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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 22, Number 2
BKCSDE 22(2)
February 20, 2001 

Analysis of Si3N4 Ultra Fine Powder Using High-pressure Acid Digestion and Slurry Injection in Inductively Coupled Plasma Atomic Emission Spectrometry
K. H. Kim, H. Y. Kim, H. B. Lim
Si3N4, Slurry nebulization, Inductively coupled plasma spectrometry, Atomic emission spectrometry, Acid digestion.
Si3N4 powder has been analyzed by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample was dissolved by high-pressure acid digestion with HF, H2SO4 (1+1), and HNO3 mixture. This technique is well suited for the impurity analysis of Si3N4 because the matrix interference is eliminated. A round-robin samples trace elements, such as Ca, W, Co, Al, Fe, Mg, and Na, were determined. For the direct analysis, slurry nebulization of 0.96 mm Si3N4 powder also has been studied by ICP-AES. Emission intensities of Fe were measured as ICP operational conditions were changed. Significant signal difference between slurry particles and aqueous solution was observed in the present experiment. Analytical results of slurry injection and high-pressure acid digestion were compared. For the use of aqueous standard solution for calibration, k-factor was determined to be 1.71 for further application.
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