Data processing method, analysis system, and program
By calculating the correction ratio and correction value in fluorescence X-ray analysis, the problem of accurately obtaining the Co content was solved, and the accurate determination of the Co content was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHIMADZU SEISAKUSHO LTD
- Filing Date
- 2024-10-07
- Publication Date
- 2026-05-05
AI Technical Summary
In the field of pharmaceutical analysis, the Kα peak of Co overlaps with the Kβ peak of Fe, making it difficult to accurately determine the Co content. Existing technologies have failed to effectively correct the spectrum to solve this problem.
The Co content is determined by calculating the correction intensity by reading the correction ratio, calculating the correction value, and subtracting the correction value from the detection intensity in the first energy range of the spectrum. The correction ratio is based on the ratio of the detection intensity of the Kβ line energy of the Fe standard sample to the Kα line energy of the Co sample.
This method enables accurate determination of Co content in fluorescence X-ray analysis, solving the problem of difficulty in accurately obtaining Co content.
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Figure CN121986258A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to data processing for processing spectra obtained by energy-dispersive fluorescence X-ray analysis. Background Technology
[0002] It is known that in the spectrum obtained by energy-dispersive X-ray fluorescence analysis (hereinafter referred to as "EDX"), the peaks of the analyte element overlap with the peaks of other elements, so even if the peak intensity of the analyte element is used directly, the accurate content of the analyte element cannot be obtained.
[0003] In response to this situation, Japanese Patent Application Publication No. 2004-138604 (Patent Document 1) proposes a technique for correcting the spectrum based on the combination of elements of the analyte with a portion of other elements.
[0004] Existing technical documents Patent documents Patent Document 1: Japanese Patent Application Publication No. 2004-138604 Summary of the Invention The technical problem that the invention aims to solve In recent years, the application of EDX in pharmaceutical analysis has been explored. In pharmaceutical analysis, obtaining the accurate content of cobalt (Co) in the analyte sample is crucial. Furthermore, iron (Fe) is frequently found in the analyte samples in pharmaceutical analysis.
[0005] The Kα energy of Co (6.92 keV) is close to that of Fe (7.06 keV). In the spectra obtained from fluorescence X-ray analysis, the Kα peak of Co overlaps with the Kβ peak of Fe. However, in previous studies on obtaining Co content, the use of Fe peaks to correct the spectrum has not been specifically explored. Therefore, especially in the field of pharmaceutical analysis, a technique that considers Fe peaks to correct the spectrum is needed to obtain accurate Co content.
[0006] The present invention was conceived in view of the above facts, and its purpose is to provide a technique for deriving the accurate content of Co in a sample in fluorescence X-ray analysis.
[0007] Solution to the above technical problems According to one aspect of this disclosure, a data processing method for processing the spectrum of a target sample obtained in an energy-dispersive fluorescence X-ray analyzer includes the following steps: reading a correction ratio, which is the ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard sample of Fe, the first energy range including the Kβ line energy of Fe and the Kα line energy of Co, and the second energy range including the Kα line energy of Fe; calculating the product of the correction ratio and the detection intensity in the second energy range of the spectrum as a correction value; and calculating the correction intensity by subtracting the correction value from the detection intensity in the first energy range of the spectrum.
[0008] According to one aspect of the present disclosure, the analysis system includes an energy-dispersive X-ray fluorescence analyzer and an information processing device configured to analyze the spectrum of a target sample in the energy-dispersive X-ray fluorescence analyzer. The information processing device reads a correction ratio, which is the ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard sample of Fe. The first energy range includes the Kβ line energy of Fe and the Kα line energy of Co, and the second energy range includes the Kα line energy of Fe. The information processing device calculates the product of the correction ratio and the detection intensity in the second energy range of the spectrum as a correction value, and calculates the correction intensity by subtracting the correction value from the detection intensity in the first energy range of the spectrum.
[0009] According to one aspect of the procedure disclosed herein, the computer performs the above-described data processing method by means of execution by the computer.
[0010] Invention Effects According to this disclosure, a technique is provided for deriving the accurate content of Co in a sample in fluorescence X-ray analysis. Attached Figure Description
[0011]
【 Figure 1 The figure shown is an example of the spectrum of a Fe and Co mixed sample obtained by energy-dispersive fluorescence X-ray diffraction analysis.
