NON-DESTRUCTIVE FIBRE ANALYSIS OF BLENDED CLOTHING FOR
FORENSIC APPLICATIONS
WONG TSUEY LYNN
UNIVERSITI TEKNOLOGI MALAYSIA
iv
NON-DESTRUCTIVE FIBRE ANALYSIS OF BLENDED CLOTHING FOR
FORENSIC APPLICATIONS
WONG TSUEY LYNN
A dissertation submitted in partial fulfilment of the
requirements for the award of the degree of
Master of Science
Faculty of Science
Universiti Teknologi Malaysia
FEBRUARY 2016
iii
To all who makes me who I am today
iv
ACKNOWLEDGEMENTS
I would like to thank my supervisor, Associate Professor Dr. Umi Kalthom
binti Ahmad for her valuable guidance that had contributed to this project in a great
amount. She had cleared my doubts and helped me to understand my project better. I
also feel grateful for the advice given by my co-supervisor, SAC Selven a/l
Tharmalingam. Despite of his busy schedule, he was willing to discuss with me.
Thanks are due to my family who had given me great support especially
helping me to collect samples for this study. They also gave me words of
encouragement when I felt unmotivated. A big thank you to all the people who gave
the samples that I needed in this project. Without these samples, this study would not
able to be carried out successfully.
The assistance from all the lecturers, science officers and laboratory
assistants in Department of Chemistry of Universiti Teknologi Malaysia (UTM) is
greatly treasured. I am thankful for their willingness to help and selfless sharing of
knowledge.
Encouragement and help from my friends are also very much appreciated.
Whenever I felt stressful, they cheered me up. They also gave me ideas whenever I
felt lost during my project. Their help is definitely a huge relief.
Last but not least, thank you to those who had helped me either directly or
indirectly. Your kindness will not be forgotten.
v
ABSTRACT
In recent years, global market demands for blended fibres are booming due to
their cost-effectiveness and enhanced properties. Therefore, the usage of blended
fibres is high and thus there are greater chances of encountering fibre blends at crime
scene in forensic cases such as assault and hit-and-run. Fibre analysts have often
relied on analytical techniques developed for single fibres to identify fibre blends.
This study was therefore conducted to characterize binary-blended samples using
light microscopy and infrared spectroscopy as well as to evaluate the effectiveness of
these techniques on analyzing fibre mixture. In this study, 5 reference fibre samples
and 25 clothing samples were subjected to physical examination, followed by
examination with stereomicroscope, polarizing and fluorescence microscopes as well
as attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR).
Stereomicroscopy was found to provide preliminary screening by furnishing
information regarding the weave or knit pattern and twist direction of yarns.
Polarized light microscopy was found to be effective in detecting fibre blends and
examining optical properties, delustrant levels and fibre diameters but it could not
confirm the generic classes of man-made fibres. Fluorescence microscopy allowed
fibre discrimination by comparing fluorescence activity. ATR-FTIR was superior in
determining types of polymeric man-made fibres compared to polarizing microscope.
However, it was found that the infrared spectra needed to be obtained from several
areas of a fabric in order to discover the presence of fibre mixtures. In most of the
blended samples, correlation of more than 80% was achieved by comparing the
blended fibres with combined spectra of individual fibres. In conclusion, non-
destructive techniques of microscopy using 3 types of microscope (stereo, polarizing
and fluorescence) followed by infrared spectroscopy (ATR-FTIR) are recommended
to be used for characterizing fibre blends effectively.
vi
ABSTRAK
Sejak kebelakangan ini, permintaan pasaran global bagi gentian campuran
semakin berkembang pesat disebabkan oleh kos yang efektif dan ciri-ciri yang lebih
baik. Maka, penggunaan gentian campuran adalah tinggi dan terdapat peluang yang
lebih luas untuk menemui gentian campuran di tempat kejadian dalam kes-kes
forensik seperti serangan dan langgar lari. Juruanalisis gentian kerap bergantung
kepada teknik-teknik analisis yang dibangunkan untuk gentian tunggal bagi
mengenalpasti identiti gentian campuran. Oleh itu, kajian ini dijalankan untuk
mencirikan sampel yang mempunyai dua jenis gentian dengan menggunakan
mikroskopi cahaya dan spektroskopi inframerah serta untuk menilai keberkesanan
teknik-teknik tersebut pada gentian campuran. Dalam kajian ini, 5 sampel kawalan
dan 25 sampel pakaian telah dianalisis dengan pemeriksaan fizikal, diikuti dengan
analisis mikroskopi stereo, pengutuban dan pendarfluor dan juga spektroskopi ATR-
FTIR. Mikroskopi stereo dapat menyediakan pemeriksaan awal dengan memberi
maklumat mengenai corak tenunan atau kaitan dan arah pusingan benang.
