The present work aims the determination of As, Co, Cr, Cu, Mn and Pb in seawater samples using coprecipitation extraction procedure before standard mode inductively coupled plasma mass spectrometry (ICP-MS) (no collision/reaction cell). The coprecipitation procedure is based on the precipitation of Mg(OH)2 from the reaction of the Mg2+ ions (present into the seawater) with ammonia added to the sample. Central composite design, desirability function, and response surface methodology were used to optimize the coprecipitation procedure. The optimum values obtained were 1200 µL of aqueous ammonia, 30 min of centrifugation time and 400 µL of nitric acid. The procedure obtained showed low limits of detection since good preconcentration factors were obtained. Good accuracy was also obtained when the reference material Trace Metals 1 in seawater was evaluated. Thus, the proposed procedure can be considered a good strategy for the determination of As, Co, Cr, Cu, Mn and Pb in seawater by ICP-MS, due to its simplicity, low cost, high analytical frequency, besides the good sensitivity and accuracy achieved.

Determining inorganic constituents in illicit drugs can indicate its purity and presence of adulterants. In this study, we analyzed 52 street cocaine samples, seized in three different regions of Espírito Santo, state of Brazil. Inductively coupled plasma optical emission spectrometry was used to determine Al, Ca, Cu, Fe, Mn, Mg, Zn concentrations and inductively coupled plasma mass spectrometry to determine Mo, Co, Pb and P concentrations. From analyte recovery tests, the accuracy was considered acceptable and the proposed method satisfactory. Most of the samples exhibited a relatively homogeneous inorganic profile with similar concentrations of investigated elements, however some samples had very discrepant concentrations. High concentrations of Al, Ca, Fe, Mg, Mn, and P were found, indicating that adulterants such as gypsum, marble powder, limestone, cement, and others must be used to increase the profitability of the illicit drug market.

Black pepper is one of the most consumed spices worldwide and the evaluation of trace elements content is essential to promote consumer safety. In this study, concentrations of the elements As, Cd, Co, Cu, Fe, Mn, Mo, Ni, Pb, Se, V and Zn was determined in samples of black peppercorn (n = 25) and ground black pepper (n = 25) to verify how processing affects element concentrations. The elements were determined by inductively coupled plasma mass spectrometry and flame atomic absorption spectrometry. A principal component analysis showed that Fe, Pb and V was influenced by the processing and ground black pepper samples showed higher levels for these elements than black peppercorn. Although specific legislation for spices is not available in Brazil, results indicated that Pb concentrations in two brands of the processed samples under investigation exceeded the maximum level established by Brazilian and European legislation for vegetables and fruits. These results point to the necessity to control the processing of the black pepper, especially the grinding step.

AbstractThe purpose of this study was to evaluate the best operating conditions of ICP OES for the determination of Na, Ca, Mg, Sr and Fe in aqueous extract of crude oil obtained after hot extraction with organic solvents (ASTM D 6470-99 modified). Thus, the full factorial design and central composite design were used to optimize the best conditions for the flow of nebulization gas, the flow of auxiliary gas, and radio frequency power. After optimization of variables, a study to obtain correct classification of the 18 samples of aqueous extract of crude oils (E1 to E18) from three production and refining fields was carried out. Exploratory analysis of these extracts was performed by principal component analysis (PCA), hierarchical cluster analysis (HCA) and linear discriminant analysis (LDA), using the original variables as the concentration of the metals Na, Ca, Mg, Sr and Fe determined by ICP OES.

No presente estudo, três procedimentos de pré-tratamento e determinação de Cr por GF AAS foram desenvolvidos e comparados: diluição da amostra com tolueno, formação de emulsão e amostragem direta do petróleo. Os limites de detecção para os procedimentos desenvolvidos foram 1,9 ng g-1 para a diluição da amostra com tolueno, 2,8 ng g-1 para a formação de emulsão e 0,73 ng g-1 para a amostragem direta. A exatidão dos três procedimentos foi avaliada analisando-se o material NIST1085b e por testes de recuperação. Em todos os procedimentos foram obtidos altos valores de recuperação e boa concordância entre os teores determinados e os teores certificados. No entanto, os resultados indicam que a diluição da amostra com tolueno não é recomendada para amostras com grau API abaixo de 15. Os outros dois procedimentos mostraram o mesmo desempenho para as amostras com diferentes graus API (8-38), mas a amostragem direta apresentou melhor sensibilidade além de minimizar as chances de perdas do analito ou contaminação.

In the present study three pre-treatment procedures were developed and compared following Cr determination by GF AAS: sample dilution with toluene, emulsion formation and direct sampling of crude oil. The limits of detection for the developed procedures were 1.9 ng g-1 for sample dilution with toluene, 2.8 ng g-1 for emulsion formation and 0.73 ng g-1 for direct sampling. The accuracy of the three procedures was assessed by analysis of NIST1085b and recovery tests. High recoveries and good agreement between found and certified values were obtained in all cases. However, results indicate that sample dilution with toluene is not recommended for samples below 15ºAPI. The other two procedures showed the same performance for the samples with different API degrees (8 to 38), but the direct sampling showed better sensitivity besides minimizing the chances of analyte losses or contamination.