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1.
Food Chem ; 454: 139780, 2024 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-38805928

RESUMO

Nickel-manganese-cobalt tetragonal spinel ternary oxide nanocomposite (NMC-TSO) was synthesized. It was utilized as an efficient sorbent for the dispersive solid phase microextraction (D-SPµE) without vortexing of cadmium. The analysis of the cadmium was carried out by FAAS. The effective analytical parameters including pH (6) contact times (no vortexing), sample volume (70 mL), eluent volume (3 mL of 2 mol L-1 HCl), linear dynamic ranges (1.07-85.7 µg L-1), and re-useability (33) on the D-SPµE efficiency were investigated. The PF, RSD% and LOD of the D-SPµE for cadmium were 23.3, ≤ 2.8% and 0.49 µg L-1, respectively. The tolerable concentrations of Ca2+, Mg2+, K+ and Na+ on Cd(II) were 50,000 mg L-1, 50,000 mg L-1, 25,000 mg L-1 and 7500 mg L-1, respectively. The method was accurated by analysis of food and water certificate reference materials (NW-TMDA-54.6 Lake water, SPS-WW1 121 Batch wastewater, 1573a Tomato Leaves and TORT-3 Lobster Hepatopancreas) and - recovery experiments. The D-SPµE-FAAS method was applied for the cadmium determination in dam water, wastewater, river water, well water, sea water, tea, cacao, nut, bitter chocolate, rice, leek, cinnamon and parsley.


Assuntos
Cádmio , Cobalto , Contaminação de Alimentos , Manganês , Nanocompostos , Níquel , Óxidos , Microextração em Fase Sólida , Poluentes Químicos da Água , Nanocompostos/química , Adsorção , Óxidos/química , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação , Cádmio/química , Cádmio/análise , Cádmio/isolamento & purificação , Níquel/química , Níquel/isolamento & purificação , Contaminação de Alimentos/análise , Manganês/química , Manganês/análise , Manganês/isolamento & purificação , Cobalto/química , Cobalto/isolamento & purificação
2.
Talanta ; 274: 126094, 2024 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-38643650

RESUMO

Metal-organic frameworks (MOFs) are good adsorbents for targeted chemicals with their adjustable properties. Herein, we prepared a zirconium based MOF (MOF-808(Zr)) and functionalized it employing 2-mercapto-4-methyl-5-thiazolacetic acid (MOF-808(Zr)-Tz). The prepared MOFs were characterized by XRD, FTIR, SEM-EDX, TGA, N2 sorption, zeta potential measurements, and elemental analysis. The surface area of MOF-808(Zr)-Tz was 1348 m2/g. Dispersive solid-phase micro-extraction (D-SPµE) method based on MOF-808(Zr)-Tz was firstly developed and applied to the extraction of chromium, silver, and rhodium in waters. The determination of the analytes was done by FAAS. The optimal pH and eluent for analytes were 7.0 and 3 mL of 2 mol L-1 HCl, respectively. The contact times were 1 min for adsorption and 3 min for elution. The LOD and PFs of the D-SPµE for analytes were 2.3 µg L-1 and 13.3 for chromium, 2.1 µg L-1 and 13.3 for silver, and 3.1 µg L-1 and 13.3 rhodium, respectively. The D-SPµE method was verified with analyses of NW-TMDA-54.6 Lake water and SPS-WW1 Batch 114 Wastewater and with spiked dam water, river water, well water, sea water, and wastewater. The recoveries of the analytes changed from 89 to 108 %. The results indicated that the method is selective, simple, effective, and rapid for extracting chromium(III), silver(I) and rhodium(III) in waters.

