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A portable, inexpensive and microcontrolled spectrophotometer based

A portable, inexpensive and microcontrolled spectrophotometer based

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Talanta 77 (2009) 1155–1159
Contents lists available atScienceDirect
A portable, inexpensive and microcontrolled spectrophotometer basedon white LED as light source and CD media as diffraction grid
Germano Veras
, Edvan Cirino Silva
, Wellington Silva Lyra
,Sófacles Figueredo Carreiro Soares
, Thiago Brito Guerreiro
,Sérgio Ricardo Bezerra Santos
Universidade Federal da Paraíba, Departamento de Química, 58.051-970, João Pessoa, PB, Brazil
Universidade Estadual da Paraíba, Departamento de Química, 58.109-753, Campina Grande, PB, Brazil
Centro Federal de Educac¸ão Tecnológica da Paraíba, 58.015-430, João Pessoa, PB, Brazil
a r t i c l e i n f o
 Article history:
Received 17 April 2008Received in revised form 18 August 2008Accepted 19 August 2008Available online 27 August 2008
White LEDCD mediaProgrammable interrupt controller (PIC)microcontrollerVisible spectrophotometerFood colorantsIron (II)
a b s t r a c t
A portable, microcontrolled and low-cost spectrophotometer (MLCS) is proposed. The instrument com-bines the use of a compact disc (CD) media as diffraction grid and white light-emitting diode (LED) asradiation source. Moreover, it employs a phototransistor with spectral sensitivity in visible region asphototransductor, as well as a programmable interrupt controller (PIC) microcontroller as control unit.The proposed instrument was successfully applied to determination of food colorants (tartrazine, sun-set yellow, brilliant blue and allura red) in five synthetics samples and Fe
in six samples of restorativeoral solutions. For comparison purpose, two commercial spectrophotometers (HP and Micronal) wereemployed. The application of the
-paired test at the 95% confidence level revealed that there are not sig-nificant differences between the concentration values estimated by the three instruments. Furthermore,a good precision in the analyte concentrations was obtained by using MLCS. The overall relative standarddeviation(R.S.D.)ofeachanalytewassmallerthan1.0%.Therefore,theproposedinstrumentoffersaneco-nomically viable alternative for spectrophotometric chemical analysis in small routine, research and/orteaching laboratories, because its components are inexpensive and of easy acquisition.Published by Elsevier B.V.
1. Introduction
Since the seventies of the last century, when researchers asFlaschka et al.[1]developed photometers based on light-emitting diode(LED),LEDshavebeenappliedonspectrophotometricinstru-mentation as radiation sources having relatively small effectivebandwidth[2,3].However, the increasing demand for chemical analyses makes necessary to develop LED-based instruments towork in a wide range of wavelengths what requires multipleradiation sources. The approach increases cost and complexityof the optical and electronic system. For example, optical fibersare usually employed to direct the radiation towards the detectorand a more elaborated hardware is necessary to control the LEDdrift.Nowadays, it is easy to acquire white LEDs that substitutesthe complex optical system obtained when monochromatic LEDsare used as sources of several wavelengths in the visible region.
Corresponding author.
E-mail address:
edvan@quimica.ufpb.br(E.C. Silva).
Therefore, it is possible to develop simple spectrophotometersusing a single white LED with an adequate disperser of thewhite light. For this purpose, the literature reports two worksonly that employ white LED as radiation source[4,5].Shimazaki et al.[4]were pioneers in the development of a white LED-based spectrophotometer which was used in determination of Fe
in river water by the
-phenantroline method. Li et al.[5]described a portable multi-function instrument using differentspectrophotometric techniques. As application, the spectropho-tometric determination of Cr
and Al
was carried out usingdiphenylcarbazide and pyrocatechol violet as chelant and chro-mogenic reagents, respectively.Commercial spectrophotometric instrumentation commonlyemploysabsorptionorinterferenceopticalfilters,prismsordiffrac-tiongridsasradiationdispersers.Inmostoftheseinstruments,thedispersive device is a diffraction grid, an optical component con-tainingseriesofgroovestracedonaglassplateorpolishedmetal.Inthiscontext,acompactdisc(CD)mediacouldbeusedasdiffractiongridduetoitsgrooves.DespitetheuseofCDmediaasradiationdis-perser[6],no application in spectrophotometric instrumentation has been found.
