Direct analysis of glass powder samples by radio frequency glow discharge atomic emission spectrometry (rf-GD-AES)

A method is described for the elemental analysis of glass powder samples by rf-GD-AES. Glass powder samples were pressed without binder to form sample disks. A brass sample holder was designed to hold the pellet onto the source and provide a good vacuum seal. Sample preparation conditions and particle sizes are shown to influence spectral characteristics and plasma stabilization times. The discharge operating parameters were optimized based on both raw analyte signal intensity (S) and signal-to-background ratio (S/B), the latter was found more useful in terms of sample-to-sample precision and quantification. A NIST Standard Reference Material (SRM 89 Lead-Barium Glass) was used to evaluate the method. The limits of detection for trace components ranged from 1-10 mu g/g for several elements, depending on the concentrations of the analytes in the SRM. Sample-to-sample reproducibilities were better than 10% RSD and linear calibration curves were obtained using either the Si (I) optical emission as an internal standard or the individual analyte's S/B characteristics.