JP2007024679A - Analyzer and analyzing processing method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an analyzer capable of simply judging the quality of an analytic result to simply find out the point at issue representing negative and an analyzing processing method. <P>SOLUTION: In an analytic result judging part 44, the quality of the analytic result of this time is judged on the basis of a criterion for judging the quality of measured data becoming the base of analysis stored in a first data memory part 43 and, in a solving method exhibiting part 46, the dissolving method to the point at issue of the analyzing result of this time is exhibited on the basis of the past point at issue and the data of the resolving method related to each other stored in a second data memory part 45. Accordingly, the quality of the analyzed result is simply judged to simply find out the point at issue becoming no. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to an analysis apparatus and an analysis processing method for performing a predetermined analysis, and more particularly to a technique for performing the predetermined analysis based on analysis conditions.

  As an analyzer, a high-frequency plasma emission analyzer will be described as an example. A high-frequency plasma optical emission spectrometer separates light emitted from a sample in plasma and performs quantitative analysis using spectral lines obtained by the spectroscopy. For example, a sequential type high-frequency plasma emission analyzer performs quantitative analysis while moving an optical system typified by a diffraction grating. On the other hand, the simultaneous analysis type high-frequency plasma emission spectrometer is equipped with a multi-channel detector, and simultaneously collects measurement data represented by spectral lines etc. for all the analysis elements and wavelengths within the measurement wavelength range of the device at the same time. Can be acquired.

  Then, analysis conditions (that is, analysis parameters) are set, and analysis is performed based on the acquired measurement data and analysis conditions. More specifically, for example, an analysis element or wavelength is set as an analysis condition, information such as a calibration curve or profile for the element / wavelength is acquired, and the element concentration in the sample calculated from the information is output. To do. Then, the analyst refers to these, and determines the quality of the analysis result.

  When a problem is found in the analysis result, that is, when it is determined that the analysis result is NO, the analyst specifies the cause of the problem. Then, (α) whether to solve the problem by newly setting the analysis parameters and recalculating the measurement data acquired this time without newly acquiring the measurement data, or (β) re-measurement of the sample The analyst determines whether it is necessary to acquire new measurement data and solves the problem.

  However, it is difficult for an analyst who has little analysis experience to judge the quality of the analysis result from information such as a calibration curve and a profile. Furthermore, even when a problem is found, it is difficult to determine whether (α) recalculation can solve the problem or (β) re-measurement of the sample is necessary.

  The present invention has been made in view of such circumstances, and provides an analysis apparatus and an analysis processing method that can easily determine the quality of an analysis result and easily find a problem that is rejected. For the purpose.

In order to achieve such an object, the present invention has the following configuration.
In other words, the invention described in claim 1 is an analyzer that includes analysis condition setting means for setting analysis conditions, and performs a predetermined analysis based on the analysis conditions set by the analysis condition setting means. First information storage means for preliminarily storing judgment criteria for judging the quality of the measurement data used as a basis, and analysis for judging the quality of the current analysis result based on the judgment criteria stored in the first information storage means The result determination means, the second information storage means for storing information in advance by associating the past problems that are rejected when the analysis result is negative and the solutions to the problems, and the information stored in the second information storage means And a solution presentation means for presenting a solution to the problem of the analysis result of this time based on the associated past problem and information of the solution. It is.

  [Operation / Effect] According to the first aspect of the present invention, when performing a predetermined analysis based on the analysis condition set by the analysis condition setting means, the analysis result determination means is stored in the first information storage means. The quality of the current analysis result is judged based on the judgment criteria for judging the quality of the measurement data that is the basis of the analysis. Therefore, even an analyst with little analysis experience can easily determine the quality of the analysis result. Then, the solution presentation means presents a solution to the problem of the current analysis result based on the past problem and solution information associated with each other stored in the second information storage means. Therefore, even an analyst with little analysis experience can easily find a problem that is not acceptable.

