Microchemical Journal 103 (2012) 62–67

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Microchemical Journal
journal homepage: www.elsevier.com/locate/microc

A portable photometer based on LED for the determination of aromatic hydrocarbons

in water
Kássio Michell Gomes de Lima ⁎
Federal University of Rio Grande do Norte, Institute of Chemistry, Grupo de Pesquisa em Quimiometria Aplicada, CEP 59072-970, Natal, RN, Brazil

a r t i c l e i n f o a b s t r a c t

Article history: The present work describes a portable photometer based on light-emitting-diodes (LED) for the determination
Received 26 December 2011 of total aromatic hydrocarbons in water contaminated with gasoline. Two LED were employed as the light source
Accepted 11 January 2012 with maximum emission at 1300 nm and 1689 nm. The radiation of each LED was collected with bundles of 24
Available online 17 January 2012
silica optical fibers, which were assembled in a single bundle pointed toward the detection cell. An InGaAs pho-
todiode was directly connected to the measuring cell. Software was written in VisualBasic.NET to control the
Keywords:
NIR
photometer through a USB interface and for data acquisition. The determination of total aromatic hydrocarbons
Photometer-LED was performed using a silicone-sensing phase (length of 5 mm and diameter of 3.2 mm), which was employed to
Optical sensor extract these compounds from the contaminated water. The extraction (60 min under constant stirring) was
Aromatic hydrocarbons performed in a 100-mL flask filled with the water sample diluted in 2.0 mol L− 1 NaCl. A repeatability of 1.8%
and 1.3% (expressed as the relative standard deviation of 10 measurements) was obtained at 1300 nm and
1689 nm, respectively. Absorbance values were calculated considering the signal at 1300 nm as reference be-
cause hydrocarbons do not absorb at this wavelength. Analytical curves up to 200 mg L− 1 and 400 mg L− 1
were constructed for benzene and toluene, providing limits of detection of 1.2 mg L− 1 and 1.7 mg L− 1, respec-
tively. The sensitivity was similar to those obtained with a FT-NIR Bomem MB 160 spectrophotometer at the
same wavelength. The photometer was applied to the determination of total hydrocarbons in water contaminat-
ed by gasoline. An analytical curve (50–300 mg L− 1) was constructed from reference solutions containing ben-
zene and toluene in the ratio of 3:7, which is a ratio commonly found in Brazilian gasoline. The results provided
by the photometer were compared with those obtained with the commercial spectrophotometer and did not
show significant differences at a confidence level of 95%.
© 2012 Elsevier B.V. Open access under the Elsevier OA license.

1. Introduction region, instruments were developed for determining sulfate in

In the interest of the miniaturization of instruments for field mea-
surements, light-emission-diodes (LEDs) have become increasing pop-
ular in optical instruments in general and in photometers LED in
particular. Among the main advantages of these instruments [1] are
their simplicity of operation, low cost and power consumption, high
stability and compatibility with optical fibers. In these LED photome-
ters, the time delay between the sequential activation of the emitters
and individual measurements on several wavelengths is very low (on
the order of tenths of seconds), as in a diode array spectrophotometer.
By employing LEDs that emit radiation at wavelengths previously se-
lected (e.g., UV, Vis, NIR and MID), the information generated by a
multi-LED photometer may be sufficient for use in analysis or discrimi-
natory simultaneous determinations based on multivariate analysis.
Several applications of LED photometers in different regions of the
electromagnetic spectrum are present in the literature. In the UV
⁎ Tel.: + 55 84 3215 3828.
E-mail address: kassio@ufrnet.br.
water [2], acidity in fruit juices [3], and nitrite and nitrate in water
[4], among others. For example, Zarate and colleagues [2] proposed
an automatic procedure for the turbidimetric determination of sulfate
in rain water based on a multicommutation flow analysis process
using a photometer with an LED (λ = 420 nm), a flow cell with an op-
tical path of 100 mm and a photodiode. In 2010, [3] Silva and col-
leagues described a low cost photometer based on an identical pair
of LEDs (λ = 531 nm): one employed as a light source and the other
as a photodetector. The equipment, including the photometer and
the analysis module, was designed for an automatic titration proce-
dure using multicommutation flow injection (MCFIA). Liu and col-
leagues [4] proposed an LED-photometer that operated in the UV
region (λ = 255 nm) for the determination of total nitrite and nitrate
in water. In this study, we found the detection limits for nitrite and
nitrate to be 7 mol L − 1 and 12 mol L − 1, respectively.
There are multiple examples of LED-photometers operating in the
UV–vis region and combined with chemometric analysis. For example,
Fonseca and colleagues [5] described the development of a portable
multi-LED photometer operating in the visible region and applied for
the simultaneous determination of Zn(II) and Cu(II) in pharmaceutical

