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Low-Cost Spectrometer for Problem-Based Learning and Teaching

by Suntorn Suwannashom1 and Roongroje Ratana-ohpas2


1
Faculty of Science and Technology
Valaya Alongkorn Rajabhat University, Thailand,
E-mail: suntorns@gmail.com
2
Department of Chemistry, School of Science
Walailak University, Thailand,
E-mail: roongro@walailak.ac.th

Abstract

We describe here the design and construction of a lab-made spectrometer which is suitable for
problem-based learning and teaching in chemistry, chemical experiments, environmental laboratory,
and high school and undergraduate senior project. Using the inexpensive electronic components,
associated with the photo-sensitive resistor for photo- detector, scrap CDR for grating dispersing
device, home-used flash light bulb for light source, and the inexpensive compact digital mill-
voltmeter for display unit. The high sensitivity spectrometer was made with the cost less than ~9 US
$. The spectrometer with a wave length accuracy ~10 nm, 400-750 nm range, CDR grating ~550
grooves/mm, stray light ± 0.6 %T (0.0026 A) at 12 hours. After condition optimization for
determination of Fe2+ in water with 1,10- phenanthroline method, the lower detection limit was less
than 0.5 mg/L, the linear working range between 0.5 – 20 mg/L was found, R2 = 0.9985. This
spectrometer was used for analysis of iron(II) in ground waters both in field work and in the
laboratory. Furthermore, it was implemented to community and industry.

Introduction

Problem-based learning (PBL) is an approach that challenges students to learn through engagement
in a real problem. Its simultaneously develops both problem solving strategies and disciplinary
knowledge bases and skills by placing students in the active role of problem-solvers confronted with
an ill-structured situation that simulates the kind of problems they are likely to face as future
managers in complex organizations. Problem-based learning is student-centered and it makes a
fundamental shift from a focus on teaching to a focus on learning. The process is aimed at using the
power of authentic problem solving to engage students and enhance their learning and motivation.
Problem-based learning is the most important recent developments in the university education of the
professions (Boud and Feletti 1977). It started with medical education in North America and has
spread across the globe and across most disciplines. Its potential to develop student learning has not
been exploited in higher education (Savin-Baden 2000). Students report that problem–based learning
is fun (The Irish Times 2002). There are several unique aspects that define the PBL approach:
1. Learning takes place within the contexts of authentic tasks, issues, and problems that are aligned
with real-world concerns.
2. In a PBL course, students and the instructor become a co-learners, co-planners, co-producers, and
co-evaluators as they design, implement, and continually refine their curricula.
3. The PBL approach is grounded in solid academic research on learning and on the best practices
that promote it. This approach stimulates students to take responsibility for their own learning, since
there are few lectures, no structured sequence of assigned readings, and so on.
4. PBL is unique in that it fosters collaboration among students, stresses the development of problem
solving skills within the context of professional practice, promotes effective reasoning and self-
directed learning, and is aimed at increasing motivation for life-long learning.
The students, individually and collectively, assume major responsibility for their own learning and
instruction. Most of the learning occurs in small groups rather than in lectures. A teacher role changes
from a sage on stage to a guide by the side and is more like that of a facilitator and coach of student
learning, acting at times as a resource person, rather than as knowledge-holder and disseminator.
Similarly student role is more active and engaged as a problem-solver, decision-maker, and meaning-
maker, rather than being merely a passive listener and note-taker. However, this process differs from
the teacher dominated approach used in most science education of the developing country.
Using Problem Based Learning in chemistry or others applied science teaching technique needed
many expensive instruments for collecting an information and data. The research projects for design
and construction of simple and low cost instruments is the alternative choice for the developing
country to improve their science and technology teaching and learning activity.
The spectrometer plays an important role in collecting data and information and provides useful
information about structure, identity, and quantity of substances, low level pollutants in environmental
and chemical reaction.

