Identification of natural textile

fibres 14
R. Nayak 1 , S. Houshyar 2 , A. Khandual 3 , R. Padhye 2 , S. Fergusson 2
1
School of Communication and Design, RMIT University Vietnam, Saigon, Vietnam; 2School
of Fashion and Textiles, RMIT University, Brunswick, Australia; 3Department of Textile
Engineering, CET Bhubaneswar, Bhubaneswar, Orissa, India

14.1 Introduction
The identification of textile fibres is important for textile and apparel manufactures,
fashion designers, automotive industries and forensic science. The identification
methods, however common across disparate industries, are conducted very differently
in each. Some methods are exclusively used by one group; others are shared, while
some shared methods have greater or lesser utility for the analyst. Differences in phys-
ical and chemical properties are the basis for fibre identification. Generally, simple
tests are enough to enable a fibre to categorize into the main groups of natural fibres
where the differences in properties are relatively large. More complicated tests are
essential to distinguish between fibres within a group. Many fibres can be identified
by fairly simple tests needing only inexpensive equipment.
Although some new instrumental identification techniques originated with the tech-
nical developments, the old methods are often considered to be the best. Most labora-
tories will still rely on the simplest microscopical examination, which provides a range
of analysis barely possible with any other method. Combined with spectroscopy,
microscopy is the quintessential fibre identification tool. Instrumental methods of
identification provide reliable means to distinguish between the main types of fibres
according to their chemical structure and closely related fibres with only minor differ-
ences in properties.
The American Association of Textile Chemists and Colourist (AATCC) technical
manual lists microscopy as useful method for fibre identification, whereas American
Society for Testing and Materials (ASTM) reports infrared (IR) spectroscopy with
additional physical properties as preferred method for fibre identification. AATCC
also lists reaction of fibres to flame (such as melts near flame, shrinks from flame
and burns in flame) as a test method for fibre identification. The amount of sample
for analysis is nearly unlimited for producers, while it is minimal in the case of forensic
analysis. Therefore, different methods are devised for fibre identification. For both the
analysis the common parameters are determining the individual fibre’s morphological,
optical and chemical properties as distinctly as possible.

Handbook of Natural Fibres. https://doi.org/10.1016/B978-0-12-818398-4.00016-5

Copyright © 2020 Elsevier Ltd. All rights reserved.
504 Handbook of Natural Fibres

14.2 Natural textile fibres

A natural fibre is any fibre that exists as such in the natural state, such as cotton, wool
or silk (Houck, 2009). Natural fibres differ from each other in cross-sectional (CS)
shape, colour, surface contour, chemical structure as well as length and width
(Ziabicki, 1976; Nayak et al., 2012). The natural textile fibres can be classified into
three groups such as vegetable, animal and mineral according to their origin. But
only the vegetable and animal fibres will be discussed in this chapter.

14.2.1 Vegetable fibres

Vegetable fibres are mainly collected from different parts such as seed (cotton, akund,
kapok, coir); bast (flax, jute, hemp, ramie, kenaf) and leaf (sisal, abaca) of various
plants. The vegetable fibres are also called cellulosic fibre as cellulose is the main
component of the fibres. Additional information on vegetable fibres can be obtained
from Chapters 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, published in Vol. 1 of the Handbook of
Natural Fibres. The identification of vegetable fibres includes the analysis of the
size and relative thickness of cell wall; shape and thickness of lumen; the presence,
type and distribution of dislocations and the direction of twist of the cellulose in the
cell wall (Greaves, 1990). Additional information on vegetable fibres can be obtained
from Chapters 2 and 3 of volume 1.

14.2.1.1 Seed fibres

Cotton is the most common seed fibre and accounts for approximately half of all textile
fibres processed annually. The unique feature of cotton fibre is the presence of lumen
and convolutions, which makes identification easier. Convolutions are twists in the
fibre with many reversals along the fibre length, which are clearly visible in the polar-
ized light of the microscope. Cotton can be distinguished from other fibres under the
microscope between crossed polars (Perry et al., 1975). It remains substantially bright
in all orientations, except that in the orthogonal positions dark bands cross the fibre at
frequent intervals indicating the reversal points of the underlying spiral structure.
The appearance of cotton can be modified by specific chemical finishing to get
desired result e.g., mercerization of cotton causes fibre swelling and untwisting. There-
fore, the convolutions in mercerized cotton may not be easily visible (because of fibre
swelling). Generally, the cross-section of cotton is kidney shaped and in case of
mercerized cotton it is circular. Resin treatment and some other chemical finishes
can alter the appearance of cotton fibre.
For preliminary identification of cotton, add a drop of cuprammonium hydroxide to
the fibres mounted on a slide and examine under microscope (a) if the fibres dissolve
readily and completely, it is scoured cotton or mercerized cotton; (b) if the fibres swell
irregularly, forming beads and finally dissolve leaving a residue of particles that float
away in the solvent, it is raw cotton and (c) if the fibres remain undissolved, it is chem-
ically modified cotton. Iodine test can also be used to distinguish between mercerized
and unmercerized cotton (Marsh, 1941). In this test cotton fibre is treated with a
Identification of natural textile fibres 505

specific iodine solution, and if the fibre decolourizes immediately, it is unmercerized

cotton. Mercerized cotton takes several hours for discolouration.
Other seed hairs such as akund, kapok and coir are readily distinguished from
cotton by thin cell wall and absence of convolutions. Akund is fine, soft and lustrous
but very weak like kapok. The appearance of akund under microscope is similar to
kapok, but the base does not show the net-like thickenings seen in kapok. Kapok fibres
are smooth, hollow, cylindrical, thin-walled, brittle and frequently bent over on it. Coir
fibres are very stiff, dense and have distinct cross-section, which makes easier to
identify by microscopy. Coir appears dark brown or opaque with very large, coarse
ultimates under microscope.

14.2.1.2 Bast fibres

The colour of the bast fibres depend upon the retting conditions, e.g., the colour of
water retted fibre is from white to yellow and the colour of dew retted fibre is from
grey to dark silver. Flax has clockwise twist, polygonal cross-section of ultimates
with thick walls and small lumina. The feature of flax fibre, which is common with
other bast fibres is the presence of dark dislocations, often in the form of an ‘X’ under
microscope that are roughly perpendicular to the longitudinal axis of the fibre. On the
other hand jute has counterclockwise twist, microscopically it appears bundled and
may have a yellowish cast. It has polygonal cross-section of the ultimates, which
are angular with medium sized lumina.
The characteristic features of hemp differ from jute with more bundled ultimates,
wider lumen and fewer nodes. Also the rounder and more flattened cross-section of
hemp helps to distinguish it from jute. Hemp has counterclockwise twist like jute
and may also have a brownish cast to it. Ramie has thick wall, flattened cross-
section, very wide ultimates with the width ranging from 25 to 75 mm. Microscopically
ramie has frequent, short dislocations, longer transverse striations and radical cracks
may be present in cross-section. Kenaf, with an ultimate fibre length from 2 to
6 mm is more lustrous, harder and stronger than jute; and lighter in colour. The reader
can find more pieces of information on bast fibres in Chapters: 3, 4, 5, 6, 7 and 18 of
volume 1 and Chapters: 2, 4, 5, 6, 7, 11, 12, 17, and 19. of volume 2.

