Your browser doesn't support javascript.
loading
Show: 20 | 50 | 100
Results 1 - 20 de 57
Filter
1.
Rev. otorrinolaringol. cir. cabeza cuello ; 80(1): 97-106, mar. 2020. tab
Article in Spanish | LILACS | ID: biblio-1099209

ABSTRACT

RESUMEN En la actualidad se hace referencia en la bibliografía a una gran variedad de métodos para evaluar la disfunción del conducto faringotimpánico (DCFT), la gran mayoría de ellos requiere de instrumental de alta complejidad y personal altamente capacitado. Pese a lo mencionado, ninguno de dichos métodos ha sido validado como herramienta gold standard para el diagnóstico de esta patología. En este contexto, se presenta una herramienta complementaria para el diagnóstico de la DCFT, el Eustachian Tube Dysfunction Questionnaire -7 ítemes (ETDQ-7); cuestionario autoadministrado que considera 7 preguntas en base a una escala de Likert, fue creado para evaluar la sintomatología asociada a la disfunción del conducto con una puntuación que va desde lo más leve (1 punto) a lo más grave (7 puntos) de acuerdo con los síntomas percibidos, y posee un puntaje máximo de 49 puntos, correspondiente a una disfunción severa. La presente revisión tiene como objetivo buscar, organizar, clasificar y describir la información disponible en publicaciones científicas indexadas sobre el ETDQ-7 como herramienta para el diagnóstico clínico complementario de la DCFT. Se incluyeron 11 artículos científicos que hacen referencia al uso del ETDQ-7 en diferentes países. Los resultados recabados sugieren que el ETDQ-7 sería una valiosa herramienta, de alta sensibilidad, especificidad y validez clínica, que permitiría discriminar la presencia de la DCFT. No se encontró evidencia respecto a la aplicación o validación de este cuestionario en nuestro país.


ABSTRACT At present, great variety of methods are described to evaluate the dysfunction of the pharyngotympanic duct (DCFT), the vast majority of them require highly complex instruments and highly trained personnel. Despite this, none of these methods has been validated as the gold standard for the diagnosis of this pathology. In this context, a complementary tool for the diagnosis of the DCFT is presented. The Eustachian Tube Dysfunction Questionnaire-7 items (ETDQ-7), a self-administered questionnaire that includes 7 questions based on a Likert scale, was created to evaluate the symptomatology associated with the dysfunction of the duet. It is scored ranging from the mildest symptomatology (1 point) to the most severe (7 points), according to the perceived symptoms, with a maximum score of 49 points, corresponding to a severe dysfunction. The present review aims to search, organize, classify and describe the available information in scientific indexed journals about the ETDQ-7 as a tool for complementary diagnosis of the DCFT. Eleven scientific articles were included, referred to the use of ETDQ-7 in different countries, describing it as a valid tool which allows to discriminate the presence of a DCFT.


Subject(s)
Humans , Surveys and Questionnaires , Ear Diseases/diagnosis , Eustachian Tube/physiopathology , Ear Diseases/physiopathology , Self Report
2.
Talanta ; 156-157: 204-208, 2016 Aug 15.
Article in English | MEDLINE | ID: mdl-27260454

ABSTRACT

In this paper, an alternative for handling the organic phase after a dispersive liquid-liquid microextraction using organic solvents lighter than water is presented. It is based on solidification (at -18°C) of the aqueous phase obtained after centrifugation, and the decantation, collection and analysis of the liquid organic layer. The extraction of nicotine in toluene, and its determination in eggplant samples was conducted as a proof of concept. The study has been carried out using standards prepared in water and the formation of the dispersion was assisted by sonication. The organic extract was analysed using gas chromatography coupled to mass spectrometry. Satisfactory analytical figures of merit as: limit of detection (0.4µgL(-1), 2ngg(-1) wet sample), limit of quantification (1.2µgL(-1), 6.5ngg(-1) wet sample), within-day precision (RSD=7%), and linearity interval (up to 384µgL(-1) nicotine) were achieved. It constituted a contribution to the handling of organic extracts after microextraction processes.

