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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
11

Determination Of Thallium By Volatile Compound Generation Atomic Absorption Spectrometry

Ataman, Seval 01 October 2011 (has links) (PDF)
Determination of thallium is important due to its toxic effects on the environment and human health. Extremely low abundance of thallium in earth crust requires very sensitive and accurate methods for determination of this element. Although volatile compound generation is a sensitive, fast and economical method, thallium determination by this method has not been sufficiently investigated in literature, because of the fact that the formation of volatile forms of this element is a difficult task. A continuous flow volatile compound generation system was developed and parameters that affect the analytical signal were optimized. Sample solutions were acidified with 0.5 mol/L HNO3 and prepared in 0.0005% (v/v) rhodamine B and 1.0 mg/L Pd while 0.5% (m/v) NaBH4 stabilized in 0.5% (m/v) NaOH was used as reductant. Fast decomposition and unstability of thallium volatile species affected system performance negatively. Flow injection volatile compound generation studies were carried out with a special system. After optimizations, LOD and LOQ values were calculated as 12 ng/mL and 40 ng/mL according to peak height values in HNO3 medium. Similarly, in HCl medium LOD and LOQ values were calculated as 14 ng/mL and 45 ng/mL. Addition of Te and Pd to the sample solution containing co-enhancement reagent rhodamine B improved volatile compound generation efficiency in peak height by 3.6 and 9.3, respectively. Type of the acid used was affected peak heights and peak shapes of Tl+ and Tl3+ volatile species and HNO3 medium gave better results. By changing the location of introduction for Ar gas, the sources of memory effects and reasons of peak broadening were investigated. Most of the memory effects were coming from the gas-liquid separator (GLS) or before the GLS, as well as T-tube atomizer. Nature and behavior of Tl volatile species were also investigated and it was found that Tl and also Pd were generated in the form of nanoparticles. Transmission electron microscopic (TEM) measurements prove the presence of Tl nanoparticles in the analyte species transported to the atomizer by the effect of carrier Ar gas.
12

On-line Preconcentration, Speciation And Determination Of Chromium By Flame Atomic Absorption Spectrometry (faas) And Chemiluminescence (cl)

Surdem, Sedat 01 June 2004 (has links) (PDF)
ABSTRACT Toxicological studies have shown that the degree of toxicity of some elements depends on the chemical form in which the element is present. Chromium (III) is considered as an essential micronutrient for human whereas chromium (VI) is a potentially carcinogenic agent. So the speciation of inorganic chromium in environmental samples is required for accurate assessment of pollution levels. The chromium content in natural water is usually very low, and a preconcentration is often necessary prior to the determination. A sensitive and selective preconcentration and speciation procedure is developed for the determination of trace and ultra trace amounts of chromium species by utilizing chemiluminescence (CL) and flame atomic absorption spectrometric (FAAS) techniques. The performances of amino silica-gel, amino sol-gel, mercapto silica-gel beads and metal oxides for solid phase extraction of chromium are examined either in column or batch type studies. Considering the advantage of concentrating Cr(III) and Cr(VI) ions separately simply by adjusting the pH of the medium, amino silica-gel resin is chosen in this study. The influences of different experimental parameters on the separation and preconcentration of chromium species such as pH, eluent concentration, flow rate, particle size of the resin are investigated. Chemiluminescence detection studies are performed by using the catalytic effect of Cr (III) on the reaction between luminol and hydrogen-peroxide and Cr (VI) is detected after reduction to Cr (III). Luminol and H2O2 concentrations and the pH of the medium are optimized to increase the sensitivity of the system. Chemiluminescence is inherently a very sensitive technique. When a preconcentration step is included in the CL mesurement of very low concentrations of chromium is possible to determine. Indeed, a 25-fold enhancement in sensitivity of chromium ions is achieved after incorporating amino silane&ndash / gel colums in the system and 0.2 &amp / #61549 / g/L of chromium (corresponds to the concentration of chromium in natural waters) was measured. A fully automated FI-CL system is designed that allows all necessary operations to be performed on-line. This system allows the pre-conditioning of micro-columns with different buffer solutions / adsorption of chromium species in micro-columns / washing these columns to remove interfering matrix components / elution of the species with minimum volume / transporting the species and chemiluminescence reagents to the cell / and, finally, cleaning of all pertinent conduits in the FIA-system in order to prevent carry-over between individual samples.
13

