Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 43
Filtrar
1.
Anal Chim Acta ; 1290: 342208, 2024 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-38246743

RESUMO

Herein, the proof-of-concept of a novel lab-in-syringe (LIS) foam microextraction platform is presented as a front-end to cold vapor atomic absorption spectrometry (CVAAS) for the simultaneous preconcentration and membraneless gas-liquid separation (GLS) of inorganic mercury in biological samples. The proposed method is based on the on-line formation of the ammonium pyrrolidine dithiocarbamate complex with mercury that was retained in the pores of polyurethane foam immobilized on the piston of the LIS system. Metal complex elution and in situ mercury vapor generation are accomplished inside the microsyringe in a flow-batch format, while the separation of vapor species is achieved via the membraneless GLS found at the top of the syringe's barrel. Under optimized operation conditions, for 90 s preconcentration time, the limit of detection was 0.02 µg L-1 and the repeatability (RSD) was 3.8% (at the 0.5 µg L-1 concentration level), within a working range extending up to 4.0 µg L-1. The practicality of the novel manifold was demonstrated using the Blue Applicability Grade Index, while the accuracy of the method was evaluated using certified reference materials and spiked samples.

2.
Talanta ; 269: 125492, 2024 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-38042142

RESUMO

A novel fully automatic continuous flow polyurethane foam solid phase microextraction lab-in-syringe system for on-line sample preconcentration/separation has been developed as a front-end to flame atomic absorption spectrometry. For the first time lab-in-syringe in continuous flow has been adopted for the determination of toxic metals. The microextraction procedure was performed after on-line metal complexation with ammonium pyrrolidine dithiocarbamate, while the elution was conducted by 400 µL of methyl isobutyl ketone. The main chemical and hydrodynamic factors that affected the performance of the method were optimized using Cd and Pb as model analytes. For 90 s preconcentration time, the limits of the detection were 0.20 and 1.7 µg L-1 for Cd and Pb, respectively, while the enhancement factors were 79 for Cd and 150 for Pb. The relative standard deviation% values were lower than 2.8 % for all analytes. As a proof-of-concept the proposed system was used for environmental water analysis, providing relative recoveries within the range of 94.0 and 104.4 %. The Green Analytical Procedure Index and Blue Applicability Grade Index proved reduced environmental impact and high practicality for the proposed method.

3.
Anal Chim Acta ; 1268: 341400, 2023 Aug 08.
Artigo em Inglês | MEDLINE | ID: mdl-37268341

RESUMO

The proof-of-concept of an integrated automatic foam microextraction lab-in-syringe (FME-LIS) platform coupled to high performance liquid chromatography is presented. Three different sol-gel coated foams were synthesized, characterized, and conveniently packed inside the glass barrel of the LIS syringe pump, as an alternative approach for sample preparation, preconcentration and separation. The proposed system efficiently combines the inherent benefits of lab-in-syringe technique, the good features of sol-gel sorbents, the versatile nature of foams/sponges, as well as the advantages of automatic systems. Bisphenol A (BPA) was used as model analyte, due to the increasing concern for the migration of this compound from household containers. The main parameters that affect the extraction performance of the system were optimized and the proposed method was validated. The limit of detection for BPA were 0.5 and 2.9 µg L-1, for a sample volume of 50 mL and 10 mL, respectively. The intra-day precision was <4.7% and the inter-day precision was <5.1% in all cases. The performance of the proposed methodology was evaluated for the migration studies of BPA using different food simulants, as well as for the analysis of drinking water. Good method applicability was observed based on the relative recovery studies (93-103%).

4.
Molecules ; 28(5)2023 Feb 23.
Artigo em Inglês | MEDLINE | ID: mdl-36903348

RESUMO

Sol-gel graphene oxide-coated polyester fabric platforms were synthesized and used for the on-line sequential injection fabric disk sorptive extraction (SI-FDSE) of toxic (i.e., Cd(II), Cu(II) and Pb(II)) metals in different distilled spirit drinks prior to their determination by electrothermal atomic absorption spectrometry (ETAAS). The main parameters that could potentially influence the extraction efficiency of the automatic on-line column preconcentration system were optimized and the SI-FDSE-ETAAS method was validated. Under optimum conditions, enhancement factors of 38, 120 and 85 were achieved for Cd(II), Cu(II) and Pb(II), respectively. Method precision (in terms of relative standard deviation) was lower than 2.9% for all analytes. The limits of detection for Cd(II), Cu(II) and Pb(II) were 1.9, 7.1 and 17.3 ng L-1, respectively. As a proof of concept, the proposed protocol was employed for the monitoring of Cd(II), Cu(II), and Pb(II) in distilled spirit drinks of different types.