14.2.1.3 Leaf fibres

The irregular lumen size, acicular crystals, spiral elements and annular vessels are the
features for identification of sisal. The cross-section of sisal looks like cut celery, and it
has counterclockwise twist. The features for identification of abaca are uniform diam-
eter of ultimates, waxy appearance, polygonal cross-section and counterclockwise
twist. Abaca may contain spiral elements but often will have stegmata, which are
visible as small crown-like structures. Sisal is distinguished from abaca by Billing-
hame’s test (Perry et al., 1975).
506 Handbook of Natural Fibres

14.2.2 Animal fibres

The animal fibres with protein as the main component include wool, hair and silk
fibres. Although the chemical structure of hair fibres are related to wool, the physical
characteristics are different, i.e., they differ in length, fineness, shapes and internal
structure, which can be used for their identification. More pieces of information on
wool are available in Chapters 11 and 12 (volume 1) and about silk in Chapters13
and 21 (volume 1) and in Chapter 3 (volume 2).

14.2.2.1 Wool
Wool is obtained from the hair of sheep and certain other animals, including cashmere
from goats; mohair from goats, alpaca and animals in the camel family and angora
from rabbits. Wool can be identified by careful microscopical examination of features
such as CS outline, pattern formed by the scale margins, regularity of fibre diameter,
type of medulla and thickness of cuticle. The morphology of these fibres is complex,
consisting of a cortex covered by a cuticle of scales and in some instances a central
medulla, often showing different patterns in different fibres. Finer wool fibres
(e.g., merino wool) have no detectable medulla. The finest merino wool appears strik-
ingly irregular in diameter when seen under microscope. The medulla in long wools
and crossbred wools is simple unbroken, medium to narrow type.
At the beginning, the animal hair fibre to be identified should be confirmed that it is
not human in origin. This is done from the banding characteristics (abrupt and
profound colour changes along the hair shaft) of the animal hair. The complete iden-
tification of animal hair fibres mainly relies on the morphological features of the
cortex, the size and shape of the scales and their pattern around the hair. The scale pat-
terns may be visualized by mounting the hairs in a semipermanent mounting medium
with a refractive index lower than that of keratin (1.55) or it can be done by a scanning
electron microscope (SEM). The advantage of SEM is its very high resolution and
relatively large depth of field, which enables a better discrimination of the surface char-
acteristics. However, in SEM no internal features are visible, and due to the thin
coating, the further examination of the fibre is not possible.
If the origin of the animal fibre is unknown, determining the diameter of the fibre
assist in the identification (Houck, 2009). The medulla types and scale patterns vary in
hairs of different species, which can be used for differentiation. Heat treatment and
some chemical finish such as alkaline treatment, bleaching or chlorination can modify
the structural characteristics of wool. Chlorination causes the scale margins gradually
less prominent and may be complete removal with severe treatment.
Hamlyn et al. (1992) applied molecular biology techniques for the identification of
animal hair fibres (wool, cashmere and mohair). In this technique, specific DNA
probes were developed, which can distinguish between DNA isolated from closely
related species. This technique is helpful for forensic analysis and biomolecular palae-
ontology. The chemical resistance of similar type of fibres such as wool, cashmere and
mohair to solvents is very similar. Therefore, solubility test cannot be used to
Identification of natural textile fibres 507

distinguish among these fibres. In these cases, scale height (Kusch and Arns, 1982;
Wiedemann, 1987; Robson, 2000), scale pattern (She et al., 2001), scale frequency
(Robson, 2000) and evenness of diameter (Langley and Kennedy, 1981) may be
used in distinguishing between wool, cashmere and mohair fibres. She et al. (2001)
used image processing and Artificial Neural Network (ANN) model to classify mohair
and merino fibres on the basis of the scale pattern.

14.2.2.2 Silk
Silk is a natural protein fibre mainly produced by the larvae of insects that complete
metamorphosis. The best type of silk is obtained from the cocoons of the mulberry
silkworm (Bombyx mori). Unlike the wool fibres, silk fibres are generally easy to iden-
tify. The filaments of B. mori in gummed state are stuck together in pairs and covered
with sericin. These silk filaments when degummed have smooth and uniform surface,
semitransparent appearance and approximate to equilateral triangles with rounded
apices cross-section.
Mulberry silk shows a triangular cross-section and a smooth surface, which mark-
edly differ from the nonmulberry (wild) silk (Sen and Babu, 2004). The wild silk
appears flat and ribbon-like with fine longitudinal lines. The cross-section of other silks
can vary in shape, e.g., crescent-like for Anaphe and elongated wedge-shaped for
tussah.
Spider silk is a protein fibre spun by spiders with mechanical properties superior to
silkworm silk (Cunniff et al., 1994). It has a unique combination of strength, elasticity
and resistance to compression, which is judged to be superior to that of synthetic fibres
made of polyamide or polyester. Some specimens exhibit over 200% elongation and
others possess tensile strengths equivalent to high performance fibres. Also compared
with silkworm silk, it is more waterproof. In spite of many superior properties, spider
silk has not been domesticated for textile applications because of difficulties associated
in raising dense populations of spiders due to their solitary and predatory nature; reel-
ing of a single fibre from the spider webs is difficult and the amount of silk generated
by spiders is small in comparison to the silkworm cocoon silk (Mukhopadhyay and
Sakthivel, 2005).
Artificial spider silk has already been spun successfully. The race is now on the
perfection of spinning technology. The most promising methods till now include con-
ventional solvent spinning of recombinant spider silk protein analogue (Du Pont Ltd)
(O’brien et al., 1998) and extruding regenerated silk into a coagulation bath using a
nanofabricated silicon spinneret (Seidel et al., 1998).
Care must be taken while identifying the silk fibre because of its similarities with
nylon fibre in fibre diameter and infrared spectra. However, silk is less regular in
appearance along its length than a nylon fibre. If difficulties are faced in identifying
these fibres, place a short segment or cross-section of the fibre in question in a hot
stage. Nylon will melt, and silk will not. Fluorescence microscopy may provide
additional features based on the fluorescence of the dyes.
508 Handbook of Natural Fibres

14.3 Identification methods

The identification of textile fibres is an important and challenging task. As there are
many ways of identifying textile fibres, there is no strict routine test method followed
by the textile analyst. Fibres are identified by one or more test methods in combination
such as physical appearance, burning test, microscopic analysis, solubility test,
staining test and physical property analysis. Although conventional approaches such
as microscopy, burning test, staining test and solubility tests are easy to conduct,
they have several limitations:
1. These methods are subjective and rely heavily on expertise.
2. These methods are destructive as there is fibre damage during the test.

14.3.1 Identification by physical appearance

It may be said with some justification that the simplest and most obvious way to iden-
tify a fibre is to look at it. As the physical appearances of fibres differ from each other,
it can give a preliminary indication for fibre identification. Successful identification of
fibres depends on experience and familiarity with the fibres. This method is subjective
and often not sufficient for the complete identification.

14.3.2 Burning test

This is the first step in the fibre identification (BIS, 1981). This test relies on the behav-
iour of the fibre when exposed to a flame depending on the chemical composition of
the fibre. In this method a small tuft of fibre is held by forceps for about 10 s in the
flame of a burner and then removed (BIS, 1981). The behaviour of the fibre to the
flame (whether it burns, shrinks, forms any bead, the type of smell emitted, nature
of remnant ash) helps in identifying the generic type of the fibre. This method is still
used in industry where the composition of an unlabelled bale of fibre needs to be iden-
tified. This method is very quick and can be performed almost anywhere. However, the
test is subjective and destructive, consumes a considerable amount of material and can
produce toxic fumes sometimes. Table 14.1 describes the burning behaviour of
different natural textile fibres.

14.3.3 Microscopic analysis

Microscopical analysis is indispensable for positive identification of several types of
cellulosic and animal fibres and also for distinguishing these fibres from man-made fi-
bres (ASTM, 2000). The distinguishing features of each fibre though not enough for
confirmatory identification, help to categorize into the correct group. The features
include convolutions, lumen and reversal zones (cotton); fibre bundles with or without
cross-markings (bast and leaf fibres); presence or absence of scales and scale margins
(animal fibres) and smooth profile without scales or convolutions (silk). The other
Identification of natural textile fibres 509

Table 14.1 The burning behaviour of natural textile fibres.

