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I THESIS
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ENHANCED LATENT FINGERPRINT DETECTION IN
MISSING AND EXPLOITED CHILDREN INVESTIGATIONS

presented by
ELLYN LEE SCHUETI’ E

has been accepted towards fulfillment
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2/05 cJCIRC/DateDueindd-p. 15

 

ENHANCED LATENT FINGERPRINT DETECTION IN MISSING AND
EXPLOITED CHILDREN INVESTIGATIONS

By

Ellyn Lee Schuette

A THESIS

Submitted to
Michigan State University
in partial fulﬁllment of the requirements
for the degree of

MASTER OF SCIENCE
Department of Criminal Justice

2005

ABSTRACT

ENHANCED LATENT FINGERPRINT DETECTION IN MISSING AND
EXPLOITED CHILDREN INVESTIGATIONS

By
Ellyn Lee Schuette

Cyanoacrylate fuming is one of the most common and effective methods of
developing latent ﬁngerprints on nonporous media. However, latent prints of pre-
pubescent children have been more difﬁcult to develop as the prints age than the prints of
adults.

A study was designed and executed to determine the efficacy of an acetic acid
treatment, when combined with fuming at high relative humidity, in regenerating
ﬁngerprints. Acetic acid treatment was found to improve print quality in 18.8% of 250
sample pairs. The treatment was signiﬁcantly more effective at improving the quality of
clean prints than oily prints. Additionally, a signiﬁcantly higher proportion of samples
under ﬂuorescent light and simulated sunlight were able to maintain their level of print
quality as opposed to samples stored in the dark. The acetic acid treatment was also
linked to reduced levels of background polymerization of aged samples regardless of

print type or lighting condition.

ACKNOWLEDGEMENTS

The author wishes to thank: Dr. Linda Lewis and Dr. Bob Smithwick of Oak Ridge
National Laboratory (ORNL) for their guidance throughout the course of this study;
Katherine Smithwick and the staff of the Farragut Presbyterian Children’s Enrichment
Center for hosting the children’s ﬁngerprint collection; the pre-schoolers at the Farragut
Presbyterian Children’s Enrichment Center for providing ﬁngerprint samples; Richard
Counts of ORNL for his assistance with the statistical analysis; Jennifer Froelich for the
initial work on adapting the Plexiglas box for use as a fuming chamber; Steve Wargacki
and Dr. Mark Dadmun of the University of Tennessee for sharing the results of relevant
but as-yet unpublished work; and Kimberly Hampton for her help with additional

photographing of developed prints.

This research was performed while on appointment as a US. Department of Homeland
Security (DHS) Fellow under the DHS Scholarship and Fellowship Program, a program
administered by the Oak Ridge Institute for Science and Education (ORISE) for DHS
through an interagency agreement with the US. Department of Energy (DOE). ORISE is
managed by Oak Ridge Associated Universities under DOE contract number DE-ACOS-
OOOR22750. All opinions expressed in this paper are the author’s and do not necessarily

reﬂect the policies and views of DHS, DOE, ORNL, or ORISE.

iii

TABLE OF CONTENTS

List of Tables ....................................................................................... vi

List of Figures ..................................................................................... ix

CHAPTER 1

INTRODUCTION ................................................................................. 1
GLAND SECRETIONS AND LATENT PRINT FORMATION ............ 3
SUMMARY OF FINGERPRINT FORMATION AND DETECTION ...... 5
OVERVIEW OF CYANOACRYLATE FUMING ............................. 6

THE EVOLUTION OF CYANOACRYLATE FUMING RESEARCH . 7
FUNDAMENTAL CYANOACRYLATE RESEARCH AT ORNL AND

UT .............................................................................. 11
CHAPTER 2
MATERIALS AND METHODS ................................................................ 15
PROTOCOL DEVELOPMENT / OPTIMIZATION STUDIES .............. 15
PREPARATION OF CHILDREN’S PRINTS .................................. l8
CYANOACRYLATE FUMING OF CHILDREN’S PRINTS ................ 21
CHAPTER 3
RESULTS AND DISCUSSION ................................................................. 25
PROTOCOL DEVELOPMENT / OPTIMIZATION STUDIES .............. 25
PREPARATION OF CHILDREN’S PRINTS ................................... 29
CYANOACRYLATE FUMING OF CHILDREN’S PRINTS ................ 30
General Print Type Eﬂects ................................................ 35
General Lighting Condition Eﬂects ....................................... 38
General Aging Eﬁ‘ects ...................................................... 40
General Treatment Option Effects ........................................ 40
Detailed Treatment Option Effects ....................................... 42
Sample Pair Comparisons .................................................. 47
CHAPTER 4
CONCLUSION .................................................................................... 52

iv

APPENDIX A

Participant Information & Sample Set Storage and Fuming Plans .......................... 56
APPENDD( B

Statistical Analysis ................................................................................ 60
REFERENCES ................................................................................... 74

Table 1:

Table 2:

Table 3:

Table 4:

Table 5:

Table 6:

Table 7:

Table 8:

Table 9:

Table 10:

Table I 1:

Table 12:

Table 13:

Table 14:

LIST OF TABLES

Letter Codes Used to Represent Each Finger .................................... 19
The 20 Individual Samples Assigned to Sample Set #1 ........................ 20
Overall Print Quality Ratings According to Print Type (All Samples) ....... 35

Background Polymerization Ratings According to Print Type (All
Samples) .............................................................................. 37

Overall Print Quality Ratings According to Lighting Conditions (Samples
Aged 2 to 7 Days) ................................................................... 38

Background Polymerization Ratings According to Lighting Conditions
(Samples Aged 2 to 7 Days) ........................................................ 39

Overall Print Quality Ratings According to Treatment Option (All
Samples) .............................................................................. 41

Background Polymerization Ratings According to Treatment Option (All
Samples) .............................................................................. 42

Overall Print Quality Ratings According to Treatment Option an_d Print
Type (All Samples) .................................................................. 44

Background Polymerization Ratings According to Treatment Option m
Print Type (All Samples) ............................................................ 44

Overall Print Quality Ratings According to Treatment Option _an_d
Lighting Condition (Samples Aged 2 to 7 Days) ................................ 46

Background Polymerization Ratings According to Treatment Option _an_d
Lighting Condition (Samples Aged 2 to 7 Days) ................................ 46

Comparisons of the Effect of Acetic Acid Regeneration Treatment on
Print Quality (All Sample Pairs) ................................................... 48

Comparisons of the Effect of Acetic Acid Regeneration Treatment on

vi

Table 15:

Table 16:

Table 17:

Table 18:

Table 19:

Table 20:

Table 21:

Table 22:

Table 23:

Table 24:

Table 25:

Table 26:

Table 27:

Table 28:

Table 29:

Print Quality and Background Polymerization (All Sample Pairs) ............ 49

Comparisons of the Effect of Acetic Acid Regeneration Treatment on
Print Quality According to Print Type (All Sample Pairs) ..................... 49

Comparisons of the Effect of Acetic Acid Regeneration Treatment on
Background Polymerization According to Print Type (All Sample Pairs)... 50

Comparisons of the Effect of Acetic Acid Regeneration Treatment on
Print Quality According to Lighting Condition (Sample Pairs Aged 2 to 7
Days) .................................................................................. 5 1

Comparisons of the Effect of Acetic Acid Regeneration Treatment on
Background Polymerization According to Lighting Condition (Sample

Pairs Aged 2 to 7 Days) ............................................................ 51
Gender and Age of Each Participant .............................................. 57
Storage Plan for 500 Samples from 25 Child Participants ..................... 58
Storage and Fuming Conditions for Each Sample Set .......................... 59

Statistical Analysis of Table 3 (Overall Print Quality Ratings According to
Print Type - All Samples) ........................................................... 62

Statistical Analysis of Table 4 (Background Polymerization Ratings
According to Print Type - All Samples) .......................................... 63

Statistical Analysis of Table 5 (Overall Print Quality Ratings According to
Lighting Conditions - Samples Aged 2 to 7 Days) ............................... 63

Statistical Analysis of Table 6 (Background Polymerization Ratings
According to Lighting Conditions - Samples Aged 2 to 7 Days) ............. 64

Statistical Analysis of Table 7 (Overall Print Quality Ratings According to
Treatment Option - All Samples) .................................................. 65

Statistical Analysis of Table 8 (Background Polymerization Ratings
According to Treatment Option - All Samples) ................................. 65

Statistical Analysis of Table 9 (Overall Print Quality Ratings According to
Treatment Option and Print Type - All Samples) ............................... 66

Statistical Analysis of Table 10 (Background Polymerization Ratings
According to Treatment Option and Print Type - All Samples) 67

vii

Table 30:

Table 31:

Table 32:

Table 33:

Table 34:

Table 35:

Statistical Analysis of Table 11 (Overall Print Quality Ratings According
to Treatment Option and Lighting Condition - Samples Aged 2 to 7 Days).. 68

Statistical Analysis of Table 12 (Background Polymerization Ratings
According to Treatment Option and Lighting Condition - Samples Aged 2
to 7 Days) ............................................................................ 70

Statistical Analysis of Table 15 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Print Quality According to Print Type - All
Samples) .............................................................................. 72

Statistical Analysis of Table 16 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Background Polymerization According to
Print Type - All Samples) .......................................................... 72

Statistical Analysis of Table 17 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Print Quality According to Lighting Condition
- Samples Aged 2 to 7 Days) ...................................................... 73

Statistical Analysis of Table 18 (Comparisons of the Effect of Acetic Acid

Regeneration Treatment on Background Polymerization According to
Lighting Condition - Samples Aged 2 to 7 Days) ................................ 73

viii

LIST OF FIGURES

Figure l: Cyanoacrylate Polymerization Mechanism ....................................... 8
Figure 2: Fuming Chamber....... .............................................................. 16
Figure 3: Sample Position Within Fuming Chamber ....................................... 17
Figure 4: Equipment Set-up for Digital Photography of Prints ........................... 23
Figure 5: Sample Illumination During Digital Photography of Prints .................... 24

Figure 6: Examples of the Four Overall Print Quality Ratings - “good” (A & B),
“fair” (C), “poor” (D & E), and “X” (F) .......................................... 33

Figure 7: Examples of the Four Background Polymerization Ratings — “none” (A),
“low” (B), “medium” (C), and “high” (D) ........................................ 34

ix

Chapter 1

INTRODUCTION

Within a four-month span of time in 1993, Knoxville (TN) Police Department
criminologist Art Bohanan was faced with two child abduction cases in which detection
of the children’s prints in the cars of the alleged abductors was essential to prosecution
[1,2]. The car involved in the ﬁrst case was processed four days after the kidnapping.
Powder dusting, although generally considered one of the least sensitive ﬁngerprint
development techniques, is routinely used on prints up to one-week—old and has even
been shown to develop prints as old as nine months [3,4]. However, although several
peOple witnessed the young girl entering the car, no prints from the victim were found.
Bohanan suspected the explanation was that “the child’s ﬁngerprints just weren’t lasting
very long” [I], and he resolved to press for processing of evidence as soon as possible in
any future child abduction cases. Less than four months later, another young girl was
abducted. The suspect’s vehicle was found seven hours after the three-year-old victim’s
disappearance, and Bohanan made ﬁngerprint processing a priority. Within thirty
minutes, palm prints belonging to the child were located on the inside surfaces of the
back windows. When the defendant recanted his confession (made while he was under
the influence of drugs and alcohol) to the abduction, rape, and murder of the child, the
recovered palm prints became even more important to the prosecution and eventual

conviction of the defendant.

Intrigued by the implication of the casework, Bohanan searched for information
on the differences between prints deposited by adults and children, but found no relevant
reports [I]. Dissatisﬁed, Bohanan devised his own experiments to investigate the
durability of children’s prints. In one ﬁeld test, Bohanan supervised children touching
the insides of all the cars in police custody. Twenty-four hours later, no prints were
detected. In another experiment, Bohanan directed adults and children to handle separate
clean plastic and glass bottles. When he examined bottles stored inside vehicles, he
found that the children’s prints were often undetectable by powder after twenty-four
hours, while adult prints could be recovered several days after deposition.

Interested in determining the reason for this difference in the limits of detection of
prints deposited by children and adults, Bohanan approached scientists at Oak Ridge
National Laboratory (ORNL). Dr. Michelle Buchanan, an analytical chemist, directed a
study of the chemical composition of ﬁngertip secretion samples from twenty-ﬁve
children (from 4 to 12 years old) and twenty-ﬁve adults (from 17 to 64 years old). The
secretions were extracted directly from the ﬁngertip through contact with rubbing alcohol
(70% v/v isopropanol in water). Analysis of the samples by gas chromatography/mass
spectrometry (GC/MS) revealed a marked difference in the chemical composition of
samples from the two different age groups [1]. Free fatty acids were found in greater
abundance in the samples from children than in those from adults. Conversely, long-
chain alkyl esters were found in much higher concentrations in the adult samples than in
the samples from children. Free fatty acids are relatively small and volatile, while the
long-chain alkyl esters are of a much higher molecular weight and less volatile. Thus,

compositional differences translate into faster evaporation rates for children’s prints than

adult prints. This in turn helps to explain why police have a much smaller window of

time to detect children’s prints.

GLAND SECRETIONS AND LATENT PRINT FORMATION

The human body contains three major types of secretory glands: eccrine,
sebaceous, and apocrine. Eccrine glands are distributed throughout the surface of the
body, with highest concentrations on the palms and the soles of the feet (together called
the volar surfaces). Sebaceous glands are associated with hair follicles and are located
throughout most of the body, particularly the face and scalp. Notable exceptions are the
volar surfaces, which contain no hairs and therefore no sebaceous glands. However,
secretions of the sebaceous glands (called sebum) are often found on volar surfaces,
especially ﬁngers and palms, due to frequent contact with other areas of the body like the
face. Apocrine glands are localized to hair follicles in the axillary regions (that is, the
armpits and genital area), and apocrine secretions rarely contact volar surfaces.

In addition to containing a high density of eccrine glands and no hair follicles or
accompanying sebaceous glands, the volar surfaces are notable for the ridges of the skin.
Designed to allow humans to grip objects, the skin ridges form intricate patterns that are
considered unique to each individual. The latent (hidden) prints of interest to forensic
scientists form when an area of this ridged skin, coated in eccrine secretions and/or
transferred sebum, touches another surface. If the ridged skin (also called friction skin) is
coated only in eccrine material, the deposited print is referred to as a “clean” print. If the

friction skin has contacted non-volar surfaces, the deposited print is termed “oily”

because it contains a mixture of eccrine and sebaceous secretions.

