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1.
Pesqui. bras. odontopediatria clín. integr ; 22: e210090, 2022. tab, graf
Artigo em Inglês | LILACS, BBO - Odontologia | ID: biblio-1386800

RESUMO

Abstract Objective: To compare the high-cycle fatigue behavior of four commercially available NiTi orthodontic wires. Material and Methods: Twelve NiTi orthodontic wires, round, 0.016-in, three per brand, were selected and divided into four groups: G1 - Heat-activated NiTi, G2 - Superelastic NiTi, G3 - Therma-Ti, and G4 - CopperNiTi. The atomic absorption spectrometry method was used to determine the chemical composition of investigated NiTi wires. We also performed a fatigue test at three-point bending using a universal testing machine for 1000 cycles in a 35 °C water bath. For the first and thousandth cycle, the average plateau load and the plateau length were determined in the unloading area of the force versus displacement diagram. In addition, we calculated the difference between the average plateau load of the first and thousandth cycle (∆F), as well as the difference between the plateau length of both cases (∆L). Results: According to our results, there were no significant differences between the average plateau load of the first and thousandth cycles of each group (p>0.05) and in the plateau length of the first and thousandth cycles of the groups (p>0.05). Conclusion: There were no significant differences between the groups changing the superelasticity property after high-cycle fatigue.


Assuntos
Fios Ortodônticos , Ortodontia , Estresse Mecânico , Instrumentos Odontológicos , Espectrofotometria Atômica/instrumentação , Análise Espectral/métodos , Técnicas In Vitro/métodos , Teste de Materiais , Análise de Variância
2.
Molecules ; 26(19)2021 Oct 03.
Artigo em Inglês | MEDLINE | ID: mdl-34641557

RESUMO

Using bamboo powder biochar as raw material, high-quality meso/microporous controlled hierarchical porous carbon was prepared-through the catalysis of Fe3+ ions loading, in addition to a chemical activation method-and then used to adsorb copper ions in an aqueous solution. The preparation process mainly included two steps: load-alkali leaching and chemical activation. The porosity characteristics (specific surface area and mesopore ratio) were controlled by changing the K2CO3 impregnation ratio, activation temperature, and Fe3+ ions loading during the activation process. Additionally, three FBPC samples with different pore structures and characteristics were studied for copper adsorption. The results indicate that the adsorption performance of the bamboo powder biochar FBPC material was greatly affected by the meso/micropore ratio. FBPC 2.5-900-2%, impregnated at a K2CO3: biochar ratio of 2.5 and a Fe3+: biochar mass ratio of 2%, and activated at 900 °C for 2 h in N2 atmosphere, has a very high specific surface area of 1996 m2 g-1 with a 58.1% mesoporous ratio. Moreover, it exhibits an excellent adsorption capacity of 256 mg g-1 and rapid adsorption kinetics for copper ions. The experimental results show that it is feasible to control the hierarchical pore structure of bamboo biochar-derived carbons as a high-performance adsorbent to remove copper ions from water.


Assuntos
Carbono/química , Cloretos/química , Cobre/química , Compostos Férricos/química , Sasa/química , Absorção Fisico-Química , Carvão Vegetal/química , Pós/química , Espectrofotometria Atômica/instrumentação , Espectrofotometria Atômica/métodos , Purificação da Água/métodos
3.
Am J Clin Pathol ; 156(2): 167-175, 2021 07 06.
Artigo em Inglês | MEDLINE | ID: mdl-33978166