Electrochemical Hydride Generation And Atom Trapping Atomic Absorption Spectrometry For Determination Of Antimony

Menemenlioglu, Ipek 01 June 2004 (has links) (PDF)
ABSTRACT ELECTROCHEMICAL HYDRIDE GENERATION AND ATOM TRAPPING ATOMIC ABSORPTION SPECTROMETRY FOR DETERMINATION OF ANTIMONY Menemenlioglu, ipek M.S., Department of Chemistry Supervisor: Prof. Dr. O. Yavuz Ataman June 2004, 82 pages Electrochemical hydride generation is a suitable alternative to common hydride generation by NaBH4 which is widely used for the detection of volatile elements such as As, Se, Sb, Sn, Bi, Ge, Te and Pb. In this study, a thin-layer flow through electrochemical cell was designed. Lead and platinum foils were employed as cathode and anode materials, respectively, for the generation of antimony hydride. Argon was used as the carrier gas. The inlet arm of the conventional quartz tube atomizer was used for on-line preconcentration of generated hydrides. A portion of the inlet arm was heated externally to the collection temperature for trapping the analyte species which were generated electrochemically. For the revolatilization of the trapped species, the trap was further heated to the revolatilization temperature and hydrogen gas was introduced into the system 10 seconds afterwards. The experimental operation conditions for electrochemical hydride generation which include the acidities and flow rates of catholyte and anolyte solutions, carrier gas flow rate and the applied electric current, were optimized. For trapping, collection and revolatilization temperatures and hydrogen flow rates were optimized. Analyses of standard reference materials were performed to check the accuracy of the proposed method. 3&amp / #963 / limit of detections were found as 1.03 ng ml-1 and 0.053 ng ml-1 with and without employing the trap, respectively. The trap has provided 20 fold sensitivity improvement.
14

Determination Of Germanium At Trace Levels By Chloride Generation Atomic Absorption Spectrometry

Kaya, Murat 01 July 2004 (has links) (PDF)
Trace amounts of germanium is determined by flame atomic absorption spectrometry by utilizing the vaporization of germanium tetrachloride. Using a continuous flow reactor, sample solution is mixed with concentrated hydrochloric acid and heated to 80&ordm / C to form volatile germanium tetrachloride which can be subsequently sent to N2O-C2H2 flame AAS. The necessary conditions for the volatilization of germanium tetrachloride are investigated in detail and the applicability of the method for the determination of trace amounts of germanium in real samples and standard reference materials are presented. Detection limit of the method, based on 3s, was 0.034 ng mL-1 using a sample of 1 mL. The precision was 0.3 %, expressed as the relative standard deviation for a germanium concentration of 1 ng mL-1. Owing to the high selectivity of the proposed method, no interference effect was observed.
15

Odstraňování olova z odpadní vody za využití umělého mokřadu / Removal of lead from wastewater using a constructed wetland

JAHODOVÁ, Jana January 2017 (has links)
Removal of lead from municipal wastewater using a constructed wetland with a horizontal subsurface flow was studied. Wastewater, wetland plant and sediment samples were analyzed using an AAS Thermo Scientific iCE 3500. Average concentrations of lead in inflow and outflow water in 2015 were 1.47 and 0.74 ?g/l, respectively. Average concentrations of lead in inflow and outflow water in 2016 were 0.75 and 0.38 ?g/l. The average efficiency of lead removal was 49.2 %. Lead concentrations in vegetation (Phragmites australis) varied in the range of 0.081-0.087 mg/kg and 0.48-0.17 mg/kg for the above and belowground biomass, respectively. Lead concentration in sediments were 9.79 and 4.86 mg/kg at distances of 1 and 10 m from inflow zone. Lead and other heavy metals were predominantly removed from wastewater at the initial part of the wetland bed.
16

