Reference concentrations for trace elements in urine for the Brazilian population based on q-ICP-MS with a simple dilute-and-shoot procedure

Biomonitoring of trace elements is of critical importance in human health assessment. However, trace element concentrations in biological fluids are affected by environmental and physiological parameters, and therefore considerable variations can occur between specific population subgroups. Brazil is a large country with large environmental diversity and with a limited knowledge of the reference values (baseline data) for trace elements in biological fluids. Atomic absorption spectrometry (AAS) and inductively coupled plasma emission spectrometry (ICP-OES) are still the dominant analytical techniques used for biomonitoring trace element analysis in clinical specimens. However, the use of ICP-MS is becoming more usual in clinical laboratory analysis. Then, we evaluated here a simple dilute-and-shoot method for sequential determination of Al, Ba, Be, Cd, Co, Cu, Cs, Mn, Ni, Pb, Pt, Sb, Se, Sn, Tl and U in urine by quadrupole inductively coupled plasma mass spectrometry (q-ICP-MS). Urine samples (500 µL) were accurately pipetted into conical tubes (15 mL) and diluted to 10 mL with a solution containing 0.5 % (v/v) HNO3 + 0.005% (v/v) Triton X-100. Diluted urine samples also contain rhodium, iridium and yttrium added as internal standards. After that, samples were directly analyzed by ICP-MS against matrix-matching calibration. Method detection limit (3s, n = 20) were in the ng L-1 range for all analytes. The method was applied to the analysis of 412 ordinary urine samples from Brazilian healthy and non-exposed subjects to establish reference values. Data validation was provided by the analysis of the standard reference material (SRM) 2670a toxic elements in urine (freeze-dried) (high and low levels) from the National Institute of Standards and Technology (NIST) and reference urine samples from the trace elements intercomparison program operated by the Institut National de Sante' Publique du Quebec, Canada.O biomonitoramento de elementos químicos é de extrema importância na avaliação da saúde humana. Entretanto, as concentrações dos elementos químicos nos fluidos biológicos são afetadas por parâmetros ambientais e fisiológicos e, consequentemente, consideráveis variações podem ocorrer entre subgrupos de populações específicas. O Brasil é um país com ampla diversidade ambiental e existe limitado conhecimento de valores de referência para elementos químicos em fluidos biológicos. A espectrometria de absorção atômica (AAS) e a espectrometria de emissão ótica com plasma acoplado indutivamente (ICP-OES) ainda são as técnicas analíticas mais comumente empregadas no biomonitoramento de elementos químicos em amostras clínicas. Entretanto, o uso da espectrometria de massas com plasma acoplado indutivamente (ICP-MS) está se tornando a cada dia mais comum nos laboratórios clínicos. Neste estudo, foi avaliado um método rápido envolvendo simples diluição da amostra para determinação de Al, Ba, Be, Cd, Co, Cu, Cs, Mn, Ni, Pb, Pt, Sb, Se, Sn, Tl e U em urina por ICP-MS. Amostras de urina (500 μL) foram pipetadas em frascos cônicos de 15 mL e diluídas para 10 mL com uma solução contendo 0,5 % (v/v) HNO3 + 0,005% (v/v) Triton X-100. Ródio, irídio e ítrio foram adicionados como padrões internos. Em seguida, as amostras foram diretamente analisadas por ICP-MS com calibração por ajuste de matriz. Os limites de detecção do método (3s, n = 20) foram da ordem de ng L-1 para todos os analitos em estudo. O método foi aplicado para a análise de 412 amostras de urina de brasileiros saudáveis e não expostos ambientalmente ou ocupacionalmente a metais para o estabelecimento de valores de referência na população brasileira. A validação dos resultados foi acompanhada pela análise de material de referência certificada de urina (SRM) 2670a proveniente do National Institute of Standards and Technology (NIST) e de materiais de referência provenientes do Institut National de Sante' Publique Du Quebec, no Canadá.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Plasma processing of closed nuclear fuel cycle waste

В работе предложен плазменный метод переработки отходов замкнутого ядерного топливного цикла в виде водно-солеорганической композиции. Этот метод имеет несколько преимуществ и позволяет безопасно перерабатывать такой материал. Определен оптимальный состав для утилизации данного отхода в плазме. Равновесные составы показали, что в процессе плазменной обработки образуются N[2], CO[2], H[2]O, а также FeCl[3] и Fe[2]O[3 в конденсированной фазе. Отсутствие сажи является показателем того, что процесс переработки является экологически безопасным.The work proposed the plasma method of processing closed nuclear fuel cycle wastes in the form of a water-salt-organic composition. This method has several advantages and allows recycling such material safely. The optimal composition for recycling in plasma was determined. Equilibrium compositions showed that in the process of plasma processing N[2], CO[2], H[2]O and also FeCl[3] и Fe[2]O[3] in the condensed phase were formed. Lack of soot is an indicator that the recycling process is environmentally safe

A study of the ultrasonic treatment effect on microstructure and mechanical properties of commercial purity titanium

This work presents a study of the ultrasonic treatment effect on microstructure and mechanical properties of ac-received and recrystallized commercial purity titanium specimens by means XRD, EBSD and TEM. It was demonstrated that the dislocation density growth and the twins with special boundaries [sigma]7b and [sigma]11b increase within the surface grains during ultrasonic treatment depend on initial structural state of the titanium specimens. The relationship between the structural parametrs change and the surface layer microhardness value of the titanium specimens subjected to ultrasonic treatment was shown. It was found that differences in the hardened surface layer depth and the surface microhardness of ac-received and recrystallized titanium specimens result in the same yield and ultimate tensile strength increment during ultrasonic treatment

LiCaFeF6 A zero strain cathode material for use in Li ion batteries

A new zero strain LiCaFeF6 cathode material for reversible insertion and extraction of lithium ions is presented. LiCaFeF6 is synthesized by a solid state reaction and processed to a conductive electrode composite via high energy ball milling. In the first cycle, a discharge capacity of 112 mAh g amp; 8315; is achieved in the voltage range from 2.0 V to 4.5 V. The electrochemically active redox couple is Fe3 amp; 8314; Fe2 amp; 8314; as confirmed by Mössbauer spectroscopy and X ray absorption spectroscopy. The compound has a trigonal colquiriite type crystal structure space group . By means of in situ and ex situ XRD as well as X ray absorption fine structure spectroscopy a reversible response to Li uptake release is found. For an uptake of 0.8 mol Li per formula unit only minimal changes occur in the lattice parameters causing a total change in unit cell volume of less than 0.5 . The spatial distribution of cations in the crystal structure as well as the linkage between their corresponding fluorine octahedra is responsible for this very small structural response. With its zero strain behaviour this material is expected to exhibit only negligible mechanical degradation. It may be used as a cathode material in future lithium ion batteries with strongly improved safety and cycle lif

Синтез новых ацильных производных бетулина

В рамках бакалаврской работы проводились новые химические превращения объекта исследования – бетулина – действием оксикарбоновой (молочной) кислоты.As part of the bachelor's work, new chemical transformations of the object of study — betulin — were performed by the action of hydroxycarboxylic (lactic) aci