RESUMO

OBJECTIVES: This review aims to describe the principles underlying different types of inductively coupled plasma mass spectrometry (ICP-MS), and major technical advancements that reduce spectral interferences, as well as their suitability and wide applications in clinical laboratories. METHODS: A literature survey was performed to review the technical aspects of ICP-MS, ICP-MS/MS, high-resolution ICP-MS, and their applications in disease diagnosis and monitoring. RESULTS: Compared to the atomic absorption spectrometry and ICP-optical emission spectrometry, ICP-MS has advantages including improved precision, sensitivity and accuracy, wide linear dynamic range, multielement measurement capability, and ability to perform isotopic analysis. Technical advancements, such as collision/reaction cells, triple quadrupole ICP-MS, and sector-field ICP-MS, have been introduced to improve resolving power and reduce interferences. Cases are discussed that highlight the clinical applications of ICP-MS including determination of toxic elements, quantification of nutritional elements, monitoring elemental deficiency in metabolic disease, and multielement analysis. CONCLUSIONS: This review provides insight on the strategies of elemental analysis in clinical laboratories and demonstrates current and emerging clinical applications of ICP-MS.


Assuntos
Laboratórios , Espectrofotometria Atômica/instrumentação , Espectrofotometria Atômica/métodos , Humanos
4.
Molecules ; 25(6)2020 Mar 21.
Artigo em Inglês | MEDLINE | ID: mdl-32245155

RESUMO

To reduce uncertainties in determining the source term and evolving condition of spent nuclear fuel is fundamental to the safety assessment. ß-emitting nuclides pose a challenging task for reliable, quantitative determination because both radiometric and mass spectrometric methodologies require prior chemical purification for the removal of interfering activity and isobars, respectively. A method for the determination of 90Sr at trace levels in nuclear spent fuel leachate samples without sophisticated and time-consuming procedures has been established. The analytical approach uses a commercially available automated pre-concentration device (SeaFAST) coupled to an ICP-DRC-MS. The method shows good performances with regard to reproducibility, precision, and LOD reducing the total time of analysis for each sample to 12.5 min. The comparison between the developed method and the classical radiochemical method shows a good agreement when taking into account the associated uncertainties.


Assuntos
Espectrometria de Massas/métodos , Resíduos Radioativos/análise , Espectrofotometria Atômica/métodos , Radioisótopos de Estrôncio/análise , Partículas beta , Modelos Lineares , Espectrometria de Massas/instrumentação , Reprodutibilidade dos Testes , Espectrofotometria Atômica/instrumentação , Radioisótopos de Estrôncio/química , Radioisótopos de Estrôncio/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química
5.
Food Chem ; 317: 126437, 2020 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-32109660

RESUMO

SO2 is a type of additive widely used in the food processing industry as preservative and anti-browning, bleaching, or effective antibacterial agent. However, the SO2 residue can have adverse effects on human health. In this work, a low-temperature microplasma generated by dielectric barrier discharge was used for the direct, in situ excitation of the molecular emission of SO2 in food samples. The food samples were acidified and heated to release SO2 and a miniaturized charge-coupled device spectrometer recorded the characteristic emission line at 301.9 nm. The linear correlation coefficient of the method was greater than 0.99 in the range of 10 to 100 mg L-1. Moreover, the limit of detection was 0.01 mg L-1, with recoveries between 72% and 108% and relative standard deviations of 1.5%-7.6%. The method is simple, accurate, low-cost, involves miniaturized and compact equipment and is suitable for the determination of total SO2 in food samples.


Assuntos
Análise de Alimentos/instrumentação , Espectrofotometria Atômica/instrumentação , Dióxido de Enxofre/análise , Desenho de Equipamento , Aditivos Alimentares/análise , Análise de Alimentos/métodos , Limite de Detecção , Miniaturização , Espectrofotometria Atômica/métodos
6.
Appl Spectrosc ; 74(5): 563-570, 2020 May.
Artigo em Inglês | MEDLINE | ID: mdl-32031011