[0012]
【 Figure 2 The figure shown is an example of the spectrum of a Fe standard sample obtained by energy-dispersive fluorescence X-ray diffraction analysis.
[0013]
【 Figure 3 The diagram is a rough representation of the overall structure of an analytical system that includes an energy-dispersive fluorescence X-ray analyzer.
[0014]
【 Figure 4 The diagram shows the hardware configuration of the information processing device 20.
[0015]
【 Figure 5This is a flowchart of the process performed to determine the Co content in an analyte sample from the spectrum obtained by energy-dispersive fluorescence X-ray diffraction analysis.
[0016]
【 Figure 6 The diagram above is an example of a data structure representing a calibration scale table that contains multiple calibration scales.
[0017]
Figure 7
[0018] Hereinafter, embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. Furthermore, identical or equivalent parts in the drawings will be labeled with the same symbols, and their descriptions will not be repeated.
[0019] [Summary of this disclosure] Figure 1 This is an example of a spectrum of a Fe and Co mixed sample obtained by energy-dispersive fluorescence X-ray diffraction analysis.
[0020] exist Figure 1 In the graph, the horizontal axis represents energy, and the vertical axis represents detection intensity. Waveform W10 represents an example of the spectrum of a sample containing a mixture of Fe and Co. Figure 1 In this context, "FeKa", "CoKa", "FeKb", and "CoKb" represent the energies of the characteristic X-rays of "Fe's Kα", "Co's Kα", "Fe's Kβ", and "Co's Kβ", respectively.
[0021] exist Figure 1 In the waveform W10, there are two peaks, P11 and P12. The profile of peak P12 (detection intensity at the peak, peak width, etc.) is based on Fe's Kα.
[0022] The characteristic X-ray energy of "Co's Kα" (6.92 keV) is close to that of "Fe's Kβ" (7.06 keV). Therefore, the profile of peak P11 is primarily based on Fe's Kβ, but is also influenced by Co's Kα. That is, not only does the Fe content in the sample affect the profile of peak P11, but the Co content also influences it. Therefore, based solely on... Figure 1 It is difficult to accurately determine the Co content from the spectrum shown.
[0023] In this disclosure, a parameter called "correction ratio" is derived using the spectrum of a standard sample containing Fe but not Co. Furthermore, the "correction ratio" is applied to, for example... Figure 1 The spectrum shown is used to derive a new value for determining the Co content. Figure 1The two regions AR1 and AR2 within will be described later in the section on the correction ratio.
[0024] [Correction ratio] Figure 2 This is an example of a spectrum of a Fe standard sample obtained by energy-dispersive fluorescence X-ray diffraction analysis. The standard sample was prepared with a Fe concentration in the range of 20–800 ppm, typical of samples used in pharmaceutical analysis. The Fe concentration in the standard sample was quantified, for example, by the fundamental parameter method (FP method).
[0025] exist Figure 2 In the diagram, waveform W20 represents an example of the spectrum of a standard Fe sample. Waveform W21 represents the intensity of the background created for waveform W20. The background intensity is derived, for example, using the Statistically Sensitive Non-linear Iterative Peak Clipping (SNIP) algorithm. For information on the SNIP algorithm, see, for example, Background elimination using the SNIP algorithm for Bragg reflections from a protein crystal measured by a TOF single-crystal neutrondiffractometer (link: https: / / iopscience.iop.org / article / 10.1088 / 1742-6596 / 664 / 7 / 072049 / pdf#:~:text=The%20statistics%2Dsensitive%20non%2Dlinear,the%20background%20under%20a%20peak.).
[0026] Figure 2 Peaks P21 and P22 correspond to Figure 1 Peaks P11 and P12. However, due to Figure 2 The standard sample does not contain Co, therefore Figure 2 Peak P21 is not affected by the Co content in the standard sample.
[0027] exist Figure 2In this model, region AR1 is predefined as the region containing peak P21. Region AR2 is predefined as the region containing peak P22. Region AR1 is, for example, set to 6.72–7.26 keV, but is not limited to this range as long as it contains the characteristic X-ray energy of Fe Kβ. Region AR2 is, for example, set to 6.17–6.62 keV, but is not limited to this range as long as it contains the characteristic X-ray energy of Fe Kα.
