Sérgio Ricardo Bezerra dos Santos

An inexpensive, portable and microcontrolled near infrared LED-photometer for screening analysis of gasoline.

A microcontrolled, portable and inexpensive photometer is proposed. It uses a near infrared light emitting diode (NIR LED) as radiation source, a PbSe photoresistor as infrared detector and a programmable interrupt controller (PIC) microcontroller as control unit. The detector system presents a thermoresistor and a thermoelectric cooling to control the detector temperature and keep the noise at low levels. The microcontroller incorporated total autonomy on the proposed photometer. As its components are inexpensive and of easy acquisition, the proposed NIR LED-photometer is an economical alternative for chemical analyses in small routine, research and/or teaching laboratories. By being portable and microcontrolled, it also allows carrying out field chemical analyses. The instrument was successfully applied on the screening analysis to verify adulteration in gasoline samples.

An automated FIA system to determine alcoholic grade in beverages based on Schlieren effect measurements using an LED-photocolorimeter

Alcoholic grade determination in beverages is usually carried out by laborious, slow and expensive processes such as distillation or chromatographic measurements. To overcome these drawbacks, a simple, automated, flow injection system using a photocolorimeter based on a light-emitting diode (LED) as source of radiation and a phototransistor as photodetector is proposed. The alcohol determination is based on refractive index gradient (Schlieren effect) measurements when beverages are injected into an inert carrier stream (water) of a FIA configuration that presents limited mixing conditions. The system was applied to wine, gin, rum, vodka and sugar cane-based beverages known as “cachaca” available in Brazil. The alcoholic grade determination in these alcoholic beverages showed a relative standard deviation of 3.4% and a mean relative error of 3.0% (n = 10). The developed system processes 120 samples per hour with consumption of 250 μl of sample and no reagent or distillation process is necessary in carrying out the analysis.

An automated flow-injection titrator for spectrophotometric determinations of total acidity in wines, using a single standard solution and gradient calibration

An automated flow-injection titrator to perform spectrophotometric determinations of acidity in wine samples is described. The proposed titrator exploits concentration gradients generated in the flow-injection system and, in contrast to the automated flow titrators previously proposed, it does not require analytical curves based on several standard solutions of tartaric acid. Only one single standard solution, the proper titrant, is directly used for gradient calibration and calculating of the analyte concentrations. A simple laboratory-made photometer that uses an LED (Light-Emitting Diode) as light source and a phototransistor as detector was built in to this titrator. Yellow LED was usually used for spectrophotometric measurements because m-cresol purple (7.4 < pH < 9.0 yellow–purple transition) was selected as acid–base indicator. The system is fully controlled by microcomputer and the software for control and for acquisition and treatment data was written in C language. A good agreement between results yielded by the proposed titrator and those produced by a reference method of the Association of Official Analytical Chemistry (AOAC) was obtained and no statistical difference between results at the 95% probability level was confirmed by applying the paired t-test. An overall relative accuracy of about 0.9% and a mean relative standard deviation lower than 1.5% were obtained with nine replicate titrations. The proposed titrator allows 72 determinations per hour to be carried out, consuming just 200 µl of the sample and 1.5 ml of the titrant.

A portable, inexpensive and microcontrolled spectrophotometer based on white LED as light source and CD media as diffraction grid.

A portable, microcontrolled and low-cost spectrophotometer (MLCS) is proposed. The instrument combines the use of a compact disc (CD) media as diffraction grid and white light-emitting diode (LED) as radiation source. Moreover, it employs a phototransistor with spectral sensitivity in visible region as phototransductor, as well as a programmable interrupt controller (PIC) microcontroller as control unit. The proposed instrument was successfully applied to determination of food colorants (tartrazine, sunset yellow, brilliant blue and allura red) in five synthetics samples and Fe(2+) in six samples of restorative oral solutions. For comparison purpose, two commercial spectrophotometers (HP and Micronal) were employed. The application of the t-paired test at the 95% confidence level revealed that there are not significant 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 standard deviation (R.S.D.) of each analyte was smaller than 1.0%. Therefore, the proposed instrument offers an economically viable alternative for spectrophotometric chemical analysis in small routine, research and/or teaching laboratories, because its components are inexpensive and of easy acquisition.