0026-265X/© 2012 Elsevier B.V. Open access under the Elsevier OA license.
doi:10.1016/j.microc.2012.01.003
 K.M.G. de Lima / Microchemical Journal 103 (2012) 62–67
formulations. Multivariate calibration models based on multiple linear
regression provided quadratic mean errors of prediction (RMSEP) of
0.06 and 0.12 mg L − 1 for Zn(II) and Cu(II), respectively. The same au-
thors applied this multi-LED photometer in 2007 [6] for the discrimina-
tion of mineral water samples using chemometric tools. In addition,
Hauser and colleagues [7] described a multi-LED photometer in the vis-
ible region to determine various species in solution, including ammonia,
Cu(II), Al(III), Ca(II), Cr(III), phosphate and nitrite. The relative errors
based on the measurements of concentration were between 0.2 and
5.0%.
The NIR region offers additional advantages for analytical applica-
tions of LED photometers, such as a non-destructive nature, versatility
and the possibility of in situ analysis. However, the large bandwidth of
the LED (30 to 50 nm), pre-concentration steps and the need for che-
mometric tools limit work in this region. However, several applications
of NIR LED-based photometers can be found in the literature for the de-
termination of chlorophylls [8], adulteration of petrol [9], moisture tufa
[10], lubricants [11] and others.
For example, McClure and colleagues [8] developed a portable NIR
photometer, coined “TWmeter” by the authors, using three LEDs with
peak emissions at 700, 880 and 940 nm for the determination of chloro-
phyll in plants and moisture in paper. In this paper, multivariate calibra-
tion by multiple linear regression was used to determine the chlorophyll,
resulting in a prediction error of 0.99 mg/cm2 of leaf surface, a dynamic
range of 1.8 mg/cm2 and a humidity range of 30–65%. Additionally,
Gaiao and colleagues [9] proposed a portable NIR photometer based on
an LED for the low-cost detection of adulteration of Brazilian commercial
gasoline with kerosene. The photometer contained an LED with a peak
emission at 1550 nm and a detection system consisting of a PbSe photo-
resistor controlled by a microcontroller. The authors showed that the in-
strument could detect samples of gasoline contaminated with kerosene
at 5% (v/v). Hyvarinen and colleagues [10] developed two NIR photome-
ters for moisture determination in peat. This integration used a photom-
eter detector and interference filters with narrow bands in a single
semiconductor. Finally, Pignalosa and colleagues [11] presented an
LED-based photometer for the analysis of lubricants with limits of detec-
tion and quantification of 0.07% and 0.16% (w/w), respectively.
LED-based instruments have a simple assembly and low cost, are ver-
satile and can be employed in the determination of many chemical pa-
rameters with promising results. Thus, the objective of this work was
the development of a portable photometer-LED in the near infrared re-
gion (NIR) for the determination of BTEX compounds in contaminated
water.
2. Experimental procedures
2.1. Reagents and solutions
Benzene, toluene, and xylenes were purchased from Merck and used
as received. Methanol (spectroscopic grade, Merck) was used to pre-
pare stock solutions of BTX aromatic hydrocarbons. Sodium chloride
(Vetec) was used to adjust the salinity of water samples. Silastic T2
(crosslinking agent) was provided by Dow Corning. Distilled and deio-
nized water was used to prepare contaminated aqueous samples.
2.2. Reference solutions
Initially, standard solutions of benzene and toluene at
50000 mg L − 1 were prepared, and ethylbenzene and xylene were pre-
pared at 10 000 mg L − 1 in methanol. Then, 5.00 mL of these solutions
