0000000000294326
AUTHOR
Boaventura F. Reis
Micropumping multicommutation turbidimetric analysis of waters
Abstract A micropumping multicommutation manifold to perform turbidity determinations in waters is described. The procedure is based on the use of a combination of hydrazine sulfate and hexamethylenetetramine, to obtain an external standard of nephelometric turbidity units (NTU), which could compare the absorbance measurements at high wavelengths for samples with a calibration line obtained from a concentrated formazine standard diluted on-line. To minimize sample and reagent consumption and waste generation, the flow system was designed with two solenoid micro-pumps, one of them for the alternative introduction of the formazine standard and samples and the other one for the water carrier. …
A chemiluminescence flow-based procedure for determination of carbaryl in natural waters exploiting multicommutation and enzymatic reaction
A chemiluminescence procedure for the determination of carbaryl in natural waters using acetylcholinesterase and choline oxidase is described. The flow system designed to implement multicommutation approach controlled by microcomputer comprised five solenoid valves, two columns with immobilized enzymes on controlled pore glass beads and chemiluminometric flow cell. In the best experimental conditions a linear response ranging from 25 to 700 µg L-1 carbaryl was obtained. Water samples were spiked with carbaryl in order to access the accuracy and recoveries between 95 and 101% were obtained for a concentration level ranging from 25 to 100 µg L-1 carbaryl. Detection limit and variation coeffic…
An environmentally friendly multicommutated alternative to the reference method for anionic surfactant determination in water
Abstract It has been developed a fully mechanized procedure for the spectrophotometric determination of anionic surfactants in water expressed in terms of SDS concentration. The reference method, based on the reaction of SDS with methylene blue (MB) followed by extraction in chloroform, was mechanized in order to reduce the consumption of organic solvents. The system was based on the multicommutation approach and provided a 35 times reduction of the waste production without sacrificing the figures of merit of the method in terms of sensitivity and repeatability, for a dynamic linear range from 0.2 to 1.7 mg l−1. Results obtained for washing water samples were comparable with those obtained …
Multi-pumping mechanised determination of selenium in natural waters by light emitting diode (LED) spectrometry
It has been developed a fully mechanised procedure for the determination of selenium in waters employing a LED based spectrometer and solenoid multi-pumps as solution propelling devices. The proposed method is based on the reaction of selenium with potassium iodide in an acidic medium to liberate iodine, which oxidizes Variamine Blue to form a violet-colour species which absorb at 530 nm. The system was mechanised using the multicommutation process and a stopped flow strategy in the final step reaction. The analytical curve was linear between 0.010 and 0.500 mg L-1, with an equation ΔA = 0.501 (± 0.004) C and r = 0.999. The limit of detection (3σ/S) obtained for the proposed method was 0.00…
Multicommutation cold vapour atomic fluorescence determination of Hg in water.
Abstract A multicommutation-based method has been developed for the on-line direct atomic fluorescence spectrometric (AFS) determination of Hg in waters without any previous sample treatment. The performance of the proposed procedure has been compared with that of a conventional AFS system based on continuous mode measurements. In short, the use of multicommutation, together with a reduction of the size of the liquid–gas phase separator, provides an increase of the laboratory productivity by improving the sample throughput by a factor of 3.6 and strongly reduces the sample consumed by a factor of 6 and reagent consumed by a factor of 8.4. The waste generation is reduced by a factor of 2.4 a…
A spectrophotometric flow procedure for the determination of cationic surfactants in natural waters using a solenoid micro-pump for fluid propulsion
An automatic flow-analysis procedure for spectrophotometric determination of cationic surfactants in surface water using a solenoid micro-pump for propelling solutions of reagents and sample is des...