3.
Biol Trace Elem Res ; 2023 Dec 20.
Artigo em Inglês | MEDLINE | ID: mdl-38117385

RESUMO

A new thiosemicarbazide-modified, sulfonamide-based poly (styrene) adsorbent (T-CSPS) was prepared starting from the reaction of chlorosulfonated polystyrene and thiosemicarbazide. It was characterized by SEM-EDX, FT-IR, and zeta potential. The T-CSPS was used as an adsorbent for the first time for the dispersive solid-phase microextraction (d-SPµE) and preconcentration of Pb(II) ions from waters and dill and lettuce extracts in the unified bioaccessibility method (UBM) saliva. Lead was then determined using the FAAS. In the first step of optimization, the solution pH was changed from 2 to 8, and pH 4 with a recovery value of 103% ± 5 was selected. Two milliliters of 2 mol L-1 HCl was chosen as eluent. Contact times were found to be only 2 min. Effects of coexisting ions and sample volume were tested. Under optimal conditions, the preconcentration factor (PF) and the adsorption capacity were 15 and 40 mg g-1. The RSD% was 2.2% and 3.1% for intra-day and inter-day precision, respectively. The LOD and LOQ were found to be 5.1 µg L-1 and 16.9 µg L-1, respectively. The accuracy of the d-SPµE was checked by TMDA-70.2 Lake water and BCR-482 Lichen-certified reference materials and also applying d-SPµE to spiked waters and lettuce and dill extracts in UBM saliva.

4.
Anal Methods ; 15(43): 5846-5854, 2023 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-37874290

RESUMO

A fast and simple dispersive solid-phase microextraction method (d-SPµE) was described for the determination of copper and lead in food, water, and sediments using FAAS. Firstly, nanoflower Al2O3@carbon spheres composite (NF Al2O3@CSs) was synthesized and then characterized. The obtained NF Al2O3@CSs was used for the d-SPµE of copper and lead in aqueous solutions. The influence of important parameters like pH, contact time, eluent conditions, volume of sample, and competing ion effects on the d-SPµE efficiency of copper and lead was investigated. They were pH, 7; eluent, 2 mol L-1 HCl (2 mL); sample volume, 250 mL for copper and 150 mL for lead with recoveries ≥90%. The adsorption and elution of analytes on NF Al2O3@CSs were realized quickly without vortexing. The LODs of the d-SPµE for copper and lead were found to be 0.69 µg L-1 and 2.8 µg L-1, respectively, while its PF was 125 for copper and 75 for lead. The intra-day precision and inter-day repeatability (RSD%, n = 7) were 1.3% and 1.6% for Cu(II) and 2.3% and 3.2% for Pb(II), respectively. Finally, the accuracy of the d-SPµE was investigated by determination of the analytes in four certified reference materials (TMDA-53.3 Lake water, NW-TMDA-54.6 Lake water, NIST 1573a Tomato leaves, and NIST RM 8704 Buffalo River Sediment). The analyte recoveries together with analyses of dam water, river water, wastewater, sea water, sumac, tea, chocolate, and lentils were studied. The results indicate that recoveries ranged from 90 to 103% in water samples and 91 to 110% in food samples.

5.
Biol Trace Elem Res ; 201(3): 1538-1546, 2023 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-35505155

RESUMO

The total, gastric, and gastro-intestinal Cu, Mn, Fe, and Zn concentrations in eight fruit and vegetable samples were investigated. The unified bioaccessibility method (UBM) developed by BARGE (Bioaccessibility Research Group of Europe) was performed for in vitro bioaccessibility experiments. Total and bioaccessible concentrations of Cu, Mn, Fe, and Zn were determined by ICP-OES and ICP-MS, respectively. The accuracy of the methods was verified using BGS 102 for the BARGE UBM and SRM 1573a for total analysis. The mean BF (%) order for Cu, Mn, Fe, and Zn was Mn (101) > Zn (88) > Fe (60) > Cu (30) in gastric phase and Mn (78) > Zn (69) > Fe (46) > Cu (29) in gastro-intestinal phase. The results show that Mn and Zn in all the samples have the greatest bioaccessible values, while the values for Cu are much lower. The relationships among total, gastric, and gastro-intestinal element concentrations were investigated using statistical analysis such as correlation analysis, principal component analysis (PCA), and cluster analysis (CA). Total and bioaccessible Cu, Mn, and Zn concentrations were significantly correlated with each other.


Assuntos
Frutas , Verduras , Europa (Continente) , Trato Gastrointestinal , Zinco , Metais Pesados/análise
6.
Spectrochim Acta A Mol Biomol Spectrosc ; 244: 118826, 2021 Jan 05.
Artigo em Inglês | MEDLINE | ID: mdl-32858449

RESUMO

A polyacrylonitrile/polyindole (PAN/PIN) [50, 50] conducting polymer composite was chemically synthesized using FeCl3 as an oxidizing agent in chloroform solution and nitrogen atmosphere at 10 °C. The formation of the composite was supported by Fourier transform infrared spectroscopy. The morphological properties of the composite were investigated by atomic force microscopy and scanning electron microscopy. The thermal properties of the composite were examined by using thermogravimetric analyses. It was found that the composite had good thermal stability. The conducting polymer composite was used for the first time as an adsorbent for solid phase extraction of Cu (II). The optimum pH was found to be 7. The adsorption and elution shaking times were 5 and 15 min, respectively. The elution was done with 5 mL of 2 mol L-1 HNO3. The accuracy of the developed method was confirmed by analyzing certified reference material (TMDA-70.2 Lake Water).