The theory underlying the spectrometer

For chemical species that appear to have color, it is a logical assumption that the intensity of the color
is proportional to the concentration of the species in solution. We see color as a complement of the
visible wavelength that has been absorbed by the sample. Substances that appear red absorb blue
visible light and reflect other visible colors to our eyes. Conversely, the blue substances are absorbing
red light. The absorption of light or more precisely electromagnetic radiation is related to available
energy levels in the molecule or ion. A molecule in its ground state or lowest energy level can absorb
energy and jump to an excited state or higher energy state. The amount of energy and therefore the
wavelength of radiation involved in this transition is a function of the electronic structure of the
molecule or ion.
The eye can see only a limited range of electromagnetic radiation, approximately from 400 to 700
nm. However, molecules, atoms, and ions are capable to absorb many different radiation energy
ranging from ultraviolet (UV) to microwaves depend on the specific energy levels being excited. For
some types of energy changes, the wavelengths of light are very specific to the chemical structure
resulting in a method of qualitatively identifying chemical species. Other types of energy absorption
may be less qualitative since it may relate only to bond types. In both cases however, our initial
premise that intensity of absorption is related to concentration can be used for quantitative analysis.
Since our vision if not quantitatively calibrated, an electronic instrument called a spectrometer is used
to precisely measure light intensities at given energy (wavelength) settings. A spectrometer is an
instrument that measures the amount of transmission of light through a substance. A simple
spectrometer system consisting of a light (energy) source, monochromator to select a given energy
range, sample holder, and light intensity detector.
Spectrometer is the instrument used to study the interaction of light or electromagnetic radiation with
matter. It is an important and versatile tool for chemist, environmental and applied technologist, much
of the information of chemical substances comes from their specific absorption or emission of light.
In analytical aspects the amount of light absorbed (or transmitted) as it passes through a solution is
related to its concentration. As we look at two solutions of the same substance, one is deeper color
than the other. The common sense tells us that the darker colored one is the more concentrated. As a
color of solution deepens mean that its concentration also increases. The principle of spectrometer is
the measurement of the correlation of color intensity and amount of a material in solution. Every
substances can absorbs or transmits certain wavelengths of radiant energy. Light energy absorbed or
transmitted must match exactly the energy required to cause an electronic transition, a movement of
an electron from one quantum level to another in the substance under consideration. Only certain
wavelength of photons satisfies this energy condition. Thus, the absorption or transmission of specific
wavelengths is a characteristic of substance, and a spectral analysis serves as a fingerprint of the
compound. In recent years spectrophotometric method become the most frequently used and
important methods of quantitative analysis. They are applied to many industrial, environmental and
clinical problems involving the quantitative determination of compounds or substances that are
colored or that react to form a colored product.
When light is absorbed by a sample, the radiant power or intensity of the light beam decreases.
Radiant power, I, refers to the energy per second per unit area of the beam. In the Figure1 light passes
through a monochromator that selects one wavelength. Light of this wavelength, with radiant power
I0, passes through a sample of path length b. The radiant power of the beam emerging from the other
side of the sample is I.

Figure 1: Monochromatic light absorbed by solution

Mathematically, the amount of light that is absorbed (A) is given by

I
T=
I0
I
%T = × 100
I0
I 
A = log 0 
 I 
1
A = log 
T
A = 2 − log%T

Note that if no light is absorbed, A = 0 and if all the light is absorbed (I = 0) then A = ∝. The amount
of light absorbed by the sample should be proportional to the probability that the molecule or ion will
absorb the electromagnetic radiation (a), the number of absorbing molecules or ions per unit volume
that the light beam passes through (C), and the length of the light path (b). This relationship is
quantified in the Beer-Lambert (or Beer's) Law which is

A=a×b×C

A= ε ×b× C

Note that this equation is in the form of Y = m × X + b where the intercept, b, is zero when X or the
concentration, C, is zero. If we measure a series of solutions of known C at a given wavelength in a
cuvet or sample cell with a constant path length, b, then we can determine the proportionality
constant, m, which is a × b. This procedure generates a "calibration curve" which allows the
determination of an unknown concentration, Cunk, from the measurement of the absorbance of the
unknown, Aunk. Determination of the slope, m, and intercept, b, of the calibration curve gives

A unk − b
C unk =
m
If the same compound is being used and the path length is kept constant, then the absorbance is
directly proportional to the concentration of the sample.
Instrumentation

The general spectrometer is composed of five main parts:- (see Figure2.)


- light source
- monochromator
- absorption cell
- detector
- readout

Figure 2: The basic components of spectrometer

1. Light source
A light source for spectrometer should have a wavelength from 400 – 800 nm in visible spectrometer,
made of tungsten lamp or halogen lamp and 190 – 340 nm in UV-region made of mercury lamp.

2. Monochromator
A monochromator is an optical device that transmits a mechanically selectable narrow band
wavelengths or single wavelength of light from light source. A device that can produce
monochromatic light has widely uses in science and optics because of many optical characteristics of
material are dependent on color. Although there are a number of useful ways to produce pure colors,
there are not so many ways to easily select any pure color in wide range.