Environmentally friendly analytical chemistry through automation: comparative study of strategies for carbaryl determination with p-aminophenol
Abstract A flow system, based on multicommutation and binary sampling, has been developed for improving the automated spectrophotometric determination of carbaryl with p -aminophenol (PAP) in order to reduce the waste volume and to preserve the maximum analytical performance. The procedure, which was implemented employing a flow network obtained by nesting five, three-way solenoid valves controlled by means of a 386 microcomputer equipped with an electronic interface running software written in quick basic 4.5, provides a limit of detection of 26 μg l −1 , comparable to that obtained using a conventional flow injection (FIA) manifold and lower than that found by sequential injection analysi…
Multicommutation ATR-FTIR: determination of sodium alpha-olefin sulfonate in detergent formulations
Abstract The mechanization of attenuated total reflectance measurements (ATR) in Fourier Transform Infrared spectrometry (FTIR) through the use of multicommutation has been evaluated in order to reduce the sample consumption and waste generation also avoiding risks of cells breaking. A new multicommutation ATR-FTIR procedure has been proposed for the determination of sodium alpha-olefin sulfonate (AOS) in liquid detergent formulations. The main advantages of this method are the low consumption of sample (96 ml per 100 determinations) and the analytical throughput (23 h −1 versus 15 h −1 for the manual mode). Results obtained for reference samples containing 7.52% to 9.52% (w/w) of AOS are i…
Improvement of the atomic fluorescence determination of mercury by using multicommutation
Atomic fluorescence spectrometry (AFS) determination of Hg has been improved by exploiting the possibilities of the multicommutation approach in order to outline a fully mechanised system which supplies the same sensitivity as the use of continuous measurements, reducing drastically the reagents consumed and waste generation. The use of multicommutation with a simultaneous reduction of the liquid–gas separator volume and the insertion point modification of argon transport gas provides a sensitivity of the AFS measurements of 300 mV ng−1 ml (using a full scale of 1000 mV), a limit of detection (3 s) of 1.3 ng l−1 and relative standard deviation values below 0.1% for 10 independent measuremen…
A portable and low cost equipment for flow injection chemiluminescence measurements.
A compact, reliable and low cost flow injection chemiluminescence system is described. The flow system consists of a set of solenoid micro-pumps that can dispense reproductive micro-volumes of solutions. The luminometer was based on a coiled cell constructed from polyethylene tubing that was sandwiched between two large area photodiodes. The whole equipment costs about US$ 750 and weights ca. 3 kg. Equipment performance was evaluated by measuring low concentrations of hydrogen peroxide by oxidation of luminol and for the determination of ammonium, based on its inhibition of the luminescence provided by the reaction of luminol and sodium hypochlorite. Linear responses were achieved within 1.…
Speciation of chromium in natural waters by micropumping multicommutated light emitting diode photometry.
Abstract A simple and sensitive multicommutated flow procedure, implemented by employing a homemade light emitting diode (LED) based photometer, has been developed for the determination of chromium (VI) and total chromium in water. The flow system comprised a set of four solenoid micro-pumps, which were assembled to work as fluid propelling and as commutating devices. The core of the detection unit comprised a green LED source, a photodiode and a homemade flow cell of 100 mm length and 2 mm inner diameter. The photometric procedure for the speciation of chromium in natural waters was based on the reaction of Cr (VI) with 1,5-diphenylcarbazide. Cr (III) was previously oxidized to Cr (VI) and…
A multicommuted stop-flow system employing LEDs-based photometer for the sequential determination of anionic and cationic surfactants in water
It has been developed an automatic stop-flow procedure for sequential photometric determination of anionic and cationic surfactants in a same sample of water. The flow system was based on multicommutation process that was designed employing two solenoid micro-pumps and six solenoid pinch valves, which under microcomputer control carry out fluid propelling and reagent solutions handling. A homemade photometer using a photodiode as detector and two light emitting diodes (LEDs) with emission at 470 nm (blue) and 650 nm (red) as radiation sources, which was tailored to allow the determination of anionic and cationic surfactants in waters. The procedure for anionic surfactant determination was b…
Multi-commutation in spectrometry
We review recent developments in manifold components and the introduction of light-emitting-diode technology in spectroscopic detection in order to evaluate the tremendous possibilities offered by multi-commutation for in-field and in-situ measurements, based on the use of multi-pumping and low-voltage, portable batteries, which make possible a dramatic reduction in size, weight and power requirements of spectrometric devices.
Monitoring of the smoking process by multicommutation Fourier Transform Infrared spectroscopy
Abstract Nicotine was selected as the target molecule for monitoring of the smoking process by multicommutation Fourier Transform Infrared spectroscopy (FTIR). The method involved the use of CHCl3 for on-line extraction of nicotine from tobacco, cigarette filters and tobacco ash from NH4OH alkalinized samples, and absorbance measurement of the characteristic band at 1316 cm−1 in the stopped-flow mode, by obtaining the peak area in the range between 1334 and 1300 cm−1. Under the best operational conditions, the procedure developed provided a detection limit of 0.05 mg mL−1 nicotine, corresponding to 0.5 mg g−1 in the solid sample, a relative standard deviation less than 2.5%, and a sampling …