was transferred to a 500 mL volumetric flask, and the solution was
brought to its final volume with deionized water. The resulting stock so-
lutions represented 500 mg L− 1 of benzene and toluene as well as
100 mg L − 1 of ethylbenzene and xylenes with 1% methanol.
63
2.3. Preparation of the sensing phase
The polymeric sensing phase consisted of a silicone-based polydi-
methylsiloxane (PDMS). The monomer and crosslinking agent was
mixed in a 10:1 ratio as recommended by the manufacturer. The
homogenization was carried out in an ultrasound bath for approxi-
mately 3 min to remove the air bubbles formed during mixing. The
mixture was subsequently transferred to Teflon containers molded
into a disc shape (height of 15 cm and diameter of 4 cm). These con-
tainers were placed in a Teflon vacuum desiccator for 30 min to re-
move any bubbles that remained after homogenizing the mixture.
The polymeric material was left for 36 h for polymerization/crosslink-
ing in an airtight plastic container. After this period, the phase sensing
polymer was placed in an oven for 6 h at 60 °C to complete the cross-
linking. The phase sensors were then removed from the Teflon molds
and cut into a cylinder with a diameter of 3.2 mm and a height of
5 mm.
2.4. Instrumentation
An FT-NIR spectrophotometer (Bomen MB 160) was used for mea-
surements in the region of 800 nm to 2500 nm. The data were
obtained using Win-Bomem Easy 3.04 software. Each spectrum was
recorded as an average of 100 scans with a resolution of 8 cm − 1. A
transmission cell was made in our laboratory for the optical fibers.
The optical path of the cell was determined by spacers of different
length (1 mm, 2 mm, 5 mm and 10 mm), with the 5 mm spacer uti-
lized in the following experiments.
2.5. NIR-LED photometer
2.5.1. Power supply
The instrument used a commercial Mean Well power supply pro-
duced and distributed by LR Industrial Informatics. The source model
was DP-2512 with a symmetrical output of ±12 V.
2.5.2. Array LED
Six LEDs emitting radiation in different areas of the NIR spectrum
were acquired from Roithner Lasertechnik. The wavelengths of the
maximum emission indicated by the manufacturer were 1200 nm,
1300 nm, 1550 nm, 1650 nm, 2150 nm and 2350 nm. Each LED was
fixed in a metal connector, and the arrangement of the LEDs was
achieved on a crafted acrylic plate.
2.5.3. Collection of NIR radiation
Twenty-four beams containing polymer optical fibers 200 μm in
diameter were each (Ocean Optics) connected to each LED to guide
the individual radiation emitters. These beams were grouped into a
single output beam containing 144 fibers, which was connected di-
rectly to the transmission cell.
2.5.4. Circuit electronic photometer
The circuit designed for activation of the LEDs allowed the use of a
diode array with up to six LED. The circuit (Fig. 1a) consisted of cur-
rent limiting resistors and drivers (commonly called transistor keys)
for driving the LEDs with virtually infinite impedance between its
input and its output. This ensured that overvoltage or short circuits
occurring in the LED drive did not reach the acquisition interface, pro-
tecting the interfaced PC. The drivers used were Darlington (ULN2001
chip), produced by Texas Instruments. Sixty-eight ohm resistors and
variable resistors with a maximum resistance of 1 kΩ were employed
to determine the current through the LED. With the variable resistors,
the emission intensities of the LEDs could be adjusted according to
the sensitivity of the detector (photodiode G8373), which provides
a stable signal to all the LEDs.
64 K.M.G. de Lima / Microchemical Journal 103 (2012) 62–67