Eccrine secretions are predominantly water (in excess of 98%), with traces of
salts (most notably sodium chloride and sodium lactate), free amino acids, urea,
mucoproteins, ammonia, and negligible amounts of lipid material [5,6]. In general,
sebum is composed of triglycerides, wax esters, free fatty acids, squalene, sterols, and
sterol esters [5 ,6]. The relative amounts of each component vary with respect to age, as
discussed earlier, and also across individuals within the same age group. A major factor
in the compositional disparity between secretions of adults and children appears to be the
production of adrenal androgens, a process that begins between the ages of seven and ten.
Sebaceous glands are underdeveloped in young children and epidermal lipids, such as
cholesterol and cholesterol esters, dominate the sebum [7]; after adrenal androgens are
produced, sebaceous lipids, such as squalene and wax esters, are prevalent at levels two
to three times larger than during early childhood [5,7]. Additionally, free fatty acids form
a larger percentage of the sebaceous material of children than of adults [5]. With more
volatile components and smaller quantities of hygroscopic components, the prints of pre-
pubescent children dry out more quickly than those of adults, provided that the ﬁngers of
the children are not contaminated with transfer sebum from an adult. The degree of
evaporation of a print has important implications on the ability of many ﬁngerprint
development techniques, including cyanoacrylate fuming, to develop prints of good
quality.

While the donor age dependency of the chemical content of general sweat
samples has been well-established for decades [5], it was not until the work of Dr.

Buchanan’s group at ORNL that age-related compositional differences speciﬁc to

ﬁngertip secretions were investigated and reported. A later study conducted at Paciﬁc
Northwest National Laboratory (PNNL) took the next step. Based on analysis of prints
left on glass ﬁber ﬁlter paper [8], chosen as a neutral substrate that was practical for the
subsequent analysis protocol, the PNNL study concluded that the compositional

differences were detectable in the deposited prints of children and adults.

SUMMARY OF FINGERPRINT FORMATION AND DETECTION

The value of a ﬁngerprint lies in its designation as individualizing evidence; that
is, it is possible to identify the origin of a ﬁngerprint as one, and only one, source. The
single most important factor affecting a print examiner’s ability to classify and
individualize a print is print clarity. The options available to an examiner to maximize
the clarity of a given print depend on how that print was produced. When a ﬁnger is
pressed into a moldable substance (e. g. wax, caulk, or gum), the resulting three-
dimensional reverse molding of the friction ridges and furrows is said to be an impressed
print. Enhancement of impressed prints is typically limited to altering lighting conditions
to increase the contrast between the ridges and furrows during photography of the print.

Prints formed by the transfer to the touched surface of a substance coating the
friction ridges other than natural gland secretions (e.g. blood, ink, dirt) are called patent
(visible) prints. Print clarity sometimes may be enhanced by lifting the print with
transparent tape and transferring it to a background of greater contrast. Optical methods
are often employed to enhance contrast of the print media and background substrate.

Additionally, various chemical reagents have been developed to enhance weak prints

deposited in blood by targeting hemoglobin (e. g. tetramethylbenzidine, phenolphthalein,
leucomalachite green) or proteins (e. g. amido black, ninhydrin, Coomassie blue, 1,8-
diazaﬂuoren-9-one, commonly known as DFO).

The third and most common method of print formation is by the transfer to the
touched surface of natural gland secretions coating the friction ridges. Because the
natural gland secretions are essentially colorless, such prints are not readily visible;
hence, they are called latent (hidden) prints. A signiﬁcant amount of scientiﬁc research
has been conducted to successfully visualize latent prints with ever-improved clarity on a
wider variety of substrates under a greater variety of conditions. Out of this research,
numerous optical, physical, chemical, and (recently) instrumental methods have been

established for the visualization of prints under speciﬁc conditions

OVERVIEW OF CYANOACRYLATE FUMING

Cyanoacrylate fuming, also known as Super Glue® fuming, is a chemical method
of ﬁngerprint development that has risen to prominence in recent years. It involves the
vaporization and polymerization of liquid cyanoacrylate ester along the ridges of exposed
ﬁngerprints to yield a hard, white-colored print. The technique is most useful on
nonporous surfaces such as plastics, metals, and glass. It is also routinely used on
semiporous surfaces like rubber and glossy paper. In fact, cyanoacrylate fuming is the
third technique (following standard visual examination and attempts at revealing inherent
ﬂuorescence by laser or alternate light source) employed by the FBI’s Latent Print Unit

on nonporous surfaces, the non-adhesive side of tapes, the semiporous paper side of

photographs, and semiporous glossy papers [9]. Cyanoacrylate fuming also appears in
the FBI’s recommended processing sequences for nonporous blood-stained specimens,
semiporous rubber, and the emulsion side of photographs [9].

The compatibility of this technique with a large number of surfaces is one of its
most notable advantages. Other advantages include the permanence of the developed
prints; the simplicity of the procedure; the lack of damage to the fumed substrate; the
ability to process many items of evidence simultaneously in the lab; the adaptability of
the technique to ﬁeld use; the ability to perform subsequent DNA testing on fumed
ﬁngerprint material; and the relatively low cost of the technique. Of course,
cyanoacrylate fuming is not without disadvantages such as the danger of releasing
cyanide gas at high fuming temperatures; the possibility of over-developing a print (i.e.
substantial background polymer growth, particularly in the furrows between ﬁngerprint
ridges); and the poor contrast of developed prints with light-colored backgrounds.

However, research has found ways around these pitfalls.

THE EVOLUTION OF CYANOACRYLATE FUMING RESEARCH

This technique originated in 1978 at the Criminal Identiﬁcation Division of the
Japanese National Police Agency [5]. However, it was not until workers from the US.
Army Criminal Investigation Laboratory in Japan (USACIL-Paciﬁc) and the Bureau of
Alcohol, Tobacco, and Firearms introduced the technique to the United States in 1982
that scientists began researching ways to improve its efﬁciency and range of use [5].

The original procedure involved placing several drops of liquid cyanoacrylate

ester in a dish at the bottom of an enclosed container in which a specimen was suspended.
Over the course of several hours at ambient conditions, the liquid cyanoacrylate
vaporized and selectively polymerized along the ridges of any exposed ﬁngerprints,
producing durable whitish-colored prints. Figure 1 shows the structure and
polymerization mechanism of the cyanoacrylate ester, where A” represents an initiator
(discussed in greater detail beginning on page 11) of the polymerization reaction, and R

represents an alkyl group (commonly an ethyl group for cyanoacrylate ﬁngerprint

 

 

development).
(Initiator)
N A- EN A- j‘N
ROOC‘ECl-l2 «v-——' ROOC 6' CH2 _> ROOC _ CHZ-A
6+
Cyanoacrylate ' - -
Ester
' N
ROOC U CH2
CN CN /
Further | I
POLYMER *——_— ROOC _ C CHz-A
Reaction I

H2
COOR
Figure l: Cyanoacrylate Polymerization Mechanism

Soon, numerous articles were published describing procedures to accelerate the
process, focusing on ways to increase the speed at which cyanoacrylate vapors were
produced and/or improve the contact of cyanoacrylate fumes with the specimens. These
ﬁrst acceleration procedures included circulating the fumes with a small fan, heating the
cyanoacrylate ester, and introducing the cyanoacrylate ester to the enclosure on absorbent
cotton containing sodium hydroxide [5]. Current incarnations of the cyanoacrylate

fuming procedure may incorporate one or more of these acceleration techniques.

However, these accelerated processes still typically require 30 to 60 minutes of fuming.

In 1986, Almog and Gabay reported a method that involved heating
polycyanoacrylate, the solid polymeric form of cyanoacrylate [10]. In spite of the
elimination of the risks associated with handling liquid cyanoacrylate, and a reduction of
the fuming time to “a few minutes,” the use of liquid cyanoacrylate still predominates.
However, the method is sometimes adapted as a remedy to the problem of over-
developed prints: careful heating of such prints can release monomeric vapors from the
solid polymer. The drawback is that re-fuming of the print in question is not possible
after such treatment [5].

A modiﬁcation that has gained popularity is the use of a vacuum chamber to
conduct the fuming at signiﬁcantly reduced pressure. First presented in 1994, the
vacuum procedure has two notable advantages over fuming at ambient pressure: the
vacuum method is able to consistently develop high-quality prints on irregular surfaces,
and the issue of over-fuming is signiﬁcantly reduced. Unfortunately, vacuum fuming
requires a relatively long fuming time and yields prints that have less cyanoacrylate
build-up, making them harder to see and less robust than counterparts fumed at ambient
pressure. Grady was able to signiﬁcantly reduce the fuming time (as short as 12 minutes)
by incorporating the heating of the cyanoacrylate, but difﬁculty with print visualization
remained [11].

An alternate modiﬁcation is the introduction of a source of humidity to the
enclosure during the fuming process. The humidity source can be as simple as a cup of
hot water or as sophisticated as a purpose-built humidity cabinet. Several references

suggest achieving 80% relative humidity for optimal results [6,12]; however, the FBI

recommends fuming between 70% and 80% relative humidity [9], and a recent study
maintained that a 60% relative humidity level produced the best quality prints [13].

With the “microburst” method of fuming conducted by the FBI using
cyanoacrylate heated to approximately 400°C, fuming time has been pushed to between
30 seconds and four minutes [9]. Therefore, the focus of the majority of recent
cyanoacrylate fuming research has shifted from acceleration to visualization
enhancement.

One of the major disadvantages plaguing cyanoacrylate fuming is the lack of
contrast of developed prints on light-colored backgrounds. A wide variety of post-
fuming treatments have been reported to overcome this issue. A sampling of such
treatments includes: dusting with standard, magnetic, or ﬂuorescent ﬁngerprint powders
[5,14]; a combination of ninhydrin and zinc chloride followed by laser examination [15];
biological stains or Rit® fabric dyes [I6]; europium-based ﬂuorescent dyes [17];
sublimation dyes from the anthraquinone family of compounds that target the
cyanoacrylate polymer [18]; sublimation-grade disperse dyes that target the background
[19]. Visualization can also be improved by analyzing fumed prints with more
sophisticated instrumentation. A recently published study employed a Fourier Transform
Infrared (FT IR) spectrometer and infrared microscope to chemically image
cyanoacrylate-fumed prints against the multi-colored background of the new Australian
polymer banknote [20].

Improving the detection sensitivity (i.e. number and quality of developed prints)
inherent to the cyanoacrylate fuming method itself is a valuable but less common area of

research. Noting that amine vapors have been used in semi-conductor production to

10

activate inert surfaces for uniform cyanoacrylate polymer deposition, Burns et al.
investigated the effect of ammonia exposure on the quality of developed prints [21]. The
authors found that greater polymer deposition was achieved by exposing prints to
ammonia vapors prior to cyanoacrylate fuming. However, they conceded that “the
greatest polymer deposition does not always lead to the best visual mark. It is found that
polymer deposits on the ridges up to a maximum point and then starts to deposit in the

troughs of the ﬁngerprint leading to a loss of detail [21].”

FUNDAMENTAL CYANOACRYLATE RESEARCH AT ORNL AND UT

Most of the research on cyanoacrylate fuming has been predicated on the
assumption that the ﬁndings of the adhesives industry hold true for ﬁngerprint
development. One such fundamental ﬁnding is that the polymerization of cyanoacrylate
ester is initiated by basic compounds, residual moisture, and trace metals [2]]. In the late
19905, researchers at Oak Ridge National Laboratory and the University of Tennessee
(UT) collaborated on a series of experiments designed to elucidate the fundamental
processes of cyanoacrylate polymerization as it applies to the forensic science
community. They hoped that a more thorough understanding of the polymerization
process would allow them to devise a means of improving the sensitivity of
cyanoacrylate fuming to aged prints of both adults and children.

To date, unpublished work by Steve Wargacki and Dr. Mark Dadmun of UT
demonstrated that both water and anionic compounds found in eccrine secretions

(speciﬁcally lactate and alanine) initiate the polymerization of cyanoacrylate ester.

ll

However, measurements of total polymer mass were greater for lactate- and alanine-
initiated samples than for water-initiated polymerization, meaning anionic compounds are
more effective initiators than water. When trials were conducted using separate solutions
of lactate and alanine at basic, neutral, and acidic pH levels, the basic solutions yielded
noticeably greater polymer mass totals than their neutral and acidic counterparts (which
provided roughly similar polymer mass measurements). When the average molecular
weights of polymer chains were compared, polymer chains formed by anions in basic and
neutral conditions were found to have substantially greater molecular weights than those
formed by pure water or anions in acidic conditions. Researchers concluded that water
yields a small number of low molecular weight oligomers, acidic solutions of anionic
initiators form a larger amount of low molecular weight polymers, and neutral and basic
solutions of the anionic initiators form a smaller number of higher molecular weight
polymers. Furthermore, researchers suspected that W played a role in early termination
of the cyanoacrylate polymerization reaction.

In aging studies conducted by ORNL researchers, cyanoacrylate fuming (at a
relatively high ambient humidity) of oily adult depositions that were aged several months
yielded prints that, though noticeably degraded, still contained some areas of adequate
deﬁnition. However, fuming of eccrine-only adult depositions produced only faint traces
of visible polymer after merely two weeks of aging [6]. While tests of individual sebum
components conﬁrmed that they are not involved in the initiation of the polymerization
reaction [22], the results of the aging studies suggested that sebaceous materials do play
some role in polymer growth. Scanning electron microscopy (SEM) images revealed a

correlation between print composition and the morphology of the growing polymer:

12

eccrine-only prints support growth of a noodle-type structure, whereas oily prints
(containing both eccrine and sebaceous components) support capsule-type formations
that suggest an emulsiﬁcation function for the sebaceous materials [6]. Together, the
results of the initiation and aging studies suggest that the increased likelihood of
developing an aged (that is, dried out) latent print at higher humidity has more to do with
the ability of the added moisture to solubilize the eccrine-based anionic initiators than
with direct initiation of the polymerization by the water.

Faced with poor results when cyanoacrylate is used on child depositions and aged
adult depositions, researchers attempted to regenerate optimal print conditions by re-
hydrating the prints prior to fuming [22]. They evaluated water and several weak acids
(formic acid, propionic acid, isobutyric acid, valeric acid, vinegar, and glacial acetic acid)
as regenerating agents and determined that glacial acetic acid provided the best results.
Exposure to acetic acid prior to cyanoacrylate fuming was found to consistently
regenerate clean prints from adults that had been aged up to ﬁve months, resulting in a
quality of developed print that was equivalent to the quality of fresh (i.e. non-aged)
prints. Lacking the hygroscopic sebaceous materials that are present in the oily prints of
adults, children’s prints are compositionally similar to the clean prints of adults. As such,
researchers reasoned that children’s prints should respond as favorably as clean adult
prints to the acetic acid exposure. Indeed, this was the case during initial tests of prints
from children. However, a subsequent large—scale study of children’s prints recorded no
meaningful improvement in the quality of prints developed with the regeneration
treatment as compared to control prints that did not receive the regeneration treatment.

