Luminescence analyzer

Abstract

The present invention provides a luminescence analysis device for performing a rapid and accurate luminescence analysis by a plurality of analyses. A control unit of a luminescence analysis device (1) selects one priority element from a plurality of elements, sets a management range, which is a range of content rates, for each of the plurality of elements, measures a plurality of positions of a sample a plurality of times, acquires detection intensities relating to the plurality of elements during each measurement, calculates the content rates of the respective elements from the detection intensities of the respective elements, and determines the content rates of the respective elements based on the calculated content rates. The difference between the content rates of the two measurements among the plurality of measurements is calculated for the priority element, and if the difference is within the management range, whether the difference between the content rates of the two measurements for each element is within the management range is determined, and if the difference is within the management range, the difference between the content rates of the two measurements for each element is within the management range. When the difference between the content ratios of each element measured twice is within the management range of each element, the average value of the content ratios of each element measured twice is calculated as a representative value and output.

Description

Technical Field

[0001] The present disclosure relates to a luminescence analysis device. Background Art

[0002] There are known luminescence analysis methods and devices (JP2020-91139A1) for performing compositional analysis of a solid sample by causing discharge between a solid sample and an opposing electrode and analyzing the generated light. The luminescence analysis method and device are used for process management in factories manufacturing metal products. Summary of the Invention

[0003] [Problems to be Solved by the Invention]

[0004] In the manufacturing process of metal products, rapid and accurate compositional analysis of samples is required. In luminescence analysis, compositional analysis is usually performed at multiple positions of the same sample, and the average value is used as a representative value. However, the composition distribution in the sample is not necessarily uniform, and there are cases where the analysis values are distributed according to the analysis positions. Therefore, when calculating the average value to obtain the representative value, it is preferable to calculate the average value by selecting measurement values with relatively small differences after excluding outliers.

[0005] The inventors of the present invention have found that: an analyst who uses a luminescence analysis device to perform compositional analysis of a metal product empirically grasps the important elements in the composition of the metal from among multiple elements that are the objects of compositional analysis. Initially, focusing on the difference in the content rates of the important elements, the position of the outlier is judged by comparing the difference in the content rates of the important elements at two measurement points with the management range. In addition, the compositional distribution is calculated based on the measurement result of the measurement point with the smallest difference in the content rates of the important elements among the measurement results of the measurement points that are not outliers, and thus it is easy to obtain a result with less deviation.

[0006] Therefore, the object of the luminescence analysis device of the present invention is to: by embodying in the device the method of calculating the compositional distribution that such an analyst silently performs, even a person who is not used to using a luminescence analysis device can easily obtain a result with less deviation.

[0007] In addition, when the measurement positions are three or more and compositional analysis values that are judged to be normal measurements (not outlier values) are obtained at two or more measurement positions by comparing the content rates of multiple elements obtained from the luminescence spectroscopy results at each measurement position with the management range, the result with the smallest deviation of the priority elements is output as the compositional analysis value of the sample.

[0008] [Technical Means for Solving the Problems]

[0009] A first aspect of the present invention is a luminescence analysis device, comprising:

[0010] A sample setting table forms a discharge chamber inside for introducing gas to perform discharge, and includes an opening that is grounded to the discharge chamber and is configured to place a sample;

[0011] Opposing electrodes are arranged at the ends in the discharge chamber, and a voltage is applied between the electrodes and the sample to generate discharge;

[0012] A spectroscope decomposes the light generated by the discharge;

[0013] Multiple detectors detect the light of each wavelength decomposed by the spectroscope; and

[0014] A control unit controls the voltage applied between the sample and the opposing electrodes, and processes the measurement data detected by the detectors to calculate the content rate of elements.

[0015] In the control unit,

[0016] One priority element is selected from multiple elements that are the object of component analysis of the sample, and a range of content rates, that is, a management range, is set for each of the multiple elements that are the object of component analysis of the sample.

[0017] The sample is measured multiple times at multiple positions. In each measurement, the detection intensities related to multiple elements are obtained, and the content rate of each element is calculated based on the detection intensity of each element.

[0018] For the priority element, the difference in the content rates of two measurements within multiple measurements is calculated. When the difference is within the management range,

[0019] For all elements for which a management range is set, it is determined whether the difference in the content rates of the two measurements of each element is within the management range.

[0020] For all elements for which a management range is set, when the difference in the content rates of the two measurements of each element is within the management range of each element,

[0021] The average value of the content rates of the two measurements of each measured element is calculated as a representative value and output.

[0022] In addition, in the present disclosure, the difference in the content rates of two measurements refers to the absolute value and cannot take a negative value.

[0023] [Effects of the Invention]

[0024] By preferentially processing the measurement results of one selected element when calculating the representative analysis value of the sample, the luminescence analysis device of the present disclosure can easily obtain results with less deviation. Description of the Drawings

[0025] Figure 1It is a schematic diagram of the entire luminescence analysis device 1 of the first embodiment.