2
1
b

Fig. 2. Overview of NIR photometer: 1) LED and fiber optic assemblies, 2) power sup-
ply, 3) electronic circuit for powering the LEDs and signal amplification, 4) cell broad-
cast and the PDMS phase sensor, 5) USB interface for data acquisition.

radiation). The absorbance in each measurement was obtained from

the difference described in Eq. (3).
Fig. 1. (a) Electronic circuit of the NIR photometer powering the LEDs. (b) Electronic
circuit built for signal conditioning of the InGaAs detector. A ¼ A1689 −A1300 ð3Þ

Fig. 2 shows a general outline of the developed NIR photometer.

2.5.5. Detector
The photometer employed here as a sensor was an InGaAs
photodiode (model G8373) produced by Hamamatsu. The electronic
circuitry used for conditioning the signal from the photodiode is
detailed in Fig. 1b. Associated with the InGaAs photodiode, a volt-
age–current converter (Module I) that also operated as a first
stage amplification was attached. The signal was amplified again in
Module II.
2.5.6. Interface and data acquisition
The interface used in this photometer facilitated communication
between the dedicated software, controlling the instrument and
data acquisition. Six of the twelve digital outputs were used to drive
the LED, providing a logic low for those that must remain turned off
and a high logic level for those that were fired. One of the twelve
analog-digital (A/D converter) inputs was used for data acquisition
from the photodiode. The interface used was a USB-6009 model
from National Instruments. A program was written in the photometer
VisualBasic.NET environment to control and acquire data from the
photodiode through the electronic interface, which had an analog/
digital (A/D) of 14 bits. The written program drove the LEDs and col-
lected the signals.
The InGaAs photodiode was connected directly to the optical fiber
to collect direct radiation from the LEDs to prevent radiation loss.
2.6. Experimental procedure
Measurements were performed by placing a PDMS monolith in an
85 mL bottle completely filled with the aqueous mixture of aromatic
hydrocarbons and subjected to constant stirring (2700 rpm) for a
time interval of 60 min at 22 ± 1 °C for the extraction of hydrocar-
bons. After this step, the monolith was removed from the mixture,
quickly blotted dry and inserted into the measurement system. An
adequate amount of NaCl was transferred to the bottle so that it
was completely filled with the hydrocarbon solution, assisting in the
transfer of compounds to the PDMS sensing phase. All extractions
were performed in sealed vials. The spectrum of PDMS, previously
immersed in an aqueous solution containing 1% methanol, was used
as the reference for absorbance measurements. All measurements
were employing new phase sensing material.

2.5.7. Calculation of absorbance and vision of the NIR photometer

The absorbance for two LEDs operating at 1689 nm and 1300 nm
can be calculated according to Eqs. (1) and (2), respectively.
 
I1689 −Esc
A1689 ¼ − log ð1Þ
R1689 −Esc
 
I1300 −Esc
A1300 ¼ − log ð2Þ
R1300 −Esc

where I is the average of the sample signals (phase sensor in contact

with the BTEX compounds), R is the average of the signals relating to
the reference measurements (only the phase sensing) and Esc is the
average of the signals relating to measurements in the dark (no Fig. 3. Emission spectra of six standard LEDs in the NIR region.
 K.M.G. de Lima / Microchemical Journal 103 (2012) 62–67 65

Table 1 0,05
Wavelengths of peak emission and bandwidths at half height for the LEDs used in the
studied photometer. Day 1
0,04 Day 2
Nominal wavelength Measured wavelength Relative Effective bandwidth at Day 3
(nm) (nm) error (%) half height (nm)

Absorbance - a.u
1200 1197 − 0.25 100 0,03
1300 1301 + 0.07 100
1550 1504 + 0.26 180
1650 1689 + 1.78 240
2150 2186 + 1.64 373 0,02
2350 2344 − 0.25 248