[0028] In this disclosure, the value obtained by dividing the peak area of region AR1 by the peak area of region AR2 is calculated as a "correction ratio".
[0029] [Quantitative analysis of Co] In this disclosure, when the analyte sample contains not only Co but also Fe, the Co content in the analyte sample is determined by using a standard curve of Co, the spectrum of the analyte sample, and the aforementioned correction ratio.
[0030] More specifically, suppose we obtain as follows Figure 1 The spectrum shown is the spectrum of the sample being analyzed. In this case, the integral value of the detection intensity in region AR1 and the integral value of the detection intensity in region AR2 are calculated first. Figure 1 Regions AR1 and AR2 in the diagram represent the regions AR1 and AR2 respectively. Figure 2 Regions AR1 and AR2 in the spectrum have the same energy range. In calculating the integral value of the detection intensity, the spectral background can be determined, and the value obtained by subtracting the background intensity from the detection intensity can be used to replace the detection intensity.
[0031] Next, the product of the region AR2 calculated as described above and the aforementioned correction ratio is calculated. The calculated value constitutes an example of the "correction value" in this disclosure.
[0032] Next, the value obtained by subtracting the aforementioned "correction value" from the integral value of the detected intensity in region AR1 of the above spectrum is calculated. The value obtained in this way constitutes an example of the "correction intensity" in this forging process.
[0033] In this disclosure, a standard curve for Co is prepared in advance. Then, in the Co standard curve, the product of the concentration corresponding to the above-mentioned "correction intensity" and the volume of the analyte sample is calculated as the Co content in the analyte sample.
[0034] [Energy-dispersive fluorescence X-ray analysis system] Figure 3 This is a diagram that roughly illustrates the overall configuration of an analytical system including an energy-dispersive fluorescence X-ray analyzer. The fluorescence X-ray analyzer system 100 includes a fluorescence X-ray analyzer 10, an information processing unit 20, a display 40, and an input unit 34.
[0035] The fluorescence X-ray analysis device 10 is an energy-dispersive fluorescence X-ray analysis device for measuring the concentration of elements contained in a sample S. It consists of a sample chamber 1 and a measurement chamber 5. The space inside the sample chamber 1 and the measurement chamber 5 is hermetically enclosed by a shell 3, which can maintain a vacuum inside as needed.
[0036] The sample chamber 1 has a sample stage 2 at its bottom. An opening 4 is formed on the sample stage 2. The sample S is placed on the sample stage 2 to cover the opening 4. The sample S is placed on the sample stage 2 such that the measurement position is exposed from the opening 4.
[0037] The XY platform 14 is configured to move the sample S along the in-plane direction of the sample stage 2. The drive mechanism 15 can drive the XY platform 14 to move along two mutually perpendicular axes in the in-plane. This allows for automatic adjustment of the measurement position of the sample S.
[0038] The measuring chamber 5 has an X-ray tube 7 and a detector 8 mounted on its wall 6. The X-ray tube 7 irradiates the sample S with primary X-rays. The X-ray tube 7 has a filament that emits thermionic electrons and a target that converts the thermionic electrons into predetermined primary X-rays for emission. The primary X-rays emitted from the X-ray tube 7 irradiate the measurement position of the sample S through the opening 4. Secondary X-rays (fluorescent X-rays) emitted by the sample S are incident on the detector 8, and the energy and intensity of the fluorescent X-rays are measured.
[0039] A shutter 9, a primary X-ray filter 11, a collimator 13, and an imaging unit 16 are installed in the measuring chamber 5. The shutter 9, the primary X-ray filter 11, and the collimator 13 are configured by a drive mechanism 12 to operate perpendicular to the x-ray beam. Figure 1 Slide it along the direction of the paper.
[0040] The shutter 9 is made of X-ray absorbing material such as lead, and can be inserted into the optical path of a primary X-ray to shield it when needed.
[0041] The primary X-ray filter 11 is formed of a metal foil selected according to the purpose. It can attenuate the background components in the primary X-rays emitted from the X-ray tube 7 and improve the signal-to-noise ratio (S / N ratio) of the necessary characteristic X-rays. In the actual device, multiple primary X-ray filters 11 formed of different types of metals are used. The primary X-ray filter 11 selected according to the purpose is inserted into the optical path of the primary X-ray by the drive mechanism 12.
