Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

摘要

The use of slurry sampling total reflection X-ray fluorescence spectrometry (S1S-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL~(-1). As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL~(-1) of boron nitride were found suitable and were used for all further measurements. The limits of detection of S1S-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g~(-1) for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, S1S-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of S1S-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al2O3, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by S1S-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a concentration range from 2.5 to 1470 μg g~(-1) were found to be 0.995, 0.991 and 0.997, respectively.