0,01
3. Results and discussion

Using the spectrometer developed in our laboratory, the emission
spectra of six LEDs were obtained. Fig. 3 shows the LED spectra after
normalization. As observed, the LEDs had six NIR emissions that were
the most informative for this application. Table 1 shows the wave-
lengths of maximum emission and the effective bandwidth at half
height for each of the devices. The nominal wavelengths (indicated by
the manufacturers) are also presented in this table. The results shown
in Table 1 reveal small deviations (less than 2%) for the six wavelengths
of the LEDs in relation to their nominal values. Variations in nominal
wavelengths could be attributed to possible non-uniformities in the
manufacturing process and/or calibration of the spectrophotometer.
However, the bandwidths at half height for LEDs at longer wavelengths
(1689 nm, 2150 nm and 2350 nm) were larger, indicating a loss of LED
monochromaticity.
The emission intensity profiles versus number of readings for all the
LEDs were drawn from the signals found in the peak emission of 1000
readings obtained after the sequential activation of emitters. Fig. 4
shows the intensity profile for the LED with a peak emission at
1689 nm. For these devices, the intensity of the LED became steady
after its minimum value was reached. The time signal “zero” was
obtained immediately after the firing of the LED. The signal strength de-
creased by 4.1% after reaching its maximum value, achieving stability
approximately 80 s after the drive.
As noted in previous works, the more intense absorption peaks
found for the BTEX compounds in NIR are 1675 nm, 2140 nm,
2165 nm and 2340 nm. As BTEX compounds do not absorb radiation at
approximately 1300 nm and the variation in signal strength in this re-
gion reflects only the position of the sensing phase, it is necessary to
use more than one LED. Therefore, the behavior of the LED with a peak
emission at 1689 nm was initially assessed using a photometer cell
0,00
0 100 200 300 400
Toluene - mg L-1
Fig. 5. Three analytical curves obtained for toluene on different days with an extraction
time of 60 min in 2 mol L− 1 NaCl using a 5 mm sensing phase.
with a PDMS sensing phase having a 5 mm optical path. Those LED at
1500 nm, 2150 nm and 2350 nm showed extremely low intensities, in-
dicating that virtually all the radiations were absorbed by the sensing
phase. For this reason, LEDs with peak emissions of 1500 nm, 2150 nm
and 2350 nm were not used in this application. The LED with a maxi-
mum intensity of 1689 nm gave a higher intensity and was instrumental
in building the photometer, as 1689 nm was in the region related to the
1st C–H stretch of BTEX compounds.
The performance of the LEDs with peak emissions at 1200 nm and
1300 nm were similar to those observed for the 1689 nm LED. As the
standard curves of the spectrophotometer for the determination of
BTEX were constructed using only the wavelengths 1300 nm and
1675 nm, the LEDs with maximum intensity at 1300 nm and
1689 nm were selected for this application. Therefore, the LED with
peak emission at 1300 nm was employed in the construction of ana-
lytical curves of BTEX compounds in the photometer as a reference
signal, and the LED with a maximum intensity at 1689 nm was used
for the signal of the analytes.
The accuracy of the proposed method using the NIR photometer
was evaluated by constructing three analytical curves for toluene in
the range from 0 to 400 mg L − 1. For this purpose, a transmission
cell with optical fibers (Fig. 5) was used, resulting in an average
slope with a standard deviation of 11.8% and a linear coefficient

Fig. 4. Profile of intensity vs. time for LED emission at 1689 nm.
66 K.M.G. de Lima / Microchemical Journal 103 (2012) 62–67

a 0,08
Table 3
Determination of total benzene and toluene (mg L− 1) in water by different instru-
Spectrophotometer NIR (1675 nm)
ments at 1689 nm.
Spectrophotometer NIR (1689 nm)
Photometer NIR Samples Photometer NIR Spectrophotometer NIR
0,06
1 156 ± 11 149 ± 14
Absorbance - a.u