7.
Artigo em Inglês | MEDLINE | ID: mdl-32083510

RESUMO

A new and rapid dispersive solid phase extraction method by using a green-synthesised UiO-66(Zr)-(COOH)2 (Zr-BTeC) adsorbent with body-centred cubic (bcu) topology was developed for determination of tartrazine in food samples. Zr-BTeC was used for the first time as an adsorbent for tartrazine. It was synthesised and characterised by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, Brunauer-Emmett-Teller surface area analysis, and zeta potential measurements. Tartrazine was determined at 405 nm spectrophotometrically. Experimental conditions were optimised in order to achieve quantitative recoveries. The sample acidity was found to be 0.02 mol L-1 HCl. The amount of Zr-BTeC was 10 mg. Both adsorption and elution contact times were only 5 s without the need for vortexing. Elution was with 2 mL of 0.5 mol L-1 NH3. A sample volume of 45 mL was selected as optimum. The adsorption capacity for tartrazine with Zr-BTeC was found to be 185 mg g-1 and the adsorbent was reusable up to 40 cycles. The tartrazine concentrations found by the developed method in food supplements were compared with the results obtained by HPLC method for the same samples. Statistical analysis results showed that there are insignificant differences between the results of the two methods (p = .05). The method was successfully applied to the determination of tartrazine in spiked chewing gums, lemon flavoured icing glaze, and jelly samples.


Assuntos
Análise de Alimentos , Corantes de Alimentos/análise , Contaminação de Alimentos/análise , Estruturas Metalorgânicas/química , Extração em Fase Sólida , Tartrazina/análise , Zircônio/química
8.
Biol Trace Elem Res ; 198(1): 332-338, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32076953

RESUMO

The stability of four major arsenic (As) species during application of the BARGE (Bioaccessibility Research Group of Europe) unified bioaccessibility method (UBM) has been assessed. The concentrations of As species in the UBM gastric and gastro-intestinal (gastric + intestinal) phases were determined using HPLC-ICP-MS whilst the total As content in the samples was determined using ICP-MS alone. The arsenic species studied were arsenite As(III), arsenate As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA). These species were separated in 10 min using an anion exchange column (Hamilton PRP-X100) with a mobile phase containing 20 mmol L-1 NH4H2PO4/1% methanol (pH 6.0). The recoveries of arsenic species spiked into the gastric and gastro-intestinal fluids were in the range 90-108%. No interconversion between As species was observed as a result of applying the BARGE UBM, which is a particularly important finding for the reliability of As(III) measurements. The accuracy of the BARGE UBM for in vitro extractable As(V) was verified using British Geological Survey (BGS) guidance material 102 (an ironstone soil). For a commercial rice sample, the bioaccessibility sequence of As was DMA > As(III) > As(V) for the gastric phase and As(III) > DMA > As(V) for the gastro-intestinal phase.


Assuntos
Arsênio , Arsenicais , Arsênio/análise , Cromatografia Líquida de Alta Pressão , Europa (Continente) , Espectrometria de Massas , Reprodutibilidade dos Testes
9.
Talanta ; 190: 397-402, 2018 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-30172525

RESUMO

In this study, tannic acid functionalized graphene as an adsorbent was synthesized and characterized by X-ray diffraction and scanning electron microscopy. It was used for the first time as an adsorbent for vortex-assisted dispersive solid phase extraction of trace Be(II) from water and street dust samples. The determination of beryllium was made by graphite furnace atomic absorption spectrometry. The effect of different parameters (pH, contact times, centrifuge rate and time, eluent type and volume, sample volume, and interfering ions) was investigated. The optimum pH was found to be 6. The adsorption and elution contact times were 3 min. The quantitative elution was carried out with 2 mL of 1.5 mol L-1 HCl. The preconcentration factor, detection limit and precision (as RSD%) of the method were found to be 125, 0.84 ng L-1, and 2.9%, respectively. The adsorbent showed good selectivity for Be(II) against interfering cations and anions and it was reusable up to 80 cycles. The accuracy of the developed method was confirmed by analyzing certified reference material (TMDA-70 Lake water) and by spiking tap water, wastewater, well water, and street dust samples.

