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Build your own

spectrophotometer
For many students the spectrophotometer has become a black box into which a sample is
placed, and from which the analytical data appear. By designing and building their own
visible-light spectrophotometers, students get to grips with the underlying principles
of this widely used analytical tool.
Stewart J. Tavener and Jane E. Thomas-Oates

Whats inside the black box?

Spectroscopy is widely taught processes that lead to the In short the intimate workings of this
at A-level and at undergraduate level measurement. Indeed, when we Take a 100W light
analytical instrument at a cost that
and, as scientific instruments asked a class of first-year bulb, a light- compares favourably with
british antarctic survey/science photo library

become more affordable yet more undergraduates who had recently dependent resistor, a conventional synthetic chemistry
sensitive and complex in their used a UVVIS spectrophotometer prism or grating in experiments. Not only do students
workings, it is increasingly important to explain its internal workings, only front of a slit, and a learn about the key components of
for students to understand their one out of 20 showed a clear curtain and voil, a the equipment, but they also gain
underlying principles. Most understanding. DIY spectrophotometer experience of calibrating the
spectrophotometers in the teaching To overcome this problem we have instrument and an understanding of
laboratory are driven by a PC, which developed a project that allows the relationships between the
controls the operations, stores files students to design and build their absorption of light and
and manipulates the data, leaving own visible-light spectrophotometer, concentration, and between
students divorced from the physical giving them hands-on experience of resolution and sensitivity. While
September 2007 | Education in Chemistry | 151
1 Fig 1 the experiments described in this
(a) Layout for article were designed for
circuit board for undergraduates, they can also be
the photometer; adapted for A-level and GCSE
and (b) trace for projects. (A summer camp of 1316-
photo-etching the year olds enthusiastically built
circuit board. (For photometers with a high degree of
further information success.)
on etching circuit The full undergraduate practical is
boards see ref 1.) run over two days, the first task being
to build a simple photometer. If time
is limited, this can be used as a stand-
alone exercise. In the second part of
the practical the students design and
construct a spectrophotometer and
use it to measure the visible
spectrum of a solution of potassium
manganate(vii).

Building the photometer


In our classes, we supply a printed
circuit board and teach the students to
solder, an important skill for anyone
who regularly deals with scientific
equipment. Alternatively, a board may
be etched and drilled (a layout is
shown in Fig 1),1 or the circuit may be
built on plug-board, which may be
more suitable for schools since many
science departments will already have
2
these, and the components can be
reused.
+9V  Fig 2 The photometer consists of a light
R4 Photometer circuit source (an LED), a light-dependent
R1
2k2
1k0 diagram. The resistor (LDR) as a detector and a
+
sample is placed simple amplifier/buffer circuit to
R3 4k7
between the LED make the output suitable to drive a
LED +9V and LDR. The voltmeter. (If a high impedence
LDR 2_ 7 6
output is multimeter is used, the amplifier
 connected to the could be omitted, but it does illustrate
+ Output
0V 3 4 voltmeter an important component of a real
   Op amp
+ photometer.) The LED and LDR face
Fig 3 one another and the sample cuvette is
9V
0V The photometer, placed between them. The resistance
showing LED, LDR, of the LDR decreases as the amount of
amplifier and light that falls on the LDR increases:
sample cuvette more light lets more current flow. The
circuit runs on two 9V batteries. To
3 avoid errors caused by stray light from
LED the room, the photometer must be
placed in a box. Figures 2 and 3 show a
photometer circuit diagram and a
photograph of the completed
photometer respectively. Components
P1, P2 and P3 are generally omitted
but may be used to replace the fixed
resistors with potentiometers, thus
allowing control over the light
intensity, and gain and offset of the
Cuvette Op amp amplifier circuit. (These could be
exploited for an extended project.)
LDR Experimental
The relationships between absorbed
and transmitted light, and between

152 | Education in Chemistry | September 2007


Parts list
Photometer work better than prisms.)
Printed circuit board (1.90 each for a run Lenses
of 104), plug-board, or photoresist board Optical bench or stands and clamps; black
Voltmeter or digital multimeter cloth
Plastic or glass cuvettes Resistors: 4.7k (0.02); 2.2k (0.02);
Total cost for photometer consumables is 1.0k (0.02)
under 4.00 LED: orange, 5mm (0.20)
Spectrophotometer LDR (0.57)
White light source Op amp: 3140 (0.65)
Diffraction grating, prisms or coloured Socket: eight-pin (0.09)
filters. (Note: gratings are available at Battery clips (0.26)
modest cost ( see, for example, Soldering iron, solder,
http: www.patonhawksley.co.uk) and Blu-Tack, tape and card