  In the above-described invention, there is no need to newly measure and acquire measurement data as a basis of analysis, and when the analysis result becomes good by setting a new analysis condition and performing the analysis, the above-described solution From the current problem and solution presented by the method presenting means, select the new analysis condition described above, recalculate the current analysis result based on the new analysis condition, and measure the above-described measurement. Preferably, each means is configured to obtain a new analysis result without newly measuring and acquiring data (the invention according to claim 2). With this configuration, if the analysis result is good by setting a new analysis condition and performing the analysis, a new analysis result is obtained without newly measuring and acquiring measurement data. be able to. Then, the obtained new analysis result is good.

  The means for outputting the current problem and the solution presented by the solution presenting means in the present invention may be separate from the apparatus or may be provided in the apparatus. When provided in the apparatus, a typical example of the output means is a display means for displaying the current problem and the solution (the invention according to claim 3). By providing such a display means, the analyst can easily browse the display of the problem and the solution. The output means is not limited to the display means for performing output display, and may be a means for output printing (for example, a printer).

  Further, the first information storage means and / or the second information storage means described above may be configured to be rewritable with the latest information (the invention according to claim 4). Thus, each storage means is configured to be rewritable so that the analysis result determination means always refers to the latest information in the case of the first information storage means and the solution presentation means in the case of the second information storage means. In the case of the first information storage means, it is possible to accurately determine the quality of the analysis result, and in the case of the second information storage means, it is possible to accurately find the problem that is negative.

  Further, an example of the predetermined analysis is an analysis in which measurement data as a basis of analysis is measured and the measurement data is collectively acquired (the invention according to claim 5). In the case of such analysis, after obtaining measurement data collectively, an analysis result is obtained based on the measurement data and analysis conditions. Therefore, when obtaining analysis results corresponding to individual analysis conditions, the analysis results are obtained based on the same measurement data and individual analysis results, so the measurement data is measured again, that is, the sample is remeasured. There is no need to do it. In particular, when the invention described in claim 6 is subordinate to the invention described in claim 2, a new analysis result can be obtained using only the same measurement data.

  Further, an example of the analysis for acquiring the measurement data collectively is a simultaneous analysis type high-frequency plasma emission analysis that includes a multi-channel detector and can simultaneously acquire the measurement data within the measurement wavelength range. Described invention). The analyzer according to the present invention is used as an apparatus for performing such high-frequency plasma emission analysis. In the case of a simultaneous analysis type high-frequency plasma emission analysis apparatus, since a multi-channel type detector is provided, measurement data represented by spectral lines and the like can be simultaneously acquired.

  The invention according to claim 7 is an analysis processing method for executing a series of analysis processes including an analysis process for performing a predetermined analysis based on the set analysis conditions, wherein the analysis conditions for setting the analysis conditions This analysis result based on the setting process, the analysis process that performs a predetermined analysis based on the analysis conditions set in the analysis condition setting process, and the criteria for determining the quality of the measurement data that is the basis of the analysis When the analysis result determination step for determining pass / fail of the past, the past problem that is rejected when the analysis result is negative, and the solution to the problem are associated with each other, the associated past problem and And a solution presentation step for presenting a solution to the problem of the analysis result based on information on the solution.

  [Operation / Effect] According to the invention described in claim 7, a predetermined analysis is performed in the analysis step based on the analysis condition set in the analysis condition setting step, and the quality of the measurement data serving as the basis of the analysis is judged. On the basis of the determination criteria, the quality of the current analysis result is determined in the analysis result determination step. Therefore, even an analyst with little analysis experience can easily determine the quality of the analysis result. And the solution method with respect to the problem of this analysis result is shown in a solution method presentation process based on the information of the past problem and solution method linked | related with each other. Therefore, even an analyst with little analysis experience can easily find a problem that is not acceptable.

