Analysis method for result of ICP emission spectral analysis measurement and analysis system for result of ICP emission spectral analysis measurement

Abstract

To prevent the occurrence of difference between the details of analysis that are automatically obtained and the details of analysis when a person conducts analysis, when automating analysis of a result of ICP emission spectral analysis measurement.SOLUTION: An analysis method for a result of ICP emission spectral analysis measurement includes: a peak wavelength preparation step; a priority setting step; a weighting step of performing weighting on an analysis value from an analysis person's subjective point of view for at least one of a plurality of peak wavelengths; an analysis value acquisition step of acquiring an analysis value in each of the plurality of peak wavelengths for each element; a grouping step of grouping the plurality of peak wavelengths into groups having the analysis values close to each other; a group selection step of selecting the most weighted group in the entire groups in the weighting step; a peak wavelength selection step of selecting the peak wavelength having the highest priority among the peak wavelengths in the group selected in the group selection step; and an analysis value determination step of adopting the analysis value corresponding to the selected peak wavelength.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a method for analyzing the results of ICP optical emission spectrometry and a system for analyzing the results of ICP optical emission spectrometry. [Background technology]

[0002] In Patent Document 1, in emission spectroscopy, a sample is excited to emit light, which is then dispersed using a spectrometer or the like, and the intensity of the spectral line of the quantified element (target element) at a specific wavelength is measured to analyze the type and amount of contained elements. In order to correct for the influence of overlapping of nearby spectral lines of coexisting elements on the measurement of the quantified element, a sample for calculating a correction coefficient is measured at the same time for each measurement, and a correction coefficient is calculated and corrected each time (see

[0012] of Patent Document 1).

[0003] Patent Document 2 discloses the following contents. For contents not described in the present specification, the description in Patent Document 2 can be referred to. "A method for analyzing analytical values ​​obtained for each element in a measurement target as a result of ICP optical emission spectroscopy measurement of the measurement target, comprising: a peak wavelength preparation step of preparing, for each element, a plurality of wavelengths that are less affected by coexisting elements when subjected to ICP optical emission spectroscopy measurement and have high sensitivity; a priority setting step of setting priorities for the plurality of peak wavelengths in descending order of sensitivity and less influence of coexisting elements when subjected to the ICP optical emission spectrometry; an analysis value acquisition step of obtaining the analysis value at each of the plurality of peak wavelengths for each of the elements; a grouping step of grouping the plurality of peak wavelengths into groups of wavelengths having similar analytical values; a peak wavelength selection step of selecting a group having the largest number of peak wavelengths and selecting the peak wavelength having the highest priority from among the peak wavelengths in the group; an analysis value determination step of adopting an analysis value corresponding to the selected peak wavelength; A method for analyzing the results of ICP optical emission spectrometry analysis, comprising: [Prior art documents] [Patent documents]

[0004] [Patent Document 1] Japanese Patent Application Publication No. 5-45287 [Patent Document 2] Japanese Patent Publication No. 2022-150584 Summary of the Invention [Problem to be solved by the invention]

[0005] By utilizing the technology described in Patent Document 2, it is possible to automate the analysis of the results of ICP optical emission spectrometry measurement as much as possible while maintaining the accuracy of the analysis.

[0006] On the other hand, the inventors' careful investigation revealed that there are differences between the analysis results obtained using the technology described in Patent Document 2 and the results obtained when a person analyzes the results, as described in the Problems section of Patent Document 2.

[0007] This difference can be explained using the peak wavelengths λ1 to λ5 (in this order of priority) described in

[0030] of Patent Document 2.

[0008] In the classification process in Patent Document 2, it is assumed that the analytical values ​​are classified into group α, which is concentrations C2 to C4 (peak wavelengths λ2 to λ4), and group β, which is concentrations C1 and C5 (peak wavelengths λ1 and λ5) (see

[0033] in Patent Document 2).

[0009] In this case, in the method described in Patent Document 2, the group α is selected by majority vote, and then the peak wavelength of λ2, which has the highest priority among the group α, is automatically selected.

[0010] On the other hand, when a person (analyst) analyzes the results of ICP optical emission spectrometry, the peak wavelength λ1, which has the highest priority because it has the best sensitivity, is selected.

[0011] As described above, there is a difference between the analysis results obtained by the technology described in Patent Document 2 and the results obtained when a person analyzes the results.

[0012] Patent Document 2 describes a salvage process for salvaging the peak wavelength λ1, which has the highest priority. However, the present inventors have made the following findings regarding this salvage process.

