Rigaku Corporation

Rigaku Industrial Corporation

Yoshiyuki Kataoka

Yasujiro Yamada

Hisayuki Kohno

Shuichi Kato

Shinya Hara

Takashi Yamada

Takashi Matsuo

Yasuhiko Nagoshi

Hisashi Honma

Yasushi Kusakabe

Kosuke Kawakyu

Shin Tanaka

Takashi Shoji

Makoto Doi

Hajime Fujimura

Takao Moriyama

Masatsugu Kuraoka

Eiichi Furusawa

Hisashi Inoue

Kenji Watanabe

Atsushi Morikawa

Noboru Yamashita

An X-ray fluorescence spectrometer according to the present invention includes a calculation unit () configured to calculate a content of each element in a sample () using an FP method, wherein the calculation unit () is configured to: in order to take into consideration an influence of unmeasured elements for which the fluorescent X-rays are not measured, use shorter-wavelength scattered X-rays of primary X-rays having a wavelength of 0.05 nm or more and 0.075 nm or less, and longer-wavelength scattered X-rays of the primary X-rays having a wavelength of 0.11 nm or more and 0.23 nm or less as scattered X-rays whose intensities are measured by a detection unit (), assume a mean atomic number for elements other than hydrogen included in the unmeasured elements, and assume a content for hydrogen.

X-ray fluorescence spectrometer

By regarding total precision of an X-ray intensity as counting precision due to statistical fluctuation and counting loss and by regarding the counting precision as a product of precision of an uncorrected intensity, which is an intensity before counting loss correction is performed, and a gradient of a corrected intensity with respect to the uncorrected intensity, a counting time calculation unit () included in an X-ray fluorescence spectrometer of the present invention calculates a counting time from specified total precision of the X-ray intensity, a given counting loss correction coefficient, and a given corrected intensity for each measurement line ().

Provided are a quantitative analysis method, a quantitative analysis program, and an X-ray fluorescence. The quantitative analysis method includes: a step of acquiring a representative composition set to represent contents of analysis components; a step of acquiring a plurality of comparative compositions, in each of which the content of one of the analysis components of the representative composition is changed by a predetermined content; a detection intensity calculation step of calculating a detection intensity indicating an intensity of fluorescent X-rays detected under the influence of the geometry effect through use of an FP method with respect to a virtual sample having a thickness set in advance and being indicated by each of the representative composition and the comparative compositions; and a step of calculating a matrix correction coefficient for each of the analysis components based on the detection intensity.

Quantitative analysis method, quantitative analysis program, and X-ray fluorescence spectrometer

A sequential X-ray fluorescence spectrometer according to the present invention includes a total analysis time display unit configured to measure, for each kind of analytical sample, a standard sample which contains a component at a known content as a standard value to determine a measured intensity of each measurement line corresponding to the component. The total analysis time display unit is further configured to calculate, for each component, a counting time which gives a specified analytical precision by using the standard value and the measured intensity and to calculate a total counting time as a sum of the counting times of respective components. The total analysis time display unit is configured to calculate a total analysis time as a sum of the total counting time and a total non-counting time and to output the calculated total analysis time and the calculated counting times of the respective components.

An X-ray fluorescence spectrometer of the present invention includes a counting time calculation unit () configured to: by a predetermined quantitative calculation method, determine each of quantitative values by using reference intensities of one standard sample and repeatedly perform a procedure of determining each of the quantitative values in a case where only a measured intensity of one of measurement lines is changed by a predetermined value, to calculate a ratio of a change in each of the quantitative values to the predetermined value as a quantitative-value-to-intensity change ratio, the one of the measurement lines having the measured intensity to be changed being different on each repetition of the procedure; and use quantitative-value-to-intensity change ratios calculated thereby for all the measurement lines to calculate a counting time for each of the measurement lines from a quantification precision specified for each of the quantitative values.

A wavelength dispersive X-ray fluorescence spectrometer includes a single one-dimensional detector () having detection elements () arranged linearly, and includes a detector position change mechanism () for setting a position of the one-dimensional detector () to either a parallel position at which an arrangement direction of the detection elements () is parallel to a spectral angle direction of a spectroscopic device () or an intersection position at which the arrangement direction intersects the spectral angle direction. At the parallel position, a receiving surface of the one-dimensional detector () is located at a focal point of focused secondary X-rays (). At the intersection position, a receiving slit () is disposed at the focal point of the focused secondary X-rays (), and the receiving surface is located at a traveling direction side of the focused secondary X-rays () farther from the spectroscopic device () than the receiving slit ().

Wavelength dispersive X-ray fluorescence spectrometer

An X-ray fluorescence analysis method according to an FP method uses a predefined theoretical intensity formula in a standard sample theoretical intensity calculation step for obtaining a sensitivity constant and in an unknown sample theoretical intensity calculation step during iterative calculation. In the formula, only in an absorption term relating to absorption of X-rays, a mass fraction of each component is normalized so that a sum of the mass fractions of all components becomes 1.