  Further, the invention according to claim 8 is the analysis processing method according to claim 7, wherein it is not necessary to newly measure and acquire the measurement data, and by performing analysis by setting new analysis conditions. When the analysis result is good, the analysis condition resetting step for selecting and resetting the new analysis condition from the current problem and the solution presented in the solution presentation step; A recalculation step for recalculating the current analysis result based on the new analysis condition, and an analysis result re-derivation step for obtaining a new analysis result without newly measuring and acquiring the measurement data. It is a feature.

  [Operation / Effect] According to the invention described in claim 8, in the case where the analysis result is good by setting the new analysis condition and performing the analysis by providing such a process, the measurement is performed. A new analysis result can be obtained in the analysis result re-derivation step without newly measuring and acquiring data. Then, the obtained new analysis result is good.

  Note that the present specification also discloses the following analysis processing method, analysis processing program, and invention relating to an analysis processing storage medium.

  (1) The analysis processing method according to claim 7 or 8, further comprising a display step for displaying the current problem and the solution presented in the solution presentation step. .

  According to the invention described in (1) above, the analyzer can easily browse the display of the problem and the solution by providing the display step.

  (2) In the analysis processing method according to any one of claims 7, 8 and (1), the predetermined analysis is detected by a multi-channel detector and measured data within a measurement wavelength range. An analysis processing method characterized by being a simultaneous analysis type high-frequency plasma emission analysis capable of simultaneously acquiring the same.

  According to the invention described in (2) above, measurement data typified by spectral lines and the like can be simultaneously acquired simultaneously by a multi-channel detector.

  (3) An analysis processing program for causing a computer to execute a series of analysis processes including an analysis process for performing a predetermined analysis based on set analysis conditions, the analysis condition setting process for setting analysis conditions; Based on the analysis conditions set in the analysis condition setting process, the quality of the current analysis results is judged based on the analysis process for performing a predetermined analysis and the judgment criteria for judging the quality of the measurement data that is the basis of the analysis. When the analysis result determination step to be performed and the past problem that is rejected when the analysis result is negative and the solution to the problem are associated with each other, the associated past problem and solution information And a computer that performs an analysis process including a solution presentation step for presenting a solution to the problem of the analysis result based on That analysis processing program.

  According to the invention described in (3) above, by causing the computer to perform an analysis process including these steps, it is possible to easily determine whether the analysis result is good or not, and to easily find the problem that is rejected. .

  (4) In the analysis processing program described in (3) above, when it is not necessary to newly measure and acquire the measurement data, and analysis is performed by setting a new analysis condition and performing analysis. Is based on the analysis condition resetting step of selecting and resetting the new analysis condition from the current problem and the solution presented in the solution presentation step, and the new analysis condition The analysis processing further includes a recalculation step for recalculating the analysis result of this time, and an analysis result re-derivation step for obtaining a new analysis result without newly measuring and acquiring the measurement data. An analysis processing program for causing a computer to execute.

  According to the invention described in (4) above, when the analysis result is good by setting the new analysis condition and performing the analysis by causing the computer to execute such a process, the measurement data It is possible to obtain a new analysis result in the analysis result re-derivation step without newly measuring and acquiring. Then, the obtained new analysis result is good.

  (5) The analysis processing program according to (3) or (4) further includes a display step for displaying the current problem and the solution presented in the solution presentation step in the analysis processing, An analysis processing program for causing a computer to execute analysis processing.

  According to the invention described in (5) above, by causing the computer to execute the display step, the analyst can easily view the display of the problem and the solution.

  (6) In the analysis processing program according to any one of (3) to (5), the predetermined analysis can be detected by a multi-channel detector, and measurement data within a measurement wavelength range can be simultaneously acquired. Analysis processing program characterized by being a simultaneous analysis type high-frequency plasma emission analysis.

  According to the invention described in (6) above, measurement data represented by spectral lines and the like can be simultaneously acquired simultaneously by a multi-channel detector.