Behaviour of
fibre Cellulosic fibres Wool Silk

When Does not fuse or Fuses and curls away Fuses and curls
approaching shrink away from flame away from flame
flame from flame
When in flame Burns quickly Burns slowly with some Burns slowly with
without melting melting some melting
After removal Continues to burn Burns very slowly, Burns very slowly,
of flame without melting usually self- sometimes self-
afterglow extinguishing extinguishing
Melts near No Yes Yes
flame
Shrinks from No Yes Yes
flame
Burns in flame Yes Yes Yes
Continues to Yes Slowly Slowly
burn
Smell Burnt paper Burnt hair Burnt hair
Appearance of Small, light grey Lumpy, blistered, Soft, round, black
ash irregular, black ash, bead, brittle,
brittle, breaks easily pulverizes easily
More data about flammability and flame retardancy of natural fibres the reader can find in chapter 10, volume 2.
Adapted from Lyle, D.S., 1977. Performance of Textiles, John Wiley and Sons, New York, USA.

features include longitudinal shape, regularity of diameter and any distinguishing char-
acteristics. But sometimes, the morphological differences among some species are not
always sufficiently distinctive for precise identification because nature tends to use the
same repertoire of cells in constructing the fibres of different plants (Goodway, 1987).
Microscopy has and will remain an important aspect of fibre examination (Palenik,
1999) primarily for both vegetable and animal fibres (Catling and Grayson, 1982;
Brunner, 1974; Palenik, 1983; Cook, 1969). This method applies various microscopies
such as light microscopy, stereomicroscopy, scanning electron microscopy and
infrared microspectroscopy. The light microscopy usually provides information about
the shape and interior structure of fibres, not about the external features. A stereomi-
croscope can record fibre characteristics such as size, crimp, colour and luster.
The external features of fibres can be observed by SEM with very high resolution
and relatively large depth of field than the optical microscope. In SEM images the
complete surface of a fibre can be seen in high detail, which gives a better discrimina-
tion of the surface characteristics. In this process, the fibres are made conductive by
coating with a layer of conducting metal to allow the charge acquired from the incident
510 Handbook of Natural Fibres

electron beam to run to earth. The ability to portray surface topographies with such
clarity has targeted the main application of SEM in fibre identification towards natural
rather than synthetic. The IR microspectroscopy is widely used in forensic analysis.
A mounting medium (such as liquid paraffin) with a refractive index about a 10th
higher than that of natural fibres can be used as a convenient method of enhancing
contrast at the surface of the fibre so that surface details become distinctly visible in
light microscopy (Perry et al., 1975). Microscopical analysis includes the longitudinal
and CS examination. In longitudinal examination a small amount of fibre is placed on a
glass slide with a suitable mounting medium and covered with a covering glass. The
fibres are examined at a specific magnification, which provides a strong indication of
the type of fibre present. If the longitudinal analysis fails for identification of a fibre, it
is necessary to go for CS analysis. The CS of different types of natural fibres are
different, and they vary in diameter, i.e., from 10 to 13 mm (cultivated silk) up to
40 mm (US wool).
In CS analysis, the CS of a fibre is prepared with a cross-sectioning device, placed
on a glass slide with a suitable mounting medium, covered with a covering glass and
examined at a specific magnification. The CS can be prepared by microtome, hand-
sectioning (by the use of a cork, a C-clamp and a razor blade) and the plate technique
(Wildman, 1947). For better quality, the hardy microtome is used for cutting the CS. In
some cases despite of cutting the fibre CS, the CS can be inferred by slow focussing
upon the fibre at fairly high powers. This method is called optical sectioning, which is
quicker and much less tedious procedure than cutting CS. The longitudinal and CS im-
ages along with the features of different natural textile fibres are shown in Table 14.2.
Langley and Kennedy (1981), by using a combination of light microscopy and
SEM examinations, suggested that the earlier criteria for identifying wool, mohair
and cashmere were unreliable. The combination may be the correct and most reliable
means of identification by microscopy, which reveals different characteristics of the
fibres involved. However, Kadikis (1987) argued that the light microscopy reveals
more information about the structure and internal characteristics of animal fibres
than SEM, and hence the optimum instrument for such analysis. He also stated that
the analyst working in this field should possess years of experience, a good visual
memory, patience and the intellectual honesty to recognize when a fibre is difficult
to be identified.
Both the light microscopy and SEM should be used in conjunction rather than being
in competition, as each will have its advantages for circumstances. Extensions of the
SEM technique include energy dispersive X-ray (EDX), scanning tunneling micro-
scopy (Spurny and St€ ober, 1981) and plasma etching (Alfy and Blakey, 1980).
Microscopic analysis is the quickest, accurate and least destructive in determining
the types of fibres. Forensic analyzers use first microscopy as preliminary identification
and then other methods for confirmatory identification.

14.3.4 Solubility test

Solubility tests were widely used for fibre identification before the development of
modern instrumental methods. The generic fibre types are identified by the solubility
Table 14.2 Microscopic views and features of natural fibres.
Longitudinal Cross-sectional
view view Longitudinal features
Ribbon-like, flattened structure with
frequent convolutions, sometimes
changing directions; distinct but
small lumen, containing
protoplasm in raw fibre. Thin walls
and few convolutions in immature
fibres.
Ribbon-like fibres and fibre regions
or less frequent depending on
degree of mercerization; with
greater part cylindrical and
smooth; very small lumen or
disappeared.
Smooth and cylindrical with rounded
base; no convolutions or other
structure except at the ends. When
mounted in water, shows large,
elongated air bubbles.
Fibre bundles with cross-markings,
longitudinal and transverse
fissures.
Identification of natural textile fibres
Cross-sectional features Fibre name
Flat, elongated or kidney Cotton (raw and
beaneshaped, seldom round or bleached)
oval; lumen as a line or oval. Some
very thin-walled sections of
immature or dead fibres.
Most fibres round or oval (number Cotton (mercerized)
depending on degree of
mercerization); very small lumen
as a small central spot or no lumen.
Circular or slightly elliptical; thin Kapok and akund
wall and large lumen.
Bundles (and possibly some Ramie (raw, before
individual fibres). degumming)
511
Continued
Table 14.2 Continued
Longitudinal Cross-sectional
view view Longitudinal features
Isolated individual fibres, very broad
and ribbon-like with infrequent
twists; cross-markings,
longitudinal and transverse
fissures.
Fibre bundles, cross-markings,
nodes, fissures, but otherwise
smooth.
More or less isolated ultimate fibres
depending on degree of bleaching;
cross-markings, nodes, fissures but
otherwise smooth.
Fibres cylindrical, smooth, few cross-
markings and nodes visible.
Mixture of bundles and single fibres.
Same as mercerized
512
Cross-sectional features Fibre name
Long and narrow lumen or same Ramie (degummed,
shape as fibre section. Elongated and possibly
polygons, often with curved side- bleached)
lines, and sometimes rounded;
thick wall, and radial fissures.
Shape and size of fibre bundles partly Flax (raw)
depends on preparation; ultimate
fibres mainly sharply polygonal
with narrow, round or oval lumen;
also rounded oblong forms with
larger lumen.
Flax (bleached)
Flax
(mercerized)
Flax (cottonized)
Handbook of Natural Fibres
(Crease-resistant)

Similar to flax.
9
Fibre bundles, very rarely cross-
markings; nodes or fissures;
ultimate fibres (bleached or
macerated) with lumen
considerably varying in size along
2 the same fibre.
Irregular diameter and prominent
scale margins. Medulla present in
some medium and coarse fibres;
may be fragmental, interrupted, or
continuous.
3 4
Regular diameter and smooth profile;
scales very shallow; small
vacuoles appearing black in some
fibres.
5 6
Fairly regular diameter with
prominent scale margins. Medulla
interrupted or continuous in coarse
fibres.
7 8
Identification of natural textile fibres
Similar to flax; often the lumen is as a Hemp (raw, bleached
mere line and indistinct. and cottonized)
Fibre bundles of varying size; Jute
ultimate fibres mainly sharply
polygonal, some with rounded
corners; lumen round to oval with
very varying size.
Oval to circular, variable in diameter. Wool
Medulla (if present) is concentric
and variable in size.
Circular to oval, medulla Mohair
occasionally fragmental or
continuous in the coarser fibres.
Fine fibres: almost circular; coarse Cashmere
fibres: oval to circular, some
flattened, often medullated.
513
Continued
Table 14.2 Continued

514
Longitudinal Cross-sectional
view view Longitudinal features Cross-sectional features Fibre name

Fine fibres or filaments, cemented in Triangular, with rounded corners, in Bombyx silk (raw)
pairs by silk gum. The gum layer is pairs.
not always continuous.