0039-9140/$ – see front matter. Published by Elsevier B.V.doi:10.1016/j.talanta.2008.08.014
G. Veras et al. / Talanta 77 (2009) 1155–1159
In the present work, a portable, microcontrolled and low-cost spectrophotometer (MLCS) having a white LED as radiationsource and a CD media as diffraction grid for measurementsusing the visible region was developed. In order to increase thesignal-to-noise ratio in the spectrophotometric measurements, aphototransistor with maximum spectral sensitivity in the visibleregion was used. In the MLCS, pulsed radiation from the whiteLED is dispersed by the CD media generating monochromaticradiation that is focalized in the phototransistor by a steppermotor. The control of the proposed instrument, the acquisitionand treatment of data are accomplished by an electronic circuitbased on a programmable interrupt controller (PIC) microcon-troller. Two analytical applications were elected to illustrate theperformance of the MLCS. The first is represented by individualdeterminations of four food colorants (tartrazine, brilliant blue,allura red and sunset yellow). The second concerns to the deter-mination of Fe
in restoratives by using the 1,10-phenantrolinemethod.
2. Experimental
 2.1. Reagents, solutions and samples
Food colorants tartrazine (E-102), sunset yellow (E-110), allurared (E-129), and brilliant blue (E-133) were purchased fromSigma–Aldrich. Stock solutions of 1000mgL
of each colorantwereprepareddissolvingitsnecessaryamountinphosphatebuffer
Fig. 1.
Schematic diagram illustrating the optical system of the MLCS.
solution at pH 7.00. Standard solutions of synthetic samples of each colorant were prepared by the appropriated dilution of therespective stock solution. The standard solutions were prepared inauthentic triplicates at the concentrations 2.0, 4.0, 6.0, 8.0, 10.0,12.0, 14.0, 16.0, 18.0, 22.0, and 26.0mgL
O was used to prepare stock solutions of Fe
. Working solutions (Fe
) were pre-pared from the stock solution after reduction of the Fe
usingascorbic acid 1.0% (w/v). Six samples of restorative oral solu-tions (containing Fe
) from different marks were acquired indrugstores at João Pessoa city, Brazil. These pharmaceutical for-
Fig. 2.
Electronic layout of the MCLS detector. Legend: PT=phototransistor; C=polyethylene capacitors; R=resistors; U1=operational amplifier; U2=quadruple operationalamplifier; U3=quadruple switches. Details in text.
G. Veras et al. / Talanta 77 (2009) 1155–1159
mulations were diluted to fit in the linear range of the analyticalcurve.Recently distilled water was used to prepare all solutions.
 2.2. Description of the proposed instrument 
Fig. 1illustrates the optical components employed in the MLCSandFig. 2,the electronic layout of the detection unit. This instru- mentwasassembledintoaboxwith30cmfront,20cmheightand30cmlength.Theoptical–mechanicalsystemiscomposedbywhiteLED, focus lens to create a small light image (2mm diameter) onthe diffraction grid (CD) and stepper motor with gear to move thediffraction grid and to promote the scan of the spectral region of interest.Toincreasethespectralresolution,thepositionofthestep-per motor was adjusted so that the phototransistor can detect theradiation from the second overtone.The instrument uses a PIC 16F877 programmable microcon-troller as control unit driven by a stabilized power supply. Thecontrol software was elaborated with C language. The microcon-troller presents a 10-bit multi-channel analog to digital converter(A/D), 8k
14 words of flash program memory, 256
8 bytes of EEPROM data memory, 368
8 bytes of RAM, three timers andthree ports with eight channels (multiplexed pins) each, for gen-eral purpose, that can be configured for data acquisition. Themicrocontroller allows drastic reduction of the number of elec-tronic components in the spectrophotometer and makes possibleto introduce or alter functionalities in the instrument without anyhardware modification.The white LED Control Module pulses the white LED radiationat7Hz.ThemoduleturnsthewhiteLEDonforreadingsoftheana-lytical signals and off for determination of instrumental noise. Thesignalsaredetected,filteredandamplifiedintheDetectionModuleoftheMLCS,showedinFig.2.Inthelayout,fiveoperationalampli- fiers are used for different purposes: to convert the photocurrentintovoltage(U1),tofilterthehighfrequencynoise(U2:A)asahigh-pass Butterworth filter; to amplify the analytical signal (U2:B), todetect the peak signal as a sample-hold unit (U2:C) and to fit theanalyticalsignal(U2:D)intheA/Dscale(5V)usingCMOSswitches(U3:B–D)tochangethegaindependingonthevalueoftheinputsig-nal.C5andR11areusedaslow-passfilterandP1isusedforoff-set.CMOSswitchU3:Aisusedtodischargethecapacitorofthesample-hold circuit. The switches are controlled by the PIC. The processedsignal E is sent to the A/D converter of the PIC to be converted intoabsorbance values. To calculate the absorbance values, the loga-rithmfunctionusedthemeasurementofblank(water)asreference.Both blank and sample measurements were registered turning theLED on to consider maximum light power and off in order to con-siderthedarksignal.Afterdigitalization,theabsorbancevaluesaresentbythemicrocontrollertotheliquidcrystaldisplay(LCD)mod-ule, a TECH2004D-FL-GBS-S character type LCD with two buses:eight bits for data and three bits for control. In this work, the com-munication between microcontroller and LCD was always carriedout with six bits, four being used for data transmission and twofor data control. The Stepper Motor Control Module controls theangular displacement of the CD media.Aclockelaboratedwitha4-MHzpiezoelectriccrystalisusedforsynchronization of the microcontroller internal functions.