[0013] When the analytical value is concentration, the effect of the sensitivity at the peak wavelength on the results is significant if the concentration of the measurement target is low. For this reason, the salvage feasibility determination process described in Patent Document 2 is effective.

[0014] On the other hand, when the concentration of the measurement target is high, not only does sensitivity affect the results, but coexisting substances (e.g., coexisting elements) contained in the measurement target also have a significant effect on the results. Specifically, noise caused by coexisting substances may be detected as spurious peaks. In this case, the salvage feasibility determination process described in Patent Document 2 may not function effectively.

[0015] The object of the present invention is to suppress the occurrence of differences between the analysis content obtained by automation and the analysis content when a human performs the analysis when the analysis of the results of ICP optical emission spectrometry measurement is automated. [Means for solving the problem]

[0016] In order to find a method for solving the above problems, the present inventors have reexamined the contents of Patent Document 2. Patent Document 2 positions the automation of analysis of analytical values ​​as one of its advantages. On the other hand, there are also drawbacks to automation, as described in the section on the problems of the present invention.

[0017] Therefore, the inventors have found that even when automating the analysis, the analyst's subjective opinion on the analytical values ​​(e.g., criteria for selecting peak wavelengths, rules of thumb, etc. However, the term "rules of thumb" may also be used to encompass the above-mentioned "criteria") should be incorporated into the analysis procedure for the measurement results.

[0018] On the other hand, the priorities are set in order of sensitivity with less influence of coexisting elements when subjected to ICP atomic emission spectrometry, and in order of objective values ​​(e.g., literature values, emission intensity as past measured values). In other words, while priorities are set based on objective values, the inventors have found that, based on the findings explained in the above section on the problems of the present invention, it is possible to pinpoint the influence of subjectivity in the selection stage and to divide the roles of objectivity and subjectivity in the analysis of the results of ICP atomic emission spectrometry.

[0019] This makes it possible to incorporate the knowledge that a human analyst has accumulated up to now into the analysis of the results of ICP optical emission spectroscopy measurements (for example, for a certain element, only a certain peak wavelength has ever been used, or conversely, a certain peak wavelength has never been used). When the analytical value is a concentration, this method does not require the concentration of the object being measured.

[0020] As a result, the inventors have discovered that when automating the analysis of the results, it is possible to prevent differences from occurring between the analysis content obtained by automation and the analysis content when the analysis is performed by a human.

[0021] Specifically, the present inventors have found that subjective weighting of analytical values ​​can be applied to at least one of a plurality of peak wavelengths. Instead of selecting a group based on the number of peak wavelengths in the group (by majority vote) as described in Patent Document 2, the inventors have come up with a method of selecting the group that has been weighted most heavily as a whole, and then selecting the peak wavelength with the highest priority from among the selected peak wavelengths.

[0022] A first aspect of the present invention is A method for analyzing analytical values ​​obtained for each element in a measurement object as a result of ICP optical emission spectrometry measurement of the measurement object, comprising: a peak wavelength preparation step of preparing a plurality of wavelengths for each of the elements that are less affected by coexisting elements when subjected to the ICP optical emission spectrometry analysis and have high sensitivity; a priority setting step of setting priorities for the plurality of peak wavelengths in descending order of sensitivity and less influence of coexisting elements when subjected to the ICP optical emission spectrometry; a weighting step of subjectively weighting the analysis value based on an analyst's subjective opinion for at least one of the plurality of peak wavelengths; an analysis value acquisition step of obtaining the analysis value at each of the plurality of peak wavelengths for each of the elements; a grouping step of grouping the plurality of peak wavelengths into groups of wavelengths having similar analytical values; a companion selection step of selecting a companion that has been given the highest weight overall by the weighting step; a peak wavelength selection step of selecting a peak wavelength having the highest priority from among the peak wavelengths in the group selected in the group selection step; an analysis value determination step of adopting an analysis value corresponding to the selected peak wavelength; The present invention provides a method for analyzing the results of ICP optical emission spectrometry measurement, comprising:

[0023] A second aspect of the present invention is In the method for analyzing the results of ICP atomic emission spectrometry according to the first aspect, the analyst's subjective weighting of the analysis values ​​in the weighting step is performed based on the analyst's empirical rule for selecting peak wavelengths.

[0024] A third aspect of the present invention is In the method for analyzing the results of ICP atomic emission spectrometric analysis according to the second aspect, the weighting in the weighting step is performed by assigning points to the peak wavelengths to be weighted.

[0025] A fourth aspect of the present invention is In the method for analyzing the results of ICP atomic emission spectrometry described in any one of the first to third aspects, the priorities set in the priority setting step are set based on sensitivity as a literature value or sensitivity as a past actual measurement value.