9
Fine fibres or filaments variable in Separated fibres, triangular, rounded Bombyx silk
diameter, single, smooth, nearly corners. (degummed)
structure-less, sometimes
flattened. Occasionally very fine
fibres are seen, formed by the
superficial splitting of the original
fibre.
Flat irregular ribbons, usually Very elongated triangles, usually Tussah silk
separate, sometimes twisted and separate.
with longitudinal striations.

Handbook of Natural Fibres

Adapted from Luniak, B., 1951. The Identification of Textile Fibres, Sir Isaac Pitman and Sons, London, UK; and Identification of Textile Materials, 1975, seventh Edition, The Textile Institute,
Manchester, UK.
Identification of natural textile fibres 515

of the fibre in various reagents and comparing the data to the known solubility of
several fibres. The reactivity of textile fibres to various solvents is different depending
upon the chemical composition of the fibres. A suitable solvent can be selected for
each fibre, which will dissolve only that fibre. Therefore, fibres which are soluble
can be distinguished from those that are not. The list of commonly used solvents
for different natural fibres is described in Table 14.3. Solubility tests are easy to
perform and can be carried out in test tubes on macroscale or on the stage of a
microscope (ideally used for just such test).
In test tube method, a small tuft of fibre is placed in a test tube containing the suit-
able solvent of the fibre. The fibres are identified by the solubility of the fibre. In micro-
scopic method, a small amount of the fibre is placed under a cover slip with a drop of
the appropriate solvent and the changes are observed under the microscope. For each
solubility test, a fresh sample must be used to avoid any risk of cumulative damage
effects. Great care must be taken to ensure that corrosive or harsh organic solvents
do not contaminate any of the optical and mechanical parts of the microscope.

14.3.5 Staining test

In this method a small tuft of fibres are dyed with a mixture of dyestuffs for 1e5 min
and washed thoroughly. The coloured fibres are compared with the known dyed sam-
ples or viewed carefully to identify the fibre. The chemical composition and reactivity
of natural fibres differ from each other leading them to have affinities for specific stain
or dye types. Therefore, mixtures of dyes have been developed for fibre identification,
which produces known colours for individual fibre types. The best known stains for
natural fibre identification are undoubtedly the Shirlastains (A and D) from Shirley
Developments Ltd. (UK) (Ford and Warwicker, 1961) and Kayastain from Nippon
Kayaku (Japan).
The satisfactory identification of natural fibres by a single identification stain ‘Shir-
lastain A’ is still widely used for identification of these fibres since it was developed in
1932. The identification between cotton and viscose obtained by Shirlastain A is not
entirely satisfactory, and hence an improved distinction may be now obtained by
new product, Shirlastain D.
In this method a small fibre tuft is stained in Shirlastain A at room temperature for
1 min, rinsed under cold tap water and compared with the colour chart for identifica-
tion. The similar orange hues of chlorinated wool and degummed silk creates problem
in distinguishing them. This can be avoided by staining a fresh sample in Shirlastain
A at the boil for 1 min. Chlorinated wool appears black while degummed silk is dark,
reddish brown. Although the same stain can be used two or three times, the recommen-
dation is to use a fresh portion of the stain for each test.
The main limitation of staining test is that the fibre samples for staining should be
undyed (pale-dyed samples are sometimes useable), wettable and free from any surface
finish. Dyed fibres need to be stripped with strong reducing or oxidizing agents.
In addition, any chemical damage to the fibre may also affect the colour of the fibre
produced. Nevertheless, staining tests can be very useful particularly if combined
with light microscopical examination.
 516
Table 14.3 Solubility of natural fibres in different reagents.

Sulphuric acid Sulphuric acid Sodium hypochlorite Sodium hydroxide Cuprammonium

Concentration (%) 60 75 0.25 10 -

Temperature (
C) 20 20 20 Boil 20
Time (minutes) 20 30 20 20 5

Cellulosic fibres I S I Sw S
Wool I I S S Sw
Silk S S S S S
I, Insoluble; S, Soluble; Sw, Swell.
Adapted from Identification of Textile Materials, seventh ed. The Textile Institute, Manchester, UK, 1975 and Textile Laboratory Manual, vol. 5, third Edition, American Elsevier Publishing
Company Inc.

Handbook of Natural Fibres

Identification of natural textile fibres 517

14.3.6 Identification from physical properties

Various physical properties of unknown fibres such as density, moisture regain, refrac-
tive index and birefringence are compared with the reference standards from which the
fibres are identified. The physical properties of natural fibres are described in
Table 14.4.

14.3.6.1 Gravimetric method (density)

Different fibres have varying densities according to the polymer from which they are
made, and this can be used as a diagnostic test. Generally, the densities of natural
textile fibres range from 1.3 (wool) to 1.6 g/cm3 (weighted silk), which may be used
to confirm the identity of a fibre. Three methods such as density gradient column, pyc-
nometer and a technique based on Archimedes principle are described in ASTM stan-
dard (ASTM, 2000).
The simplest approach for determining fibre density is by using a density gradient
column. In a glass tube, a liquid of high density (pentachloroethane-1.71 g/cm3) and a
liquid of low density (xylene-0.87 g/cm3) are used to form a linear density gradient re-
gion with the density increasing from the top to the bottom. The other commonly used
liquids include ethanol/water mixture and varying strengths of salt solutions. Fibres of
known density are used as calibration markers. Fibre of unknown density is allowed to
sink in the tube until it reaches the region of equivalent density, i.e., where the density
of the fibre matches that of the liquid. The density value of the fibre may be read off
and compared with the standard values for identification (Table 14.4).
Thermogravimetric methods, titrimetric methods, kinetic measurements (rate of
fall) and centrifuging techniques are variants of this method. The use of a single instru-
ment to simultaneously identify cotton, wool, silk, viscose and synthetic fibres by ther-
mogravimetry and differential scanning calorimetry has been reported (Crighton and
Holmes, 1998; Perkins et al., 1966). In thermogravimetric method, the sample mass
is monitored in a thermal balance as the temperature is raised linearly and the mass-
temperature curves are plotted. The fibres are identified from the degree of mass
change with temperature. In titrimetric method the volume of liquid adjusting the
density is measured through a burette and the ‘end point’ of no movement of the sam-
ple is noted.
The gravimetric method requires very small sample, and the colour of the fibre do
not interfere with the test. Also, this method is applicable to all fibre types, i.e., ther-
moplastic and nonthermoplastic. However, the possible interactions (mainly sorption
or swelling) between the liquid and the fibre, as well as the trapped air bubbles must be
avoided as this leads to a change in the density. This method cannot be used solely for
confirmatory test as there is considerable overlapping in densities between different
fibre types and difficulty in determining exact density values. Also, in all the
density-based measurements, the temperature should be controlled accurately.
 518
Table 14.4 Physical properties of natural fibres.
Refractive Tenacity
Fibre Density (g/cm3) Moisture regain (%) index nk nt Birefringence Dn (g/den) Extension at break (%)