Minerais essenciais em meis / Essential minerals in honey

Torrezan, Marina Alvarez 30 July 2008 (has links)
Orientador: Marcelo Alexandre Prado / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-11T09:10:51Z (GMT). No. of bitstreams: 1 Torrezan_MarinaAlvarez_M.pdf: 599247 bytes, checksum: 94d08561b45519ee935426b1a68419e9 (MD5) Previous issue date: 2008 / Resumo: O mel é um dos alimentos mais antigos conhecido pelo ser humano, sendo que suas propriedades terapêuticas já eram descritas desde a antiguidade. É produzido por meio de abelhas melíferas a partir do néctar das flores ou outras secreções das plantas, o qual é transformado, combinado com enzimas salivares, armazenado e amadurecido nos favos das colméias. Os elementos minerais essenciais são divididos entre macroelementos (cálcio, fósforo, potássio, sódio, cloro, magnésio, enxofre) e microelementos (ferro, cobre, zinco, cobalto, manganês, iodo, flúor, selênio, cromo, silício), de acordo com as quantidades, maiores ou menores em que são encontrados no organismo humano. Quimicamente, trata-se de uma matriz complexa, composta por água, glicose, frutose, sacarose, cinzas, ácidos, grãos de pólen, partículas de cera, proteínas, pigmentos, álcoois, aminoácidos, dextrinas, enzimas, compostos voláteis, vitaminas e minerais. A composição depende da origem e da constituição do néctar, sendo que a concentração de minerais normalmente varia de 0,1 a 1,0%. É um desafio analítico determinar metais em alimentos ricos em açúcar, devido à interferência da matriz. A técnica mais comum de espectrometria de absorção atômica é a com atomização por chama, a qual foi utilizada neste trabalho. Quando há amostra, o vapor atômico absorve parte da radiação ressonante emitida pela fonte, que é demonstrado pelo enfraquecimento da cor do feixe que passa pela chama. Tal processo está relacionado com a concentração do analito a ser determinado. Trata-se de uma técnica analítica notável por sua seletividade, velocidade, baixo custo operacional, simplicidade e estabilidade. Este trabalho teve como objetivo determinar valores de cálcio, cobre, ferro, magnésio, manganês, potássio, sódio e zinco. Os valores encontrados variaram de 1,91- 4,52 mg/g, <0,35-1,04 mg/g, 1,00-3,66 mg/g, traços de magnésio (<0,1 mg/g), 0,24-4,65 mg/g, 1,58-55,9 mg/g, 1,01-20,02 mg/g, e <0,18-3,17 mg/g, respectivamente. Também foram determinados parâmetros de otimização da metodologia e os resultados encontrados de minerais foram comparados com os valores de Ingestão Diária Recomendada (IDR) / Abstract: Honey is one of the oldest known food for mankind, and that its therapeutic properties were already described since antiquity. It is produced by honey bees from the nectar of flowers or other secretions plant, which is turned, combined with salivates enzymes, stored and mature honeycombs in the hives. The elements essential minerals are divided between macro (calcium, phosphorus, potassium, sodium, chloride, magnesium, sulfur) and microelements (iron, copper, zinc, cobalt, manganese, iodine, fluorine, selenium, chromium, silicon), according to the quantities, more or less where they are found in the human body. Chemically, it is a complex matrix, composed of water, glucose, fructose, sucrose, ash, acids, grains of pollen, particles of wax, proteins, pigments, alcohols, amino acids, dextrin, enzymes, volatile compounds, vitamins and minerals. The composition depends on the origin and composition of nectar, and the concentration of minerals typically ranges from 0.1 to 1.0%. It is an analytical challenge to determine metals in foods high in sugar, due to the interference of the matrix. The most common technique of atomic absorption spectrometry is to spray a flame, which was used in this work. When there are sample, the atomic vapors absorbs part of resonant radiation emitted by the source, which is demonstrated by the weakening of the color of the beam that passes through the flame. This process is related to the concentration of the analyte to be determined. This is a notable analytical technique for its selectivity, speed, low operational cost, simplicity and stability. This study aimed to determine values of calcium, copper, iron, magnesium, manganese, potassium, sodium and zinc. The amounts found ranged from 1,91-4,52 mg / g <0,35-1,04 mg / g, 1,00-3,66 mg / g, traces of magnesium (<0.1 mg / g), 0,24-4,65 mg / g 1,58-55,9 mg / g 1,01-20,02 mg / g, and <0,18-3,17 mg / g, respectively. They also were certain parameters to optimize the methodology and results of minerals were compared with the values of Recommended Dietary Allowance (RDA) / Mestrado / Mestre em Ciência de Alimentos
17

Desenvolvimento de métodos para determinações elementares em cimentos por espectrometria de absorção atômica com forno de grafite e amostragem direta de sólidos / Development of methods for elemental determination in cements by atomic absorption spectrometry with graphite furnace and direct solid sampling