[0026] A fifth aspect of the present invention is the analytical value is a concentration, The weighting of the analysis values ​​in the weighting step is performed based on the analyst's subjective judgment criteria used in selecting peak wavelengths in the past and the analyst's empirical rules for selecting peak wavelengths, The weighting in the weighting step is performed by assigning points to the peak wavelengths to be weighted, In the method for analyzing the results of ICP atomic emission spectrometry according to the first aspect, the priorities set in the priority setting step are set based on sensitivity as a literature value or sensitivity as a past actual measurement value.

[0027] A sixth aspect of the present invention is A system for analyzing analytical values ​​obtained for each element in a measurement object as a result of ICP optical emission spectrometry measurement of the measurement object, a peak wavelength acquisition unit that acquires a plurality of wavelengths with high sensitivity and little influence from coexisting elements when subjected to the ICP optical emission spectrometry analysis for each of the elements; a priority setting unit that sets priorities for the plurality of peak wavelengths in descending order of sensitivity and less influence from coexisting elements when subjected to the ICP optical emission spectrometry; a weighting unit that performs subjective weighting of the analysis value based on an analyst's subjective opinion on at least one of the plurality of peak wavelengths; an analysis value acquisition unit that acquires the analysis value at each of the plurality of peak wavelengths for each of the elements; a grouping unit that groups the plurality of peak wavelengths into groups having similar analysis values; a companion selection unit that selects the companion that has been given the highest weight as a whole by the weighting unit; a peak wavelength selection unit that selects the peak wavelength with the highest priority from among the peak wavelengths in the group selected by the group selection unit; an analysis value determination unit that adopts an analysis value corresponding to the selected peak wavelength; The present invention relates to an analysis system for the results of ICP optical emission spectrometry analysis, which has the above-mentioned features.

[0028] A seventh aspect of the present invention is In the system for analyzing the results of ICP atomic emission spectrometry according to the sixth aspect, the weighting of the analysis values ​​in the weighting unit is performed based on the analyst's empirical rule for selecting peak wavelengths.

[0029] An eighth aspect of the present invention is In the system for analyzing the results of ICP atomic emission spectrometric analysis according to a seventh aspect, the weighting in the weighting section is performed by assigning points to the peak wavelengths to be weighted.

[0030] A ninth aspect of the present invention is a method for manufacturing a semiconductor device comprising: In the system for analyzing the results of ICP atomic emission spectrometry analysis described in any one of the sixth to eighth aspects, the priorities set by the priority setting unit are set based on sensitivity as a literature value or sensitivity as a past actual measurement value.

[0031] A tenth aspect of the present invention is a method for manufacturing a semiconductor device comprising: the analytical value is a concentration, the weighting of the analysis values ​​by the weighting unit is performed based on the analyst's subjective judgment criteria used in selecting peak wavelengths in the past and the analyst's rule of thumb for selecting peak wavelengths; the weighting in the weighting unit is performed by assigning points to the peak wavelengths to be weighted; In the system for analyzing the results of ICP atomic emission spectrometry according to a sixth aspect, the priorities set by the priority setting unit are set based on sensitivity as a literature value or sensitivity as a past actual measurement value. [Effects of the Invention]

[0032] According to the present invention, when automating the analysis of the results of ICP atomic emission spectrometric analysis, it is possible to prevent differences from occurring between the analysis content obtained by automation and the analysis content when the analysis is performed by a person. [Brief explanation of the drawings]

[0033] [Figure 1]FIG. 1 is a flowchart of the analysis method according to this embodiment. DETAILED DESCRIPTION OF THE INVENTION

[0034] FIG. 1 is a flowchart of the analysis method according to this embodiment.

[0035] This embodiment relates to a method for analyzing analytical values ​​obtained for each element in a measurement target as a result of ICP atomic emission spectroscopy measurement of the measurement target. In particular, this embodiment relates to a method for selecting one peak wavelength and an analytical value corresponding to that peak wavelength based on analytical values ​​obtained for each element at multiple peak wavelengths, and evaluating the effectiveness of the selected peak wavelength and the corresponding analytical value. Other details (e.g., creating a calibration curve when obtaining analytical values, using an internal standard, confirming the reproducibility of analytical values, etc.) may be achieved by using known techniques related to ICP atomic emission spectroscopy measurement. In this specification, "to" indicates a value greater than or equal to a predetermined value and less than or equal to a predetermined value.

[0036] It should be noted that "automation" as used in this specification refers only to the automation of the analysis of the results, and is not limited to, for example, automating everything from placing a sample on an ICP optical emission spectrometer to outputting the analysis results.