10.
Food Chem ; 263: 232-239, 2018 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-29784312

RESUMO

In the present study, core-shell Fe3O4 polydopamine nanoparticles were synthesized and used for the first time as an adsorbent for the vortex assisted magnetic dispersive solid phase extraction of copper from food samples. After elution, copper in the solutions was determined by FAAS. The adsorbent was characterized using X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. Various parameters affecting the magnetic dispersive solid-phase extraction were evaluated. The optimum pH and magnetic adsorbent amount were found to be 5 and 40 mg, respectively. Elution was made by 3 mL of 2 mol L-1 HNO3.The major advantage of the method is the fast equilibration during adsorption without the need for vortexing or shaking. The preconcentration factor and detection limit of the method were found to be 150 and 0.22 mg L-1, respectively. The precision (as RSD%) and adsorption capacity of the method were 3.7% and 28 mg g-1, respectively. The method was successfully verified by analyzing four certified reference materials (SPS-WW1 Batch 114 Wastewater, TMDA-53.3 Lake water, BCR-482 Lichen and 1573a Tomato Leaves) and by addition/recovery tests of copper standard solution in organic baby food, muesli, macaroni, honey, and milk samples.


Assuntos
Cobre/análise , Indóis/química , Nanopartículas de Magnetita/química , Polímeros/química , Adsorção , Cobre/isolamento & purificação , Óxido Ferroso-Férrico/química , Análise de Alimentos , Água Doce/análise , Concentração de Íons de Hidrogênio , Limite de Detecção , Extração em Fase Sólida , Espectrometria por Raios X , Espectroscopia de Infravermelho com Transformada de Fourier , Águas Residuárias/análise , Difração de Raios X
11.
Food Chem ; 237: 707-715, 2017 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-28764057

RESUMO

In this study, zirconium-based highly porous metal-organic framework, MOF-545, was synthesized and characterized. The surface area of MOF-545 was found to be 2192m2/g. This adsorbent was used for the first time as an adsorbent for the vortex assisted-solid phase extraction of Pb(II) from cereal, beverage and water samples. Lead in solutions was determined by FAAS. The optimal experimental conditions were as follows: the amount of MOF-545, 10mg; pH of sample, 7; adsorption and elution time, 15min; and elution solvent, 2mL of 1molL-1HCl. Under the optimal conditions of the method, the limit of detection, preconcentration factor and precision as RSD% were found to be 1.78µgL-1, 125 and 2.6%, respectively. The adsorption capacity of the adsorbent for lead was found to be 73mgg-1. The method was successfully verified by analyzing two certified reference materials (BCR-482 Lichen and SPS-WW1 Batch 114) and spiked chickpea, bean, wheat, lentil, cherry juice, mineral water, well water and wastewater samples.


Assuntos
Bebidas , Grão Comestível , Água/química , Chumbo , Extração em Fase Sólida , Espectrofotometria Atômica , Poluentes Químicos da Água , Zircônio
12.
Talanta ; 159: 222-230, 2016 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-27474302

RESUMO

In this study a new adsorbent, ionic liquid (1,8-naphthalene monoimide bearing imidazolium salt) coated carbon nanospheres, was synthesized for the first time and it was used for the solid phase extraction of copper and lead from various samples prior to determination by flame atomic absorption spectrometry. The ionic liquid, carbon nanospheres and ionic liquid coated carbon nanospheres were characterized by using Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, (1)H NMR and (13)C NMR, Brunauer, Emmett and Teller surface area and zeta potential measurements. Various parameters for method optimization such as pH, adsorption and elution contact times, eluent volume, type and concentration, centrifuge time, sample volume, adsorption capacity and possible interfering ion effects were tested. The optimum pH was 6. The preconcentration factor, detection limits, adsorption capacity and precision (as RSD%) of the method were found to be 300-fold, 0.30µgL(-1), 60mgg(-1) and 1.1% for copper and 300-fold, 1.76µgL(-1); 50.3mgg(-1) and 2.2%, for lead, respectively. The effect of contact time results showed that copper and lead were adsorbed and desorbed from the adsorbent without vortexing. The equilibrium between analyte and adsorbent is reached very quickly. The method was rather selective for matrix ions in high concentrations. The accuracy of the developed method was confirmed by analyzing certified reference materials (LGC6016 Estuarine Water, Reference Material 8704 Buffalo River Sediment, and BCR-482 Lichen) and by spiking sea water, wastewater, street dust and spice samples.

