JP4255012B2 - X-ray fluorescence analyzer - Google Patents

Description

  The present invention is an X-ray fluorescence analyzer that performs qualitative analysis, and searches for and displays candidate line types from a database for the peak of a fluorescent X-ray spectrum specified by an operator for identifying the line type. Relates to the device.

Many fluorescent X-ray analysis apparatuses that perform qualitative analysis automatically identify the peak of the obtained fluorescent X-ray spectrum by searching for a corresponding line type from a database (see Non-Patent Document 1). However, it is impossible in principle to automatically and definitely identify all the peaks of every sample, and it is also performed manually by an operator. At that time, with respect to the peak of the fluorescent X-ray spectrum designated by the operator for identifying the line type, the line type having a wavelength close to the peak is retrieved from the database as a candidate and displayed on the display unit together with the corresponding 2θ angle. The operator selects the line type that seems to be correct from the displayed candidates in consideration of the information obtained so far about the sample, and manually identifies it.
“Guide to fluorescent X-ray analysis” published by Rigaku Denki Kogyo Co., Ltd., September 1982, p. 43-44

  Conventionally, however, candidates are searched from the line types of all the elements in the database. In particular, in the light element region, a large number of candidates such as L-line, M-line, and higher-order line of heavy elements are displayed and identified for the operator. May not be easy.

  The present invention has been made in view of such problems, and searches for a candidate line type from the database for the peak of the fluorescent X-ray spectrum specified by the operator in order to identify the line type in the qualitative analysis. An object of the present invention is to provide an apparatus that allows an operator to easily select and identify a line type in a fluorescent X-ray analyzer to be displayed.

In order to achieve the above object, an X-ray fluorescence spectrometer according to the present invention is an X-ray fluorescence spectrometer that first performs qualitative analysis by irradiating primary X-rays to obtain a fluorescence X-ray spectrum, For the peak of the fluorescent X-ray spectrum designated for identifying the line type, manual identification means for searching for candidate line types from the database and displaying them on the display, and elements for which the search range by the manual identification means has been identified And an input means for inputting information to limit to the line types .

According to the X-ray fluorescence spectrometer of the present invention, the operator can limit the search range by the manual identification means to the line types of the identified elements, so that a small number of candidates that are likely to be correct are displayed and identified for the operator. Is easy. In the present invention, with respect to the input means, the manual identification means preferably is that the addition of first-order lines of the Kα line of elements unidentified search range inputted by.

  Hereinafter, an X-ray fluorescence spectrometer according to an embodiment of the present invention will be described. First, the configuration of this apparatus will be described with reference to FIG. This apparatus is a fluorescent X-ray analyzer that performs qualitative analysis by irradiating a sample 1 with primary X-rays 3 to obtain a fluorescent X-ray spectrum, and includes a sample stage 2 on which the sample 1 is placed and a sample 1 An X-ray source 4 such as an X-ray tube that irradiates primary X-rays 3, a spectroscopic element 6 that splits fluorescent X-rays 5 generated from the sample 1, and fluorescent X-rays 7 that are split by the spectroscopic element 6 are incident. And a detector 8 for detecting the intensity thereof. The output of the detector 8 is input to the qualitative analysis means 11 through an amplifier, a wave height analyzer, a counting means, etc. (not shown).

  This apparatus is a wavelength dispersive and scanning X-ray fluorescence analyzer, and interlocking means for interlocking the spectroscopic element 6 and the detector 8 so that the wavelength of the fluorescent X-ray 7 incident on the detector 8 changes. 10, that is, a so-called goniometer. When the fluorescent X-ray 5 is incident on the spectroscopic element 6 at a certain incident angle θ, the extended line 9 of the fluorescent X-ray 5 and the fluorescent X-ray 7 dispersed (diffracted) by the spectroscopic element 6 have a spectrum that is twice the incident angle θ. Although the angle 2θ is formed, the interlocking unit 10 changes the wavelength of the fluorescent X-ray 7 that is split by changing the spectral angle 2θ, so that the split fluorescent X-ray 7 is incident on the detector 8. The spectroscopic element 6 is rotated about an axis O perpendicular to the paper surface passing through the center of the surface, and the detector 8 is rotated along the circle 12 about the axis O by twice the rotation angle. The value of the spectral angle 2θ (2θ angle) is input from the interlocking unit 10 to the qualitative analysis unit 11.

  The qualitative analysis unit 11 includes an automatic identification unit 13, a manual identification unit 14, and a database 15. In the database 15, as a spectrum table, all line types that can be detected by this apparatus are preliminarily stored together with corresponding 2θ angles and relative intensities (intensities where the intensity of the largest line type generated from the same element is 100). Have been entered. The automatic identification means 13 performs a process such as smoothing based on the intensity and 2θ angle of the input fluorescent X-ray 7 to obtain a fluorescent X-ray spectrum, and performs a peak search to detect a corresponding line from the database 15. The seed is automatically identified by searching under a predetermined condition.