Danielle Polidorio Intima 18 September 2008 (has links)
O objetivo desse trabalho foi o desenvolvimento de métodos analíticos para a determinação de Cd, Pb, Cu, Ni, Co, Cr e Mn em cimentos Portland por espectrometria de absorção atômica com atomização em forno de grafite e amostragem direta de sólidos. Não foi necessário nenhum tipo de pré-tratamento das amostras, pois apresentaram tamanhos médios de partículas (~12 &#181;m) adequados para aplicação em análise direta de sólidos. Os programas de aquecimento foram otimizados a partir da avaliação térmica de cada um dos elementos (curvas de pirólise e atomização), do uso de modificadores químicos e de matriz e da comparação de curvas de calibração em solução aquosa e na presença da amostra sólida. Todas as determinações dos elementos foram feitas usando curvas de calibração obtidas em meio de solução aquosa. Devido a alta concentração nas amostras, no caso do Cu, Ni, Co, Cr e Mn foi necessário o uso da correção de fundo por efeito Zeeman com 3 campos, aumentando a representatividade. Nessa condição, foi possível a pesagem de alíquotas da amostra de até 200 &#181;g para análise. As melhores condições para as determinações de Cd e Pb foi com o uso do modificador químico 5 &#181;g de Pd em 0,1 % m v-1 de Triton X-100. Nessa condição, as melhores temperaturas de pirólise e atomização foram 600&#176;C e 2000&#176;C para Cd e 900&#176;C e 2100&#176;C para Pb, respectivamente. As determinações de Cu e Ni foram possíveis sem o uso de modificador químico ou de matriz. As temperaturas de pirólise e atomização foram 1200&#176;C e 2600&#176;C, respectivamente, para os dois elementos. As determinações de Co, Cr e Mn foram realizadas com o uso de modificador de matriz (Na2CO3 + ZnO) que promoveu uma fusão in situ durante o programa de aquecimento. Nessas condições, as temperaturas de pirólise e atomização foram 1400 &#176;C e 2600 &#176;C, respectivamente. Os limites de detecção (3&#963;) para as determinações diretas em cimento Portland foram 0,011 &#181;g g-1 para Cd, 0,28 &#181;g g-1 para Pb, 0,25 &#181;g g-1 para Cu, 0,24 &#181;g g-1 para Ni, 0,11 &#181;g g-1 para Co, 1,1 &#181;g g-1 para Cr e 1,97 &#181;g g-1 para Mn. As concentrações características foram 0,0098 &#181;g g-1 para Cd, 0,21 &#181;g g-1 para Pb, 0,17 &#181;g g-1 para Cu, 0,24 &#181;g g-1 para Ni, 0,068 &#181;g g-1 para Co, 0,62 &#181;g g-1 para Cr e 0,14 &#181;g g-1 para Mn. As exatidões dos métodos foram avaliadas a partir da análise de materiais de referência de cimento Protland (NIST 1886a e 1889a) e de sedimentos marinhos (NBCC MESS-1 e NBCC BCSS-1). Todos os resultados concordaram a um nível de 95% de confiança, quando aplicado o teste t-Student. / The objective of this work was the development of analytical methods for the determination of Cd, Pb, Cu, Ni, Co, Cr e Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry. It was not necessary any pretreatment of the samples, because the particles size (12 &#181;m) were apropriated for direct solid analysis. The heating programs were optimized by thermal evaluation of each element (pyrolysis and atomization curves), using chemical and matrix modifiers and comparison of the calibration curves obtained in presence of aqueous solutions and solid samples. All determinations of the elements were performed against aqueous calibration curves. Due to the high concentration in the samples, for Cu, Ni, Co, Cr e Mn determinations were necessary 3-field Zeeman background correction, improving the representativity. Using this condition, it was possible weight aliquots of samples up to 200 &#181;g. The best condition for Cd and Pb determinations was 5 &#181;g of Pd in 0.1% m v-1 de Triton X-100 as chemical modifier. The pyrolysis and atomization temperatures were 600&#176;C and 2000&#176;C for Cd and 900&#176;C and 2100&#176;C for Pb, respectively. The determinations of Cu e Ni were possible without chemical modifier. The pyrolysis and atomization temperatures were 1200&#176;C and 2600&#176;C, respectively, for both elements. For the determinations of Co, Cr e Mn were used a matrix modifier (Na2CO3 + ZnO) for the in situ fusion, during the heating program. In this condition, the pyrolysis and atomization temperatures were 1400&#176;C and 2600&#176;C, respectively, for all elements. The detection limits (3&#963;) for the direct determination of Portland cement were 0.011 &#181;g g-1 for Cd, 0.28 &#181;g g-1 for Pb, 0.25 &#181;g g-1 for Cu, 0.24 &#181;g g-1 for Ni, 0.11 &#181;g g-1 for Co, 1.1 &#181;g g-1 for Cr and 1.97 &#181;g g-1 for Mn. The characteristic concentrations were 0.0098 &#181;g g-1 for Cd, 0.21 &#181;g g-1 for Pb, 0.17 &#181;g g-1 for Cu, 0.24 &#181;g g-1 for Ni, 0.068 &#181;g g-1 for Co, 0.62 &#181;g g-1 for Cr and 0,14 &#181;g g-1 for Mn. The accuracy of the methods was evaluated by reference materials of Portland cement (NIST 1886a and 1889a) and marine sediments (NBCC MESS-1 and NBCC BCSS-1) analysis. All results are in good agreement with the recommended concentration at 95 % (t-Student test) as confidence level.
18