X-ray fluorescence analysis method, X-ray fluorescence analysis program, and X-ray fluorescence spectrometer

A wavelength dispersive X-ray fluorescence spectrometer of the present invention includes: a position sensitive detector () configured to detect intensities of secondary X-rays () at different spectral angles, by using detection elements () corresponding to the secondary X-rays () at different spectral angles; a measured spectrum display unit () configured to display a relationship between a position, in an arrangement direction, of each detection element (), and a detected intensity by the detection element (), as a measured spectrum, on a display (); a detection area setting unit () configured to be set a peak area and a background area; and a quantification unit () configured to calculate, as a net intensity, an intensity of the fluorescent X-rays to be measured, based on a peak intensity in the peak area, a background intensity in the background area, and a background correction coefficient, and to perform quantitative analysis.

Wavelength dispersive x-ray fluorescence spectrometer and x-ray fluorescence analyzing method using the same

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

A scanning-type X-ray fluorescence spectrometer according to the present invention includes a quantitative analysis condition setting unit configured to determine whether or not to add, as an analytical element, a new detected element other than preset sample constituting elements, from an absorption-enhancement effect degree of fluorescent X-rays on an analytical value of an analytical element and an overlapping effect degree by an interfering line on an analytical line of the analytical element, on the basis of qualitative analysis results and semi-quantitative analysis results of standard samples.

In the wavelength dispersive X-ray fluorescence spectrometer of the present invention, a counting loss correcting unit (), when correcting a counting rate of pulses determined by a counting unit () on the basis of a dead time of a detector (), stores beforehand a correlation between a predetermined pulse height range, within which pulses are selected by a pulse height analyzer (), and the dead time and determines the dead time so as to correspond to the predetermined pulse height range during a measurement on the basis of the stored correlation.

An X-ray fluorescence analyzing method includes irradiating a liquid sample (A) containing hydrogen and at least one element of carbon, oxygen and nitrogen with primary X-rays (); measuring the intensity F of fluorescent X-rays () from each of elements in the sample (A) and having the atomic number 9 to 20, and the intensity S of scattered X-rays () from the sample (A) caused by continuous X-rays in the primary X-rays; and calculating the concentration of each of the elements, based on the ratio between the measured intensity F, and the measured intensity S. The wavelength of the scattered X-rays () is so chosen as to be shorter than that of the fluorescent X-rays () and is so set that the measured intensity S and the mass absorption coefficient thereof are inversely proportional to each other within the range of variation of a composition of the sample (A).

X-ray fluorescence analyzing method

An X-ray fluorescence spectrometer for measuring the concentration of sulfur contained in a sample (S), by irradiating the sample (S) with primary X-rays from an X-ray tube (), monochromating fluorescent X-rays emitted from the sample (S) with a spectroscopic device, and detecting monochromated fluorescent X-rays with an X-ray detector. The spectrometer includes the X-ray tube () having a target with an element including chromium, an X-ray filter () disposed on a path of travel of X-rays between the X-ray tube () and the sample (S) and having a predetermined transmittance for Cr&#x2014;K&#x3b1; line from the X-ray tube () and made of a material which is an element of which absorption edges do not exist between energies of S&#x2014;K&#x3b1; line and Cr&#x2014;K&#x3b1; line, and a proportional counter () having a detector gas containing a neon gas or a helium gas.

A scanning X-ray fluorescence spectrometer includes a quantitatively analyzing device () which calculates the concentration of hexavalent chrome based on the fact that the peak spectroscopic angle, at which the maximum intensity is attained in Cr&#x2014;K&#x3b1; line (), changes depending on the ratio of the concentration of the hexavalent chrome vs. the concentration of the intensity of the total chrome. A plurality of detecting device () having different resolutions as a combination of a divergence slit (), a spectroscopic device (), a receiving slit () and a detector () is provided such that when the change of the peak spectroscopic angle is to be detected, a detecting device (B) having a higher resolution than that of the detecting device (A), which is selected when the concentration or the intensity of the total chrome is to be determined, is selected.

X-ray fluorescence spectrometer and program for use therewith

An X-ray fluorescence spectrometer includes an X-ray sourcefor irradiating a sampleat a predetermined incident angle &#xf8; with primary X-rays, and a detecting devicefor measuring an intensity of fluorescent X-raysgenerated from the sample at a predetermined detection angle &#x3b1; and &#x3b2;, wherein with two combinations of the incident angle &#xf8; and the detection angle &#x3b1; and &#x3b2;, in which combinations the incident angles &#xf8; and/or the detection angles &#x3b1; and &#x3b2; are different from each other, each intensity of the fluorescent X-raysis measured and, also, the incident angle &#xf8; and the detection angle &#x3b1; and &#x3b2; in each of the combination are so set that with respect to a measurement depth represented by the coating weight, at which the intensity of the fluorescent X-raysattains a value equal to 99% of the uppermost limit when the coating weight of a target coating to be measured is increased, respective measurement depths in the two combinations may be a value greater than the coating weight of a coating

Growing community of inventors

Takatsuki, Japan

Yoshiyuki Kataoka