ISIJ International
Online ISSN : 1347-5460
Print ISSN : 0915-1559
ISSN-L : 0915-1559
Determination of Trace Impurities in Graphite and Silicon Carbide by Total Reflection X-ray Fluorescence Spectrometry after Homogeneous Liquid–Liquid Extraction
Hitoshi YamaguchiShinji ItohShukuro IgarashiKunishige NaitohRyosuke Hasegawa
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2000 Volume 40 Issue 8 Pages 779-782


Using homogeneous liquid–liquid extraction as a pre-concentration method, a determination procedure of trace impurities (Fe, Ni and Cu) by total reflection X-ray fluorescence (TXRF) analysis was developed and optimized for graphite and silicon carbide samples. The samples were decomposed by alkali fusion. The residue was dissolved in a mixture of pentadeca-fluorooctanoic acid (PFOA), acetone and water, and the analytes were homogeneously dispersed by the aid of phenanthroline (phen). After phase separation with pH-adjustment, a portion of the sedimented water-immiscible liquid was pipetted on the polyester film that covered a silicon wafer sample-carrier. Then, the droplet was dried in a vacuum and analyzed by TXRF. Analytical values in the sub-ppm or ppm level were well agreed with the certified values of the standard samples or the values observed by ICP-OES for a few samples.

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