Edvaldo N. Gaião

Digital image-based flame emission spectrometry

A digital image-based flame emission spectrometric (DIB-FES) method for the quantitative chemical analysis is proposed here for the first time. The DIB-FES method employs a webcam to capture the digital images which are associated to a radiation emitted by the analyte into an air-butane flame. Since the detection by webcam is based on the RGB (red-green-blue) colour system, a novel mathematical model was developed in order to build DIB-FES analytical curves and estimate figures of merit for the proposed method. In this approach, each image is retrieved in the three R, G and B individual components and their values were used to define a position vector in RGB three-dimensional space. The norm of this vector is then adopted as the RGB-based value (analytical response) and it has revealed to be linearly related to the analyte concentration. The feasibility of the DIB-FES method is illustrated in three applications involving the determination of lithium, sodium and calcium in anti-depressive drug, physiological serum and water, respectively. In comparison with the traditional flame emission spectrometry (trad-FES), no statistic difference has been observed between the results by applying the paired t-test at the 95% confidence level. However, the DIB-FES method has offered the largest sensitivities and precision, as well as the smallest limits of detection and quantification for the three analytes. These advantageous characteristics are attributed to the trivariate nature of the detection by webcam.

A digital image-based method for determining of total acidity in red wines using acid–base titration without indicator

This work proposes the use of digital image-based method for determination of total acidity in red wines by means of acid-base titration without using an external indicator or any pre-treatment of the sample. Digital images present the colour of the emergent radiation which is complementary to the radiation absorbed by anthocyanines present in wines. Anthocyanines change colour depending on the pH of the medium, and from the variation of colour in the images obtained during titration, the end point can be localized with accuracy and precision. RGB-based values were employed to build titration curves, and end points were localized by second derivative curves. The official method recommends potentiometric titration with a NaOH standard solution, and sample dilution until the pH reaches 8.2-8.4. In order to illustrate the feasibility of the proposed method, titrations of ten red wines were carried out. Results were compared with the reference method, and no statistically significant difference was observed between the results by applying the paired t-test at the 95% confidence level. The proposed method yielded more precise results than the official method. This is due to the trivariate nature of the measurements (RGB), associated with digital images.

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 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.

Automatic determination of chlorine without standard solutions using a biamperometric flow-batch analysis system

This study presents an automatic analysis system that does not require the use of standard solutions. The system uses an electrochemical flow cell for in line generation of the standards, and operates under the standard addition technique. The versatility of this system was demonstrated by the development of a one key touch fully automatic method for the determination of total available chlorine in real samples. The extremely simple, accurate and inexpensive method was based simply on the biamperometric monitoring of the well known redox reaction of chlorine with iodide ions in a flow-batch system, where the produced iodine (triiodide ions) generates an electrical current proportional to the chlorine concentration in the sample. The flow-batch parameters were optimized to maximize the sensitivity without losses on the precision of the analysis. An excellent linear dependence between the biamperometric signal and the chlorine concentration for the standard additions and a good agreement between the proposed approach and a reference method were obtained. The method was successfully applied to determine chlorine in several different bleach and chlorinated water samples (r=0.9995, LOD=8.261 x 10(-7) mol L(-1)) and could be easily extended to other oxidants and samples. Comparison to a reference method and recoveries close to 100% demonstrated the reliability of the proposed method. In addition, low residue disposal and reagent consumption, allied with high accuracy and precision, make it very promising for routine applications.

Flow Injection Determination of Metronidazole through Spectrophotometric Measurement of the Nitrite Ion Produced upon Alkaline Hydrolysis

A new method for metronidazole determination, based on spectrometric monitoring of a diazonium salt produced in-line by alkaline hydrolysis released nitrite ions, was developed and successfully applied to pharmaceutical tablets (r = 0.9993, 2.0-20.0 mg L-1, DL = 0.7 mg L-1) with no interference from common ingredients accompanying the drug.

Um sistema microcontrolado para o monitoramento on-line, in situ e remoto de pH, condutividade e temperatura de águas

A portable microcontrolled system is proposed to monitor conductivity, temperature and pH in on-line, in situ and remote way from a water reservoir faraway 200 m. The system comprises two modules: one for data reception (located in laboratory) and another for data acquisition/transmission (located near water reservoir). It uses a microcontroller and a transceiver to remote data transmission/reception by radio frequency. Variations of water parameters were simultaneously monitored without interruption during a period of ten hours with a relative error about 4.0 %. The developed system showed simple, stable, accurate, robust and low-cost to determine parameters of water in field.

Um fotômetro multi-led microcontrolado, portátil e de baixo custo

A microcontrolled, portable and inexpensive photometer is described. It uses six light-emitting diodes (LEDs) as radiation sources and a phototransistor as detector, as well as a microcontroller (PIC - Programmable Controller of Interruption). This device provided total autonomy to the proposed photometer, which was successfully applied to determination of Fe2+ in ferrous syrups and of seven clinical biochemical parameters. As the components are cheap (~U

Screening analysis of seston from a domestic wastewater treatment plant using digital images

30.00) and easy to find, the proposed photometer is an economical alternative for routine chemical analyses in small laboratories, for research and teaching. Being portable and microcontrolled, it allows doing field chemical analyses.

Classification of distilled alcoholic beverages and verification of adulteration by near infrared spectrometry

This paper concerns the use of digital images of seston to monitor different ponds of a domestic wastewater treatment plant. For this purpose, a commercial camera was employed to photograph the seston samples and an automatic procedure based on the Hough Circle Transform was used to segment the resulting picture. Multivariate techniques were then employed to analyze the seston images in terms of their RGB colour components. The results indicate that such colour components undergo a significant change after each stage of the wastewater treatment process, according to a Hotelling T2 test (p-value smaller than 10−4). This finding was corroborated by the use of quadratic discriminant analysis (QDA), which resulted in the correct classification of all samples according to the treatment stage. In addition, it was found that differences in the illumination of the samples can be standardized by converting the RGB data to the YCbCr format and correcting the luminance (Y) component. This correction may unveil changes in the seston features that were previously masked by the illumination variability.