RESUMO

Depth profiling investigation plays an important role in studying the dynamic processes of the ocean. In this paper, a newly developed hyphenated underwater system based on multi-optical spectrometry is introduced and used to measure seawater spectra at different depths with the aid of a remotely operated vehicle (ROV). The hyphenated system consists of two independent compact deep-sea spectral instruments, a deep ocean compact autonomous Raman spectrometer and a compact underwater laser-induced breakdown spectroscopy system for sea applications (LIBSea). The former was used to take both Raman scattering and fluorescence of seawater, and the LIBS signal could be recorded with the LIBSea. The first sea trial of the developed system was taken place in the Bismarck Sea, Papua New Guinea, in June 2015. Over 4000 multi-optical spectra had been captured up to the diving depth about 1800 m at maximum. The depth profiles of some ocean parameters were extracted from the captured joint Raman-fluorescence and LIBS spectra with a depth resolution of 1 m. The concentrations of SO42- and the water temperatures were measured using Raman spectra. The fluorescence intensities from both colored dissolved organic matter (CDOM) and chlorophyll were found to be varied in the euphotic zone. With LIBS spectra, the depth profiles of metallic elements were also obtained. The normalized intensity of atomic line Ca(I) extracted from LIBS spectra raised around the depth of 1600 m, similar to the depth profile of CDOM. This phenomenon might be caused by the nonbuoyant hydrothermal plumes. It is worth mentioning that this is the first time Raman and LIBS spectroscopy have been applied simultaneously to the deep-sea in situ investigations.


Assuntos
Clorofila/análise , Água do Mar/química , Espectrofotometria Atômica/instrumentação , Análise Espectral Raman/instrumentação , Ésteres do Ácido Sulfúrico/análise , Metais/análise , Oceano Pacífico , Espectrofotometria Atômica/métodos , Análise Espectral Raman/métodos , Temperatura
7.
Food Chem ; 302: 125336, 2020 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-31419772

RESUMO

This study reports a stepwise optimization of switchable liquid-liquid microextraction (SLLME) for cobalt determination by flame atomic absorption spectrometry (FAAS) coupled with a slotted quartz tube (SQT). The main purpose of this study was to develop an accurate and sensitive analytical method for cobalt. Extraction method was used to separate and preconcentrate cobalt from sage tea and vitamin B12 samples after complexing with a Schiff base ligand. 107.7 folds enhancement in detection power under the optimum conditions was recorded with respect to direct FAAS. This enhancement correlated to 3.1 µg/L limit of detection and 10 µg/L limit of quantification. The SLLME-SQT-FAAS method was linear over a broad concentration range and low %RSD values established high precision for the method. Appreciable percent recovery results (94-108%) obtained from spiked sage sample and from cobalamin also validated the accuracy of the method.


Assuntos
Cobalto/análise , Microextração em Fase Líquida/métodos , Espectrofotometria Atômica/métodos , Chás de Ervas/análise , Vitamina B 12/análise , Limite de Detecção , Quartzo , Reprodutibilidade dos Testes , Salvia officinalis/química , Bases de Schiff/química , Espectrofotometria Atômica/instrumentação , Vitamina B 12/química
8.
Food Chem ; 310: 125825, 2020 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-31753689

RESUMO

Preconcentration of cobalt was carried out with deep eutectic solvent based liquid phase microextraction (DES-LPME) for trace determination by a slotted quartz tube (SQT) attached flame atomic absorption spectrometry (FAAS) system. Choline chloride and phenol in a 1:2 M ratio was used as a green solvent to extract cobalt from the aqueous sample solution. Key parameters influencing the extraction efficiency of cobalt were examined and optimized. Under the conditions optimized, the linear dynamic range was found between 5.0 and 50 µg L-1, and the limits of detection and quantification (LOD and LOQ) were calculated as 2.0 and 6.6 µg L-1, respectively. The detection power of the conventional FAAS was improved upon by 67 folds using the optimized DES-LPME-SQT-FAAS method. The developed analytical method was successfully applied for the determination of cobalt in linden tea samples and the recovery results obtained for different spiked concentrations (20, 30 and 40 µg L-1) were remarkable (≈100%).