13.
Food Chem ; 194: 463-9, 2016 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-26471580

RESUMO

In this paper, a nanosized spongelike Mn3O4 was synthesized and used for the first time as an effective adsorbent for vortex-assisted separation and preconcentration of lead and copper from various food samples. Copper and lead were determined by flame atomic absorption spectrometry. The characterization of the nanosized spongelike Mn3O4 was performed by X-ray diffraction, scanning electron microscopy, Raman spectroscopy, Brunauer, Emmett and Teller surface area and zeta potential measurement. The contact times for both adsorption and elution were only 3min. Under the optimized conditions, detection limits for copper and lead were found to be 2.6µgL(-1) and 3.0µgL(-1), respectively. The relative standard deviations were found to be ⩽3.2%. The accuracy of the method was confirmed by analyzing the standard reference materials (BCR-482 Licken and SRM 1573a Tomato Leaves) and spiked real food and herb samples.


Assuntos
Cobre/química , Alimentos/efeitos adversos , Intoxicação por Metais Pesados , Chumbo/química , Compostos de Manganês/química , Óxidos/química , Extração em Fase Sólida/métodos , Metais Pesados/análise , Metais Pesados/química , Nanotecnologia , Intoxicação
14.
Ecotoxicol Environ Saf ; 124: 369-376, 2016 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-26595510

RESUMO

A total of 36 street dust samples were collected from the streets of the Organised Industrial District in Kayseri, Turkey. This region includes a total of 818 work places in various industrial areas. The modified BCR (the European Community Bureau of Reference) sequential extraction procedure was applied to evaluate the mobility and bioavailability of trace elements (Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and Zn) in street dusts of the study area. The BCR was classified into three steps: water/acid soluble fraction, reducible and oxidisable fraction. The remaining residue was dissolved by using aqua regia. The concentrations of the metals in street dust samples were determined by flame atomic absorption spectrometry. Also the effect of the different grain sizes (<38µm, 38-53µm and 53-74µm) of the 36 street dust samples on the mobility of the metals was investigated using the modified BCR procedure. The mobility sequence based on the sum of the first three phases (for <74µm grain size) was: Cd (71.3)>Cu (48.9)>Pb (42.8)=Cr (42.1)>Ni (41.4)>Zn (40.9)>Co (36.6)=Mn (36.3)>Fe (3.1). No significant difference was observed among metal partitioning for the three particle sizes. Correlation, principal component and cluster analysis were applied to identify probable natural and anthropogenic sources in the region. The principal component analysis results showed that this industrial district was influenced by traffic, industrial activities, air-borne emissions and natural sources. The accuracy of the results was checked by analysis of both the BCR-701 certified reference material and by recovery studies in street dust samples.


Assuntos
Poeira/análise , Poluição Ambiental/estatística & dados numéricos , Metais Pesados/análise , Análise por Conglomerados , Monitoramento Ambiental , Indústrias , Análise Multivariada , Tamanho da Partícula , Análise de Componente Principal , Espectrofotometria Atômica , Oligoelementos/análise , Turquia
15.
Artigo em Inglês | MEDLINE | ID: mdl-25974670

RESUMO

In this study, a fast and simple vortex assisted solid phase extraction method was developed for the separation/preconcentration of basic fuchsin in various water samples. The determination of basic fuchsin was carried out at a wavelength of 554 nm by spectrophotometry. Reduced graphene oxide which was used as a solid phase extractor was synthesized and characterized by X-ray diffraction, scanning electron microscopy and the Brunauer, Emmett and Teller. The optimum conditions are as follows: pH 2, contact times for adsorption and elution of 30 s and 90 s, respectively, 10 mg adsorbent, and eluent (ethanol) volume of 1 mL. The effects of some interfering ions and dyes were investigated. The method was linear in the concentration range of 50-250 µg L(-1). The adsorption capacity was 34.1 mg g(-1). The preconcentration factor, limit of detection and precision (RSD, %) of the method were found to be 400, 0.07 µg L(-1) and 1.2%, respectively. The described method was validated by analyzing basic fuchsin spiked certified reference material (SPS-WW1 Batch 114-Wastewater) and spiked real water samples.