4.
Talanta ; 138: 190-195, 2015 Jun 01.
Article in English | MEDLINE | ID: mdl-25863390

ABSTRACT

In this work, dispersive liquid-liquid microextraction (DLLME) method was applied for high performance liquid chromatography (HPLC) determination of 15 PAHs in aqueous matrices.The extraction procedure was automated using a system of multisyringe flow injection analysis coupled to HPLC instrument with fluorescence detector. Factors affecting the extraction process, such as type and volume of extraction and dispersive solvent, extraction time and centrifugation step were investigated thoroughly and optimized utilizing factorial design. The best recovery was achieved using 100 µL of trichloroethylene as the extraction solvent and 900 µL of acetonitrile as the dispersive solvent.The results showed that extraction time has no effect on the recovery of PAHs. The enrichment factors of PAHs were in the range of 86-95 with limits of detection of 0.02-0.6 µg L(-1). The linearity was 0.2-600 µg L(-1) for different PAHs. The relative standard deviation (RSD) for intra- and inter-day of extraction of PAHs were in the range of 1.6-4.7 and 2.1-5.3, respectively, for five measurements.The developed method was used to assess the occurrence of 15 PAHs in tap water, rain waters and river surface waters samples.


Subject(s)
Chromatography, High Pressure Liquid/methods , Liquid Phase Microextraction/methods , Polycyclic Aromatic Hydrocarbons/analysis , Water Pollutants, Chemical/analysis , Polycyclic Aromatic Hydrocarbons/chemistry , Water Pollutants, Chemical/chemistry
5.
Chem Commun (Camb) ; 51(38): 8169-72, 2015 May 11.
Article in English | MEDLINE | ID: mdl-25872979

ABSTRACT

A fully automated method for the controlled growth of metal-organic framework coatings on flow-through functional supports is reported. The obtained hybrid flow-through supports show high performance for the automated extraction of water pollutants.

6.
Anal Chim Acta ; 874: 1-10, 2015 May 18.
Article in English | MEDLINE | ID: mdl-25910440

ABSTRACT

A fully automated modified three-step BCR flow-through sequential extraction method was developed for the fractionation of the arsenic (As) content from agricultural soil based on a multi-syringe flow injection analysis (MSFIA) system coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS). Critical parameters that affect the performance of the automated system were optimized by exploiting a multivariate approach using a Doehlert design. The validation of the flow-based modified-BCR method was carried out by comparison with the conventional BCR method. Thus, the total As content was determined in the following three fractions: fraction 1 (F1), the acid-soluble or interchangeable fraction; fraction 2 (F2), the reducible fraction; and fraction 3 (F3), the oxidizable fraction. The limits of detection (LOD) were 4.0, 3.4, and 23.6 µg L(-1) for F1, F2, and F3, respectively. A wide working concentration range was obtained for the analysis of each fraction, i.e., 0.013-0.800, 0.011-0.900 and 0.079-1.400 mg L(-1) for F1, F2, and F3, respectively. The precision of the automated MSFIA-HG-AFS system, expressed as the relative standard deviation (RSD), was evaluated for a 200 µg L(-1) As standard solution, and RSD values between 5 and 8% were achieved for the three BCR fractions. The new modified three-step BCR flow-based sequential extraction method was satisfactorily applied for arsenic fractionation in real agricultural soil samples from an arsenic-contaminated mining zone to evaluate its extractability. The frequency of analysis of the proposed method was eight times higher than that of the conventional BCR method (6 vs 48 h), and the kinetics of lixiviation were established for each fraction.


Subject(s)
Arsenic/analysis , Chemical Fractionation/methods , Soil Pollutants/analysis , Soil/chemistry , Agriculture , Arsenic/isolation & purification , Chemical Fractionation/instrumentation , Equipment Design , Flow Injection Analysis/instrumentation , Flow Injection Analysis/methods , Limit of Detection , Soil Pollutants/isolation & purification , Spectrometry, Fluorescence/instrumentation , Spectrometry, Fluorescence/methods , Spectrophotometry, Atomic/instrumentation , Spectrophotometry, Atomic/methods
8.
Appl Radiat Isot ; 86: 28-35, 2014 Apr.
Article in English | MEDLINE | ID: mdl-24462943