concentration and absorbance, may information as a voltage. This is true may be set to zero manually, which
be explored with the photometer. of commercial instruments, though simplifies the maths.
However, the photometer must first these contain an internal processor to The absorbance is calculated by
be calibrated using standard do the necessary mathematics. combining equations (i) and (ii) into
concentrations of a suitable coloured However, the conversion is Fig 4 (iii). After calibration, using a set of
chemical. We have used potassium straightforward and can readily be Calibration plot of standard solutions to determine ,
manganate(vii), cobalt salts, done with a calculator or absorbance versus measurement of A allows the
molybdenum blue (sodium spreadsheet. concentration for concentration of unknown solutions
molybdate(vi), crystal violet As well as absorption by the solutions of KMnO4 to be determined.
(hexamethylpararosaniline chloride) compound, other processes reduce (student data)
A = log10((Vsample Vzero)/(Vsolvent Vzero))
and food colourings, though it may the intensity of light that passes
= cl (iii)
be necessary to change the colour of through the cuvette, so it is essential Fig 5
the LED to improve the sensitivity. to take a background reading for the The DIY Figure 4 shows a student calibration
All compounds absorb some of the solvent and the cell, which spectrophotometer. plot of concentration against the
light that falls upon them, the energy corresponds to Io. Do not assume The lens forms an voltage ratio. The completed
from the radiation being used to that the circuit sends out 0V when image of the photometers have proved suitable for
excite electrons to higher energy no light falls on the detector, and aperture at the monitoring kinetics of reactions that
levels. The absorbance, A, of a make the correction by subtracting plane of the slit involve a colour change, eg
solution of the compound at a the voltage at zero light (Vzero) from
particular wavelength is described by all readings. These two procedures 4
the BeerLambert law (i), which is zero the photometer. Over the range 0.08 Absorbance
widely used in quantitative analysis. of wavelengths and light intensities in
which we are interested, the
0.07 
A = log10(I / Io) = cl (i) 0.06
photometer exhibits a linear 
The absorbance is directly related relationship between incident light 0.05
to the concentration, c, of the and the voltage ratio described in 0.04 
compound, the pathlength of the equation (ii). (This assumption holds 
sample, l, and the molar absorption true for useful concentration ranges, 0.03
coefficient, , a wavelength- and the calibration plot will let the 0.02

dependent constant characteristic of user know if they have entered a 
0.01 
the compound. Io is the incident light region of non-linear behaviour.)
intensity and I, the transmitted light
I/I0 = Isample/Isolvent
0 
intensity. 0 1.0 2.0 3.0 4.0 5.0
= (Vsample Vzero)/(Vsolvent Vzero) (ii) Concentration/104moldm3
Rather than measuring absorbance
directly, the photometer gives Some older needle-type voltmeters

Aperture 5
Lens
Grating Slit
CC STUDIO/SCIENCE PHOTO LIBRARY

Amplifer
_
+
V
Detector
Lamp
Sample Meter

September 2007 | Education in Chemistry | 153


Table 1 Typical perceived colours and correct way of assembling a 6
wavelengths of visible light.2 (The spectrophotometer, and we find that 0.6 Absorbance Key
perceived colours vary between students often have ideas that we  Commerical
spectrophotometer
individuals, especially at the boundary have not anticipated. A simple 0.5
   DIY spectrophotometer
wavelengths.) instrument can be created by using
Colour Wavelength Wavelength
coloured filters in place of the 0.4 
centre/nm range/nm
gratinglensslit assembly, though  
the number of data points is limited 
0.3
Violet 410 400430 to the number of available filter  
Blue 470 430490 colours.  
0.2 
Green 520 490570 
A valuable experience
Yellow 580 570595
This hands-on, discovery-based 0.1 
Orange 610 595650
learning encourages ingenuity and
 
Red 650 650700
creativity, and gives the students a 0
real sense of achievement. If 450 500 550 600 650 700
measuring the rate of bleaching constructed with care and ambient Wavelength/nm
crystal violet in the presence of light is excluded effectively, the
sodium hydroxide. photometer is sufficiently precise to
make measurements that are Fig 6 commercial instruments at a fraction
The spectrophotometer comparable with the students Visible region of the cost (Fig 6). We have found
In addition to a light source (100W abilities to make up calibration spectrum of that the learning outcomes are worth
light bulb or other polychromatic solutions. It is certainly good enough KMnO4 from a the work after running the
sources) and detector, a to measure unknown concentrations commercial experiment, all the students
spectrophotometer also requires a and the rates of simple reactions to spectrophotometer understood the BeerLambert law
prism or grating* to obtain different within a few per cent. and data points and how a spectrophotometer works.
wavelengths from the light source, Building the spectrophotometer is measured using
and a slit to select a narrow range of challenging and we deliberately avoid the DIY Acknowledgements: we thank Ed T.
wavelengths. The latter determines giving explicit instructions, though spectrophotometer Bergstrm and Laura Karran for their help in
the resolution of the instrument. some students require more developing this experiment.
There is, however, an inherent guidance than others depending on
compromise between sensitivity and their ability, confidence and Dr Stewart Tavener is a research fellow, and
resolution a narrower slit gives experience. The process of trial and Jane Thomas-Oates is professor of analytical
better resolution, but fewer photons error ensures that every component science in the department of chemistry at the
with which to make the is explored and its purpose University of York, Heslington, York YO10 5DD.
measurement. The slit may be made understood. The ability to resolve the
carefully from card, and placed either spectrum is limited by how widely References
between grating and sample, or the light source is diffracted, and Molecular 1. See, for example, http://www.technologystudent.
between sample and detector. though the fine structure of the spectroscopy com/pcb/pcbdex.htm
2. Data from various sources, including D.A. Skoog, D. M.
Figure 5 shows a typical layout of a KMnO4 spectrum cannot be shedding light on West, F. J. Holler and S. R. Crouch, Fundamentals of
DIY spectrophotometer, where the resolved, the spectra obtained chemical analytical chemistry (8th edn). Belmont, US: Brooks/Cole-
spectrum produced by the grating is broadly resemble those from composition Thomson Learning, 2004.
projected onto graph paper to
produce a scale of wavelength. The
grating may be rotated, or the slit and
sample moved, to select different
wavelengths of light. Calibration of
the wavelength is performed by eye,
using the numbers in Table 1 as a
guide.
To construct a spectrum, the
absorbance must be calculated for
each wavelength, and therefore Vzero,
Vwater and Vsample must be measured
at each point. Ambient light
interferes with the
spectrophotometer and causes
PHANTATOMIX/SCIENCE PHOTO LIBRARY

inaccuracies, and so either large


cardboard boxes, or thick blackout
curtains draped between two or
three retort stands, are used to keep
out light. The latter is preferable
because the students can work under
the material. There is no single

154 | Education in Chemistry | September 2007

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