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M838
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This is to certify that the
thesis entitled

FORENSIC ANALYSIS OF BLACK MASCARA VIA
MICROSCOPY, FOURIER TRANSFORM INFRARED
SPECTROSCOPY (Fl'lR), SCANNING
ELECTRON MICROSCOPY-ENERGY DISPERSIVE
SPECTROSCOPY (SEM-EDS), ANO VISIBLE
MICROSPECTROPHOTOMETRY (MSP)

presented by
JoAnn I. Bilek

has been accepted towards fulfillment
of the requirements for the

Master of degree in
Science Forensic Science

 

 

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2/05 alcfiC/Dateoueindd-p. 15

 

FORENSIC ANALYSIS OF BLACK MASCARA VIA MICROSCOPY, FOURIER
TRANSFORM INFRARED SPECTROSCOPY (FTIR), SCANNING ELECTRON
MICROSCOPY-ENERGY DISPERSIVE SPECTROSCOPY (SEM-EDS), AND
VISIBLE MICROSPECTROPHOTOMETRY (MSP)

By

JoAnn I. Bilek

A THESIS
Submitted to
Michigan State University
in partial fulfillment of the requirements
for the degree of
MASTER OF SCIENCE

School of Criminal Justice

2005

ABSTRACT
FORENSIC ANALYSIS OF BLACK MASCARA VIA MICROSCOPY, FOURIER
TRANSFORM INFRARED SPECTROSCOPY (FT IR), SCANNING ELECTRON
MICROSCOPY-ENERGY DISPERSIVE SPECTROSCOPY (SEM-EDS), AND
VISIBLE MICROSPECTROPHOTOMETRY (MSP)
By
mm 1. Bilek

Four analysis techniques were utilized in this project in an attempt to differentiate
between twenty-four black mascara samples from fourteen different brands. A sample of
black lash tint was analyzed along with the mascara samples, but was easily distinguished
from the mascara samples by each analysis technique.

Microscopic examination by traditional light microscopy separated the mascara
samples into four groups. Analysis by Fourier transform infrared spectroscopy (FTIR)
was able to separate the samples into twenty-two groups. The analysis by scanning
electron microscopy-energy dispersive spectroscopy (SEM-EDS) excluded and
distinguished between 99.67% of the 600 comparisons based on calculated weight
percent ratios. The elements which were quantified and compared were iron, silicon,
magnesium, aluminum, and sodium. The analysis performed by visible
microspectrophotometry (MSP) did not yield any discriminatory data for the mascara
samples in this study.

A proposed analysis scheme for black mascara based on the findings of this study
involves a preliminary examination by microscopy, followed by FTIR and SEM-EDS
analysis. The overall incorporation of these three techniques to this study lefi only two

samples from being distinguished from one another. The indistinguishable samples were

from different mascara brands, but both share the same manufacturer.

COPYright by
JOANN IRENA BILEK
2005

In loving memory of my grandfather, Czeslaw Bilek

iv

ACKNOWLEDGMENTS

I would first like to thank my advisor, Dr. Jay Siegel, for the project concept, his
advice, and analysis contribution. I am also very appreciative to those who assisted me
even though they had no Obligation to do so: Ewa Danielewicz of the Michigan State
University Center for Advanced Microscopy, Christopher Bommarito of the Michigan
State Police Forensic Science Laboratory, and Dr. Kathy Severin of the Michigan State
University Chemistry Department.

I would also like to thank my family and friends for all of their support. I am
especially grateful for the help and support I received fiom my parents and my boyfriend

Tom throughout my time at MSU.

TABLE OF CONTENTS

LIST OF TABLES ................................................................................. vii
LIST OF FIGURES ............................................................................... viii
1. INTRODUCTION ................................................................................ 1
1.1 Mascara .............................................................................. l

1.2 Analysis Techniques ............................................................... 3

A. Microscopic Examination ................................................ 3

B. FTIR ........................................................................ 4

C. SEM-EDS .................................................................. 5

D. Visible MSP ............................................................... 6

2. MATERIAL AND METHODS ................................................................. 7
2.1 Samples .............................................................................. 7

2.2 Microscopic Examination ......................................................... 9

2.3 FTIR ................................................................................. 9

2.4 SEM-EDS ......................................................................... 10

2.5 Visible MSP ....................................................................... 11

3. RESULTS AND DISCUSSION ............................................................... 12
3.1 Microscopic Examination ....................................................... 12

