X-ray analyzer, method for controlling same, and

Abstract

Provided is a technique for appropriately removing superimposed peaks in the analysis results of an X-ray analysis device. The control method of the X-ray analysis apparatus includes the steps of: acquiring a value related to a characteristic of the X-ray analysis apparatus (S200); and calculating an adjustment value for the gain of the determination waveform caused by the X-rays of the sample detected by the X-ray analysis device on the basis of the numerical value related to the characteristics (S202). The determination waveform is derived for accumulation determination, and in the accumulation determination, the gain of the determination waveform is adjusted on the basis of the adjustment value.

Description

Technical Field

[0001] The present invention relates to an X-ray analysis device, and more particularly to a pile-up determination method for removing sum peaks in an X-ray analysis device. Background Art

[0002] In the distribution of analysis results from a fluorescence X-ray analyzer, there are not only main peaks (e.g., Kα rays) but also superposition peaks. The intensity of the superposition peaks depends on the count rate and the time resolution of the detector. Non-patent document 1 (Ryohei Tanaka, Koretaka Yuge, Jun Kawai, Hussain Alawadhi, Artificial peaks in energy dispersive X-ray spectra: sum peaks, escape peaks, and diffraction peaks, X-RAY SPECTROMETRY, John Wiley & Sons, Ltd., 2017, 46, p5-p11) discloses the following method: using the count rate and peaking time to derive the ratio of the intensity I(m+1) of the mth superposition peak to the intensity I(1) of the main peak.

[0003] Prior art literature

[0004] Non-patent literature

[0005] Non-patent literature 1: Ryohei Tanaka, Koretaka Yuge, Jun Kawai, Hussain Alawadhi, Artificial peaks in energy dispersive X-ray spectra: sum peaks, escape peaks, and diffraction peaks, X-RAY SPECTROMETRY, John Wiley & Sons, Ltd., 2017, 46, p5-p11 Summary of the Invention

[0006] Problems to be solved by the invention

[0007] When superimposed peaks are removed from the distribution of analysis results using the conventional method disclosed in Non-Patent Document 1, there is a case where the superimposed peaks are not sufficiently removed.

[0008] The present invention has been conceived in view of such actual circumstances, and an object of the present invention is to provide a technique for appropriately removing superimposed peaks in analysis results of an X-ray analyzer.

[0009] Solutions for solving problems

[0010] According to one aspect of the present disclosure, an X-ray analysis device is provided, comprising: an X-ray detector that detects X-rays from a sample; a differential wave conversion unit that converts a step wave caused by the X-rays detected by the X-ray detector into a differential wave; a first conversion unit that converts the differential wave into a trapezoidal wave; a second conversion unit that converts the differential wave into a determination waveform with a peaking time shorter than that of the first conversion unit; and a pile-up determination unit that performs a pile-up determination on the determination waveform, wherein the pile-up determination unit adjusts a gain in the second conversion unit based on a numerical value related to characteristics of the X-ray analysis device.

[0011] According to another aspect of the present disclosure, an X-ray analysis device is provided, comprising: an X-ray detector that detects X-rays from a sample; a differential wave conversion unit that converts a step wave caused by the X-rays detected by the X-ray detector into a differential wave; a first conversion unit that converts the differential wave into a trapezoidal wave; a second conversion unit that converts the differential wave into a determination waveform with a peaking time shorter than the peaking time of the first conversion unit; and a pile-up determination unit that performs pile-up determination on the determination waveform, wherein the pile-up determination unit adjusts one or more threshold values ​​used in the pile-up determination based on a numerical value related to the characteristics of the X-ray analysis device.

[0012] According to an aspect of the present disclosure, a method for controlling an X-ray analysis device includes the following steps: obtaining a numerical value related to a characteristic of the X-ray analysis device; and calculating an adjustment value for the gain of a determination waveform caused by X-rays of a sample detected in the X-ray analysis device based on the numerical value related to the characteristic, wherein the determination waveform is derived to perform a pile-up determination, and in the pile-up determination, the gain of the determination waveform is adjusted based on the adjustment value.

[0013] According to another aspect of the present disclosure, a control method for an X-ray analysis device includes the following steps: obtaining a numerical value related to a characteristic of the X-ray analysis device; and calculating, based on the numerical value related to the characteristic, an adjustment value for one or more threshold values ​​used for pile-up determination in the X-ray analysis device, wherein, in the pile-up determination, the adjustment value is used to adjust one or more threshold values ​​for a determination waveform caused by X-rays of a sample detected in the X-ray analysis device.