Cotton 1.52e1.56 8.5 1.577 1.529 0.048 1.7e6.3 3-12

Flax 1.48e1.50 12.0 1.58e1.60 1.52e1.53 0.060 2.6-8.0 1.5-5
Hemp 1.48e1.49 12.0 3.0-7.0 1.5-5
Jute 1.44e1.50 17.0 2.0e6.3 1-2
Sisal 1.33 14.0
Ramie 1.51e1.55 8.5 1.599 1.529 0.070 4.5e8.8 1.5-5
Wool 1.31 18.25 1.557 1.547 0.010
Silk 1.32e1.60 11.0 1.591 1.538 0.053
Remark: Physicomechanical properties of natural fibres, especially lignocellulosic fibres, depend on cultivation conditions and mainly on primary processing (especially on fibre extracting)

Handbook of Natural Fibres

methods.
Adapted from Houck, M.M., 2009. Identification of Textile Fibres, Woodhead Publishing Limited, CRC Press, USA.
Identification of natural textile fibres 519

14.3.6.2 Moisture regain

Different textile fibres can absorb and hold different amounts of moisture from the
atmosphere depending on the chemical structure. The standard measure of the mois-
ture termed as regain of natural fibres ranges from 8.5% (cotton) to 18.25% (wool).
The standard regain (Table 14.4) of an unknown fibre can be determined which can
help in identifying the fibre.

14.3.6.3 Refractive index

The refractive index of a fibre is directly related to its specific chemical composition.
As the fibres are optically anisotropic, the refractive indices along and across the fibre
axis will be different. Hence, the fibres are said to be birefringent. The refractive index
is an extension of the microscopical method and can be used directly or in combination
with melting and solubility behaviour for complete fibre identification. The birefrin-
gence (Dn) is the difference between the two refractive indices:

Dn ¼ nk e nt,

where nk and nt are the refractive indexes parallel and perpendicular to the fibre axis,
respectively.
Refractive index and birefringence are the two most distinguishing features for the
identification of a fibre’s generic class. Although the refractive indices can be obtained
by a light microscope with a polarizer, the most accurate method is to use monochro-
matic light and an interference microscope. The refractive indices (nk and nt) of
undyed fibres can be determined by simply mounting the fibre in different liquids of
know refractive index until the two are found, which causes the fibre to become invis-
ible for polarized light along and across the fibre axis. The Refractive Index (RI) and
birefringence values of different natural fibres are shown in Table 14.4.
The fibres dyed with dark shade require dye removal or stripping before their refrac-
tive index can be determined. The refractive index of some fibres (such as cotton and
nylon) and the varieties of one group of fibre (wool and mohair) lie very close to one
another, which necessitates the measurement of some other properties such as melting
point and solubility for complete fibre identification. More training and experience are
required in this method compared with other methods such as staining and solubility
tests.

14.3.6.4 Other properties

Other properties not generally recognized as relevant in fibre identification (such as
tensile strength, modulus and melting point) can also be used for identification of
the fibres. Subramanian et al. (1983) proposed a method to distinguish between
wool and mohair fibres by the examination of their tensile properties. The tensile
strength and extension at break values of different natural fibres are shown in
Table 14.4. The determination of melting point for fibre identification is mainly
520 Handbook of Natural Fibres

used for synthetic fibre identification as natural fibres do not melt. Some other proper-
ties such as the fibre length, the length of ultimates and fibre diameter (Table 14.5) can
be used for fibre identification. In addition, the plant fibres can be distinguished by
their chemical composition (mainly the cellulose and lignin content) as shown in
Table 14.6. In addition, by testing flammability of fibres using cone-calorimeter and
by estimating heat release rate, the fibres can also be identified.
There are significant differences in the burning characteristics of major natural
fibres and hence can be used for their identification. One of the important properties
used to compare the flammability of textile fibres is the limiting oxygen index
(LOI). LOI is the quantity of minimum oxygen content (%) in nitrogen necessary to
sustain candle-like burning. The LOI values for some important natural fibres are:
Cotton-18, Silk-23 and Wool-25.

14.3.7 IR and Raman spectra analysis

The IR spectra of fibres are obtained by a double-beam spectrophotometer or by a
Fourier transform infrared (FTIR) spectrophotometer. The identification of generic
fibre types in question is made by comparing the absorption spectrum of these fibres
with reference spectra of known samples done on the same instrument until a match is
found. This technique is more valuable for distinguishing between different fibres of
the same generic class (Tungol et al., 1990) and subclass (Tungol et al., 1991,
1993; Grieve et al., 1988; Bartick and Tungol, 1993). When the IR radiation interacts
with a fibre, certain frequencies of energy are absorbed while others are transmitted or
reflected depending on the functional groups (bonds) of the fibre which is used as a
means for identification. Although the IR spectrometer is expensive, it offers an

Table 14.5 Length and diameter of natural fibres.

Length of commercial fibre Length of ultimate fibre Diameter
Fibre (mm) (mm) (mm)

Cotton 15e56 14e21

Jute 750e1500 0.8e6 5e25
Flax 700e900 13e60 12e30
Ramie 800 40e250 16e125
Kenaf 750e1500 2e6 12e36
Hemp 2500 5e55 16e50
Sisal 600e1000 0.8-8 100e400
Wool 25e300 18e55
Silk Very long 8e15
Remark: Length and diameter of natural fibres, especially lignocellulosic fibres, depend on cultivation conditions and
mainly on primary processing (especially on fibre extracting) methods.
Adapted from Identification of Textile Materials, seventh ed. The Textile Institute, Manchester, UK, 1975.
Identification of natural textile fibres 521

Table 14.6 Chemical composition (%) of plant fibres.

Fat
Water and
Fibre Cellulose Hemicellulose Pectin Lignin soluble wax Moisture

Cotton 82.70 5.70 1.00 0.60 10.00

Jute 64.40 12.00 0.20 11.90 1.10 0.50 10.00
Flax 64.10 16.70 1.80 2.00 3.90 1.50 10.00
Ramie 68.60 13.10 1.90 0.60 5.50 0.30 10.00
Hemp 67.00 16.10 0.80 3.30 2.10 0.70 10.00
Sisal 65.80 12.00 0.80 9.90 1.20 0.30 10.00
Abaca 63.20 19.60 0.50 5.10 1.40 0.20 10.00

Turner, B.A.J. 1988. “The structure of textile fibres”. In C. Jarman, Plant fibre and processing: A handbook, Intermediate
Technology Publications, UK.

unambiguous means of chemically identifying unknown fibres. Furthermore, when

only few fibres are available, this method is found to be the most valuable single test.
The IR spectrum of a sample is obtained by passing a beam of IR through the sam-
ple over a range of energies within the IR region; either a monochromatic beam or a
Fourier transform instrument is used. In modern instruments, energy from an IR source
is directed through the fibre by an interferometer. The track of the wavelength and the
amount of light transmitted through the fibre at each wavelength is saved by a com-
puter and the result is represented by a plot of wave number (cm1) against intensity
(T%). The IR spectroscopy along with a microscope can be used for the complete
analysis of a single textile fibre.
The natural fibres exhibit more intrasample variation in the absorption spectrum
compared with synthetic fibres. The amount of twist in the fibres should be reduced
by teasing apart and straightening the fibres before FTIR test. The IR absorption spec-
trum of various natural textile fibres is shown in Fig. 14.1. Table 14.7 shows the
assignments of absorbance frequencies of natural fibres.
Sometimes the fibre may have to be flattened to reduce the effects of spectral distor-
tion due to the diffraction caused by fibre’s cross-section. A metal roller in combina-
tion with a clean glass microscope slide is used for flattening the fibre, which is then
carefully transferred to the specimen holder. As the fibres are flattened during the test
and the morphology is destroyed, the minimum fibre length should be used. In some
cases, the available fibre is too short or too thin to obtain an FTIR spectrum by
conventional means. In these cases, attenuated total reflectance (ATR) also known
as internal reflection spectroscopy may be used. In ATR mode, the fibre is placed in
tight contact with an IR transparent, higherefractive index crystal. IR spectrum is
obtained by passing the IR radiation into the sample and crystal at angles greater
than the critical angle. Recently, FTIR plays an important role in the forensic analysis
of fibres (Grieve, 2000).
522 Handbook of Natural Fibres