[0026] Figure 2 It is a diagram showing the first position 1A, the second position 2B, the third position 3C, and the fourth position 4D on the surface of the cylindrical specimen S facing the discharge chamber 11.

[0027] Figure 3 It is a diagram schematically showing calibration curve data (a diagram showing the relationship between the detection intensity and the content rate).

[0028] Figure 4 It is a flowchart showing the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0029] Figure 5 It shows following Figure 4 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0030] Figure 6 It shows following Figure 5 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0031] Figure 7 It shows following Figure 6 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0032] Figure 8 It shows following Figure 7 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0033] Figure 9 It shows following Figure 8 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0034] Figure 10 It shows following Figure 9 A flowchart of the analysis method of a specimen using the luminescence analysis device of the first embodiment.

[0035] Figure 11 It is a flowchart showing the analysis method of a specimen using the luminescence analysis device of the second embodiment.

[0036] Figure 12 It shows following Figure 11 A flowchart of the analysis method of a specimen using the luminescence analysis device of the second embodiment.

[0037] [Description of reference symbols]

[0038] 1: Luminescence analysis device

[0039] 10: Specimen setting table

[0040] 11: Discharge chamber

[0041] 12: Opening

[0042] 13: Condensing lens

[0043] 14: Gas supply path

[0044] 15: Gas discharge path

[0045] 20: Opposing electrodes

[0046] 41: Measurement chamber

[0047] 42: Spectrometer

[0048] 43: Detector

[0049] 50: Control unit

[0050] 51: CPU

[0051] 52: Memory

[0052] 53: Operation unit

[0053] 54: Display unit Detailed implementation manners

[0054] <First Embodiment>

[0055] (1) Structure of the luminescence analysis device 1

[0056] As Figure 1 shown, the luminescence analysis device 1 of this embodiment includes a specimen setting table 10, opposing electrodes 20, a spectrometer 42, a plurality of detectors 43, and a control unit 50.

[0057] Inside the specimen setting table 10, a discharge chamber 11 is formed. In the specimen setting table 10, an opening 12 is formed facing the discharge chamber 11. The specimen S is arranged to block the opening of the specimen setting table 10. In the specimen setting table 10, opposing electrodes 20 are installed facing the specimen S. The ends of the opposing electrodes 20 are arranged inside the discharge chamber 11.

[0058] In the specimen setting table 10, a gas supply path 14 for supplying gas to the discharge chamber 11 and a gas discharge path 15 for discharging the gas from the discharge chamber 11 are formed. During analysis, an inert gas is introduced into the discharge chamber 11 from the gas supply path 14 and overflows and is discharged from the gas discharge path 15. As described above, the air in the discharge chamber is replaced with an inert gas, thereby suppressing the influence of the components in the air on the analysis result. An example of the inert gas is argon.

[0059] Gas is introduced into the discharge chamber 11, and a voltage is applied between the specimen and the opposing electrode 20 to cause a discharge. The light generated by the discharge passes through the condenser lens 13 installed on the specimen stage 10 and is guided to the measurement chamber 41.

[0060] A spectroscope 42 and a plurality of detectors 43 are arranged in the measurement chamber 41. The spectroscope 42 is a concave diffraction grating. The light generated in the discharge chamber 11 is incident on the spectroscope 42 and decomposed, and is guided to the plurality of detectors 43 according to each wavelength n of the bright line spectrum unique to each element. Each detector 43 detects the intensity of the bright line spectrum unique to each element at the wavelength n.

[0061] The control unit 50 is a computer. The control unit 50 includes a central processing unit (CPU) 51, a memory 52, an operation unit 53, and a display unit 54. The control unit 50 controls the gas introduction into the discharge chamber 11, the voltage application between the specimen S and the opposing electrode 20, etc. to perform the composition analysis of the specimen S. In addition, the control unit 50 receives the measurement data from each detector 43 and performs data processing. The CPU 51 performs calculations. The CPU 51 executes programs. In addition, the CPU 51 stores programs or data in the memory 52 and reads programs or data from the memory. Here, the memory 52 includes not only a random access memory (RAM) or a read only memory (ROM), but also an external storage memory such as a hard disk drive (HDD). The CPU 51 outputs measurement programs, measurement data, calculation results, etc. and displays them on the display unit 54. The display unit 54 is a display. The operation unit 53 accepts user input. The CPU 51 executes programs according to the instructions input from the operation unit 53. The operation unit 53 is a keyboard, a mouse, a touch panel integrated with the display unit, etc.

[0062] Calibration curve data is stored in the memory 52. The calibration curve data is data representing the relationship between the detection intensity and the content rate (concentration) of the element according to each wavelength n of the bright line spectrum unique to each element (illustrated in Figure 3 ). At the time of analysis, the control unit 50 receives the data of the detection intensity from each detector 43 and calculates the content rate of the element based on the calibration curve data stored in the memory 52. Furthermore, the calculated content rate is displayed on the display unit 54.