3. Absorption cell
An absorption cell or sample cell is used to contain the sample solution. It made of quartz,
borosilicate or plastic and did not absorb the UV or visible light. There are two type of absorption cell,
normal absorption cell and flow cell. Both of the cell are rectangular shape with 1x1x4 centimeter in
size but the flow cell have filling hold for continuous flow of sample solution. The tubing shape is
rarely used in laboratory except some in school laboratory.

4. Detector
A detector is an electronics device used for measurement the light intensity which transmitted from
sample cell. A good detector should be sensitive all type of working wavelength of radiation.

5. Readout unit
The old design spectrometer used analog milliamp meter for readout unit and recalibrated the scale to
%T and Absorbance (A). The modern spectrometer used an analog to digital converter integrated
circuit (IC) and microprocessor for data processing so its can display the result in %T, Absorbance,
concentration mode selectable.

Design concept

The simple spectrometer is made of a used data CD/ or DVD storage for grating or a dispersing
device, the inexpensive electronic components, associated with commercial photo-sensitive resistor
(LDR) for photo-detector, home-used flash light bulb for light source, and the inexpensive compact
digital milli-voltmeter for display unit. The circuit diagram of a simple spectrometer is shown in
Figure3.

Figure 3: The circuit diagram of a simple spectrometer

Construction

A simple spectrometer is made of home used material, common electronics components, plastics box,
PVC tube, flash light bulb. Most of components can purchase from an electronics shop or grocery
store. A simple spectrometer was made by modify a plastics box for components attachment following
the diagram in Figure4 and isometric drawing in Figure5. The cell holder was made by a PVC tube
and attached a photo resistor on the opposite of the other site, the entrance slit. The lamp box is made
of aluminum and compact size digital mill volts meter for readout. The power supply was connected
to the light source and mill volt meter with variable resistor for 100%T adjustment.

Figure 4: A diagrammatic design of the simple spectrometer


Figure 5: Isometric drawing diagram of a simple spectrometer

Calibration

The wavelength calibration procedure can be made by switch on the instrument and put a white paper
strip in a cell holder compartment. Turn a wavelength control knob until the red light appear, mark the
wavelength control for ~650 nm and turn the wavelength control knob in the other direction until the
violet light is appear on the paper strip and mark on the wavelength control for ~400 nm. The next
step is dividing the wavelength scale from 400 to 650 nm by 20 nm incremented. The wavelength of
the simple spectrometer is re-checking with standard Fe(II)-phenanthroline complex and adjusts scale
for 510 nm.

Reagents

1. Fe2+(II)1,000 mg/L stock solution


2. hydroxylamine hydrochloride solution
3. DI water
4. conc. H2SO4
5. 1,10-phenanthroline solution

Procedure

An iron (II), Fe2+, exhibits pale orange color in solution. When Fe2+ reacts with the ligand of o-
phenanthroline (or 1,10-phenathroline), a stable, intense red colored complex is formed and can be
used to determine the quantity of iron in sample solution. The intensity of the color varies over the pH
range of 2 to 9, an ammonium acetate buffer can be used to control the pH between 6 and 9.
The evaluating procedure of a simple spectrometer is conducted on the determination of iron(II) in
freshwater by from complex with 1,10-phenanthroline solution. The maximum absorption of the
iron(II) complex is 510 nm. There are two procedure step:-

1. Determination of maximum absorption wavelength (λmax)

The spectrometer is more sensitive to absorbance changes at this wavelength. The procedure begin by rinse
a clean cuvette with 2-3 mL of DI water and then fill the cuvette to about 2/3 of cell with DI water. Rinse
another cuvette with 2-3 mL of the most concentrated iron standard, refill to about 2/3 cell with the iron-
phenanthroline standard. Calibrate the Spectrometer at 400 nm using the blank. Measure the absorbance of
the iron-phenanthroline standard at 400 nm. Repeat the calibration and measurement of the iron-
phenanthroline standard for wavelengths from 420 to 650 nm at 20 nm increments.
Determine the maximum absorption wavelength (λmax ) of orange-red [Fe(o-Phen)3]2+ ions. This
wavelength will be use for measuring the absorbance of the standards and sample solutions.