Avaliação de indicadores biológicos de exposição para As, Be, Cd, Hg, Ni, e Pb em trabalhadores de incineradores de resíduos de serviços de saúde / Evaluation of biological indicators of expousure for As, Be, Cd, Hg, Ni and Pb in workers of medical wastes incineration

Thelma Pavesi 28 August 2006 (has links)
Este trabalho avalia indicadores biológicos de exposição ocupacional de trabalhadores de incineradores de resíduos de serviços de saúde. Os elementos estudados são arsênio, berílio, cádmio, mercúrio, níquel (amostras de urina) e chumbo (amostras de sangue). Os índices obtidos são comparados com (a) os limites estabelecidos pela legislação brasileira, (b) os limites estabelecidos pela American Conference of Governmental Industrial Hygienists (ACGIH) e (c) com os mesmos índices medidos em outros trabalhadores das mesmas usinas trabalhando em diferentes áreas, funções e turnos. As determinações foram realizadas por espectrometria de absorção atômica: por forno de grafite para berílio, cádmio, níquel e chumbo; através da geração de hidreto para arsênio; por geração de vapor frio para mercúrio. Os métodos foram otimizados e validados através de material certificado e ensaios de recuperação. As amostras foram coletadas em 5 dias consecutivos, antes e após cada jornada de trabalho. As médias de concentração para os indicadores biológicos foram inferiores aos limites para exposição ocupacional para os agentes estudados. No caso do arsênio, entretanto, alguns indivíduos apresentaram valores de concentração acima do estabelecido pela legislação brasileira. / The biological occupational exposure indices of workers in medical waste incineration plants is evaluated. Arsenic, beryllium, cadmium, mercury and nickel (urine samples) and lead (blood samples) are studied. The measured indices are compared with (a) the limits imposed by Brazilian law, (b) limits established by American Conference of Industrial Governmental Hygienists and (c) the same indices measured for co-workers in different workplaces, activities and workshifts. The measurements have been carried through atomic absorption spectrometry: by graphite furnace for of beryllium, cadmium, nickel and lead; using the hidride generation for arsenic; and by cold vapor generation for Hg. The employed methods have been optimized and validated through certified samples and recovery essays. The samples were collected in 5 consecutive workdays, before and after each working shift. The measured indices are found to be below their respective occupational exposure limits when the average for each group of workers is taken. In the case of the arsenic, however, some individual workers have shown levels above the limits imposed by Brazilian law.
19

\"Avaliação da espectrometria de absorção atômica com atomização eletrotérmica em filamento de tungstênio para determinação de alumínio\" / \"Evaluation of tungsten coil electrothermal atomic absorption spectrometry for aluminium determination\"

