X-ray fluorescence spectrometer

Patent metadata

Field	Value
Publication number	US-10161889-B2
Application number	US-201815901244-A
Country	US
Kind code	B2
Filing date	Feb 21, 2018
Priority date	Aug 28, 2015
Publication date	Dec 25, 2018
Grant date	Dec 25, 2018

Abstract

A quantitative analysis condition setting unit (13) included in a sequential X-ray fluorescence spectrometer according to the present invention: performs qualitative analyses of a plurality of standard samples (14); sets, on the basis of the qualitative analysis results, a peak measurement angle of each measurement line for analytical samples (1) in quantitative analysis conditions; and obtains a single virtual profile by synthesizing peak profiles of the plurality of standard samples (14) subjected to the qualitative analyses and sets, on the basis of the virtual profile and a preset half value width of the peak profile, background measurement angles of each measurement line for the analytical samples (1) in the quantitative analysis conditions.

First claim

What is claimed is:

1. A sequential X-ray fluorescence spectrometer which irradiates a sample with primary X-rays and measures the intensities of generated secondary X-rays, the spectrometer comprising:
a plurality of standard samples to create calibration curves corresponding to analytical samples; and
a quantitative analysis condition setting unit configured to preset, as quantitative analysis conditions, with measurement lines for the analytical samples, a half value width of a peak profile of each measurement line, sample constituting elements and their contents of each standard sample, wherein
the quantitative analysis condition setting unit
performs qualitative analyses of the plurality of standard samples, to obtain, for each of measurement lines identified in each standard sample, a peak angle obtained through peak search, background angles based on the peak angle and the preset half value width of the peak profile, and a net intensity based on a peak intensity at the peak angle and background intensities at the background angles,
sets, for each of the measurement lines, the peak angle of the standard sample at which no interfering line is identified within a predetermined angle range centered on the measurement line and the peak intensity is maximum, as a peak measurement angle of the measurement line for the analytical samples in the quantitative analysis conditions, and
obtains, for each of the measurement lines, a single virtual profile by synthesizing peak profiles of the plurality of standard samples subjected to the qualitative analyses, and sets the background angle on each of a lower angle side and a higher angle side relative to the measurement line, as a background measurement angle of the measurement line for the analytical samples in the quantitative analysis conditions, the background angles being based on the virtual profile and the preset half value width of the peak profile.

2. The X-ray fluorescence spectrometer as claimed in claim 1 , wherein
the quantitative analysis condition setting unit sets, as new background measurement angles of the measurement line for the analytical samples in the quantitative analysis conditions, the background measurement angles by which the background intensity at the peak measurement angle of the measurement line is minimized when, in the virtual profile, the background measurement angles of the measurement line which are set on the lower angle side and the higher angle side relative to the measurement line are alternately brought closer to the measurement line within a predetermined angle range, at a predetermined angle step.

3. The X-ray fluorescence spectrometer as claimed in claim 1 , wherein
the quantitative analysis condition setting unit obtains, for each of the measurement lines, a net intensity based on the set background measurement angles of the measurement line for each of the plurality of standard samples subjected to the qualitative analyses, and
when, in at least one of the standard samples, the obtained net intensity is negative and the absolute value of the obtained net intensity is greater than a theoretical standard deviation of the net intensity, the quantitative analysis condition setting unit cancels setting of the background measurement angle at which the background intensity is higher in the virtual profile, of the background measurement angles of the measurement line which are set on the lower angle side and the higher angle side relative to the measurement line.

4. A sequential X-ray fluorescence spectrometer which irradiates a sample with primary X-rays and measures the intensities of generated secondary X-rays, the spectrometer comprising:
a plurality of standard samples to create calibration curves corresponding to analytical samples; and
a quantitative analysis condition setting unit configured to preset, as quantitative analysis conditions, with measurement lines for the analytical samples, a half value width of a peak profile of each measurement line, sample constituting elements and their contents of each standard sample, wherein
the quantitative analysis condition setting unit
performs qualitative analyses of the plurality of standard samples, to obtain, for each of measurement lines identified in each standard sample, a peak angle obtained through peak search, background angles based on the peak angle and the preset half value width of the peak profile, and a net intensity based on a peak intensity at the peak angle and background intensities at the background angles,
sets, for each of the measurement lines, the peak angle of the standard sample at which no interfering line is identified within a predetermined angle range centered on the measurement line and the peak intensity is maximum, as a peak measurement angle of the measurement line for the analytical samples in the quantitative analysis conditions, and
obtains, for each of the measurement lines, background measurement angle ranges on the basis of the peak profile of the corresponding standard sample and the preset half value width of the peak profile, and sets an angle, which is closest to the measurement line within the background measurement angle range, on each of a lower angle side and a higher angle side relative to the measurement line, as a background measurement angle of the measurement line for the analytical samples in the quantitative analysis conditions, the background measurement angle range being common to the plurality of standard samples subjected to the qualitative analyses.

5. The X-ray fluorescence spectrometer as claimed in claim 4 , wherein
the quantitative analysis condition setting unit sets, as new background measurement angles of the measurement line for each of the standard samples, the background measurement angles by which the background intensity at the peak measurement angle of the measurement line is minimized when, in the peak profile of the corresponding standard sample, the background measurement angles of the measurement line which are set on the lower angle side and the higher angle side relative to the measurement line are alternately brought closer to the measurement line within a predetermined angle range, at a predetermined angle step, and
sets, on each of the lower angle side and the higher angle side relative to the measurement line, as a new background measurement angle of the measurement line for the analytical samples in the quantitative analysis conditions, the background measurement angle of the measurement line which is farthest from the peak measurement angle of the measurement line, among the new background measurement angles of the measurement line for the plurality of standard samples subjected to the qualitative analyses.

Assignees

• Rigaku Denki Co Ltd

Inventors

• Hara Shinya
• Matsuo Takashi
• Yamada Yasujiro
• Honma Hisashi
• Kataoka Yoshiyuki

Classifications

• G01N2223/076

  X-ray fluorescence · CPC title

• G01N23/2076

  for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS · CPC title

• G01N23/2209

  using wavelength dispersive spectroscopy [WDS] · CPC title

• G01N23/207

  Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions · CPC title

• G01N23/223 Primary

  by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence · CPC title