(a) (b)
1236

1178
1372 2850
2849 1445

Tr an s m i s s i o n
Transmission

1282
1235
3260 3260
1130

1092 1092

4000 3600 3200 2800 2400 2000 1600 1200 800 600 4000 3600 3200 2800 2400 2000 1600 1200 800 600
–1
Wave number cm Wave number cm

Cotton Flax
(c) (d)

1737 1654
1654
Tr an s m i s s i o n

Tr an s m i s s i o n
2918 2920
1384
3294 1259 3210 1384

1130 1015

4000 3600 3200 2800 2400 2000 1600 1200 800 600 4000 3600 3200 2800 2400 2000 1600 1200 800 600
Wave number cm Wave number cm
Jute Hemp
(e) (f)

1259
1736
2924
Tr an s m i s s i o n

Tr an s m i s s i o n

1384 1250-1280
3210
3230 1158
1447

1130 1652 1552

4000 3600 3200 2800 2400 2000 1600 1200 800 600 4000 3600 3200 2800 2400 2000 1600 1200 800 600
Wave number cm Wave number cm
Sisal Wool

(g)
Tr an s m i s s i o n

3210
1260

1625 1528

4000 3600 3200 2800 2400 2000 1600 1200 800 600
Wave number cm
Silk
Figure 14.1 The infrared absorption spectrum along with the assignment of vibrations of
various natural fibres (a) cotton, (b) flax, (c) jute, (d) hemp, (e) sisal, (f) wool and (g) silk.
Table 14.7 The FTIR assignments (absorbance frequencies) of natural textile fibres.

Identification of natural textile fibres

Cotton Hemp Flax Jute Sisal Wool Silk Assignment

1042 CeO stretching

1092 1000e1162 1000e1162 1000e1162 1000e1162 CeC stretching
1130 Asym. Bridge CeOeC
1158 CeN stretching
1178 Asym. Bridge CeOeC
1236 1235 OeH in-plane bending
1250e1280 CeN stretching
1259 1259 CeH bending
1260 Absorption by amide III
1282 CeH stretching
1372 1384 1372 1384 1384 1447 CeH bending
1445 CeH3 asym. Stretching
1552 1528 Absorption by amide II
1652 1625 Absorption by amide I
1654 1654 1654 C¼C stretching
1737 1736 C¼O stretching
2849 2850 Sym. CeH2 stretch
2920 2918 2924 CeH vibration
3260 3200e3570 3200e3570 3200e3570 3200e3570 3200e3570 3200e3570 OeH stretching

523
524 Handbook of Natural Fibres

Garside and Wyeth (2003) developed an ATR technique using FTIR for the iden-
tification of natural fibres and used the peak intensity ratio for their differentiation on
the basis of relative lignin content. If the composition of cellulosic fibres is considered,
the relative proportion of lignin with respect to other cellular components seems
distinctive. According to harvesting time and degree of maturity of lignocellulosic
fibrous plants, the lignin content in the fibre is changeable (liable). The authors applied
ATR spectroscopy for the comparison of the lignin-to-cellulose content of the plant
fibres for identification.
Raman spectroscopy is complementary to IR spectroscopy and is also a powerful
tool that can be applied in routine fibre analysis following optical microscopy (OM)
and microspectrophotometry (MSP) measurements. The fundamental principles of
Raman spectroscopy and IR spectroscopy are different, the former being a scattering
process while the latter is a pure absorption phenomenon. The spectroscopic selection
rules for Raman and IR activities are different, and they produce complementary vibra-
tional data. Many IR modes that are weak or not permitted in IR spectrum are very
strong in Raman spectrum, e.g., molecular vibrations which involve nonpolar bonds
are strong in the Raman spectrum, and those vibrations involving polar bonds are
strong in the IR spectrum.
Raman spectroscopy can be conducted while the fibre remains mounted on a glass
slide under cover slip as glass produces little response to Raman spectroscopy. But
FTIR cannot be conducted with the fibres mounted to the glass slide due to the strong
absorption of IR radiation by glass. Raman spectroscopy is very useful for the discrim-
ination of dyed fibres and for complete fibre characterization sequence.
Raman spectroscopy was used to discriminate amongst untreated plant fibres on the
basis of peak ratios derived from the associated CeH and CeOeC vibrations
(Edwards et al., 1997). Raman spectroscopy has been used for the analysis (industrial
and forensic) of fibres and has the potential as an analytical tool for fibre examination.
The application of Raman spectroscopy for characterizing natural and synthetic fibres,
and forensic analysis by European Fibres Group (Wiggins, 2003) has been reported.
Raman spectroscopy can also be used to identify the main dye type present in a
coloured fibre.

14.3.8 Other approaches

In several cases other techniques such as transmission electron microscopy (TEM),
chromatography and pyrolysis can be used for the fibre analysis. These techniques
along with some other methods (burning or solubility test) can be used for complete
fibre identification. Unlike the light microscope and SEM, the TEM cannot be used
to examine whole textile fibres directly. TEM is mainly confined in studying the
fine internal structure of single fibres or parts of fibres and chemical reactivity.
TEM is not directly used for fibre identification (Johnson, 1965) rather it is used indi-
rectly by resolving the structure of the crystalline regions in the fibre (Sikorski, 1975).
Various chromatography such as gas, high-pressure liquid and thin-layer tech-
niques can be used for the chemical analysis of textile materials (Weaver, 1984).
Pyrolysis is mainly used for the identification of synthetic fibres. A method of
Identification of natural textile fibres 525

qualitatively identifying a fibre without any elaborate equipment, with the aid of a sim-
ple solvent separation process combined with preliminary tests was suggested by Rist
(Rist, 1987).

14.4 Practical approach

Microscopy and burning test are described (Garner, 1967) as the first step towards the
fibre identification. An unknown fibre is investigated under the microscope for the
longitudinal and CS appearance (Refer Table 14.2). Then the burning behaviour of
the fibre is observed by holding a small tuft of the unknown fibre in forceps into the
flames of a micro-burner for about 10 s (Refer Fig. 14.2). For the confirmation of
the fibres, solubility test (Fig. 14.3) and staining test (Section 14.3.5) should be
used. In staining test, a small fibre tuft is stained in Shirlastain A at room temperature
for 1 min, rinsed under cold tap water and compared with the colour chart for identi-
fication. The ultimate fibre identification is done by repeating the above tests, carefully
considering the inferences given on various methods of identification in Section 14.3
and considering the physical properties.
ASTM (ASTM, 2000) describes solubility test for the preliminary identification of
the generic type of an unknown fibre. Alternatively, the IR spectra (obtained by an
FTIR or a double-beam spectrophotometer) can be compared with the decision chart
for the preliminary identification. The plant (native cellulose) and animal hair fibres
are distinguished by the microscopical examination of longitudinal and cross-
sections. Additional physical properties such as density, melting point, regain,
refractive indices and birefringence are used for confirmatory identification.