Assuntos
Cádmio , Grafite , Chumbo
5.
Anal Chem ; 94(38): 12943-12947, 2022 09 27.
Artigo em Inglês | MEDLINE | ID: mdl-36098462

RESUMO

A novel dual lab-in-syringe flow-batch (D-LIS-FB) platform for automatic fabric-disk-in-syringe sorptive extraction followed by oxidative back-extraction as a front end to inductively coupled plasma atomic emission spectrometry (ICP-AES) is presented for the first time. Sol-gel poly(caprolactone)-poly(dimethylsiloxane)-poly(caprolactone)-coated polyester fabric disks were packed at the top of the glass barrel of a microsyringe pump as an alternative to column preconcentration. Herein lie multiple significant advantages including effectiveness, compactness, lower back-pressure, and lower time of analysis. Copper, lead, and cadmium were used as model analytes for the exploration of the capabilities of the developed platform. The online retained metal-diethyldithiophosphate complexes were eluted using diisopropyl ketone prior to atomization. Undesirable incompatibility of organic solvents for direct injection into the ICP-AES system was overcome ingeniously in a flow manner by oxidative back-extraction of the analytes utilizing a second lab-in-syringe setup. Following its optimization, the D-LIS-FB platform showed excellent linearity, in combination with good method precision (i.e., RSD < 3.4%) and trueness. Moreover, the limits of detection were 0.25 µg L-1 for Cd(II), 0.13 µg L-1 for Cu(II), and 0.37 µg L-1 for Pb(II), confirming the applicability of the proposed system for metal analysis at trace levels. As a proof-of-concept, the developed versatile system was utilized for the analysis of different environmental, food, and biological samples.


Assuntos
Cádmio , Cobre , Cádmio/química , Cobre/análise , Cetonas , Chumbo , Poliésteres , Solventes , Análise Espectral , Seringas
6.
Food Chem ; 394: 133548, 2022 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-35759833

RESUMO

A novel sol-gel pyridylethylthiopropyl functionalized silica-based sorbent was synthesized and utilized in an on-line column preconcentration system coupled with flame atomic absorption spectrometry for metal determination. The developed platform was used for the determination of Pb(II) and Cu(II) in beer samples, since there are limited automatic methods for routine analysis of alcoholic beverage. For a preconcentration time of 60 s, the calculated enhancement factors were 96 for Cu(II) and 130 for Pb(II). The limits of detection were 0.33 µg L-1 and 1.98 µg L-1 for Cu(II) and Pb(II), respectively. Moreover, the RSDs were less than 2.9% indicating good method precision. The method was successfully employed for the analysis of commercially available beers. The Cu(II) content of the samples was 1.6-21.8 µg L-1 and the Pb(II) content was 7.3-17.6 µg L-1. The developed manifold exhibited operational simplicity and good performance characteristics, indicating its potential utilization for routine analysis in beer industry.


Assuntos
Cerveja , Cobre , Cerveja/análise , Cobre/química , Chumbo/análise , Sílica Gel , Extração em Fase Sólida/métodos , Espectrofotometria Atômica/métodos
7.
Talanta ; 244: 123423, 2022 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-35397326