  (7) A computer-readable analysis processing storage medium recording a program for causing a computer to execute a series of analysis processes including an analysis step for performing a predetermined analysis based on set analysis conditions, An analysis condition setting process for setting analysis conditions, an analysis process for performing a predetermined analysis based on the analysis conditions set in the analysis condition setting process, and a criterion for determining the quality of measurement data that is the basis of the analysis The analysis result determination step for determining the quality of the current analysis result based on the above, the past problem that is rejected when the analysis result is negative, and the solution to the problem are associated with each other. A solution presentation step for presenting a solution to the problem of the analysis result based on the past problem information and solution information obtained. Analysis processing storage medium characterized by recording a program for executing the analysis process on the computer.

  According to the invention described in (7) above, by causing the computer to perform an analysis process including these steps, it is possible to easily determine whether the analysis result is good or not, and to easily find a problem that is rejected. .

  (8) In the analysis processing storage medium according to (7), it is not necessary to newly measure and acquire the measurement data, and the analysis result is improved by performing analysis by setting new analysis conditions. In the case, the analysis condition resetting step of selecting and resetting the new analysis condition from the current problem and the solution presented in the solution presentation step, and the new analysis condition The analysis process further includes a recalculation step for recalculating the present analysis result based on this, and an analysis result re-derivation step for obtaining a new analysis result without newly measuring and acquiring the measurement data. An analysis processing storage medium for recording a program for causing a computer to execute processing.

  According to the invention described in (8) above, when the analysis result is good by setting the new analysis condition and performing the analysis by causing the computer to execute such a process, the measurement data It is possible to obtain a new analysis result in the analysis result re-derivation step without newly measuring and acquiring. Then, the obtained new analysis result is good.

  (9) In the analysis processing storage medium according to (7) or (8), the analysis processing further includes a display step for displaying the current problem and the solution presented in the solution presentation step, An analysis processing storage medium for recording a program for causing a computer to execute the analysis processing.

  According to the invention described in (9) above, by causing the computer to execute the display step, the analyst can easily view the display of the problem and the solution.

  (10) In the analysis processing storage medium according to any one of (7) to (9), the predetermined analysis is detected by a multi-channel detector, and measurement data within a measurement wavelength range is simultaneously acquired. An analysis processing storage medium characterized by being capable of simultaneous analysis type high frequency plasma emission analysis.

  According to the invention described in (10) above, measurement data represented by spectral lines and the like can be simultaneously acquired simultaneously by a multi-channel detector.

  According to the analysis apparatus and the analysis processing method according to the present invention, the analysis result determination means is based on the determination criteria for determining the quality of the measurement data that is the basis of the analysis stored in the first information storage means. The analysis method determination unit determines whether the analysis result is good or not, and the solution presentation unit determines a solution for the problem of the current analysis result based on the past problem and the solution information stored in the second information storage unit. Present. Therefore, it is possible to easily determine whether the analysis result is good or not, and to easily find the problem that is rejected.

Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 is a block diagram illustrating an outline of the analyzer according to the embodiment. In this example, as an analysis, simultaneous analysis type high frequency plasma emission analysis (hereinafter referred to as “Echelle type high frequency plasma emission analysis”) using an echelle spectroscope capable of acquiring measurement data in a lump. (Abbreviated) will be described as an example.

  As shown in FIG. 1, the echelle-type high-frequency plasma emission analysis is performed by quantitatively analyzing the spectral lines L emitted from the sample S in the plasma using a diffraction grating G which is a dispersion element utilizing the diffraction effect of light. Do. More specifically, the analyzer 1 that performs an echelle-type high-frequency plasma emission analysis includes a light source unit 10, a spectroscopic unit 20, a photometric unit 30, and an analysis processing control unit 40.