[0014] The program according to one aspect of the present disclosure is executed by one or more processors of a computer to cause the computer to implement the above-described method for controlling the X-ray analysis device.

[0015] Effects of the Invention

[0016] According to one aspect of the present disclosure, there is provided a technique for appropriately removing overlapping peaks in analysis results of an X-ray analysis apparatus. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 1 is a schematic structural diagram of an X-ray analysis device 1 according to one embodiment of the present disclosure.

[0018] Figure 2 This is a diagram for explaining an example of the processing content of the output waveform from the first conversion filter 46.

[0019] Figure 3 It is a diagram for explaining the content of width determination.

[0020] Figure 4 This is a diagram for explaining the details of interval determination.

[0021] Figure 5 This is a diagram showing a specific example of a waveform in which deposition determination cannot be performed normally.

[0022] Figure 6 This is a flowchart of processing performed in the X-ray analyzer 1 for analyzing a sample.

[0023] Figure 7 yes Figure 6 Flowchart of the subroutine of step S20.

[0024] Figure 8 This is a diagram for explaining an example of threshold adjustment.

[0025] Figure 9 yes Figure 6 Flowchart of a modified example of the processing of .

[0026] Figure 10 This is a flowchart of the subroutine of step S22. DETAILED DESCRIPTION

[0027] Hereinafter, embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. The same or corresponding parts in the drawings are denoted by the same reference numerals, and their description will not be repeated.

[0028] [Structure of X-ray Analyzer]

[0029] Figure 1 FIG. 1 is a schematic structural diagram of an X-ray analysis device 1 according to an embodiment of the present disclosure. In one implementation example, the X-ray analysis device 1 is an energy dispersive fluorescence X-ray analysis device. Figure 1As shown, X-ray analysis apparatus 1 includes an X-ray tube 10, an X-ray detector 12, a preamplifier 14, a differential circuit 16, an amplifier 18, an ADC (Analog to Digital Converter) 20, a CPU (Central Processing Unit) 30, a memory 31, and a signal processing device 40. X-ray detector 12 is an energy dispersive spectrometer. Signal processing device 40 is a signal processing device for X-ray analysis.

[0030] The X-ray tube 10 emits primary X-rays toward the sample S. The X-ray tube 10 includes, for example, a target serving as an anode, a filament serving as a cathode, and a housing for housing the target and filament. When a high voltage is applied to the target and a low voltage is applied to the filament, thermal electrons radiated from the filament collide with the end face of the target, generating primary X-rays at that end face. The primary X-rays generated at the end face of the target are emitted toward the sample S. When the primary X-rays irradiate the sample S, fluorescent X-rays excited by the primary X-rays are emitted from the sample S and enter the X-ray detector 12.

[0031] The X-ray detector 12 detects the intensity of fluorescent X-rays within a predetermined wavelength range. The X-ray detector 12 is disposed within a housing and includes a detection element for detecting the intensity of fluorescent X-rays within the aforementioned wavelength range. The detection element is, for example, a lithium drift-type Si semiconductor element.

[0032] The output signal of the X-ray detector 12 is amplified by the preamplifier 14. The output signal is transformed into a step-wave signal by the preamplifier 14. Each step of the step-wave signal indicates the detection of fluorescent X-rays. The height of each step indicates the wavelength λ, that is, the X-ray energy E.

[0033] The output signal amplified by preamplifier 14 is sent to differentiating circuit 16. Differentiating circuit 16, consisting of capacitor C and resistor R, converts the step wave into a differential wave represented by the following equation (1). By converting the step wave into a differential wave, the dynamic range can be expanded, resulting in high resolution. The differential wave is amplified by amplifier 18 and sent to ADC 20.

[0034] [Number 1]

[0035] y = exp(-nT / τ) = a n …(1)

[0036] Wherein, τ (=RC) is the time constant, T is the sampling period, n is the number of samples, and a is (exp(-T / τ)).

[0037] The ADC 20 samples the differential wave, which is an analog signal, at a predetermined sampling cycle and converts it into a digital signal (hereinafter referred to as a differential wave digital signal). The differential wave digital signal is input to the signal processing device 40 .

[0038] The signal processing device 40 is generally composed of logic devices such as an FPGA (Field-Programmable Gate Array).