[0042] Collimator 13 is a centrally located circular aperture that determines the size of the primary X-ray beam irradiating sample S. Collimator 13 is made of X-ray absorbing materials such as lead or brass. In actual setups, multiple collimators 13 with different aperture diameters are positioned perpendicular to the X-ray beam. Figure 1The paper planes are arranged side by side, and the collimator 13, selected according to the purpose, is inserted into the beam line of a primary X-ray by the drive mechanism 12.
[0043] An imaging unit 16 is disposed in the lower part of the measurement chamber 5. The imaging unit 16 is configured to image the measurement position of the sample S through an opening 4 formed on the sample stage 2. The imaging unit 16 includes an image sensor divided into multiple pixels, such as a CMOS (Complementary Metal-Oxide-Semiconductor) or CCD (Charge-Coupled Device). The image data of the imaging unit 16 is transmitted to the information processing device 20.
[0044] Figure 4 This is a diagram showing the hardware configuration of the information processing device 20.
[0045] The information processing device 20 is mainly composed of a CPU (Central Processing Unit) 22, which serves as the arithmetic processing unit. For example, a personal computer can be used as the information processing device 20.
[0046] The information processing device 20 also has a storage unit for non-temporarily storing programs and data. The information processing device 20 executes programs via CPU 22 and performs operations according to those programs. The storage unit includes ROM (Read Only Memory) 24, RAM (Random Access Memory) 26, and HDD (Hard Disk Drive) 30. Furthermore, specific examples of the storage unit are not limited to these.
[0047] The information processing device 20 also has an I / O (Input / Output) interface 28 and a communication interface 32. The communication interface 32 is the interface used by the information processing device 20 to communicate with external devices, including the fluorescence X-ray analysis device 10. The I / O interface 28 is the interface for inputting to or outputting from the information processing device 20. For example... Figure 2 As shown, the I / O interface 28 is connected to the input section 34 and the display 40. The input section 34, for example, is a keyboard and / or mouse, and receives input including instructions from the user to the information processing device 20.
[0048] return Figure 1 In addition to the input unit 34 and the display 40, the information processing device 20 is also connected to an X-ray tube 7, a detector 8 and an imaging unit 16.
[0049] The information processing device 20 controls the fluorescence X-ray analysis device 10 based on the measurement conditions input through the input unit 34. Specifically, the information processing device 20 controls the tube voltage, tube current, and irradiation time in the X-ray tube 7, and drives the shutter 9, the primary X-ray filter 11, and the collimator 13 respectively.
[0050] During measurement, the information processing device 20 acquires the spectrum of the secondary X-rays detected by the detector 8. Based on the spectrum of the secondary X-rays detected by the detector 8, the information processing device 20 performs quantitative analysis on each element.
[0051] The information processing device 20 also controls the imaging unit 16 and automatically detects the measurement position of the sample S based on the image data acquired by the imaging unit 16 before measurement. The information processing device 20 also selects the collimator 13 with the most suitable aperture from a plurality of collimators 13 for the detected measurement position. In addition to displaying the image of the sample S captured by the imaging unit 16, the display 40 can also display a report format created by the information processing device 20.
[0052] [Processing Flow] Figure 5 This is a flowchart illustrating the process performed to determine the Co content in an analyte sample based on the spectrum of the sample obtained using energy-dispersive X-ray fluorescence analysis. The HDD30 stores a program that enables a computer to perform the process shown in the flowchart. In the fluorescence X-ray analysis system 100, the CPU22 executes this program to perform the process. Figure 5 The processing can also be performed by storing the above-mentioned program in a storage device external to the fluorescence X-ray analysis system 100 and accessing that storage device via the CPU 22. Figure 5 The processing.
[0053] In the fluorescence X-ray analysis system 100, the spectrum of a standard Fe sample is acquired in the fluorescence X-ray analysis device 10, and then the aforementioned "correction ratio" is calculated using this spectrum. The "correction ratio" is stored, for example, in an HDD 30. The HDD 30 also stores information determining the standard curve for Co, and information determining the energy ranges of regions AR1 and AR2. In the following description, the energy range of region AR1 is sometimes referred to as the "first energy range," and the energy range of region AR2 is sometimes referred to as the "second energy range."