An improved leaping detector for flow analysis applied to iron speciation in drugs

A low inner volume (ca. 64 ml) probe was built up in an injector-commutator in order to behave as a photometric leaping detector in flow analysis. It comprises a bicolour light-emitting diode (BLED), as a source of pulsed radiation in the red and green visible region, and two phototransistors as transducers. Sample injection, detector relocation, analytical signal recording, data treatment and definition of the spectral working range were computer-controlled. The feasibility of the system was initially demonstrated in the flow-injection speciation of iron, and the overall standard deviation of results was estimated as ± 1.6 and ± 1.4% for 1.6–4.0 mg l−1 Fe(II) or total iron after eightfold processing of synthetic samples. The system was further applied to drug analysis: the mean deviations of results for typical samples were estimated as ± 5.2 and ± 3.3%, and the relative standard deviation as ± 1.6 and ± 1.3% for Fe(II) and total iron, respectively. Results were compared with those obtained by a conventional spectrophotometric procedure and no statistic differences at the 95% confidence level were found. In relation to an earlier system with multi-site detection, the proposed system is more stable, presenting low drift with a relative standard deviation of 0.026% and 0.039% for measurements (n=120 during 4 h of observation) with green and red emission. It is also faster with a sampling rate of 133 h−1 and carryover problems are not found. The possibility of compensating the Schlieren noise by dual-wavelength spectrophotometry is discussed.

Um fotômetro de fluxo para análises clínicas a base de um diodo emissor de luz bicolor

The construction and evaluation of an inexpensive flow photometer for clinical analysis, using a bicolour LED and a phototransistor adapted for tubular flow cell, are described. The instrument presents some new features such as: automatic zero, electronic calibration and peak-hold signal. When compared with a classical photometer, it is simpler and has the advantages of a flow analysis system: lower volumes of reagents and samples, lower levels of contamination, shorter time for analysis and lower analysis costs. The instrument was used in the determination of the constituents in blood samples. The results obtained agree with those obtained by a classical photometer and the precision was better.

Flow injection photometric determination of NaCl, KCl and glucose in injectable drugs exploiting Schlieren signals

A flow injection photometric system that exploits Schlieren signals for analytical measurement is described. The system was designed to be used as a new strategy for determining the contents of sodium chloride, potassium chloride and glucose, each respectively in injectable drugs. The proposed methodology was based on the difference between the refractive indices of the sample zone and of the carrier stream. With this perspective, a lab-made photometer based on LED-phototransistor technology was employed as a detection system to investigate the different analytical profiles related to the Schlieren effect in low flow rate conditions. The parameters of the flow system, such as flow-rate, optical path length, and sampling loop, were adjusted in order to obtain suitable Schlieren profiles for the measurements. Data evaluation was performed with the application of partial least squares regression (PLS-1). The obtained results demonstrated the predictive ability of the constructed PLS models, and the predicted concentration values were in agreement with the reference values, with a 95% confidence level.

Automated flow-rate meter for flow-analysis systems

An automated flow-rate meter easy to construct and operate is described. This is contralled by a micracomputer connected to an analog/digitai converter interface and by a contrai software. It uses two acrylic flow cells, each comprising a bicolor light-emitting diode anda phototransistor piaced on opposite sides. The performance of this flow-rate meter was evaiuated by appiying it to three flow manifoids: one monosegmented flow titration system by binary sampling; one conventionai monosegmented flow system, and one singie-iine FIA system. The FIA system flow rate was assessed by means of a Vanderslices expression. The time range of measurement of the flow rates was of 3.5-19.5 seconds and relative errars of 0.2-2.6% as well as relative stanCorrespondence to: Mario Cesar U. Araujo.