Assuntos
Cobalto/análise , Análise de Alimentos/métodos , Microextração em Fase Líquida/métodos , Espectrofotometria Atômica/métodos , Cobalto/isolamento & purificação , Química Verde , Limite de Detecção , Quartzo/química , Solventes/química , Espectrofotometria Atômica/instrumentação , Chás de Ervas/análise , Tilia/química , Água/química
9.
Food Chem ; 310: 125824, 2020 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-31732245

RESUMO

In this work, a home-made portable dielectric barrier discharge-atomic emission spectrometer (DBD-AES) was explored to the determination of heavy metal in foodstuffs. A rapid and simple method was developed for Cd determination in rice based on this instrument. Rice was pretreated with diluted acid dissolution without complex operations and apparatus. The detection time by DBD-AES is about 3 min and the total analysis time for rice sample is within 11 min. The effects of some key experiment parameters were investigated. The limit of detection was 11.9 µg kg-1 for Cd in rice, much lower than the maximum allowable level established by EC (200 µg kg-1). The practical performance of this method was demonstrated by analyzing real and CRM rice samples. With the portability of DBD-AES, the method is suitable for rapid and in-field analysis of Cd in rice. It will be a useful tool for the routine analysis of rice.


Assuntos
Cádmio/análise , Análise de Alimentos/instrumentação , Contaminação de Alimentos/análise , Oryza/química , Espectrofotometria Atômica/instrumentação , Análise de Alimentos/métodos , Limite de Detecção , Espectrofotometria Atômica/métodos , Fatores de Tempo
10.
Anal Bioanal Chem ; 411(27): 7251-7260, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31612256

RESUMO

Chloride widely exists in the environment and will cause serious interference for arsenic speciation analysis. The determination of four arsenic species including arsenite (As(III)), arsenate (As(V)), monomethylarsenate (MMA), and dimethylarsonate (DMA) in samples containing high concentrations of Cl- was carried out in this work by coupling of liquid chromatography (LC) with hydride generation atomic fluorescence spectrometry (HG-AFS). The interference of Cl- was successfully eliminated by coupling two anion-exchange chromatographic columns in series and eluting with 35.0 mmol L-1 (NH4)2HPO4 (pH = 6.00). A novel pre-treatment system was subsequently developed to realize on-line column switch and pre-reduction of As(V). The analysis time was shortened by an isocratic elution but programmed flow rate method, and the sensitivity of As(V) was also enhanced by the introduction of pre-reduction using the developed system. The proposed method can resist at least 10 g L-1 Cl- without any pre-treatment operations. Since LC-HG-AFS is low-cost and can be afforded or self-assembled by most labs, the developed method can be adopted as a routine analysis method for arsenic species in chloride-bearing samples, such as urine and seawater. Graphical abstract.


Assuntos
Arseniatos/análise , Arsenicais/análise , Arsenitos/análise , Poluentes Químicos da Água/análise , Arseniatos/urina , Arsênio/análise , Arsênio/urina , Arsenicais/urina , Arsenitos/urina , Cloretos/análise , Cloretos/urina , Cromatografia Líquida de Alta Pressão/instrumentação , Desenho de Equipamento , Humanos , Limite de Detecção , Metilação , Água do Mar/análise , Espectrometria de Fluorescência/instrumentação , Espectrofotometria Atômica/instrumentação , Poluentes Químicos da Água/urina
11.
Analyst ; 144(17): 5117-5126, 2019 Aug 16.
Artigo em Inglês | MEDLINE | ID: mdl-31309214

RESUMO

Many species of Dalbergia are prized hardwoods, generally referred to as 'Rosewood,' and used in high-end products due to their distinctive hue and scent. Despite more than 58 species of Dalbergia being listed as endangered in Appendix 1 of The Convention on International Trade in Endangered Species of Fauna and Flora (CITES), the illegal logging and trade of this timber is ongoing. In this work, a handheld laser induced breakdown spectrometer (LIBS) was used to analyze seven Dalbergia species and two other exotic hardwood species to evaluate the ability of handheld LIBS for rapid classification of Dalbergia in the field. The KNN model of the classification presented 80% to 90% sensitivity for discriminating between Dalbergia species in the training set. PLS-DA models were based on a binary decision tree structure. Cumulatively, the PLS-DA decision tree model showed greater than 97% sensitivity and 99% selectivity for prediction of Dalbergia species included in the training set. The data presented in the following study are promising for the use of handheld LIBS devices and both KNN and PLS-DA models for applications in customs screenings at the port of entry of hard woods, among others.