3.2 FTIR ................................................................................ 13

3.3 SEM-EDS ......................................................................... 20

3.4 Visible MSP ....................................................................... 24

4. CONCLUSION .................................................................................. 31
5. FUTURE WORK ................................................................................ 33
APPENDICES ...................................................................................... 34
APPENDIX A. Microscopic Examination Data .................................... 35
APPENDIX B. FT IR Spectra ......................................................... 37
APPENDIX C. SEM—EDS Data and Spectra ....................................... 58
REFERENCES ..................................................................................... 87

vi

LIST OF TABLES

Table l: Mascara sample information ............................................................. 7
Table 2: Brands and manufacturer information for mascara samples ........................ 8
Table 3: Example of elemental ratio calculation results for two mascara samples ........ 23
Table 4: Example of inclusion rule comparison for two mascara samples .................. 23
Table 5: Observations from the microscopic examination of mascara samples ............ 36
Table 6: SEM-EDS average elemental weight percent data for mascara samples .........59
Table 7: SEM-EDS ratio calculation results for mascara samples ........................... 83

vii

LIST OF FIGURES

Figure 1: FTIR spectrum of lash tint sample Revlon- solvent ................................ 15
Figure 2: FTIR spectrum of mascara sample Cover Girl- solvent ........................... 16
Figure 3: FT IR spectrum of mascara sample Max Factor- solvent .......................... 17
Figure 4: FTIR spectrum of mascara sample Cover Girl- water ............................. 18
Figure 5: FTIR spectrum of mascara sample Max Factor- water ............................ 19
Figure 6: SEM-EDS spectrum of mascara sample Maybelline- water ...................... 21
Figure 7: SEM-EDS spectrum of lash tint sample Revlon- solvent ......................... 22
Figure 8: Visible MSP spectrum of mascara sample Almay- water ......................... 25
Figure 9: Visible MSP spectrum of mascara sample Cover Girl- solvent .................. 26
Figure 10: Visible MSP spectrum of mascara sample L’Oreal- hybrid ..................... 27
Figure 11: Visible MSP spectrum of lash tint sample Revlon- solvent Blue ............... 28
Figure 12: Visible MSP spectrum of lash tint sample Revlon- solvent Red ............... 29
Figure 13: Visible MSP spectrum of lash tint sample Revlon- solvent Yellow ............ 30
Figure 14: FT IR spectrum of mascara sample Almay- hybrid ............................... 38
Figure 15: FTIR spectrum of mascara sample Almay- water ................................. 39
Figure 16: FTIR spectrum of mascara sample Aziza 11- water ............................... 40
Figure 17: FT IR spectrum of mascara sample Bonne Bell- water ........................... 41
Figure 18: FT IR spectrum of mascara sample Jane- hybrid .................................. 42
Figure 19: FTIR spectrum of mascara sample Jane- water .................................... 43
Figure 20: FTIR spectrum of mascara sample L’Oreal- hybrid .............................. 44
Figure 21: FTIR spectrum of mascara sample L’Oreal- water ............................... 45
Figure 22: FTIR spectrum of mascara sample Maybelline- hybrid .......................... 46

viii

Figure 23:
Figure 24:
Figure 25:
Figure 26:
Figure 27:
Figure 28:
Figure 29:
Figure 30:
Figure 31:
Figure 32:
Figure 33:
Figure 34:
Figure 35:
Figure 36:
Figure 37:
Figure 38:
Figure 39:
Figure 40:
Figure 41:
Figure 42:
Figure 43:
Figure 44:

Figure 45:

FTIR spectrum of mascara sample Maybelline- solvent ......................... 47

FTIR spectrum of mascara sample Maybelline- water ........................... 48
FTIR spectrum of mascara sample Neutrogena- water ........................... 49
FTIR spectrum of mascara sample Physicians Formula- water ................. 50
FTIR spectrum of mascara sample Revlon— hybrid ............................... 51
FTIR spectrum of mascara sample Revlon- water ................................ 52
FTIR spectrum of mascara sample Rimmel— solvent ............................. 53
FTIR spectrum of mascara sample Rimmel- water ............................... 54
FT IR spectrum of mascara sample Sally Hansen- water ........................ 55
FTIR spectrum of mascara sample Wet’n’Wild- hybrid ......................... 56
F TIR spectrum of mascara sample Wet’n’Wild- solvent ........................ 57
SEM-EDS spectrum of mascara sample Almay- hybrid ......................... 6O
SEM-EDS spectrum of mascara sample Almay- water .......................... 61
SEM-EDS spectrum of mascara sample Aziza 11- water ........................ 62
SEM-EDS spectrum of mascara sample Bonne Bell- water ..................... 63
SEM-EDS spectrum of mascara sample Cover Girl- solvent ................... 64
SEM-EDS spectrum of mascara sample Cover Girl- water ..................... 65
SEM-EDS spectrum of mascara sample Jane- hybrid ............................ 66
SEM-EDS spectrum of mascara sample J ane- water ............................. 67
SEM-EDS spectrum of mascara sample L’Oreal- hybrid ........................ 68
SEM-EDS spectrum of mascara sample L’Oreal- water ......................... 69
SEM-EDS spectrum of mascara sample Max Factor- solvent .................. 70
SEM-EDS spectrum of mascara sample Max Factor- water ..................... 71

ix

Figure 46: SEM-EDS spectrum of mascara sample Maybelline- hybrid ................... 72