While reviewing the data, researchers realized that the trials with adult prints were

13

conducted in the spring, when ambient indoor relative humidity levels were
approximately 75%. The study of children’s prints, on the other hand, was conducted in
the winter with ambient indoor relative humidity readings of apprdximately 25%. To
determine if the difference in relative humidity could be responsible for the disappointing
results in the children’s study, two child prints that had aged eight months were fumed
under high relative humidity conditions in the summer, one without the acetic acid
treatment and the other with the treatment. In the demonstration, the quality of the
treated print was clearly superior to the quality of the untreated print. Based on this
demonstration, and the results of the initial trials, the ORNL researchers deduced that
humidity conditions within the fuming chamber have a crucial effect on the quality of
developed prints.

In an attempt to substantiate the favorable results that had been obtained during
the initial trials of children’s prints and the demonstration, the author of this thesis
designed and executed a study of prints deposited by 25 two— to ﬁve-year-old children.
The previous children’s print study [22] was used as a model, but the present study
included several signiﬁcant changes. Most notably, all fuming was conducted at high
humidity. Additionally, the regeneration treatment was substantially modiﬁed such that
acetic acid exposure and cyanoacrylate fuming were incorporated into a one—step print
development method. Finally, a third lighting option was evaluated. Lactate, a main
initiator of the polymerization process, is known to undergo photodegradation. The
sample size of this study was deemed large enough to accommodate investigation of the
effect of sample aging under sunlight, in addition to ﬂuorescent lighting and darkness.

Exposure to continuous natural sunlight was impossible, so simulated sunlight was used.

14

Chapter 2

MATERIALS AND METHODS

PROTOCOL DEVELOPMENT / OPTIMIZATION STUDIES

For the initial investigations into optimal fuming parameters, clean adult prints
were used in place of children’s prints. Latent prints were placed on clean glass
microscope slides. Clean adult prints (composed of eccrine material only) were prepared
as follows: hands were thoroughly washed and rinsed; palms were swabbed with an
ethanol-soaked wipe; hands were air-dried; thumb and foreﬁnger were rubbed together to
create an even coating of eccrine material; and thumbs were ﬁrmly pressed on the glass
slides. Oily adult prints (composed of both eccrine and sebaceous material) were
prepared in a similar manner, except once hands were dry, the thumb was swiped across
an oily region of the face (the side of the nose) before deposition on the glass slides. The
prints were stored in the dark in a laboratory drawer for periods of time up to seventeen
days.

The fuming chamber (Figure 2 on the following page) was constructed from a
thick-walled Plexiglas box with internal dimensions measuring 30.1 cm (length) x 30.1
cm (width) x 31.0 cm (height). The bottom of the box was removed, and the box was
placed on a metal platform with a square hole (14.0 cm x 15.9 em) out out of the center.

A hotplate (Ceramag Midi IKA Works Inc., Wilmington, NC) was positioned within this

IS

hole so its surface was level with the platform. A T—shape connector was used to direct
both a stream of air and the output from a PUMlOO Bionaire Humidiﬁer (SIRCHIE
Fingerprint Labs, Youngsville, NC) through tubing that was inserted into a l-inch-
diameter hole in the wall of the fuming chamber. The ﬂow rate of the stream of air was
monitored by an airﬂow meter (Dwyer Instruments Inc., Michigan City, IN) placed
before the T-shape connector. The voltage supplied to the humidiﬁer was controlled by a

VARIAC variable autotransforrner (Technipower LLC, Danbury, CT).

    

Figure 2: Fuming Chamber
(Images in this thesis are presented in color.)

A digital hygro-thermometer (Control Company, Friendswood, TX) was mounted
to the back wall of the fuming chamber approximately 3 inches from the bottom. Faced
with some discrepancy within the literature on the relative humidity level that achieves
optimal fuming results [6, 9, 12,13], FBI recommendations to fume between 70% and 80%

humidity were followed, with the range restricted to its lower half based upon the

inﬂuence of recent ﬁndings that advocated lower relative humidity levels for best results
[13]. To achieve this targeted relative humidity range (70% - 75%) within the fuming
chamber, the humidiﬁer was set on operating level 2, the VARIAC was set at
approximately 70V, and the airﬂow was regulated to 10 Umin. Once the humidity
reading reached an appropriate level, an aluminum dish (VWR Scientiﬁc Products, West
Chester, PA) containing the fuming compound was positioned on the hotplate which was
heated to a surface temperature of 150°C. Fuming compounds included ethyl—2-
cyanoacrylate ester (SRCHIE Fingerprint Labs, Youngsville, NC) and glacial acetic acid
(Aldrich Chemical Company, Milwaukee, WI). The glass microscope slide was afﬁxed
with double-sided tape to a large spatula, which was inserted into a 2-inch-diameter hole
in the wall opposite the humidity inlet. The slide was positioned approximately 3 inches

above the fuming compound (Figure 3).

 

Figure 3: Sample Position Within Fuming Chamber
(Images in this thesis are presented in color.)

Throughout the optimization trials, the amounts and sequences of the fuming

compounds were varied, as were fuming times. (Relevant details about these variations
are provided in the Results and Discussion section of this thesis.) The ﬁnalized protocol
for the regeneration treatment called for 90 seconds of fuming using approximately 0.36g

of a 2:1 (wzw) cyanoacrylatezacetic acid mixture.

PREPARATION OF CHILDREN’S PRINTS

Approval to conduct research involving human subjects was obtained from the
Oak Ridge Site-wide Institutional Review Board and the Michigan State University
Committee on Research Involving Human Subjects.

One-inch diameter mirrored glass disks (Darice Inc., Strongville, OH) were
soaked in 70% nitric acid (Mallinckrodt Laboratory Chemicals, Phillipsburg, NJ) to
remove the silver backing. The resulting glass disks were cleaned, dried, and afﬁxed to
the bottom of plastic collection dishes.

A local pre-school agreed to host the ﬁngerprint collection activity. Parental
consent was obtained and documented with signed informed consent forms. A total of
500 prints were collected from 25 children between the ages of two and ﬁve years.
Guided by a gloved researcher, each child ﬁrmly pressed each ﬁnger against a separate
clean glass disk for three seconds. Each child washed his/her hands with soap and water,
allowed them to air-dry, and then repeated the print collection procedure. (Thus, each
child deposited twenty total prints.) Each child was assigned a participant number, which
was recorded along with the child’s age and gender (but not the child’s name). Each

collection dish was labeled with the child’s participant number, a code letter representing

18

which of the child’s ten digits produced the print, and the word “before” (for oily prints
deposited prior to hand-washing) or “after” (for clean prints deposited after hand-
washing). The code letter assignments are summarized in Table 1.

Table 1: Letter Codes Used to Represent Each Finger

 

 

 

 

 

 

 

 

 

 

 

 

 

Code Letter Hand Finger
a Left Thumb
b Left I Index Finger]
c - Left Middle Finger
d Left Fourth Finger
e Left Little Finger
f Right Thumb
g Right Index Finger
h Right [Middle Finger
i Right IFourth Finger]
j Right | Little Finger |

 

 

All prints were transported to the lab and stored in the dark while a storage plan
was created speciﬁc to the overall study size and the age and gender distribution of the
participants. For a list of the gender and age of each participant, see Appendix A (page
57). The storage plan divided the total number of collected prints into 25 sample sets.
Each sample set contained a pair of clean prints (those collected after hand—washing)
from the same digit of both hands of ﬁve different children, as well as a pair of oily prints
(those collected before hand-washing) from the same digit of both hands of another ﬁve
children. Thus, each sample set contained pairs of prints from 10 different participants.
This was done to prevent the possibility of skewed data for any sample set due to the
inherent inferior print quality of a single participant. Print quality can be affected by
factors particular to individuals such as skin conditions and secretion amounts; therefore,
some people consistently deposit poorer quality prints than others. The left-hand print

(labeled a—e) of each pair was designated for development by cyanoacrylate fuming at

19

high humidity without the acetic acid regeneration treatment; the right-hand print (labeled
f-j) of each pair was designated for development by cyanoacrylate fuming at high
humidity with the acetic acid regeneration treatment.

Reﬂecting the gender ratio of the overall population, three of the pairs of clean
prints and three of the pairs of oily prints in each sample set belonged to female
participants, while two pairs of clean prints and two pairs of oily prints had been
deposited by male participants. Attempts were also made to reﬂect the overall age
distribution within sample sets. Table 2 provides an illustration of these assignments
using the 20 individual samples assigned to Sample Set #1.

Table 2: The 20 Individual Samples Assigned to Sample Set #1

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Designated
Participant Participant Participant Finger for Acetic Print
# Gender Age Code Acid? Type
1 F 5 a No Clean
5 F 4 b No Clean
18 F 3 c N 0 Clean
4 M 5 d No Clean
6 M 5 e No Clean
2 F 5 a No Oily
13 F 4 b N o Oily
19 F 3 c No Oily
8 M 5 d No Oily
20 M 3 e N o = Oil;
1 F 5 f Yes Clean
5 F 4
18 F 3 h
4 M 5 i
6 M 5 '
2 F 5 f
13 F 4
19 F 3 h
8 M 5 i
20 M 3 '

 

2O

CYANOACRYLATE FUMING OF CHILDREN’S PRINTS

Sample Set #1 was pulled aside for immediate fuming; the remaining 24 sample
sets were divided equally among three storage conditions. Eight of the sample sets were
stored in the dark inside a laboratory cabinet. Eight of the sample sets were stored under
continuous ﬂuorescent illumination, approximately 22 inches below two 18—inch, lS—watt
F15T8-WW Warm White ﬂuorescent bulbs (General Electric Company, Cleveland, OH)
with spectral distribution from 380 nm to 730 nm (primary peaks at 530-540 nm and 580-
600 nm). The ﬁnal eight sample sets were stored under continuous “simulated sunlight”
illumination, approximately 22 inches below two l8-inch, lS-watt F15T8 Natural
Sunlight bulbs (Philips Lighting Company, Somerset, NJ) with spectral distribution from
360 nm to 738 nm (primary peak at 444 nm). The speciﬁc storage plan used in this study
is summarized in Appendix A (page 58).

After designated aging times, speciﬁed sample sets were removed from storage
conditions and fumed. The choice of aging times under investigation was limited by the
number of available sample sets. The samples sets kept in the dark were fumed after 2, 3,
4, 5, 7, 14, 21, and 28 days of storage. Three of the sample sets under ﬂuorescent and
“simulated sunlight” illumination were fumed within one day of storage (at 1.5 hrs, 3 hrs,
and 18 hrs). These early fumings of illuminated samples were completed because a
previous study [22] had concluded that lactate photodegradation, a major contributor to
poor print development, occurs rapidly. The remaining ﬁve samples sets subjected to
each type of illumination were fumed after 2, 3, 4, 5, and 7 days of storage. All sample
sets were fumed with the humidiﬁer operating at setting ‘2’ and an airﬂow rate of 10

Umin. However, three different VARIAC settings were employed over the course of the

21

study. Sample Set #1 (the initial fuming) was developed with the VARIAC supplying
85V to the humidiﬁer. Sample Sets #2-6 (the sets under illumination for less than one
day) were developed with the VARIAC supplying 70V to the humidiﬁer. Sample Sets
#7-25 (all sets in dark storage and those sets under illumination for two or more days)
were developed with the VARIAC supplying 75V to the humidiﬁer.

Prints not receiving the regeneration treatment were fumed using approximately
0.24 g of ethyl-2-cyanoacrylate ester in an aluminum dish placed on a hotplate heated to a
surface temperature of 150°C. Prints were initially exposed to fumes for 30 seconds;
additional fuming time was added for visibly underdeveloped prints in 30-second
increments up to a maximum total fuming time of 120 seconds.

Treated prints were fumed using approximately 0.36 g of a 2:1 (w:w) ethyl-2-
cyanoacrylate ester: glacial acetic acid mixture. Prints were initially exposed to fumes for
90 seconds; additional fuming time was added for visibly underdeveloped prints in 30-
second increments up to a maximum total fuming time of 180 seconds. The fuming time,
temperature within the chamber, and humidity level within the chamber were recorded
for all prints.

Once the fuming of all sample sets was completed, a visual examination of each
print was conducted under ambient room lighting. Each print was assigned a rating for
the overall print quality (“good,” “fair,” “poor,” or “X” for undeveloped prints).
Essentially, print quality is analogous to the clarity and quantity of ridge detail. To
receive a quality rating of “good,” a print had to have a substantial area of well-deﬁned
ridge detail. That is, several Level 2 ridge details (also called minutiae) used by trained

print examiners to make print identiﬁcations, such as ridge endings and bifurcations

22

(forkings), had to be discernible. A rating of “fair” was assigned to prints having only
limited Level 2 ridge detail, either because the area of adequate clarity was small, or
because the ridge detail was difﬁcult to visualize. The “poor” rating was assigned to
prints with no visible minutiae. In addition to overall print quality, a rating was assigned

99 (6

to indicate the amount of background development (“none,” “low, medium,” or
“high”).

Digital images were obtained using a Panasonic Color Digital Camera GP-KR22
with Navitar 7000 Zoom lens (Figure 4) and Interface Industrial Image capture board
equipped with Oculus TCiPro Version 2.20 imaging software (Coreco Inc., Saint—
Laurent, Quebec, Canada). The glass disks were photographed against a black
background with oblique lighting from a Fiber-Lite High Intensity Illuminator (Dolan—
Jenner Industries Inc., Lawrence, MA). The two light sources of the dual gooseneck

illuminator were positioned on opposite sides of the disk (Figure 5, following page), at

distances of between 1.5 and 3.5 inches.

 

Figure 4: Equipment Set-up for Digital Photography of Prints
(Images in this thesis are presented in color.)

23

  

,c

Figure 5: Sample Illumination During Digital Photography of Prints
(Images in this thesis are presented in color.)

24

Chapter 3

RESULTS AND DISCUSSION

PROTOCOL DEVELOPMENT / OPTIMIZATION STUDIES

Clean adult prints were used as a substitute for child prints while the optimal
fuming parameters were investigated. During the trials, slight adjustments were made to
the voltage setting of the VARIAC to maintain the target relative humidity level.
Increasing the voltage setting would increase the output from the humidiﬁer and raise the
humidity level in the fuming chamber; conversely, decreasing the voltage setting would
decrease the humidiﬁer output and subsequently lower the humidity level in the fuming
chamber. The targeted humidity level range was 70-75%. Because the fuming chamber
was open to the surrounding environment by way of the sample insertion port, precise
control and maintenance of the humidity measurement was limited. In practice, anything
between 68% and 78% was considered acceptable.