[0039] In this embodiment, the signal processing device 40 includes an offset correction unit 44, a first conversion filter 46, a second conversion filter 47, a baseline correction unit 48, a pile-up determination processing unit 49, a gain / offset adjustment unit 50, a peak detector 52, and a histogram memory 54. In the signal processing device 40, the offset correction unit 44, the first conversion filter 46, the second conversion filter 47, the baseline correction unit 48, the pile-up determination processing unit 49, the gain / offset adjustment unit 50, the peak detector 52, and the histogram memory 54 can be implemented as independent hardware resources, or two or more of them can be implemented as shared hardware resources.

[0040] The offset correction unit 44 performs offset correction on the differential wave digital signal supplied from the ADC 20 , and outputs the corrected differential wave digital signal to the first conversion filter 46 and the second conversion filter 47 .

[0041] Each of the first conversion filter 46 and the second conversion filter 47 is a digital filter configured to convert the differential wave corrected by the offset correction unit 44 into a trapezoidal wave represented by equation (2).

[0042] [Number 2]

[0043]

[0044] Here, in equation (2), M corresponds to the time of the upper and lower bases of the trapezoidal wave, and N represents the rise and fall times of the trapezoidal wave. M is also called the flat time, and N is also called the peaking time. The first conversion filter 46 is a so-called slow filter, and the second conversion filter 47 is a so-called fast filter. More specifically, the values ​​of M and N for the second conversion filter 47 are smaller than those for the first conversion filter 46.

[0045] The accumulation determination processing unit 49 uses the waveform converted by the second conversion filter 47 as a “determination waveform” for accumulation determination.

[0046] The output waveform from the first conversion filter 46 is input to the peak detector 52 after the baseline and gain are adjusted by the baseline correction unit 48 and the gain / offset adjustment unit 50 .

[0047] Peak detector 52 detects peaks in the output waveform and acquires the peak height (peak top value) of each peak. The accumulation determination processing unit 49 determines the occurrence of accumulation as a result of the accumulation determination and outputs information about superimposed peaks resulting from accumulation to peak detector 52. Peak detector 52 removes peaks from the output waveform for which peak top values ​​are acquired, those peaks identified as superimposed peaks by the accumulation determination processing unit 49. For each peak, peak detector 52 increments the count value of X-ray energy E corresponding to the peak top value and stores it in histogram memory 54.

[0048] The memory 31 includes a program storage area 31A for non-transitory storage of program data and a data storage area 31B for data storage. The X-ray analyzer 1 performs various processes by having the CPU 30 execute programs stored in the program storage area 31A (or a storage device other than the X-ray analyzer 1).

[0049] The CPU 30 generates a peak height distribution graph (energy spectrum histogram) based on the count values ​​stored in the histogram memory 54. In the peak height distribution graph, the horizontal axis represents the fluorescent X-ray energy E, and the vertical axis represents the element content (intensity). In the peak height distribution graph, a peak unique to each element appears at a position corresponding to the fluorescent X-ray energy E emitted by the element contained in the sample S. Based on the peak's location and X-ray intensity, the CPU 30 performs qualitative and quantitative analysis of the contained elements.

[0050] Figure 2 4 is a diagram for explaining an example of the processing content of the output waveform from the first conversion filter 46. Figure 2 In the graph, the vertical axis represents amplitude and the horizontal axis represents time.

[0051] exist Figure 2 The graph shown shows waveforms WF01, WF02, and WF03 related to X-rays obtained for a certain sample. Waveform WF01 is a waveform output from the preamplifier 14. Waveform WF02 is a waveform output from the second conversion filter 47. Waveform WF03 is a waveform output from the first conversion filter 46. Figure 2 , the amplitudes of the waveforms WF01 , WF02 , and WF03 are appropriately offset so that these waveforms can be easily viewed in a single graph.

[0052] Waveform WF01 contains five height differences. Figure 2In the waveforms WF02 and WF03 , the numbers “1” to “5” are assigned to the five level differences. In the waveforms WF02 and WF03 , the numbers “1” to “5” are assigned to the portions corresponding to the five level differences of the waveform WF01 .

[0053] In one implementation example, during pile-up determination using waveform WF02, the peak labeled "2" and the peak labeled "3" are too close together, so pile-up is determined to have occurred between these peaks. Consequently, the peaks labeled "2" and "3" in waveform WF03 are excluded from the peak top values ​​acquired by peak detector 52. Pile-up determination based on the distance between two adjacent peaks is hereinafter referred to as "interval determination."

[0054] Furthermore, in the pile-up determination using waveform WF02, the peak labeled "4" and the peak labeled "5" were processed as a single peak. Furthermore, because the width of this single peak was excessively wide, it was determined that pile-up had occurred between the peaks labeled "4" and "5." Consequently, the peaks labeled "4" and "5" in waveform WF03 were excluded from the peak top value acquisition by peak detector 52. Pile-up determination based on peak width will be referred to as "width determination" below.