Figure 47: SEM-EDS spectrum of mascara sample Maybelline- solvent .................. 73
Figure 48: SEM-EDS spectrum of mascara sample Neutrogena- water ..................... 74
Figure 49: SEM-EDS spectrum of mascara sample Physicians Formula- water ........... 75
Figure 50: SEM-EDS spectrum of mascara sample Revlon- hybrid ........................ 76
Figure 51: SEM-EDS spectrum of mascara sample Revlon- water .......................... 77
Figure 52: SEM-EDS spectrum of mascara sample Rimmel- solvent ....................... 78
Figure 53: SEM-EDS spectrum of mascara sample Rimmel- water ........................ 79
Figure 54: SEM-EDS spectrum of mascara sample Sally Hansen- water .................. 80
Figure 55: SEM-EDS spectrum of mascara sample Wet’n’Wild- hybrid .................. 81
Figure 56: SEM-EDS spectrum of mascara sample Wet’n’Wild- solvent .................. 82

1. INTRODUCTION

Cosmetics are potentially important forensic evidence because most women apply
them on a daily basis. Cosmetics may not be found at every crime scene, but when they
are present it is important to have a scheme for the analysis of or knowledge of the
significance of such evidence. A woman who is sexually assaulted, or the victim of a
violent crime, may transfer her cosmetics to her attacker. If a woman is smothered with a
pillow or blanket, the transfer of her cosmetics may help identify the murder weapon or
even the murderer.

Trace evidence is seldom used to positively identify a questioned sample as
having originated from a known sample and no other source. However, if the examiner
concludes that the questioned sample could have originated from the known sample,
along with additional circumstantial evidence, than the likelihood of guilt will also
accumulate. Although trace evidence may not always lead to a positive or negative

conclusion by itself, it should not be disregarded or deemed irrelevant.

1.1 Mascara

Mascara is a commonly used eyelash cosmetic. The purpose of mascara is to
darken, thicken, and lengthen eyelashes (1). Liquid mascara is the modern formulation
used today, while cake and cream mascaras are the older, less encountered formulations.
Liquid mascara can be divided into water-based, solvent-based, and water/solvent hybrid-
based (1). Water-based mascaras are classified as oil-in-water emulsions, and are
formulated by dispersing waxes, pigments and resins in water. Solvent-based mascaras

are formulated with petroleum distillates or other hydrocarbon solvents to which

pigments and waxes are added, making them waterproof. Hybrid-based mascaras
combine both water and solvent-based formulations to form either a water-in-oil or oil-in-
water emulsion (1). The common waxes used in the formulation of mascara are beeswax,
camauba wax, candelilla wax, and paraffin. Some examples of pigments used in the
formulation of mascara are iron oxides, chromium oxides, ultramarine blue, carmine, and
titanium dioxide.

Mascara is best classified as a surface coating. The following terminology from
the coatings industry pertains to mascara: surface coating, pigment, and vehicle. A
surface coating is a suspension of a pigment in a vehicle designed for the protection of a
surface or for decoration, or both (2). A pigment is a finely powdered solid that is
insoluble in the coating in which it is dispersed. Pigments impart color to a coating and
are usually inorganic (2). A vehicle is a portion of a surface coating other than the
pigment, which enables the pigment to be dispersed over the surface (2). Mascara is
hence a suspension of pigments in a wax vehicle.

In a case submitted to the Michigan State Police (MSP) forensic science division
a few years ago, a wash cloth with what was believed to be mascara was submitted as
evidence along with numerous mascara tubes belonging to a murder victim and several
suspects. The deceased was found in her bathroom, which is where the homicide was
thought to have occurred. The investigators hypothesized that the murderer may have
used the wash cloth to clean blood off of her face and in the process transferred her
mascara. The forensic scientist who was given the case, Ms. Cheryl Lozen of the
Northville MSP Forensic Laboratory, analyzed the questioned and known mascara

samples, along with ten known outside samples, using Fourier transform infrared

spectroscopy (FTIR) in order to compare the chemical composition of each sample.
Ultimately, Ms. Lozen determined that all of the samples could be differentiated from
one another based on their spectra and that the mascara submitted as evidence could have
originated fiom one of the mascara tubes belonging to the victim (3). Had the
determination been that the mascara evidence could have originated from one of the
mascara tubes belonging to a suspect, the evidence could have assisted the investigators
had it supported other circumstantial evidence.

There are hundreds of black mascaras on the market today, and these same types
of mascara are also available in numerous colors. An exploratory study to determine the
best approach(s) to examining mascara is required prior to a more exhaustive sample
study of the cosmetic. Black mascara is the most commonly worn mascara, hence was

chosen to be analyzed in this study.

1.2 Analysis techniques
A. Microscopic Examination
Traditional light microscopy is used as an analysis technique in this
research because it is an important tool for the preliminary examination of trace
evidence. The microscope is a standard piece of equipment in a forensic
laboratory, which will not consume or change the evidence sample being

examined.