3. Results and discussion
 3.1. Calibration of the MLCS optical–mechanical system
Anoceanopticsspectrometer,modelUSB450,whichsubstitutedthe phototransistor as detector, was used to calibrate the MLCSoptical–mechanical system. Since the slit for the light entranceon the probe and the sensitive area of the phototransistor havethe same dimensions (ca. 0.3mm), the spectra registered by theoceanopticsspectrometerrepresenttheprofileoftheradiationthatreaches the phototransistor. In this process, the spectrometer reg-istersthereflectedspectrumresultingfromtheradiationdiffractedon the CD media. It was carried out five scans to obtain an averagespectrum for each step of the stepper motor. Average spectra wereused to build a calibration curve between the number of steps andthewavelengthofmaximumemissionofthespectrum.Inthiscase,anequationwasestimatedbyusingthelinearleast-squaresandtheresult is presented below.Step
7837The number of steps and peak wavelengths are linearly cor-related in the spectral range 440–640nm with a correlationcoefficient of 0.99968. Therefore, practically the entire visiblespectral region can be exploited for spectrophotometric measure-ments by the MLCS. The overall standard deviation at the peakwavelengths was 0.30nm, indicating a good repeatability asso-ciated to the wavelengths obtained starting from the number of steps.Thecollecteddatawerealsoemployedtoestablishtheeffectivebandwidths at maximum wavelength for each step and the value13nm was estimated in the range 440–640nm.The dispersion of the maximum signals measured for eachstep was also assessed and the overall relative standard deviation(R.S.D.)wasestimatedas2.6%.Thisresultindicatesagoodrepeata-bility of the signals associated to the radiant power of the whiteLED.
 3.2. Determination of food colorants in synthetic samples
The performance of the MLCS was initially evaluated by ana-lyzing food colorants in the synthetic samples. The absorbancemeasurements were accomplished at the wavelengths of itsmaximum absorption: 486nm (sunset yellow), 500nm (allurared) and 582nm (brilliant blue). However, in the case of tar-trazine solutions, the measurements were performed at 440nmdue to the low sensibility of the MLCS in the wavelength of maximum absorption of this colorant (426nm). For referencemeasurements, the food colorants were also analyzed by an HPdiode-array,model8453,andaMicronalspectrophotometer,modelB34211.In order to investigate the maximum concentration for linearresponse(thelimitoflinearity—LOL),ANOVA(analysisofvariance)and
-test for lack of fit were applied to the models elaboratedwith the concentration range 2.0–26.0mgL
, for each colorant.The results showed no lack of fit up to the LOL as presented inTable 1.An
-test for the regression significance revealed that theperformed linear regressions are highly significant up to the LOLvalues.The values of limits of detection (LOD) and limits of quan-tification (LOQ), which were estimated according to IUPACrecommendations[7],are also shown inTable 1.It is worth not- ing that LOL, LOD and LOQ present similar values for the threeinstruments and for the four food colorants.After the study above, the analytical curves were constructedemployingthefollowingconcentrationranges:2.0–12.0mgL
fortheothercolorants.InTable2are presented the results for the colorants determinations in syntheticsamples.Ascanbeseen,thereisagoodagreementbetweentheresultsof concentration determined by the proposed instrument and those

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