[0063] In the compositional analysis of the specimens of the present disclosure, there are important elements according to the specimens measured, and the operator focuses on and determines the important components for determining the variety from the contained elements based on experience (in the present disclosure, the most important one element is referred to as the priority element). The analysis device of the present disclosure has a structure that can effectively utilize such insights.

[0064] For each specimen of the same type, the control unit 50 selects a priority element from the multiple elements measured for analysis. The priority element is input by the operator from the operation unit 53. The input priority element is stored in the memory 52. Regarding the way the operator selects the priority element, the operator can input by selecting the priority element from the multiple elements displayed on the display unit 54.

[0065] The priority element is not limited to the element with the highest content rate. The priority element can be the nth (n is an integer from 2 to 50) most abundant element. For example, in the case of carbon steel, carbon C, silicon Si, manganese Mn, etc. can be used as important components for determining the variety of carbon steel, and any one of these elements can be selected as the priority element.

[0066] A management range is set for the elements that are the object of the compositional analysis of the specimen. For all the elements that are the object of the compositional analysis, including the priority element, a management range is set for each element. Here, the management range is the allowable distribution range of the content rate.

[0067] Generally, for specimens of the same type, a common priority element is selected and a common management range is set.

[0068] (2) Method for Analyzing Specimens Using the Luminescence Analysis Device 1

[0069] In the analysis of the specimens in the present embodiment, multiple measurements are performed on multiple positions of the specimen. The control unit 50 obtains the detection intensities related to multiple elements in each measurement and calculates the content rate of each element based on the detection intensity of each element.

[0070] The specimen S is shaped into a cylindrical shape and set on the specimen setting table 10. The specimen shape can be a cuboid, mushroom shape, coin shape, or other shapes. The analysis positions on the specimen S are changed in each analysis. In Figure 2 they are the first position 1A, the second position 2B, the third position 3C, and the fourth position 4D. The reason is that the deviation of the composition caused by the positions within the specimen S is taken into the measured values. Additionally, the reason is that if the discharge positions overlap, correct analysis cannot be performed.

[0071] Refer to Figures 4 to 10 the flowchart to describe the method for analyzing the composition of specimens using the luminescence analysis device 1 of the present embodiment.

[0072] InFigure 4 In the flowchart of Figure 4 , initially, in step S100, one priority element is selected from among a plurality of elements that are the objects of component analysis of the specimen. Regarding the priority element, for the same type of measurement, an element that has been previously determined by the operator and stored in the memory 52 of the control unit 50 can be used. The priority element can be input by the operator when measuring a set of specimens. Additionally, an element input by the operator to the control unit 50 after the first measurement or the second measurement of a single specimen can also be used.

[0073] In step S100, a priority element is selected, and a range of content rates, i.e., a management range, is set for a specified element among the plurality of elements that are the objects of component analysis of the specimen. Here, the elements for which the management range is set include the priority element and one or more other elements that are the objects of component analysis of the specimen.

[0074] In the present embodiment, multiple measurements are performed at multiple positions of a single specimen. In each measurement, detection intensities related to a plurality of elements that are the objects of component analysis of the specimen are acquired, and the content rate of each element is calculated based on the detection intensity of each element. For all elements for which a management range is set, it is determined whether the difference in the content rates of the two measurements is within the management range of each element. For all elements for which a management range is set, when it is within the management range of each element, the two measurements are regarded as successful. In the case where the measurement is successful, the average value of the content rates of each element (all the measured elements or a part of them as required) of the two measurements is calculated as the representative value of the content rate of each element. Furthermore, the calculated representative value is output. By output, for example, it means that the computer of the control unit 50 outputs to the display unit 54. Output includes the case of being stored in the memory 52. In addition, in the present disclosure, the difference in the content rates of the two measurements refers to the absolute value and is not a negative value.

[0075] In step S101, first, the specimen S is placed at the opening 12 of the specimen setting table 10. The control unit 50 performs a first measurement on the first position 1A of the specimen S. That is, the control unit 50 introduces gas into the discharge chamber 11 and applies a voltage between the first position 1A of the specimen S and the opposing electrode 20 to cause a discharge. The emitted light is decomposed by the spectroscope 42 according to each wavelength n of the bright line spectrum unique to each element and detected by each detector 43. The data of the detection intensity detected by each detector 43 is acquired by the control unit 50.

[0076] The control unit 50, based on the detection intensity of each wavelength n of the bright line spectrum unique to each element (the detection intensity based on the first analysis is referred to as the first detection intensity; the same applies to subsequent measurements), and using the calibration curve data stored in the memory 52 (illustrated in Figure 3The content ratio (first content ratio) of each element is calculated based on the results of the first analysis (S102). The content ratio of each element (the ratio based on the first analysis is called the first content ratio; the same applies to subsequent analyses) is output by the CPU 51 to the display unit 54 and the memory 52. Thus, the first analysis is completed.