B. FTIR

Fourier transform infrared spectroscopy (FTIR) is a common technique
used for analyzing trace evidence in forensic laboratories. FTIR is used to
analyze paint, fibers, adhesives, as well as other substances.

In infrared spectroscopy, infrared light is focused on the sample being
analyzed. The molecules in the sample absorb the infrared radiation causing the
chemical bonds in the sample to vibrate. Functional groups tend to absorb
infrared radiation in the same wavenumber range regardless of the remaining
structure of the molecule. Thus, the vibrations detected at specific frequencies are
characteristic of certain frmctional groups creating a correlation between the
wavenumbers at which a molecule absorbs radiation and its structure. A spectrum
is then produced that displays the wavenumbers vs. the percent of light
transmitted for the sample analyzed.

Infrared spectroscopy is used in the analysis of coatings, such as paint, to
characterize the vehicle, which is primarily organic. The wax vehicle used in
mascara is comprised of hydrocarbons. FT IR is a technique that can identify such
functional groups and allow for the comparison of samples based on chemical
composition.

Unfortunately, there are also disadvantages to this analysis technique.
Pigments and other inorganic components are weak absorbers in the infiared
region and are not ofien detected. In addition, the analysis of complex mixtures
gives rise to complex spectra leading to difficult spectral interpretation and the

masking of minor component peaks by major components.

C. SEM-EDS

Scanning electron microscopy-energy dispersive spectroscopy (SEM-
EDS) may also be used for forensic trace evidence analysis. This technique is
commonly used for the elemental analysis of glass, explosives and gunshot
residue.

In SEM, a beam of electrons is used to excite the electrons on the surface
of a sample. These excited electrons, or secondary electrons, are emitted from the
sample and collected by a detector that ultimately generates a magnified image of
the sample. X-rays, which have a specific energy characteristic of the element
that produced it, are also emitted from the sample surface. The SEM may be
coupled with an x-ray detector allowing for the detection and spectroscopic
analysis of the emitted x-rays. The elements in a sample can then be determined
by measuring the energy of the x-rays produced, also referred to as energy
dispersive spectroscopy (EDS).

The use of elemental analysis by SEM-EDS will allow for the quantitation
of inorganic components in mascara, such as elements present in the pigments and
additives. Unfortunately, this technique will not produce quantified data for
specific compounds; however the overall weight percent of specific elements in a

sample will allow for the differentiation of samples if properly compared.

D. Visible MSP

Visible microspectrophotometry (MSP) is a technique used to discriminate
between samples on the basis of sample interaction with light in the visible region
(400—700 nm). This instrument yields absorption spectra displaying the
wavelengths at which a sample absorbs visible light. The MSP is used for
distinguishing between closely colored materials, which could not be
distinguished using the naked eye. This technique may be applied to evidence
such as paint, fibers, and ink.

The mascara samples to be analyzed in this project are black. Typically
black objects are referred to as achromatic, because they absorb all wavelengths
and lack what is perceived as color. In a recent forensic science thesis by Kristen
Kopchick, several apparently black, achromatic automotive paint samples
displayed positive spectral results when analyzed using visible
microspectrophotometry (4). The positive spectral results were the consequence
of chromatic secondary pigments added to the paints for an intended color effect
or the formulation of a unique coating (4). Although chromatic pigments may not
be observed in achromatic paint samples in reflected light, discriminating data
may be obtained by utilizing visible MSP. The application of chromatic
secondary pigments may also occur in the formulation of black, achromatic,

mascara samples.

2. MATERIAL AND METHODS
2.1 Samples
Twenty-four different mascaras and one lash tint from fourteen brand names were

purchased from a local store. All of the samples are labeled as a shade of black. Detailed

sample and manufacturer information is displayed in Table 1 and 2.

Table 1: Mascara sample information

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Brand Mascara Name Based Color
Almay® Bright Eyes® Water Black
Almay® Bright Eyes® Waterproof Hybrid Black

Aziza II Lengthening Water Black

Bonne Bell® Eye StyleTM Water Basic Black
Cover Girl® Professional Smudgeproof ‘ Water Black

Cover Girl® Professional Waterproof Solvent Black

Jane Hi-Fiber Water Basic Black
Jane Hi-Fiber Waterproof Hybrid Basic Black
L'Oreal® Voluminous® Water Black
L'Oreal® Voluminous® Waterproof Hybrid Black

Max Factor® 2000 Calorie Water Rich Black
Max Factor® 2000 Calorie Aqua Lash® Solvent Rich Black
Maybelline® Great Lash® Water Very Black
Maybelline® Great Lash® Waterproof Solvent Very Black
Maybelline® Volum' Express® Ultra-Thick Waterproof Hybrid Very Black
Neutrogena® Full Volume® Water Rich Black
Physicians To Any Lengths® Water Midnight Blk.
Formula

Revlon® Colorstay® Extra Thick Lashes Water Black
Revlon® Colorstay® Ex. Thick Lashes Waterproof Hybrid Black
Revlon® Colorstay OvertimeTM Lash Tint Solvent Black
Rimmel Extra Super Lash Water Black
Rimmel Extra Super Lash Waterproof Solvent Black

Sally Maximum Growtlr® Water Blackest Blk.
Hansen®

Wet'n'Wild® Protein Mascara Hybrid Black
Wet'n'Wild® H20 Proofm Waterproof Solvent Blackest Blk.