[0055] [Accumulation Judgment]

[0056] Next, two determination methods (width determination and interval determination) will be described as specific examples of the accumulation determination in the accumulation determination processing unit 49. The accumulation determination processing unit 49 implements at least one of the following two determination methods.

[0057] <Width determination>

[0058] Figure 3 This figure explains the width test. Width test is also called a width test. In width test, whether pile-up has occurred is determined based on whether the peak width of each peak in the waveform exceeds a given threshold.

[0059] exist Figure 3 1 shows a waveform WF11. The waveform WF11 is output from the second conversion filter 47. In the graph including the waveform WF11, the vertical axis represents amplitude and the horizontal axis represents time.

[0060] Width determination utilizes a first threshold value TH11 and a second threshold value TH12. More specifically, within waveform WF11, peaks are identified for portions exceeding the first threshold value TH11. The peak width of each peak is then calculated and compared with the second threshold value TH12.

[0061] Signal SG11 represents an output signal of a circuit (constituent element of the accumulation determination processing unit 49 ) whose output value changes depending on whether the amplitude of waveform WF11 exceeds a predetermined value (a value having a specific ratio to the peak amplitude).

[0062] exist Figure 3 In the example, peak width WD11 is calculated for peak PK11. Peak width WD12 is calculated for peaks PK12 and PK13. Peak width WD11 is less than the second threshold value TH12 for width determination. Therefore, it is determined that no accumulation has occurred in peak PK11. On the other hand, peak width WD12 is greater than the second threshold value TH12 for width determination. Therefore, it is determined that accumulation has occurred in peaks PK12 and PK13.

[0063] <Interval determination>

[0064] Figure 4 This figure explains the details of the separation test. Separation testing is also called an isolation test. In separation testing, whether pile-up has occurred is determined based on whether the distance between adjacent peaks is closer than a given threshold.

[0065] exist Figure 4 The waveform WF21 is shown in FIG. The waveform WF21 is output from the second conversion filter 47. Figure 4 In the figure, the vertical axis represents amplitude and the horizontal axis represents time.

[0066] Interval determination utilizes a first threshold value TH21 and a second threshold value TH22 for interval determination. More specifically, within waveform WF21, peaks are identified for portions exceeding the first threshold value TH21 for interval determination. The first threshold value TH21 for interval determination can also be the same value as the first threshold value TH11 for width determination. The interval between two adjacent peaks is then calculated and compared with the second threshold value TH22 for interval determination.

[0067] exist Figure 4 In the example shown in Figure 2, four peaks PK21, PK22, PK23, and PK24 are identified in waveform WF21. The interval SP21 between peaks PK21 and PK22 is greater than the second threshold TH22 for interval determination. Therefore, it is determined that no accumulation has occurred between peaks PK21 and PK22. On the other hand, the interval SP22 between peaks PK23 and PK24 is less than the second threshold TH22 for interval determination. Therefore, it is determined that accumulation has occurred between peaks PK23 and PK24.

[0068] [Specific example of a waveform where accumulation determination cannot be performed normally]

[0069] Figure 5 : is a diagram showing a specific example of a waveform in which the accumulation determination cannot be performed normally. Figure 5 In FIG. 4 , a waveform WF31 is shown as an example of a waveform output from the second conversion filter 47. Figure 5 In the figure, the vertical axis represents amplitude and the horizontal axis represents time.

[0070] In the X-ray analysis apparatus 1, for example, due to individual differences in the mounted X-ray detectors 12, the waveform output from the second conversion filter 47 may vary from one X-ray analysis apparatus to another. For example, even when X-rays are detected for the same sample, the waveform output from the second conversion filter 47 may differ from one X-ray analysis apparatus 1 to another. Figure 3 The waveform WF11 is shown as having a portion exceeding the first threshold value TH11 for width determination, but in other X-ray analysis devices 1, as in Figure 5 The waveform WF31 does not have a portion exceeding the first threshold value TH11 for width determination. If a waveform does not have a portion exceeding the first threshold value TH11 for width determination, peaks that are the target of pile-up determination cannot be identified in that waveform. Therefore, it is conceivable that appropriate pile-up determination is not performed, and that peak detector 52 fails to sufficiently remove superimposed peaks from the output waveform of first conversion filter 46.