RESUMO

A novel automatic flow-batch platform coupled with atomic spectrometry for on-line acidic extraction induced by emulsion breaking with heating (FB-EIEBH) for metal determination in edible oils (corn, sunflower and olive oil), was developed for the first time. The proposed system was demonstrated for copper determination in conjunction with flame atomic absorption spectrometry. The extraction of metal is accomplished after the oil emulsification with an aqueous solution consisted of Triton X-114 and nitric acid, in an on-line programmed manner. All the main parameters affecting the extraction procedure, such as oil dilution, type and concentration of surfactant and nitric acid as well as temperature and time for the emulsion breaking and phase separation, have been investigated and optimized. A mixture of oil/xylene at 10:2 proportion was found to be appropriate to use in the flow manifold. Optimum conditions were verified employing 8.0 mL of oil sample, 990 µL of extractant solution containing 10.0% m/v Triton X-114 and 10.0% v/v HNO3. Emulsion breaking and phases separation were completed at temperature 90 °C, and time 300 s. The detection and quantification limit for copper determination was found to be 5.8 µg L-1 and 19.3 µg L-1, employing aqueous standards, which are proved to produce similar performance characteristics with oil-based standards. Recovery tests were executed by appropriate additions of oil-based standard solution of copper and the recoveries ranged between 94.2 and 102.4%.


Assuntos
Cobre , Ácido Nítrico , Cobre/análise , Emulsões , Óleos , Espectrofotometria Atômica/métodos , Água/química
8.
Molecules ; 26(15)2021 Jul 24.
Artigo em Inglês | MEDLINE | ID: mdl-34361614

RESUMO

A sol-gel thiocyanatopropyl-functionalized silica sorbent was synthesized and employed for an automated on-line microcolumn preconcentration platform as a front-end to inductively coupled plasma atomic emission spectroscopy (ICP-AES) for the simultaneous determination of Cd(II), Pb(II), Cu(II), Cr(III), Co(II), Ni(II), Zn(II), Mn(II), Hg(II), and V(II). The developed system is based on an easy-to-repack microcolumn construction integrated into a flow injection manifold coupled directly to ICP-AES's nebulizer. After on-line extraction/preconcentration of the target analyte onto the surface of the sorbent, successive elution with 1.0 mol L-1 HNO3 was performed. All main chemical and hydrodynamic factors affecting the effectiveness of the system were thoroughly investigated and optimized. Under optimized experimental conditions, for 60 s preconcentration time, the enhancement factor achieved for the target analytes was between 31 to 53. The limits of detection varied in the range of 0.05 to 0.24 µg L-1, while the limits of quantification ranged from 0.17 to 0.79 µg L-1. The precision of the method was expressed in terms of relative standard deviation (RSD%) and was less than 7.9%. Furthermore, good method accuracy was observed by analyzing three certified reference materials. The proposed method was also successfully employed for the analysis of environmental water samples.

9.
Molecules ; 26(1)2020 Dec 22.
Artigo em Inglês | MEDLINE | ID: mdl-33375078

RESUMO

A novel simple and sensitive, time-based flow injection solid phase extraction system was developed for the automated determination of metals at low concentration. The potential of the proposed scheme, coupled with flame atomic absorption spectrometry (FAAS), was demonstrated for trace lead and chromium(VI) determination in environmental water samples. The method, which was based on a new sorptive extraction system, consisted of a microcolumn packed with glass fiber coated with sol-gel poly (diphenylsiloxane) (sol-gel PDPS), which is presented here for the first time. The analytical procedure involves the on-line chelate complex formation of target species with ammonium pyrrolidine dithiocarbamate (APDC), retention onto the hydrophobic sol-gel sorbent coated surface of glass fibers, and finally elution with methyl isobutyl ketone prior to atomization. All main chemical and hydrodynamic factors, which affect the complex formation, retention, and elution of the metal, were optimized thoroughly. Furthermore, the tolerance to potential interfering ions appearing in environmental samples was also explored. Enhancement factors of 215 and 70, detection limits (3 s) of 1.1 µg·L-1 and 1.2 µg·L-1, and relative standard deviations (RSD) of 3.0% (at 20.0 µg·L-1) and 3.2% (at 20.0 µg·L-1) were obtained for lead and chromium(VI), respec tively, for 120 s preconcentration time. The trueness of the developed method was estimated by analyzing certified reference materials and spiked environmental water samples.