[0037] In this embodiment, first, a peak wavelength preparation step is performed in which a plurality of wavelengths that are less affected by coexisting elements and have high sensitivity when subjected to ICP optical emission spectrometry are prepared for each element.

[0038] "Influence of coexisting elements" refers to spectral interference in which the peak of a coexisting element overlaps with the peak of each element, or excitation interference in which the coexisting element affects the luminescence phenomenon of each element. "Wavelengths that are less affected by coexisting elements and have high sensitivity (hereinafter sometimes abbreviated as "high sensitivity wavelengths")" refers to the wavelength at the (top of the) peak (peak wavelength) when a sample containing a specific element is subjected to ICP optical emission spectroscopy. There are multiple peak wavelengths.

[0039] A priority setting step is performed to set priorities for the plurality of peak wavelengths in descending order of sensitivity and least influence by coexisting elements when subjected to ICP optical emission spectrometry. The peak wavelength preparation step and the priority setting step may be collectively referred to as the preparation step.

[0040] Priorities are set for the multiple peak wavelengths prepared for each element. Specifically, the order of sensitivity refers to the analytical value (and the peak wavelength corresponding to that analytical value) with the lowest lower limit of quantitation among peak wavelengths with the least influence from coexisting elements being ranked first. The "analytical value with the lowest lower limit of quantitation" can also be rephrased as the peak with the greatest maximum intensity relative to the background intensity. The analytical value with the next lowest lower limit of quantitation and its corresponding peak wavelength are ranked second, the next analytical value and its corresponding peak wavelength are ranked third, and so on. The ranking may be set based on the total number of peak wavelengths, or on a portion of them (for example, the top five).

[0041] The fact that "the effect of coexisting elements is small and the sensitivity is high" can be determined by objective values. A specific example of the objective values ​​is as follows:

[0042] For example, known academic textbooks on ICP optical emission spectroscopy measurements describe wavelengths that are less affected by coexisting elements and have high sensitivity, along with their approximate emission intensities. These values ​​(hereinafter also referred to as "literature values") may be used to carry out the peak wavelength priority setting process (described in Patent Document 2) described below, in descending order of value.

[0043] Instead of adopting the literature value, if there is a past measured value of the luminescence intensity that is less affected by coexisting elements, that value may be adopted and the peak wavelength priority setting process (described in Patent Document 2) described below may be carried out in descending order of value.

[0044] An analytical value acquisition step is performed to obtain analytical values ​​for each element at each of a plurality of peak wavelengths. The analytical value acquisition step may employ a known method for obtaining analytical values ​​by ICP atomic emission spectrometry. The analytical values ​​are preferably the concentrations of each element in the measurement target.

[0045] A grouping step is performed in which the plurality of peak wavelengths are grouped into groups having similar analysis values ​​obtained in the analysis value obtaining step.

[0046] The specific details of the grouping process are as follows: For example, if five peak wavelengths (e.g., λ1 to λ5 (unit: nm), with the above priority being λ1, λ2, etc.) are prepared for one element, the five analytical values ​​(e.g., C1 to C5 (unit: mg / L)) corresponding to the five peak wavelengths are divided into two groups (hereinafter also referred to as clusters).

[0047] A specific method for dividing the data into two groups involves dividing each analytical value into two groups, calculating the average value of each group in each case, and then adopting the grouping of analytical values ​​that results in the smallest difference from the average value. When dividing the data into two groups, the data are divided into groups of three analytical values ​​and two analytical values, or groups of four analytical values ​​and one analytical value. The number of analytical values ​​constituting each group may be the same, or the data may be divided into three or more groups.

[0048] One of the features of this embodiment is that the analyst subjectively weights at least one of the plurality of peak wavelengths. This weighting step selects the group that is most weighted overall. Of the peak wavelengths in the group selected in this group selection step, the peak wavelength with the highest priority is selected (the peak wavelength selection step described below).

[0049] The priorities are set in order of sensitivity with minimal influence of coexisting elements when subjected to ICP atomic emission spectrometry, and in order of objective values ​​(e.g., sensitivity as the literature value and the sensitivity as the past actual measurement value). In other words, while the priorities are set based on objective values, subjective influence is pinpointed in the selection of partners based on the knowledge explained in the above assignment section, and objective and subjective roles are divided.

[0050] The above features make it possible to select the peak wavelength λ1, which has the highest priority in the above example, in the same way as when a person analyzes the results, without relying on the salvage process described in Patent Document 2 (without relying on the level of the concentration if the analytical value is a concentration).