[0071] [Gain Adjustment]

[0072] In the X-ray analysis apparatus 1 , gain adjustment is performed on the waveform output from the second conversion filter 47 so that the accumulation determination processing unit 49 can appropriately perform accumulation determination and sufficiently remove the superimposed peak from the output waveform of the first conversion filter 46 .

[0073] More specifically, a gain adjustment value is determined based on individual differences in the X-ray analyzer 1. Then, the accumulation determination processing unit 49 processes the product of the original amplitude and the gain adjustment value in the entire waveform output from the second conversion filter 47 as the amplitude after gain adjustment.

[0074] Imagine that the output Figure 5 The waveform WF31 of the X-ray analysis device 1 is output with Figure 3 The X-ray analyzer 1 having the waveform WF11 has the characteristic of deriving the amplitude lower as a whole. The accumulation determination processing unit 49 of the X-ray analyzer 1 having such a characteristic (individual difference) will Figure 5 The product of the amplitude of the waveform WF31 and the gain adjustment value is processed as the amplitude after gain adjustment. Figure 5 The amplitude of the waveform WF31 is enhanced as a whole to approach Figure 3 The amplitude of waveform WF11.

[0075] In one implementation example, a gain adjustment value is determined based on the analysis results of a standard sample in each X-ray analyzer 1. An example of a standard sample is an alloy of tin and aluminum. More specifically, X-ray analysis is performed on the standard sample in each X-ray analyzer 1. Then, the energy position A of the Kα rays of tin is determined in the analysis results. In this sense, tin constitutes an example of a "standard substance." A reference value X related to the energy position of the Kα rays of tin is stored in the data storage area 31B of each X-ray analyzer 1. The CPU 30 calculates "X / A" as the gain adjustment value. The pile-up determination processing unit 49 uses the calculated gain adjustment value to perform pile-up determination.

[0076] The smaller the value of the energy position determined for the reference material, the larger the gain adjustment value described above. Therefore, in gain adjustment using the gain adjustment value described above, the smaller the value of the energy position determined for the reference material, the higher the magnification used to enhance the waveform output from the second conversion filter 47 during pile-up determination.

[0077] [Processing Flow]

[0078] Figure 6 This is a flowchart of the processing performed for analyzing a sample in the X-ray analyzer 1. For example, the processing is performed by the CPU 30 executing a given program. Figure 6 In addition, when the power of the X-ray analyzer 1 is turned on (after the initial setting is completed), the Figure 6 processing.

[0079] In step S10, the X-ray analyzer 1 determines whether an instruction to set a gain adjustment value has been received. In one embodiment, the X-ray analyzer 1 includes an input device such as a keyboard or buttons, and an instruction to set a gain adjustment value is input to the X-ray analyzer 1 by operating the input device. If the X-ray analyzer 1 determines that an instruction to set a gain adjustment value has been received ("Yes" in step S10), control proceeds to step S20. Otherwise ("No" in step S10), control proceeds to step S30.

[0080] In step S20, the X-ray analyzer 1 sets the gain adjustment value. Figure 7 The content of step S20 will be described later.

[0081] In step S30, the X-ray analyzer 1 determines whether a sample analysis instruction has been received. In one embodiment, the X-ray analyzer 1 includes an input device such as a keyboard or buttons, and the sample analysis instruction is input to the X-ray analyzer 1 by operating the input device. If the X-ray analyzer 1 determines that a sample analysis instruction has been received ("Yes" in step S30), control proceeds to step S40. Otherwise ("No" in step S30), control returns to step S10.

[0082] In step S40, the X-ray analyzer 1 performs X-ray analysis on the sample. At this point, if a gain adjustment value is stored in the data storage area 31B, the accumulation determination processing unit 49 uses this gain adjustment value to adjust the gain of the waveform output from the second conversion filter 47 as described above. The X-ray analyzer 1 then returns control to step S10.

[0083] Figure 7 yes Figure 6 Flowchart of the subroutine of step S20.

[0084] In step S200, the X-ray analyzer 1 acquires the analysis result of the X-rays of the standard substance in the X-ray analyzer 1. At this time, the X-ray analysis of the standard substance may be performed in the X-ray analyzer 1.

[0085] In step S202, the X-ray analyzer 1 calculates a gain adjustment value using the analysis result acquired in step S200. An example of calculation of the gain adjustment value is the calculation of "X / A" described above.

[0086] In step S204, the X-ray analysis device 1 stores the gain adjustment value calculated in step S202 in the data storage area 31B and returns the control to Figure 6 .