ABSTRACT

There has been increasing interest recently in the capacity of water treatment plants to concentrate and eliminate radionuclides from raw water. As the normal operation in these plants generates high quantities of sludge, which can be considered a naturally occurring radioactive material, it is important to gather information about its radiological content. Therefore, in order to determine the activity values of two radioactive beta emitters with minimal sample manipulation, an automated lab-on-valve and multisyringe flow injection system has been developed to achieve the sequential preconcentration and separation of (90)Sr and (210)Pb using an extraction chromatographic resin (Sr-spec). Activities of both isotopes were measured by liquid scintillation counting (LSC). The developed method was validated by analyzing three samples from three different intercomparison exercises and good Z-score values (between 0.1 and 1) and trueness values (between 10% and 17%) were obtained. The method was then also satisfactorily applied to sludge samples taken from a Spanish drinking water treatment plant which treats water from the Ebro River. The proposed method offers advantages over existing methods as it allows the sequential separation of both isotopes, simply by changing the elution conditions and using a semi-automated approach. Therefore, the method is less time consuming and environmentally friendly.

9.
Environ Monit Assess ; 185(1): 695-706, 2013 Jan.
Article in English | MEDLINE | ID: mdl-22402991

ABSTRACT

Metals were determined in surface bottom marine sediments of the Bay of Palma de Mallorca (Spain) by microwave-assisted acid-oxidant digestion and inductively coupled plasma-optical emission spectrometry in order to assess the level and distribution of potentially metallic pollutants. Average concentrations found were 1.2 ± 0.3 Al and 1.9 ± 0.9 Fe (in milligrams per gram), and 8 ± 2 Cr, 2 ± 1 Cu, 60 ± 10 Mn, 4 ± 1 Ni, 6 ± 4 Pb, 50 ± 7 Sn and 10 ± 3 Zn (in micrograms per gram). Enrichment factors using normalized values to Al were also calculated which indicated that sediments were Sn and Pb enriched. Sediments were fractionated by grain size: <63, 63-250, 250-500 and >500 (in micrometres), and the metals' affinity towards the different fractions was studied. The metals' affinity to the finer fraction was evidenced, excluding Sn and Mn that showed practically no affinity for fine grains. Latent variables were extracted from the data using principal components analysis. It allowed samples to be grouped in two clusters, and most of the metals (Al, Cr, Cu, Fe, Ni, Pb and Zn) showed a similar distribution pattern. Sn and Mn showed a distinct pattern.


Subject(s)
Geologic Sediments/chemistry , Metals/analysis , Water Pollutants, Chemical/analysis , Bays/chemistry , Environmental Monitoring , Spain , Water Pollution, Chemical/statistics & numerical data
10.
Talanta ; 99: 730-6, 2012 Sep 15.
Article in English | MEDLINE | ID: mdl-22967617

ABSTRACT

In this work, the potential of a membrane optode coupled to a multisyringe flow injection system (MSFIA) was assessed for determining the Cr(VI) concentration in paint samples. The detection is based on the color obtained from the reaction of Cr(VI) with 1,5-diphenylcarbazide in the presence of sulfuric acid (H(2)SO(4)). The redox product was immobilized on a poly(styrene-divinylbenzene) (SDB-XC) membrane optode. The analyte in the sample was then directly quantified at the surface of the disk by measuring the intensity of reflected incident light using a bifurcated optical fiber at 540 nm. Experimental parameters (concentration of reagents, sample volume, flow rate of sample solutions, eluent concentration, and effect of diverse ions) were studied in detail. The overall time required for the complete procedure was 4 min and only required 0.2 mL of the sample volume. The dynamic working response of Cr(VI) was found within the concentration range of 2.4-1000 µg L(-1) with a limit of detection (LOD) of 0.7 µg L(-1), while the relative standard deviation (RSD) for 400 µg L(-1) Cr(VI) was lower than 2% (n=6). This developed method was used to determine Cr(VI) concentrations in the paint samples, for which an alkaline extraction procedure was proposed. The extraction procedure was based on the use of a 7.5% Na(2)CO(3)/5% NaOH solution at 90 °C for 30 min. Under optimal conditions, the recoveries ranged from 99% to 101%. The complete method was validated using a certified reference material (ERA-QC540, soil sample) and by comparing the results with those obtained using atomic absorption spectrometry (AAS).

