Chronic Urticaria After Implantation of a Mitral Annuloplasty Ring in a Nickel-Allergic Patient

Flow injection-spectrophotometric determination of cresol compounds in water by reaction withp-aminophenol

A spectrophotometric method has been developed for the simultaneous determination ofo-cresol andm-cresol in water by reaction withp-aminophenol (PAP). Three different methodologies have been assayed; (i) batch analysis, after reaction in an alkaline medium in the presence of dissolved molecular oxygen as oxidizing agent, (ii) a stopped-flow procedure, carried out in the presence of KIO4 and (iii) a flow injection method based on the same approach. The batch procedure requires 22 min for the full development of colour witho-cresol and 12 min form-cresol. In the stopped-flow mode, using KIO4 and a reaction time of 12 min, better sensitivity can be obtained for both compounds and limits of det…

LaboratorioRPGDocente: Un game-based learning para combatir la situación causada por la COVID-19 en instituciones educativas.

[EN] Due to the pandemic caused by COVID-19, several educational institutions have been forced to close their facilities, and practical courses -such as laboratory practices- were impossible to carry out. Game-based learning can be found among many different digital learning techniques, and it consists in teaching the contents as a transversal inmersive element. This work will be focused on a simulation videogame, which allows the students to understand the simulated environment and to develop certain skills based on their interaction with the game interface. One of the main characteristics of these kind of video games is their high degree of realism. More specifically, in this project, stu…

Direct determination by portable ED-XRF of mineral profile in cocoa powder samples

Abstract The present study has exploited the rapidity of the analysis and the multi-elemental capability of the energy dispersive X- ray fluorescence (ED-XRF) technique for the mineral profile determination in cocoa powder. A fast, cheap and environmental sustainable method without reagent consumption or toxic waste generation has been proposed. The samples can be prepared in the form of pellets of 13 mm in diameter and 2–3 mm thickness. The different internal calibrations used by ED-XRF equipment did not provide accurate results when comparing the mineral profile with the concentration obtained by Inductively Couple Plasma Optical Emission Spectroscopy (ICP-OES) after microwave assisted di…

Green methodology for quality control of elemental content of infant milk powder

Abstract A green methodology for the direct determination of elemental content in infant milk powder samples from 0 to 3 years was developed. A portable energy dispersive X-ray fluorescence (ED-XRF) tool has been used as a direct method for the quantification of five essential elements (Ca, K, Fe, Cu and Zn). For analysis pellets from 0.8 g of each sample weight were made and analyzed. Due to the high dependence of the ED-XRF signal with the sample matrix, external calibrations using cocoa powder diluted with glucose were performed. Infant milk samples were diluted with lactose and the signals were interpolated in the external calibrations. Concentrations obtained by ED-XRF were compared wi…

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…

Electrothermal Atomic Absorption Determination of Chromium in Sediments

Abstract An electrothermal atomic absorption spectrometric method has been developed to determine total chromium concentration in natural sediment samples. Samples were mineralized by dry ashing at 550°C and fused at 1100°C for 30 min with lithium metaborate. Dissolved samples were injected in graphite tubes, mineralized at 1100°C, and atomized at 2600°C. Standard addition calibration made unnecessary the use of chemical modifiers. The method provided a limit of detection from 23 to 45 ng liter −1 . The relative standard deviation for chromium determination was between 3 and 14%. Results obtained for a standard reference material agree well with the certified value. A series of natural samp…

Chromium speciation in liquid matrices: a survey of the literature

A thorough review of the literature published (1983 - March 1999) on chromium speciation in liquid samples is presented, and analytical techniques used in the 404 articles are summarized. The discussion focuses on atomic spectrometric techniques, which are mainly employed for chromium speciation in liquid matrices (134 articles). Details on the type of pretreatment, species, samples, techniques and analytical features of the methodologies proposed are given.