Assuntos
Análise de Injeção de Fluxo , Géis/química , Vidro/química , Metais/química , Siloxanas/química , Soluções/química , Espectrofotometria Atômica , Técnicas Biossensoriais , Quelantes/química , Quelantes/farmacologia , Fenômenos Químicos , Concentração de Íons de Hidrogênio , Metais/toxicidade , Extração em Fase Sólida , Espectrofotometria Atômica/métodos , Espectroscopia de Infravermelho com Transformada de Fourier , Propriedades de Superfície , Água/análise , Água/química
10.
Molecules ; 25(7)2020 Mar 29.
Artigo em Inglês | MEDLINE | ID: mdl-32235335

RESUMO

An innovative automatic purge-and-trap (P&T) system coupled with fluorimetric sequential injection (SI), for the on-line separation and preconcentration of volatile compounds, is presented. The truth of concept is demonstrated for the ammonium fluorimetric determination in environmental water samples with complex matrices without any pretreatment. The P&T flow system comprises a thermostated purge-vessel where ammonium is converted into gaseous ammonia and a trap-vessel for ammonia collection. This configuration results in matrix removal as well as analyte preconcentration, avoiding membrane-associated problems. All the main parameters affecting the efficiency of a P&T system were studied and optimized. The proposed method is characterized by a working range of 2.7-150.0 µg L-1 of NH4+, with a detection and quantification limit of 0.80 and 2.66 µg L-1, respectively, for a 10-mL sample consumption. The accuracy of the method was assessed by recovery assays in seawater, estuarine, and lake water samples as well as by the analysis of standard reference material.


Assuntos
Compostos de Amônio/análise , Análise de Injeção de Fluxo/métodos , Gases/análise , Água do Mar/química , Poluentes Químicos da Água/análise , Estuários , Análise de Injeção de Fluxo/instrumentação , Fluorometria/métodos , Ácido Clorídrico/química , Concentração de Íons de Hidrogênio , Limite de Detecção , Temperatura
11.
Anal Chim Acta ; 1033: 73-80, 2018 Nov 29.
Artigo em Inglês | MEDLINE | ID: mdl-30172334

RESUMO

A novel pressure-assisted dual-headspace lab-in-syringe microextraction technique is presented as an alternative approach for automatic on-line membraneless gas separation of volatile compounds. The developed gas-liquid microextraction procedure is based on the lab-in-syringe (LIS) concept by using two independent micro-syringe pumps which are connected to each other for the application of negative and positive pressure inside the common headspace area of the syringe barrels. The adoption of reduced and increased pressure conditions is facilitated by the programmable LIS strategy resulting in increased extraction rates. The analytical process includes the in-situ ammonia vapor generation in the headspace of the first microsyringe, under reduced pressure environment, and its subsequent transportation into the headspace of the second microsyringe. Then, positive pressure is applied inside the second microsyringe enabling the ammonia vapor dissolution into the extraction solution to produce a fluorescent product (isoindol-1-sulfonat). The reaction is time and temperature affected, thus after an optimized time of delay inside the thermostated syringe barrel at 60 °C, it is delivered into the flow-cell of the miniSIA system where it is quantified at 425 nm (excitation wavelength, 365 nm). The proposed preconcentration system has been fully tested and optimized regarding the relevant parameters affecting the generation of gaseous ammonia, its effective transportation into the headspace of the second syringe barrel and its quantitative dissolution and reaction with the extraction solution. For a sample volume of 3000 µL, the sample frequency is 8 h-1, the precision expressed as relative standard deviation (RSD) is 3.6 (at 5.0 µg L-1) and a detection limit (3s) of 0.05 µg L-1 for ammonium is obtained. The detection is linear in the concentration range of 0.15 and 10.0 µg L-1 with a correlation coefficient of 0.9987. The accuracy of the proposed method has been evaluated by analyzing a standard reference material (relative error: 3.8%) as well as using the Certified Method (relative error < 5.5%) for ammonium determination. The potential of this novel schema has been demonstrated for ammonia determination in natural water samples.

12.
Talanta ; 166: 364-368, 2017 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-28213247

RESUMO

A novel simple fully automatic on-line magnetic stirring-assisted liquid-liquid microextraction method, based on the lab-in-syringe (LIS) concept, has been developed as an alternative approach for sample pretreatment and atomic spectrometric assays. The analytical process includes the in-syringe reaction of the metal ion with the chelating reagent, the analyte micro-extraction and the subsequent transportation of the extractant to the detection system for electrothermal atomic absorption spectrometric (ETAAS) quantification. This novel platform has been demonstrated for trace silver determination in various types of water samples. The method is linear from 19 to 450ngL-1 using a small volume of extraction solvent of 120µL. The entire procedure is accomplished within 240s resulting in a sampling frequency of 15h-1. The enhancement factor is 80, while the detection limit and the precision are 5.7ngL-1 and 3.3%, respectively. The developed method was evaluated by analyzing standard reference materials and spiked water samples with satisfactory recoveries.