  The manual identification unit 14 is a fluorescent X-ray spectrum that is specified by the operator for manually identifying the line type when there is a peak that cannot be identified by the automatic identification unit 13 or when the operator verifies the identification result. The candidate line type is searched from the database 15 for the peak of, and displayed on the display 16 such as a CRT display. Here, the operator can limit the search range by the manual identification means 14 to the line types of the identified elements. Further, the search range can be limited to the line type of the identified element and the primary line of the Kα line of the unidentified element.

  Next, with regard to the operation of this apparatus, there is an example in which there is a peak that could not be automatically identified at a position of 107.9 degrees in the vicinity of the S-Kα ray at a 2θ angle in the obtained fluorescent X-ray spectrum, and this is manually identified. I will explain it. In order to manually identify this line type, the operator uses the input means such as a mouse (not shown) in the fluorescent X-ray spectrum shown in FIG. Specify the peak at the position.

  Then, the screen changes to a screen for specifying a search condition (search range) as shown in FIG. As the search range in the initial state, since “all line types” is selected as the “search level”, the search range is not limited to the Kα line, Kβ line, Lα line, Lβ line, and Mα line, but weak lines (such as Lγ1 line). All line types are included, and the check box for “High-order line” is checked, so high-order lines are also included without being limited to the primary line, and the check box for “Identification element” is checked. Therefore, the line type of the identified element is not limited, and the line type of the unidentified element is also included.

  When the operator clicks “search”, the manual identification unit 14 in FIG. 1 searches the database 15 for a specified line type, that is, a line type that is close to a predetermined range of 2θ angle of 107.9 degrees. The search is performed in the range, and the display unit 16 displays the “search result” as shown in FIG. 3 together with the corresponding 2θ angle and relative intensity. When searching for candidate line types in the search range in the initial state, particularly in the light element region, there are many high-order and weak lines of fluorescent X-rays of elements having higher atomic numbers, for example, 62 line types (FIG. 3). (Only six of them are visible, but if you scroll, you can see all the line types). It is not easy for an operator to select a line type that seems to be correct from a large number of candidates and manually identify it, and the conventional technique cannot solve this problem.

  On the other hand, in the apparatus of this embodiment, as shown in FIG. 4, the operator selects a search range by the manual identification unit 14 by checking a check box of “identification element” on a screen for specifying a search range. Can be limited to line types of elements that have already been identified by automatic or manual identification. Then, if the operator clicks “Search” again, a small number of candidates having a high possibility of being correct, for example, only four line types here are searched and displayed. Of these, As is known that the As-Kα line having the maximum peak intensity appearing in the qualitative analysis region of heavy elements is not detected, but the operator has a 2θ angle of the remaining two line types. The close Fe-Kβ1 cubic line can be easily identified as corresponding to the peak appearing at the 107.9 degree position. Click the “Fe-KB1-3rd” row to highlight it, and click “Add” to identify it. As the “search result”, for the line type of the identified element, the maximum peak intensity from the element may be displayed together.

  In addition, in the apparatus of this embodiment, the operator specifies, for example, a check box (not shown) of “Kα primary line of unidentified element” in addition to the check box of “identified element” on the screen for specifying the search range. By checking the check box, the search range by the manual identification means 14 can be limited to the line type of the identified element and the primary line of the Kα line of the unidentified element. For example, in the spectrum of the S-Kα ray in the light element region, the peak intensity was very low and no peak was detected by the peak search. In other words, that is effective when the peak is the L line, M line, weak line or higher order of the identified element having an atomic number larger than S, or the primary line of the unidentified S Kα line. It is. According to this limitation, a small number of candidates that are likely to be correct are displayed, and the target element and the interfering element can be confirmed at the same time, so that the operator can easily identify.

  In the apparatus of this embodiment, when only a single peak is measured and manually identified, there is no identified element, so the search range by the manual identification means 14 is the line of the identified element. Do not limit to species.

  The apparatus of this embodiment is a wavelength dispersion type, but the present invention can also be applied to an energy dispersion type X-ray fluorescence analyzer, and the same effects can be obtained. In this case, energy (keV) is used instead of the 2θ angle, and a pile-up peak (sum peak) and an escape peak due to the detector used are included instead of including the higher order line in the search range.

1 is a schematic view showing a fluorescent X-ray analyzer according to an embodiment of the present invention. It is an example of the fluorescent X-ray spectrum which the display of the apparatus displays. It is an example of the search condition and search result which the indicator of the apparatus displays. It is another example of the search condition and search result which the indicator of the apparatus displays.

Explanation of symbols

1 Sample 3 Primary X-ray 14 Manual identification means 15 Database 16 Display

Claims (2)

A fluorescent X-ray analyzer that performs qualitative analysis by irradiating a sample with primary X-rays to obtain a fluorescent X-ray spectrum,
For fluorescent X-ray peak of the spectrum that was specified for the operator to identify the line type, and manual identification means for displaying on the display by searching the line type as a candidate from the database,
X-ray fluorescence analyzer and an input means for indicating to limit the search range of the previous SL manual identification means linetype previously identified elements are input. In claim 1,
An X-ray fluorescence analyzer for inputting to the input means that a primary line of Kα rays of an unidentified element is added to a search range by the manual identification means.

Images