Sample Preparation Improvement in Polycyclic Aromatic Hydrocarbons Determination in Olive Oils by Gel Permeation Chromatography and Liquid Chromatography with Fluorescence Detection

Abstract The determination of 15 polycyclic aromatic hydrocarbons (PAHs) in olive oil samples has been improved in order to obtain a fast methodology with a low limit of detection through the combination of liquid–liquid extraction with acetonitrile and preparative gel permeation chromatography (GPC) prior to the injection of purified extracts into a C18 column. Acetonitrile–water was used as the mobile phase with a gradient from 50 to 95%, w/w, acetonitrile in 30 min. The oven temperature was maintained at 15°C, and fluorometric detection was made at a fixed excitation wavelength of 264 nm and variable, optimal emission wavelength for each analyte ranging from 352 nm for 11-H-benzo(b)fluor…

Microwave muffle furnace assisted decomposition of vegetable samples for flame atomic spectrometric determination of Ca, Mg, K, Fe, Mn and Zn

Calcium, magnesium, potassium, iron, manganese and zinc can be accurately determined in vegetable samples by flame atomic absorption and flame emission spectrophotometry after a previous dry ashing of the sample in a microwave muffle furnace. This treatment is carried out in 45 min using a new accessory developed by us to obtain high temperatures on a domestic microwave oven. Sample ashes, obtained in the muffle, are diluted with nitric acid and the obtained slurry is introduced directly into an air-C2H2 flame for the analysis of Fe, Mn, and Zn, or injected into a double-channel FIA manifold to determine Ca, Mg and K. The obtained results agree with those certified and also with those obtai…

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…

Preliminary results on the influence of car characteristics on their gases emissions using gas sensors

Abstract A method, based on the use of monitoring portable sensors, has been successfully employed for the determination of the composition of car exhausts from 11 diesel and 5 gasoline cars. These emissions include nitrogen oxides (NOx), carbon monoxide (CO), carbon dioxide (CO2) and volatile organic compounds (VOCs). The measures were taken in different places where each car was parked. In this study it has been tried to correlate the emitted gases with some of the car characteristics, such as the power (varied from 68 to 143 HP), the number of kilometers traveled and the age of the car (between 2 and 19 years). Results found show a significant variation of the emission values, which rang…

Spectrophotometric determination of phenol and resorcinol by reaction with p-aminophenol

Abstract Based on the reaction with p-aminophenol, a series of procedures have been developed for the spectrophotometric determination of phenol and resorcinol. Three basic approaches have been studied: (i) a batch procedure, using the dissolved oxygen as oxidant, (ii) a stopped-flow procedure by use of KIO4 as oxidant and (iii) a flow injection (FI) procedure developed in the presence of KIO4. Phenol can be accurately determined at 626 nm, in the stopped-flow mode, after a reaction time of 45 min in 0.005M NaOH, 0.004M KIO4 and 500 μg/ml of PAP. The development of a manifold, which incorporates a sample parking, is a convenient approach which makes it possible to measure, in the stopped-fl…

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…

Scientometric Picture of the Evolution of the Literature of Automation in Spectroscopy and Its Current State

Abstract The current study focuses on the status of automation and mechanization in spectroscopy for analytical chemistry publications compiled during the period 1980–2006, in Analytical Abstracts. Flow injection analysis (FIA), sequential injection analysis (SIA), multicommutation, and monosegmented and segmented flow strategies were considered. For assessing the evolution of scientific productivity, the total number of publications concerned with the different methodologies was evaluated. In order to provide a picture of the state of the art of this field, the most important journals, the most active authors, and the most productive countries in the field of automation were evaluated in t…

Multicommutation as an environmentally friendly analytical tool in the hydride generation atomic fluorescence determination of tellurium in milk.

The aim of this study is to show the advantages of the emerging multicommutation methodology based on the use of solenoid valves for Te determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS). The delivery of a series of alternating sequential insertions of small volumes of samples and reagents gives rise to new hydrodynamic processes and exciting analytical potentials by controlling the time of flow through the on/off-switched solenoid valves. This drastically reduces the reagent consumption by a factor of 4 and the generation of effluents (590 mL h(-1) instead of 750 mL h(-1) generated by the continuous-mode measurement) and also provides an improvement in th…

Multipumping Nitrite Determination in Exhaled Breath Condensate

Abstract A flow system based on multicommutation is proposed for the rapid, clean, and inexpensive determination of nitrites in small volumes of breath condensates. The procedure exploits the colorimetric detection of nitrite with the Griess reagent [0.03% naphthylethylene diamine dihydrochloride (NED), 0.5% sulpfhanilamide, and 3.0% phosphoric acid] in acidic medium at 540 nm correcting the variations of the baseline with measurements at 424 nm. The flow system was designed with a set of solenoid micropumps to minimize sample and reagent consumption and waste generation. The detection limit was estimated as 3.8 ng mL−1 (99.7% confidence level) with a linear response ranging up to 500 ng mL…

Flow injection flame atomic spectrometric determination of iron, calcium, magnesium, sodium and potassium in ceramic materials by using a variable-volume injector

A series of different ceramic materials, such as porcelain, feldspar, kaolin, varnish, clay and stoneware have been analyzed. Iron, calcium and magnesium have been determined in these materials by flame atomic absorption and sodium and potassium by flame emission. The use of a variable-volume injector enables one to carry out these analyses in a flow system (after fusion of samples with lithium metaborate) and does not require different dilutions for the determination of each type of sample considered, nor the use of different flow injection manifolds. The developed procedure provides a limit of detection of 100 μg/l for Na, 70 μg/l for Ca, 50 μg/l for both Fe and K and 8 μg/l for Mg. The c…

Analytical methodologies for chromium speciation in solid matrices: a survey of literature

The analytical literature about chromium speciation in solid samples has been surveyed. From 451 articles published on the speciation of chromium from 1983 to 1997, the methodologies to do speciation in solids after sample pretreatment are discussed, through consideration of the types of samples and their dissolution, the analytical techniques employed for chromium measurement, and the figures of merit of the 86 papers reported in the Analytical Abstracts data base.

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...

Multicommutation-NIR determination of Hexythiazox in pesticide formulations.

A multicommutated flow-system was designed in order to increase analytical throughput and for controlling thermal effects on the NIR spectra for determination of Hexythiazox in pesticide formulations. An on-line standard addition was carried out showing the versatility and repeatability of multicommutation for the on-line mixing and dilution of solutions. Results obtained for commercial samples were statistically comparable with those obtained by an HPLC-reference method. Multicommutation-NIR allows the analysis of 52 samples per hour, in front of the 30 samples per hour analyzed by the NIR-batch procedure and the 7 samples per hour analyzed by HPLC-reference method.

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…

Simultaneous Kinetic Determination of Carbamate Pesticides after Derivatization withp-Aminophenol by Using Partial Least Squares

Abstract A method has been developed for the fast spectrophotometric determination of propoxur, carbaryl, and ethiofencarb in water samples using injection analysis in the stopped-flow mode. The method is based on the reaction between p -aminophenol and the phenolic compounds obtained from the pesticides, after a previous hydrolysis with 0.05 M NaOH at room temperature for 15 min. The partial least-squares treatment of the spectrophotometry kinetic data provides a simultaneous determination of the three carbamate pesticides assayed with a relative accuracy error lower than 5% in complex mixtures also containing formetanate, which is only partially hydrolyzed under the experimental condition…

Extraction of polycyclic aromatic hydrocarbons from cookies: a comparative study of ultrasound and microwave-assisted procedures.

The chromatographic determination of 15 polycyclic aromatic hydrocarbons (PAHs) in cookies has been improved in order to obtain a fast method with a low limit of detection through the combination of microwave-assisted extraction (MAE), oil saponification and solid-phase extraction clean-up before the injection of purified extracts in a C18 201TP52 (5 microm, 250 x 2.1 mm) column. Using acetonitrile-water as mobile phase, with a 50% to 95% w/w acetonitrile gradient for a fixed flow of 0.250 ml min(-1), 15 PAHs were separated in 45 min. The column temperature was maintained at 15 degrees C; and fluorimetric detection was made at a fixed excitation wavelength of 264 nm and emission measurement…

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…

A clean analytical method for the spectrophotometric determination of formetanate incorporating an on-line microwave assisted hydrolysis step

Abstract A fast and completely automated procedure is proposed for the spectrophotometric determination of formetanate in waters by means of its reaction with p-aminophenol (PAP). The method involves the on-line alkaline hydrolysis of formetanate to m-aminophenol (MAP) and its reaction, in the presence of KIO 4 as oxidant agent, with the quinoneimine form of PAP, to form a blue indophenol dye which absorbs at 576 nm. The on-line hydrolysis can be carried out in a 6 m reaction coil located inside the cavity of a domestic microwave oven operated at 650 W, or in a 4 m reaction coil located inside the cavity of a Microdigest 301 microwave system operated at 60 W and allows us, in both cases, a …

Partial least squares modelization of energy dispersive X-ray fluorescence.

As a proof of concept, a green methodology has been developed for the energy dispersive X-ray fluorescence (ED-XRF) determination of calcium, potassium, iron, magnesium, aluminum, chromium, strontium, phosphorus and nickel in the peel of untreated kaki fruit (Diospyros kaki. L) samples. ED-XRF spectra of fifty-six kakis purchased in the local area of LLombay (Valencia) were obtained directly from samples without any previous treatment and without sample damage just after cleaning the fruit with distilled water. Inductively Couple Plasma Optical Emission Spectrometry (ICP-OES) was used as a reference method to determine the mineral elements after microwave assisted acid digestion. XRF spectr…

A multicommuted flow system with solenoid micro-pumps for paraquat determination in natural waters.

A flow system designed with solenoid micro-pumps is proposed for the determination of paraquat in natural waters. The procedure involves the reaction of paraquat with dehydroascorbic acid followed by spectrophotometric measurements. The proposed procedure minimizes the main drawbacks related to the standard chromatographic procedure and to flow analysis and manual methods with spectrophotometric detection based on the reaction with sodium dithionite, i.e. high solvent consumption and waste generation and low sampling rate for chromatography and high instability of the reagent in the spectrophotometric procedures. A home-made 10-cm optical-path flow cell was employed for improving sensitivit…

Determination of total arsenic in soft drinks by hydride generation atomic fluorescence spectrometry

Abstract A highly sensitive and simple method has been developed for the determination of total arsenic, by continuous hydride generation and atomic fluorescence spectrometry (HGAFS), in refreshing drink samples as colas, teas and fruit juices. Samples were mixed with concentrated HCl and KI to obtain final concentrations of 2 mol l−1 and 1%, respectively. These solutions were aspirated and merged with a reducing NaBH4 3% (m/v) solution, with sample and NaBH4 flow rates of 12.5 and 1.5 ml min−1, respectively. The hydride generated in a 170 cm reaction coil was transported to the detector with an Ar flow of 400 ml min−1. The recovery values of added concentrations, from 0.1 to 0.9 ng ml−1, o…

A multicommutated flow system for determination of bismuth in milk shakes by hydride generation atomic fluorescence spectrometry incorporating on-line neutralization of waste effluent

Abstract A highly sensitive method was developed for determination of bismuth in milk shakes by multicommutation hydride generation atomic fluorescence spectrometry (HG-AFS) based on off-line sonication for 10 min with aqua regia 8% (v/v) and on-line waste treatment. The instrumentation and chemistry variables were studied in order to provide the best performance. The limit of detection in the original samples, established for a probability level of 99.6% (k = 3), was 1.67 ng/g Bi. The method provides a fast alternative in control analysis with a sampling throughput of 72 h as compared with 31 h obtained by the classical continuous measurement. Additionally, multicommutation reduces waste g…

A clean method for flow injection spectrophotometric determination of cyclamate in table sweeteners

Abstract A flow system based on the multicommutation is proposed for fast and clean determination of cyclamate. The procedure exploits the reaction of cyclamate with nitrite in acidic medium and the spectrophotometric determination of the excess of nitrite by iodometry. The flow system was designed with a set of solenoid micro-pumps to minimize reagent consumption and waste generation. The detection limit was estimated as 30 μmol L −1 (99.7% confidence level) with linear response ranging up to 3.0 mmol L −1 . The coefficient of variation was estimated as 1.7% for a solution containing 2.0 mmol L −1 cyclamate ( n  = 20). About 60 samples can be analyzed per hour, consuming only 3 mg KI and 1…

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…

Atomic fluorescence determination of total and inorganic arsenic species in beer

A simple and nearly direct procedure has been developed for the determination of As in beers, based on hydride generation and atomic fluorescence detection. Using 2 mol l−1 HCl with a carrier flow of 6 ml min−1, 3% m/v NaBH4 with a flow of 1.3 ml min−1, a reaction coil of 200 cm and an argon flow of 400 ml min−1, total arsenic in beer could be determined in samples diluted 1∶10 with a final concentration of 2 mol l−1 HCl, 1% m/v KI and 0.08% v/v of an antifoam agent. For the estimation of AsIII and AsV concentrations in beer samples, the difference between the analytical sensitivities of the fluorescence signals obtained for As hydride, without and with previous treatment of samples with KI…

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.…

Rapid microwave assisted hydrolysis of formetanate

Abstract A fast microwave-assisted hydrolysis procedure has been developed for the derivatization of formetanate previously to the flow-injection spectrophotometric determination of m -aminophenol by reaction with p -aminophenol. Formetanate is quantitatively hydrolyzed with 0.1 M NaOH in 150 s using a closed polyetrafluoroethylene reactor with 115 ml internal volume and a radiation power of 390 W. The above procedure has been applied, as a previous step, for the flow-injection spectrophotometric determination of formetanate in spiked water samples and accurate and precise results have been found. The method permits to obtain a limit of detection of 0.025 mg 1 −1 of formetanate. The relativ…

Use of semipermeable membrane devices for assessment of air quality in Tangier (Morocco)

Semipermeable membrane devices (SPMDs) have been used for the evaluation of the contamination of air in both the urban and the industrial area in Tangier (Morocco). Benzene, toluene, ethylbenzene a...

Atomic fluorescence spectrometric determination of trace amounts of arsenic and antimony in drinking water by continuous hydride generation

A highly sensitive and simple method has been developed for the determination of As(III), total As, Sb(III) and total Sb in drinking water samples by continuous hydride generation and atomic fluorescence spectrometry (HGAFS). For As determination, water samples aspirated in a carrier of 2 mol l(-1) HCl were merged with a reducing NaBH(4) 3%(m/v) solution, with sample and NaBH(4) flow rates of 12.5 and 1.5 ml min(-1) respectively. The hydride generated in a 170 cm reaction coil was transported to the detector with an Ar flow of 400 ml min(-1), and a limit of detection between 5 and 20 ng l(-1) was obtained. For Sb determination, 2.5 mol l(-1) HCl and 2%(m/v) NaBH(4) were employed, with respe…

Mineral profiles of legumes and fruits through partial least squares energy dispersive X-ray fluorescence

Abstarct Energy dispersive X-ray fluorescence (ED-XRF) has been employed for the determination of mineral elements in 15 varieties of legumes and 14 cherry samples. ED-XRF signals directly obtained from pulverized samples were modelized by partial least squares (PLS) using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) of a selected number of samples, after microwave assisted acid digestion, as reference data. Models were built to predict the concentration of Al, Ca, Cu, Fe, K, Mg, P, Sr and Zn. Average concentrations predicted were 6, 930, 7, 40, 6400, 990, 2100, 4 and 15 μg g−1 for Al, Ca, Cu, Fe, K, Mg, P, Sr and Zn, respectively with relative errors from 7 till 26%. …

Multicommutation Fourier transform infrared determination of benzene in gasoline

A fully mechanized method to determine benzene in motor gasolines has been developed based on the use of Fourier transform infrared spectroscopy (FT-IR) and multicommutation. The flow network comprised a set of three-way solenoid valves and was controlled by means of a microcomputer furnished with an electronic interface and running by a software written in QUICK BASIC 4.5. The flow network and control software were designed to implement the multicommutation approach providing facilities to handle sample and reagent solutions, so that, sample dilution, external calibration and standard addition could be easily performed on-line. The method permits the direct determination of benzene without…

Trace element determination in sediments: a comparative study between neutron activation analysis (NAA) and inductively coupled plasma-mass spectrometry (ICP-MS)

An inductively coupled plasma-mass spectrometry (ICP-MS) method has been employed for trace element determination in five real sediment samples and a standard reference material. These samples were mineralized by dry ashing at 550°C and fused at 1100°C for 30 min with lithium metaborate. Dissolved samples were measured by a semiquantitative methodology with external calibration and with Rh as an internal standard. More than 50 elements have been measured. As a reference technique, a direct analysis of the solid samples was carried out by neutron activation analysis. Results obtained by ICP-MS have been compared with those obtained by neutron activation analysis (NAA) by applying the paired …

Cold vapour atomic fluorescence determination of mercury in milk by slurry sampling using multicommutation

Abstract A highly sensitive mechanized method has been developed for the determination of mercury in milk by atomic fluorescence spectrometry (AFS). Samples were sonicated for 10 min in an ultrasound water bath in the presence of 8% (v/v) aqua regia, 2% (v/v) antifoam A and 1% (m/v) hydroxilamine hydrochloride, and after that, they were treated with 8 mmol l −1 KBr and 1.6 mmol l −1 KBrO 3 in an hydrochloric medium. Atomic fluorescence measurements were made by multicommutation, which provides a fast alternative in quality control analysis, due to the easy treatment of a large number of samples (approximately 70 h −1 ), and is an environmentally friendly procedure, which involves a waste ge…

Preconcentration of aluminium by micellar-enhanced ultrafiltration

Abstract Traces of aluminium were preconcentrated in water samples by forming a complex with lumogallion, and successfully accumulated in the micellar phase obtained from cationic or non-ionic surfactants and filtered through 10 000 molecular weight cut-off ultrafiltration membranes. Studies indicated that, at pH 5.9, with 1 X 10 −3 M lumogallion and 2 X 10 −2 M cetyltrimethylamonium bromide, quantitative retention of aluminium present at μg ml −1 concentration levels was achieved. A micellar-enhanced fluorimetric procedure was employed to analyse the permeate solutions, whereas nitrous oxide-acetylene flame atomic emission spectrometry was used to determine aluminium in the retentate. The …

Clean analytical method for the determination of propoxur

Abstract A method has been developed for the determination of propoxur, a carbamate pesticide, by means of its reaction with p-aminophenol (PAP). The method involves the reaction, in the presence of KIO4, between the quinoneimine form of PAP and the deprotonated form of 2-isopropoxyphenol, obtained by the alkaline hydrolysis of propoxur, to provide an indophenol dye which absorbs at 600 nm. The analysis is carried out in a flow system and, after the measurement step, the waste, the reaction product and the unreacted derivatising agent is detoxified in a UV-irradiated coil placed after the measurement flow-cell and after mixing the waste with a TiO2(anatase) catalyst slurry, which can be reu…

Evaluation of extraction alternatives for Fourier transform infrared spectrometric determination of oil and greases in water

