JPH0678997B2 - Qualitative analysis method by electron probe microanalyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application The present invention mainly relates to a method for qualitatively analyzing measurement data obtained by applying an electron probe microanalyzer (EPMA).

(B) Prior art Generally, in order to perform constant analysis of elements contained in a sample by applying EPMA, a characteristic X-ray intensity is measured to obtain a wavelength profile. In this case, since the lowest excitation voltage of the element has not been taken into consideration in the past, the wavelength profile obtained especially when the sample contains a trace element, whether it is a simple background or not It is not possible to clearly determine whether or not it is the peak indicated by, and the peak certification may be mistaken. Therefore, there is a problem that the reliability of the qualitative analysis is still insufficient.

(C) Objective The present invention aims to solve the conventional problems described above, improve the detection accuracy of contained elements, and improve the reliability of analysis.

(D) Structure In order to achieve such an object, the present invention adds the accelerating voltage of EPMA as a condition for qualitative analysis. That is, the present invention applies an electron probe microanalyzer (EPMA), measures the characteristic X-ray intensity of a sample to obtain a wavelength profile, and determines the element based on the wavelength showing the maximum peak value contained in this wavelength profile. Is a qualitative analysis method for identifying, comparing the lowest excitation voltage of the identification element and the acceleration voltage of the EPMA, the lowest excitation voltage of the identification element is EPMA
If it is higher than the accelerating voltage of, it is judged that the identifying element does not exist and is excluded from the target of qualitative analysis,
If it is equal to or lower than the acceleration voltage of EPMA, it is determined that the identifying element exists, and the element is subjected to qualitative analysis.

(E) Example Hereinafter, an example of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a block configuration diagram including a qualitative analysis device and EPMA applied for implementing the present invention. In the figure, reference numeral 1 is EPMA, 2 is a qualitative analysis device, and 4 is an interface that connects the EPMA 1 and the qualitative analysis device 2. The qualitative analyzer 2 includes a central control unit 6 for performing various control processes, a first storage unit in which characteristic X-ray wavelength data file and various program data are stored, characteristic X-ray intensity data measured by EPMA1 and central control unit 6 Second storage section for temporarily storing the data processed in step 2, peak detection section 12 for detecting the presence / absence of a peak included in the characteristic profile of characteristic X-rays, and operation processing for performing calculation processing such as subtraction of intensity data of characteristic X-rays Part 14,
It comprises a comparison unit 16 for comparing the lowest excitation voltage specific to the element and the acceleration voltage of EPMA 1, and a display unit 18 for displaying the calculation result.

Next, a qualitative analysis method using this apparatus will be described with reference to the flow chart in FIG.

First, using EPMA1, perform point analysis on the analysis sample, and
Then, the intensity of the characteristic X-rays emitted from the sample is measured by rotating the X-ray spectroscope, and the obtained wavelength profile data is sent to the qualitative analyzer 2 through the interface 4 (step n ₁ ). The wavelength profile data input to the central controller 6 of the qualitative analyzer 2 is transferred to the peak detector 12. The peak detector 12 detects whether or not a peak exists in the obtained wavelength profile (step n ₂ ).
For example, when the wavelength profile has a peak as shown in FIG. 3 (a), the maximum peak in the measurement target section X (P _A1 in FIG. 3 (a)) is the primary line intensity of the element A. Therefore, the central control unit 6 identifies the element indicating the peak P _A1 based on the peak detection signal of the peak detector 12 by referring to the characteristic X-ray wavelength data file stored in the first storage unit 8 (step n ₃ ). Subsequently, the comparison section 16 compares the lowest excitation voltage E _A of the identified element _A with the acceleration voltage V _{0 of} EPMA (step n ₄ ). When the lowest excitation voltage E _A of the identification element is higher than the acceleration voltage V _{0 of} EPMA, the element A does not exist, so the central control unit 6 excludes the element A from the analysis target (step n ₅ ). X-ray intensity P of the lowest excitation voltage E _A secondary line or higher order line of said element A in the arithmetic processing unit 14 is lower than the acceleration voltage V ₀ which EPMA identification element A
_{A2 to} P _A4 are calculated from the ratio of primary line intensity P _A1 . And
This identification element A and the intensity data P _{A1 to} P _A4 it shows are
The data is stored in the storage unit 10 (step n ₆ ). Further, the wavelength profile (the third
The intensity data P _{A1 to} P _A4 of the identification element A is subtracted from the figure (a)) (step n ₇ ). Then, the peak detector determines whether or not there is a peak in the remaining subtracted wavelength profile.
Detect at 12 (step n ₈ ). If the peak as shown in FIG. 3 (b) is still present, the process returns sequentially to step n _3, step n ₄ from step _{n 3, n 6, n 7} , n 8 or step n ₄ from step n ₃ , n ₅ , n ₈ are repeated. In this way, the lowest excitation voltage of an element and the accelerating voltage of EPMA are always compared in the analysis process, so if an element that should not exist originally is identified, false identification of peaks is prevented. Become. Then, the processing result is displayed on the display unit 18.

(F) Effect As described above, according to the present invention, the accelerating voltage of EPMA and the excitation voltage of the element are sequentially compared and taken into consideration in the analysis process, so that the peak recognition error is prevented and the detection accuracy of the contained element is improved. Therefore, an excellent effect that the reliability of analysis is further improved can be obtained.

[Brief description of drawings]

The drawings show an embodiment of the present invention, FIG. 1 is a block diagram of an apparatus applied to implement the present invention, FIG. 2 is a flow chart for explaining the procedure of qualitative analysis, and FIG.
The figure is a diagram showing a wavelength profile.

Claims (1)

[Claims] 1. An electron probe microanalyzer (EPMA) is applied to measure the characteristic X-ray intensity of a sample to obtain a wavelength profile, and the element is based on the wavelength showing the maximum peak value contained in this wavelength profile. In the qualitative analysis method for identifying, by comparing the lowest excitation voltage of the identification element and the acceleration voltage of the EPMA, if the lowest excitation voltage of the identification element is equal to or lower than the acceleration voltage of EPMA, it is determined that the identification element does not exist. Qualitative analysis by an electron probe microanalyzer characterized by removing from the target of qualitative analysis and determining that the identifying element exists if the lowest excitation voltage of the identifying element is equal to or lower than the acceleration voltage of EPMA Method.