Mikroskopi pengutuban didapati berkesan dalam mengesan gentian campuran dan
memerhati ciri-ciri optik, tahap agen penyahrelap dan diameter gentian tetapi
mikroskopi tersebut tidak dapat mengesahkan kelas generik gentian sintetik.
Mikroskopi pendarfluor membolehkan diskriminasi gentian dengan membandingkan
aktiviti pendarfluor. Berbanding dengan mikroskopi pengutuban, ATR-FTIR lebih
baik dalam menentukan kelas generik gentian sintetik yang jenis polimer. Akan
tetapi, spektra inframerah didapati perlu diperolehkan daripada beberapa kawasan
fabrik untuk mengesan kehadiran gentian campuran. Bagi kebanyakan sampel yang
mempunyai gentian campuran, korelasi yang lebih daripada 80 peratus dapat dicapai
dengan membandingkan gentian campuran dengan gabungan spektrum-spektrum
gentian individu Kesimpulannya, teknik tanpa musnah 3 jenis mikroskopi, iaitu
mikroskopi stereo, pengutuban dan pendarfluor diikuti dengan spektroskopi
inframerah (ATR-FTIR) disyorkan untuk digunakan bagi mencirikan gentian
campuran secara berkesan.
vii
TABLE OF CONTENTS
CHAPTER TITLE PAGE
DECLARATION ii
DEDICATION iii
ACKNOWLEDGEMENT iv
ABSTRACT v
ABSTRAK vi
TABLE OF CONTENTS vii
LIST OF TABLES x
LIST OF FIGURES xi
LIST OF ABBREVIATIONS AND SYMBOLS xv
LIST OF APPENDICES xvi
1 INTRODUCTION 1
1.1 Background of Study 1
1.2 Problem Statement 2
1.3 Objectives 3
1.4 Scope 3
1.5 Significance of Study 4
2 LITERATURE REVIEW 5
2.1 Manufacturing of Clothing 5
2.2 Types of Fibres 8
2.2.1 Natural Fibres 9
2.2.2 Man-Made Fibres 11
2.2.3 Fibre Blends 12
2.3 Importance of Fibres in Forensic Investigation 13
viii
2.3.1 Factors in Fibre Transfer 14
2.3.2 Shedding and Persistence of Fibres 14
2.4 General Trend in Clothing Market 15
2.5 Analysis of Fibres 17
2.5.1 Colour of Fibres 18
2.5.2 Microscopic Examination 19
2.5.3 Infrared (IR) Spectroscopy 22
2.6 Previous Studies on Fibre Blends 23
3 METHODOLOGY 25
3.1 Chemical and Materials 25
3.2 Apparatus 26
3.3 Instruments 26
3.4 General Experimental Procedure 26
3.5 Procedure 28
3.5.1 Preparation of Samples 28
3.5.2 Physical Examination 28
3.5.3 Stereomicroscopic Examination 28
3.5.4 Examination with Polarizing Microscope 28
3.5.5 Examination with Fluorescence Microscope 30
3.5.6 ATR-FTIR Analysis 31
4 RESULTS AND DISCUSSION 32
4.1 Description of Samples 32
4.2 Preparation of Reference Samples 36
4.2.1 Cotton and Rayon 36
4.2.2 Polyester 40
4.2.3 Silk and Wool 43
4.3 Analysis of Blended Samples 46
4.3.1 Physical Examination 46
4.3.2 Stereomicroscopic Examination 47
4.3.3 Examination with Polarizing Microscope 50
4.3.4 Examination with Fluorescence Microscope 61
4.3.5 ATR-FTIR Analysis 63
ix
5 CONCLUSIONS AND RECOMMENDATIONS 77
5.1 Conclusions 77
5.2 Limitations of Study 79
5.3 Recommendations 79
REFERENCES 80
Appendices A - C 89 - 93
x
LIST OF TABLES
TABLE NO. TITLE PAGE
3.1 Excitation and emission wavelengths of DAPI, TRITC
and FITC filters
31
4.1 Description of reference samples for 100% cotton,
polyester, silk, rayon and wool
33
4.2 Description of clothing and fabric samples
33
4.3 Median diameters of man-made fibres measured in
longitudinal view and delustrant concentrations for
warp/wale and weft/course fibres in the samples
58
4.4 Correlation data for cotton/polyester blended samples with
combined spectra of S100C and S100P
68
4.5 Correlation data for wool/polyester blended samples with
combined spectra of 100WBL and S100P.