Assuntos
Corantes/análise , Grafite/química , Corantes de Rosanilina/análise , Extração em Fase Sólida/métodos , Espectrofotometria/métodos , Poluentes Químicos da Água/análise , Água/análise , Adsorção , Corantes/isolamento & purificação , Água Doce/análise , Limite de Detecção , Modelos Moleculares , Óxidos/química , Corantes de Rosanilina/isolamento & purificação , Água do Mar/análise , Águas Residuárias/análise , Poluentes Químicos da Água/isolamento & purificação , Difração de Raios X
16.
Artigo em Inglês | MEDLINE | ID: mdl-25082436

RESUMO

Concentrations of Mn, Fe, Co, Ni, As, Se, Cd, Ag and Pb in scale, skin, muscle, gills, liver and the gonads of Gilthead seabream (Sparus aurata), European seabass (Dicentrarchus labrax), Black Sea salmon (Salmo trutta labrax), Horse mackerel (Trachurus trachurus), Red mullet (Mullus barbatus) and Whiting (Merlangius merlangius euxinus) from the Black Sea, in Turkey, were investigated. Elemental analyses were performed with inductively coupled plasma-mass spectrometry after sample preparation by microwave digestion. Mean metal concentrations in different tissues were in the following ranges: Mn 0.09-23.1, Fe 0.58-326, Co 0.01-0.22, Ni 0.03-1.34, As 0.13-3.40, Se 0.13-4.42, Ag 0.01-0.18, Cd 0.32-6.25, Pb 0.02-0.38 mg kg⁻¹ wet weight. Metal concentrations in the muscles of the examined species were generally lower than those in scale, skin, gills, liver and the gonads. The described method was validated by analysis of Dogfish Liver-certified reference material, DOLT-4.


Assuntos
Peixes , Contaminação de Alimentos , Inspeção de Alimentos/métodos , Metais Pesados/análise , Alimentos Marinhos/análise , Oligoelementos/análise , Poluentes Químicos da Água/análise , Métodos Analíticos de Preparação de Amostras , Animais , Mar Negro , Peixes/crescimento & desenvolvimento , Brânquias/química , Gônadas/química , Fígado/química , Espectrometria de Massas , Micro-Ondas , Músculo Esquelético/química , Alimentos Marinhos/economia , Pele/química , Especificidade da Espécie , Espectrofotometria Atômica , Turquia
17.
Talanta ; 133: 162-9, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25435243

RESUMO

A flow injection manifold incorporating a solid phase chelating resin (Toyopearl AF-Chelate-650) is reported for the preconcentration of dissolved metals from seawater, with a focus on investigating the effect of the loading pH, wash solution composition and wash time. Cobalt, iron, lead and vanadium have been used as target analytes with contrasting oceanographic behaviour. Quadrupole ICP-MS has been used for detection to make the approach accessible to most laboratories and a collision/reaction cell has been incorporated to minimise polyatomic interferences. Results for the seawater CRM NASS-6 and two GEOTRACES reference materials were in good agreement with the certified/consensus values, demonstrating the suitability of the approach for the determination of trace metals in seawater. The experimental design used allowed a thorough investigation of the uncertainty contribution from each method parameter to the overall expanded uncertainty of the measurement. The results showed that the parameters making the largest contributions were the precision of the peak area measurement and the uncertainty associated with the slope of the calibration curve. Therefore, these are the critical parameters that should be targeted in order to reduce the overall measurement uncertainty. For iron, the wash blank also gave a measureable contribution.


Assuntos
Espectrometria de Massas/instrumentação , Metais Pesados/análise , Água do Mar/química , Extração em Fase Sólida/instrumentação , Cobalto/análise , Análise de Injeção de Fluxo/instrumentação , Ferro/análise , Chumbo/análise , Limite de Detecção , Incerteza , Vanádio/análise
18.
Talanta ; 128: 31-7, 2014 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-25059126