2 145 ± 16 140 ± 10
3 157 ± 14 147 ± 11

0,04

maximum absorption for the 1st C−H stretch of the compounds stud-
ied, are shown for comparison.
0,02 As observed in the figures above, the sensitivity obtained for the
spectrophotometer at 1675 nm was 1.7 to 2.6 times higher for ben-
zene and toluene when compared to the results obtained by observ-
0,00 ing the maximum emission of the LED at 1689 nm. Comparing the
0 50 100 150 200 sensitivities between the two instruments at 1689 nm (Table 2), it
Benzene - mg L-1 could be concluded that the sensitivities of the two instruments
were quite similar. Ideally, the sensitivity would be greatly improved
b 0,10
if the maximum emission of the LED was exactly 1675 nm. In addi-
Photometer NIR tion, the detection limits for benzene and toluene in the NIR photom-
Spectrophotometer NIR (1675 nm) eter were 1.2 and 1.7 mg L − 1, respectively, as calculated from the
0,08 Spectrophotometer NIR (1689 nm) analytical curves shown in Fig. 6.
To evaluate the developed NIR photometer against actual contam-
Absorbance - a.u

ination, water samples were contaminated with type A gasoline (ratio

0,06
0,04
0,02
0,00
0 100 200 300
Toluene - mg L-1
Fig. 6. Comparison of analytical curves obtained for benzene (a) and toluene (b) from the
photometer and the spectrophotometer employing a PDMS phase containing a sensing
optical path length of 5 mm in 2 mol L− 1 NaCl with an extraction time of 60 min.
with a standard deviation of 7.64%. Each of these curves was built on
different days and with new standard solutions. These results indicat-
ed that the proposed method requires daily calibration.
Analytical curves were obtained for benzene and toluene using the
photometer operating under the following experimental conditions:
5 mm optical path, 2 mol L − 1 NaCl and 60 min of extraction. In this
case, measurements were carried out on two different instruments,
an NIR photometer and a commercial instrument (FT-NIR), to com-
pare sensitivity. Once the signals from the LED emission maximums
at 1689 nm and 1300 nm were registered by the photometer, the
phase sensor was removed from the transmission cell photometer
and immediately inserted into the other transmission cell coupled
to the spectrophotometer for the registration of trade spectra.
Fig. 6a shows the standard curves obtained for benzene compounds
in the range from 0 to 200 mg L − 1, and Fig. 6b shows the standard
curves for toluene in the range from 0 to 400 mg L − 1. The measure-
ments performed at 1675 nm, which matched the wavelength of
Table 2
Comparison of slopes obtained for the analytical curves of benzene and toluene using
both the photometer and the spectrophotometer at 1689 nm.
Compounds Instruments
Spectrophotometer
Benzene 1.22 × 10− 4
Toluene 1.13 × 10− 4
of 2.5% (v/v)). Table 3 shows the results of the content of benzene and
toluene for the three samples measured in triplicate using the total
optical sensor developed for the photometer and the NIR spectropho-
tometer, both at 1689 nm. A t test of the results obtained from the
two instruments (photometer and spectrophotometer) showed no
statistically significant differences at a confidence level of 95%. There-
fore, the NIR photometer-based LED could be considered a viable,
low-cost alternative for the determination of benzene and toluene
in water.
400
4. Conclusion
The potential of a multi-channel NIR photometer based on an array
of LEDs was investigated in the determination of BTEX in gasoline-
contaminated water using a PDMS sensing phase. The photometer
based on LEDs was a simple, low-cost assembly, which was much
cheaper than most NIR spectrophotometers currently available on the
market. These results indicated that the instrument developed could
be an economical and simple alternative for the application studied.
Acknowledgments
The author is grateful to professors Dr. Ivo M. Raimundo Jr. (UNI-
CAMP-Brazil) and M.F Pimentel (UFPE-Brazil) for technical assistance
and to CNPq and CAPES/PROCAD for financial support.
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