Quienly Godoi 27 October 2006 (has links)
Este trabalho teve como objetivo avaliar o filamento de tungstênio de 150 W (OSRAM) como atomizador eletrotérmico para determinação de alumínio em amostras de águas, incluindo um estudo sistemático sobre o seu comportamento eletrotérmico na presença de até 1000 mg l-1 de sódio, potássio, cálcio, magnésio e/ou da mistura destes elementos. Alguns parâmetros, como comprimento de onda, corrente da lâmpada de catodo oco, altura de observação e temperatura de atomização do alumínio foram avaliados visando à melhoria da qualidade dos resultados e do limite de detecção. Após uma primeira avaliação, fixaram-se o comprimento de onda em 309,3 nm e a corrente da lâmpada de catodo oco em 10 mA, elegendo-se altura de observação de 1,5 mm e temperatura de atomização de 2860 oC (13,0 V). No programa de aquecimento usado no desenvolvimento deste trabalho adotou-se rampa invertida de voltagem variando entre 0,65 a 0,30 V durante 50 s para secagem de 10 µl, 2,8 V durante 10 s para pirólise e 13,0 V durante 1 s para atomização. As soluções usadas no desenvolvimento deste trabalho formam preparadas, em sua maioria, em meio 0,1 % v/v HNO3. A avaliação dos potenciais interferentes Na, K, Ca, Mg e a mistura desses elementos foi realizada nas alturas de observação de 0,0 a 2,0 mm e nas composições do gás de proteção de 90% Ar/10% H2, 80% Ar/20% H2, 65% Ar/35% H2. Pode-se inferir que o aumento do hidrogênio na composição do gás de proteção não acarretou melhora significativa na ação dos interferentes na atomização do alumínio. Não foram observadas interferências significativas em até 1000 mg l-1 Na e K na atomização de 100 µg l-1 Al na altura de observação de 0,0 mm. Na mesma condição de altura de observação, a mistura dos interferentes não afetou significativamente a atomização do alumínio. Observaram-se interferências em torno de 40 % na atomização de 100 µg l-1 Al em 0,1 % v/v HNO3 na altura de observação de 0,0 mm na presença de até 100 mg l-1 de Ca e Mg. Nessa mesma condição, mas com a mistura 65 % Ar/35 % H2, a supressão do sinal de absorbância de alumínio foi da ordem 90%. Os resultados obtidos na determinação de alumínio em amostras de água foram obtidos nas condições anteriormente citadas, utilizando gás de proteção 90% Ar/ 10% H2. Nestas condições, o limite de detecção foi de 2,3 µg l-1 Al e a massa característica de 69 pg Al. Os resultados encontrados foram satisfatórios e concordantes com aqueles encontrados quando se utilizou o forno de grafite como método de comparação. Aproximadamente 500 queimas foram feitas com um único filamento de tungstênio. / The aim of this paper was to evaluate the 150 W (OSRAM) tungsten coil as electrothermal atomizer in order to determine aluminum in water samples as well as a systematic study of its electrothermal behavior in the presence of up to 1000 mg l-1 of sodium, potassium, calcium, magnesium and/or of mixture of these elements. Some parameters, such as wavelength, hollow cathode lamp current, observation height and atomization temperature were evaluated in order to improve the quality of results and the detection limit. After a first evaluation, measurements were always carried out at 309,3 nm as well as the hollow cathode lamp current at 10 mA, and it was adopted an observation height of 1,5 mm and atomization temperature at 2860 oC (13,0 V). In the heating program defined experimentally, the inverted voltage ramp was adopted for drying 10 &#956;l of sample solution by varying the applied voltage from 0,65 to 0,30 V during 50 s, with further application of 2,8 V for 10 s in the pyrolysis step and 13,0 V for 1 s in the atomization step. Most solutions were prepared in 0,1% v/v HNO3. The evaluation of the potential interfering elements such as Na, K, Ca, Mg an the mixture of these elements, was carried out in observations heights from 0,0 to 2,0 mm at different gas compositions: 90% Ar/ 10% H2 , 80 % Ar/ 20% H2 and 65 % Ar/ 35% H2. It can be inferred that the hydrogen increase in the protection gas did not change the interference behavior of the studied concomitants on aluminum atomization. Significant interferences were not observed up to 1000 mg l-1 of Na and K in the atomization of 100 &#956;g l-1 Al when the optical beam was intercepting the atomizer (0,0 mm observation height). In the same condition, the mixture of the interfering species did not significantly affect the aluminum atomization. In addition, 100 mg l-1 of Ca and Mg depressed the absorbance of 100 &#956;g l-1 Al in 0,1 % v/v HNO3 by approximately 40 %. When the atomization was made in the presence of 65 % Ar/ 35 % H2, the suppression of the aluminum absorbance signal was about 90 %. The results obtained in the determination of aluminum in water samples were achieved in the conditions previously mentioned, using protection gas of 90 % / 10 % H. In these conditions, the detection limit was 2,3 &#956;g l-1 Al and the characteristic mass was 69 pg Al. The results were reasonable and in agreement with those found by atomic absorption with graphite furnace as a comparative method. Approximately 500 firings were made with a single tungsten coil.
20