Assuntos
Microextração em Fase Líquida/métodos , Prata/análise , Prata/isolamento & purificação , Espectrofotometria Atômica/instrumentação , Seringas , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação , Automação , Limite de Detecção , Prata/química , Solventes/química , Fatores de Tempo , Poluentes Químicos da Água/química
13.
Anal Sci ; 31(5): 383-9, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-25958867

RESUMO

A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L(-1) HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h(-1). The detection limits were found to be 3.0, 0.06 and 2.0 ng L(-1) for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9 - 3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm(TM) trace elements urine) and spiked urine samples.


Assuntos
Cádmio/urina , Chumbo/urina , Extração em Fase Sólida , Temperatura , Vanádio/urina , Automação , Humanos , Espectrofotometria Atômica
14.
Talanta ; 133: 77-81, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25435230

RESUMO

A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 µL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 µg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 µg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples.

15.
Anal Chem ; 85(19): 8968-72, 2013 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-23977837

RESUMO

This manuscript reports the proof-of-concept of a novel integrated lab-in-syringe/gas-liquid separation (LIS/GLS) batch-flow system based on a programmable flow for automatic cold vapor atomic absorption spectrometric assays. Homogeneous mixing of metered volumes of sample and reagent solutions drawn up in a sandwich-type mode along with in situ vapor generation are accomplished inside the microsyringe in a closed manner, while the separation of vapor species is achieved via the membraneless GLS located at the top of the syringe's valve in the upright position. The potentials of the proposed manifold were demonstrated for trace inorganic mercury determination in drinking waters and seawater. For a 3.0 mL sample, the limit of detection and repeatability (RSD) were found to be 0.03 µg L(-1) Hg(II) and 3.1% (at the 2.0 µg L(-1) concentration level), respectively, with a dynamic range extending up to 10.0 µg L(-1). The proposed system fulfills the requirements of US-EPA, WHO, and EU Council Directives for measurements of the maximum allowed concentrations of inorganic mercury in drinking water.

16.
Anal Chim Acta ; 789: 1-16, 2013 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-23856225

RESUMO

The use of magnetic materials in solid phase extraction has received considerable attention in recent years taking into account many advantages arising from the inherent characteristics of magnetic particles. Magnetic solid phase extraction (MSPE) methodology overcomes problems such as column packing and phase separation, which can be easily performed by applying an external magnetic field. The use of magnetic particles in automatic systems is growing over the last few years making the on-line operation of MSPE a promising technique in the frame of green chemistry. This article aims to provide all recent progress in the research of novel magnetic materials as sorbents for metal preconcentration and determination coupled with different detection systems as well as their implementation in sequential injection and microfluidic systems. In addition, a description of preparation, characterization as well as applications of various types of magnetic materials, either with organic or inorganic coating of the magnetic core, is presented. Concluding remarks and future trends are also commented.


Assuntos
Magnetismo , Metais/análise , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos , Técnicas Analíticas Microfluídicas , Sistemas On-Line , Dióxido de Silício/química , Zircônio/química
17.
Talanta ; 110: 58-65, 2013 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-23618176

