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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