Unknown natural fibre

Hold in flame for

about 10 seconds

Melts and shrinks in Shrinks from flame,

flame, burns quickly, burns very slowly, self-
burnt paper smell and extinguishing and burn
leaves light grey ash hair smell

Cellulosic fibres Wool/Silk

If the ash is lumpy, If the ash is soft, round,

blistered, irregular, black, contains black bead, brittle
brittle and breaks easily and pulverizes easily

Wool Silk
Figure 14.2 Scheme for identification of fibres according to burning test.
526 Handbook of Natural Fibres

Unknown natural fibre

Treat with 10% NaOH @

boil for 20 min

The fibre swells without The fibre dissolves

dissolving completely

Cellulosic fibres Wool/Silk

Treat with 75% H2SO4@

for 30 min

The fibre does not The fibre dissolves

dissolve completely

Wool Silk
Figure 14.3 Scheme for identification of fibres according to solubility test.

14.5 Forensic analysis

Forensic analysis of fibres which rarely follows the industrial practice requires knowl-
edge of fibre manufacturing processes and methods. Textile fibres are one of the most
important forms of trace evidence in the context of criminal evidence. Forensic scien-
tist can examine these trace evidence and compare them to a known fibre to discover
possible common origins. The factors influencing the nature of fibre adherence to
materials include type of fibre transferred, type of receiving material and the extent
to which the receiving material is used after transfer.
In case of forensic analysis, apart from the murky origin and uncertain provenance,
the sample size is limited (sometimes may be 1 or 2 fibres). Therefore, microscopy is
the primary method of fibre identification. The preservation of the sample is also the
concern. The focus of forensic scientists is fast nondestructive, selective and sensitive
examination methods. In forensic analysis, FTIR and Raman spectroscopy are mainly
used to determine the chemical composition of fibres, providing a generic fibre class
and subclass.

14.5.1 FTIR and Raman spectroscopy

FTIR and ATR-FTIR are the widely used techniques used for the forensic identifica-
tion of textile fibres by molecular structure characterization. They can also be used to
identify the fibres present in the archeological textiles and differentiae among different
textile fibres. These methods are fast, accurate and inexpensive, which is the main
reason for their wide acceptance. Qualitative analysis and semiquantitative analysis,
such as discriminant analysis and principal component analysis (PCA), are possible
by using ATR-FTIR and chemometric tools. Furthermore, multicomponent fibre
analysis can be performed by using these techniques.
Identification of natural textile fibres 527

Raman spectroscopy is an essential tool in many forensic laboratories in recent

years because of good resolution, smaller sample size, ease of preparation and ability
to use aqueous samples. It can be used for the identification of fibres, minerals,
lipsticks and other evidences left by the criminals. Several studies have shown that
Raman spectroscopy is one of the modern tolls to be used for the forensic analysis
in recent times. Raman spectroscopy is appropriate for very small samples such as
single fibres or very small amount of pigments or particles of 1 mm or less. Micro-
Raman spectroscopy is also found to be an appropriate tool for forensic examination
of dyes and pigments, which can also be used for textile fibres.
For example, Peets et al. (2017) identified and classified textile fibres using ATR-
FTIR spectroscopy with chemometric methods. PCA and discriminant analysis was
performed on the single-component and bicomponent textile materials. The PCA clas-
sification was suitable for single- to three-component fibres to identify each fibre.
However, the limitations were the differentiation among the cellulose-based fibres
(cotton, linen and in some cases viscose) were not possible, and distinguishing
between silk and wool were partially possible (Peets et al., 2017).
Thomas et al. (2005) used Raman spectroscopy for the forensic analysis of black/
grey and blue cotton fibres (reactively dyed) by varying the laser wavelength. The
study has shown that this technique can be used for dyed fibre identification without
interference from the cotton substrate, thereby, providing molecular information about
the main dye used. However, caution must be taken in the choice of wavelengths, as
the fluorescence and changes in sample spectra can occur with laser wavelength.
Wiggins et al. (2007) investigated the use of calculating the first derivative of the
absorbance spectra of fibres as a tool for forensic analysis. The first derivative of
the absorbance spectra provided more points of comparison that facilitated discrimina-
tion when the absorbance spectra produced for some samples were broad and feature-
less. Although it was found that the calculation of the first derivative can be a useful aid
in the comparison of spectra, a high degree of caution is required while applying this
method to fibres which exhibit a large intrasample variation in colour.
The application of the new combined micro-Raman and micro-X-ray fluorescence
(XRF) spectrometer (PRAXIS apparatus) in the forensic analysis of fibres and other
materials has been reported (Zieba-Palus et al., 2008). The studies confirmed the use-
fulness of the apparatus in criminalistic traces and the strong point of the instrument is
that it provides a combination of two nondestructive methods in one instrument. The
analysis is characterized by good repeatability, reproducibility and compatibility.
Lepot et al. (2008) analyzed five forensic fibre cases by Raman spectroscopy and
found it is a good complementary method for MSP. The forensic analysis of dyed
textile fibres by using chromatography, spectroscopy and mass spectrometry were
reported in this work. For certain dye class, the absorption spectra in the visible region
is a characteristic feature, which be subsequently identified by the Raman spectroscopy
using a spectral library. This study showed that the Raman spectroscopy showed only
little interference from the mounting resin and glass. Therefore, Raman spectroscopy is
a powerful method that can be applied in routine fibre analysis following OM and MSP
measurements. There are also other important works in forensic analysis by several
528 Handbook of Natural Fibres

researchers (Paulsson and Stocklassa, 1999; Causin et al., 2006; Miller and Bartick,
1978; Lang et al., 1986; Goodpaster and Liszewski, 2009).
Both the test methods FTIR and Raman spectroscopy require very small amount of
sample and are nondestructive test. The samples used in these tests can be used for
analysis of other properties. In several instances, FTIR and Raman work as comple-
mentary to each other. Some bonds that can’t be detected effectively with FTIR can
be detected with Raman and vice versa.
Although Raman spectroscopy has several advantages over other analytical tools
with respect to simple fibre preparation and accurate identification, it suffers from
some disadvantages such as fluorescence is the major concern assisted with the anal-
ysis of the fibre samples. Fluorescence occurs after a high-intensity visible or UV light
excited the electronic molecular states. This influence can be reduced by changing the
laser wavelength or application of metal colloids and surface enhanced Raman
spectroscopy.

14.5.2 Analysis of dyed textile fibres

The identification of dyed textile fibre can be completed using spectroscopy, chroma-
tography and mass spectrometry in addition to the microscopy. Microscopic analysis is
an important aspect of fibre analysis as discussed in the previous section. For forensic
analysis the stereomicroscope can be used to characterize the colour, dimension, crimp
and luster of fibres. The dyed textile fibres can be easily identified by the polarized
light microscopy as it can provide information on the polymer group by the rotation
of incident polarized light put in the fibre. The description for identification of dyed
textile fibres has been given in Fig. 14.4.
The measurement of dichroism of pigmented fibres can also help to identify the
fibres for the forensic analysis (De Wael and Lepot, 2012). The use of OM and
MSP with plane polarized light can measure the dichroic behaviour. For example,
Wael and Lepot (De Wael and Lepot, 2012) observed strong dichroic behaviour in
half of the samples with 20% showing weak dichroic behaviour. Regular dichroic
effect was observed in 80% cases and inverse dichroic effect was observed in 20%
of the cases. The dichroic behaviour strongly depends on the draw ratio and the crystal
structure of the pigmented fibres.

