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

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...

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Bibliographic Details
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
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Summary: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.
ISSN:0584-8547
1873-3565
DOI:10.1016/j.sab.2018.07.008