74
xi
LIST OF FIGURES
FIGURE NO. TITLE PAGE
2.1 Twist direction of a yarn
5
2.2 Components of a fabric
6
2.3 Direction of warp and weft yarns
6
2.4 Basic weave patterns showing (a) plain weave, (b) twill
weave and (c) satin weave
7
2.5 Manufacturing process of textile products
8
2.6 General classification of fibres
9
2.7 Molecular structure of cellulose
10
2.8 Basic structure of amino acid
10
2.9 Molecular structure of PET
11
2.10 Research trend for identification of textile fibres for year
2004 to December 2015
18
3.1 General procedure for fibre identification in blended
clothing
27
3.2 Steps to prepare slide for fibre examination using
polarizing microscope
30
4.1 Photomicrographs of cotton fibres of S100C (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
37
4.2 Photomicrographs of cotton fibres of 100CR (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
38
xii
4.3 Photomicrographs of rayon fibres of 100RB (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
38
4.4 Average infrared spectrum of S100C, which is the
reference sample for 100% cotton
39
4.5
Average infrared spectrum of 100RB, which is the
reference sample for 100% rayon
40
4.6 Photomicrographs of polyester fibres of S100P (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
41
4.7 Average infrared spectrum of S100P, which is the
reference sample for 100% polyester
42
4.8 Photomicrographs of polyester fibres of 100PG (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
42
4.9 Photomicrographs of silk fibres of 100SBr (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
43
4.10 Photomicrographs of wool fibres of 100WBL (a) under
plane-polarized light and (b) between crossed-polars with
magnification of 400x
44
4.11 Average infrared spectrum of 100SBr, which is the
reference sample for 100% silk
45
4.12 Average infrared spectrum of 100WBL, which is the
reference sample for 100% wool
45
4.13 Yarn of 100CG viewed under stereomicroscope
(magnification of 50x).
47
4.14 Face sides of (a) 100CW and (b) 50C50P being viewed
under stereomicroscope with magnification of 20x
48
4.15 Weave patterns of (a) 35C65P with plain weave, (b)
100SO with satin weave and (c) 65C35P with twill weave
49
4.16 Course yarn of 60C40P viewed under (a) polarized light
microscope (magnification of 200x) and (b)
stereomicroscope (magnification of 50x).
49
xiii
4.17 Wale yarns of 20C80P were crimped while (b) weft yarn
of S-B composed of a single fibre instead of a bundle of
fibres
50
4.18 Fibres in wale yarns of 100CG viewed under polarizing
microscope at magnification of 400x (a) under plane-
polarized light and (b) between crossed polars
51
4.19 Fibres in wale yarns of 100PW viewed under polarizing
microscope at magnification of 400x (a) under plane-
polarized light and (b) between crossed polars
52
4.20 (a) Warp and (b) weft fibres of 100SO viewed under
polarizing microscope at magnification of 400x between
crossed polars
53
4.21 A cross (marked with red circle) in pink warp fibres of
45S55P viewed under polarizing microscope at
magnification of 400x between crossed polars.