[0054] In one implementation example, Figure 5 The processing begins when the spectrum of the analyte sample is acquired in the fluorescence X-ray analysis device 10, and an instruction for determining the Co content in the analyte sample is input to the information processing device 20 via the input unit 34. The following explanation follows. Figure 5 The processing flow.
[0055] In step S10, the fluorescence X-ray analysis system 100 reads the spectrum of the sample to be analyzed. Furthermore, the spectrum of the sample to be analyzed is stored in HDD 30 after being acquired by the fluorescence X-ray analysis device 10. In step S10, the spectrum is read from HDD 30.
[0056] In step S20, the fluorescence X-ray analysis system 100 reads the “correction ratio” from the HDD30.
[0057] In step S30, the fluorescence X-ray analysis system 100 determines the integral values of the detection intensity of the "first energy range" and the "second energy range" from the spectrum read in step S10.
[0058] In step S40, the fluorescence X-ray analysis system 100 calculates the product of the integral value of the detection intensity of the "second energy range" and the "correction ratio" as the "correction value".
[0059] In step S50, the fluorescence X-ray analysis system 100 calculates the value of "correction ratio" as the integral value of the detection intensity in the "first energy range" minus the "correction ratio".
[0060] In step S60, the fluorescence X-ray analysis system 100 determines the Co content in the analyte sample based on the "corrected intensity" and the Co standard curve. The fluorescence X-ray analysis system 100 can display the determined Co content on the display 40. Afterwards, the fluorescence X-ray analysis system 100 terminates. Figure 5 The processing.
[0061] As described above, in this disclosure, to determine the Co content in the analyte sample, a "calibration ratio" calculated for a standard sample of Fe is used. The "calibration ratio" is a value obtained by dividing the detection intensity of a first energy range containing the characteristic X-ray range of Fe and Co by the detection intensity of a second energy range containing the characteristic X-ray range of Fe but not Co. Furthermore, the product of the detection intensity of the second energy range of the analyte sample and the "calibration ratio" is calculated as a "calibration value," and the value obtained by subtracting the "calibration value" from the detection intensity of the first energy range of the analyte sample is calculated as a "calibration intensity." Then, in the Co standard curve, the product of the concentration corresponding to the "calibration intensity" and the amount of the analyte sample is determined as the Co content in the analyte sample.
[0062] In “Corrected Intensity”, the detection intensity caused by Fe characteristic X-rays has been removed within the energy range that includes Fe and Co characteristic X-rays.
[0063] Therefore, according to this disclosure, the accurate Co content in the analyte sample can be derived in fluorescence X-ray analysis.
[0064] [Variation Example] The "calibration ratio" disclosed herein can be set for each of the various Fe content rates in a sample. Furthermore, the "calibration ratio" can also be set separately for each parent material of various samples. When determining the Co content in the analyte sample, the user can specify the desired Fe content rate of the analyte sample. The user can also specify the desired material as the parent material of the analyte sample. Figure 5 The processing can be changed to utilize a specific correction ratio selected according to these specifications from a variety of "correction ratios".
[0065] Figure 6 This is a diagram illustrating an example of a data structure for a calibration scale table containing multiple calibration scales. In one implementation example, the calibration scale table is stored in HDD30.
[0066] like Figure 6 As shown, the calibration ratio table contains eight calibration ratio values set for four Fe concentrations and two base materials. For example, the calibration ratio for Fe concentrations between 200 ppm and 600 ppm, and for a base material that is an aqueous solution, is shown as "CV21". Each of these eight calibration ratios is a specific example of a calibration ratio candidate. The calibration ratio to be used is selected from these eight candidates.
[0067] Figure 6 Each of the eight calibration ratios shown was created based on the spectra of standard samples with corresponding Fe concentrations and base materials. For example, in the standard sample used to create "CV21", the Fe concentration was in the range of 200 ppm or higher and less than 600 ppm, and the base material was an aqueous solution.
[0068] The first and second energy ranges used in the calculation of the correction ratio and the determination of the Co content can be changed according to the type of correction ratio used.
[0069] For example, when using a correction ratio corresponding to a high Fe concentration, the first energy range and / or the second energy range can be further expanded compared to a correction ratio corresponding to a low Fe concentration. More specifically, regarding the case where the parent material is an aqueous solution, for a correction ratio corresponding to an Fe concentration of 200 ppm or more but less than 600 ppm, the second energy range is set to 6.17–6.62 keV; for a correction ratio corresponding to an Fe concentration of 1000 ppm or more, the second energy range is set to 6.09–6.68 keV.