[0077] Similarly, the control unit performs a second analysis on the second position 2B of the specimen S. That is, a second measurement is performed on the second position 2B of the specimen S (S103), and the content ratio (second content ratio) of each element is calculated based on the obtained detection intensity (second detection intensity) (S104). The content ratio (second content ratio) of each element is output by the CPU 51 to the display unit 54 and the memory 52.

[0078] Next, the control unit 50 calculates the difference between the first content ratio and the second content ratio for the priority elements (here, the absolute value of the difference; the same applies hereinafter). Then, it is determined whether the difference in content ratios is within the specified value (management range) or not (S105). When the difference in content ratios is within the management range, the process proceeds to step S106. When the difference in content ratios exceeds the management range, the process proceeds to step S110, and a third analysis (measurement) is further performed.

[0079] On the other hand, in step S106, for each element other than the priority elements among the multiple elements contained in the specimen and for which a management range is set, it is determined whether the difference between the first content ratio and the second content ratio is within the management range. Then, when the difference between the first content ratio and the second content ratio of all elements for which a management range is set is within the management range, it is determined that the first measurement (S101, S102) and the second measurement (S103, S104) are successful.

[0080] Next, in step S107, the average value of the first content ratio and the second content ratio of each element is calculated. The calculated value is used as the representative value of the content ratio of the element. The CPU 51 of the control unit 50 outputs the calculated representative value to the display unit 54. The display unit 54 displays the representative value of each element output to it. Then, the analysis of the specimen is completed.

[0081] Next, in step S106, for one or more elements among all elements for which a management range is set, when the difference in content ratios between the two measurements exceeds the management range of the element, the process proceeds to step S110, and a third analysis (measurement) is further performed.

[0082] The control unit 50 performs a third measurement on the third position 3C of the specimen S (S110), calculates the content rate (third content rate) of each element using the calibration curve based on the obtained detection intensity (third detection intensity) (S111). The content rate (third content rate) of each element is displayed on the display unit 54.

[0083] Next, in the same manner as in step S105, the control unit 50 calculates the difference between the first content rate and the third content rate and the difference between the second content rate and the third content rate for the priority elements. Then, it selects the combination of measurements with a smaller difference in content rates. Then, for the priority elements, it determines whether the difference in content rates of the selected two measurements is within the management range (S112). When the difference in content rates of the selected two measurements is within the management range, it proceeds to step S113, and when the difference exceeds the management range, it proceeds to the fourth measurement (S120).

[0084] In step S113, for all elements other than the priority elements for which a management range is set, it determines whether the difference in content rates of the selected two measurements is within the management range. For all elements other than the priority elements for which a management range is set, when the difference in content rates of the selected two measurements is within the management range, the selected two measurements are regarded as successful, and it proceeds to step S114. For one or more elements among all elements other than the priority elements for which a management range is set, when the difference in content rates of the selected two measurements exceeds the management range, it proceeds to step S115.

[0085] In step S114, for the selected two measurements, it calculates the average value of the content rate of each element. The CPU 51 of the control unit 50 outputs the calculated representative value to the display unit 54. The display unit 54 displays the output representative value of each element on the display unit 54. Then, the analysis of the specimen is ended. In addition, in step S114, the elements for which the representative value of the content rate is calculated may include not only the elements for which a management range is set, but also the elements for which no management range is set.

[0086] Next, the case where the difference in content rates of the selected two measurements of the element exceeds the management range in step S112 or step S113 will be described. In this case, for the priority elements, it selects the combination of measurements with a larger difference in content rates between the difference between the first content rate and the third content rate and the difference between the second content rate and the third content rate. Then, for the priority elements, it determines whether the difference in content rates of the selected two measurements is within the management range (S115). When the difference in content rates of the selected two measurements is within the management range, it proceeds to step S116, and when the difference exceeds the management range, it proceeds to the fourth measurement (S120).

[0087] In step S116, for all elements with a set management range other than the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. For all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements is within the management range, the two selected measurements are regarded as successful, and the process proceeds to step S117. For one or more elements among all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements exceeds the management range, the process proceeds to the fourth measurement (S120).

[0088] In step S117, for the two selected measurements, the average value of the content rate of each element is calculated. The CPU 51 of the control unit 50 outputs the calculated representative value to the display unit 54. The display unit 54 displays the representative value of each element output on the display unit 54. Then, the analysis of the sample ends. In addition, in step S117, the elements for which the representative value of the content rate is calculated may include not only the elements with a set management range but also the elements without a set management range.

[0089] In step S120, a fourth analysis (measurement) is further performed. The control unit 50 performs a fourth measurement on the fourth position 4D of the sample S, and calculates the content rate (fourth content rate) of each element based on the obtained detection intensity (fourth detection intensity). The content rate (fourth content rate) of each element is output by the CPU 51 to the display unit 54 and the memory 52 (S121).