The ﬁrst parameter of interest was the amount of acetic acid exposure necessary
for developing prints of good quality. Prints developed by cyanoacrylate fuming at high
humidity without any exposure to acetic acid served as controls. In previous work with
the acetic acid regeneration treatment [22], samples were “slightly fogged” with heated
acetic acid vapors three successive times, with time allowed for mist dissipation between
each exposure. In the current study, this “slight fogging” was achieved by exposure to

heated acetic acid for 5 seconds. In multiple trials of samples aged up to three days,

25

limiting acetic acid exposure to one 5-second fogging yielded developed prints of better
quality than prints developed after three 5-second exposures to acetic acid. Prints treated
in the latter manner had high levels of background development plus beading along the
ﬁngerprint ridges, which served to obscure ridge detail.

Another variation under investigation was fuming the samples in an environment
of acetic acid vapors combined with high humidity. Acetic acid was heated for 3 to 4
minutes to allow the vapors to saturate the fuming chamber. Then the dish of acetic acid
was removed and replaced with a dish of cyanoacrylate. In multiple trials of samples
aged up to three days, the prints developed in the acetic acid environment were faint (i.e.
low polymer build-up along ridges) with moderate to substantial background
development that obscured ridge detail. In trials that altered the amount of time acetic
acid vapors were allowed saturate the chamber (approximately 2 minutes and 18
minutes), the subsequent development yielded substantial background that interfered with
the ridge details. Thus, fuming in an acetic acid environment led to adverse results, and
further work in this direction was abandoned.

A second major parameter of interest was the mass of cyanoacrylate necessary for
good development of prints. Trials were conducted using fresh samples and samples
aged 3 and 4 days. In the modiﬁed “microburst” method of fuming employed throughout
this study, with samples fumed individually (or at most two-at-a-time) while held 3
inches directly above the heated cyanoacrylate, relatively small amounts of cyanoacrylate
would be required. Therefore testing began with the smallest possible mass (one drop,
average mass of 0.033 g) and increased by whole number increments of drops. Less than

0.10g of cyanoacrylate (three drops) was unable to sustain vapor production for a length

26

of time necessary for adequate polymerization of the ridges, yielding faint
underdeveloped prints. Samples fumed for 30 seconds with between 0.14g and 0.24g
(four to seven drops) of cyanoacrylate yielded prints of adequate quality. Samples fumed
for 30 seconds with 0.27g or more (eight or more drops) of cyanoacrylate yielded prints
with high levels of interfering background development. In subsequent testing of lO—day-
old oily adult prints, fuming with less than approximately 0.24g (seven drops) of
cyanoacrylate yielded developed prints that could be smeared. Permanence of developed
prints is a desirable advantage of cyanoacrylate fuming. Therefore, 0.24g (seven drops)
of cyanoacrylate was chosen as the amount able to achieve the best development of both
clean and oily prints under the given fuming conditions (i.e. samples of a small size
positioned close to the source of the cyanoacrylate fumes).

The next important parameter to investigate was the method of acetic acid
exposure. While good results were produced by earlier trials of sequential exposure to
acetic acid and cyanoacrylate, a one-step simultaneous exposure to both compounds
would simplify the process and make acetic acid regeneration more appealing to forensic
scientists. Unfortunately, it was not possible to precisely measure the amount of acetic
acid that vaporized in 5 seconds. Additionally, it was noted that there was typically a 5-
to lO-second delay between the placement of the acetic acid on the hotplate and the
introduction of the ﬁngerprint sample into the humidity chamber. A starting volume of
0.1 mL of acetic acid was found to completely evaporate in an average of 45 seconds,
well surpassing the total 10- to 15-second evaporation time that was estimated as
necessary. However, in trials of simultaneous fuming by 0.1 mL acetic acid and

approximately 0.24g (seven drops) of cyanoacrylate, the resulting prints were found to

27

have a print quality (i.e. clarity of ridge detail) analogous to those developed by the
earlier runs of sequential fuming with only 5 seconds of acetic acid exposure. During
simultaneous fuming, the production of visible cyanoacrylate fumes was delayed, and
longer total fuming times were necessary to achieve the same print quality (105 seconds,
as compared to the 30 seconds typically adequate during sequential fuming). However, it
was suspected that some polymerization of the cyanoacrylate had begun before all the
acetic acid had evaporated, thereby neutralizing the deleterious effects of using larger
quantities of acetic acid (as demonstrated in the earliest sequential-fuming trials). The
conditions for simultaneous fuming were repeated in numerous trials of prints aged up to
7 days; all trials yielded prints of good quality and clarity.

A volume of 0.1 mL acetic acid has a corresponding average mass of 0. 105 g;
therefore, the initial mixture was roughly 20 parts (0.24g) cyanoacrylate to 9 parts
(0.105g) acetic acid. Because the selection of 0.1 mL of acetic acid had been somewhat
arbitrary, trials were conducted using mixtures with different ratios of the components.
Using the 20:9 (or 10:4.5) initial ratio as a starting point, tested ratios included 10:4, 10:5,
and 10:6 cyanoacrylatezacetic acid. As always, multiple trials were conducted on clean
adult prints. The 10:5 mixture (or 2:] mixture) yielded prints within 90 seconds of
fuming that had the best combination of high ridge detail and low background. When
tested on oily prints, the 2:1 mixture was found to be equally effective. Because the 2:1
mixture was bracketed on both sides (i.e. both more and less acetic acid content) by
mixtures that performed worse, further ratio variation experiments were discontinued.

Thus, at the conclusion of the optimization trials, a method of administering the

acetic acid regeneration treatment was available. When fumed at high humidity, samples

28

of clean and oily adult prints aged up to 17 days that were subjected to the regeneration
treatment (consisting of approximately 0.35 g of cyanoacrylate and acetic acid in a 2:1
(w:w) mixture) developed with comparatively greater print clarity and less background
polymerization than samples fumed with the standard cyanoacrylate-only treatment. This

reﬁned acetic acid treatment method was next applied to the study of children’s prints.

PREPARATION OF CHILDREN’S PRINTS

A total of 500 prints were collected from 25 children for use in this study. The
population included 15 females and 10 males, and the ages of the participants ranged
from two to ﬁve years. For a list of the gender and age of each study participant, see
Appendix A (page 57). The prints were divided into 25 sample sets of 20 prints, as
discussed in the Materials and Methods section of this thesis, and stored under one of
three lighting conditions. Lewis et al. previously reported on the photodegradation of the
lactate present in ﬁngerprint material [22], a phenomena that occurs in prints exposed to
sunlight as well as ﬂuorescent lighting. Storage under natural sunlight was impractical
due to the inability to maintain continuous lighting and the possibility of rain harming the
ﬁngerprint samples. Instead, sunlight was “simulated” using a specially-marketed light
with a spectral distribution that penetrated further into the UV wavelengths than standard
ﬂuorescent lighting. The speciﬁc storage assignments are provided in Appendix A (page

58).

29

CYANOACRYLATE FUMING OF CHILDREN’S PRINTS

On the day that fuming was scheduled to begin, the hotplate used throughout the
optimization trials (Ceramag Midi IKA Works Inc., Wilmington, NC) failed to heat. No
hotplate with similar dimensions was available; therefore, the non-functioning hotplate
was replaced with a larger one (Corning Inc., Acton, MA). Not able to ﬁt within the
metal platform’s hole, the larger hotplate was positioned directly below the platform. To
achieve the target humidity range (70% - 75%), the voltage output to the humidiﬁer was
increased to 85V.

The ﬁrst set of 20 samples was fumed under the conditions described above. The
majority of the samples (18 of 20) had little to no ridge detail. Two samples failed to
develop any print detail at all, and only two samples received a “good” rating for the
overall quality of the print development. In addition, 18 of the 20 samples had moderate
or high levels of background polymerization. These results were unexpectedly poor
given the relatively short time interval between deposition and development (the prints of
Sample Set #1 were only subject to the day-long dark storage common to all samples
while the detailed storage plan was created and the prints were sorted according to the
plan). Also of note was the tendency of the polymer build-up to be easily brushed off the
substrate surface. Together, these factors indicated that the relative humidity during
fuming was too high.

When data was reviewed, it was realized that the temperature within the fuming
chamber was more than 10 degrees higher than it had been during the optimization trials.
The surface contact between the larger hotplate and the metal platform caused this

elevation. Because humidity levels are relative to the temperature and volume of the air,

30

and the volume of air in the fuming chamber was fixed, more moisture output by the
humidiﬁer was required to maintain the target humidity readings at the higher
temperatures. However, this increase in the total moisture content of the air hindered the
efﬁcacy of the cyanoacrylate fuming. During optimization trials, voltage settings
between 70V and 75V had produced a moisture content in the fuming chamber effective
at improving the quality of cyanoacrylate fuming results. Returning the voltage setting to
70V ensured that the same moisture content would be present, even though the relative
humidity measurements would be lower than they had been during the optimization trials
due to the increased temperature.

Another noteworthy issue from the initial fuming was that the fuming compounds
(whether cyanoacrylate-only or the 2:1 (w:w) cyanoacrylatezacetic acid mixture) did not
produce visible fumes as readily as they had in the optimization trials. Jostling the
hotplate was found to aid in the timely production of such visible fumes. It is not
understood why the difﬁculty arose, but the jostling motion was adopted during all
subsequent fumings to overcome the issue.

The adjusted conditions (large hotplate; 70V voltage setting; jostling motion to
increase fume production) were used to fume the next six sample sets, comprised of
prints stored under ﬂuorescent lighting or “simulated sunlight” for 1.5, 3, or 18 hours.
Following these fumings, a smaller hotplate (Cole-Parmer Instrument Co., Vernon Hills,
IL) was located. The hole in the platform was slightly widened to allow this newest
hotplate to be raised into a position level with the bottom of the fuming chamber.

Despite removing the direct hotplate-to-platform contact, temperatures within the fuming

chamber remained elevated as compared to temperatures during the optimization trials

31

conducted with the ﬁrst hotplate. The reason for this disparity remains unknown. The
voltage setting was increased to 75V (the high end of the voltage range employed during
the optimization trials), and all remaining sample sets were fumed under these adjusted
conditions. A summary of storage and fuming conditions for all sample sets is presented
in Appendix A (page 59).

Once all sample sets were fumed, the individual samples were examined visually
under ambient room lighting. Each sample was assigned one of four overall print quality

9, 66

ratings (“good,” “fair, poor,” or “X”) based upon the clarity and quantity of ridge detail
as previously described on pages 22 and 23. Development traits that impeded the clarity
of a print included smearing, interference due to background polymerization (often hazy,
sometimes spotty), faint polymer deposition along ridges (considered “underdeveloped”
prints), indistinct ridges (presumably from excess pressure or slight shifting of ﬁngers
while laying down prints), and spotty polymer deposition along ridges (which permitted
visualization of the general ridge pattern, but not of minutiae). The presence of these
traits often led to “fair” or “poor” ratings, but a connection was not automatic; as long as
several minutiae were visible, a print could receive a “good” rating despite having a
negative characteristic such as an area of spotty development.

Examples of the four overall quality ratings are shown in Figure 6 (following
page). Image 6A depicts a clean print from Participant #12 assigned a rating of “good.”
Note that the print appears as a reverse image of darker ridges against a white haze of
background polymerization. Image 63 depicts an oily print from Participant #6 that also

received a rating of “good.” Image 6C presents a clean print from Participant #9 assigned

a rating of “fair.” Although the top of the print is not well developed, the bottom of the

32

print is clear enough to visualize some minutiae. Image 6D depicts a clean print from
Participant #17 assigned a rating of “poor.” Only a few short ridges developed distinctly,
and no Level 2 ridge detail is visible. Image 6E presents an oily print from Participant #1
that also received a rating of “poor” because of the widespread discontinuities along the
ridges. While Level 1 ridge detail (general print pattern) was visible, the numerous
discontinuities prevented any Level 2 ridge detail from being seen. Image 6F shows an
oily print deposited by Participant #18 that was assigned a rating of “X” because no
development was visible after fuming. All prints in Figure 6 had been stored for 2 days

under simulated sunlight prior to cyanoacrylate fuming with acetic acid treatment.

 

.r, . ., ﬁ..\ 1",
Figure 6: Examples of the Four Overall Print Quality Ratings —
“good” (A & B), “fair” (C), “poor" (D & E), and “X” (F)
(Images in this thesis are presented in color.)

33

In addition to the print quality rating, each print was assigned a rating based on
the relative amounts of background polymerization using the following scale: “none,”

’9 66

“low, medium,” or “high.” Examples of prints categorized as one of the four
background polymerization ratings are shown in Figure 7. Image 7A depicts a clean print
from Participant #11 fumed with acetic acid treatment, and assigned a rating of “none.”
Image 78 depicts an oily print from Participant #14 fumed without exposure to acetic
acid, and assigned a rating of “low.” Image 7C depicts a clean print from Participant #22
fumed with acetic acid treatment, and assigned a rating of “medium.” Image 7D depicts
a clean print from Participant #3 fumed without exposure to acetic acid, and assigned a

rating of “high.” All prints in Figure 7 were stored for 2 days under ﬂuorescent lighting

prior to cyanoacrylate fuming.

 

Figure 7: Examples of the Four Background Polymerization Ratings —
“none” (A), “low” (B), “medium” (C), and “high” (D)
(Images in this thesis are presented in color.)

In addition to the print clarity and background polymerization ratings,

34

descriptions of the print appearance were recorded. The ratings were then analyzed to
determine what inﬂuence, if any, each of the main experimental design parameters had
on successful print development. These parameters included print type, lighting

condition, aging time, and (most notably) treatment option.

General Print Type Eﬁ‘ects

A combined 63% (199 + 116 = 315 out of 500) of all samples developed with
“good” or “fair” overall print quality. Although quality rating percentages were not
presented in the report of the previous children’s print study [22], discussions with the
authors of that report indicated that this present study’s “success rate” was substantially
improved over that of the previous study where the children’s prints had been fumed at
low relative humidity levels. When the samples were divided according to print type
(Table 3), no statistically signiﬁcant difference was found between clean and oily prints
in any of the four quality ratings. The statistical test used on this data, and all subsequent

data presented in this thesis, was the test of differences between proportions. A detailed

explanation of this test can be found in Appendix B.

Table 3: Overall Print Quality Ratings According to Print Type (All

 

 

 

 

 

 

Samples)
500 250 250
Total Clean Oily
Samples Samples Samples
= >‘ m good 199 (39.8%) 95 (38.0%) 104 (41.6%)
gg é” fair 116 (23.2%) 58 (23.2%) 58 (23.2%)
5 5, a“ poor 174 (34.8%) 91 (36.4%) 83 (33.2%)
X 11 (2.2%) 6 (2.4%) 5 (2.0%)

 

 

 

 

 

 

35

This result was unexpected. In past research on the acetic acid regeneration
method, higher quality prints developed from oily deposits than from eccrine-only
deposits [6,22]. One possible explanation for the deviation from this general trend relates
to an unforeseen difﬁculty encountered during print collection. Although care was taken
to standardize the print collection procedure as much as possible, researchers were not
able to control all variables at the pre-school collection site. Notably, the print collection
procedure was initiated after two participants had recently washed their hands. It was
unknown whether or not the children had collected any oily residue through touch in the
interim between their personal hand-washing and their participation in the print collection
procedure. Therefore, the “before hand-washing” prints of these participants may or may
not have contained oily components. Indeed, when the data was sorted according to
participant, the “oily” prints of the two participants in question were assigned lower
ratings than similarly labeled prints of other participants. The potential for skewed data
exists if the same phenomena unknowingly occurred with additional participants.