[0070] Figure 7 yes Figure 5 The flowchart shows a variation of the processing. Figure 7 processing and Figure 5 Compared to the previous processing, it also includes the control of steps S12 to S16.
[0071] More specifically, after reading the spectrum of the sample to be analyzed in step S10, the fluorescence X-ray analysis system 100 advances the control to step S12.
[0072] In step S12, the fluorescence X-ray analysis system 100 acquires the base material specification from the user. In one implementation example, the user uses the input unit 34 to specify the type of base material to be used in the sample to be analyzed.
[0073] In step S14, the fluorescence X-ray analysis system 100 acquires a specified Fe concentration range from the user. In one implementation example, the user uses input unit 34 to specify a range containing the desired Fe concentration in the sample to be analyzed.
[0074] In step S16, the fluorescence X-ray analysis system 100 selects one of multiple calibration ratios from a calibration ratio table based on the base material type and Fe concentration range specified by the user. Then, the fluorescence X-ray analysis system 100 proceeds to step S20. In step S20, the value of the calibration ratio selected in step S16 is read. Furthermore, if the fluorescence X-ray analysis system 100 fails to obtain the user's specification of the base material type and / or Fe concentration, a default type and / or range can be used when selecting a calibration ratio.
[0075] According to this modified example, the "calibration ratio" is a value derived from a standard sample prepared under conditions identical to the expected parent material and / or Fe concentration range of the analyte. Therefore, the Co content in the analyte sample can be determined more accurately in the fluorescence X-ray analysis system 100.
[0076] [plan] Those skilled in the art should understand that the above-described exemplary embodiments are specific examples of the following solutions.
[0077] (Item 1) A data processing method according to one scheme is a data processing method for processing the spectrum of an object sample obtained in an energy-dispersive fluorescence X-ray analyzer, comprising: a step of reading a correction ratio, said correction ratio being a ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard sample of Fe, the first energy range including the Kβ line energy of Fe and the Kα line energy of Co, and the second energy range including the Kα line energy of Fe; a step of calculating the product of said correction ratio and the detection intensity in the second energy range of the spectrum as a correction value; and a step of calculating the correction intensity by subtracting the correction value from the detection intensity in the first energy range of the spectrum.
[0078] According to the data processing method described in item 1, a technique is provided for deriving the accurate content of Co in a target sample in fluorescence X-ray analysis.
[0079] (Item 2) The data processing method described in Item 1 may further include the step of determining the Co content in the object sample using the correction intensity and the standard curve of Co.
[0080] According to the data processing method described in item 2, a specific technique for deriving Co content is provided.
[0081] (Item 3) In the data processing method described in Item 2, the Fe concentration in the standard sample may also be 50 to 800 ppm.
[0082] According to the data processing method described in item 3, the value derived from a standard sample having the Fe concentration in a general sample can be used as a correction ratio.
[0083] (Item 4) The data processing method of any one of items 1 to 3 may further include: receiving a specified Fe concentration corresponding to the object sample; and selecting, according to the specified, a correction ratio from two or more correction ratio candidates prepared for each of two or more Fe concentrations.
[0084] According to the data processing method described in item 4, a correction ratio corresponding to the expected Fe concentration in the target sample can be selected from two or more correction ratio candidates and used to derive the Co content.
[0085] (Item 5) According to an analysis system, an energy-dispersive fluorescence X-ray analyzer is provided, and an information processing device is configured to analyze the spectrum of a target sample in the energy-dispersive fluorescence X-ray analyzer. The information processing device reads a correction ratio, which is the ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard sample of Fe. The first energy range includes the Kβ line energy of Fe and the Kα line energy of Co, and the second energy range includes the Kα line energy of Fe. The information processing device calculates the product of the correction ratio and the detection intensity in the second energy range of the spectrum as a correction value, and calculates the correction intensity by subtracting the correction value from the detection intensity in the first energy range of the spectrum.
[0086] According to the analytical system described in item 5, a technique is provided for deriving the accurate content of Co in a target sample in fluorescence X-ray analysis.
