Ayang Aplacador Garcia Thesis Flame Emission Spectrometry

FABRICATION AND METHOD DEVELOPMENT FOR AN
IMPROVISED FLAME EMISSION SPECTROMETER FROM LOW

COST MATERIALS
A Thesis
Presented to
The Faculty of the Department of Physical Sciences
College of Science
Polytechnic University of the Philippines
Sta. Mesa, Manila
In Partial Fulfillment
Of the Requirements for the Degree
Bachelor of Science in Chemistry
By
APLACADOR, LUIS BERNARD B.

AYANG, NOEL ANGELO L.
GARCIA, JON JAY M.
March 2016
Acknowledgement
The researchers thank all who in one way or another contributed in the
completion of this thesis. First, we would like to give thanks to God for giving us
the knowledge, wisdom, protection and understanding throughout the study.
We also express our sincere gratitude to our advisor, Prof. Christian Jay B.
Cambiador for his continuous support of our research, for his patience, motivation,
enthusiasm and immense knowledge. His guidance helped us throughout our
research and writing of this thesis.
Moreover, we would like to thank the Oral Defense Panel, Prof. Jose Mari
M. Felicita, Prof. Melody Clerigo, Dr. Lorna T. Enerva, Mr. Mark Kristian Cabello,
Ms. Ann Selma Morata, Ms. Grace Ann Samson and Mr. Sherwin Escayo for their
constructive criticism and recommendations to improve our study.
The researchers also express their appreciation for the contribution of Julian
Victor Beldeniza, a Mechanical Engineering student, for the betterment of this
study.
To our beloved classmate and friends in the BS Chemistry family, we deeply
appreciate the stimulating discussions and the moral support that you shared to
us.
Most importantly, none of this could have happened without our family. We
would like to thank our parents who continuously offered their prayers and support
for us throughout the duration of our research. This research stands as a testament
to their unconditional love and encouragement.
iii
Abstract
Combustion flames contain strong emissions from excited radical species
produced by the combustion process. The monitoring and characterization of such
emissions is important for an in-depth understanding for the elemental analysis of
metal ions especially alkali, alkaline earth, and transition metals. This study
includes the fabrication of an improvised Flame Emission Spectrometer and testing
of the instruments system linearity. This paper also incorporates Digital ImageBased analysis of emitted radiation and reproducibility of the acquired results.
Methodology for this research is comprised of the design and assembly of the said
instrument, standard preparation to be used for the experimentation proper,
accuracy, precision, bias and recovery test of the instrument. The data from the
instrument were obtained using the Amadeus Spectrometer and its corresponding
Quantum Software. The data for the standards were then analyzed for its linearity
and regression, while the instrument was tested for its limit of detection and limit
of quantification. The said instrument was able to provide an accepted analysis for
the quantification of intensities of common metal ions while being much less
expensive, heavy, and bulky than comparable commercial instruments.
Keywords: emission spectroscopy, system linearity.
iv
TABLE OF CONTENTS
Page
TITLE PAGE . i
APPROVAL SHEET ii
ACKNOWLEDGEMENT . iii
ABSTRACT iv
TABLE OF CONTENTS ...v
LIST OF FIGURES ix
LIST OF TABLES ..x
CHAPTER I INTRODUCTION .1
1.1. Statement of the Problem .2
1.2. Objectives of the Study .....2
1.3. Scope and Limitations 2
1.4. Significance of the Study .. 3
1.5. Outline ..... 4
1.6. Definition of Terms . 5
CHAPTER II BACKGROUND AND REVIEW OF RELATED LITERATURE .. 6
2.1. Background of the Study ...... 6

2.2. Review of Related Literatures .. 7
2.2.1 Spectroscopy and the Electromagnetic Spectrum ..... 7
2.2.2 Atomic Emission Spectroscopy as an Analytical Method . 11
2.2.3 Flame Emission Spectroscopy .. 13
2.2.4 Determination of sodium and calcium in powder milk using
digital image-based flame emission spectrometry ..... 20
CHAPTER III RESEARCH METHODOLOGY ............................ 22
3.1 Introduction 22
3.2 Proposed Schematic Diagram for Flame Emission Spectrometry ...... 22
3.3 Improvisation of Atomic Absorption Spectrophotometer to Flame
Emission Spectrometer .. 22
3.4 Digital Image Based FES Analysis 25
3.5 Preparation of Standard Calibration Solutions 26
3.6 Limit of Detection and Limit of Quantitation . 27
3.7 Precision, Accuracy, Bias and Recovery Test .... 29
Conceptual Framework ..... 30
CHAPTER IV RESULTS AND DISCUSSION 31
4.1 Setup Parameters for FES Analysis . 31
vi
4.2 FES Analysis ....... 32

I. Na+ Analysis 32
a. 200 to 1000 ppm 32
b. 20 to 100 ppm .... 33
c. 2 to 10 ppm . 33
II. K+ Analysis ..... 34
a. 200 to 1000 ppm 34
b. 20 to 100 ppm .... 35
c. 2 to 10 ppm ................... 35
4.3. FES Analysis Discussion ............................ 36
4.4 Digital Image-Based FES Analysis ........................ 38
I. Sr2+ Analysis 39
a. 200 to 1000 ppm - Analysis of Green Values ... 39
b.1 20 to 100 ppm - Analysis of Red Values ............ 39
b.2 20 to 100 ppm - Analysis of Green + Red Values ..... 40
II. Ba2+ Analysis .. 41
a. 200 to 1000 ppm - Analysis of Red Values ................. 41
4.5. Digital Image-Based FES Analysis Discussion .. 41
General specifications of the fabricated flame emission spectrometer ........ 43
CHAPTER V CONCLUSION AND RECOMMENDATION .. 44
Conclusion ...... 44
vii
Recommendation ... 45
References .. 47
APPENDICES .... 51
Appendix A .. 52
Appendix B .. 64
Appendix C .. 81
Appendix D .. 84
Appendix E .. 86
Appendix F .. 88
viii
LIST OF FIGURES
Figure 1.
The Electromagnetic Spectrum
Figure 2.
A wave in an electric field
Figure 3.
Seven Stages of an Analytical Method
Figure 4.
The Solar Spectrum
Figure 5.
Notable milestones in the development of FES
Figure 6.
Temperature of flame generated from different sources in relation to

number of excited population
Figure 7.
Diagram of a turbulent flow burner
Figure 8.
A Perkin-Elmer design of a laminar flow burner
Figure 9.
Flame spectrum of sodium
Figure 10.
Flame spectrum of Calcium
Figure 11.
Schematic Diagram of AAS
Figure 12.
Schematic Diagram of the modified AAS for the fabrication of FES
ix
LIST OF TABLES
Table 1.
Na+ FES Analysis
1.1
200 1000 ppm Na+
1.2
20 100 ppm Na+
1.3
2 10 ppm Na+
Table 2.
K+ FES Analysis
2.1
200 1000 ppm K+
2.2
20 100 ppm K+
2.3
2 10 ppm K+
Table 3.
Sr2+ DIB-FES Analysis
3.1
200 1000 ppm Sr2+ (Green Values)
3.2
20 100 ppm Sr2+ (Red Values)
3.3
20 100 ppm Sr2+ (Red + Green Values)
Table 4.
Ba2+ DIB-FES Analysis 200 to 1000 ppm Ba2+
Chapter 1 INTRODUCTION
One of the most common procedures used to characterize a sample is
through elemental analysis. It is useful in most areas of human endeavor and is
commonly applied to samples of importance in geology, toxicology, forensic
science, prospecting, health, nanotechnology, materials science, industrial
process control, semiconductor processing, automobile manufacturing, and
others. Because of its wide range of application and importance, a broad suite of
methods for elemental analysis has been devised. These methods range from
long-established procedures such as those based on precipitation and titration to
more modern ones that rely as much on physical principles as on chemistry
(Hieftie, 2000). A common of method of Atomic Emission Spectroscopy is the
Flame Emission Spectroscopy. In flame emission spectroscopy, the flame
provides a means of converting analytes in a solution to atoms in the vapor phase
freed of their chemical surroundings. These free atoms are then transformed into
excited electronic states by one of two methods: absorption of additional thermal
energy from the flame or absorption of radiant energy from an external source of
radiation. The energy from the flame also supplies the energy necessary to move
the electrons of the free atoms from the ground state to excited states. The
intensity of radiation emitted by these excited atoms returning to the ground state
provides the basis for analytical determinations in FES.
1.1
Statement of the Problem
Methods that will be involved in the fabrication of the improvised Flame

Emission Spectrometer.
Methods that will be involved for the accuracy and precision of the said
instrument.
1.2
Efficiency and System linearity of the said instrument.
Reliability and Reproducibility of acquired results.
Objectives of the study

The general objective of this study is to fabricate a cost efficient butane-
propane mixed fuel based flame emission spectrometer. Specific objectives of the
study involve the quantitative and qualitative analysis of selected Alkali and
Alkaline Earth Metals, specifically Na, K, Sr and Ba via FES and test for system
linearity of the said instrument using known standards.
1.3
Scope and Limitation

This study focuses on the fabrication and method development of the said
instrument, test for system linearity using a known set of standards and for the
determination and analysis of the emission lines of selected Group 1A and 2A
metal ions such as Li, Na, K, Ca, Sr, and Ba. This research extend its analysis for
selected transition and post-transition metals with distinguishable spectral lines
such as Cr and Cu. The said instrument was limited in determining the emission
spectra of the mentioned metal ions. An optical fiber (detector) along with an
appropriate software (Ocean Optics Quantum software) was used to project the
2
signals live on screen. The fabrication of the instrument is limited in several

aspects. The research title is mainly used to describe and only limited to the
affordability of the fuel used. This research exclude the electrical output used,
running time and the lifespan of the fabricated instrument. The researchers only
account for the testing and method development of the instrument. This paper also
employed Digital Image-Based Flame Emission Spectrometry (DIB-FES) to
analyze for the digital images coming from the emitted radiation of metal ions
captured by a camera (MyPhone A848i duO) that acts as a detector, on the basis
of the Red-Green-Blue (RGB) color system. The treatment of the captured digital
images will be done by means of image analysis software (Microsoft Paint Tools:
Color Picker).
1.4
Significance of the study