Assuntos
Dalbergia/classificação , Madeira/química , Árvores de Decisões , Análise Discriminante , Espécies em Perigo de Extinção , Análise dos Mínimos Quadrados , Espectrofotometria Atômica/instrumentação , Espectrofotometria Atômica/métodos
12.
Food Chem ; 297: 124947, 2019 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-31253290

RESUMO

Newly developed combination of magnetic cobalt particles based dispersive solid-phase microextraction (Co-MP-DSPME) and slotted quartz tube attached flame atomic absorption spectrometry (SQT-FAAS) was utilized to determine lead at trace levels in tea samples. Co-MPs' adsorbent properties were tested and validated for their selectiveness to lead. Only with a few and short extraction steps (i.e. adding MPs, mixing, decanting and eluting) analyte was extracted from sample solution rapidly and efficiently. Limit of detection (LOD) and limit of quantification (LOQ) for the developed method (Co-MP-DSPME-SQT-FAAS) were found to be 7.77 µg/L and 25.9 µg/L, respectively. Matrix matching strategy was performed and outcomes indicated that the developed method is applicable with the high percent recovery values of 110.1 ±â€¯4.5 and %102.9 ±â€¯4.2 for 100 and 300 µg/kg lead standard spiked black tea samples, respectively. The method was also applied to standard reference material to check the accuracy of the method.


Assuntos
Contaminação de Alimentos/análise , Chumbo/análise , Microextração em Fase Sólida/métodos , Espectrofotometria Atômica/métodos , Chá/química , Cobalto/química , Análise de Alimentos/métodos , Limite de Detecção , Quartzo/química , Sensibilidade e Especificidade , Microextração em Fase Sólida/instrumentação , Espectrofotometria Atômica/instrumentação
13.
Talanta ; 202: 178-185, 2019 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-31171167

RESUMO

A novel direct sampling (DS-HG) system consisting of an enlarged gas liquid separator (GLS) coupled with a foam breaker was firstly utilized for the in-situ dielectric barrier discharge atomic fluorescence spectrometer (DBD-AFS). After direct dilution using 5% HCl (v:v), a prepared blood sample was introduced into the DS-HG with a UV digestion unit, of which arsenic hydrides directly generated from sample under 5% HCl (v:v) and 5 g/L KBH4 in 1.5 g/L KOH. Herein, the newly designed DS-HG is capable of effectively eliminating foam generation deriving from protein in blood sample. Then, arsenic hydrides were trapped by 11 kV discharging at 110 mL/min air, and released by 13 kV at 180 mL/min H2 orderly. Under the optimized conditions, the linearity ranged from 0.05 to 50 ng/mL with a regression coefficient (R2) = 0.996. The method detection limit (LOD) was 7 pg arsenic (0.14 ng/mL), and relative standard deviation (RSD) of 10 repeated measurements for a real blood sample was 4.2%, indicating a good precision. The spiked recoveries for real samples were in the range of 97%-102%. Furthermore, arsenic presence in real blood samples measured by the proposed method were consistent (P > 0.05) with the microwave digestion ICP-MS. The whole analytical time can be controlled within 8 min including sample dilution. As a matter of fact, it is a favorable progress for DBD technique to eliminate matrix interferences of real samples based on the gas phase enrichment (GPE) principle, with advantages such as excellent sensitivity, digestion-free, fast and simple operation. Thus, the recommended DS-HG-in-situ DBD-AFS are suitable to the fast analysis of ultratrace arsenic in blood samples to protect human's health.