Estudo da influência de processos de conservação na distribuição de espécies elementares em água de coco por espectrometria de absorção e emissão atômica / Study of influence of conservation processes in the distribution of elemental species in coconut water by atomic absorption spectrometry and optical emission spectrometry

Juliana Naozuka 23 July 2004 (has links)
A água de coco é um isotônico natural, uma bebida pouco calórica e muito nutritiva, representando 1,4 % do mercado de refrigerantes e de isotônicos artificiais. Aliado ao crescente mercado interno e externo, surge os processos de conservação com o intuito de preservação da água de coco fora do fruto, facilitando a comercialização e aumentando o tempo de vida de prateleira. Considerando o pressuposto, esse trabalho teve como objetivo principal avaliar a influência dos processos de conservação, ultrafiltração, congelamento e pasteurização, na concentração de Al, Ca, Cu, Fe, K, Mg, Mn, Na, Se e Zn em água de coco. As determinações foram feitas por espectrometria de emissão óptica com plasma indutivamente acoplado e espectrometria de absorção atômica com atomização eletrotérmica. Investigação no sentido de determinar espécies livres de Se4+ e Se6+, em água de coco, por geração de hidretos e pré-concentração na superfície de um tubo de grafite modificada com Ir também foi objetivo desse trabalho. Os estudos foram realizados por meio das determinações das concentrações totais dos elementos e em diferentes frações (filtrado e resíduo), obtidas após ultrafiltração com membrana de celulose (0,100 e 0,025 &#181;m). Em todos os processos de conservação estudados, exceto na ultrafiltração, as concentrações totais dos elementos de interesse foram preservadas. A ultrafiltração com filtro de 0,025 &#956;m promoveu a retenção de uma quantidade significativa de Fe (30%) e Zn (50 %). A influência dos processos de conservação, com base na distribuição dos elementos de interesse, mostrou uma tendência de variação na distribuição de Cu, Fe e Zn na água de coco pasteurizada e em todos os elementos na congelada, sobretudo para aquelas com tempo de congelamento superior a 30 dias. A especiação de Se6+ e Se4+ foi feita após redução do Se6+ com 2,0 mol L-1 HCl + 1 mol L-1 KBr e aquecimento por microondas focalizadas em microfrascos, apresentando cerca de 95 % de eficiência na redução na ausência da amostra de água de coco. / The coconut water is a natural isotonic, nutritive and low caloric drink, corresponding to 1.4 % of the soft drink and artificial isotonic market store. The conservation processes of the coconut water appear in association to the expansion of the internal and external market, increasing the shelf-life of the product and its comercialization. The objective of this work was evaluate the influence of the conservation processes, such as, ultrafiltration, freezing and pasteurization based on the concentrations of Al, Ca, Cu, Fe, K, Mg, Mn, Na, Se and Zn in the coconut water. The determinations were done by inductively coupled plasma-optical emission spectrometry and electrothermal atomic absorption spectrometry. The investigation of free-species of Se4+ and Se6+, in coconut water, by hydride generation and pre-concentration on the modified graphite tube surface with Ir was also the aim of this project. The studies were carried out through the determinations of the total concentration of the interest elements and in different fractions (filtrate and residue), obtained after ultrafiltration with cellulose membrane filters (0.100 and 0.025 &#181;m). In all processes of conservation studied, except the ultrafiltration, the total concentrations were preserved. The ultrafiltration with filters of 0.025 &#181;m promoted the retention of significant concentration of Fe (30%) e Zn (50%). Considering the distribuituion of the interest elements, the influence of the conservation processes showed a tendency of the variation in the Cu, Fe and Zn distribuition for the pasteurized coconut water, and for all elements in the frozen, mainly for frozen samples storaged for more than 30 days. The speciation of Se4+ and Se6+ was carried out after reduction of Se6+ with 2 mol L-1 HCl + 1 mol L-1 KBr and using microvials heated in a focused microwave. The reduction efficiency of the Se6+ to Se4+ was 95 %, in absence of coconut water.

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