Flame Flame Emission Spectrometer has both quantitative and qualitative
applications. Most applications of FES have been the determination of trace

metals, especially in liquid samples. It offers a simple, inexpensive and sensitive
method for detecting common metals, including the alkali and alkaline earths, as
well as several transition metals such as Mn, Cu, Zn, and Cr. The said instrument
is also capable of providing analyses for the quantification of intensities of common
metal ions while being less expensive than comparable commercial instruments.
Analysis of soft drinks, fruit juices, alcoholic beverages and water (e.g. industrial,
well, sea) in terms of its Na+, Ca2+ and K+ contents can also be conducted by using
FES. The fabricated Flame Emission Spectrometer would be able to provide
inexpensive quantitative analyses for the alkali metals and qualitative analyses for
3
alkaline earth metals without compromising the reliability and the validity of the
generated results. The instrument would also be notable for the inexpensiveness
and convenience of its fuel source since the employed propane-butane gas
mixture or LPG can be easily accessed in the market. Ultimately, the instrument
would be able to educate the universitys undergraduate students with the basic
principles of Flame Emission Spectrometry with minimal financial hindrance and
also provide them with one of the most established forms of instrumental analysis.
1.5
Outline
The outlines of this research were as follows: The following chapter contains
a brief review of the background study and related literatures applied in this study.
Theory involving the principles of atomic emission and absorption spectroscopy
were discussed, as well as various information from related studies of professional
researchers regarding this study. The next chapter describes the experimental
setup and the components used or suggested for the flame and the engine part
respectively. Preparation of standard solutions was also elaborated in this chapter.
Thereafter, implementation of the simulations was described, as well as the
methods for the experiments. The remaining chapters involved the tabulation and
discussion of result, conclusion, recommendation and listing of the acquired
references. Timeline review and budget proposed for this study was also
presented and discussed.
1.6
Definition of Terms
a.) Emission Spectroscopy involves the quantitative measurement of the optical

emission from excited atoms to determine analyte concentration.
b.) Spectrometer - is any instrument used to view and analyze a range (or a
spectrum) of a given characteristic for a substance (for example, a range of massto-charge values as in mass spectrometry), or a range of wavelengths.
c.) System Linearity ability of an analytical procedure to obtain test results that
are directly proportional to the concentration of analyte in the sample.
d.) Signal in analytical chemistry, are generated responses coming from the
interactions between species of the analyte or between certain forms of intrinsic
energy.
Chapter 2 - BACKGROUND AND REVIEW OF RELATED LITERATURE

2.1
Background
This study focuses on one of the most widely used collection of physical-
based techniques commonly known as atomic spectroscopy, specifically on Flame

Emission Spectroscopy. Atomic Spectroscopy consists of analytical techniques
that measure the concentration of chemical elements in the sample. In atomic
spectroscopy, the sample or substance of interest is decomposed into its
component atoms. All techniques in atomic spectroscopy involve atomization of
the sample, which is usually in the form of a solution. The field of atomic
spectroscopy includes Atomic Emission, Atomic Absorption, Atomic Fluorescence
and Atomic Mass Spectroscopy. In the case of Flame Emission Spectrometry, the
sample is nebulized and introduced into the flame, where it will be subsequently
vaporized and atomized. Emission or absorption of light may occur when the
substance is transformed into atomic vapor when exposed to high temperatures.
A certain proportion of these atoms emit radiation at wavelengths in the UV or
visible regions after undergoing subsequent excitation. These emissions or
absorptions are characteristic to different elements, and is proportional to the
number of excited atoms. In the case of emission spectrometry, the amount of
radiation emitted by the sample can be used to estimate the concentration/s of
element/s present in it.
Although Flame Emission Spectrometry is considered as a simple and
straightforward technique, it is however, not free of interferences. Examples of
such interferences are blank interference (i.e. Spectral Interference), and Analyte
interference (Physical and/or Chemical interference). Flame temperature is also
an important factor that determines the efficiency of atomization. The relative
number of excited and unexcited atoms also depends on flame temperature.
2.2
Review of Related Literature
2.2.1 Spectroscopy and the Electromagnetic Spectrum

Electromagnetic radiation (EMR) is generally known as a form of energy
that propagates through space in extremely high velocities, and can be described
as having both particle and wave properties. Although the wave model fails to
account for the absorption and emission phenomena, both properties are
complementary rather than mutually exclusive (Skoog, West, Holler and Crouch;
2014). The optical properties of electromagnetic radiation are better described by
its wave property, while treating electromagnetic radiation as particles or packets
of energy (photons) explains most of its interactions with matter including
absorption and emission (Harvey, 2000).
Figure 1. The Electromagnetic Spectrum
Figure 2. A wave in an electric field
The wave characteristic of electromagnetic radiation is often elaborated

through the depiction of a sine wave. It propagates in a linear path with constant
velocity. The wavelength of a wave is the linear distance between a waves
maxima or minima. Its frequency is the number of oscillations of the electric field
vector per unit of time. The frequency is dependent only on the emission source,
regardless of the medium being traversed, in contrast with its velocity v (in ms-1)
which is equal to the product of its wavelength and frequency given by the
equation:
Equation 1. Relationship of Velocity to Wavelength and Frequency
In a vacuum, electromagnetic radiation travels at the speed of light c at

2.99792 x108 ms-1 and about >0.1% slower in other media, and is often
approximated as 3.00 x108 ms-1 for most cases (Harvey, 2000). For interactions of
EMR with matter, the energy of a photon can be related to its wavelength and
frequency:
Equation 2. Relationship of Energy (photon) to Wavelength and Frequency
Where h is the Plancks constant which has a value of 6.626 x10-34 Js.
Spectroscopy can be generally defined as the interactions of matter and
radiation. These interactions can be used to quantitatively and qualitatively
understand the sample of interest. Spectroscopic analyses in analytical chemistry
dwell on the concept of electromagnetic radiation. It consists of measurements
based on electromagnetic radiation including light. Such techniques can be
classified based on what type of radiation is produced or used, according to the
electromagnetic spectrum (Skoog et. al, 2014). According to S. Thompson and J.
Staleys Foundations of Spectroscopy (n.d.), the two most commonly used
approaches in spectroscopic analyses are emission and absorption spectroscopy.
When matter is excited through the introduction of energy (e.g. thermal, radiant,
nuclear or electrical), it emits electromagnetic radiation as it reverts back to its
original state. The spectrum or range of the emitted radiation from an energized
substance is called an emission spectrum. According to Harvey (2000), the
intensity of the emission line is proportional to the number of atoms N* in the excited
state given by the equation:
Equation 3. Relationship of Intensity to the no. of atoms in excited state.
Where k is a constant related to the efficiency of the transition. The

population of the excited state for a system in thermal equilibrium is related to the
total concentration of atoms N, by the Boltzmann distribution. The Boltzmann
distribution for the excited state for many elements at temperatures below 5000 K
can be approximated as
Equation 4. Boltzmann distribution equation.
Where gi and g0 are statistical factors that account for the number of
equivalent
energy levels for the excited state and ground state respectively, Ei is the energy
of the excited state relative to that of the ground state (E0 = 0), k is Boltzmanns
constant equal to1.3807 1023 J/K, and T is the temperature in Kelvin. From
here we can observe that excited states with lower energies have larger
populations, therefore giving the most intense emission lines.
10
In the case of absorption, a substance is subjected to a continuous range

of radiation (e.g. white light) and the absorbed frequencies are analyzed. The
resultant spectrum retains the original range of radiation but with dark spaces
which may correspond to a missing or absorbed frequency, and is called the
absorption spectrum.
2.2.2 Atomic Emission Spectroscopy as an Analytical Method
Atomic Emission Spectroscopy (AES) was considered unique among the
other forms of Atomic Spectroscopy because it was the first to be used in
qualitative and quantitative analyses alike (Hieftje, 2000). Despite several
advances and changes in its methodology and instrumentation, it remains one of
the prevalent and widely used analytical techniques up to this day. Hieftje (2000)
stated that according to V. A. Fassel, an analytical method undergoes seven
stages in its existence. Any analytical method begins as an idea until it is published
and given design and structure.
Its figures of merit will then be tested and
improved up to its maturity, until it is receives general acceptance. Its fundamental

principles are further solidified through understanding until it reaches senescence
as an established technique.
Figure 3. Seven Stages of an Analytical Method
11
However, Hieftje (2000) wrote in his paper entitled Atomic Emission

