Microwave assisted volatilization of silicon as fluoride for the trace impurity determination in silicon nitride by dynamic reaction cell inductively coupled plasma-mass spectrometry

摘要

A low pressure microwave assisted vapor phase dissolution procedure for silicon nitride and volatilization of in situ generated SiF4 has been developed using H2SO4,HF and HNO3 for the determination of trace impurities present in silicon nitride.Sample was taken in minimum amount (0.5 mL for 100 mg) of.H2SO4 and treated with vapors generated from HF and HNO3 mixture in presence of microwaves in a closed container.An 80 psi pressure with ramp and hold times of 30min and 60min respectively,operated twice,resulted in 99.9% volatilization of Si.Matrix free solutions were analyzed for impurities using DRC-ICP-MS.The recoveries of Cr,Mn,Fe,Ni,Co,Cu,Zn,Sr,Y,Cd,Ba and Pb were between 80 and 100% after volatilization of Si.The blanks were in lower ng g~(-1) with method detection limits in lower ng g~(-1) to sub ng g~(-1) range.The method was applied for the analysis of two silicon nitride samples.