. London.

2. Kothari, V.K. (Ed.) Quality Control. (Sen, K. Chapter 4 Textile Fibres:

Classification and Identification, Pp.46-54.) Textile Dept. IIT, New Delhi.

3. Sreenivasa Murthy, H.V. 1987. Introduction to Textile Fibres. The Textile

Association (India), Mumbai.

3.15 Suggested Further Reading

4. British Standards Institute. British Standards Handbook No.11. 1963. Pp.
391-432.

5. Dave, M.S. (Ed.). 1980. Textile Fibres. (Chapter 6 Chemical properties of

fibres).Textile Association (India), Ahmedabad Unit, Ahmedabad.

3.16 Glossary
1. Polarizing Cause to vibrate in one direction only instead of
all directions

2. Refractive index The ratio of the velocity of light in a vacuum to

that in the medium

3. Medium the carrier

4. Ignition The act of starting a fire

5. Bunsen flame A gas burner used in laboratories; has an air

valve to regulate the mixture of gas and air

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