Spectroscopy It Lasts and Lasts and Lasts a proposed revision of these seven
stages as follows:
Seven Stages of an Analytical Method (Modified)
1. Conception of idea
2. Successful demonstration and publication of idea
3. Improvement of instrumentation; figures of merit
4. Maturity; general acceptance; automation
5. Improved understanding of fundamental principles;
Introduction of new instrumentation
6. Iteration of steps 35
7. Old age and senescence
Hieftje pointed out in his revision of the stages laid down by Fassel that an
analytical method will continuously undergo improvement, acceptance of such
improvement and a further understanding of its principles. As the technique
matures, further study would allow opportunities to create more improvement,
promote acceptance and provide a deeper understanding of the technique. These
stages are reiterated until no more improvement can be done or another technique
proved to be more dominant. When such limit is reached, the technique can then
be considered to be in its old age. Moreover, Hieftje associated the widespread
success of AES as a superior analytical method in accordance to his revised
stages as this technique was subjected to several improvements especially in its
instrumentation and emission sources, and deeper understanding as it
12
progressed. This is what made AES a resilient technique that has undergone
several defining changes but still relies on its most fundamental principles.
2.2.3 Flame Emission Spectroscopy
The principle of Flame Emission can date back to 1556 where Georgius
Agricola wrote in his De Re Metallica about the color of fumes from various types
of ores (Schrenk, 1986). Although the very first observations of atomic emission
can date even back to the discovery of fire in the prehistoric era, Agricolas work
is one of the earliest known records that introduce the role of flame in substance
identification, especially in metals. And that this breakthrough marks the start of
the utilization of flame in chemical analysis especially in Atomic Spectroscopy.
Aside from Newtons study about the solar spectrum including nature of light and
its colors, another notable early account was in 1752 by Thomas Melville who
observed distinguishable color changes in a flame that was incorporated with sea
salt and other substances. Further accounts helped solidify the foundations of what
would now be known as Flame Emission Spectrometry (FES, a.k.a. flame
photometry). Additionally, further description of the spectral features of the solar
spectrum was conducted in 1802 by Wollaston, who distinguished dark lines in a
photographic image of the solar spectrum. These lines were studied in detail by
Fraunhofer in 1817 who labeled them with letters of the alphabet starting from the
red end of the spectrum (Skoog et. al, 2014). Also, it was W.H. Fox Talbot in 1834
that iterated the promising potential of flame emission spectrometry as an
analytical tool (Schrenck, 1986).
13
Figure 4. The Solar Spectrum
Later works of R.W. Bunsen and G. Kirchhoff in 1859 to 1860 recognized

the independence of the spectral lines emitted by the metals to the anions with
which they are bound and confirmed the coincidence of these emission lines to the
absorption lines discovered earlier by Fraunhofer (Hieftje, 2000). Kirchhoff proved
that the D lines previously labeled by Fraunhofer was due to the absorption of
solar radiation by sodium atoms at about 589 nm (Harvey, 2000) and the A and
B lines were due to potassium (Skoog et. al, 2014). (Hieftje also acknowledged
the most important milestones in flame photometry which were in 1879 on L.P.
Gouys employment of a pneumatic nebulizer for the introduction of a sample
solution into the flame and Lundegrdhs coupled air-acetylene flame, pneumatic
nebulizer and a spray chamber for the nebulized solution. He provided a brief
summary of the major breakthroughs in the development of the Flame Emission
Spectrometry starting from the 1850s.
14
Figure 5. Notable milestones in the development of FES represented by the bar at the top. The
darker shades represent a higher level of activity in the particular period.
Further development in the late 1800s was very minimal. During this period
the flames used were generated only from either natural gas or alcohol lamps, and
utilizing air as an oxidant. The flames yielded by these sources were stable and
reproducible yet allowed only the analysis of easily excited elements due to its
relatively low temperature. It was until 1928 when Lundegrdh utilized an airacetylene burner which provided a considerably stable flame but with a higher
temperature than those generated by the previously used sources, and marked
the modern period for FES. He was able to produce sufficient data for twenty-four
elements namely Li, Na, K, Rb, Cs, Ca, Sr, Tl, Mn, Cu, Ag, Cr, Fe, Ni, Ba, Er, Mg,
Pb, Pd, Ra, Y, Au, Cd, and Nd. (Schrenk, 1986). This was due to the principle that
the intensity of the emission is directly proportional to the population of the atoms
in the excited state. Although the acetylene flame burner provided a hotter flame,
15
the butane flame gives off a better signal (Neel, Crespo, Perret, Cherubini, Bakker;
2014).
Figure 6. Temperature of flame generated from different sources in relation to number of excited
population
Developments in the late 1900s were focused on the improvement of the

instruments nebulizer and burner designs. Researchers were focused on
developing a stable flame but with even higher temperature for the inclusion of
even more elements into the technique. Early burner designs include the Turbulent
Flow Burners by the Beckman Corporation in 1948 (Schrenk, 1986) in which the
fuel and oxidant flow from separate vessels and are mixed at the orifice/s of the
burner. The oxidant is sometimes used to aspirate the sample.
16
Figure 7. Diagram of a turbulent flow burner
Figure 8. A Perkin-Elmer design of a laminar flow burner
17
Although FES was further developed through the utilization of the

Inductively Coupled Plasma as the means of excitation (ICP-AES), the technique
itself is not free from interferences. One of the known interferences is Blank
Interference which produces an effect independent of the analyte (Skoog, et. al,
2014). A decent example of this is Spectral Interference which emits radiation
within the wavelength of the analyte or produces a stray radiation. These
interferences can be best reduced or prevented by preparing a perfect blank.
Another type of interference is the Analyte Interference which changes the
magnitude analyte signal, and can be further categorized into Physical or Chemical
Interference. Physical Interferences include effects in atomization, nebulization,
volatilization and other physical constraints, including viscosity that may affect the
flow rate of the solution. Chemical interferences include solute volatilization
interferences which hinders the volatilization of the analyte by forming nonvolatile
complexes. Substances that suppress the ionization of the analyte are also
considered as interferences. To counteract such chemical disturbances, protective
or releasing agents are utilized. Protective agents form a stable but volatile
complex with the analyte, while Releasing agents are used to react with the
interference to prevent its interaction with the analyte. Another notable interference
is self-absoprtion which is the absorption of emitted radiation by the other atoms
in the ground state, weakening the intensity of the emission. This interference is
easily alleviated by increasing the flame temperature (Harvey, 2000).
18
Spectral Lines of common Alkali and Alkaline Earth Metals (Na, Ca)
The sodium spectrum is dominated by a line of 589 nm wavelength, coming
from the transition from the 3p state to the 3s state.
Figure 9. Flame spectrum of sodium. Scale: wavelength in nm. (Data from: Sansonetti and Martin,
Handbook of Basic Atomic Spectroscopic Data)
If there are more than one electron in the outermost shell, there are many
more possibilities of electronic transitions and the spectra accordingly become
more involved.
Figure 10. Flame spectrum of Calcium. (Only the stronger lines are shown.) Scale: wavelength in nm.
19
Most elements give no conspicuous color to flames. If the valence electrons

are more strongly bound, the energies of the lowest excitations correspond to the
ultraviolet region; the strongest spectral lines therefore are invisible for us.
2.2.4 Determination of sodium and calcium in powder milk using digital
image-based flame emission spectrometry
A research conducted by W. da Silva Lyra, et. al. proves the efficiency of
the use of digital image-based flame emission spectrometry to overcome the
inherent spectral interference in Flame Emission Spectrometry (FES) when
sodium and calcium are present in the same sample. Digital Image-Based Flame
Emission Spectrometry (DIB-FES) is a variant of traditional FES. The main
difference with respect to FES is how the analytical signal is obtained. According
to the study, In DIB-FES a digital camera or video camera (webcam) is used along
with digital image analysis to obtain the analytical signal. This new approach has
produced excellent results for direct determinations of lithium in anti-depressives
(tablets), sodium in Normal Saline (NS), and calcium in waters, with similar results
for indirect determinations of sodium diclofenac, sodium dipyrone, and calcium
gluconate in injections (medicine). Since DIB-FES employs a simple webcam and
no wavelength selector, the images (and analytical response) are susceptible to
spectral interference in analysis. By applying chemometric methods, especially
inverse calibration which does not need explicit interference modeling, the DIBFES has the potential to overcome this drawback. Metals in the airbutane flame
mit radiation which is revealed in the digital images captured by a webcam
(detector), on the basis of the Red-Green-Blue (RGB) color system. The results of
20
the study confirm the model's discriminating power in isolating each analyte's
information from a single digital image, even with spectral interference.
This study will be able to provide an insight to the researchers on how to
employ an alternative method of detection for the emission spectra of metal ions
which offers a simple and economically viable alternative to the conventional FES.
21
Chapter 3 RESEARCH METHODOLOGY

3.1
Introduction
This chapter discusses the methodology that was used in this study. The
first section describes the modification and fabrication of the instrument, followed
by development of a method for analyzing metal ions. The third part describes the
preparation of the standard solutions that were subjected in the analysis.
Subsequent sections explicate the conducted experiments and analysis to
investigate the efficiency, accuracy, precision and system linearity of the fabricated
instrument.
This research was conducted based on the methodology. This methodology
plays an important role in implementing this research study accordingly. The
details of the methodology are explained in detailed in this chapter.
3.2
Improvisation of Atomic Absorption Spectrophotometer to Flame

