Determination of Boron in Silicon Carbide by ICP-OES and ICP-MS after Sample Preparation using Pyrohydrolysis

Cristiano C Muller,Thieli S Nunes,Valderi L Dressler,Edson I Muller,Erico M M Flores,Aline L H Muller

doi:10.5935/0103-5053.20140222

Abstract

Pyrohydrolysis was used for sample preparation of silicon carbide (SiC) and subsequent determination of B using inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Important parameters for pyrohydrolysis method as temperature, air and water flow rates, reaction time and use of V2O5 were evaluated. In addition, a study of W spectral interference on B emission lines was evaluated for ICP-OES determination. Accuracy was evaluated using certified reference material (CRM BAM S003) and bias value lower than 1% between the certified and determined value was achieved. Limit of detection (LOD) of 0.010 μg g−1 was obtained using pyrohydrolysis and ICP-MS. Pyrohydrolysis is a very simple sample preparation method that allowed the use of deionized water as absorbing solution for B determination in SiC.

Highlights

Silicon carbide (SiC) is an advanced ceramic material used in the semiconductor industry
Isobaric or polyatomic interferences were not observed in 11B determination by inductively coupled plasma mass spectrometry (ICP-MS) and this isotope was used for the analysis of SiC wet digestion solutions
SiC I and SiC II samples showed the highest values for B, while sample SiC III e Si IV had B levels lower than the limit of detection obtained by ICP-MS

Summary

Introduction

Silicon carbide (SiC) is an advanced ceramic material used in the semiconductor industry. Volatilization of B compounds during pyrohydrolysis is probably explained by the formation of gaseous HBO2 or H3BO3.30 Sometimes, the use of auxiliary reagents (such as, V2O5) is required in order to assure the complete recovery of analytes during the pyrohydrolysis procedure.[41] In this work, a pyrohydrolysis method was proposed for high purity SiC powder digestion and further B determination by ICP-OES and ICP-MS Important pyrohydrolysis parameters, such as, air and water flow rates, temperature, reaction time, sample mass and use of catalyst were evaluated. Boron determination was carried out in this solution without dilution

Pyrohydrolysis procedure

Results and Discussion

Evaluation of reaction time

Conclusions

Method