RESUMO

A dedicated pressure-driven mesofluidic platform incorporating on-chip sample clean-up and analyte preconcentration is herein reported for expedient determination of trace level concentrations of waterborne inorganic mercury. Capitalizing upon the Lab-on-a-Valve (LOV) concept, the mesofluidic device integrates on-chip micro-solid phase extraction (µSPE) in automatic disposable mode followed by chemical vapor generation and gas-liquid separation prior to in-line atomic fluorescence spectrometric detection. In contrast to prevailing chelating sorbents for Hg(II), bare poly(divinylbenzene-N-vinylpyrrolidone) copolymer sorptive beads were resorted to efficient uptake of Hg(II) in hydrochloric acid milieu (pH=2.3) without the need for metal derivatization nor pH adjustment of prior acidified water samples for preservation to near-neutral conditions. Experimental variables influencing the sorptive uptake and retrieval of target species and the evolvement of elemental mercury within the miniaturized integrated reaction chamber/gas-liquid separator were investigated in detail. Using merely <10 mg of sorbent, the limits of detection and quantification at the 3s(blank) and 10s(blank) levels, respectively, for a sample volume of 3 mL were 12 and 42 ng L(-1) Hg(II) with a dynamic range extending up to 5.0 µg L(-1). The proposed mesofluidic platform copes with the requirements of regulatory bodies (US-EPA, WHO, EU-Commission) for drinking water quality and surface waters that endorse maximum allowed concentrations of mercury spanning from 0.07 to 6.0 µg L(-1). Demonstrated with the analysis of aqueous samples of varying matrix complexity, the LOV approach afforded reliable results with relative recoveries of 86-107% and intermediate precision down to 9% in the renewable µSPE format.


Assuntos
Automação , Mercúrio/análise , Microfluídica/métodos , Extração em Fase Sólida/métodos , Poluentes Químicos da Água/análise , Limite de Detecção , Pressão
18.
Talanta ; 110: 229-35, 2013 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-23618196

RESUMO

A new automatic sequential injection (SI) system for on-line magnetic sorbent extraction coupled with electrothermal atomic absorption spectrometry (ETAAS) has been successfully developed for metal determination. In this work, we reported effective on-line immobilization of magnetic silica particles into a microcolumn by the external force of two strong neodymium iron boron (NdFeB) magnets across it, avoiding the use of frits. Octadecylsilane functionalized maghemite magnetic particles were used as sorbent material. The potentials of the system were demonstrated for trace cadmium determination in water samples. The method was based on the on-line complex formation with diethyldithiocarbamate (DDTC), retention of Cd-DDTC on the surface of the MPs and elution with isobutyl methyl ketone (IBMK). The formation mechanism of the magnetic solid phase packed column and all critical parameters (chemical, flow, graphite furnace) influencing the performance of the system were optimized and offered good analytical characteristics. For 5 mL sample volume, a detection limit of 3 ng L(-1), a relative standard deviation of 3.9% at 50 ng L(-1) level (n=11) and a linear range of 9-350 ng L(-1) were obtained. The column remained stable for more than 600 cycles keeping the cost down in routine analysis. The proposed method was evaluated by analyzing certified reference materials and natural waters.

19.
Anal Chim Acta ; 771: 50-5, 2013 Apr 10.
Artigo em Inglês | MEDLINE | ID: mdl-23522112

RESUMO

A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 µL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 µg L(-1) and the precision expressed as relative standard deviation (RSD) at 50.0 µg L(-1) of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples.

20.
Talanta ; 97: 181-6, 2012 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-22841064

RESUMO

A simple and sensitive on-line solid-phase extraction methodology for preconcentration and determination of trace amounts of Cd(II), Pd(II) and Cu(II) in natural water samples has been developed using the strong cation exchange capability of Bond Elut(®) Plexa™ PCX polymer resin. Plexa PCX is a mixed-mode sorbent, commercially available in a cartridge format and as far as we know, there is no application into the field of metal determination. The analytes were retained on the resin, eluted with 1 mol L(-1) hydrochloric acid and subsequently directed to FAAS for quantification. The influence of chemical and flow variables which affect the performance of the system have been studied, providing the appropriate conditions for the analysis of real samples. For preconcentration time of 90 s, an enrichment factor of 90, 95 and 95 and a detection limit (3 s) of 0.1, 1.8 and 0.5 µg L(-1) for Cd(II), Pb(II) and Cu(II), respectively were obtained along with a sampling frequency of 30 h(-1). The accuracy of the proposed method was evaluated by analyzing certified reference materials. This procedure was successfully applied for metal determination in environmental and biological samples.


Assuntos
Métodos Analíticos de Preparação de Amostras/métodos , Resinas de Troca de Cátion/química , Análise de Injeção de Fluxo/métodos , Metais Pesados/análise , Metais Pesados/química , Espectrofotometria Atômica/métodos , Adsorção , Concentração de Íons de Hidrogênio , Metais Pesados/isolamento & purificação , Extração em Fase Sólida , Fatores de Tempo , Água/química , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA