O principal objetivo desse trabalho foi investigar a possibilidade da detecção sub-ppb (10-9 g/g) de elementos químicos presentes em amostras líquidas, analisadas por meio da espectrometria de raios-X, seja por STXRF (Synchrotron Total reflection X-ray Fluorescence), ou PIXE (Particle Induced X-ray Emission). Na ausência de padrões certificados, foram preparados em laboratório padrões líquidos multielementares com concentrações variando de 1 a 20 ppm, posteriormente micropipetados sobre substrato de Lucite, constituindo assim amostras adequadas para análises STXRF. Visando controlar a manipulação volumétrica, foi utilizado como padrão interno ítrio, em função do qual foi determinada a curva de sensibilidade relativa para o método. Após pré-concentração das amostras, estas foram micropipetadas sobre substratos de Lucite, Mylar e Kimfoil e as análises foram realizadas no Laboratório Nacional de Luz Síncontron LNLS, em Campinas, SP e no Laboratório de Análise de Materiais por feixes Iônicos LAMFI, no IFUSP. Os limites de detecção para ambos os métodos foram determinados e comparados. Como esperado, a STXRF apresenta limites de detecção uma ordem de grandeza inferior ao PIXE para elementos com 20

Title in English

Analysis sub-ppb of liquid samples by PIXE and STXRF methods

Keywords in English

Acceleration of particles
nuclear physics

Abstract in English

The main goal of this work was to investigate the feasibility of sub-ppb (10-9 g/g) detection of trace elements in liquid samples analyzed by STXRF (Synchrotron Total reflection X-ray Fluorescence) and by PIXE (Particle Induced X-ray Emission). For STXRF calibration, and due to the absence of certified liquid standards, a set of multielementary liquid standards was prepared in house, with concentrations varying from 1 to 20 ppm in water, and then micro-pipetted on regular 30 mm diameter Lucite discs. Ytrium was used as an internal standard and the relative sensitivity curves were found relative to it. Real water samples for trace element analysis, were first preconcentrated (to a factor of 5) and then micropipetted on Lucite and also on Lylar and Kimfoil thin films. All the STRXF and PIXE analysis were made respectively in the Laboratório Nacional de Luz Síncrotron LNLS , in Campinas, SP, and in the Laboratório de Análise de Materiais por feixes Iônicos LAMFI, USP. As expected, the minimum elementary detection limits for STXRF for elements with 20

 

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Publishing Date

2015-06-17

 

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