Emission Spectrometer
Figure 11. Schematic Diagram of AAS
22
Figure 12. Schematic Diagram of the modified AAS for the fabrication of FES
Figure 11 and Figure 12 demonstrates the schematic diagram of the

nonfunctional AAS and the fabricated FES. Unlike its original specifications, the
fabricated instrument no longer requires the use of a hollow cathode lamp, a
photomultiplier tube and an oxidant gas and only utilizes an inexpensive detector
and fuel. Instead of a Hollow-cathode lamp and a photomultiplier tube, a readily
available optical fiber with a corresponding spectrometer was used as a detector
for the FES. The reason for this modification was the availability and accessibility
of instruments that can be used to remake, reuse and modified the nonfunctional
AAS to FES by applying the principle of emission spectroscopy. The optical fiber
cable enables the light to propagate into the spectrometer, it was then connected
to a computer and uses a corresponding digital software to determine the spectrum
of the detected light signal.
Additionally, a phone camera (Model: Myphone A848i Duo) was also used
as a detector. The generated images of the flame were analyzed for its RGB values
23
using an appropriate software (Microsoft Paint Tools) in order to determine if there

was a relationship between the concentration of the analyte and its corresponding
RGB values.
Air-Acetylene together with an oxidant gas was commonly used as a fuel
source of AAS. The fabricated instrument no longer used Air-Acetylene as a fuel
source, but instead used an inexpensive fuel, in this case, a butane-propane mixed
fuel to carry out the flame generation.
Assembly. The coupled burner-nebulizer of the Universitys Buck Scientific
210VGP Atomic Absorption Spectrometer was subjected to the fabrication of the
instrument. It has a Polypropylene spray chamber with pre-mix burner and high
efficiency adjustable nebulizers (SS) and Titanium burner heads. Liquefied
Petroleum Gas (Propane-Butane Mixture) was used as fuel a source for the
burner. The introduction of the sample solutions were regulated with the aid of an
air compressor, connected to the nebulizer for a stable fluid flow within the system
and to avoid extinguishing the flame. The fiber optic probe of the Amadeus
Spectrometer was clamped onto an iron stand and placed at about 1 inch
horizontally away from the flame source and linked to a spectrometer that was
connected similarly to a computer for collection and analysis of data.
Nebulization. An analytical Pneumatic Nebulizer coupled with an air compressor
was used to aspirate the solution into the flame with a consistent regulated
pressure.
24
Flame generation. The outlet of the nebulizer was guided to the air inlet of the
burner. The compressed air nebulizing the sample was adjusted to the highest
possible velocity before resulting in a dimming of the flame. The used air was from
an air compressor instrument.
Flame analysis. The analysis was carried out in a room with minimal light
interference to avoid stray light from reaching the detector. A fiber optic probe (1.8
meter, flame resistant) was directed 1 inch horizontally away to the widest part of
the flame transmitting the light to a USB powered spectrometer (Amadeus
Spectrometer, 350850 nm range, 3 nm resolution). The optical signal was sent
through a USB port to a Windows computer with the appropriate software (Ocean
Optics Quantum software) from where it can be projected live on screen. Emission
Spectra results will then be analyze for their peak intensities.
3.3
Digital Image-Based FES Analysis.

A phone camera (Model: MyPhone A848i Duo) was used to capture the
images, and was connected by a universal serial bus (USB) to an Intel I3 2.3GHz
Laptop computer (PC). The camera captures at a rate of 30 frames per s, with 5.0
Mega Pixels Dynamic Images. The atomizer/emitter module of a flame emission
spectrometer was coupled to the camera, and the combined system was used to
generate and record the image of the flame. The recorded images were then
transferred to the laptop computer for the image analysis. The treatment of the
captured digital images were done in the basis of RGB color system by means of
using an image analysis software: Microsoft Paint Tools, Color Picker.
25
3.4
Preparation of Standard Calibration Solutions

Chemicals and Reagents that were used in the experiment were obtained
from the Universitys Laboratory. For powdered standards, the researchers oven
dried the powdered reagents for about 120 degrees Celsius for 180 minutes to
eliminate moisture present in the powdered reagents before subjecting it in the
preparation of standard solutions.
For 1000 ppm Sodium Chloride stock solution.
2.542 g of sodium chloride was dissolved with enough de-ionized water and
then transferred into a 1000 ml volumetric flask and diluted to mark.
For 1000 ppm Potassium Chloride stock solution.
1.907 g of potassium chloride was dissolved with enough de-ionized water
and then transferred into a 1000 ml volumetric flask and diluted to mark.
For 1000 ppm Strontium Chloride stock solution.
1.405 g of strontium chloride was dissolved with enough de-ionized water
For 1000 ppm Barium Chloride stock solution.
1.7785 g of barium chloride was dissolved with enough de-ionized water
For 1000 ppm Copper Sulfate stock solution.
2.511 g of copper sulfate was dissolved with enough de-ionized water and
diluted to mark into a 1000 ml volumetric flask.
The standard solutions used in this research covers a set of range of
concentration from a relatively higher concentration (200 to 1000 ppm range) to a
26
relatively lower concentration of standard solutions (2 to 10 ppm range). This was

done in order to test for system linearity of the fabricated instrument using a
broader range of standards.
3.5
Limit of Detection and Limit of Quantitation

For this study, the test for the LOD will be determined based on the standard
deviation of the Response and the Slope through the formula:
Equation 5. Formula for the calculation of LoD
Where Sb is the standard error of the y-intercept, or simply the standard

deviation of the response and m is the slope of the calibration curve.
The slope of the calibration curve S may be approximated from the
calibration curve of the analyte. The estimate of may be carried out based on the
standard deviation of the blank or based on the calibration curve, studied using
samples with analyte concentrations within the DL where the residual standard
deviation of a regression line or the standard deviation of y-intercepts of regression
lines may be used as the standard deviation.
The limit of quantitation of this study was determined similarly based on the
standard deviation of the response and slope and can be expressed as:
27
Equation 6. Formula for the calculation of LoQ
Likewise, S can be approximated from the calibration curve of the analyte;

and the standard deviation may be carried out based on the standard deviation of
the blank or based on the calibration curve studied with samples at the range of
QL. Similarly, the residual standard deviation of a regression line or the standard
deviation of y-intercepts of regression lines may be used as the standard deviation.
Linearity
The linearity was evaluated through visual inspection of the plotted signals
with respect to analyte concentration, and then evaluated by statistical methods
specifically the calculation of the regression line by the least square method.
Uncertainty
The expected uncertainties of result of this study were due to a number of
different interferences that may be caused by any or either of the following: (i)
unstable pressure outflow, (ii) wind and light interferences and (iii) contamination
of solutions.
28
3.6
Precision, Accuracy, Bias and Recovery Test.

The test for the precision of the instrument were carried out by conducting
repeated measurements of the intensities of each standard solutions that were

analyzed under the same given conditions. Values from the repeated
measurements that are relatively close to each other would indicate a rather
precise result.
The test for the accuracy and correction for bias of the instrument were
evaluated through the Calibration method which involves the selection of reference
standards with known values to cover the range of interest, measurements on the
reference standards with the instrument to be calibrated and functional relationship
between the measured and known values of the reference standards (usually a
least-squares fit to the data) called a Calibration Curve (Skoog, et.al. 2007). The
closer the value of correlation coefficient to 1, the better the fit of the line or curve
to the data which reflects the accuracy and system linearity of the instrument.
Recovery Test was employed in this study in order to evaluate the
accuracy and correction for bias in the proposed method. In this study, the referred
evaluation was made by spiking. According to this strategy, the spiked sample is
prepared by addition of the analyte(s) after sampling and before all analytical
procedures. The analytical signal of the spiked sample was recorded within the
linear response range of the method. The original sample was prepared by dilution
of the same aliquot used in the spiked procedure to the same final volume. The
recovery (or recovery factor) is calculated according to the following equation:
29
Equation 7. Formula for the calculation of Recovery factor.
Where x(obs) is the observed/recovered value obtained from the analytical

process via calibration graph, and x(ref) is the reference value.
Conceptual Framework
Start
Fabrication of the
Instrument
Method
Development of
the Instrument
Precision,
Accuracy,
Correction for Bias
and Recovery Test
LoD and LoQ

Calculation
Test for System

Linearity
Write Up
End
30
Chapter 4 RESULTS AND DISCUSSION

4.1
Setup Parameters for FES Analysis

The analysis was conducted in a room with minimal light and wind
interference. The room is also provided with a fully functional fire extinguisher in
case fire hazard occurs. In case of emergency, notify all safety personnel and
remove all sources of heat and ignition immediately.
For the calibration curve of standards ranging from 100 to 1000 ppm NaCl,
the pressure flow of the air compressor is controlled and maintained at level 4
(regardless of the amount of pressure that the air compressor provide) and the fuel
output of the burner is regulated at level 2. The optical detector is clamped to an
iron stand and focused horizontally at least 1 inch away from the burner and
pointed slightly above the hottest region of the flame (middle part of the flame). In
addition, the data was obtained using Quantum Software through a point and click
scheme. Once a stable flame was obtained, the tip of the projected peak was
identified by the researchers and a screenshot was taken in order to corroborate
the findings acquired.
However, for the calibration curve of 20 to 100 ppm NaCl and the entire
calibration range of KCl standards, we adjusted the pressure flow of the air
compressor down to level 3. This is because of the instability of the flame at higher
pressures especially when analyzing standards of relatively low concentration.
Adjustment of pressure flow changes the intensity reading of the fiber optics, but
as long as the pressure level output for a given calibration range is consistent all
31
throughout the duration of the analysis, it will still yield an intensity that corresponds
to the given concentration.
4.2
FES Analysis
I. Na+ Analysis
a. 200 to 1000 ppm
Table 1.1 Respective intensities of various standard solutions for triplicate trials together with the
obtained R Squared Value, LoD, LoQ and Percentage Recovery.
200 - 1000 ppm Calibration Range

Concentration (mg/L) (N=3) Mean Intensity SD
1000
61730 1467
800
50845 1549
600
40500 2053
400
30628 1330
200
20216 819.8
R-Squared Value:
0.9997
LoD (mg/L):
20
LoQ (mg/L):
61
% Recovery:
95.2 %
The results obtained from the average of triplicate trials for concentrations
200 to 1000 ppm exhibits a linear behavior with a regression coefficient of 0.9998
and a percentage recovery of 95.2%.
32
b. 20 to 100 ppm
R-Squared Value: 0.9999
Concentration (mg/L)
(N=3) Mean Intensity SD
LoD (mg/L):
1.2
100
6835 20.00
LoQ (mg/L):
3.7
80
5680 0.5800
% Recovery:
102.2 %
60
4475 142.5
40
3285 70.44
20
2059 46.70
The results obtained from the average of triplicate trials for concentrations
20 to 100 ppm exhibits a linear behavior with a regression coefficient of 0.99995
and a percentage recovery of 102.2%.
c. 2 to 10 ppm
10
2021 94.06
1811 51.87
1615 5.77
1406 32.51
1224 71.23
33
LoD (mg/L):
0.29
LoQ (mg/L):
0.88
% Recovery:
95.2 %
Analysis for linear regression of data obtained from average of triplicate

trials for concentrations 20 to 100 ppm exhibits a linear behavior with a regression
coefficient of 0.99975 and a percentage recovery of 95.2%.
II. K+ Analysis
a. 200 to 100 ppm

1000
32099 51.00
800
28262 690.5
600
24361 332.0
400
19844 211.4
200
16064 219.4
R-Squared Value:
0.9992
LoD (mg/L):
36
LoQ (mg/L):
110
% Recovery:
105.5 %
The average of triplicate trials for 200 to 1000 ppm of KCl yielded a linear
calibration plot with a regression coefficient of 0.9996 and a percentage recovery
of 105.5%. Calculation of percentage recovery was done by employing an
analytical technique called spike method.
34
b. 20 to 100 ppm
Table 2.2 Respective intensities of various standard solutions for triplicate trials together with
the obtained R Squared Value, LoD, LoQ and Percentage Recovery.