2. Preparation of Standards Curve

All measurement is a comparative process. To calibrate an instrument, one needs to measure one or
more reference materials. A series of standard Fe2+ solution is needed for calibration.
2.1. Prepare a stock Fe2+ solution by accurately weighing to the nearest 0.0001 g Fe2+
approximately 0.0700 g of pure iron (II) ammonium sulfate hexahydrate and quantitatively
transferring to a 1 L volumetric flask.
2.2. Add 200 mL water and shake to dissolve any remaining solid.
2.3. Add 5 mL of 1:1 sulfuric acid.
2.4. Dilute to the mark with distilled water and homogenize thoroughly.
2.5. Calculate the concentration of the solution in mg Fe2+/L.
2.6. Prepare a series of standards by pipeting into each of five 100 mL volumetric flasks, 1.00,
5.00, 10.00, 25.00, and 50.00 mL aliquots of the stock Fe2+ solution
2.7. Into a sixth 100 mL volumetric flask pipet 50 mL of distilled water to serve as a blank.
2.8. To all of the solutions add, in sequence
1 mL of hydroxylamine hydrochloride solution,
10 mL of 1,10-phenanthroline, and
8 mL of sodium acetate buffer.
2.9. Dilute to the mark, mix thoroughly, and allow standing for 10 minutes.
2.10 Set the wavelength to 510 nm, set 100%T by insert a cuvette with DI water in the sample
holder and adjust to 100%T reading and transfer a series of standard solution in to cuvette and
measure the %T, calculated the absorbance from the previous equation and plot Fe2+ concentration vs.
absorbance

3. Determination of Fe2+ in water sample:


In order to obtain an accurate results the concentration of Fe2+ in water sample should be in a
concentration range of a standard curve, otherwise it will be necessary to do a serial dilution if the
concentration is out of standard curve range.
1. Quantitatively transfer 100 mL of water sample in to the 100 mL volumetric flask.
2. Add 5 mL of 1:1 H2SO4 and mix well.
3. Dilute to the mark and mix thoroughly
4. Pipette a 10.00 mL aliquot into a 100 mL volumetric flask.
5. Dilute to the mark and mix thoroughly
Finally prepare the actual sample for analysis.
1. Take a 20 mL aliquot of this second solution and place it in a 100 mL volumetric flask.
2. Treat this as you did your standards by adding
1 mL of the hydroxylamine solution,
10 mL of the 1,10-phenanthroline solution, and
8 mL of sodium acetate.
3. Dilute to the mark, mix thoroughly and allow standing for 10 minutes.

Results

The test result of the instrument absorbance drift ~ 0.002A/12 h


The linear measurement of standard Fe2+ in water solution by lab-made spectrometer is shown
in table 1 and Figure6 is the linear plot by Microsoft Excel, its correlation coefficient (r2 = 0.9985),
The result of iron in ground water sample by lab-made spectrometer at Valaya Alongkorn Rajabhat
University main campus, Patumthani, Thailand is 6.502+/- 0.2431 mg/L (see table 2 for detail)

Table 1 Standards curve of Fe2+ solution

Fe(II) conc. %T Absorbance


(mg/L)
0.000 100.00 0.00
0.5 94.00 0.03
1.0 89.00 0.05
5.0 63.10 0.20
10.0 42.70 0.37
15.0 29.80 0.53
20.0 20.80 0.68

Table 2 Determination of Fe2+ in fresh water sample


Repeat no. %T Absorbance Fe(II) conc. (mg/L)
1 71.5 0.156 4.018
2 72.3 0.141 3.570
3 71.9 0.143 3.630
average 71.9 0.147 3.374
S.D. 0.4 0.0081 0.2431
%RSD - 5.553 6.502

Figure 6: Standard curve for iron(II) 1,10-phenanthroline complex


Conclusion

The simple spectrometer made of the inexpensive components is easy to construction, have a good
precision and accuracy, suitable for used in class room, environmental monitoring and basic
experiments in chemistry, environment and other applied science. And the advantage of this
instrument is its simple design and easy to assembly and calibration procedure and suitable for
science projects and PBL teaching strategies (see Figure7.).

Figure 7: The photo of simple spectrometer


Acknowledgements

I was grateful to Dr Roongroje Ratana-ohpas for revisions to the first manuscript; Mr Robert James
Santos for clearly providing information of theory and practical PBL; the Chemistry Programme,
School of Science, Walailak University and Faculty of Science, Valaya Alongkorn Rajabhat
University for supported chemical, equipment and facilities.

References

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2. Ivo M. Raimundo, Jr. and Celio Pasquini., Journal of Automatic Chemistry, Vol. 15, No. 6
(November-December 1993), pp. 227-232
3. The Irish Times (2002, April 23rd). Education and Living. 15.
4. Savin-Baden, M. (2000). Problem-based Learning in Higher Education: Untold Stories.
Buckingham:
SRHE and Open University.
5. Boud, D. and G. Feletti (1977). Changing-problem learning. Introduction to the Second
Edition.
In D. Boud and G. Feletti (Eds.), The Challenge of Problem-based learning. London:
Kogan Page.