11.
Talanta ; 96: 140-6, 2012 Jul 15.
Article in English | MEDLINE | ID: mdl-22817941

ABSTRACT

Heavy metals, as cadmium, attract a rising attention in environmental studies due to their increasing release by human activities and acute toxicity. In situ analytical methods are needed to minimize current uncertainties caused by the transport and conservation of samples. Here, we present the completely automatic determination of Cd in natural waters using a newly developed screen printed electrode sensor (SPE), inserted in a homemade purpose-built flow cell coupled to a Multi-Syringe Flow Injection Analysis system (MSFIA). The working electrode of SPEs was constituted by a carbon film modified with Nafion. Cd was plated on an in situ bismuth film and determined using Square Wave Anodic Stripping Voltammetry. Different chemical conditions of deposition and stripping were studied. A sample/acetic buffer mixture was found to be a well suited medium to form the Bi film and perform the analysis. Cd was quantified via calibration by on line standard additions. The limit of detection was found to be 0.79µgL(-1), well below the limit stipulated by the European directive (5µgL(-1)). Good sample throughput (14h(-1)) and low consumption of reagent and sample (1.3mL) were also obtained in line with previous works in Cd flow analysis.


Subject(s)
Cadmium/analysis , Flow Injection Analysis/instrumentation , Printing/instrumentation , Syringes , Water Pollutants, Chemical/analysis , Water/chemistry , Automation , Bismuth/chemistry , Cadmium/chemistry , Carbon/chemistry , Electrochemistry , Electrodes , Ink , Time Factors , Water Pollutants, Chemical/chemistry
12.
Anal Bioanal Chem ; 404(5): 1589-95, 2012 Sep.
Article in English | MEDLINE | ID: mdl-22733249

ABSTRACT

A multisyringe flow-injection approach has been coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) with UV photo-oxidation for dimethylarsinic (DMA), inorganic As and total As determination, depending on the pre-treatment given to the sample (extraction or digestion). The implementation of a UV lamp allows on-line photo-oxidation of DMA and the following arsenic detection, whereas a bypass leads the flow directly to the HG-AFS system, performing inorganic arsenic determination. DMA concentration is calculated by the difference of total inorganic arsenic and measurement of the photo-oxidation step. The detection limits for DMA and inorganic arsenic were 0.09 and 0.47 µg L(-1), respectively. The repeatability values accomplished were of 2.4 and 1.8%, whereas the injection frequencies were 24 and 28 injections per hour for DMA and inorganic arsenic, respectively. This method was validated by means of a solid reference material BCR-627 (muscle of tuna) with good agreement with the certified values. Satisfactory results for DMA and inorganic arsenic determination were obtained in several water matrices. The proposed method offers several advantages, such as increasing the sampling frequency, low detection limits and decreasing reagents and sample consumption, which leads to lower waste generation.

13.
Anal Bioanal Chem ; 403(9): 2705-14, 2012 Jul.
Article in English | MEDLINE | ID: mdl-22585054

ABSTRACT

Simultaneous determination of three herbicides (dicamba, 2,4-D, and atrazine) has been achieved by on-line solid-phase extraction (SPE) coupled to multisyringe chromatography (MSC) with UV detection. The preconcentration conditions were optimized; a preconcentration flow rate of 0.5 mL min(-1) and elution at 0.8 mL min(-1) were the optimum conditions. A C(18) (8 mm i.d.) membrane extraction disk conditioned with 0.3 mol L(-1) HCl in 0.5% MeOH was used. A 3-mL sample was preconcentrated, then eluted with 0.43 mL 40:60 water-MeOH. A C(18) monolithic column (25 mm × 4.6 mm) was used for chromatographic separation. Separation of the three compounds was achieved in 10 min by use of 0.01% aqueous acetic acid-MeOH (60:40) as mobile phase at a flow rate of 0.8 mL min(-1). The limits of detection (LOD) were 13, 57, and 22 µg L(-1) for dicamba, 2,4-D, and atrazine, respectively. The sampling frequency was three analyses per hour, and each analysis consumed only 7.3 mL solvent. The method was applied to spiked water samples, and recovery between 85 and 112% was obtained. Recovery was significantly better than in the conventional HPLC-UV method. These results indicated the reliability and accuracy of this flow-based method. This is the first time this family of herbicides has been simultaneously analyzed by on-line SPE-MSC using a monolithic column.


