An analytical method for multi-elementary determination in powder refreshment, based on sample digestion using dilute mineral acids and detection by inductively plasma coupled optical emission spectrometry (ICP OES) is proposed. Chemometric tools, such as fractional factorial design and principal component analysis (PCA) and hierarchical cluster analysis (HCA) were applied to optimize the sample preparation conditions in closed block digester, and Doehlert design for spectrometer operation. Addition and recovery tests and analyses of certified reference material were performed to evaluate the precision and accuracy, and the results confirm the reliability of the proposed method. Limits of quantification (LOQ) between 0.02 and 36 µg g−1 were obtained. The analytical method was applied for determination of 24 inorganic constituents in 20 powder refreshment samples. Calcium, K, Mg, Na, P, S and Ti presented the highest concentrations. The analytical method was adequate for the determinations of inorganic constituents in powder refreshment samples by ICP OES.

In this work, an analytical method for determination of Ba, Cu, Ni, V, and Zn, in medicinal herbs, through direct solid sample analysis by energy dispersive X-ray fluorescence spectrometry (EDXRF), was applied. Accuracy and precision (intra and inter day) of the analytical method were confirmed through analysis of certified reference material, tomato leaves (CRM NIST 1573a). Principal component analysis (PCA) and hierarchical cluster analysis (HCA) allowed to observe the formation of two groups. Group I was composed by highest levels of Cu and Zn, and the group II with highest concentrations of Ba, V, and Zn. Group I also was subdivided into two subgroups. The concentration of Ni in some samples exceeded the maximum allowed limit. In all samples, Cu and Zn concentration were below the maximum limit allowed by Brazilian legislation. However, for Ba and V, the evaluation was not possible, because there are no maximum limits in legislation.

Cat and dog feed production has increased worldwide, and much emphasis has been placed on the importance of determining the mineral composition of pet foods. In this work, the concentrations of Al, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Ni, P, Sr, V and Zn in dry feed for cats and dogs employing inductively coupled plasma-optical emission spectrometry (ICP OES) were determined and evaluated according to regulatory agencies. Forty-one dry feed samples (24 dog feed and 17 cat feed) were analyzed. The obtained concentrations ranged from 2.3 mg kg-1 (Ba) to 2.8 g kg-1 (Ca) in cat feeds, and from 3.8 mg kg-1 (Cu) to 3.4 g kg-1 (Ca) in dog feeds. The concentrations of P are in accordance with the Brazilian legislation, and Mn and Zn contents met the American legislation. The concentration values of Cu, K and Mg presented in some samples were below the limits established by American regulatory agency. Based on multivariate data analysis evaluated from flavors of the products and brands, it was concluded that the feed samples were uniform since there was no trend to group formation and classification according to their mineral composition, except one dog feed brand, which had a significant content of Al and Cu.

The simultaneous determination of thorium and uranium in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES) was optimized. The three-level factorial design was applied to optimize the operating conditions of radiofrequency power and nebulizer gas flow rate. The analytical method was specific and selective for both elements.

A cloud-point extraction (CPE) method using the surfactant (30)p-tert-octylphenol polyoxyethylene (OPEO30) was proposed as the preceding step for the determination of polycyclic aromatic hydrocarbons (PAHs) by gas chromatography-mass spectrometry (GC-MS). Given the need for surfactant derivatization before the chromatographic analysis, the reaction conditions of coacervate derivatization were studied. The extraction process was also optimized, where surfactant concentration, temperature and time were analyzed as variables. The limits of detection obtained were between 0.02 and 0.05 µg L-1, and the recoveries of analytes were between 70 and 98%, with coefficient of variation better than 10.3%. The analytical method developed provides an efficient, precise and accurate method for the determination of the 16 priority PAHs, generating results in accordance with the USEPA 3510C method. The method was applied to the analysis of groundwater samples collected from artesian wells located at retail fuel stations.

Um método para determinação sequencial de Cu e Fe em material particulado atmosférico (APM) coletado em filtro de fibra de vidro por amostragem em suspensão e espectrometria de absorção atômica com chama é proposto. A otimização do método foi realizada utilizando-se uma massa de amostra seca em pó (filtro + APM) de 50 mg, dispersa em solução de ácido nítrico 0,5 mol L-1 e tratada por 10 min em banho ultrassônico. Os limites de detecção (n = 10) foram 4 e 14 µg g-1 para Cu e Fe no filtro, respectivamente. A repetitividade expressa como desvio padrão relativo foi melhor do que 7 e 8% (n = 3) para Cu e Fe, respectivamente. A exatidão do método foi confirmada analisando-se material de referência certificado de cinzas atmosféricas (BCR 176R). Os resultados obtidos para seis amostras de APM utilizando o método proposto não apresentaram diferenças significativas em comparação com os valores obtidos usando o método de extração ácida e determinação por espectrometria de massas com plasma indutivamente acoplado. O método analítico mostrou-se simples, rápido e confiável.