A second explanation for the unexpected equivalency of oily and clean print
quality ratings is that the beneﬁts associated with fuming at high humidity may balance
out the inherent differences between print types. In reviewing previous cyanoacrylate
print development studies, it was discovered that the only studies that speciﬁcally
mentioned using clean adult test prints or children’s prints [6,22] did not control the
humidity levels during cyanoacrylate fuming. Without a study of clean adult prints
and/or children’s prints fumed at high humidity to which the present study’s results can
be compared, it is unknown whether the observed similarity between clean and oily print

quality ratings is due to high humidity alone, or the combination of high humidity and

36

acetic acid treatment.

Table 4: Background Polymerization Ratings According to Print Type

 

 

 

 

 

 

 

 

(All Samples)
500 250 250
Total Clean Oily
Samples Samples Samples
,5 m none 204 (40.8%) 77 (30.8%) 127 (50.8%)
3., g g“ low 165 (33.0%) 100 (40.0%) 65 (26.0%)
mgg medium 71 (14.2%) 43 (17.2%) 28 (11.2%)
m high 60 (12.0%) 30 (12.0%) 30 (12.0%)

 

 

When the background polymerization ratings were totaled (Table 4, above),
73.8% of all samples (204 + 165 = 369 out of 500) showed little or no polymerization on
the glass background material. When the data were separated into two groups based on
print type, statistically signiﬁcant differences were found for both the “none” and the
“low” ratings between the proportion of clean prints and the proportion of oily prints
receiving each rating. However, because “low” levels of background polymerization
rarely impinged on the more crucial evaluation of overall print quality, a consideration of
greater relevance may be the combined total of the “low” and “none” ratings. When
combined, the resulting proportions for clean and oily prints (70.8% and 76.8%,
respectively) were not found to be signiﬁcantly different.

Print type is essentially a description of print composition. The composition of
the print was not expected to have any direct bearing on the degree of polymerization of
the background material, which was reﬂected in the similarity of the combined values for
the “low” and “none” ratings. However, print type/composition was seen to have a direct

effect on fuming time. Namely, oily depositions generally required a shorter amount of

37

time to produce visible prints than their clean counterparts. The shorter exposure times to
cyanoacrylate fumes of oily print samples account for the greater number of oily prints

garnering a rating of “none” as compared to clean print samples.

General Lighting Condition Eﬁ‘ects

Of the 500 total samples, 20 were fumed without storage (Sample Set #1) and the
remaining samples were distributed evenly among the following three lighting
conditions: dark storage, ﬂuorescent lighting, and simulated sunlight. However, because
samples from the three different lighting conditions were not always fumed at the same
time (see the explanation on page 21), a comparison of the results from all 160 samples
under each lighting condition could be misleading. To avoid misconstruing an aging
effect as a lighting condition effect, only the samples fumed at aging durations common
to all three lighting conditions (2, 3, 4, 5, and 7 days) were considered for analysis.
When this restriction was imposed, no signiﬁcant difference was found among any of the

lighting conditions with respect to the overall print quality distribution (Table 5).

Table 5: Overall Print Quality Ratings According to Lighting Conditions (Samples
Aged 2 to 7 Days)

300 100 100 100
Total Samples Dark Samples Fluor. Samples Sunlight" Sample
aged 2-7 days aged 2-7 days aged 2-7 days aged 2-7 days
good 113 (37.7%) 37 (37.0%) 38 (38.0%) 38 (38.0%)
fair 65 (21.7%) 21 (21.0%) 20 (20.0%) 24 (24.0%)
poor 1 16 (38.7%) 40 (40.0%) 40 (40.0%) 36 (36.0%)
X 6 (2.0%) 2 (2.0%) 2 (2.0%) 2 (2.0%)

 

 

 

 

 

 

Overall
Quality
Ratrngs

 

 

 

 

 

 

 

 

 

 

38

The similarity in rating percentages of samples subjected to ﬂuorescent lighting
and simulated sunlight is not surprising. Although marketed as two very different
lighting conditions, the bulbs used in this study emitted light with similar spectral
distributions. However, the lack of signiﬁcant difference between the samples stored in
the dark with those stored under either form of illumination is of interest. Such results
seem to contradict the expectation that prints stored in the dark, and therefore not subject
to photodegradation of the main polymerization initiator (lactate) found in ﬁngerprint
depositions, would yield developed prints of higher quality. This indicates that either the
lactate photodegradation was not substantial enough to become a major factor within the
seven days that samples were subjected to continuous illumination, or that the fuming
conditions employed in this study were able to compensate for any detrimental lactate
photodegradation that did occur.

When background polymerization was considered in relation to lighting
conditions for the restricted sample groups (Table 6), no signiﬁcant differences were
found among the three lighting conditions. Like overall print quality, background
polymerization levels were not found to be linked to variation in the lighting conditions

used in this study.

Table 6: Background Polymerization Ratings According to Lighting Conditions
(Samples Aged 2 to 7 Days)

300 100 100 100
Total Samples Dark Samples Fluor. Samples 'Sunlight" Sample
aged 2-7 days aged 2-7 days aged 2-7 days aged 2-7 days
none 149 (49.7%) 51 (51.0%) 49 (49.0%) 49 (49.0%)

 

 

 

 

 

 

 

 

 

si
3, g 3 low 106 (35.3%) 39 (39.0%) 32 (32.0%) 35 (35.0%)
no .55 medium 34 (11.3%) 9 (9.0%) 12 (12.0%) 13 (13.0%)
a- high 11 (3.7%) 1 (1.0%) 7 (7.0%) 3 (3.0%)

 

 

 

 

 

 

 

39

General Aging Effects

Clean and oily prints were successfully developed at high humidity both with and
without acetic acid treatment from 7-day-old samples stored under ﬂuorescent lighting
and simulated sunlight, and from 28-day-old samples stored under dark conditions.
These ages represent the oldest samples available within this study for each lighting
condition, not the aging limits for each.

Unfortunately, the design of this study did not provide large enough sample sizes
at each aging time for a nuanced analysis of the effects of aging. However, several
general trends were apparent. For instance, a cursory analysis of fuming times indicated
that, in general, the longer a print was aged prior to fuming, the longer the fuming time
necessary to produce a visible print. Also, longer aging times generally yielded fewer
prints that were assigned a “good” quality rating, but this decrease did not follow a
smooth drop-off curve. Background polymerization results appeared to be independent
of aging, because the ratings distributions followed no general trend over time, but were

rather erratic.

General Treatment Option Eﬁ‘ects

The main focus of this thesis was to assess the efﬁcacy of the acetic acid
regeneration treatment in developing children’s prints when combined with cyanoacrylate
fuming under conditions of high humidity. Therefore, an analysis of the quality of
treated versus untreated samples was paramount.

When samples were divided into groups of 250 according to treatment option

40

(Table 7), a smaller proportion of treated samples were considered “good” quality prints
than untreated samples. This difference was substantial enough to be considered
statistically signiﬁcant (whereas all differences for other rating levels were not
signiﬁcant). A close inspection of the samples indicated that the presence of acetic acid
vapors had retarded the polymer deposition along ﬁngerprint ridges, leaving many of the
treated prints with fainter deposition than the untreated prints. Sometimes ridge detail
was still clear enough and in enough abundance to warrant a “good” rating. But often a

faint print was classiﬁed as “fair” quality.

Table 7: Overall Print Quality Ratings According to Treatment Option

(All Samples)
500 250 250
Total Untreated Treated ‘
Samples Samples Samples

 

good 199 (39.8%) 1 12 (44.8%) 87 (34.8%)
fair 1 16 (23.2%) 51 (20.4%) 65 (26.0%)
poor 174 (34.8%) 82 (32.8%) 92 (36.8%)
X 1 1 (2.2%) 5 (2.0%) 6 (2.4%)

 

 

Overall
Quality
Ratings

 

 

 

 

 

 

 

While surveying the reasons for individual print quality classiﬁcations, it was
noted that many more treated samples than untreated samples were assigned the “fair”
rating because the ridge detail was faint. In contrast, the most common reason for
placing untreated samples into the “fair” category was the discontinuities found along the
ﬁngerprint ridges. It is possible to overcome the problem of faint print development by
any of multiple post—fuming enhancement techniques currently available. But one cannot
enhance what is not present in the ﬁrst place; namely, discontinuities cannot be

artiﬁcially connected to yield a smooth ridge. Therefore the application of post-fuming

41

enhancement techniques would very likely improve the quality ratings of treated samples
more than untreated samples. Further investigation is warranted to test this hypothesis,
since the investigation of post-fuming enhancement techniques fell outside the scope of
this study.

When assessing the background polymerization ratings in relation to treatment
option (Table 8), samples treated with acetic acid were placed into the “none” and “low”
categories 89.2% of the time. Only 58.4% of those samples not exposed to acetic acid
developed with similarly low levels of background polymerization. The difference
between these two proportions was found to be statistically signiﬁcant. Cyanoacrylate
build-up on the substrate is due to polymerization initiation by the silanol groups of glass.
When acetic acid was present, the “capping” of these silanol groups by the available H"

ions led to a polymerization reduction.

Table 8: Background Polymerization Ratings According to Treatment

 

 

 

 

 

 

 

 

 

Option (All Samples)
500 250 250
Total Untreated Treated
Samples Samples Samples
.13 w none 204 (40.8%) 73 (29.2%) 131 (52.4%)
3,, g E“ low 165 (33.0%) 73 (29.2%) 92 (36.8%)
m .3 32 medium 71 (14.2%) 50 (20.0%) 21 (8.4%)
0‘ high 60 (12.0%) 54 (21.6%) 6 (2.4%)

 

 

 

 

 

 

Detailed Treatment Option Effects
In order to gain a more detailed picture of the impact of acetic acid treatment, the

groups of samples were subdivided according to additional experimental parameters.

42

Tables 9 and 10 on the following page display the results when all 500 samples were
divided into four groups based on treatment option and print type. The differences
between groups were subjected to statistical analysis (making use of the Bonferroni
correction for multiple signiﬁcance tests performed on the same data set, as explained in
Appendix B). In terms of overall print quality (Table 9, following page), the only
difference of signiﬁcance was between the number of oily untreated prints and oily
treated prints receiving a “good” rating.

When background polymerization was considered (Table 10, following page),
both clean treated samples and oily treated samples had signiﬁcantly greater numbers of
prints with assigned ratings of “none” and “low” than their untreated counterparts, a
difference that was more pronounced in the case of oily prints. When the comparison
was made between clean treated prints and oily treated prints, the clean treated prints had
a signiﬁcantly lower proportion receiving a designation of “none” but a signiﬁcantly
higher proportion receiving a rating of “low” than the oily treated prints. These
variations offset one another, for when the “none” and “low” ratings were combined, the
resulting difference between clean treated and oily treated prints was not found to be
signiﬁcant. Though the same general trend marked the comparison of clean untreated
prints with oily untreated prints, the differences were statistically insigniﬁcant.

In summary, acetic acid treatment signiﬁcantly reduced the number of oily

prints receiving a “good” print quality rating. In terms of background polymerization,
acetic acid treatment was found to have a signiﬁcant effect on limiting background build-

up, particularly with oily prints.

43

 

 

 

 

 

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The results for the grouping of the 300 samples in the restricted sample set (those
prints fumed after 2 to 7 days of aging) according to treatment option gig lighting
condition are displayed in Tables 11 and 12 (following page). While ﬂuorescent and
simulated sunlight provided similar print quality results when treatment option was not
taken into account (see Table 5, page 38), separating the samples by acetic acid treatment
(Table 11, following page) revealed a difference between the two lighting conditions.
Exposure to acetic acid halved the number of prints stored under ﬂuorescent light that
were assigned a “good” quality rating, which was determined to be a difference of
signiﬁcance. However, acetic acid treatment only slightly diminished the proportion of
“good” prints that had been stored under the simulated sunlight, a difference that was
found to be statistically insigniﬁcant. Statistical analysis of all other relevant
comparisons among the six groups yielded no signiﬁcance to any differences in the
proportions of prints receiving various quality assessments.

In general, the use of the acetic acid treatment resulted in greater numbers of
prints developing with little or no background polymerization (Table 12, following page)
for all three lighting types. This was the expected result, due to the capping of the glass
substrate’s polymerization-initiating silanol groups by the available H” ions. Of note is
that this difference was validated as signiﬁcant by statistical analysis in the cases of the
fluorescent lighting and simulated sunlight, but was not found to be signiﬁcant in the case
of dark storage. This situation serves to highlight the fact that the use of the Bonferroni
correction, while necessary, results in the reduced likelihood that a particular perceived
difference will be labeled as signiﬁcant. However, it must be stressed that failure to be

designated a “signiﬁcant” difference does not preclude the possibility that the parameter

45

 

 

 

 

 

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46

in question may yet have an effect on the results. In cases where the calculated z-value is
just slightly less than the critical z-value, additional testing of just that parameter is
warranted. (By limiting the parameters under consideration to only one, the number of
signiﬁcance tests drops to one test, which can be performed without consideration of the

Bonferroni correction.)

Sample Pair Comparisons

Whereas the previous analyses were based on the aggregate ratings for 500
individual samples (or, when lighting conditions were being analyzed, 300 individual
samples), a second type of analysis was based upon direct comparisons of the 250
available sample pairs. Depositions collected under the same conditions (either before or
after hand-washing) from corresponding ﬁngers of the left and right hands of a study
participant were considered “sample pairs.” Both samples in a pair were stored together
under the same lighting conditions for the same length of time. The left-hand sample was
then fumed without acetic acid treatment, while the right-hand sample was fumed with
the acetic acid regeneration treatment. Assuming that the depositions from opposite
hands were equivalent, the samples in a pair could be compared with each other to
directly elucidate the effect of acetic acid treatment. In the following tables, information
is presented in relation to the treated samples. That is, the term “better” indicates the
treated sample had a more desirable rating than the untreated sample; the term “same”
indicates that the ratings of both samples in the pairing were equal; the term “worse”

indicates the treated sample had a less desirable rating than the untreated sample.

47

Results of the comparison of overall print quality between treated and untreated
prints are presented in Table 13. The majority of all comparisons (129 out of 250, or
51.6%) demonstrated no change in the overall print quality rating due to acetic acid
treatment. An improved quality rating due to acetic acid treatment was apparent in
18.8% of the comparisons (47 out of 250), while closer to one-third of the comparisons

(74 out of 250, or 29.6%) depicted a deterioration in the print quality when exposed to

acetic acid.