Subject(s)
2,4-Dichlorophenoxyacetic Acid/isolation & purification , Atrazine/isolation & purification , Dicamba/isolation & purification , Herbicides/isolation & purification , Solid Phase Extraction/instrumentation , Water Pollutants, Chemical/isolation & purification , 2,4-Dichlorophenoxyacetic Acid/analysis , Atrazine/analysis , Chromatography, High Pressure Liquid/instrumentation , Dicamba/analysis , Drinking Water/analysis , Equipment Design , Herbicides/analysis , Limit of Detection , Water Pollutants, Chemical/analysis
14.
Anal Chim Acta ; 708(1-2): 11-8, 2011 Dec 05.
Article in English | MEDLINE | ID: mdl-22093339

ABSTRACT

In this paper, a novel automatic approach for the speciation of inorganic mercury (Hg(2+)), methylmercury (MeHg(+)) and ethylmercury (EtHg(+)) using multisyringe chromatography (MSC) coupled to cold-vapor atomic fluorescence spectrometry (CV/AFS) was developed. For the first time, the separation of mercury species was accomplished on a RP C18 monolithic column using a multi-isocratic elution program. The elution protocol involved the use of 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (99:1, v/v), followed by 0.005% 2-mercapthoethanol in 240 mM ammonium acetate (pH 6)-acetonitrile (90:10, v/v). The eluted mercury species were then oxidized under post-column UV radiation and reduced using tin(II) chloride in an acidic medium. Subsequently, the generated mercury metal were separated from the reaction mixture and further atomized in the flame atomizer and detected by AFS. Under the optimized experimental conditions, the limits of detection (3σ) were found to be 0.03, 0.11 and 0.09 µg L(-1) for MeHg(+), Hg(2+) and EtHg(+), respectively. The relative standard deviation (RSD, n=6) of the peak height for 3, 6 and 3 µg L(-1) of MeHg(+), Hg(2+) and EtHg(+) (as Hg) ranged from 2.4 to 4.0%. Compared with the conventional HPLC-CV/AFS hyphenated systems, the proposed MSC-CV/AFS system permitted a higher sampling frequency and low instrumental and operational costs. The developed method was validated by the determination of a certified reference material DORM-2 (dogfish muscle), and was further applied for the determination of mercury species environmental and biological samples.

15.
Rev. ANACEM (Impresa) ; 5(1): 38-40, oct. 2011. tab
Article in Spanish | LILACS | ID: lil-613294

ABSTRACT

Introducción: El Síndrome de Guillain-Barré (SGB) es una enfermedad autoinmune caracterizada por debilidad muscular, arreflexia y disociación albúmino-citológica en líquido cerebroespinal, cuya incidencia clásica a nivel internacional suele uniformarse alrededor de 0,6 a 4 casos por 100.000 al año. Presentación del caso: Paciente de 45 años, sexo femenino, quien ingresó al Servicio de Urgencia del Hospital de Temuco derivada desde Lonquimay, por debilidad progresiva de las cuatro extremidades. En Lonquimay la paciente requirió sonda vesical por retención urinaria. Es diagnosticada con SGB, hospitalizándose en Unidad de Cuidados Intensivos, requiriendo ventilación asistida y tratada mediante plasmaféresis, presentando neumonía como complicación relacionada a la ventilación mecánica y recuperando íntegramente función vesical. Discusión: El compromiso vesical no es descrito como un factor importante en el diagnóstico, siendo controversial aquella afirmación por varios autores.