A slurry sampling flame atomic absorption spectrometric method for sequential determination of Cu and Fe in airborne particulate matter (APM) collected on glass fiber filters is proposed. The method optimization was carried out using a dry powdered sample (filter + APM) mass of 50 mg, dispersed in 0.5 mol L-1 nitric acid solution and under ultrasonic bath for 10 min. The limits of detection (n = 10) were 4 and 14 µg g-1 for Cu and Fe on the filter, respectively. The repeatability expressed as the relative standard deviation was better than 7 and 8% (n = 3) for Cu and Fe, respectively. The accuracy of the method was confirmed by analysis of the fly ash certified reference material (BCR 176R). The results obtained for six samples of APM using the proposed method showed no significant differences with those obtained after microwave-assisted acid extraction and determination by inductively coupled plasma mass spectrometry. The analytical method proved to be simple, fast and reliable.

As distribuições de Co, Cr, Cu, Mn, Ni, Pb, Fe e Al foram investigadas em sedimentos superficiais coletados em 19 sítios da Bacia Hidrográfica do Rio Sergipe, Nordeste do Brasil. Foi definida uma base geoquímica para a região (RGB) usando o ferro como elemento de referência. Fatores de enriquecimento (EF) e índice de geoacumulação (Igeo) foram empregados para determinar a contribuição por origem antropogênica. Valores de EF mostraram que os sedimentos dos sítios 1, 5 e 13 podem ser considerados contaminados por Pb, Cr e Cu, respectivamente. Valores de Igeo mostraram que o sítio 13 pode ser considerado contaminado. Há uma grande predominância nos sedimentos de metais de origem natural. A possível toxicidade foi avaliada comparando com os valores PEC-TEC dos guias de qualidade de sedimentos (SQG). Análise de componentes principais (PCA) separou claramente os pontos em dois grupos e a análise de agrupamento hierárquico (HCA) confirmou as interpretações feitas pela PCA.

The distributions of Co, Cr, Cu, Mn, Ni, Pb, Fe and Al were investigated in surface sediments collected at 19 sites in the Sergipe River Hydrographic Basin of Northeast Brazil. A regional geochemical baseline (RGB) was defined using iron as a reference element. Enrichment factors (EF) and geoaccumulation indices (Igeo) were used to determine the extent of anthropogenic metal pollution. EF values showed that sediments from sites 1, 5 and 13 could be considered contaminated by Pb, Cr and Cu, respectively. Igeo values showed that only site 13 could be considered contaminated. For other sites, results indicated that naturally occurring metals predominated in the sediments. Possible toxicity related to these metals was examined using the comparing sediment chemical data with sediment quality guidelines (SQG) PEC-TEC values. Principal component analysis (PCA) clearly separated the sites into two groups and hierarchical cluster analysis (HCA) confirmed the interpretations made from the PCA results.

Neste trabalho, foi avaliada a composição mineral da farinha de trigo consumida no Brasil. Na etapa de amostragem foram coletadas 54 amostras em 15 cidades, incluindo as principais cidades brasileiras como: São Paulo, Rio de Janeiro, Salvador, Porto Alegre, Recife e outras. Os elementos determinados foram: cálcio, cobre, magnésio, manganês, ferro, fósforo, potássio e zinco. As amostras foram digeridas usando acido nítrico e peróxido de hidrogênio em sistema aberto. A técnica analítica empregada foi a espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). A validação do método (incluindo digestão e determinação) foi confirmada usando um material de referência certificado de farinha de trigo fornecido pelo National Institute of Standards & Technology (NIST). Considerando as 54 amostras analisadas, os resultados demonstraram que os macronutrientes: cálcio, magnésio, potássio e fósforo encontram-se em média de 0,27; 0,35; 1,71 e 1,92 mg g-1, com variação da concentração de 0,11-1,96; 0,19-0,51; 0,76-3,16 e 0,81-7,15 mg g-1, respectivamente. Os micronutrientes: cobre, ferro, manganês e zinco encontram-se em média de 1,84; 37,82; 8,25 e 9,41 µg g-1, com a variação de concentração de 1,00-2,80; 10,46-146,58; 3,89-14,74 e 5,07-13,93 µg g-1, respectivamente. Os resultados foram também avaliados usando as técnicas de análise multivariadas: análise de componente principal (PCA) e análise de agrupamento hierárquico (HCA).

In the present paper, the mineral composition of wheat flour consumed in Brazil was evaluated. In the sampling step 54 samples were collected in 15 cities, including principal Brazilian cities such as: São Paulo, Rio de Janeiro, Salvador, Porto Alegre, Recife and others. The elements determinate were: calcium, copper, magnesium, manganese, iron, phosphorus, potassium and zinc. The samples were digested using nitric acid and hydrogen peroxide in open system. The analytical technique employed was Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES). The method validation (including digestion and determination) was performed using a certified reference material of wheat flour furnished by National Institute of Standards & Technology (NIST). Considering the 54 samples analyzed, the results demonstrated that the macronutrients: calcium, magnesium, potassium and phosphorus have average contents of 0.27, 0.35, 1.71 and 1.92 mg g-1, for concentration ranges of 0.11-1.96, 0.19-0.51, 0.76-3.16 and 0.81-7.15 mg g-1, respectively. The micronutrients: copper, iron, manganese and zinc have average contents of 1.84, 37.8, 8.2 and 9.4 µg g-1, for concentration ranges of 1.00-2.80, 10.5-146.6, 3.9-14.7 and 5.1-13.9 µg g-1, respectively. The results were also evaluated using the multivariate analysis techniques: principal component analysis (PCA) and hierarchical cluster analysis (HCA).