4.6 Article

High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

Journal

SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY
Volume 129, Issue -, Pages 42-48

Publisher

PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.sab.2017.01.005

Keywords

Graphite furnace atomic absorption spectrometry; Trace elements; Polymer analysis; Contaminants; Polymers; Solid sampling; Electrothermal atomic absorption spectrometry

Categories

Funding

  1. Conselho Nacional de Desenvolvimento Cientifico e TecnolOgico (CNPq)
  2. Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior (CAPES)
  3. Fundacao de Amparo a Pesquisa do Estado do Rio Grande do Sul (FAPERGS)

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In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10.mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 25, 1.7, 17 and 0.12 ng g(-1) for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration. (C) 2017 Elsevier B.V. All rights reserved.

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