Table 13: Comparisons of the Effect of Acetic Acid Regeneration
Treatment on Print Quality (All Sample Pairs)

250
Total
Comparisons
'73 E? o;- better 47 (18.8%)
4:5 E 7'; same 129 (51.6%)
0 0’ worse 74 (29.6%)

 

 

 

 

 

 

A more favorable link was found between acetic acid treatment and background
polymerization levels (Table 14, following page). Of the 250 comparisons, acetic acid
exposure was shown to improve the background development in half of the sample pairs.
Background development was unaffected by the acetic acid treatment in an additional
40.0% of the sample pairs, leaving only 25 comparisons (10.0%) in which the acetic acid

treatment led to a worse background polymerization rating.

48

Table 14: Comparisons of the Effect of Acetic Acid Regeneration
Treatment on Background Polymerization (All Sample Pairs)

250
Total
Comparisons
better 125 (50.0%)
same 100 (40.0%)
worse 25 (10.0%)

 

 

 

Bkgd
Polymer
lzatron

 

 

 

When the comparisons were separated by print type (Table 15), acetic acid
exposure was linked to an improvement in print quality in 25.6% (32 out of 125
comparisons) of the clean samples, a proportion more than twice as large as the
improvement for oily samples (12.0%, or 15 out of 125 comparisons). The difference
between the proportions of clean and oily samples that responded unfavorably to the
acetic was not signiﬁcant. While most of the comparisons, regardless of print type,
reﬂected no change in print quality due to acetic acid treatment, the treatment was found

to be more beneﬁcial for clean samples than oily samples.

Table 15: Comparisons of the Effect of Acetic Acid Regeneration
Treatment on Print Quality According to Print Type (All Sample Pairs)

250 125 125
Total Clean Oily
Comparisons Comparisons Comparisons

 

 

better 47 (18.8%) 32 (25.6%) 15 (12.0%)
same 129 (51.6%) 61 (48.8%) 68 (54.4%)
worse 74 (29.6%) 32 (25.6%) 42 (33.6%)

 

 

Overall
Print
Quality

 

 

 

 

 

 

 

 

 

When background polymerization was under consideration (Table 16, following

page), clean and oily prints responded similarly to acetic acid exposure, with half of the

49

comparisons showing an improvement in cyanoacrylate build-up (i.e. lower background
polymerization level) on the glass background. Only approximately 10% of the cases for
both print types showed higher background polymerization levels in the treated sample in
a sample pair. Thus, acetic acid was shown to be equally effective at reducing the

background polymerization of both print compositions.

Table 16: Comparisons of the Effect of Acetic Acid Regeneration
Treatment on Background Polymerization According to Print Type

 

 

 

 

 

 

 

 

 

 

 

(All Sample Pairs)
250 125 125
Total Clean Oily
Comparisons Comparisons Comparisons
_D a“) r: better 125 (50.0%) 62 (49.6%) 63 (50.4%)
Egg same 100 (40.0%) 47 (37.6%) 53 (42.4%)
m o? 9 worse 25 (10.0%) 16 (12.8%) 9 (7.2%)

 

 

To analyze the effect of the acetic acid treatment relative to lighting condition
(Table 17, following page), the number of comparisons was restricted to 150
(representing the 150 sample pairs, or 300 total samples, that were fumed after aging
times common to all three lighting options). Within this subset, maintaining the same
level of print quality regardless of treatment occurred in a substantially larger percentage
of sample pairs under ﬂuorescent lighting (52.0%) and simulated sunlight (54.0%) than
sample pairs kept in dark storage (28.0%). The differences among lighting options in the
proportions of sample pairs yielding better print quality or worse print quality were

statistically non-signiﬁcant.

50

Table 17: Comparisons of the Effect of Acetic Acid Regeneration Treatment on Print

Quality According to Lighting Condition (Sample Pairs Aged 2 to 7 Days)

 

 

 

 

 

 

 

 

 

 

 

150 50 50 50
Total Dark Fluor. "Sunlight"
Comparisons Comparisons Comparisons Comparisons
a E g better 30 (20.0%) 13 (26.0%) 6 (12.0%) 11 (22.0%)
§°E '75? same 67 (44.7%) 14 (28.0%) 26 (52.0%) 27 (54.0%)
0 0’ worse 53 (35.3%) 23 (46.0%) 18 (36.0%) 12 (24.0%)

 

 

 

In terms of background polymerization (Table 18), similar responses were found

across all three lighting conditions, with any differences among lighting options being

ruled statistically insigniﬁcant. Thus, acetic acid treatment is effective in relation to

background polymerization ratings regardless of lighting conditions.

Table 18: Comparisons of the Effect of Acetic Acid Regeneration Treatment on Print

Quality and Background Polymerization According to Lighting Condition

 

 

 

 

 

 

 

 

 

 

 

150 50 50 50
Total Dark Fluor. "Sunlight"
Comparisons Comparisons Comparisons Comparisons
.6 g 8 better 63 (42.0%) 20 (40.0%) 24 (48.0%) 19 (38.0%)
54° 2;. '«3 same 69 (46.0%) 22 (44.0%) 21 (42.0%) 26 (52.0%)
m o? -5 worse 18 (12.0%) 8 (16.0%) 5 (10.0%) 5 (10.0%)

 

 

51

 

Chapter 4

CONCLUSION

The results of a study of the efﬁcacy of acetic acid as a regeneration agent for
children’s prints, when coupled with cyanoacrylate fuming at high humidity, have been
presented. A regeneration treatment protocol was modiﬁed and optimized into a one-step
fuming process utilizing a 2:1 w/w cyanoacrylate ester: acetic acid mixture. The process
was applied to 500 individual samples from 25 pre-pubescent children after given periods
of storage in one of three lighting conditions: dark storage, ﬂuorescent lighting, and
simulated sunlight. After development, each print was classiﬁed by background
polymerization and overall print quality.

In direct comparisons of treated and untreated samples, the acetic acid treatment
was found to substantially improve the background polymerization of a sample to low or
unnoticeable levels. Exactly 50.0% of the samples receiving the acetic acid treatment
were classiﬁed with lower background polymerization than their untreated counterparts;
only 10.0% of treated samples were classiﬁed with higher background polymerization.
The two print types were affected similarly by the treatment. Likewise, the three lighting
conditions responded similarly to acetic acid exposure. However, moving away from
direct comparisons of sample pairs and shifting focus to totals of each of the four
background levels, there were some signiﬁcant differences. Substantially more oily

prints developed with “none” or “low” background ratings than clean prints. Treatment

52

was linked with a larger increase in the number of prints given the “none” or “low”
ratings from those stored in ﬂuorescent and simulated sunlight than those stored in the
dark.

Background polymerization can interfere with and even obscure ridge details, so
it plays a role in print quality (a more important consideration for print examiners than
background cyanoacrylate build—up). However, a reduction of background
polymerization is not always synonymous with an improvement in overall print quality.
Additionally, prints with elevated levels of background build-up can still be considered
prints of good quality if the background is not localized to print furrows, or if the ridge
development is well-deﬁned to compensate for any background interference.

Based on direct comparisons of sample pairs, 18.8% of the treated samples had
improved quality ratings over the untreated sample in the pair. An additional 51.6% of
the samples had quality ratings that remained unchanged by exposure to acetic acid,
leaving a sizeable 29.6% of the cases with worse quality ratings after treatment. The
treatment was signiﬁcantly more effective at improving quality in clean samples than in
oily samples. When lighting option was analyzed, signiﬁcantly more samples under
ﬂuorescent light and simulated sunlight maintained the same quality rating than samples
stored in the dark. Analyzing the data in terms of the totals of each of the four speciﬁc
quality levels, oily prints and prints subjected to ﬂuorescent lighting were found to have
signiﬁcantly higher quality ratings without the acetic acid treatment, but the remaining
print type and lighting conditions were not signiﬁcantly affected by the treatment.

The results of this study are promising. With reﬁnement, and in combination with

post-fuming enhancement techniques, the acetic acid technique may be capable of

53

producing consistent improvement in the quality of samples fumed at high humidity.

54

 

 

APPENDICES

55

APPENDD( A

Participant Information & Sample Set Storage and Fuming Plans

56

 

Table 19: Gender and Age of Each Participant
PARTICIPANT
NUMBER GENDER AGE

 

 

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57

was; Emu co 088 38058 a smack: L: 652 £2 05 mo Swan 2:: smack: 98:5 05 282%.. :o: smacks“ :5: 6:6 .1. .20..

9“...

m; .6 m9. .6 :5 .6 N; .6 as .6 4;. .6 84 .6 6. .6 2.. .6 4% .6 855 s .55... mm
4;. .6 m8 .6 :4 .6 Q .6 4% .6 o; .6 NS. .6 o; .6 m4 .6 :4 .6 855 m .55.. 2
8... .6 5;. .6 m5 .6 :4 .6 5;. .6 5;. .6 5;. .6 Q .6 5% .6 54 .6 853. .59. 2
5;, .6 25 .6 Q. .6 5% .6 M5 .6 5;. .6 m... .6 E .6 55 .6 8.. .6 855 m .55.. 2
m6 .6 :6 .6 e4 .6 E .6 w; .6 :5 .6 N; .6 54 .6 m; .6 85 .6 853 .59. 2
a; .6 54 .6 m; .6 24 .6 :4 .6 a... .6 4% .6 4;. .6 8... .6 5.. .6 a; M: .55.. 5
a. .6 4% .6 3.... .6 85 .6 E... .6 m4 .6 :4 .6 5:5 .6 mg. .6 5;. .6 a; m .55.. m
6 .6 5;. .6 mg. .6 o; .6 m4 .6 5% .6 M5 .6 a; .6 m; .6 Na .6 a; 2 .55.. m
56 .6 S... .6 e; .6 m5 .6 E. .6 ma .6 5;. .6 5;. .6 N5 .6 59.. .6 8.55 5 .56 a
we. .6 5;. .6 m; .6 Na .6 5% .6 8.. .6 5;. .6 we .6 6 .6 on .6 855 n 56 M:
5;. .6 3 .6 E .6 on .6 E .6 no... .6 :4 .6 N; .6 9.. .6 m; .6 8554 .56 2
:4 .6 NE .6 as. .6 m; .6 8.... .6 55 .6 S .6 4% .6 4;. .6 5% .6 8.55 m 56 E
55 .6 Q. .6 4% .6 4;. .6 85 .6 5; .6 m... .6 :5 .6 5;. .6 N9... .6 855 N 56 5
me. .6 E. .6 5;. .6 Se .6 5;. .6 ms. .6 5% .6 5.... .6 5;. .6 m3. .6 a; M: .56 5
N6 .6 5% .6 M5 .6 5;. .6 m; .6 z. .6 54 .6 a... .6 5;. .6 ms. .6 a: m .56 v
on .6 s5 .6 5;. .6 Q .6 E .6 54.6 24 .6 was. .6 :4 .6 E. .6 a: 2 .56 N
8 .6 5;. .6 Q .6 E .6 es. .6 m; .6 35 .6 E... .6 NE .6 a... .6 8.55 mm 6:5 mm
3.. .6 :5 .6 N3. .6 a... .6 25 .6 85 .6 :4 .6 a. .6 4% .6 4;. .6 855 _N 6:6 4m
8... .6 55 .6 3. .6 4% .6 4;. .6 85 .6 5;. .6 ma .6 :5 .6 5;. .6 £5 E 6:3 mm
5;. .6 ms. .6 :4 .6 5;. .6 mg. .6 m; .6 N4 .6 5% .6 54 .6 5;. .6 8.55 5 6:6 om
5;. .6 N4 .6 5% .6 54 .6 5;. .6 Q .6 :6 .6 on .6 E. .6 5;. .6 855 m 6:3 t
g. .6 54 .6 8.. .6 w; .6 we .6 m; .6 55 .6 m; .6 mg. .6 :5 .6 8554 56 E
54 .6 m; .6 mg. .6 :4 .6 NE .6 5% .6 4; .6 85 .6 E... .6 to. .6 8.55 m 56 :
4% .6 4;. .6 85 .6 as. .6 a. .6 :4 .6 5;. .6 8... .6 e; .6 me .6 8.53 6:8 w
58 .6 we. .6 5;. .6 my... .6 N4 .6 on .6 s... .6 5;. .6 m4 .6 z. .6 252 252 _
. _5 a .o 5 5 5 . .
_ 55653556559551:0 _ 556536555525 266 _ mama.
- 855586 26 mm :55 555% 55m 6 6 5865 5m 635.5

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

   

  

 
 
 

 

 

 

 

 

 

 

58

Table 21: Storage and Fuming Conditions for Each Sample Set

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Storage Conditions. Fumingﬁonditions
q, 00 a 9 9‘ .§ § ‘5 o o c: v a) O
5.5 .5 5.5:5§5§5§5§5.g52a
a5 : 'a‘oegoE-—-~='Ev&o&'a.9~‘t:m
5”§<55%§§52§£2£a£5§
> a {I} :1: m E—
1 None None 85 2 10 Coming under 150
2 Fluor. l 5 hrs 70 2 10 Coming under 150
3 "Sun" 1 5 hrs 70 2 10 Coming under 150
4 Fluor. 3 hrs 70 2 10 Coming under 150
5 "Sun" 3 hrs 70 2 10 Coming under 150
6 Fluor. 18 hrs 70 2 10 Coming under 150
7 "Sun" 18 hrs 70 2 10 Coming under 150
8 Dark 2 days 75 2 10 [Cole-Pal. level 150
9 Fluor. 2 days 75 2 10 [Cole-Pal. level 150
10 "Sun" 2 days 75 2 10 ICole-Pal level 150
11 Dark 3 days 75 2 10 [Cole-Pal. level 150
12 Fluor. 3 days 75 2 10 ICole-Pal. level 150
13 "Sun" 3 days 75 2 10 [Cole-Pal. level 150
14 Dark 4 days 75 2 10 [Cole-Pal. level 150
15 Fluor. 4 days 75 2 10 [Cole-Pal level 150
16 "Sun" 4 days 75 2 10 [Cole-Pal. level 150
17 Dark 5 days 75 2 10 [Cole-Pal level 150
18 Fluor. 5 days 75 2 10 [Cole-Pal. level 150
19 "Sun" 5 days 75 2 10 [Cole-Pal. level 150
20 Dark 7 days 75 2 10 [Cole-Pal. level 150
21 Fluor. 7 days 75 2 10 [Cole-Pal. level 150
22 "Sun" 7 days 75 2 10 [Cole-Pal. level 150
23 Dark 14 days 75 2 10 [Cole-Pal. level 150
24 Dark 21 days 75 2 10 [Cole-Pal. level 150
25 Dark 28 days 75 2 10 [Cole-Pal. level 150

 

 

where “under” means the hotplate was positioned underneath the fuming Chamber’s
metal platform, and “level” means the hotplate was raised so it was level with the bottom
of the fuming chamber

59

APPENDIX B

Statistical Analysis

60

To determine if the differences in ratings between two categories of prints (for
example, clean prints versus oily prints) were of relevance, the test of differences
between proportions was performed for each rating level. For each test, the null
hypothesis, that the two proportions under consideration are equal, is written Ho: p1 = p2.
The alternate hypothesis, that the two proportions are not equal, is written H]: p; at p2.