Introduction: Guillain-Barre syndrome (GBS) is an autoimmune disease characterized by muscle weakness, areflexia and albumin-cytological dissociation in cerebrospinal fluid, the incidence has been reported to be relatively uniform between 0.6 to 4 cases per 100.000 per year. Case report: Patient of 45 years old, female, admitted to the emergency department of Hospital de Temuco derived from Lonquimay by progressive weakness of four extremities. In Lonquimay the patient required bladder catheterization for urinary retention. It was diagnosed with GBS, hospitalized in intensive care unit, requiring assisted ventilation and treated with plasmapheresis, developing pneumonia as a complication related to mechanical ventilation and fully recovered bladder function. Discussion: The bladder involvement is not described as an important factor in diagnosis and remains controversial this statement by several authors.


Subject(s)
Humans , Female , Middle Aged , Guillain-Barre Syndrome/diagnosis , Guillain-Barre Syndrome/therapy , Urinary Bladder/physiopathology , Plasmapheresis , Polyradiculoneuropathy , Urinary Retention/etiology , Urinary Retention/therapy , Guillain-Barre Syndrome/complications
16.
Anal Chim Acta ; 685(2): 132-7, 2011 Jan 31.
Article in English | MEDLINE | ID: mdl-21168561

ABSTRACT

A device for membrane assisted solvent extraction from an aqueous sample to an organic solvent within a micro-vial compatible with a chromatography auto-sampler was used to extract trace amounts of seven polycyclic aromatic hydrocarbons from seawater. The device consisted in an assembly of a volumetric flask containing the sample and a micro-vial containing the organic solvent by means of a screw stopper in which the septum was replaced by a sized piece of a membrane. Extraction conditions (nature of the organic solvent, extraction time, presence of ethanol in the donor phase, ionic content of the donor phase, characteristics of the membrane and volumes of donor and acceptor phases) were studied in order to find the conditions for maximum extraction. Analytical performance characteristics have also been established. The extraction efficiency was between 12.5 and 23%, which implies an enrichment factor value above 40. The repeatability and reproducibility were in the range of 8.6-10.0% and 13-19%, respectively. Detection limits were in the range of 24-39 ng L(-1). Nine seawater samples have been studied. Most of the concentrations were under the limits of detection. Naphthalene and phenanthrene contents have been determined in a sample using the method of standard additions, and concentrations 100 and 91 ng L(-1), respectively.

17.
Talanta ; 82(1): 137-42, 2010 Jun 30.
Article in English | MEDLINE | ID: mdl-20685448

ABSTRACT

A methodology based on multisyringe chromatography with a monolithic column was developed to determine three sulphonated azo textile dyes: Acid Yellow 23, Acid Yellow 9 and Acid Red 97. An ion pair reagent was needed because of the low affinity between the monolithic column and the anionic dyes. The proposed analytical system is simple, versatile and low-cost and has great flexibility in manifold configuration. The method was optimized through experimentation based on experimental design methodology. For this purpose two blocks of full factorial 2(3) were done sequentially. In the first experimental plan, the factors studied were: the % of acetonitrile in organic phase, the % of H(2)O in the mobile phase and the kind of ion pair reagent. In this stage, a simple configuration was used which has only one syringe for the mobile phase. After the first experimentation, we added a second syringe with a second mobile phase to the multisyringe module and performed a second full factorial 2(3). The factors studied in this case were: the % of acetonitrile in the second mobile phase, the pH and the concentration of ion pair reagent in both mobile phases. After this design, the optimal conditions were selected for obtaining a good resolution between the peaks of yellow dyes (1.47) and the elution of red dye in less than 8 min. The methodology was validated by spiking different amounts of each dye in real water samples, specifically, tap water, well water and water from a biological wastewater lagoon.


Subject(s)
Azo Compounds/analysis , Azo Compounds/chemistry , Chromatography/methods , Coloring Agents/analysis , Coloring Agents/chemistry , Sulfonic Acids/chemistry , Syringes , Calibration , Injections , Reproducibility of Results , Water/chemistry , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry
18.
Talanta ; 81(1-2): 572-7, 2010 Apr 15.
Article in English | MEDLINE | ID: mdl-20188964