[0087] In the embodiment described above, the gain of the waveform used for pile-up determination (the waveform output from the second conversion filter 47) is adjusted based on individual differences between X-ray analyzers 1. Differences in the position of incidence of X-rays on the X-ray detector 12, for example, can sometimes produce a signal with a slow rise. In such cases, the amplitude of the waveform used for pile-up determination is appropriately enhanced, thereby more reliably detecting superposition peaks. Furthermore, superposition peaks caused by elements with low-energy fluorescent X-rays and by X-rays incident on the X-ray detector 12 due to scattering by the sample, etc., can be more reliably detected.

[0088] [Threshold adjustment]

[0089] In the X-ray analysis apparatus 1 , the threshold used in the accumulation determination may be changed instead of adjusting the gain of the waveform output from the second conversion filter 47 .

[0090] Due to individual differences in the X-ray analysis device 1, there are cases where Figure 3 The same specimen of waveform WF11 is made as in Figure 5 3 shows a waveform that does not have a portion exceeding the first threshold value TH11 for width determination, such as the waveform WF31 .

[0091] In this case, the X-ray analyzer 1 adjusts the threshold for peak determination (first threshold TH11 for width determination) instead of adjusting the gain of the waveform to appropriately detect the peak included in the waveform, thereby enabling appropriate accumulation determination.

[0092] Figure 8 This is a diagram for explaining an example of threshold adjustment. Figure 8 The waveform WF31 shown is Figure 5 The waveform WF shown is the same. Figure 8 In the example of FIG, the value of the first threshold value TH11 for width determination is changed to a value indicated as threshold value TH19. Thus, the waveform WF31 includes a portion exceeding threshold value TH19, and the peak in the waveform WF31 is appropriately detected.

[0093] Such threshold adjustment is similarly performed on the first threshold TH21 for interval determination.

[0094] To adjust the threshold as described above, the threshold adjustment value is calculated in the X-ray analyzer 1. An example of the threshold adjustment value is expressed as "A / X" using the energy position A determined based on the analysis results of the standard substance and the reference value X.

[0095] The accumulation detection processing unit 49 adjusts the thresholds by multiplying the first threshold TH11 for width determination and the first threshold TH21 for interval determination by the threshold adjustment value. Specifically, the adjusted thresholds are represented by the product of the first threshold TH11 for width determination and "A / X" and the product of the first threshold TH21 for interval determination and "A / X."

[0096] Figure 9 yes Figure 6 Flowchart of a modified example of the processing of . Figure 9 In the process of setting the threshold adjustment value to replace Figure 6 More specifically, Figure 9 The processing includes steps S12 and S22 to replace Figure 6 Steps S10 and S20.

[0097] In step S12, the X-ray analyzer 1 determines whether an instruction to set a threshold adjustment value has been given. If the X-ray analyzer 1 determines that an instruction to set a threshold adjustment value has been given ("YES" in step S12), the control proceeds to step S22. Otherwise ("NO" in step S12), the control proceeds to step S30.

[0098] In step S22 , the X-ray analysis apparatus 1 sets a threshold adjustment value.

[0099] Figure 10 This is a flowchart of the subroutine of step S22.

[0100] In step S220, the X-ray analyzer 1 acquires the analysis result of the X-rays of the standard substance in the X-ray analyzer 1. At this time, the X-ray analysis of the standard substance may be performed in the X-ray analyzer 1.

[0101] In step S222, the X-ray analyzer 1 calculates a threshold adjustment value using the analysis result acquired in step S200. An example of calculation of the threshold adjustment value is the calculation of "A / X" described above.

[0102] In step S224, the X-ray analysis device 1 stores the threshold adjustment value calculated in step S202 in the data storage area 31B and returns the control to Figure 9 .

[0103] Above, in reference Figure 9 and Figure 10 In the process described above, the adjustment values ​​for adjusting the first threshold value TH11 for width determination and the first threshold value TH21 for interval determination are calculated. Figure 8 As described above, the threshold value for peak detection is changed based on individual differences among the X-ray analyzers 1 .

[0104] The smaller the energy position value determined for the standard substance, the smaller the threshold adjustment value described above. Therefore, the smaller the energy position value determined for the standard substance, the smaller the threshold value adjusted using the threshold adjustment value.

[0105] [Way]

[0106] It will be understood by those skilled in the art that the above-mentioned exemplary embodiments are specific examples of the following aspects.