[0051] In other words, in this embodiment, instead of selecting a group based on the number of peak wavelengths in the group (majority vote) as described in Patent Document 2, the group that is weighted the most as a whole is selected using the weighting, and then the peak wavelength with the highest priority among the peak wavelengths in the selected group is selected.

[0052] As a result, when automating the analysis of the results of ICP atomic emission spectrometric analysis, it is possible to prevent differences from occurring between the analysis content obtained by automation and the analysis content when the analysis is performed by a person.

[0053] The weighting of the analysis values ​​in the weighting step may be performed subjectively by the analyst based on the analyst's rule of thumb for selecting peak wavelengths.

[0054] The following example is provided as a "rule of thumb for selecting a peak wavelength," although it is merely an example.

[0055] For an analyst, if the emission intensity at a predetermined peak wavelength is a predetermined multiple or more of the emission intensity at other peak wavelengths, and that predetermined peak wavelength is always selected, then that predetermined peak wavelength should be selected when a new measurement is made.

[0056] It also refers to selecting a predetermined peak wavelength in a new measurement when a predetermined peak wavelength has always been selected in multiple past analyses.

[0057] In the above case, the weighting step assigns a positive weight to the predetermined peak wavelength (for example, adding a score that is a deciding factor in selecting a companion). Instead of adding a score, an initial score may be set for each peak wavelength, and the initial score may be multiplied by a coefficient greater than 1.

[0058] Conversely, a negative rule of thumb for selecting a peak wavelength is that if the luminescence intensity at a given peak wavelength is less than a certain multiple (for example, less than 0.5 times) compared to the luminescence intensity of another peak wavelength, the analyst will never select that given peak wavelength, and will not select that given peak wavelength in a new measurement.

[0059] It also means that if a predetermined peak wavelength has never been selected in multiple past analyses, the predetermined peak wavelength will not be selected in a new measurement.

[0060] In the above case, the weighting step applies a negative weight to the predetermined peak wavelength (for example, by subtracting points from the score that is a deciding factor in selecting a companion). Instead of subtracting points, an initial score may be set for each peak wavelength, and the initial score may be multiplied by a coefficient less than 1.

[0061] The above-mentioned addition or subtraction of points may be performed on only some of the multiple peak wavelengths (peak wavelengths that stand out in the above-mentioned rule of thumb) or on all peak wavelengths. The weighting rules are not limited to addition, subtraction, multiplication, and division (collectively referred to as "assigning points"), and weighting other than the point system may also be used.

[0062] The subjective weighting of analytical values ​​based on the analyst's judgment may not always be the same. For example, if a specific peak wavelength was never selected in multiple past analyses, but the specific peak wavelength is now selected, the rule that assigned a negative weighting may be changed so that the specific peak wavelength is no longer assigned a negative weighting. In other words, the subjective weighting of analytical values ​​based on the analyst's judgment may be updateable. This updating process may be automated, for example, by using the EXPERT system (Symbolic AI) described in Patent Document 2.

[0063] In the content described in Patent Document 2, the group with the largest number of peak wavelengths belonging to one group is selected, but in this embodiment, the group that is weighted most as a whole in the weighting step is selected.

[0064] That is, the friends compete against each other in weighting. As an example, the friends compare the total points of the weighting points of the peak wavelengths belonging to the friends, and the friend with the highest total point is selected.

[0065] Then, a peak wavelength selection step is performed in which the peak wavelength with the highest priority is selected from the peak wavelengths in the group selected in the group selection step. If the number of analysis values ​​constituting each group is the same, both groups are selected, and then the group to which the peak wavelength with the highest priority belongs is selected, and the peak wavelength with the highest priority is also selected.

[0066] It is assumed that in the grouping step, the wavelengths are grouped into group α consisting of C2 to C4 (peak wavelengths λ2 to λ4) and group β consisting of C1 and C5 (peak wavelengths λ1 and λ5).

[0067] <Case 1> If the peak wavelength λ1 for a given element has always been empirically selected in the analysis of the results of past ICP optical emission spectrometry measurements, add +5 points to λ1. No points are added or subtracted for other wavelengths.

[0068] In Case 1, the total score of member α is 0 points, and the total score of member β is +5 points. As a result, member β is selected in the member selection process. Then, the peak wavelength with the highest priority among members β, i.e., λ1, is selected in the peak wavelength selection process.

[0069] In case 1, when the results are analyzed by a person, λ1 is selected due to its high sensitivity. In other words, there is no difference between the analysis of the results according to this embodiment and the analysis of the results by a person.