LoD (mg/L):
4.0
100
10182 563.5
LoQ (mg/L):
12
80
8346 153.1
% Recovery:
97.1 %
60
6571 265.8
40
4745 109.7
20
3214 228.1
The establishment of calibration curve from the average of triplicate trials

for 20 to 100 ppm of KCl exhibits a linear behavior with a regression coefficient of
0.9995 and percentage recovery of 97.1%.
c. 2 to 10 ppm
R-Squared Value:
0.9999
LoD (mg/L):
0.14
10
1509 6.000
LoQ (mg/L):
0.41
1360 41.00
% Recovery:
101.8 %
1208 23.07
1066 16.64
912 10.00
35
Establishment of calibration curve from the average of triplicate trials for 2

to 10 ppm of KCl yielded a linear plot with a regression coefficient of 0.99995 and
percentage recovery of 101.8%.
4.3
FES Analysis - Discussion

The flame analysis using the fabricated Flame Emission Spectrometer was
conducted by using standard solutions of metal ions of varying concentrations,

namely Na+, K+, Ba2+, Sr2+ and Cu2+. Utilizing various concentration ranges of each
standard solution enabled the researches to determine the effect of concentration
on the intensity of the flame emission. Intensities of the respective metal ions were
analyzed quantitatively using the fabricated FES and projected into a computer
using an Amadeus Spectrometer and its accompanying Quantum Software.
Only the sodium and potassium ions proved to be viable for quantitative
analysis. This is due mainly to temperature constraint since the propane-butane
based LPG fuel used for the analysis can only reach a temperature of 2243.15 K,
which is not sufficient to excite metal ions beyond the alkali group. The data
obtained from Quantum Software were encoded into MS Excel and analyzed for
its linearity. For the analysis of the Linear Regression for each set of data, the
researchers used the Linest and the Analysis Toolpak feature of MS Excel for a
more comprehensive analysis.
The test for the linear regression for each set of data yielded a considerably
justifiable outcome. Each set of data were found to exhibit a significantly linear
behavior. Also, since the fabricated instrument does not have an Auto Zero
36
function, the calibration curve was baseline corrected in order to approximate the
intensity of a blank sample. The Linest feature was carried out in order to verify the
regression and slope of the line and determine the standard deviation of each data.
The Significance F- Values from the F-test were also determined in order to verify
if the regression was just a merely a chance occurrence (other supporting
statistical data are included in Appendix A). For this parameter the accepted values
are less than or equal to 0.05. The values obtained from the analysis of each set
of data were found to be substantially less than 0.05, which validates the statistical
significance of the obtained results. The P-value on the other hand was determined
in order to validate if the values of the Y- intercept or the X variable are merely a
result of chance. The considerably low P-values from the obtained statistical
treatment depict the reliability and the likelihood that the results did not occur by
chance.
From the statistical output acquired, the researchers were able to calculate
the Limit of Detection (LoD), and Limit of Quantification (LoQ) for each set of data.
The LoD represents the lowest possible concentration that can be detected by the
instrument while the LoQ is the lowest possible concentration that can not only be
detected but is also viable for statistical treatment. The researchers managed to
obtain relatively low concentration values for the LoD and LoQ for each set of data.
Such recovery test was carried out by using measurements of the standards used
which were not included for the determination of the mean. This was done by
selecting the mean intensity of a certain concentration within each range of
standards and determining the resulting intensity when a sample or in this case, a
37
synthetic sample is spiked. The percent recovery was then calculated for each of
the concentration ranges. A percent recovery of about 100% 10 % for each range
demonstrates a substantial recovery and renders the validity of the results.
4.4
Digital Image-Based FES Analysis

For metal salts beyond the Group I Alkali Metals, the researchers utilized a
method known as Digital Image-Based FES. This analytical technique relies on the
principle of RGB values of pixels from images captured and projected digitally on
an LCD screen. For this purpose, the researchers used a smartphone camera
(Model: MyPhone A848i Duo) to capture images of the flame while running
standard solutions of varying concentrations of a specific metal salt. The captured
images were then transferred to a computer and analyzed for their respective RGB
values. This was carried out by selecting a representative pixel from the flame
image in quintuplicate and using the Color Picker feature of Microsoft Paint.
A Flame image subjected to DIB-FES Analysis
38
I. Sr2+ Analysis
a. 200 to 1000 ppm Green Values

1000
54.4 2.70
800
25
LoQ (mg/L):
75
% Recovery:
102.6 %
44.6 2.30
600
36.0 0.71
400
26.8 2.39
200
LoD (mg/L):
18.0 1.22
A recovery percentage of 102.6% is obtained from the analysis of 200 to

1000 ppm SrCl2. The Green values were taken and plot against each of its
corresponding concentration. These values were found to be of linear behavior
with a linear regression value of 0.9998.
b. 20 to 100 ppm Red Values
Concentration (mg/L) (N=3) Mean Intensity SD
LoD (mg/L):
1.6
107.8 2.170
LoQ (mg/L):
4.8
60
87.2 3.270
% Recovery:
105 %
40
66.4 3.440
20
44.8 1.920
100
128.0 2.550
80
39
For the analysis of 20 to 100 ppm SrCl2, the Red values were taken and
plot against each of its corresponding concentration. These values were found to
be of linear behavior with a linear regression value of 0.9999 and a recovery
percentage of 105% was obtained from the calibration curve via spike method.
c. a. 20 to 100 ppm - Green + Red Values

100
145.4 38.87
80
124.0 33.38
60
106.2 27.08
40
84.4 21.06
20
64.8 14.21

LoD (mg/L):
0.14
LoQ (mg/L):
0.41
% Recovery:
101.8 %
A recovery percentage of 101.8% obtained from the analysis of 20 to 100

ppm SrCl2. The sum of Mean Red and Mean Green values were taken and plot
against each of its corresponding concentration. These values were found to be of
linear behavior with a linear regression value of 0.99965.
40
II. Ba2+ Analysis

a. 200 to 1000 ppm Red Values
Table 4. Respective intensities of various standard solutions for triplicate trials together with the

1000
146.25 2.070
800
0.9995
LoD (mg/L):
28
LoQ (mg/L):
84
% Recovery:
92.5 %
133.75 1.340
600
123.00 1.670
400
111.00 2.700
200
R-Squared Value:
98.75 1.640
For the analysis of 200 to 1000 ppm BaCl2, the mean Red were taken and
plot against each of its corresponding concentration. These values were found to
be of linear behavior with a linear regression value of 0.99975 and recovery
percentage of 92.5% was obtained via spike method.
4.5
Digital Image-Based FES Analysis - Discussion

For metal salts beyond the Group I Alkali Metals, the researchers utilized a
method known as Digital Image-Based FES. This analytical technique relies on the
principle of RGB values of pixels from images captured and projected digitally on
an LCD screen. For this purpose, the researchers used a smartphone camera
(Model: MyPhone A848i Duo) to capture images of the flame while running
standard solutions of varying concentrations of a specific metal salt. The captured
images were then transferred to a computer and analyzed for their respective RGB
41
values. This was carried out by selecting a representative pixel from the flame
image in quintuplicate and using the Color Picker feature of Microsoft Paint. These
values were subjected to linear regression analysis in order to determine which of
the Red, Green and Blue values would exhibit a linear behavior with respect to the
concentration. Afterwards, in-depth analysis using the Linest and Analysis Toolpak
feature of MS Excel was carried out to determine the Linear Regression, Standard
Deviation, and the Significance F and P-Values for each set of data.
The calibration curve for each set of test concentration were found to have
linear regression values approximately very close to 1, which exhibits the direct
relation of the intensity with respect to the concentration. Likewise, the Significance
F and P values were also determined in order to validate the statistical reliability of
the obtained output (other supporting statistical data are included in Appendix A).
The researchers were able to obtain Significance F and P-values which are notably
less than 0.05 which depicts the likelihood that the regression and the x variable
and the y-intercept values are not obtained by chance. In a similar manner, the
LoD and LoQ for each set of data were determined and found to be of substantially
low concentration values. Ultimately, a recovery test was carried out in a similar
manner for the data obtained for each of the concentration ranges. Likewise the
researchers were able to acquire an approximately 100% 10 % percent recovery
for each of the ranges, illustrating the considerable trueness of the generated
results.
42
GENERAL SPECIFICATIONS OF THE FABRICATED FLAME EMISSION

SPECTROMETER
Electrical
Computer: Acer Aspire 5740 5847

AC 120/230 V, 50/60 Hz, and Power Consumption: 65W
Oil less Air Compressor: Buck Scientific 3HBE-10-M303X