14.5.3 Analysis of blended materials

In several instances, different types of textile fibres are mixed together to form blended
yarn and fabric as the desirable properties that cannot be obtained by using a single
fibre type is achieved in the blend. The use of blended fabrics is in rise, which has
necessitated the development appropriate methods for the analysis of the blends. Of
the identification methods described, burning test and quantitative method of blend
analysis are used by many industries for fibre identification purposes in the blend.
The burning test as described in Section 16.3.2 is used for the preliminary identifica-
tion of the fibres. Once an idea has been made on the presence of the tentative fibres in
Identification of natural textile fibres 529

Raman
spectroscopy

FTIR
Spectroscopy spectroscopy

UV-vis

LC-MS
Dyed
textile CE-MS
fibres Mass
spectroscopy
Desorption
techniques

TLC

Separations CE

HPLC

Figure 14.4 Methods used for the identification of dyed textile fibres.

the blend, the solubility test is performed to find the composition of the blend in the
fibre mixture.
The solubility test has been described in Section 16.3.4. In blend analysis, 100 g of
fabric is taken and conditioned in standard atmosphere. Appropriate solvent is used to
dissolve one component of the blend. From the initial weight (100 g), the percentage of
the fibre present in the blend is identified. In binary blends, the remaining percentage is
the amount of the second fibre in the blend. In tertiary or higher blends, the other fibres
are dissolved in suitable solvents and percentage of each component has been calcu-
lated from the initial weight till all the fibres are completed. Other approaches such
as moisture regain, image analysis, physical properties, IR spectroscopy, fibre density
and nuclear magnetic resonance. Several fashion brands provide the information on the
blend of the fabric in the final garment (Nayak and Padhye, 2015a, b; Nayak and
Padhye, 2015a; Nayak and Ratnapandian, 2018). However, it is essential to confirm
these blends for exact reproducibility of the textile blends.

14.5.4 Other approaches

Other approaches such as the pyrolysis in combination with the gas chromatography
and the mass spectroscopy can also be used for the forensic analysis of textile fibres
form a small sample size. Scanning electron microscope (SEM) combined with the
530 Handbook of Natural Fibres

energy dispersive X-ray can also be used to identify and detect the elemental compo-
sition of the fibres containing the inorganic synthetic dyes and finishes applied to the
fibres.
The confocal microscopy can be used to identify the hair and other textile fibres for
forensic purposes. The CS shape of each fibre differs from the other, which can be used
for the identification purposes. As the manual preparation of cross-section is rather
difficult, the confocal microscopy can provide better image for identification. The
confocal microscope with laser can collect the microscopical images with some
additional capability. The laser beam can be focused onto the specimen, and by means
of a photomultiplier, the 3D fluorescence image of the specimen can be recorded.
The confocal microscopy technology was used by Kirkbride and Tridico to
generate the virtual transverse and longitudinal CS images of a wide range of fibres
including hair. It was found to be easier and accurate as there was no need to prepare
the fibre cross-sections for microscopic image. Although confocal microscopy can be
successfully used to produce virtual transverse cross-sections from a wide range of
fibres including hairs, autofluorescence signal can interfere with the image, which
can be attenuated by the presence of heavy pigmentation or the presence of an opaque
medulla in hairs. The presence of air-filled voids and heavy delustering agent on the
fibres can produce wrong results.
In several occasions the drugs resemble textile fibres such as the cannabis represent
tee flax fibre. Therefore, identifying may be difficult without a proper instrument. The
use of gas chromatography and mass spectrometry can help to identify the fibres. For
example, Broséus et al. (2010) used this technique to identify the textile fibres and
differentiated from the illegal drugs. The compounds that distinguish between the
fibres and the illegal drugs were identified by using a support vector machines. A clas-
sification rate above 99% was achieved with a false-positive rate less than 2%. This
model successfully helped to differentiate between fibre and drug-type cannabis during
the early growth stage.
The combination of FTIR and energy dispersive X-ray fluorescence (EDXRF)
spectroscopy can be used to identify the textiles, buttons and metal garment compo-
nents extracted during excavations. For example, Akyuz et al. (2014) used FTIR
and EDXRF to investigate textiles and trims (buttons and metals) excavated from
ancient Ainos (Enez in Turkey). The presence of partially degummed B. mori silk
was confirmed using FTIR spectroscopy. Furthermore, the FTIR results also showed
that the buttons were filled with some cellulosic fillings. The EDXRF spectroscopy re-
sults showed the silver-plated copper ornaments in the clothing. The SEM images
showed that the textiles were almost degraded.
For the analysis of the historic materials various nondestructive techniques can be
used. For example, Akyuz et al. (2014) used the combination of ATR-FTIR, EDXRF
and scanning electron microscope (SEM) techniques, to identify the historical textiles
from the imperial pavilion of the new mosque Eminonu-Istanbul (Turkey). The com-
bined techniques identified linen fabric used in the preparation of the textiles. EDX
findings showed that metallic gold was used for gilding in the original textiles. No
gold gilding was observed in the repaired part of the textile. Both lead white
[2PbCO3.Pb(OH)2] and gypsum [CaSO4.2H2O] were used in the paint layers of the
Identification of natural textile fibres 531

original part of the textile. However, in the repaired part, the white pigment was mainly
gypsum and contained only a small amount of the lead white. FTIR spectroscopy was
used in quantifying the degradation of historic textiles in terms of the crystalline
structure of cellulosic fibres.

14.6 Conclusions and future trends

Textile fibre identification is essential to know the composition of a textile material to
reproduce the material, understand the composition or to compare among different
materials. As there are a wide range of textile fibres, both natural and synthetic, it is
a difficult task to uniquely identify these fibres from their visual appearances. Accurate
identification of textile fibres is essential for fashion and textile industries, garment
design houses and forensic science. This chapter has discussed various identification
techniques of natural textile fibres from their appearance, physical and chemical prop-
erties and microscopic images. Although there have been several technological
advancements in the fibre identification such as FTIR spectroscopy, Raman spectros-
copy, EDX, confocal microcopy, gas chromatography and the mass spectroscopy, the
traditional methods are prevalent in the industries as they are the cheapest alternative.
Recently, a wide range of analytical methods such as FTIR, Raman spectroscopy,
electron microscopy, atomic force microscopy and vibrational spectroscopy are avail-
able apart from the OM for fibre identification. Yet as far as the analysis is concerned,
the old methods are the best as they are cheaper and affordable by many large indus-
tries and Small to Medium Enterprises (SMEs). Microscopy still dominates in fibre
identification by providing a range of analysis barely possible with any other methods.
Combined with an analytical bench, such as IR or Raman, it is the quintessential fibre
identification tool. Microscopy should be the first method of choice for any fibre
scientist.
New developments in technical and medical textiles, microfibres and nanofibres
and speciality fibres broaden and deepen the analytical world of fibre analyst. Some
of the other new techniques include multiphoton fluorescence microscopy, optical
coherence tomography and confocal microscopy. Although the first of the two instru-
ments were developed especially for biosciences, it is likely that these will become
more valuable in relation to fibre identification. Confocal microscopy is the advanced
form of OM, which can measure lower than 200 nm (not feasible by OM).

Abbreviations
AATCC American Association of Textile Chemists and Colourist
ASTM American Society for Testing and Materials
ATR Attenuated total reflectance
CS Cross section
EFG European Fibres Group
532 Handbook of Natural Fibres

EDX Energy dispersive X-ray

EDXRF Energy dispersive X-ray fluorescence
FTIR Fourier transform infrared
HRR Heat release rate
IR Infrared
LOI Limiting oxygen index
MSP Microspectrophotometry
NMR Nuclear magnetic resonance
OM Optical microscopy
PCA Principal component analysis
PLM Polarized light microscopy
PPL Plane polarized light
SEM Scanning electron microscopy
SERS Surface enhanced Raman spectroscopy
STM Scanning tunnelling microscopy
SVM Support vector machine
TEM Transmission electron microscopy
XRF X-ray fluorescence

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