[0070] <Case 2> If the peak wavelength λ3 for a given element has always been empirically selected in past analysis of ICP optical emission spectroscopy measurement results, +5 points are added to λ3. No points are added or subtracted for other wavelengths. Case 2 is quite likely to occur. This is because, while it is appropriate to select the peak wavelength λ3, it is also possible that a peak wavelength close to λ3 (λ2 in this case) may have a higher emission intensity in certain measurement results. In this embodiment, it is possible to first select group α, which includes a peak wavelength close to λ3, and then select wavelength λ2, which is more suitable for analyzing the results.

[0071] In case 2, when a person analyzes the results, the analyst first tries to select the peak wavelength λ3 empirically. On the other hand, if the peak wavelength λ2 closer to λ3 has better sensitivity (higher emission intensity), the analyst will select λ2. In other words, there is no difference between the analysis results according to this embodiment and the analysis results by a person.

[0072] In either case 1 or 2, an analytical value determination step is then performed in which the analytical value corresponding to the peak wavelength selected in the peak wavelength selection step is adopted, thereby automating the analysis as much as possible while maintaining the accuracy of the analysis of the results of ICP optical emission spectrometry measurement.

[0073] The following preferred examples described in Patent Document 2 can also be applied to this embodiment.

[0074] A grouping step may be performed in which the plurality of peak wavelengths before the grouping step are grouped into ion beams and neutral atomic beams.

[0075] In ICP optical emission spectroscopy, it is possible to separate excitation of ions and excitation of single atoms, so the peak wavelengths can be grouped into ion lines and neutral atomic lines.

[0076] Then, a group validity evaluation step may be performed in which the results of the ICP atomic emission spectrometry analysis are deemed valid if the difference between the groups in the average analytical values ​​within each group is less than a predetermined value set for each element.

[0077] The predetermined value used in the group effectiveness evaluation process may be either an absolute value or a relative value. When a relative value is used, for example, the peak wavelengths of copper are 224.7 nm and 324.8 nm for ion beams and neutral atomic beams, respectively. Considering the ionization rate in plasma, ion beams have less influence when there are many coexisting elements, so ion beams are preferred over neutral atomic beams. Considering the influence of these coexisting elements, the predetermined value is 10% or less, preferably 5% or less.

[0078] In ICP atomic emission spectrometry, it is possible to separate excitation of ions from excitation of single atoms, but the large difference between the two groups means that the analytical values ​​vary greatly depending on which group they belong to. This can cause uncertainty in the analytical values, as shown in the copper example above. The group validity evaluation process can eliminate such factors in advance.

[0079] The group validity evaluation step may be performed before the classification step, before or after the peak wavelength selection step, or at the end (i.e., after the salvage step, as shown in Figure 3). If it is performed before the classification step, it may be possible to reduce the number of candidates for analytical values ​​to be handled after the classification step, thereby reducing the calculation load.

[0080] Assuming that one peak wavelength is arbitrarily removed from the group with the largest number of peak wavelengths belonging to that group, it is preferable to perform an outlier detection step in which the analysis values ​​of the remaining peak wavelengths in the group are evaluated to see whether they remain in the group.

[0081] For example, even if three analytical values ​​belong to the same group, one of the three analytical values ​​may be smaller or larger than the remaining two analytical values. In this case, if the smaller or larger analytical value and its corresponding peak wavelength are selected, this will cause uncertainty in the analytical values. The outlier detection process can eliminate such factors in advance.

[0082] Specifically, in the above example, among C2 to C4 belonging to one group α, if C3 is a large value, excluding C2 would increase the average value of the analysis values ​​in group α. In this case, applying the rule used in the grouping step would likely result in the remaining C3 and C4 not belonging to the same group. On the other hand, if C3 is excluded, the remaining C2 and C4 have similar values, so their average values ​​would be roughly the same as those of C2 and C4. Therefore, even if applying the rule used in the grouping step, they would still belong to the same group. In this case, C3 would be determined to be an abnormal value. Instead of the rule used in the grouping step, a rule based on whether the percentage of variation from the average value before the exclusion of the analysis value is below a predetermined value (10%, preferably 5%) may be used.

[0083] It is preferable to perform the outlier detection process according to the above content, and to exclude analytical values ​​determined to be outliers and the peak wavelengths corresponding to those analytical values ​​before the peak wavelength selection process. The outlier detection process may be performed before the classification process (as shown in Figure 3) or before the peak wavelength selection process. Performing the outlier detection process before the classification process may reduce the number of analytical value candidates to be handled after the classification process, thereby reducing the computational load. Note that the outlier detection process may also be performed on analytical values ​​corresponding to the peak wavelengths in order of peak wavelength priority.