AC 220 V
Detector and Spectrometer
Fiber Optic Probe - 1.8 meter, flame resistant, capable of detecting light at
350-850 nm range.
Amadeus Spectrometer USB Powered, 350850 nm range, 3 nm

resolution.
Fuel Source
Commercial Propane-Butane Mixed Liquefied Petroleum Gas 1.5 Kg
Burner Assembly
Design: Polyethylene Pre-mix chamber, glass impact bead dispersion
Burner Head: Titanium; Air-butane-propane head 4 x 0.026 single slot
Adjustments: Horizontal g
Operating Modes
Emission: Detection and quantification of Intensity via excitation of Atoms.
Concentration: to 5 Significant digits
Screen Refresh (Projection of Signal - Quantum Software) 0.5 to 1.5

seconds
43
Chapter 5 CONCLUSION AND RECOMMENDATION

Conclusion
The fabrication and method development of the said instrument were
considerably carried out in accordance to the proposed methodology of the
researchers. The results obtained are substantially sufficient and statistically
reliable. This research also proved that the improvised FES doesnt compromise
the validity of its acquired result even though it is a product of the modification of
the nonfunctional AAS. It is supported by statistically reliable results obtained from
the conducted flame analyses. The findings of this research verified the fabricated
FES to be a cost efficient, inexpensive and practical instrument for both qualitative
and quantitative analysis of Na+, K+, Ba2+ and Sr2+. This study was also able to
demonstrate the effect of pressure on the intensity emitted by the solution that is
subjected to the flame analysis. A higher pressure results in distinguishably higher
emission intensity. Results of the analysis produced calibration curves which are
generally of approximately linear behavior. This support the direct relation of the
emission intensity with respect to the concentration. In line with this, system
linearity, precision and accuracy of the fabricated FES were sufficiently satisfied.
The researchers also employed a recent method of analysis called Digital
Image Based Flame Emission Spectrometry in order to quantitatively and
qualitatively analyzed Sr2+ and Ba2+ since the Quantum software was incapable of
projecting distinct signals due to a relatively low flame temperature. The results of
this method produced linear calibration curves from the analyzed RGB Values from
44
the flame images of varying concentrations of Sr2+ and Ba2+ standard solutions.
This illustrates the direct relationship of RGB Values of the image and the
concentration of the solution being analyzed.
Recommendation
Birds Eye View
Side View
Top View
Figure 5. Proposed room plan for the viable storage of the fabricated FES.
45
Figure 5 exhibits the proposed room plan for the viable storage, utilization
and maintenance of the fabricated FES. Ideally, the room should be fully airconditioned, contains a fume hood/exhaust fan and has a functional fire
extinguisher. Also, the room should be most likely free from wind interference and
contains minimal light interference as much as possible.
The researchers suggest utilizing a compressed air tank with the aid of an
air compressor in order to regulate and maintain a constant pressure flow all
throughout the analysis.
To minimize the time consumed for the assembly of the instrument, the
researchers recommend providing an air compressor and a fiber optic detector
(Amadeus Spectrometer) that will solely be used for the operation of the
instrument.
For financially abled future research involving the fabricated FES, the
researchers advise the use of Acetylene Fuel in place of the Propane-Butane LPG
mixture to be able to expand the scope of analysis of metal ions beyond the group
I and II metals.
46
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50
APPENDICES
51
APPENDIX A
Summary of Statistical
Evidence and Supporting Data
52
APPENDIX A
SUMMARY OF STATISTICAL EVIDENCE AND SUPPORTING DATA OBTAINED
FOR EACH SET OF CONCENTRATION RANGE FOR FES ANALYSIS
The following tables were the statistical values obtained from the treatment of given data
from FES Analysis using MS Excel Functions. Residual values were also obtained from
the analysis of results.
200 1000 ppm Na+ Calibration Range

STATISTICAL OUTPUT
STATISTICAL OUTPUT
R-squared Value
0.9999
Standard deviation
22.36
Slope P-value
3.96E-07
Slope-intercept P-value
3.60E-05
Significance F
3.96E-07
95.2 %
Percentage Recovery
102.2 %
LoD (mg/L)
20.23
LoD (mg/L)
1.24
LoQ (mg/L)
61.32
LoQ (mg/L)
3.74
R-squared Value
0.9997
Standard deviation
316.53
Slope P-value
1.74E-06
7.38.E-05
Significance F
1.74E-06
Percentage Recovery
Table A.1 Data for 200 1000 ppm Na+
200 1000 ppm K+ Calibration Range
STATISTICAL OUTPUT
STATISTICAL OUTPUT
R-squared Value
0.9992
Standard deviation
221.66
Slope P-value
9.91E-06
1.40E-05
Significance F
9.91E-06
95.2 %
Percentage Recovery
105.5 %
LoD (mg/L)
0.29
LoD (mg/L)
36.13
LoQ (mg/L)
0.88
LoQ (mg/L)
109.50
R-squared Value
0.9995
Standard deviation
8.84
Slope P-value
5.22E-06
1.45E-06
Significance F
5.22E-06
Percentage Recovery
Table A.4 Data for 200 1000 ppm K+
53
STATISTICAL OUTPUT
R-squared Value
0.9989
Standard deviation
106.26
Slope P-value
1.34E-05
1.05E-03
Significance F
1.34E-05
Percentage Recovery
97.1 %
LoD (mg/L)
4.00
LoQ (mg/L)
12.12
Table A.5 Data for 20 100 ppm K+.
STATISTICAL OUTPUT
R-squared Value
0.9999
Standard deviation
3.06
Slope P-value
5.30 E-07
1.42E-07
Significance F
5.30E-07
Percentage Recovery
101.8 %
LoD (mg/L)
0.14
LoQ (mg/L)
0.41
Table A.6 Data for 2 10 ppm K+.
54
SUMMARY OF STATISTICAL EVIDENCE AND SUPPORTING DATA OBTAINED FOR

EACH SET OF CONCENTRATION RANGE FOR DIB-FES ANALYSIS.
The following tables were the RGB values and statistical values obtained from the
treatment of given data from DIB-FES Analysis using MS Excel Functions. Residual
values were also obtained from the analysis of results.
200 - 1000 ppm Sr2+
Analysis of Green values
Quintuplicate Trials of RGB Values Analysis

100 ppm
R
G
B
Mean
252
56
60
251
57
60
255
50
60
255
54
60
254
55
62
80 ppm
R
G
B
Mean
255
48
66
255
43
65
255
45
67
255
42
62
253
45
59
60 ppm
R
G
B
254.60
44.60
63.80
Mean
252
35
62
254
36
63
255
36
58
254
36
62
255
37
62
40 ppm
R
G
B
253.40
54.40
60.40
254.00
36.00
61.40
Mean
251
25
65
253
28
65
247
27
62
254
24
62
253
30
59
20 ppm
251.60
26.80
62.60
Mean
R
G
177
20
179
17
153
18
151
18
166
17
165.20
18.00
75
77
74
71
75
74.40
Table A.7 RGB Values obtained from the Image analysis of standard solutions 200 to 1000 ppm
SrCl2.
55
20 - 100 ppm Sr2+
Analysis of Red Values

100 ppm
Mean
129
130
124
130
127
128.00
19
19
12
18
19
17.40
66
72
70
74
71
70.60
80 ppm
Mean
110
109
105
106
109
107.80
20
16
12
17
16
16.20
72
73
69
73
73
72.00
60 ppm
Mean
92
87
86
88
83
87.20
18
22
17
18
20
19.00
69
76
71
72
75
72.60
40 ppm
Mean
71
64
69
63
65
66.40
21
13
21
20
15
18.00
74
72
73
76
68
72.60
20 ppm
Mean
47
42
45
44
46
44.80
19
18
21
20
22
20.00
68
70
73
72
74
71.40
SrCl2.
56
200 1000 ppm Ba2+ Analysis
Analysis of Red Values

1000 ppm
Mean
146
147
145
147
142
146.25
137
138
132
133
132
135.00
120
121
113
122
120
119.00
800 ppm
Mean
134
134
135
132
132
113.75
120
122
117
116
116
118.75
109
106
107
101
103
105.75
600 ppm
Mean
125
123
121
123
121
123.00
112
113
114
112
111
112.75
104
111
108
110
109
108.25
400 ppm
Mean
110
111
108
115
113
111.0
95
96
94
99
99
96.00
90
90
94
99
99
93.25
200 ppm
Mean
98
98
98
101
101
98.75
85
85
82
85
85
84.25
86
99
96
101
95
95.50
BaCl2
57
20 100 ppm Sr2+ - Red values
200 - 1000 ppm Sr2+ - Green values

STATISTICAL OUTPUT
STATISTICAL OUTPUT
R-squared Value
0.9996
R-squared Value
0.9998
Standard deviation
0.34
Standard deviation
0.50
Slope P-Value
3.20E-06
Slope P-Value
8.16E-07
Slope intercept P-Value
1.28E-04
1.27E-04
Significance F
3.20E-06
Significance F
8.16E-07
Percentage Recovery
102.6 %
Percentage Recovery
105 %
LoD (mg/L)
24.80
LoD (mg/L)
1.57
LoQ (mg/L)
75.14
LoQ (mg/L)
4.76
Table A.10 Data for 200 1000 ppm Sr2+.
20 100 ppm Sr2+ - (Green +Red values)
200 1000 ppm Ba2+ - Red Values

STATISTICAL OUTPUT
STATISTICAL OUTPUT
R-squared Value
0.9993
R-squared Value
0.9995
Standard deviation
1.04
Standard deviation
0.50
Slope P-Value
8.30E-06
Slope P-Value
4.50E-06
2.74E-05
4.03E-07
Significance F
8.30E-06
Significance F
4.50E-06
Percentage Recovery
93.2 %
Percentage Recovery
92.5 %
LoD
3.41
LoD (mg/L)
27.76
LoQ
10.32
LoQ (mg/L)
84.11
Table A.12 Data for 200 1000 ppm Ba2+.
58
CALIBRATION CURVE OF VARIOUS SET OF CONCENTRATION RANGE

Concentration (mg/L) vs. Mean Intensity
8000
7000
y = 59.735x + 882.7
R = 0.9999
Mean Intensity
6000
5000
4000
3000
2000
1000
0
0
20
40
60
80
100
120
Figure A.1 Calibration curve of NaCl standard solution ranging from 20 ppm to 100 ppm.

