Method development for the analysis of poorly soluble solids by total reflection X-ray fluorescence spectrometry

• Published in: Spectrochimica acta. Part B: Atomic spectroscopy 2018-11, Vol.149, p.276-280
• Main Authors: Takahara, Hikari, Ohbuchi, Atsushi, Murai, Kensuke
• Format: Article
• Language: English
• Subjects: Correlation; Correlation coefficients; Dispersion; Electron spin; Fluorescence; Manganese; Matrix; Matrix effect; Methods; Physical characteristics; Physical properties; Polymer films; Polymers; Powder; Reference materials; Reflection; Sample shape effect; Scanning electron microscopy; Scattered radiation internal standard method; Scientific imaging; Silicon; Silicon nitride; Silicon substrates; Spectrometry; Spin coating; Suspension; Trace element analysis; Trace elements; X ray fluorescence analysis; X ray reflection; X-ray fluorescence
• ISSN: 0584-8547; 1873-3565
• DOI: 10.1016/j.sab.2018.07.008

Non-dissolution preparation method was developed for powder sample analysis by total reflection X-ray fluoresce spectrometry (TXRF). The certified reference materials (CRMs) of silicon nitride powder were suspended in polymer solution and the suspension was spin-coated on substrate. The fine silicon nitride particles dispersed on a few tens of nm thin polymer film were observed by surface profiler and scanning electron microscope (SEM) observation. For spin-coated specimens, TXRF results show not good correlation between the X-ray intensities and standard values for impurity components Cr, Mn, and Fe in silicon nitride powder CRMs. However, taking background ratio can effectively improve the correlation factor by correcting matrix effect and physical characteristics such as surface condition, grain size, and irregular sample shape. [Display omitted] •Silicon nitride powders suspended in polymer solution were spin-coated on substrate.•Correlation of net intensities to certified values for impurity elements is not good.•The background intensity ratio effectively improved the correlation coefficient.•Scattered radiation internal standard method corrects matrix effect and sample shape effect.