Assuntos
Arsênio/sangue , Gases/química , Boroidretos/química , Humanos , Ácido Clorídrico/química , Hidróxidos/química , Compostos de Potássio/química , Espectrometria de Fluorescência/instrumentação , Espectrofotometria Atômica/instrumentação
14.
Nutr Hosp ; 36(4): 753-757, 2019 Aug 26.
Artigo em Espanhol | MEDLINE | ID: mdl-31192688

RESUMO

INTRODUCTION: Introduction: a black precipitate was observed in the filter during the infusion of a parenteral nutrition without lipids. There are similar findings published in which copper and sulphur (from cysteine) were found in the composition of the precipitate. Objective: to determine if copper and cysteine are involved in the formation of the precipitate. Methods: samples of the parenteral nutrition solution were taken before and after its passage through the filter. Amino acids concentrations were analysed in both samples by ion exchange chromatography and post-column derivatization with ninhydrin in a Biochrom 30 device. Copper concentrations were measured by atomic absorption spectrometry in a PerkinElmer AAnalyst™ 200 device. Results: a decrease in cysteine concentration of 29.3% was found. The concentration of copper decreased by 75.9%. Conclusions: the decrease in the concentrations of cysteine and copper in the filtered solution suggest that both are involved in the formation of the black precipitate observed in the filter.


INTRODUCCIÓN: Introducción: durante la infusión de una nutrición parenteral sin lípidos se observó un precipitado negro en el filtro. Hay hallazgos similares publicados en los que se han detectado cobre y azufre (proveniente de la cisteína) en la composición del precipitado. Objetivo: comprobar que la cisteína y el cobre intervienen en la formación del precipitado. Métodos: se tomaron muestras de la solución de nutrición parenteral antes y después de su paso por el filtro. Se analizaron en ambas muestras las concentraciones de aminoácidos mediante cromatografía de intercambio iónico y derivatización post-columna con ninhidrina en un equipo Biochrom 30 y las de cobre mediante espectrometría de absorción atómica en un equipo PerkinElmer AAnalyst™ 200. Resultados: las concentraciones de cisteína y cobre en la solución disminuyeron en un 29,3% y 75,9%, respectivamente. Conclusiones: la disminución de las concentraciones de cisteína y cobre en la solución filtrada sugieren que ambos están involucrados en la formación del precipitado negro observado en el filtro.


Assuntos
Precipitação Química , Cobre/análise , Cisteína/análise , Soluções de Nutrição Parenteral/química , Nutrição Parenteral , Aminoácidos/análise , Cor , Filtração/instrumentação , Nutrição Parenteral/instrumentação , Espectrofotometria Atômica/instrumentação
15.
Anal Chem ; 91(4): 2701-2709, 2019 02 19.
Artigo em Inglês | MEDLINE | ID: mdl-30615435

RESUMO

A simple and miniature analytical system was developed to determine Hg and Cd in small amounts of samples by integrating flow injection capillary liquid electrode discharge (CLED) optical emission spectrometry (OES) and microplasma-induced vapor generation (PIVG) atomic fluorescence spectrometry (AFS). With the assistance of the inherent capillary driving force and the force arising from the solution vaporization in the microplasma, the sample solution was automatically transported into the discharge chamber wherein analytes were simultaneously excited to generate their atomic emission lines and converted to their volatile species. Subsequently, the volatile species were further swept into AFS for their further determination. Therefore, the same sample could be successively analyzed by OES and AFS. Owing to the unique independent linear-range and sensitivity of CLED-OES and PIVG-AFS, the developed system not only significantly extended its linear range to 6 orders of magnitude but also remarkably reduced the sample consumption to several microliters. Thus, wide linear-range and ultrasensitive determination of Hg and Cd in limited amounts of samples were accomplished simply by sharing one single capillary liquid electrode discharge source. Under the optimized conditions, limits of detection (LODs) of 10 µg L-1 were obtained for both Hg and Cd when CLED-OES was used as a detector, whereas the LODs for Hg and Cd were improved to 0.03 µg L-1 and 0.04 µg L-1 with AFS detector, respectively. In addition, the extremely wide linear-range of 0.001-100 mg L-1 and 0.001-40 mg L-1 were obtained for Hg and Cd, respectively. The potential application of this method was validated by successfully analyzing three Certified Reference Materials (ZK021-1, GBW(E)090033, and GBW(E)090034) and six human blood samples.