70000
Mean Intensity
60000
y = 51.623x + 9810.3
R = 0.9997
50000
40000
30000
20000
10000
0
0
200
400
600
800
1000
1200
59

2500
Mean Intensity
2000
y = 99.95x + 1015.7
R = 0.9995
1500
1000
500
0
0
10
12

35000
y = 20.244x + 11980
R = 0.9992
30000
Mean Intensity
25000
20000
15000
10000
5000
0
0
200
400
600
800
1000
1200
Figure A.4 Calibration curve of KCl standard solution ranging from 200 ppm to 1000 ppm.
60

12000
10000
y = 87.685x + 1350.5
R = 0.999
Mean Intensity
8000
6000
4000
2000
0
0
20
40
60
80
100
120

1600
1400
y = 74.4x + 764.6
R = 0.9999
Mean Intensity
1200
1000
800
600
400
200
0
0
10
61
12
Concentration (mg/L) vs. Mean Green Values

60
Mean Green Values
50
40
y = 0.0453x + 8.78
R = 0.9996
30
20
10
0
0
200
400
600
800
1000
1200
Figure A.7 Calibration curve of SrCl2 standard solution vs. Mean Green Values ranging from
200 ppm to 1000 ppm.
Concentration (mg/L) vs. Mean Red Values
140
Mean Red Values
120
y = 1.039x + 24.5
R = 0.9998
100
80
60
40
20
0
0
20
40
60
80
100
120
Figure A.8 Calibration curve of SrCl2 standard solution vs. Mean Red values ranging from 20 ppm
to 100 ppm.
62
Concentration (mg/L) vs. Mean Red + Mean Green Values
Mean Red + Mean Green Values
160
140
120
y = 1.004x + 44.72
R = 0.9993
100
80
60
40
20
0
0
20
40
60
80
100
120
Figure A.9 Calibration curve of SrCl2 standard solution vs. Mean Red + Mean Green values
ranging from 20 ppm to 100 ppm.
Concentration (mg/L) vs Mean Red Values

160.00
140.00
y = 0.0589x + 87.225
R = 0.9995
Mean Red Values
120.00
100.00
80.00
60.00
40.00
20.00
0.00
0
200
400
600
800
1000
1200
Figure A.10 Calibration curve of SrCl2 standard solution vs. Mean Red + Mean Green values
ranging from 20 ppm to 100 ppm
63
APPENDIX B
Spreadsheet Functions
64
APPENDIX B
SPREADSHEET FUNCTIONS
Excel: Using the Linest Function

Trend lines are used to graphically display trends in data and to analyze
problems of prediction. Such analysis is also called regression analysis. Trend
line are useful but it does not give the error in the slope.
The Linest Function in Excel gives the error (or uncertainty) for data in the
lab. It calculates the statistics for a line by using the "least squares" method to
calculate a straight line that best fits your data, and returns an array that describes
the line. Because this function returns an array of values, it must be entered as an
array formula.
The Excel LINEST function returns statistical information on the line of best
fit, through a supplied set of x- and y- values.
The syntax of the Linest function is:
LINEST( known_y's, [known_x's], [const], [stats] )
Where the function arguments are listed in the table below:

known_y's
An array of known y-values.
[known_x's]
An optional argument, providing an array of one or more sets

of known x-values.
(If provided the [known_x's] array should have the same
length
as
65
theknown_y's
array;
If omitted, the [known_x's] array takes on the default value

{1, 2, 3, ...}).
[const]
An optional logical argument that determines how the

constant 'b' is treated in the equation y = m1x1 + m2x2 + ... +
b.
This argument can have the value TRUE or FALSE,
meaning:
TRUE
omitted)
(or
FALSE
[stats]
the constant
normally;
is
treated
the constant b is set to have the

value 0.
An optional logical argument which specifies whether or not

you want the function to return additional regression statistics
on the line of best fit.
This argument can have the value TRUE or FALSE,
meaning:
FALSE (or
omitted)
Do NOT return additional regression

statistics.
I.e. just return the array of values mn,
mn-1, ... , b.
TRUE
DO return
statistics.
additional
regression
I.e. Return the array of values mn, mn1, ... , b and also return the additional
regression statistics listed in the table
below.
Table B.1 Function arguments of Linest function
66
The array of statistics returned from the Excel Linest function has the following
form:
mn
mn-1
...
m1
sen
sen-1
...
se1
seb
r2
sey
df
ssreg
ssresid
Table B.2 Array of Statistics returned from Excel Linest
where the statistics returned are:

mi
The array of constant multipliers for the straight line

equation
The constant value of y when x=0
sei
The standard error values for the coefficients, mi
seb
The standard error value for the constant b

(returns the #N/A error if the [const] argument is
FALSE)
r2
The coefficient of determination
sey
The standard error for the y estimate
The F statistic, or the F-observed value
df
The number of degrees of freedom

67
ssreg
The regression sum of squares
ssresid
The residual sum of squares
Table B.3 Statistic returned by Linest Function
As the Linest function returns an array of values, it must be entered as

an array formula. If the function is not entered as an array formula, only the first 'm'
value in the calculated array of statistical information is returned.
Inputting an Array Formula
To input an array formula, you need to first highlight the range of cells for
the function result. Type your function into the first cell of the range, and press
CTRL-SHIFT-Enter.
Linest Function Example
Cells A2 - A10 and B2 - B10 of the spreadsheet below list a number of
known x and known y values, and also shows these points, plotted on a chart.
Cells D1 - E5 of the spreadsheet show the results of the Excel Linest function,
which has been used to return statistical information relating to the line of best fit
through these points.
As shown in the formula bar, the format of the Linest function is:
= LINEST( B2:B10, A2:A10, TRUE, TRUE )
68
Figure B.1 Example of a Linest Function in Excel
The curly brackets around this function show that it has been entered as an array
formula.
Cells D1 and E1 give the values of the slope, m as 1.88452381, and the yintercept, b as 2.419642857. Therefore, the equation for the line of best fit through
the given points is:
y = 1.88452381 x + 2.419642857
The remaining cells in the range D2 - E5 give the following additional statistics for
this curve:
The standard error value for the base m is 0.185347077
The standard error value for the constant b is 0.925189538
69
The coefficient of determination is 0.936582064
The standard error for the y estimate is 1.201186347
The F statistic is 103.3788683
The number of degrees of freedom is 7
The regression sum of squares is 149.1600595
The residual sum of squares is 10.09994048
Excel: Using the Analysis Toolpak to perform complex data analysis

The Analysis Tookpak Excel 2007 has a built-in regression analysis tool
thats packaged as part of its Analysis Toolpak. The Analysis Toolpak is a
standard component of Excel. Analysis Toolpak provides a complex statistical or
engineering analyses that saves steps and time.
If the Add-In is ALREADY Installed
If the Analysis Tookpak add-in is already installed, youll see an Analysis
group in the Data tab of Excels ribbon. Click the Data Analysis button in that
group to open the Data Analysis dialog. Then scroll down to find the Regression
option.
70
Figure B.2 Installed Analysis Toolpak in Excel 2007
If the Add-In is NOT ALREADY Installed

If youre using your own computer and you do not yet have the add-in
installed, follow these steps to install it:
1. Close Excel if you have it open.
2. Make your installation medium (probably a CD) available to your computer.
3. Restart the Excel installation routine. (Note that you need not reinstall Excel
entirely.)
4. Find the option to modify the installation and choose the Analysis Tookpak
as an add-in that should be activated.
5. Exit the installation process.
71
6. Open Excel and confirm that the Data Analysis dialog is available.
Steps to Follow When Running a Regression with Excel
1. Rearrange the Data as Necessary.
With Excels regression tool the independent X variables you use in your
analysis must be located together in the worksheet. There must be no blank
columns or columns with non-relevant data interrupting the range of X variables.
The dependent Y variable need not be located adjacent to the X variables, but all
Y variable values must be in a single range. These location specifications are
required by Excels built-in regression tool.
For the data in our sample, the data need not be rearranged. The X
variables are together in Columns F through K and the Y variable values are all in
Column E.
Figure B.3 Sample X and Y Data for Regression Analysis.
72
2. Open the Regression Analysis Tool.

In the Data tab on Excels ribbon find the Analysis group and click the
Data Analysis button.
Figure B.4 Location of Data Analysis button.
Excel opens its Data Analysis dialog. Scroll down and find the
Regression option. Click OK.
Figure B.5 Regression under Data Analysis dialog.
73
Excel 2007s Regression dialog displays. This is the sole interface to

Excels regression tool. All your interaction with Excels regression tool happens in
this dialog
Figure B.6 Sole interface of Refression Tool (Analysis Toolpak)
74
3. Complete the Regression Dialog Box.
Figure B.7 The X and Y Range for the Regression Analysis
- Specify Unit Sales as the Input Y Range. Include the column header cell (the
cell that holds the text Unit Sales) in your range specification.
- Specify the range of data in Columns F through K as the Input X Range. Include
only one row of column headers with your range specification (that is, include only
the labels directly above the data).
- In the Regression dialog box make sure the Labels box is checked. With this
option checked Excel will recognize that the first cell in each column of data is a
data label.
- Direct Excel to put its results on a new worksheet by choosing the option New
Worksheet Ply.
- For outputs, select Residuals, and Standardized Residuals.
75
With data ranges and choices specified, your dialog should now look like the one
below.
Figure B.8 Filled dialog box from the Regression Analysis function.
4. Run the Regression Analysis and View the Results.