[0090] Next, the control unit 50 calculates the difference between any one of the first content rate to the third content rate and the fourth content rate for a priority element selected from among the multiple elements. Then, a combination of measurements with the smallest difference between any one of the first content rate to the third content rate and the fourth content rate is selected. Next, for the priority element, it is determined whether the difference in the content rates of the two selected measurements is within the management range (S122). When the difference in the content rates of the two selected measurements is within the management range, the process proceeds to step S123, and when the difference exceeds the management range, it is set as unsuccessful and the process proceeds to step S131. In step S131, as an output indicating unsuccessful measurement, the content rates of all elements are output as 0 (zero) and displayed on the display unit 54, and the measurement ends. Here, "unsuccessful" means that even after four measurements, the deviation of the content rates of the elements with a set management range is not within the desired management range. In addition, the output indicating unsuccessful measurement (S131) may be any output that can clearly determine unsuccessful measurement, and is not limited to the above output form.

[0091] In step S123, for all elements with a set management range other than the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. For all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements is within the management range, the two selected measurements are regarded as successful, and the process proceeds to step S124. For one or more elements among all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements exceeds the management range, the process proceeds to step S125.

[0092] In step S124, for the two selected measurements, the average value of the content rate of each element is calculated. The CPU 51 of the control unit 50 outputs the calculated average value as a representative value to the display unit 54. The display unit 54 displays the representative value of each element output on the display unit 54. Then, the analysis of the sample is ended. In addition, in step S124, among the elements for which the representative value of the content rate is calculated, not only the elements with a set management range but also the elements without a set management range may be included.

[0093] In the case of proceeding to step S125, for the priority elements, the difference between any one of the first content rate to the third content rate calculated in step S122 and the fourth content rate is compared. The combination of the measurements with the second smallest difference among the differences between any one of the first content rate to the third content rate and the fourth content rate is selected. Next, for the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. When the difference in the content rates of the two selected measurements is within the management range, the process proceeds to step S126. When the difference exceeds the management range, it is regarded as unsuccessful, and the process proceeds to step S132. In step S132, as the output of unsuccessful measurement, the content rates of all elements are output as 0 (zero) and displayed on the display unit 54, and the measurement is ended. Here, "unsuccessful" means that even after four measurements, the deviation of the content rate of the element with a set management range is not within the desired management range. In addition, the output of unsuccessful measurement (S132) may be any output as long as it can clearly determine that the measurement is unsuccessful, and is not limited to the above output form.

[0094] In step S126, for all elements with a set management range other than the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. For all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements is within the management range, the two selected measurements are regarded as successful, and the process proceeds to step S127. For one or more elements among all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements exceeds the management range, the process proceeds to step S128.

[0095] In step S127, for the two selected measurements, the average value of the content rate of each element is calculated. The CPU 51 of the control unit 50 outputs the calculated representative value to the display unit 54. The display unit 54 displays the representative value of each element output on the display unit 54. Then, the analysis of the sample is ended. In addition, in step S127, the elements for which the representative value of the content rate is calculated may include not only the elements for which the management range is set, but also the elements for which the management range is not set.

[0096] In the case of proceeding to step S128, for the priority element, the difference between any one of the first content rate to the third content rate calculated in step S122 and the fourth content rate is compared. The combination of measurements with the largest difference within the difference between any one of the first content rate to the third content rate and the fourth content rate is selected. Next, for the priority element, it is determined whether the difference in the content rates of the two selected measurements is within the management range. When the difference in the content rates of the two selected measurements is within the management range, proceed to step S129. When the difference exceeds the management range, it is set as unsuccessful and proceed to step S133. In step S133, as the output of unsuccessful measurement, the content rates of all elements are output as 0 (zero) and displayed on the display unit 54, and the measurement is ended. Here, "unsuccessful" means that even if four measurements are performed, the deviation of the content rate of the element for which the management range is set is not within the desired management range. In addition, the output of unsuccessful measurement (S133) may be any output that can clearly determine the unsuccessful measurement, and is not limited to the above output form.

[0097] In step S129, for all elements with a set management range other than the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. For all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements is within the management range, proceed to step S130. For one or more elements among all elements with a set management range other than the priority elements, when the difference in the content rates of the two selected measurements exceeds the management range, it is considered unsuccessful, and proceed to step S134. In step S134, as the output of unsuccessful measurement, the content rates of all elements are output as 0 (zero) and displayed on the display unit 54, and the measurement is ended. Here, being unsuccessful means that even after four measurements, the deviation of the content rate of the element with a set management range is not within the desired management range. In addition, the output of unsuccessful measurement (S134) only needs to be an output that can clearly determine unsuccessful measurement, and is not limited to the above output form. Additionally, the reason for being unsuccessful in step S129 is that the difference in the content rates of the elements with a set management range other than the priority elements exceeds the management range. Therefore, to clarify the situation, as the output of step S134, for the priority elements, the average value of the content rates of the two selected measurements in step S128 can be calculated as a representative value, while the content rates of other elements are output as 0 (zero) and displayed on the display unit 54.