 

 

 

Table 2: Brands and manufacturer information for mascara samples

 

 

 

 

 

 

 

 

 

 

Brand Manufacturer/Distributor
Almay® Revlon, Inc.

Aziza II Inter Parfirms, Inc.

Bonne Bell® Bonne Bell Company®
Cover Girl® Procter & Gamble

Jane Jane and Company LLC
L'Oreal® L'Oreal Group

Max Factor® Proctor & Gamble
Maybelline® L'Oreal Group
Neutrogena® Neutrogena Corp.

 

Physicians Formula

Physicians Formula Cosmetics, Inc.

 

Revlon®

Revlon, Inc.

 

 

 

 

Rimmel Coty, Inc
Sally Hansen® Del Laboratories, Inc.
Wet'n'Wild® Markwins® Beauty Products, Inc.

 

The samples were labeled as water, hybrid or solvent-based according to the
ingredients listed on the manufacturer packaging of each mascara tube. A sample was
designated as water-based if water was listed as the primary ingredient. The solvent-
based samples listed petroleum distillates or isododecane as the primary ingredients and

did not contain water. The hybrid-based samples listed water and a hydrocarbon solvent,

such as isododecane, as the primary ingredients.

Thirteen of the samples are water-based, six of the samples are solvent-based, and
the remaining six samples are a water/solvent hybrid-based. In order to simplify the
nomenclature involved in sample identification, the mascara samples will be designated

by brand and either water, solvent, or hybrid-based as opposed to the actual mascara

name.

 

2.2 Microscopic Examination -

Microscopy is a technique that may be employed quickly, without sample
consumption. Sample preparation for analysis was achieved by spreading a thin layer of
each sample onto a clean microscope slide using the applicator wand located on the
inside cap of each mascara tube. A cover slip was placed onto the slide with enough
pressure to flatten the sample. The samples were allowed to dry and then examined via
traditional light microscopy with an Olympus BX41 microscope at 400x magnification.
Polarized light microscopy (PLM) was not implemented in this study due to the author’s

limited experience with the technique.

2.3 FTIR

Three studies were performed using FTIR to analyze the mascara samples. As
before, sample preparation involved spreading a thin layer of each mascara sample onto a
clean microscope slide using the mascara tube applicator wand. Each sample to be
analyzed was transferred from the microscope slide with a metal spatula and smeared
onto a potassium bromide (KBr) disk. The KBr disk was then placed onto the F TIR
microscope stage for analysis. The instrument utilized was a Perkin Elmer Auto Image
FTIR Microscope. A background scan was performed prior to the collection of each
sample spectra, which was acquired with 16 scans. The baseline of each spectrum was
corrected using the Spectrum 1.0 software.

Initially a drying study was performed to determine when each type of mascara
sample would be dry; this would be based on the lack of excessive variation between

spectra over time. The water, hybrid, and solvent based mascaras of the Maybelline

brand were analyzed at the following time increments: fresh, after four hours, eight hours,
one day, two days, three days, and four days.

After the appropriate drying time was determined, a reproducibility study was
performed. This study was conducted to assure that the three types of mascara would
give consistent spectra between analysis of the same sample smear and different smears
of the same sample. The water, hybrid, and solvent based mascaras of the Maybelline
brand were analyzed on ten separate occasions within the same day to determine whether
the spectra were reproducible.

Finally each of the twenty-five mascara samples was analyzed using the

instrument after the time period determined by the drying study.

2.4 SEM-EDS

The mascara samples dried on the microscope slides were placed in a desiccator
under vacuum for a week in order to maintain them in a dry atmosphere. A small amount
of each of the samples was scraped from the microscope slide and mounted on an
aluminum stub using double sided carbon tape. The samples were made conductive
using an Ernest F Fullam Inc.EFFA MKII Carbon Coater. The sample holder used to
place the samples inside the SEM sample chamber held four sample stubs. The samples
were analyzed using a ISM-6400 Scanning Microscope coupled with a Thermo Electron
Corporation X-ray Detector. The samples were analyzed under high vacuum at an
accelerating voltage of 25,000 volts. Samples were analyzed at a working distance of 15
mm at 500x magnification, with a scanning area of 240 microns by 180 microns for 100

live seconds.