Assuntos
Cádmio/sangue , Análise de Injeção de Fluxo/métodos , Mercúrio/sangue , Espectrometria de Fluorescência/métodos , Espectrofotometria Atômica/métodos , Adulto , Desenho de Equipamento , Análise de Injeção de Fluxo/instrumentação , Humanos , Limite de Detecção , Espectrometria de Fluorescência/instrumentação , Espectrofotometria Atômica/instrumentação
16.
Food Chem ; 273: 130-135, 2019 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-30292358

RESUMO

A method for simultaneous determination of Fe (232.036 nm) and Ni (232.195 nm) in vegetable oil samples by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) after an acid extraction of the analytes is proposed. In the extraction step, hydrochloric, nitric and acetic acid solutions were tested. The optimization of the procedure was performed by applying Doehlert matrix, and multiple response was used for simultaneous evaluation of the performance of the extraction. The optimum conditions were: extraction time of 17 min, extraction temperature of 39 °C and sonication amplitude of 42%, employing 0.5 mol L-1 HCl as the extracting solvent. The limits of quantification were 60 and 160 ng g-1 for Fe and Ni, respectively. The method was applied to the analysis of vegetable oil samples and the results were compared with a method employing inductively coupled plasma optical emission spectrometry (ICP OES).


Assuntos
Fracionamento Químico/métodos , Análise de Alimentos/métodos , Ferro/análise , Níquel/análise , Óleos de Plantas/análise , Fracionamento Químico/instrumentação , Análise de Alimentos/instrumentação , Contaminação de Alimentos/análise , Grafite/química , Análise Multivariada , Óleos de Plantas/química , Espectrofotometria Atômica/instrumentação , Espectrofotometria Atômica/métodos , Temperatura , Ultrassom
17.
Anal Chem ; 90(10): 6332-6338, 2018 05 15.
Artigo em Inglês | MEDLINE | ID: mdl-29688699

RESUMO

The mechanisms of arsenic gas phase enrichment (GPE) by dielectric barrier discharge (DBD) was investigated via X-ray photoelectron spectroscopy (XPS), in situ fiber optic spectrometer (FOS), etc. It proved for the first time that the arsenic species during DBD trapping, release, and transportation to the atomic fluorescence spectrometer (AFS) are probably oxides, free atoms, and atom clusters, respectively. Accordingly, a novel in situ DBD trap as a GPE approach was redesigned using three-concentric quartz tube design and a modified gas line system. After trapping by O2 at 9.2 kV, sweeping for 180 s, and releasing by H2 at 9.5 kV, 2.8 pg detection limit (LOD) was achieved without extra preconcentration (sampling volume = 2 mL) as well as 4-fold enhancement in absolute sensitivity and ∼10 s sampling time. The linearity reached R2 > 0.998 in the 0.1-8 µg/L range. The mean spiked recoveries for tap, river, lake, and seawater samples were 100-106%; and the measurements of the certified reference materials (CRMs) were in good agreement with the certified values. In situ DBD trap is also suitable to atomic absorption spectrometry (AAS) or optical emission spectrometry (OES) for fast and on-site determination of multielements.


Assuntos
Arsênio/análise , Espectrofotometria Atômica/instrumentação , Espectrofotometria Atômica/métodos
18.
Anal Bioanal Chem ; 410(19): 4715-4723, 2018 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-29675708

