Determination of trace impurities in boron nitride by graphite ftimace atomic absorption spectrometry and electrothermal vaporization inductively coupled plasma optical emission spectrometry using solid sampling

摘要

Two diuestion-free methods for trace analysis of boron nitride based on graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma spectrometry optical emission (ETV-ICP-OES) using direct solid sampling have been developed and applied to the determination of Al, Ca, Cr, Cu, Fe, Mg, Mn, Si, Ti and Zr in four boron nitride materials in concentration intervals of 1-23, 54-735 0.05-21 0.005-1.3, 1.6-112, 4.5-20, 0.03-1.8, 6-46, 38-170 and 0.4-2.3 lig g(-1), respectively. At optimized experimental conditions, with both methods, effective in-situ analyte/matrix separation was achieved and calibration could be performed using calibration curves measured with aqueous standard solutions. In solid sampling GFAAS, before sampling, the platform was covered with graphite powder and, for determination of Si, also the Pd[Mg(NO3)2 modifier was used. In the determination of all analyte elements by solid sampling ETV-ICPOES. Freon R12 was added to argon carrier -as. For solid sampling GFAAS and ETV-ICP-OES, the achievable limits of detection were within 5 (Cu)-130 (Si) ng g(-1) and 8 (Cu)-200 (Si) ng respectively. The results obtained by these two methods for four boron nitride materials of different purity grades are compared each with the other and with those obtained in analysis of digests by ICP-OES. The performance of the two solid sampling methods is compared and discussed. (C) 2007 Elsevier B.V. All rights reserved.