53
4.22 (a) Warp and (b) weft fibres of S-B viewed under
polarizing microscope at magnification of 400x between
crossed polars
53
4.23 Black and blue wool fibres, which are indicated by blue
and red arrows respectively, in weft yarns of 100WB
viewed under polarizing microscope at magnification of
400x (a) under plane-polarized light and (b) between
crossed polars
54
4.24 Man-made fibres in 100SO with dichroic effect in (a)
parallel and (b) perpendicular positions, as pointed by the
arrows
55
4.25 (a) Warp fibres of 65C35P and (b) weft fibres of 60C40P-
Br viewed under polarizing microscope at magnification
of 400x under plane-polarized light
56
4.26 (a) Warp fibres and (b) weft fibres of WS-P viewed under
polarizing microscope at magnification of 400x under
plane-polarized light
56
4.27 Presence of nubs in samples of (a) 35C65P and (b) PW-B 60
4.28 Fluorescence activities displayed by (a) 50C50P, (b)
100CW, (c) 55C45P and (d) 100PW
62
4.29 Fluorescence activities displayed by (a) warp fibres of
65C35P under TRITC filter and (b) weft fibres of the
same sample under DAPI filter
63
xiv
4.30 Average infrared spectrum of three 100% cotton samples,
which are 100CR, 100CB and 100CW
64
4.31 Average infrared spectrum of three 60% cotton/40%
polyester samples, which are 60C40P, 60C40P-Br and
60C40P-W
65
4.32 Combined spectrum of reference samples for 100% cotton
(S100C) and 100% polyester (S100P)
66
4.33 Average infrared spectra of (a) 20C80P, (b) 35C65P, (c)
50C50P, (d) 55C45P, (e) 60C40P and (f) 65C35P
67
4.34 Comparison of spectra obtained from 100CG and 100CR
with 100% cotton
69
4.35 Combined spectrum of reference samples for 100% rayon
(100RB) and 100% polyester (S100P)
70
4.36 Average infrared spectrum of 80P20R with 80% polyester
and 20% rayon
70
4.37 Average infrared spectrum of 53R47C with 53% rayon
and 47% cotton
71
4.38 Comparison of average infrared spectra obtained from S-B
and reference sample for 100% silk (100SBr)
72
4.39 Infrared spectra of warp (top) and weft (bottom) fibres of
S-B
72
4.40 Molecular structure of nylon 6 72
4.41 Average infrared spectrum of 45S55P 73
4.42 Infrared spectra of face (top) and back (bottom) sides of
W-B150
74
4.43 Average infrared spectrum of W-G 74
4.44 Average infrared spectrum of PW-B 75
4.45 Average infrared spectrum of 100WB 75
4.46 White substance adhered to fibres of W-B150 being
viewed under stereomicroscope at magnification of 50x
with reflected light
76
4.47 Infrared spectrum of white particles found in W-B150 76
xv
LIST OF ABBREVIATIONS AND SYMBOLS
AATCC - American Association of Textile Chemists and Colorists
ATR - Attenuated Total Reflectance
ATR-FTIR - Attenuated Total Reflectance Fourier Transform Infrared
Spectroscopy
DNA - Deoxyribonucleic acid
DTGS - Deuterated triglycine sulphate
IR - Infrared
< - Less than
MKMA - Malaysian Knitting Manufacturers Association
MITI - Malaysia International Trade and Industry
µm - Micrometre
MSP - Microspectrophotometry
mm - Millimetre
nm - Nanometre
N - Newton
% - Percent
PLM - Polarized light microscope
PBT - Polybutylene terephthalate
PET - Polyethylene terephthalate
cm-1 - Reciprocal centimetre
SEM - Scanning electron microscope
SIMCA - Soft Independent Modeling of Class Analogy
xvi
LIST OF APPENDICES
APPENDIX TITLE PAGE
A Abstract for AFSN 2015 89
B Reference Photomicrographs 90
C IBM SPSS Statistics output 93
CHAPTER 1
INTRODUCTION
1.1 Background of Study
From the clothes you wear, the seat you sit to the carpet you step on, there are
some tiny objects that follow you. These tiny objects called fibres can associate you
to your surrounding. In the same way, a criminal, who had committed a crime such
as hit-and-run, assault and break-in, would either leave or carry away fibres that can
link him or her to the crime scene. High sheddability and ubiquitous nature of fibres
cause them to be one of the most common trace evidence found at crime scene
(Grieve, 2000; DeBattista et al., 2014). Association can be made from the fibres at
crime scene to the suspect’s articles such as clothes, car seat and rope. In accordance
with Locard’s Exchange Principle, fibres from the suspect’s belongings can shed and
transfer to the victim or to the crime scene upon contact. The existence of the fibres
is a proof of contact and thus it is possible to provide a link to the suspect (Hong et
al., 2014). It can help to disprove a suspect’s alibi by supporting his or her presence
at the crime scene. If the fibres are uncommon and match with the accused's
belongings, it can lead to conviction (Deadman, 1984). For example, in a case
reported by Deadman (1984), the rare yellowish green fibres on the victims matched
the carpet fibres in the suspect’s office, resulting in the fibres having strong forensic
evidential value.