[0098] In step S130, for the two selected measurements, the average value of the content rate of each element is calculated. The CPU 51 of the control unit 50 outputs the calculated average value as a representative value to the display unit 54. The display unit 54 displays the representative value of each element output on the display unit 54. Then, the analysis of the sample is ended. In addition, in step S130, the elements for which the representative value of the content rate is calculated may include not only the elements with a set management range but also the elements without a set management range.

[0099] In the above embodiment, the case where the measurement is repeated four times is described. Depending on the application purpose, the maximum number of measurements can be three, five, or six or more.

[0100] (3) Features of the First Embodiment

[0101] (3-1) In this embodiment, the control unit 50 pre-sets a management range as the allowable range of variation of the content rate for important elements. Then, for all elements with a set management range, when the difference in the content rates of the two measurements is within the management range, the two measurements are adopted. Then, the average value of the measurement results (content rates) in the two measurements is calculated, and the average value is calculated as a representative value. Since the management range is set for important elements to process the measurement data, reliable measurement results can be obtained simply.

[0102] (3-2) In this embodiment, the control unit 50 designates the most important element as the priority element in advance. Then, after measuring the content rate multiple times (twice or three times), initially, for the priority element, it is determined whether the difference in the content rate based on the two measurements is within the management range. Then, when the average value of the content rate of the priority element exceeds the management range, the next measurement is performed. By initially focusing on the priority element for determination, in most cases, the validity of the measurement results can be quickly determined in one go. As a result, in the measurement of a large number of samples, the measurement time can be shortened.

[0103] (3-3) In this embodiment, after performing three or more measurements, for the priority element, calculate the difference between the content rate of the last measurement and the content rate of each previous measurement, and check whether all elements are within the management range. Initially, for the priority element, within the difference in the content rate of the two measurements, initially select the two measurements with the smallest difference. Then, for the priority element, determine whether the difference in the content rate of the selected two measurements is within the management range. For the priority element, when the difference in the content rate of the selected two measurements is within the management range, for all elements with a management range set, determine whether the difference in the content rate of the selected two measurements is within the management range. For all elements with a management range set other than the priority element, when the difference in the content rate of the selected two measurements is below the management range, the selected two measurements are regarded as successful, and the representative value is calculated. When the difference in the content rate of the selected two measurements exceeds the management range for one or more elements within all elements with a management range set, for the priority element, the measurements of the two times with the smallest difference are regarded as failed. Then, for the priority element, select the measurements of the two times with the second smallest difference and repeat the above operation.

[0104] As described above, in the case of performing three or more measurements, for the priority element, in ascending order of the difference in the content rate of the two measurements, check the deviation of the priority element and the elements with a management range set other than the priority element, so that an appropriate measurement result can be quickly obtained with less computational effort.

[0105] <Second Embodiment>

[0106] (4) Analysis method of the sample using the luminescence analysis device 1 of the second embodiment

[0107] In this embodiment, the same luminescence analysis device 1 as in the first embodiment is used, and the measurement (analysis) method for each sample S is also the same as in the first embodiment.

[0108] The analysis method of the second embodiment is different from that of the first embodiment in that: in the second embodiment, four measurements (analyses) of the same sample are performed all at once. In contrast, in the first embodiment, first, two measurements are performed, and the number of measurements is increased one by one as needed.

[0109] Use Figure 11 , Figure 12 The flowchart of to illustrate the analysis method of the sample in this embodiment.

[0110] First, in step S200, in the same manner as step 100 of the first embodiment, a priority element is selected, and a specified range of the content rate, that is, a management range, is set for a specific element within the elements that are the object of the component analysis of the sample. The management range can also be set for all the elements that are the object of the component analysis of the sample.

[0111] Next, in step S201, the sample S is placed at the opening 12 of the sample setting table 10, and the first measurement is performed on the first position 1A of the sample S. Subsequently, the content rate of each element is calculated based on the detection intensity of the measurement. The details of the measurement are the same as those in steps S101 and S102 of the first embodiment. Subsequently, the second to fourth measurements are performed in the same manner as the second measurement (S103, S104) of the first embodiment, and data on the second to fourth content rates are obtained for each element.

[0112] In step S202, for the priority element, the difference in the content rates of the two measurements is calculated. Regarding the combination of the two measurements, calculations are performed for all cases of combining two measurements out of the four measurements. That is, the six combinations are the first and second, the first and third, the first and fourth, the second and third, the second and fourth, and the third and fourth.

[0113] In step S203, the nth (n = 1) smallest content rate difference among the six content rate differences of the priority element calculated in step S202 is selected.