[0084] If the corresponding analysis value among the multiple peak wavelengths before the grouping step is an abnormal analysis value outside the calibration curve range, an inappropriate value omission step may be performed in which only normal analysis values ​​other than the abnormal analysis value are valid.

[0085] This inappropriate value omission process may be performed before the classification process (as shown in Figure 3). If performed before the classification process, it may be possible to reduce the number of candidates for analysis values ​​to be handled after the classification process, thereby reducing the calculation load. Note that the inappropriate value omission process may also be performed on analysis values ​​corresponding to peak wavelengths in order of priority of the peak wavelengths.

[0086] Of the above steps, the analytical value acquisition step requires minimal manual labor to obtain analytical values ​​as results of ICP optical emission spectrometry using known techniques, but the other steps can be automated. While known software can be used on known computer terminals for automation, it is preferable to use an EXPERT system (Symbolic AI). This AI is a rule-based AI, rather than a learning AI such as deep learning.

[0087] The technical scope of the present invention is not limited to the above-described embodiments, but also includes forms in which various modifications and improvements are made within the scope that can derive specific effects obtained by the constituent elements of the invention and their combinations.

[0088] Even if there is only one peak wavelength for a certain element, this embodiment is applicable to other elements, and therefore such cases are also included in the scope of the present invention.

[0089] For example, one of the major features of this embodiment is that the optimum peak wavelength is automatically selected, and therefore this embodiment is also technically significant as a peak wavelength selection method in ICP optical emission spectrometry.

[0090] Furthermore, although this embodiment relates to a method for analyzing the results of ICP atomic emission spectroscopic analysis, this analysis method can be realized by a system or a program that causes a computer to execute the contents of the system.

[0091] An example of the configuration of an analysis system (or peak wavelength selection system) using the method for analyzing the results of ICP optical emission spectroscopy measurement described in this embodiment is as follows: Contents that overlap with the content of the method for analyzing the results of ICP optical emission spectroscopy measurement will be omitted. A peak wavelength acquisition unit that obtains multiple wavelengths with high sensitivity and minimal influence from coexisting elements when measuring each element using ICP optical emission spectroscopy. Priority setting section for multiple peak wavelengths, which prioritizes the wavelengths in order of sensitivity and minimizes the influence of coexisting elements when measuring with ICP optical emission spectroscopy. -Analysis value acquisition unit that obtains analysis values ​​at each of multiple peak wavelengths for each element A grouping section that sorts multiple peak wavelengths into groups with similar analytical values a weighting unit that weights the analysis value based on the analyst's subjective opinion for at least one of the plurality of peak wavelengths; A companion selection section that selects the companion with the highest weighting as a whole by the weighting section. a peak wavelength selection unit that selects the peak wavelength with the highest priority among the peak wavelengths in the group selected by the group selection unit; An analysis value determination unit that adopts an analysis value corresponding to a selected peak wavelength

[0092] A more preferred configuration is as follows. ·Grouping department that performs the grouping process ·Group Effectiveness Evaluation Department, which performs the group effectiveness evaluation process Anomaly detection unit that performs the anomaly detection process - Inappropriate value omission section that performs the inappropriate value omission process

[0093] Each of the above components is controlled by a control unit included in the analysis system for the results of ICP atomic emission spectrometry. In this embodiment, the case where each component is installed in a computer is exemplified. However, some of the components described in this embodiment (for example, a measurement unit when an existing ICP atomic emission spectrometry measurement device is used) may be configured as a separate component connected to a network, rather than being installed in a computer.

[0094] The peak wavelength acquisition unit may be a recording unit (such as a hard disk drive) of a computer. In this case, the data is stored in the hard disk drive. On the other hand, the peak wavelength acquisition unit may be something other than a hard disk drive. For example, the peak wavelength acquisition unit may be configured to have a function of reading the data stored in a cloud connected to a network.

[0095] The analytical value acquisition unit is not limited as long as it can perform ICP optical emission spectroscopic analysis of a sample, and an existing ICP optical emission spectroscopic analysis measurement device may be used.

[0096] The functions of the above components other than the peak wavelength acquisition unit and the analysis value acquisition unit may be performed by a calculation mechanism mounted on a known computer and the above EXPERT system (Symbolic AI).

[0097] It should be noted that the salvage process described in Patent Document 2 may be adopted in this embodiment. For example, if the analysis value is a concentration, if the concentration exceeds a threshold, the companion selection process described in this embodiment is performed, whereas if the concentration is equal to or less than the threshold, the companion selection process described in Patent Document 2 is not performed, but a method (concentration confirmation process, concentration confirmation unit) may be separately adopted.