RESUMO

A simple, highly efficient, batch, and centrifuge-less dispersive liquid-liquid microextraction method based on a magnetic ionic liquid (MIL-DLLME) and electrothermal atomic absorption spectrometry (ETAAS) detection was developed for ultra-trace Cd determination in honey. Initially, Cd(II) was chelated with ammonium diethyldithiophosphate (DDTP) at pH 0.5 followed by its extraction with the MIL trihexyl(tetradecyl)phosphonium tetrachloroferrate(III) ([P6,6,6,14]FeCl4) and acetonitrile as dispersant. The MIL phase containing the analyte was separated from the aqueous phase using only a magnet. A back-extraction procedure was applied to recover Cd from the MIL phase using diluted HNO3 and this solution was directly injected into the graphite furnace of ETAAS instrument. An extraction efficiency of 93% and a sensitivity enhancement factor of 112 were obtained under optimal experimental conditions. The detection limit (LOD) was 0.4 ng L-1 Cd, while the relative standard deviation (RSD) was 3.8% (at 2 µg L-1 Cd and n = 10), calculated from the peak height of absorbance signals. This work reports the first application of the MIL [P6,6,6,14]FeCl4 along with the DLLME technique for the successful determination of Cd at trace levels in different honey samples. Graphical abstract Preconcentration of ultratraces of Cd in honey using a magnetic ionic liquid and dispersive liquid-liquid microextraction technique.


Assuntos
Cádmio/análise , Mel/análise , Líquidos Iônicos/química , Microextração em Fase Líquida/métodos , Imãs/química , Espectrofotometria Atômica/métodos , Cádmio/isolamento & purificação , Desenho de Equipamento , Limite de Detecção , Microextração em Fase Líquida/instrumentação , Magnetismo/instrumentação , Magnetismo/métodos , Concentração Osmolar , Espectrofotometria Atômica/instrumentação
19.
Talanta ; 175: 150-157, 2017 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-28841972

RESUMO

A novel flowing liquid cathode glow discharge (LCGD) was developed as an excitation source of the atomic emission spectrometry (AES) for the determination of Ca and Zn in digested calcium and zinc gluconates oral solution and blood samples, in which the glow discharge is produced between the electrolyte (as cathode) overflowing from a quartz capillary and the needle-like Pt anode. The electron temperature and electron density of LCGD were calculated at different discharge voltages. The discharge stability and parameters affecting the LCGD were investigated in detail. In addition, the measured results of real samples using LCGD-AES were verified by ICP-AES. The results showed that the optimized analytical conditions are pH = 1 HNO3 as supporting electrolyte, 4.5mLmin-1 solution flow rate. The power consumption of LCGD is 43.5-66.0W. The R2 and the RSD ranged from 630 to 680V are 0.9942-0.9995 and 0.49%-2.43%, respectively. The limits of detections (LODs) for Zn and Ca are 0.014-0.033 and 0.011-0.097mgL-1, respectively, which are in good agreement with the closed-type electrolyte cathode atmospheric glow discharge (ELCAD). The obtained results of Ca and Zn in real samples by LCGD-AES are basically consistent with the ICP-AES and reference value. The results suggested that LCGD-AES can provide an alternative analytical method for the detection of metal elements in biological and medical samples.


Assuntos
Cálcio/análise , Gluconatos/análise , Espectrofotometria Atômica/instrumentação , Zinco/análise , Cálcio/sangue , Eletrodos , Desenho de Equipamento , Gluconatos/sangue , Humanos , Limite de Detecção , Soluções Farmacêuticas/análise , Espectrofotometria Atômica/métodos , Temperatura , Zinco/sangue
20.
Talanta ; 175: 406-412, 2017 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-28842009

RESUMO

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO3, HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL-1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg-1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg-1 which were below the limits of 300, 200 and 100µgkg-1 set by the Brazilian, Chinese and European legislation, respectively.


Assuntos
Arsênio/análise , Arsenicais/análise , Ácido Cacodílico/análise , Análise de Alimentos/métodos , Alimentos Infantis/análise , Espectrofotometria Atômica/métodos , Desenho de Equipamento , Análise de Alimentos/instrumentação , Contaminação de Alimentos/análise , Humanos , Lactente , Recém-Nascido , Micro-Ondas , Oryza/química , Sonicação/instrumentação , Sonicação/métodos , Espectrofotometria Atômica/instrumentação
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