With the dialog box options completed as described above, click OK to
execute the regression. The New Worksheet Ply default output option means that
Excel locates the regression outputs on a new, separate worksheet that it creates
and puts to the left of the worksheet that holds the original data.
76
Excel completes the regression analysis leaving a large range of the

worksheet selected. Click any cell to turn off the range selection. Because the
Regression tool generates many outputs on a single sheet, you may want to use
Excels Zoom Control option to reduce the new worksheet size in order to get a
view of how the outputs are arranged.
Figure B.9 Regression Analysis output
Widen the columns on the new worksheet in order to see all the text results
properly. A quick way to do this is to select the blank square at the intersection of
the row numbers and column headers (to select the entire worksheet), and then
double-click the dividing line between any two column headers. Excel widens each
column so the widest entry in that column displays completely.
77
The Regression Results Areas

Selecting the Residuals, and Standardized Residuals options in the
Regression dialog produces the output partially shown below.
In this view columns have been widened to show the results completely.
Figure B.10 Complete Image of Result from the Regression Analysis.
Excel labels the output areas SUMMARY OUTPUT, ANOVA, and RESIDUAL
OUTPUT.
Run another Regression Analysis

Perhaps after viewing the results of the first analysis you decide youd like
to run another regression analysis using different variables or a different
78
combination of variables. To do so, go through the same steps as above. Excel

adds a new worksheet to hold the new results. The original results (from the first
analysis) remain in place.
Calculation of Recovery Factor.

Recovery or Recovery Factor is the yield of a preconcentration or
extraction stage of an analytical process for an analyte divided by amount of
analyte in the original sample. Recovery Factor is calculated in order to evaluate
the accuracy and correction for bias a method development or method validation.
Figure B.11 Calculated Recovery Percentage from Synthetic Recovery test.
In the image shown above, the sample standard and the sample used was
the original standard solution included in the calibration range, the only difference
was that the intensity for the sample standard was obtained from the mean of all
its acquired intensity while the intensity of the sample was obtained from the
intensity of excess trials that were not included in the mean intensity of the sample.
Intensity of the spiked sample was also obtain from the excess trials.
79
The concentration of the sample standard, spiked sample and sample were
calculated using the linear regression equation that can be obtained from a
calibration plot. Recovered analyte is then obtained by subtracting the calculated
concentration of sample from the concentration of spiked sample.
Recovery factor can now be calculated using the following equation:
Figure B.12 Formula for the calculation of Recovery factor.
Where x(obs) is the observed/recovered value obtained from the analytical

process via calibration graph, and x(ref) is the reference value. In the example,
the concentration of the recovered value of the analyte was 384.09 ppm while the
reference value was 403.27 ppm (Rounded off 2 decimal places). Multiplication
of the acquired recovery factor by 100 % yields the Recovery percentage. A
recovery percentage of 100 % 10 % illustrates a considerable trueness of the
generated results.
80
APPENDIX C
Documentation
81
EXPERIMENTAL SETUP
Detector Setup
Air Compressor connected to the

air inlet of the Instrument
Actual Flame Analysis
The Fiber Optic Probe along with

the Spectrometer
82
GENERATED IMAGE OF FLAME FROM THE FES AND DIB-FES ANALYSIS

AND INTENSITY PEAK SIGNALS PROJECTED LIVE ON SCREEN
SrCl2 Flame
BaCl2 Flame (low concentration)
BaCl2 Flame (high concentration)

K+ Peak Intensity Reading
83
APPENDIX D
Budget Plan
84
APPENDIX D
BUDGET PLAN
Description
Propane-Butane
Tank
Price (Peso)
Mixed
Fuel
P 1,300
LPG Hose and Regulator with

P 300
Clamp
Printing
P 2000
Reagents/Chemicals
P 500
Transportation
P 200
Other
P 500
Total:
85
P 4,800
APPENDIX E
Gantt chart of Activities
86
APPENDIX E
GANTT CHART OF ACTIVITIES
Activities
1. Formulation
the topic
May
June
July
Aug.
of
2. Planning Period
3. Preparation for
the title defense
4. Title defense
5. Gathering
of
Materials,
Preparation for
Experimentation
Proper
6. Experimentation
7. Analysis of data
8. Preparation for
the final defense
9. Final defense
10. Revision of the
manuscript
11. Bookbinding
87
Sept.
Oct. Nov. Dec. Jan.
Feb. Mar.
APPENDIX F
Curriculum Vitae
88
LUIS BERNARD BRIOSO APLACADOR

Contact No.: +639086721149
Address: 376 F. Orrtigas Street, Mandaluyong City
Email address: luis_21_aplacador@yahoo.com
Personal Information
Date of Birth
June 21, 1996
Place of Birth
Mandaluyong City
Citizenship
Filipino
Gender
Male
Height
56
Educational Background
Tertiary:

Sta. Mesa, Manila
2012- Present
Secondary:
City of Mandaluyong Science High School
Mandaluyong City, Metro Manila

2008 2012
Primary:
San Felipe Neri Parochial School

Mandaluyong City
2002 - 2008
Training
On-The-Job Training:
United Laboratories Incorporated

United Street, City of Mandaluyong
April 2015 May 2015
89
NOEL ANGELO LAZARO AYANG

Contact No.: +639066758751
Address: #5 B Yakal St. Feria Rd., Old Balara, Quezon City
Email address: noelangelo29@gmail.com
Date of Birth
August 3, 1995
Place of Birth
Quezon City
Citizenship
Filipino
Gender
Male
Height
55
Tertiary:

Sta. Mesa, Manila
2012- Present
Secondary:
New Era High School

Tandang Sora, Quezon City
2008 2012
Primary:
Universal Evangelical Christian School

Diliman, Quezon City
2002 - 2008
Training
Silverstar Packaging Co. Inc.

Holy Spirit, Quezon City
April 2015 May 2015
90
JON JAY MULAT GARCIA

Contact No.: +639774194249
Address: Betina St., Sampaloc, City of Manila
Email address: yahiromutsuuji@gmail.com
Date of Birth
January 24, 1996
Place of Birth
Cebu City
Citizenship
Filipino
Gender
Male
Height
510
Tertiary:

Sta. Mesa, Manila
2012- Present
Secondary:
Ma. Therese Montessori School

Malolos, Bulacan
2008 2012
Primary:
Ma. Therese Montessori School

Malolos, Bulacan
2002 - 2008
Training
United Laboratories Incorporated

United Street, City of Mandaluyong
April 2015 May 2015
91

Ayang Aplacador Garcia Thesis Flame Emission Spectrometry

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Ayang Aplacador Garcia Thesis Flame Emission Spectrometry

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FABRICATION AND METHOD DEVELOPMENT FOR AN

IMPROVISED FLAME EMISSION SPECTROMETER FROM LOW

APLACADOR, LUIS BERNARD B.

2.1. Background of the Study ...... 6

4.2 FES Analysis ....... 32

The Electromagnetic Spectrum

A wave in an electric field

Seven Stages of an Analytical Method

The Solar Spectrum

Notable milestones in the development of FES

Temperature of flame generated from different sources in relation to

Diagram of a turbulent flow burner

A Perkin-Elmer design of a laminar flow burner

Flame spectrum of sodium

Flame spectrum of Calcium

Schematic Diagram of AAS

Schematic Diagram of the modified AAS for the fabrication of FES

Na+ FES Analysis

200 1000 ppm Na+

20 100 ppm Na+

200 1000 ppm K+

Sr2+ DIB-FES Analysis

200 1000 ppm Sr2+ (Green Values)

20 100 ppm Sr2+ (Red Values)

20 100 ppm Sr2+ (Red + Green Values)

Ba2+ DIB-FES Analysis 200 to 1000 ppm Ba2+

Statement of the Problem

Methods that will be involved in the fabrication of the improvised Flame

Efficiency and System linearity of the said instrument.

Reliability and Reproducibility of acquired results.

Objectives of the study

Scope and Limitation

signals live on screen. The fabrication of the instrument is limited in several

Significance of the study

applications. Most applications of FES have been the determination of trace

a.) Emission Spectroscopy involves the quantitative measurement of the optical

Chapter 2 - BACKGROUND AND REVIEW OF RELATED LITERATURE

based techniques commonly known as atomic spectroscopy, specifically on Flame

Review of Related Literature

2.2.1 Spectroscopy and the Electromagnetic Spectrum

Figure 1. The Electromagnetic Spectrum

Figure 2. A wave in an electric field

The wave characteristic of electromagnetic radiation is often elaborated

Equation 1. Relationship of Velocity to Wavelength and Frequency

In a vacuum, electromagnetic radiation travels at the speed of light c at

Equation 2. Relationship of Energy (photon) to Wavelength and Frequency

Equation 3. Relationship of Intensity to the no. of atoms in excited state.

Where k is a constant related to the efficiency of the transition. The

Equation 4. Boltzmann distribution equation.

In the case of absorption, a substance is subjected to a continuous range

Its figures of merit will then be tested and

improved up to its maturity, until it is receives general acceptance. Its fundamental

However, Hieftje (2000) wrote in his paper entitled Atomic Emission

Figure 4. The Solar Spectrum

Later works of R.W. Bunsen and G. Kirchhoff in 1859 to 1860 recognized

Developments in the late 1900s were focused on the improvement of the

Figure 7. Diagram of a turbulent flow burner

Figure 8. A Perkin-Elmer design of a laminar flow burner

Although FES was further developed through the utilization of the

Most elements give no conspicuous color to flames. If the valence electrons

Chapter 3 RESEARCH METHODOLOGY

Improvisation of Atomic Absorption Spectrophotometer to Flame

Figure 11. Schematic Diagram of AAS

Figure 11 and Figure 12 demonstrates the schematic diagram of the