[0107] (Item 1) An X-ray analysis device according to one embodiment may be an X-ray analysis device comprising: an X-ray detector for detecting X-rays from a sample; a differential wave conversion unit for converting a step wave caused by the X-rays detected by the X-ray detector into a differential wave; a first conversion unit for converting the differential wave into a trapezoidal wave; a second conversion unit for converting the differential wave into a determination waveform with a peaking time shorter than a peaking time of the first conversion unit; and a pile-up determination unit for performing a pile-up determination on the determination waveform, wherein the pile-up determination unit adjusts a gain in the second conversion unit based on a numerical value related to the characteristics of the X-ray analysis device.

[0108] According to the X-ray analysis apparatus described in the first aspect, a technique for appropriately removing superimposed peaks in analysis results of the X-ray analysis apparatus is provided.

[0109] (Item 2) Another embodiment of the X-ray analysis device may be an X-ray analysis device comprising: an X-ray detector for detecting X-rays from a sample; a differential wave conversion unit for converting a step wave caused by the X-rays detected by the X-ray detector into a differential wave; a first conversion unit for converting the differential wave into a trapezoidal wave; a second conversion unit for converting the differential wave into a determination waveform with a peaking time shorter than a peaking time of the first conversion unit; and a pile-up determination unit for performing a pile-up determination on the determination waveform, wherein the pile-up determination unit adjusts one or more threshold values ​​used in the pile-up determination based on a numerical value related to the characteristics of the X-ray analysis device.

[0110] According to the X-ray analysis apparatus described in the second aspect, a technique for appropriately removing superimposed peaks in the analysis results of the X-ray analysis apparatus is provided.

[0111] (Item 3) In the X-ray analysis device described in Item 1 or Item 2, the accumulation determination may include at least one of determination based on the width of the peak in the determination waveform and determination based on the interval between the peaks in the determination waveform.

[0112] According to the X-ray analysis apparatus described in the third aspect, by performing pile-up determination in multiple aspects, it is possible to more appropriately remove superimposed peaks from the analysis results of the X-ray analysis apparatus.

[0113] (Item 4) In the X-ray analyzer according to any one of Items 1 to 3, the numerical value related to the characteristic may be based on the energy position of a standard substance in an analysis of a standard sample performed by the X-ray analyzer.

[0114] According to the X-ray analysis apparatus described in the fourth aspect, the gain or the threshold is adjusted appropriately.

[0115] (Item 5) In the X-ray analysis apparatus described in Item 4, the standard sample may be an alloy containing tin and aluminum, and the standard substance may be tin.

[0116] According to the X-ray analysis apparatus described in the fifth aspect, gain or threshold value adjustment can be appropriately performed using relatively easily available standard samples.

[0117] (Item 6) A control method for an X-ray analysis device according to one embodiment may be a control method for an X-ray analysis device, comprising the following steps: obtaining a numerical value related to a characteristic of the X-ray analysis device; and calculating an adjustment value for the gain of a determination waveform caused by X-rays of a sample detected in the X-ray analysis device based on the numerical value related to the characteristic, wherein the determination waveform is derived to perform a pile-up determination, and in the pile-up determination, the gain of the determination waveform is adjusted based on the adjustment value.

[0118] According to the control method of the X-ray analysis apparatus described in the sixth aspect, a technique for appropriately removing superimposed peaks in the analysis results of the X-ray analysis apparatus is provided.

[0119] (Item 7) Another embodiment of the control method of an X-ray analysis device may also be a control method of an X-ray analysis device, comprising the following steps: obtaining a numerical value related to a characteristic of the X-ray analysis device; and calculating an adjustment value for one or more threshold values ​​used for pile-up determination in the X-ray analysis device based on the numerical value related to the characteristic, wherein, in the pile-up determination, the adjustment value is used to adjust the one or more threshold values ​​for a determination waveform caused by X-rays of a sample detected in the X-ray analysis device.

[0120] According to the control method of the X-ray analysis apparatus described in the seventh aspect, a technique for appropriately removing superimposed peaks in the analysis results of the X-ray analysis apparatus is provided.

[0121] (Item 8) In the control method of the X-ray analysis device described in Item 7 or Item 8, the pile-up judgment may include at least one of a judgment based on the width of the peak in the judgment waveform and a judgment based on the interval of the peak in the judgment waveform.

[0122] According to the control method of the X-ray analyzer described in the eighth aspect, the pile-up determination is performed in multiple aspects, thereby making it possible to more appropriately remove superimposed peaks in the analysis results of the X-ray analyzer.

[0123] (Item 9) In the control method of an X-ray analyzer described in any one of Items 7 to 9, the numerical value related to the characteristic may be based on the energy position of a standard substance in the analysis of a standard sample performed by the X-ray analyzer.