RESUMO

In this study, a nano sponge Mn2O3 adsorbent was synthesized and was used for the first time. Various parameters affecting the recovery values of Pd(II) and Rh(III) were examined. The tolerance limits (≥ 90 %) for both Pd(II) and Rh(III) ions were found to be 75,000 mg L(-1) Na(I), 75,000 mg L(-1) K(I), 50,000 mg L(-1) Mg(II) and 50,000 mg L(-1) Ca(II). A 30s contact time was enough for both adsorption and elution. A preconcentration factor of 100 was obtained by using 100mg of the nano sponge Mn2O3. The reusability of the adsorbent was 120 times. Adsorption capacities for Pd(II) and Rh(III) were found to be 42 and 6.2 mg g(-1), respectively. The detection limits were 1.0 µg L(-1) for Pd(II) and 0.37 µg L(-1) for Rh(III) and the relative standard deviations (RSD, %) were found to be ≤ 2.5%. The method was validated by analyzing the standard reference material, SRM 2556 (Used Auto Catalyst Pellets) and spiked real samples. The optimized method was applied for the preconcentration of Pd(II) and Rh(III) ions in water (sea water and wastewater), rock, street sediment and catalytic converter samples.


Assuntos
Compostos de Manganês/química , Nanopartículas/química , Óxidos/química , Paládio/análise , Ródio/análise , Espectrofotometria Atômica/métodos , Adsorção , Catálise , Sedimentos Geológicos/química , Concentração de Íons de Hidrogênio , Microscopia Eletrônica de Varredura , Nanopartículas/ultraestrutura , Paládio/química , Tamanho da Partícula , Porosidade , Reprodutibilidade dos Testes , Ródio/química , Água do Mar/química , Transdutores , Águas Residuárias/análise , Águas Residuárias/química , Difração de Raios X
19.
J AOAC Int ; 97(2): 598-604, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-24830173

RESUMO

A solid phase extractor, poly(N,N'-dipropionitrile methacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid), was synthesized and used for separation/preconcentration of traces of Ni(II), Co(II), Cu(II), Mn(II), Cd(II), Zn(II), and Pb(II) from various water samples prior to their determination by flame atomic absorption spectrometry. The characterization of the synthesized resin was performed by elemental analysis and IR spectrometry. Parameters such as pH, volume and concentration of the eluent, flow rate of the sample solution, sample volume, and interfering ions affecting the column SPE were examined. The optimum pH was found to be 3. The retained metal ions were desorbed from the column with 10 mL of 1 M HCI eluent. A high preconcentration factor, 40-100; low RSD, < or = 2.8%; and low LOD values, < or = 1.74 microg/L, were obtained. The adsorption capacity of the resin was in the range of 6.80-12.4 mg/g for all the elements. The reusability of the resin was excellent. The accuracy of the method was confirmed by analyzing certified reference materials (TMDA-70 Lake Water and SPS-WW1 Batch 111-Wastewater) and spiked water samples. The method was successfully applied to the determination of metal ions in tap, lake, and dam waters.


Assuntos
Metais/química , Resinas Sintéticas/química , Oligoelementos/química , Água/química , Quelantes/química , Monitoramento Ambiental , Água Doce/química , Concentração de Íons de Hidrogênio , Estrutura Molecular , Espectrofotometria Atômica/métodos , Poluentes Químicos da Água/química
20.
Food Chem ; 150: 321-7, 2014 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-24360457

RESUMO

In this study, the Unified Bioaccessibility Research Group of Europe (BARGE) in vitro method was used to assess the bioaccessibility of Cr, Cu, Fe, Mg, Mn, Mo, Se, and Zn in ten nutritional supplement samples and three certified reference materials. The total digest, gastric phase and gastro-intestinal phase concentrations of Cu, Fe, Mg, Mn and Zn were determined by ICP-OES and Cr, Mo and Se by ICP-MS. The bioaccessible fractions of the elements in the gastric phase for the nutritional supplements were in the range 13-89% for Cr, 9-79% for Cu, 55-99% for Fe, 33-95% for Mg, 83-94% for Mn, 42-101% for Mo, 74-125% for Se and 81-104% for Zn. The range for the gastrointestinal phase was 6-65% for Cr, 27-66% for Cu, 3-14% for Fe, 34-91% for Mg, 53-62% for Mn, 40-109% for Mo, 53-146% for Se and 3-35% for Zn.


Assuntos
Suplementos Nutricionais/análise , Oligoelementos/análise , Disponibilidade Biológica , Europa (Continente) , Trato Gastrointestinal/metabolismo , Humanos , Metais Pesados/análise , Metais Pesados/farmacocinética , Modelos Biológicos , Selênio/análise , Selênio/farmacocinética , Oligoelementos/farmacocinética
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