Abstract Liquid-liquid extraction (LLE), solid phase extraction (SPE) and microwave-assisted extraction are evaluated for Fourier transform infrared (FTIR) spectrometric determination of oil and grease in polluted waters. A fast microwave-assisted quantitative procedure is proposed for the total extraction of oil and grease into CCl 4 from water samples, with an irradiation time of 1 min at an exit power of 520 W using closed PTFE vessels. The FTIR quantification of oil and grease is carried out by the measurement of the area under the absorbance spectra in the range between 3058 and 2780 cm −1 , with a baseline established between 3200 and 2700 cm −1 . The analytical features of the propos…

Continuous monitoring of photocatalytic treatment by flow injection. Degradation of dicamba in aqueous TiO2 dispersions

The possible use of flow injection (FI) to monitor the photocatalytic mineralization of dicamba (3,6-dichloro-2-methoxybenzoic acid) present at the trace level in aqueous solutions containing TiO2 suspensions has been evaluated. Experiments were performed in a stirred photochemical reactor equipped with a simple FI manifold, integrating an online filtration unit able to perform the monitoring of the UV absorbance of the irradiated solution every 4 min. The light source used was a medium pressure mercury lamp (125 W). During the initial steps of the reaction the formation of UV absorbing intermediates, which completely disappear in less than 80 min, was evidenced. Additional HPLC, DOC and ch…

Chromium speciation using activated alumina microcolumns and sequential injection analysis-flame atomic absorption spectrometry

Abstract A new procedure has been developed for chromium speciation in water by sequential injection analysis and flame atomic absorption spectrometry. The method involves the online retention of Cr(VI) anionic species and Cr(III) cationic species on alumina microcolumns, prepared by packing activated alumina in polytetrafluoroethylene tubes, followed by selective elution of Cr(VI) with 2 mol l −1 NH 4 OH and of Cr(III) with 0.2 mol l −1 HNO 3 . Studies were carried out on the effect of retention and elution conditions for both Cr species. The limit of detection values, established as the concentration corresponding to three times the standard deviation of blank measurements divided by the …

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.

Smartphone determination of fat in cured meat products

Abstract A method has been developed to determine the fat content in different cold meat products by image processing using the camera of a mobile phone. Salchichon , chorizo , salami and cured ham pictures were taken with a Meizu M2 Mini mobile phone camera under fixed lighting conditions of the light emitting diode flash of the mobile phone. Images were treated with Matlab to obtain the mean pixels of average red, green and blue camera values colours (RGB) of the pixels and different data pretreatments were taken into account to correlate colour parameters with fat content values determined in a series of commercially available samples by the Soxhlet method. RGB values were used as input …

Multicommutation hydride generation atomic fluorescence determination of inorganic tellurium species in milk

Abstract A multicommutated flow system has been developed for hydride generation, atomic fluorescence (HG-AFS) determination of tellurate (Te VI ) and tellurite (Te IV ) in milk samples. After a batch leaching of Te by sonication at room temperature for 10 min with aqua regia, sample slurries in acidic medium were merged with sodium borohydride and HCl to obtain data on Te IV . Another portion of the acidic slurry was mixed with KBr and passed through a reaction coil introduced inside a microwave oven to reduce quantitatively Te VI to Te IV which was analyzed by HG-AFS. The detection limit was 0.57 ng g −1 in the original samples. The linear range obtained was till 4 ng ml −1 and the averag…

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 …

Evaluation of the Soil Contamination of Tangier (Morocco) by the Determination of BTEX, PCBs, and PAHs

Benzene, toluene, ethylbenzene, and xylenes (BTEX), twelve polycyclic aromatic hydrocarbons (PAHs) and seven polychlorinated biphenyls (PCBs), were selected as pollutants to evaluate the contamination of soils in the urban and industrial areas of Tangier (Morocco). PAHs and PCBs were determined by gas chromatography-mass spectrometry (GC-MS) after a microwave-assisted extraction (MAE) and gel permeation chromatography (GPC) clean-up. BTEX were directly determined by head-space GC-MS. Results obtained in this study show the presence of high levels of BTEX and PAHs in the soil near the urban waste deposit. However, the analysis of pollutants in the other sampling sites provided comprehensive …