The computations involved are:

= P1+P2
p 2
= 2120-13)
Spl-Pz n
P1‘P2
zcalc :—
SPl-Pz

where n is the sample size (or total number of prints) in a given category, p. is the
proportion of n with the given rating level in the ﬁrst category, p2 is the proportion of n

with the given rating level in the second category, and Spl-pz is the estimated standard

error of the difference between proportions. Slightly more complicated equations would
have been necessary if the two categories under comparison contained different sample
sizes (n1 and n2). No such incident occurred in the analysis of the data used in this study.

Once ZCALC is determined, it is compared with the appropriate critical value, zcm,
from the z-table. If ZCALC is less than 2cm, the null hypothesis is accepted and no
statistical signiﬁcance is found. If ZCALC is less than 2cm, the null hypothesis is rejected
and the difference between the two proportions is said to be statistically signiﬁcant. In
the analyses presented in this appendix:

(1 =- 0.05 (a conﬁdence interval of 95%)

61

2cm, 0.05 = 1-96

However, if multiple statistical tests are performed on a data set, the Bonferroni

correction must be used. According to this correction, multiple tests increase the

likelihood beyond 5% that a chance occurrence will be incorrectly interpreted as a

signiﬁcant correlation. To reset the 5% limit, a for each test must be adjusted downward.

The new value, 013, is related to the number of signiﬁcance tests, k, as follows:

(13 = a/k = 0.05/k

In the tables presented in this appendix, statistical analysis is summarized for the

data presented in Table 3 through Table 12 and Table 15 through Table 18 in the main

text of this thesis. Below each table, the values for n, k, and 013 are presented.

Table 22: Statistical Analysis of Table 3 (Overall Print Quality Ratings According to
Print Type - All Samples)

2mm Ldlfference

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level p1 p2 p sp,_p2 zCALC igniﬁcant‘l
good 0.380 0.416 0.398 0.044 0.822 1.96 no
5 w 2.» ,0 fair 0.232 0.232 0.232 0.038 0.000 1.96 no
5 £5 lg, poor 0.364 0.332 0.348 0.043 0.751 1.96 no
.. g I; g x 0.024 0.020 0.022 0.013 0.305 1.96 no
5‘” “m (good+fair) 0.612 0.648 0.630 0.043 0.834 1.96 no
(poor-I-X) 0.388 0.352 0.370 0.043 0.834 1.96 no
n=500
k=l

a3 = a/k = 0.05/1 = 0.05

62

Table 23: Statistical Analysis of Table 4 (Background Polymerization Ratings According
to Print Type - All Samples)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level P1 P2 P Spl-pz anrc zc11rr0.05 Ldlfferenced
lgnlflcant.
none 0.308 0.508 0.408 0.044 4.550 1.96 yes
5 a, .2» a, low 0.400 0.260 0.330 0.042 3.329 1.96 yes
5 645 ‘3’, medium 0.172 0.112 0.142 0.031 1.922 1.96 no
.. gt § hi h 0.120 0.120 0.120 0.029 0.000 1.96 no
63‘” ‘3‘” (none+1ow)I 0.708 0.768 0.738 0.039 1.526 1.96 no
(med.+high)| 0.292 0.232 0.262 0.039 1.526] 1.96 | no ]

 

a3 = a/k = 0.05/l = 0.05

Table 24: Statistical Analysis of Table 5 (Overall Print Quality Ratings According to

Lighting Conditions - Sam

ples Aged 2 to 7 Days)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level P1 P2 P Spl-p2 ZCALC ZCRrr.0.Ol7 lelfference
lgnlflcant‘l
good 0.370 0.380 0.375 0.068 0.146 2.39 no
1‘5 ,0 5 m fair 0.210 0.200 0.205 0.057 0.175 2.39 no
3 £5 7‘; poor 0.400 0.400 0.400 0.069 0.000 2.39 no
u g .. §= x 0.020 0.020 0.020 0.020 0.000 2.39 no
5"” a?” (good+fair) 0.580 0.580 0.580 0.070 0.000 2.39 no
(poor+X) 0.420 0.420 0.420 0.070 0.000 2.39 no
good 0.370 0.380 0.375 0.068 0.146 2.39 no
.2 m 3: m fair 0.210 0.240 0.225 0.059 0.508 2.39 no
3 6.6 42, poor 0.400 0.360 0.380 0.069 0.583 2.39 no
u g]. g x 0.020 0.020 0.020 0.020 0.000 2.39 no
5“” a.” (good+fair) 0.580 0.620 0.600 0.069 0.577— 2.39 no
(poor+X) 0.420 0.380 0.400 0.069 0.577 2.39 no
good 0.380 0.380 0.380 0.069 0.000 2.39 no
5 m a: ,0 fair 0.200 0.240 0.220 0.059 0.683 2.39 no
6 43;; 53,—, poor 0.400 0.360 0.380 0.069 0.583 2.39 no
.. g1. E x 0.020 0.020 0.020 0.020 0.000 2.39 no
:51” 51'” (good+fair) 0.580 0.620 0.600 0.069 0.577 2.39 no
(poor+X) 0.420 0.380 0.400 0.069 0.577 2.39 no
n=300
k=3

as = a/k = 0.05/3 = 0.017

63

Table 25: Statistical Analysis of Table 6 (Background Polymerization Ratings According
to Lighting Conditions — Samples Aged 2 to 7 Days

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating LCVCI P1 P2 P Spl-pz ZCALC chrr.0.017 dlfference
Slgnlflcant?
none 0.510 0.490 0.500 0.071 0.283 2.39 no
as w 5- ” low 0.390 0.320 0.355 0.068 1.034 2.39 no
5 £5 2 medium 0.090 0.120 0.105 0.043 0.692 2.39 no
u g” g high 0.010 0.070 0.040 0.028 2.165 2.39 no
9‘” é?“ (none+low) 0.900 0.810 0.855 0.050 1.807 2.39 no
(med.+high) 0.100 0.190 0.145 0.050 1.807 2.39 no
none 0.510 0.490 0.500 0.071 0.283 2.39 no
i (0:: w low 0.390 0.350 0.370 0.068 0.586 2.39 no
g 65% fat medium 0.090 0.130 0.110 0.044 0.904 2.39 no
u g]. g high 0.010 0.030 0.020 0.020 1.010 2.39 no
a” a" (none+low) 0.900 0.840 0.870 0.048 1.262 2.39 no
(med.+high) 0.100 0.160 0.130 0.048 1.262 2.39 no
none 0.490 0.490 0.490 0.071 0.000 2.39 no
.5 (0:: w low 0.320 0.350 0.335 0.067 0.449 2.39 no
52552 medium 0.120 0.130 0.125 0.047 0.214 2.39 no
.. 61]. 6] high 0.070 0.030 0.050 0.031 1.298 2.39 no
a” 3‘“ (none+low) 0.810 0.840 0.825 0.054 0.558 2.39 no
(med.+high) 0.190 0.160 0.175 0.054 0.558 2.39 no
n=300
k=3

(:3 = a/k = 0.05/3 = 0.017

Table 26: Statistical Analysis of Table 7 (Overall Print Quality Ratings According to

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Treatment Option - All Samples)
Rating Level P1 P2 P spl-pZ ZCALC lemons :‘lﬁeggﬁfq
1, good 0.448 0.348 0.398 0.044 2.284 1.96 yes
L; m :3 m fair 0.204 0.260 0.232 0.038 1.483 1.96 no
.93 in: § 2 poor 0.328 0.368 0.348 0.043 0.939 1.96 no
6 E: g x 0.020 0.024 0.022 0.013 0.305 1.96 no
:‘im a“ (good+fair) 0.652 0.608 0.630 0.043 1.019 1.96 no
(poor+X) 0.348 0.392 0.370 0.043 1.019 1.96 no
n =500
k=l

013 = a/k = 0.05/l = 0.05

Table 27: Statistical Analysis of Table 8 (Background Polymerization Ratings According

to Treatment Option - All Samples

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating LCVCI pl P2 P SpI-pz ZCALC ZCRIT.0.05 (.jlfferencci
Slgnlﬁcant‘?

U none 0.292 0.524 0.408 0.044 5.278 1.96 yes
:3 mg ., low 0.292 0.368 0.330 0.042 1.807 1.96 no
gas: medium 0.200 0.084 0.142 0.031 3.716 1.96 yes
:5 g: g high 0.216 0.024 0.120 0.029 6.606 1.96 yes
22"” a” (none+low) 0.584 0.892 0.738 0.039 7.831 1.96 yes

(med.+high) 0.416 0.108 0.262 0.039 7.831 1.96 yes
n=500
k=1

0.3 = a/k = 0.05/1 = 0.05

65

Table 28: Statistical Analysis of Table 9 (Overall Print Quality Ratings According to
Treatment Option and Print Type - All Samples)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level P1 P2 P Spl-pz anrc chrr,0.0125 dlfference
Slgnlflcant?

U. 3 ﬁ 5 good 0.400 0.360 0.380 0.061 0.651 2.5 no
5:; ~ g — fair 0.208 0.256 0.232 0.053 0.899 2.5 no
g g g 6 poor 0.360 0.368 0.364 0.061 0.131 2.5 no
5 2!: 2 x 0.032 0.016 0.024 0.019 0.826 2.5 no
"_2’ a2 (good+fair) 0.608 0.616 0.612 0.062 0.130 2.5 no
‘3‘” L“ (poor+X) 0.392 0.384 0.388 0.062 0.130 2.5 no
5 m - mi good 0.496 0.336 0.416 0.062 2.566 2.5 yes
g 23 2 fair 0.200 0.264 0.232 0.053 1.199 2.5 no
1.: g g §| poor 0.296 0.368 0.332 0.060 1.209 2.5 no
5 ma: if x 0.008 0.032 0.020 0.018 1.355 2.5 no
"_5 5.8 (good+fair) 0.696 0.600 0.648 0.060 1.589 2.5 no
°‘ (poor+X) 0.304 0.400 0.352 0.060 1.589 2.5 no
13. 3 U. -. good 0.400 0.496 0.448 0.063 1.526 2.5 no
:3 3% 2| fair 0.208 0.200 0.204 0.051 0.157 2.5 no
g Sg 3 poor 0.360 0.296 0.328 0.059 1.078 2.5 no
5 25 w x 0.032 0.008 0.020 0.018 1.355 2.5 no
“_2 13,-; (good+fair) 0.608 0.696 0.652 0.060 1.461 2.5 no
a” ‘3‘ (poor+X) 0.392 0.304 0.348 0.060 1.461 2.5 no
a, good 0.360 0.336 0.348 0.060 0.398 2.5 no
1333132 fair 0.256 0.264 0.260 0.055 0.144 2.5 no
1.36:3 g poor 0.368 0.368 0.368 0.061 0.000 2.5 no
ET. 2: if x 0.016 0.032 0.024 0.019 0.826 2.5 no
5% .35 (good+fair) 0.616 0.600 0.608 0.062 0.259 2.5 no
(poor+X) 0.384 0.400 0.392 0.062 0.259 2.5 no

 

 

 

 

 

 

 

 

 

 

 

 

Comparisons not of interest: p. = Untreated, Clean samples; p2 = Treated, Oily samples
p. = Treated, Clean samples; p2 = Untreated, Oily samples

as = a/k = 0.05/4 = 0.0125

66

Table 29: Statistical Analysis of Table 10 (Background Polymerization Ratings

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

According to Treatment 0 ation and Print Type - All Samples)
Rating Level P1 P2 P Spl-p2 lease lemomzsLdlfference
lgmflcant‘l
U. 3 . 3 none 0.232 0.384 0.308 0.058 2.603 2.5 yes
2 32 5 low 0.320 0.480 0.400 0.062 2.582 2.5 yes
2 Egg é medium 0.224 0.120 0.172 0.048 2.179 2.5 no
5 3:? hi h 0.224 0.016 0.120 0.041 5.060 2.5 es
"_2 a2 (none+low)I 0.552 0.864 0.708 0.058 5.425 2.5 yes
“‘0 U (med.+high)| 0.448 0.136 0.292 0.058 5.425 2.5 yes
5 w . w none I 0.352 0.664 0.508 0.063 4.934 2.5 yes
2 21,3 2 low 0.264 0.256 0.260 0.055 0.144 2.5 no
2 5 g E medium 0.176 0.048 0.112 0.040 3.209 2.5 yes
5 gt}: w hi h 0.208 0.032 0.120 0.041 4.282 2.5 es
' "_g 25 (none+low) 0.616 0.920 0.768 0.053 5.694 2.5 JCS
°‘ (med.+high)| 0.384 0.080 0.232 0.053 5.694 2.5 yes
6. 3'6 m none’ 0.232 0.352 0.292 0.058 2.086 2.5 no
2 a 2 2 low 0.320 0.264 0.292 0.058 0.974 2.5 no
2 ﬁg 2 medium 0.224 0.176 0.200 0.051 0.949 2.5 no
5 ‘25 m high 0.224 0.208 0.216 0.052 0.307 2.5 no
'L 2’ [Lg (none-How) 0.552 0.616 0.584 0.062 1.027 2.5 no
“U °‘ (med.+high) 0.448 0.384 0.416 0.062 1.027 2.5 no
a, m non? 0.384 0.664 0.524 0.063 4.432 2.5 yes
2’ £2“ 2 low 0.480 0.256 0.368 0.061 3.672 2.5 yes
.3 g 2 2 medium 0.120 0.048 0.084 0.035 2.052 2.5 no
:3: w hi h 0.016 0.032 0.024 0.019 0.826 2.5 no
532 gglmoneuow) 0.864 | 0.920| 0.892 0.039 1.426 2.5 no
|(med.+high) 0.136] 0.080] 0.108 0.039| 1.426 L 2.5 | no |

 

Comparisons not of interest: p, = Untreated, Clean samples; p2 = Treated, Oily samples
p1 = Treated, Clean samples; p2 = Untreated, Oily samples

(13 = a/k = 0.05/4 = 0.0125

67

Table 30: Statistical Analysis of Table 11 (Overall Print Quality Ratings According to
Treatment Option and Lighting Condition - Samples Aged 2 to 7 Days)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

. difference
Ratln Level 5 , z z
8 P1 P2 P pl p2 cane CRrr,0.0056 Signiﬁcant?