10

The following fifieen elements were detected during trial sample runs: carbon
(C), oxygen (0), sodium (Na), magnesium (Mg), aluminum (Al), silicon (Si), phosphorus
(P), sulfur (S), chlorine (Cl), potassium (K), calcium (Ca), titanium (Ti), manganese
(Mn), iron (Fe), and copper (Cu). However, only the following elements were selected
for quantitation: iron (Fe), silicon (Si). magnesium (Mg), aluminum (Al), and sodium
(Na). The elements were selected based on the ingredients listed on the packaging of the
mascara samples and the abundance of the elements determined during several trial
sample nms. Iron is present in iron oxide, a common pigment in mascara, while the
remaining elements are present in numerous additives used to manufacture mascara.

The above analysis was performed three times, each time in a different location,
for each mascara sample. The calculated weight percent of each element mentioned was
provided by the Vontage 1.5.1 software by Noran Instruments, which applies a ZAF

correction to compensate for matrix effects and provide accurate quantitation.

2.5 Visible MSP

The dried mascara samples on the microscope slides were individually analyzed
by Dr. Jay Siegel using a CRAIC QDI 2000, UV-visible-near IR
Microspectrophotometer. The instrument was initially calibrated using NI ST standards.
Dark and reference scans were performed prior to the analysis of each sample. The

samples were each analyzed in five different areas using ten scans.

11

3. RESULTS AND DISCUSSION
3.1 Microscopic Examination

Microscopic examination of the samples resulted in the differentiation of only
some of the samples. All of the samples consisted of black particles, except for the lash
tint, Revlon- solvent, sample. This sample contained red, blue, and yellow pigments.

The remaining twenty-four samples could then be separated into the following
four groups: contains orange flakes, contains blue specks, contains brown particles, and
could not be distinguished. Two of the samples contained orange flakes, the Almay-
hybrid and Almay- water samples. Two of the samples contained blue specks, the Aziza
11- water and L’Oreal- hybrid samples. Two of the samples contained brown particles,
the Cover Girl- solvent and Max F actor- solvent samples. The remaining eighteen
samples could not be distinguished by microscopic examination. The complete
microscopic examination observations are displayed in Appendix A, Table 5.

Four of the samples were observed to contain fibers. Nylon and rayon fibers are
sometimes added to mascara to increase the length of eyelashes when applied. These
fibers could be identified with the use of polarized light microscopy, which allows for the
observation of interference colors in anisotropic substances between crossed polars, and
the Michel-Levy chart, which in turn allows the microscopist to identify a substance
based on thickness and observed interference colors. The presence of these fibers is
significant, however the absence should not be considered important when comparing
mascara samples. The fibers may or may not transfer with the mascara, thus the lack of
fibers in a questioned sample should not eliminate it from originating fi'om a known

sample containing fibers.

12

3.2 FTIR

The drying study determined that the Maybelline-water, solvent, and hybrid
mascara samples displayed the least amount of variation afier two days of drying time.
The peaks which changed over the time increments in the study were not identified
because any questioned mascara submitted as evidence would likely already be dry prior
to laboratory analysis. In the event that known mascara samples from manufacturer tubes
are analyzed for comparison with a dry questioned sample, these samples must also be
dried for two days prior to analysis in order to perform a proper comparison.

The reproducibility study provided reproducible spectra for the Maybelline-
water, solvent and hybrid mascara samples. The ten spectra produced for each of the
mascara samples rendered peaks which were consistent within the variation normally
observed between spectra in FTIR analysis.

The FT IR spectra of beeswax, carnauba wax, candelilla wax and paraffin wax
displayed a strong absorption band in the 2970-2830 cm'1 range, accompanied by
absorption bands in the 1480-1455 cm'1 and 735-710 cm'1 ranges (5). These absorption
bands are characteristic of long chain hydrocarbons, which are the constituents of wax.
Beeswax, carnauba wax, and candelilla wax also display an absorption band in the region
between 1750 and 1680 cm'l, which is characteristic of a carbonyl group (-COOH). This
band may be indicative of cerotic acid, a fatty acid, (CH3(CH2)24COOH), occurring in
waxes (6). All twenty-four of the analyzed mascara samples displayed absorption bands
in the above mentioned regions, which indicates the presence of ‘wax’ in each sample.

The lash tint, Revlon- solvent, sample (see Figure 1) did not yield a significant absorption

13

band in the 735-710 cm'1 range, which was observed in all of the spectra produced from
the mascara samples.

In order to distinguish between the spectra from the twenty-four mascara samples,
it was necessary to observe the regions of the spectra where waxes did not have common
absorptions. The region between 1650 cm'I and 1500 cm", along with the portion of the
fingerprint region in the 1400-750 cm’1 range displayed absorptions which varied
between twenty of the mascara samples. Thus, twenty-one of the samples could be
distinguished from one another based on the analysis provided by FTIR.

The remaining four samples resulted in two pairs of spectra which were unable to
be differentiated from each other. The FTIR spectra of Cover Girl- solvent (see Figure 2)
and Max Factor- solvent (see Figure 3) mascara samples could not be distinguished from
one another. The spectra of Cover Girl- water (see Figure 4) and Max Factor- water (see
Figure 5) mascara samples also could not be distinguished from one another. All of the

remaining FTIR spectra of the mascara samples can be found in Appendix B.