[0124] According to the control method of the X-ray analysis device described in claim 9, the gain or the threshold is adjusted appropriately.

[0125] (Item 10) In the control method of the X-ray analysis device described in Item 9, the standard sample may be an alloy containing tin and aluminum, and the standard substance may be tin.

[0126] According to the control method of the X-ray analyzer described in the tenth aspect, the gain or threshold value can be appropriately adjusted using relatively easily available standard samples.

[0127] (Item 11) The program according to one aspect may be executed by one or more processors of a computer to cause the computer to implement the method for controlling an X-ray analysis device according to any one of Items 6 to 10.

[0128] According to the program described in the eleventh item, a technique for appropriately removing superimposed peaks in analysis results of an X-ray analysis apparatus is provided.

[0129] The embodiments disclosed herein should be considered in all respects to be illustrative and non-restrictive. The scope of this disclosure is not indicated by the description of the embodiments described above but by the claims, and is intended to include all modifications within the meaning and scope equivalent to the claims. In addition, each technique in the embodiments is intended to be implemented independently or in combination with other techniques in the embodiments as needed.

[0130] Description of Reference Numerals

[0131] 1: X-ray analyzer; 10: X-ray tube; 12: X-ray detector; 14: preamplifier; 16: differential circuit; 18: amplifier; 20: ADC.

Claims

1. An X-ray analysis device comprising: an X-ray detector for detecting X-rays from the sample; a differential wave conversion unit that converts a step wave caused by the X-ray detected by the X-ray detector into a differential wave; a first conversion unit, which converts the differential wave into a trapezoidal wave; a second conversion unit that converts the differential wave into a determination waveform with a peaking time shorter than that of the first conversion unit; and a pile-up determination unit configured to perform pile-up determination on the determination waveform; in, The pile-up determination unit adjusts the gain in the second conversion unit based on a numerical value related to characteristics of the X-ray analysis device.

2. An X-ray analysis device comprising: an X-ray detector for detecting X-rays from the sample; a differential wave conversion unit that converts a step wave caused by the X-ray detected by the X-ray detector into a differential wave; a first conversion unit, which converts the differential wave into a trapezoidal wave; a second conversion unit that converts the differential wave into a determination waveform with a peaking time shorter than that of the first conversion unit; and a pile-up determination unit configured to perform pile-up determination on the determination waveform; in, The accumulation determination unit adjusts one or more threshold values ​​used in the accumulation determination based on a numerical value related to characteristics of the X-ray analysis device.

3. The X-ray analysis device according to claim 1 or 2, wherein: The accumulation determination includes at least one of determination based on a width of a peak in the determination waveform and determination based on an interval between peaks in the determination waveform.

4. The X-ray analysis device according to claim 1 or 2, wherein: The numerical values ​​related to the characteristics are based on the energy position of the standard substance in the analysis of the standard sample by the X-ray analyzer.

5. The X-ray analysis device according to claim 4, wherein The standard sample is an alloy containing tin and aluminum, The standard substance is tin.

6. A method for controlling an X-ray analysis device, comprising the following steps: acquiring numerical values ​​related to characteristics of the X-ray analysis device; and Based on the numerical value related to the characteristic, an adjustment value of the gain of the determination waveform caused by the X-rays of the sample detected in the X-ray analyzer is calculated; wherein the determination waveform is derived to perform a pile-up determination, In the deposition determination, the gain of the determination waveform is adjusted based on the adjustment value.

7. A method for controlling an X-ray analysis device, comprising the following steps: acquiring numerical values ​​related to characteristics of the X-ray analysis device; and calculating, based on the numerical value related to the characteristic, an adjustment value for one or more threshold values ​​used for pile-up determination in the X-ray analysis device; Here, in the deposition determination, the one or more threshold values ​​are adjusted using the adjustment value with respect to a waveform for determination caused by X-rays of a sample detected by the X-ray analyzer.

8. The method for controlling an X-ray analysis device according to claim 6 or 7, wherein: The accumulation determination includes at least one of determination based on a width of a peak in the determination waveform and determination based on an interval between peaks in the determination waveform.

9. The X-ray analysis device according to claim 1 or 2, wherein: The numerical values ​​related to the characteristics are based on the energy position of the standard substance in the analysis of the standard sample by the X-ray analyzer.

10. The control method of an X-ray analysis device according to claim 9, wherein: The standard sample is an alloy containing tin and aluminum, The standard substance is tin. 11 . A program that, when executed by one or more processors of a computer, causes the computer to implement the control method of the X-ray analysis device according to claim 6 or 7 .

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