Claims

1. A method for analyzing analytical values ​​obtained for each element in a measurement object as a result of ICP optical emission spectrometry measurement of the measurement object, comprising: a peak wavelength preparation step of preparing a plurality of wavelengths for each of the elements that are less affected by coexisting elements when subjected to the ICP optical emission spectrometry analysis and have high sensitivity; a priority setting step of setting priorities for the plurality of peak wavelengths in descending order of sensitivity and less influence of coexisting elements when subjected to the ICP optical emission spectrometry; a weighting step of subjectively weighting the analysis value based on an analyst's subjective opinion for at least one of the plurality of peak wavelengths; an analysis value acquisition step of obtaining the analysis value at each of the plurality of peak wavelengths for each of the elements; a grouping step of grouping the plurality of peak wavelengths into groups of wavelengths having similar analytical values; a companion selection step of selecting a companion that has been given the highest weight overall by the weighting step; a peak wavelength selection step of selecting a peak wavelength having the highest priority from among the peak wavelengths in the group selected in the group selection step; an analysis value determination step of adopting an analysis value corresponding to the selected peak wavelength; A method for analyzing the results of ICP optical emission spectrometry analysis.

2. 2. The method for analyzing the results of ICP atomic emission spectrometry according to claim 1, wherein the weighting of the analytical values ​​in the weighting step is performed subjectively by an analyst based on an analyst's empirical rule for selecting peak wavelengths.

3. 3. The method for analyzing the results of ICP optical emission spectrometry according to claim 2, wherein the weighting in the weighting step is performed by assigning points to the peak wavelengths to be weighted.

4. The priority set in the priority setting step is set based on sensitivity as a literature value or sensitivity as a past measured value. The analysis method for the results of ICP optical emission spectroscopy analysis according to any one of claims 1 to 3.

5. the analytical value is a concentration, The weighting of the analysis values ​​in the weighting step is performed based on the analyst's subjective judgment criteria used in selecting peak wavelengths in the past and the analyst's empirical rules for selecting peak wavelengths, The weighting in the weighting step is performed by assigning points to the peak wavelengths to be weighted, 2. The method for analyzing the results of ICP atomic emission spectrometry according to claim 1, wherein the priorities set in the priority setting step are set based on sensitivity as a literature value or sensitivity as a past actual measurement value.

6. A system for analyzing analytical values ​​obtained for each element in a measurement object as a result of ICP optical emission spectrometry measurement of the measurement object, comprising: a peak wavelength acquisition unit that acquires a plurality of wavelengths with high sensitivity and little influence from coexisting elements when subjected to the ICP optical emission spectrometry analysis for each of the elements; a priority setting unit that sets priorities for the plurality of peak wavelengths in descending order of sensitivity and less influence from coexisting elements when subjected to the ICP optical emission spectrometry; a weighting unit that performs subjective weighting of the analysis value based on an analyst's subjective opinion on at least one of the plurality of peak wavelengths; an analysis value acquisition unit that acquires the analysis value at each of the plurality of peak wavelengths for each of the elements; a grouping unit that groups the plurality of peak wavelengths into groups having similar analysis values; a companion selection unit that selects the companions that have been given the highest weighting as a whole by the weighting unit; a peak wavelength selection unit that selects the peak wavelength with the highest priority from among the peak wavelengths in the group selected by the group selection unit; an analysis value determination unit that adopts an analysis value corresponding to the selected peak wavelength; A system for analyzing the results of ICP optical emission spectrometry analysis, comprising:

7. 7. The system for analyzing the results of ICP atomic emission spectrometry analysis according to claim 6, wherein the weighting of the analysis values ​​in the weighting unit is performed subjectively by an analyst based on an analyst's rule of thumb for selecting peak wavelengths.

8. 8. The system for analyzing the results of ICP optical emission spectrometry according to claim 7, wherein the weighting in the weighting section is performed by assigning points to the peak wavelengths to be weighted.

9. The priority set by the priority setting unit is set based on sensitivity as a literature value or sensitivity as a past measured value. The analysis system for the results of ICP optical emission spectrometry analysis according to any one of claims 6 to 8.

10. the analytical value is a concentration, the weighting of the analysis values ​​by the weighting unit is performed based on the analyst's subjective judgment criteria used in selecting peak wavelengths in the past and the analyst's rule of thumb for selecting peak wavelengths; the weighting in the weighting unit is performed by assigning points to the peak wavelengths to be weighted; 7. The system for analyzing the results of ICP atomic emission spectrometry according to claim 6, wherein the priorities set by the priority setting unit are set based on sensitivity as a literature value or sensitivity as a past actual measurement value.

Images