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3.3 SEM-EDS

The elemental weight percentages determined from the three analyses of each
sample were averaged to ascertain which quantified elements were most abundant in each
sample. Iron (Fe) was determined to have the largest average weight percentage in
twenty-three of the twenty-four mascara samples. The Maybelline-water (see Figure 6)
mascara sample was determined to have the highest percentage of iron, 96.7%. The lash
tint, Revlon-solvent (see Figure 7) sample, had a very minute percentage of iron (0.4%)
and in contrast had the largest percentage of silicon (85.3%) when compared to the
mascara samples. The percentage of iron is so minute in the sample that the iron peak is
not visible and was not labeled on the SEM-EDS spectrum. Silicon (Si) was determined
to be the second most abundant element in the mascara samples based on the average
weight percentages calculated for the quantified elements. Calculated averages of the
elemental weight percentage data for the mascara samples can be found in Appendix C,
Table 6. All of the remaining SEM-EDS spectra of the mascara samples can also be
found in Appendix C.

Ratios were then calculated from the elemental weight percents determined from
each SEM-EDS sample run. The following elemental ratios were calculated: Fe/Si,
Si/Al, Mg/Al, Si/Mg, Fe/Na, Si/Na, Mg/Na, Al/Na, Fe/Mg, and Fe/Al. The three ratios
calculated for each sample were averaged and a standard deviation was determined. In
order to establish whether the twenty-five mascara samples could be differentiated from
one another using SEM-EDS data, an inclusion rule was implemented from a previous
forensic study involving crayons (7). Each of the ratios of one sample will be determined

to be either inclusive or exclusive of another sample based on whether the ratio average

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22

falls within (inclusive) or out (exclusive) of a low and high range within three standard
deviations of the sample to which it is compared. Examples of these elemental ratio
calculations and inclusion rule comparisons are displayed in Tables 3 and 4. Samples
were labeled as lower case letters to allow for a more simplified nomenclature during
sample comparisons. SEM-EDS ratio calculation results for all of the mascara samples

can be found in Appendix C, Table 7.

Table 3: Example of elemental ratio calculation results for two mascara samples

 

Sample Calculations Fe/Si Si/Al WA] Si/M Fe/N a
Maybelline-hybrid Ratio Average 1.48 32.14 18.23 1.76 20.14
Standard Dev 0.18 5.14 2.00 0.12 1.47
(m) Low 0.95 16.71 12.25 1.40 15.73
High 2.01 47.57 24.22 2.11 24.56
Maybelline-solvent Ratio Average 2.71 3.00 2.20 1.36 45.86
Standard Dev 0.11 0.22 0.10 0.05 15.42

(n) Low 2.39 2.35 1.91 1.22 -0.39
High 3.04 3.65 2.49 1.51 92.12

 

 

 

 

 

 

 

 

 

 

 

Table 4: Example of inclusion rule comparison for two mascara samples

 

 

 

 

 

 

 

 

 

 

Comparison Fe/Si Si/Al Mg/Al Si/Mi Fe/Na
(m) in (n) Exclusive exclusive exclusive exclusive inclusive
(n) in (m) Exclusive exclusive exclusive exclusive exclusive

 

The elemental ratios of the twenty-five samples were compared to each other
based on the inclusion rule which resulted in a total of 600 separate sample comparisons.
Two comparisons were all inclusive for the ten ratios, (q) in (d) and (e) in (k). Thus,

Physicians- water(q) could not be distinguished from Bonne Bell- water ((1), and Cover

23

Girl- solvent(e) could not be distinguished from Max Factor- solvent(k) based on the
SEM-EDS data compared using the inclusion rule.

If at least one of the ratios from each sample is outside of the range of another
sample, the two samples are excluded as originating from the same source. Two
comparisons resulted in a single exclusion for the ten ratios, ((1) in (q) and (d) in (0).
Thus, Bonne Bell- water(d) is distinguished from Physicians- water(q) by the Al/N a ratio,
and Bonne Bell- water(d) is distinguished from Maybelline- water(o) by the Mg/N a ratio.
Ten comparisons resulted in two exclusions from the ten ratios. Considering all 600
comparisons: 0.33% was all inclusive, 0.33% had one exclusion, and 1.67% had two

exclusions.

3.4 Visible MSP

All twenty-four of the mascara samples provided a very broad absorbance curve
in the visible region, which is between 400 and 700 nm. This ‘flat’ absorption is
characteristic of achromatic samples. None of the mascara samples could be
differentiated based on the acquired spectra. Three of these spectra have been displayed
and are labeled as Figures 8, 9, and 10.

However, the lash tint, Revlon- solvent sample, yielded a different spectral result
for each of the three colored pigments observed: blue, red, and yellow. These spectra are

labeled as Figures 11, 12, and 13.