[0114] Next, in step S204, for the priority elements, it is determined whether the difference in the content rates of the two measurements selected in step S203 is within the management range. When the difference in the content rates of the two selected measurements is within the management range, proceed to step S205. When the difference exceeds the management range, it is set as unsuccessful and proceed to step S207. In step S207, as the output of unsuccessful measurement, the content rates of all elements are output as 0 (zero) and displayed on the display unit 54, and the measurement ends. Here, by "unsuccessful" it means that even after four measurements, the deviation of the content rate of the elements with the management range set is not within the desired management range. In addition, the output of unsuccessful measurement (S207) can be any output that can clearly determine unsuccessful measurement, and is not limited to the above output form.

[0115] In step S205, for all elements with a management range set other than the priority elements, it is determined whether the difference in the content rates of the two selected measurements is within the management range. For all elements with a management range set other than the priority elements, when the difference in the content rates of the two selected measurements is within the management range, the two selected measurements are regarded as successful and proceed to step S206. For one or more elements among all elements with a management range set other than the priority elements, when the difference in the content rates of the two selected measurements exceeds the management range, return to step S203.

[0116] In the case of returning to step S203, for the difference in the content rates of the priority elements, increment n by 1 and select the combination of measurements with the second smallest difference. Then, repeat steps S204 and S205. Repeat the loop as needed until n reaches 6. When n exceeds 6, the measurement is set as unsuccessful and proceed to step S207. In step S207, as the output of unsuccessful measurement, the content rates of all elements are output as 0 (zero), displayed on the display unit 54, and the process ends.

[0117] In step S206, for the two selected measurements, calculate the average value of the content rates of each element. The CPU 51 of the control unit 50 outputs the calculated representative value to the display unit 54. The display unit 54 displays the representative value of each element output on the display unit 54. Then, the analysis of the sample ends. In addition, in step S206, the elements for which the representative value of the content rate is calculated may include not only the elements with the management range set, but also the elements without the management range set.

[0118] In the above embodiment, the case of performing four measurements is described. Depending on the application purpose, the maximum number of measurements can be three, five, or six or more.

[0119] The features of this embodiment are the same as those of (3-1) to (3-3) of the first embodiment.

[0120] In this embodiment, since a prescribed number of measurements (four times in this case) are carried out from the beginning, in the case of the first embodiment, it may not be carried out sometimes, and the number of measurements may increase due to the implementation of the third measurement and the fourth measurement. However, since it is necessary to carry out a prescribed number of measurements (four times) and the measurement results with a smaller difference in the content rate of the priority element can be selected from the combinations of six measurement results, it is possible to obtain highly accurate results.

[0121] The above describes one embodiment of the present disclosure, but the present disclosure is not limited to the above embodiment, and various modifications can be made without departing from the gist of the present disclosure. In particular, the embodiments described in this specification can be arbitrarily combined as needed.

[0122] (5) Forms

[0123] Those skilled in the art should understand that the multiple exemplary embodiments are specific examples of the following forms.

[0124] (First item) A luminescence analysis device of one form includes:

[0125] A sample setting table, which forms a discharge chamber inside for introducing gas to carry out discharge, and includes an opening formed in contact with the discharge chamber for placing a sample;

[0126] Opposing electrodes, the ends of which are arranged in the discharge chamber, and a voltage is applied between the electrodes and the sample to generate discharge;

[0127] A spectroscope for decomposing the light generated by the discharge;

[0128] Multiple detectors for detecting the light of each wavelength decomposed by the spectroscope; and

[0129] A control unit for controlling the voltage applied between the sample and the opposing electrodes, and processing the measurement data detected by the detectors to calculate the content rate of the element,

[0130] In the control unit,

[0131] One priority element is selected from multiple elements that are the object of component analysis of the sample, and a range of content rates, that is, a management range, is set for each of the multiple elements that are the object of component analysis of the sample,

[0132] Multiple positions of the sample are measured multiple times. In each measurement, the detection intensities related to multiple elements are obtained, and the content rate of each element is calculated based on the detection intensity of each element.

[0133] For the priority element, the difference in the content rate between two measurements within multiple measurements is calculated. When the difference is within the management range,

[0134] For all elements for which a management range is set, it is determined whether the difference in the content rates of the two measurements of each element is within the management range.

[0135] For all elements for which a management range is set, when the difference in the content rates of the two measurements of each element is within the management range of each element,

[0136] The average value of the content rates of the two measurements of each measured element is calculated as a representative value and output.

[0137] The luminescence analysis device according to the first item sets one element as a priority element from the elements to be measured and processes the measurement data, so that measurement results with less deviation can be obtained simply.

[0138] (Second item) According to the luminescence analysis device described in the first item, wherein,

[0139] The control unit measures the sample three or more times.

[0140] For the priority element, the difference in the content rates of two measurements within three or more measurements is calculated, and the two measurements with the smallest difference are preferentially selected. When the difference in the content rates of the two selected measurements is within the management range,

[0141] For all elements for which a management range is set, it is determined whether the difference in the content rates of the two selected measurements of each element is within the management range.