ABSTRACT

In the present work, a solid phase extraction (SPE) is hyphenated with an automatic MSFIA system to improve the selenite determination based on the reaction of selenite with aromatic o-diamines (such as 2,3-diaminonaphthalene (DAN)) to form the piazselenol complex. This reaction is greatly influenced by acid concentration, temperature, the time needed for colour development, and presence of foreign ions. For these reasons a thermostatic bath, glycine, and Na(2)-EDTA are used as heater, buffer, and masking agent, respectively. The principle of the determination is based on the sorption of the piazselenol onto a C(18) membrane disk, followed by its elution by acetonitrile. The piazselenol can then be detected by absorptiometry or fluorometry, both detection techniques being tested in our system. The best detection limit (1.7 microg L(-1)) and RSD (3.04%) are obtained by absorptiometry at 380 nm. Environmental samples were spiked and analyzed, with recoveries close to 100%.


Subject(s)
2-Naphthylamine/analogs & derivatives , Flow Injection Analysis/methods , Selenium/analysis , Selenium/chemistry , Solid Phase Extraction/methods , Spectrophotometry/methods , Syringes , 2-Naphthylamine/chemistry , Azoles/chemistry , Environment , Membranes, Artificial , Organoselenium Compounds/chemistry , Reproducibility of Results , Selenium/isolation & purification , Water/chemistry
19.
Talanta ; 79(4): 1011-20, 2009 Sep 15.
Article in English | MEDLINE | ID: mdl-19615501

ABSTRACT

Leading-edge urban solid waste ashing plants use burning heat energy to obtain electrical power. Water fed to their boilers for conversion into steam should be highly pure in order to minimize corrosion, scaling and similar phenomena, which can lead to malfunctioning and a reduced useful life but can be avoided by proper management and control of the water supply. In this work, we developed a multiparameter monitor based on multisyringe sequential injection for the sequential determination of up to eight important parameters, namely: pH, specific and acid conductivity, hydrazine, ammonium, phosphate, silicate and total iron. Acid conductivity was determined by passing the sample through a cation-exchange resin in order to retain ammonium ion and release protons. This parameter was deemed the most accurate indicator of dissolved solids in boiler water. Chemical parameters were determined spectrophotometrically: hydrazine by reaction with p-dimethylaminobenzaldehyde, ammonium by the modified Berthelot reaction, iron with o-phenanthroline, and phosphate and silica by formation of a molybdoheteropoly blue dye in the presence of ascorbic acid as reductant. Use of the optimum chemical and physical operating conditions provided 3s(blank) detection limits of 0.01 mg l(-1) N(2)H(4), 0.13 mg l(-1) NH(4)(+), 0.04 mg l(-1) Fe, 0.03 mg l(-1) SiO2 and 0.05 mg l(-1) PO(4)(3-), and relative standard deviations not greater than 2.5%. The methods integrated in the proposed monitor were successfully applied to real samples from the water-steam cycle at the Son Reus ashing plant in Palma de Mallorca (Spain).

20.
Talanta ; 78(3): 790-4, 2009 May 15.
Article in English | MEDLINE | ID: mdl-19269429

ABSTRACT

A new methodology for the in-line preconcentration, clean-up and speciation of mercury by use of an anion-exchange membrane is proposed. The speciation of mercury is based on retention of its tetrachloro complex onto the membrane while organic mercury flows freely through it. A multisyringe is used as a liquid driver and a cold vapour atomic fluorescence detector is employed to ensure a high sensitivity. Organic mercury is decomposed into to inorganic mercury by using a UV lamp. The carrier and reductant streams consist of 1.5% (m/v) hydrochloric acid and 2% (m/v) tin chloride, respectively. Certified reference material DORM-2 was digested with 37% hydrochloric acid and analysed directly without the need for extraction. The proposed system is more environmental friendly than the classical liquid-liquid extraction procedure. Mercury recoveries from spiked samples and the reference material were all close to 100%. An LOD of 14 and 16 ng/L was obtained for total and organic mercury, respectively, both with an RSD less than 1.3%.


Subject(s)
Ion Exchange , Mercury/isolation & purification , Organomercury Compounds/isolation & purification , Green Chemistry Technology , Membranes, Artificial , Mercury/analysis , Methods , Organomercury Compounds/analysis , Reference Standards
SELECTION OF CITATIONS
SEARCH DETAIL
...