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4. CONCLUSION
Each of the four techniques utilized in this project provided a unique level of

discrimination for the twenty-four mascara samples. The microscopic examination
technique was able to separate the samples into four groups which could not be
distinguished from one another; three groups of two samples, and one group of eighteen
samples. The F TIR analysis technique was able to separate the samples into twenty-two
groups; two groups of two samples and twenty groups of one sample. The SEM-EDS
analysis was able to exclude and distinguish between 99.67% of the 600 comparisons
based on weight percent ratios. The visible MSP analysis did not yield any
discriminatory data for the samples analyzed.

Overall, the incorporation of microscopic examination, FTIR analysis, and SEM-
EDS analysis lefi only two samples, the Cover Girl- solvent and Max F actor- solvent
samples, from being distinguished from one another. Proctor & Gamble Inc. is the
manufacturer of both the Cover Girl and Max Factor brands, which explains the inability
to differentiate the two samples. There are several other mascara brands on the market
that also share the same manufacturers (see Table 2). Thus, caution must be taken when
comparing questioned mascara samples with such brands.

The lash tint, Revlon- solvent sample, was easily distinguished from all of the
mascara samples by each of the analysis techniques.

In regards to the forensic analysis of black mascara evidence, the best technique
to employ would be SEM-EDS, followed by FTIR, and finally microscopy. However, in
regards to an analysis scheme, this order would not be recommended. Microscopy is a

preliminary examination tool and should remain as such. F1" IR would be employed next,

31

due to the lack of sample consumption, sample preparation and time required for
analysis. Although questioned mascara submitted as evidence would likely be dry prior
to laboratory analysis, samples should be dry for two days prior to analysis in order to
perform a proper comparison. Finally, SEM-EDS should be utilized last in the analysis
scheme because it requires sample alteration. The sample preparation of mascara for
SEM-EDS analysis involves carbon sputter coating, which will alter the chemical

composition of the sample.

32

5. FUTURE WORK

-As a continuation of this research, more black samples of different brands and mascaras

of the same brand could be analyzed and compared with the results of this study.

-Analysis should also be performed on different colors of mascara, such as brown, navy,
auburn, etc. This research will likely yield more useful results with visible

microspectrophotometry.

-The analysis of mascara via pyrolysis gas chromatography-mass spectroscopy should be

attempted.

-Blind studies using samples from within and outside of this study should be attempted to

determine the accuracy in comparing and identifying mascara samples.

-A study involving the transfer of mascara from one individual to another, in order to

compare the transferred samples to pristine samples, such as the samples analyzed in this

study.

33

 

APPENDICES

34

APPENDIX A.

Microscopic Examination Data

35

Table 5: Observations from the microscopic examination of mascara samples

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Brand Based Observation

Almay Hybrid Black particles, orange flakes
Almay Water Black particles, orange flakes
Aziza 11 Water Black particles, blue specks
Bonne Bell Water Black particles

Cover Girl Solvent Black particles, few brown particles
Cover Girl Water Black particles

Jane Hybrid Black particles, fibers

Jane Water Black particles, fibers
L'Oreal Hybrid Black particles, blue specks
L'Oreal Water Black particles

Max Factor Solvent Black particles, few brown particles
Max Factor Water Black particles

Maybelline Hybrid Black particles

Maybelline Solvent Black particles

Maybelline Water Black particles

Neutrogena Water Black particles

Physicians Formula Water Black particles

Revlon Hybrid Black particles, fibers
Revlon Solvent Red, blue, and yellow spots
Revlon Water Black particles, fibers
Rimmel Solvent Black particles

Rimmel Water Black particles

Sally Hansen Water Black particles

Wet'n'Wild Hybrid Black particles

Wet'n'Wild Solvent Black particles

 

 

36

 

APPENDIX B.

FTIR Spectra

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REFERENCES

1. Draelos, Z. Cosmetics in Dermatology. New York: Churchhill Livingstone, 1990.

2. Saferstein, R. Foren_sic Science Handbook. Volume 1. New Jersey: Pearson
Education, 2002.

3. Lozen, C. Telephone Interview. April 2005.

4. Kopchick, K. “Color Analysis of Apparently Achromatic Automotive Paint by Visible
Microspectrophotometry”. MS thesis. Michigan State University, 2005.

5. Pouchert, C. The Aldrich Library of FT-IR Spectra. Volume 2. Milwaukee: Aldrich
Chemical Co., 1985.

6. Mabrouk, S. “The Preparation and Testing of a Common Emulsion and Personal Care
Product: Lotion”. Journal of Chemical Education 81.2 (2004): 83-86.

7. Bommarito, C. “Forensic Analysis of Crayon via Fourier Transform Infrared

Spectroscopy (FTIR) and Scanning Electron Microscopy/Energy Dispersive
Spectroscopy (SEM-EDS)”. MS thesis. Michigan State University, 2001 .

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