[0087] (Item 6) In the analytical system described in Item 5, the information processing device may also use the correction intensity and the standard curve of Co to determine the Co content in the object sample.
[0088] According to the analytical system described in item 6, a specific technique for deriving Co content is provided.
[0089] (Item 7) In the analytical system described in Item 5 or Item 6, the Fe concentration in the standard sample may also be 50 to 800 ppm.
[0090] According to the analytical system described in item 3, the value derived from a standard sample having the Fe concentration in a typical sample can be used as a calibration ratio.
[0091] (Item 8) In the analytical system of any one of items 5 to 7, the information processing device may also receive a specification of the Fe concentration corresponding to the object sample, and select the correction ratio from two or more correction ratio candidates prepared for each of two or more Fe concentrations according to the specification.
[0092] According to the analytical system described in item 8, a correction ratio corresponding to the expected Fe concentration in the target sample can be selected from two or more correction ratio candidates and used to derive the Co content.
[0093] (Item 9) According to a procedure of one scheme, the computer can perform the above data processing method by execution by the computer.
[0094] According to the procedure described in item 9, a technique is provided for deriving the accurate content of Co in a sample in fluorescence X-ray analysis.
[0095] The embodiments disclosed herein should be considered illustrative rather than limiting in all respects. The scope of this disclosure is defined not by the description of the embodiments above but by the scope of the claims, and is intended to include all modifications within the meaning and scope of the claims. Furthermore, the techniques in the embodiments are intended to be implemented individually or, where possible, in combination with other techniques in the embodiments as needed.
[0096] Explanation of reference numerals in the attached figures 1 Sample chamber, 2 Sample stage, 3 Housing, 10 Fluorescence X-ray analysis device, 11 Primary X-ray filter, 20 Information processing device, 100 Fluorescence X-ray analysis system, A2, AR1, AR2 regions, P11, P12, P21, P22 peaks, W10, W20, W21 waveforms.
Claims
1. A data processing method for processing the spectrum of an object sample obtained in an energy-dispersive fluorescence X-ray analyzer, characterized in that, include: The step of reading the calibration ratio is a ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard sample of Fe. The first energy range includes the Kβ line energy of Fe and the Kα line energy of Co, and the second energy range includes the Kα line energy of Fe. The step of calculating the product of the correction ratio and the detection intensity in the second energy range of the spectrum as the correction value; and The step of calculating the correction intensity by subtracting the correction value from the detected intensity in the first energy range of the spectrum.
2. The data processing method as described in claim 1, characterized in that, It also includes the step of determining the Co content in the object sample using the correction intensity and the standard curve of Co.
3. The data processing method as described in claim 1, characterized in that, The Fe concentration in the standard sample is 50–800 ppm.
4. The data processing method as described in claim 1, characterized in that, Also includes: The specified step corresponds to the Fe concentration of the object sample; as well as The step of selecting the correction ratio from two or more correction ratio candidates prepared for each of two or more Fe concentrations, as specified.
5. An analysis system, characterized in that, have: Energy-dispersive fluorescence X-ray analyzer; and An information processing device configured to analyze the spectrum of a target sample in the energy-dispersive fluorescence X-ray analyzer. The information processing device reads the correction ratio, which is the ratio of the detection intensity in a first energy range to the detection intensity in a second energy range for a standard Fe sample. The first energy range includes the Kβ line energy of Fe and the Kα line energy of Co. The second energy range includes the Kα line energy of Fe. Furthermore, the information processing device is configured to calculate the product of the correction ratio and the detection intensity of the second energy range of the spectrum as the correction value. The correction intensity is calculated by subtracting the correction value from the detected intensity in the first energy range of the spectrum.
6. The analysis system as described in claim 5, characterized in that, The information processing device is configured to determine the Co content in the object sample using the correction intensity and the standard curve of Co.
7. The analysis system as described in claim 5, characterized in that, The Fe concentration in the standard sample is 50–800 ppm.
8. The analysis system as described in claim 5, characterized in that, The information processing device receives a specification corresponding to the Fe concentration of the object sample. And, according to the specified designation, the correction ratio is selected from two or more correction ratio candidates prepared for each of the two or more Fe concentrations.
9. A program, characterized in that, The computer performs the data processing method of claim 1 by means of execution by the computer.
Citation Information
Patent Citations
Fluorescence x-ray analyzer
JP2004138604A