U. m w good 0.420 0.320 0.370 0.097 1.036 2.77 no
2 2'2 2 fair 0.160 0.260 0.210 0.081 1.228 2.77 no
2 g 2 2 poor 0.420 0.380 0.400 0.098 0.408 2.77 no
5 g 7 g x 0.000 0.040 0.020 0.028 1.429 2.77 no
"_5 3,2 (good+fair) 0.580 0.580 0.580 0.099 0.000 2.77 no
‘1 T (poor+X) 0.420 0.420 0.420 0.099 0.000 2.77 no
_O. V, .,, good 0.520 0.240 0.380 0.097 2.884 2.77 yes
2 ~33 3 fair 0.120 0.280 0.200 0.080 2.000 2.77 no
‘“ E .5 2

g “12 ., poor 0.320 0.480 0.400 0.098 1.633 2.77 no
5 f T ‘ij x 0.040 0.000 0.020 0.028 1.429 2.77 no
"_2 g§|(good+fair) 0.640 0.520 0.580 0.099 1.216 2.77 no
“‘5 L“l (poor+X) 0.360 0.480 0.420 0.099 1.216 2.77 no
. V, . ,,, good 0.400 0.360 0.380 0.097 0.412 2.77 no
2&2 2 fair 0.220 0.260 0.240 0.085 0.468 2.77 no
is §§ S poor 0.360 0.360 0.360 0.096 0.000 2.77 no
‘= i” E- l” x 0.020 0.020 0.020 0.028 0.000 2.77 no
D E: II 1:

“_5; 35; (good+fair) 0.620 0.620 0.620 0.097 0.000 2.77 no
‘3“ = (poor+X) 0.380 0.380 0.380 0.097 0.000 2.77 no
13. m U. u, good 0.420 0.520 0.470 0.100 1.002 2.77 no
.2 22 2 fair 0.160 0.120 0.140 0.069 0.576 2.77 no
2 g2 E poor 0.420 0.320 0.370 0.097 1.036 2.77 no
5 :5 ”3| x 0.000 0.040 0.020 0.028 1.429 2.77 no
”_5 ”N El<good+fair) 0.580 0.640 0.610 0.098 0.615 2.77 no
Q ‘1“ (poor+X) 0.420 0.360 0.390 0.098 0.615 2.77 no
. - w ood 0.420 0.400 0.410 0.098 0.203 2.77 no
'13 W “O Q g

2 2 2 ~ fair 0.160 0.220 0.190 0.078 0.765 2.77 no
cu 0- 6: E

g 22 .5 poor 0.420 0.360 0.390 0.098 0.615 2.77 no
5 :5 3’ x 0.000 0.020 0.010 0.020 1.005 2.77 no
”_5 1,3; (good+fair) 0.580 0.620 0.600 0.098 0.408 2.77 no
‘3“ 5“ (poor+X) 0.420 0.380 0.400 0.098 0.408 2.77 no
U. “a. a, good 0.520 0.400 0.460 0.100 1.204 2.77 no
2 432 2 fair 0.120 0.220 0.170 0.075 1.331 2.77 no
2 £2 E goor 0.320 0.360 0.340 0.095 0.422 2.77 no
5 ‘25: x 0.040 0.020 0.030 0.034 0.586 2.77 no
”_2 ”~53 (good+fair) 0.640 0.620 0.630 0.097 0.207 2.77 no
“‘1‘ C“ | (poor+X) 0.360 0.380 0.370 0.097 0.207 2.77 no

 

68

 

Table 30 (con’d)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating LCVCI P1 P2 P Spl-pz ZCALC Zc11rr,0.0056 (.hffierence

Signiﬁcant?
m U, good 0.320 0.240 0.280 0.090 0.891 2.77 no
2’ 22' 2 fair 0.260 0.280 0.270 0.089 0.225 2.77 no
2 g 2 6 poor 0.380 0.480 0.430 0.099 1.010 2.77 no
E; 2F; 5' x 0.040 0.000 0.020 0.028 1.429 2.77 no
£5 ail(good+fair) 0.580 0.520 0.550 0.099 0.603 2.77 no
(poor+X) 0.420 0.480 0.450 0.099 0.603 2.77 no
m ,,, good 0.320 0.360 0.340 0.095 0.422 2.77 no
1.3“ 213' 3 fair 0.260 0.260 0.260 0.088 0.000 2.77 no
2 gg 5 poor 0.380 0.360 0.370 0.097 0.207 2.77 no
E; 2: :l x 0.040 0.020 0.030 0.034 0.586 2.77 no
.53 35;; (good+fair) 0.580 0.620 0.600 0.098 0.408 2.77 no
‘ (poor+X) 0.420 0.380 0.400 0.098 0.408 2.77 no
m ,,, good 0.240 0.360 0.300 0.092 1.309 2.77 no
"53’ £153“ 2 fair 0.280 0.260 0.270 0.089 0.225 2.77 no
§ 53 §I poor 0.480 0.360 0.420 0.099 1.216 2.77 no
7. :33: :l x 0.000 0.020 0.010 0.020 1.005 2.77 no
,53 .35; (good+fair) 0.520 0.620 0.570 0.099 1.010 2.77 no
L“ = | (poor+X) 0.480 0.380 0.430 0.099 1.010 2.77 no

 

Comparisons not of interest: pl = Untreated, Dark samples; p2 = Treated, Fluor. samples
p. = Untreated, Dark samples; p2 = Treated, “Sun” samples
p1 = Treated, Dark samples; p2 = Untreated, Fluor. samples
p1 = Treated, Dark samples; p2 : Untreated, “Sun” samples
p1 = Untreated, Fluor samples; p2 = Treated, “Sun” samples
p1 = Treated, Fluor samples; p2 = Untreated, “Sun” samples

(13 = a/k = 0.05/9 = 0.0056

69

 

Table 31: Statistical Analysis of Table 12 (Background Polymerization Ratings

According to Treatment 0

3tion and Lighting Condition - Samples Aged 2 to 7 Days)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level P1 P2 P Spl-pZ ZCALC ZCRrr,0.0056. (.hffsrence
Signiﬁcant?
a w . m none 0.420 0.600 0.510 0.100 1.800 2.77 no
2 22 2 low 0.420 0.360 0.390 0.098 0.615 2.77 no
g 22 5 medium 0.140 0.040 0.090 0.057 1.747 2.77 no
5 3 [if ”3 high 0.020 0.000 0.010 0.020 1.005 2.77 no
"_ g 22 (none+low) 0.840 0.960 0.900 0.060 2.000 2.77 no
Q _(med.+high) 0.160 0.040 0.100 0.060 2.000 2.77 no
1:“ 8 2 8 none 0.340 0.640 0.490 0.100 3.001 2.77 yes
2 a2 3'? low 0.340 0.300 0.320 0.093 0.429 2.77 no
,9; 512 E medium 0.180 0.060 0.120 0.065 1.846 2.77 no
5 f I: ‘3 high 0.140 0.000 0.070 0.051 2.744 2.77 no
"_2 2,3 (none+low) 0.680 0.940 0.810 0.078 3.314 2.77 yes
QQ L"(med.+high) 0.320 0.060 0.190 0.078 3.314 2.77 yes
13. 3 ' 8 none 0.380 0.600 0.490 0.100 2.200 2.77 no
2 32 ~ low 0.320 0.380 0.350 0.095 0.629 2.77 no
2 E 2 6| medium 0.240 0.020 0.130 0.067 3.271 2.77 yes
5 TI: 2" high 0.060 0.000 0.030 0.034 1.759 2.77 no
"_53 avg) (none+low) 0.700 0.980 0.840 0.073 3.819 2.77 yes
Q‘ = (med.+high) 0.300 0.020 0.160 0.073 3.819 2.77 yes
13. m U. 3 none 0.420 0.340 0.380 0.097 0.824 2.77 no
2 22 a low 0.420 0.340 0.380 0.097 0.824 2.77 no
2 22 2| medium 0.140 0.180 0.160 0.073 0.546 2.77 no
5 :5 ‘jj. high 0.020 0.140 0.080 0.054 2.212 2.77 no
"_5 'LE (none+low) 0.840 0.680 0.760 0.085 1.873 2.77 no
Q Q”‘(med.+high) 0.160 0.320 0.240 0.085 1.873 2.77 no
13. w v. 5 none 0.420 0.380 0.400 0.098 0.408 2.77 no
2 2 2 ~ low 0.420 0.320 0.370 0.097 1.036 2.77 no
2 22 E medium 0.140 0.240 0.190 0.078 1.275 2.77 no
5 g 5 :| high 0.020 0.060 0.040 0.039 1.021 2.77 no
"_5 LL; (none+low) 0.840 0.700 0.770 0.084 1.663 2.77 no
Q Q: (med.+high) 0.160 0.300 0.230 0.084 1.663 2.77 no
1). 813. 5 none 0.340 0.380 0.360 0.096 0.417 2.77 no
2 32 ~ low 0.340 0.320 0.330 0.094 0.213 2.77 no
2 E}? E medium 0.180 0.240 0.210 0.081 0.737 2.77 no
525:” high 0.140 0.060 0.100 0.060 1.333 2.77 no
“_3 LL c§,l(none+low) 0.680 0.700 0.690 0.092 0.216 2.77 no
QQ Q: [(med.+high) 0.320 0.300 0.310 0.092 0.216 2.77 no

 

 

 

70

Table 31 (con’d)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Rating Level P1 P2 P Spl-pZ ZCAI.C ZCRIT,0.0056 difference

51gn1ﬁcant?
m .,, none 0.600 0.640 0.620 0.097 0.412 2.77 no
2 22' 3 low 0.360 0.300 0.330 0.094 0.638 2.77 no
2 § 2 El medium 0.040 0.060 0.050 0.044 0.459 2.77 no
E: 2i: ‘2] high 0.000 0.000 0.000 0.000 — 2.77 no
015 aERnoneHow) 0.960 0.940 0.950 0.044 0.459 2.77 no
(med.+high) 0.040 0.060 0.050 0.044 0.459 2.77 no
2 U, none 0.600 0.600 0.600 0.098 0.000 2.77 no
2 22' i; 16w 0.360 0.380 0.370 0.097 0.207 2.77 no
2 2 2 g medium 0.040 0.020 0.030 0.034 0.586 2.77 no
1: 2%; :1 high 0.000 0.000 0.000 0.000 — 2.77 no
55 £55; (none+low) 0.960 0.980 0.970 0.034 0.586 2.77 no
’ (med.+high) 0.040 0.020 0.030 0.034 0.586 2.77 no
m V, none 0.640 0.600 0.620 0.097 0.412 2.77 no
2' £2 2 low 0.300 0.380 0.340 0.095 0.844 2.77 no
:2 $2 a medium 0.060 0.020 0.040 0.039 1.021 2.77 no
1: (:37 :4 high 0.000 0.000 0.000 0.000 — 2.77 no
.53 a; (none+low) 0.940 0.980 0.960 0.039 1.021 2.77 no
”‘ ‘ |(med.+high) 0.060 0.020 0.040 0.039 1.021 2.77 no

 

Comparisons not of interest: p. = Untreated, Dark samples; p2 = Treated, Fluor. samples
p1 = Untreated, Dark samples; p2 = Treated, “Sun” samples
pi = Treated, Dark samples; p2 = Untreated, Fluor. samples
p1 = Treated, Dark samples; p2 = Untreated, “Sun” samples
p; = Untreated, Fluor samples; p2 = Treated, “Sun” samples
pi = Treated, Fluor samples; p2 = Untreated, “Sun” samples

as = (11k = 0.05/9 = 0.0056

71

 

Table 32: Statistical Analysis of Table 15 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Print Quality According to Print Type — All Samples)

 

 

 

 

 

 

 

 

 

 

 

 

Rating difference
Comparisons p] p2 p Spl'pz ZCALC ZCRrr,0.05 ignificant‘l
" g u > better 0.256 0.120 0.188 0.049 2.752 1.96 | yes 1
52 25 same 0.488 0.544 0.516 0.063 0.886 1.96 | no
worse 0.256 0.336 0.296 0.058 1.385 1.96 | no
n=125
k=1

(13 = a/k = 0.05/1 = 0.05

Table 33: Statistical Analysis of Table 16 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Background Polymerization According to Print Type - All

 

 

 

 

 

 

 

 

 

 

 

 

Samples)
Rating difference
Comparisons pl p; p Sp1-p2 20” ZCRH'O'OS Ligniﬁcant‘!
H 2 n > better 0.496 0.504 0.500 0.063 0.126 1.96 | no
52 :25 same 0.376 0.424 0.400 0.062 0.775 1.96 1 no
worse 0.128 0.072 0.100 0.038 1.476 1.96 | no
n =125
k =1

(13 = a/k = 0.05/1 = 0.05

72

 

Table 34: Statistical Analysis of Table 17 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Print Quality According to Lighting Condition - Samples
Aged 2 to 7 Days)

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Co::::§ons P1 P2 P Spl-pZ ZCALC ZCRrr,0.Ol7 Liifgzgﬁfq

u 25 n 3 better 0.260 0.120 0.190 0.078 1.784 2.39 no

a a 8'. if same 0.280 0.520 0.400 0.098 2.449 2.39 yes

worse 0.460 0.360 0.410 0.098 1 .017 2.39 no

11 .2 11 =: better 0.260 0.220 0.240 0.085 0.468 2.39 no

6. a Si 5; same 0.280 0.540 0.410 0.098 2.643 2.39 yes

’ worse 0.460 0.240 0.350 0.095 2.306 2.39 no

11 5; 11 =: better 0.120 0.220 0.170 0.075 1.331 2.39 no

5‘. 3 8'. 5; same 0.520 0.540 0.530 0.100 0.200 2.39 no

L“ = worse 0.360 0.240 0.300 0.092 1.309 2.39 no
n=50
k=3

ag=alk=0.05/3=0.017

Table 35: Statistical Analysis of Table 18 (Comparisons of the Effect of Acetic Acid
Regeneration Treatment on Background Polymerization According to Lighting Condition

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

-SamplesAged2to7Days)
Ratin difference
Comparifons p, p2 p SPLPZ 2mm chrr,0.017 Ligniﬁcant‘!
” 2 u ,5. better 0.400 0.480 0.440 0.099 0.806 2.39 no
a: g 23 same 0.440 0.420 0.430 0.099 0.202 2.39 no
”* worse 0.160 0.100 0.130 0.067 0.892 2.39 no
N 2 u 2 better 0.400 0.380 0.390 0.098 0.205 2.39 no
a. 5 a; same 0.440 0.520 0.480 0.100 0.801 2.39 no
' worse 0.160 0.100 0.130 0.067 0.892 2.39 no
u .5. H 2 better 0.480 0.380 0.430 0.099 1.010 2.39 no
53 a; same 0.420 0.520 0.470 0.100 1.002 2.39 no
L“ = worse 0.100 0.100 0.100 0.060 0.000 2.39 no
n=50
k=3
ag=alk=0.05/3=0.017

73

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