Fibres can originate from numerous types of objects; clothing being the most
frequently encountered textile at crime scenes (Robertson & Grieve, 1999). In
addition, the most common material for clothing is cotton/polyester blend (Davis et
2
al., 2011). Such situation concurs with Luniak’s prediction that currently there is a
greater chance to encounter fibre blends rather than a single fibre in an unknown
specimen (Luniak, 1953). In fact, the demand for blended clothing in apparel
industries is still growing.
Increasing number of fibre mixture in clothing requires well-researched
characterization of fibre blends. The characterization methods of single fibre can be
applied to fibre blend. In fact, the conventional tool for samples with mixture of
fibres is microscope (Espinoza et al., 2006), which is also a common technique for
specimen with single fibre component. Infrared spectroscopy is another popular
instrument that is employed in the analysis of fibre mixture (Espinoza et al., 2006;
Dozono et al., 2011; Koyama et al., 2013). Other instruments include X-ray
diffraction (Abraham et al., 2007), Raman spectroscopy (Lepot et al., 2008) and
microspectrophotometer (Palmer et al., 2009). Dye composition is also frequently
studied to discriminate the fibre samples (Houck, 2009). Besides, chemical method
such as selective dissolution is often carried out to find out the composition of
blended product (AATCC, 2011). However, non-destructive means are preferred for
forensic evidence since most of the time they are of small quantities. Nayak et al.
(2012) believed that light microscopy and infrared spectroscopy were sufficient to
analyze single fibres. Therefore, this study used these approaches to characterize the
fibres present in blended clothing.
1.2 Problem Statement
Despite of the increasing number of blended clothes, there are inadequate
amount of researches on fibre blends, especially in forensic examination. Studies
have been carried out on analysis of blended fibres but the existing investigations did
not focus on fibre mixture or only employed one or two techniques. Current protocol
also suggested separating blended fibres prior to analysis (ASTM International,
2012), which may damage forensic evidence. Although forensic examination of
fibres is well established, there are some obstacles in characterization of fibre blends
(Espinoza et al., 2006). Examiners have to do thorough analysis in a proper manner
3
so that they do not erroneously conclude fibre mixture as single fibre. Since fibre
blends have different types of fibres, one of the fibre constituents may interfere with
detection of other components in the mixture. Therefore, the effectiveness of the
approaches for single fibre characterization has to be evaluated when the methods are
performed on fibre blends. This study was conducted using four non-destructive
techniques to analyze specifically fibre mixtures.
1.3 Objectives
The objectives of the study are as follows.
i. To characterize several binary fibre blends using three types of light
microscopies (stereo, polarizing and fluorescence) in terms of fibre
morphologies and optical properties as well as infrared spectroscopy.
ii. To evaluate the effectiveness of light microscopy and infrared
spectroscopy for non-destructive analysis of fibre blends.
1.4 Scope
The scope of this research encompasses the analysis of binary-blended fibres
using several non-destructive analytical techniques, i.e. stereomicroscope, polarizing
microscope, fluorescence microscope and ATR-FTIR. Samples of blended clothes
obtained through convenience sampling were analysed in this study after the clothes
were examined physically for possible presence of fibre mixtures. Clothes with
binary mixture were focused on in this study because fabrics with more than two
fibre types are not common in practice (Sengupta & Debnath, 2012). Fibre blends
containing cotton, polyester, rayon, silk and wool were chosen because these fibres
are common in Malaysia (Sieh Lee, 2007) and thus there are high probability of
encountering the fibre at crime scene.
4
1.5 Significance of Study
Through this study, characterization of fibre blends in forensic perspectives
can be better understood. It can aid in identification of blended clothing for forensic
purpose. Proper characterization of fibre blends is crucial in criminal investigation
when blended textile products are encountered at crime scene. Misinterpretation as
single fibres can be avoided if fibre mixture can be discovered when the same
methods for single fibres are employed. It helps to differentiate the fibre samples and
narrow down the suspect pool.
Besides, this study can also contribute to the assessment of manufactured
clothes in apparel industries. The data obtained in this research may also be useful in
a Malaysian fibre database in future.
80
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