[0142] For all elements for which a management range is set, when the difference in the content rates of the two selected measurements of each element is within the management range of each element,

[0143] The average value of the content rates of the two selected measurements of each measured element is calculated as a representative value and output.

[0144] The luminescence analysis device according to the second item, in the case of performing three or more measurements, for the priority element, preferentially selects the two measurements with the smallest difference in the content rates for data processing, so that appropriate measurement results can be obtained quickly with less calculation amount.

[0145] (Third item) According to the luminescence analysis device described in the first item, wherein,

[0146] The control unit measures the sample twice.

[0147] For the priority element, the difference in the content rates of the two measurements is calculated. When the difference is within the management range,

[0148] For all elements with a set management range, it is determined whether the difference in the content rates of the two measurements of each element is within the management range.

[0149] For all elements with a set management range, when the difference in the content rates of the two measurements of each element is within the management range of each element,

[0150] Calculate the average value of the content rates of the two measurements of each measured element as a representative value and output it.

[0151] The luminescence analysis device described in the third item can obtain highly reliable measurement data only through two measurements.

[0152] (Item 4) According to the luminescence analysis device described in the first item, wherein,

[0153] The control unit performs two measurements on the sample.

[0154] For priority elements, calculate the difference in the content rates of the two measurements. When the difference exceeds the management range, output that the results of the two measurements exceed the management range.

[0155] In the luminescence analysis device described in the fourth item, for priority elements, the judgment of the management range is prioritized, so it is possible to quickly decide to perform additional measurements, which helps to simplify and quickly perform the measurements.

[0156] (Item 5) According to the luminescence analysis device described in the fourth item, wherein,

[0157] When the control unit performs a third measurement, for priority elements, it is determined whether the smaller of the difference between the content rate of the first measurement and the content rate of the third measurement and the difference between the content rate of the second measurement and the content rate of the third measurement exceeds the management range. When it exceeds, the sample is subjected to a fourth measurement.

[0158] In the luminescence analysis device described in the fifth item, for priority elements, the judgment of the management range is prioritized, so it is possible to quickly decide on the fourth measurement, which helps to simplify and quickly perform the measurements.

Claims

1. A luminescence analysis device, comprising: A sample setting table, wherein a discharge chamber is formed inside for introducing gas to perform discharge, and includes an opening formed in contact with the discharge chamber for placing the sample; The end of the counter electrode is arranged in the discharge chamber, and a voltage is applied between the counter electrode and the sample to generate discharge; A spectrometer to decompose the light generated by the discharge; A plurality of detectors for detecting the light of each wavelength decomposed by the spectrometer; and The control unit controls the voltage applied between the sample and the counter electrode, and processes the measurement data detected by the detector to calculate the content rate of the element. In the control unit, A priority element is selected from a plurality of elements as the target of component analysis of the sample, and a range of content, i.e., a management range, is set for each of the plurality of elements as the target of component analysis of the sample. Perform multiple measurements on multiple locations of the sample, obtain detection intensities related to multiple elements in each measurement, and calculate the content of each element based on the detection intensity of each element. For the priority element, the difference in content between two measurements in multiple measurements is calculated. If the difference is within the management range, For all elements for which a management range is set, it is determined whether the difference between the two measured contents of each element is within the management range. For all elements for which a management range is set, when the difference between the content rates of the two measurements of each element is within the management range of each element, The average value of the content of each element measured twice is calculated as a representative value and output.

2. The luminescence analysis device according to claim 1, wherein: The control unit performs measurement on the sample three or more times, For the priority element, the difference in content between two measurements within three or more measurements is calculated, and the two measurements with the smallest difference are preferentially selected. If the difference in content between the selected two measurements is within the management range, For all elements for which a management range is set, it is determined whether the difference between the content rates of the two selected measurements of each element is within the management range. For all elements for which a management range is set, when the difference between the content rates of the two selected measurements of each element is within the management range of each element, The average value of the content of each element measured in the selected two measurements is calculated as a representative value and output.

3. The luminescence analysis device according to claim 1, wherein: The control unit performs two measurements on the sample. For the priority elements, the difference between the two measured contents is calculated. If the difference is within the management range, For all elements for which a management range is set, it is determined whether the difference between the two measured contents of each element is within the management range. For all elements for which a management range is set, when the difference between the content rates of the two measurements of each element is within the management range of each element, The average value of the content of each element measured twice is calculated as a representative value and output.

4. The luminescence analysis device according to claim 1, wherein: The control unit performs two measurements on the sample. For the priority element, the difference between the content rates of two measurements is calculated, and when the difference exceeds the management range, it is output that the two measurement results exceed the management range.

5. The luminescence analysis device according to claim 4, wherein: When the control unit performs the third measurement, for the priority element, whether the smaller difference between the difference between the content measured for the first time and the content measured for the third time and the difference between the content measured for the second time and the content measured for the third time exceeds the management range, and if so, performs a fourth measurement on the sample.

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