  The light source unit 10 includes a plasma processing chamber that generates plasma generated by argon (Ar) gas, a plasma torch, and a high-frequency power source, and introduces the sample S into the plasma processing chamber. Sample S is a solution sample or the like. When the sample S is introduced into the light source unit 10, it is vaporized by the high temperature plasma to be in an atomic state and excited simultaneously. The atom in the excited state emits light peculiar to each element as the spectral line L when the state transitions from the excited state to the steady state.

  The spectroscopic unit 20 includes a diffraction grating G and an order separation diffraction grating 21, and spectral lines L are split by the gratings G and 21.

  The photometry unit 30 is composed of a multi-channel type detector such as a CCD camera or a line sensor, and converts each separated light into an electric signal. The intensity for each wavelength of light based on the electrical signal is sent to the analysis processing control unit 40 as measurement data. This measurement data is data that is the basis of analysis.

  The analysis processing control unit 40 is configured by a personal computer, and includes an analysis parameter setting unit 41, an analysis result deriving unit 42, a first information storage unit 43, an analysis result determination unit 44, a second information storage unit 45, and a solution presentation unit 46. And a monitor 47. The analysis parameter setting unit 41, the analysis result deriving unit 42, the analysis result determining unit 44, and the solution presentation unit 46 are configured by a central processing unit (CPU) or the like, and include a first information storage unit 43 and a second information storage. The unit 45 includes a storage medium represented by ROM (Read-only Memory), RAM (Random-Access Memory), and the like.

  The analysis parameter setting unit 41 sets analysis parameters (that is, analysis conditions) such as elements and wavelengths to be analyzed. The analysis parameter setting unit 41 sets analysis parameters based on input data from an input unit (not shown). This input unit is configured by a pointing device represented by a mouse, a keyboard, a joystick, a trackball, a touch panel, and the like. Specific functions of the analysis parameter setting unit 41 in this embodiment will be described later. The analysis parameter set by the analysis parameter setting unit 41 is sent to the analysis result deriving unit 42. The analysis parameter setting unit 41 corresponds to the analysis condition setting means in this invention.

  The analysis result deriving unit 42 calculates the light intensity to the concentration based on the analysis parameter set by the analysis parameter setting unit 41 and the measurement data measured by the photometry unit 30 to obtain the analysis result. Specific functions of the analysis result deriving unit 42 in this embodiment will be described later. The analysis result obtained by the analysis result deriving unit 42 is sent to the analysis result determining unit 44.

  The 1st information storage part 43 memorizes beforehand the judgment standard for judging the quality of the measurement data used as the basis of analysis. The criteria for judgment in this embodiment will be described later. The determination criterion stored in the first information storage unit 43 is sent to the analysis result determination unit 44. The first information storage unit 43 corresponds to the first information storage means in this invention.

  Note that, by configuring the first information storage unit 43 with a rewritable storage medium such as a RAM, the contents can be updated to the latest information. The update method may be batch rewriting by a device manufacturer or the like, or may be a self-learning type.

  The analysis result determination unit 44 determines pass / fail of the current analysis result based on the information of the determination criterion stored in the first information storage unit 43. A specific configuration of the analysis result determination unit 44 in this embodiment will be described later. The quality of the current analysis result determined by the analysis result determination unit 44 is sent to the solution presentation unit 46. The analysis result determination unit 44 corresponds to the analysis result determination means in this invention.

  The second information storage unit 45 stores information in advance by associating past problems that are rejected when the analysis result is negative and solutions to the problems. Information on the associated past problems and solutions in this embodiment will be described later. Information on past problems and solutions stored in the second information storage unit 45 is sent to the solution presentation unit 46. The second information storage unit 45 corresponds to the second information storage means in this invention. Note that the second information storage unit 45 may also be configured by a rewritable storage medium such as a RAM similarly to the first information storage unit 43.

  The solution presentation unit 46 determines whether the current analysis result determined by the analysis result determination unit 43 is good or bad based on the associated past problem and solution information stored in the second information storage unit 45. A solution to the problem that will be rejected is presented. A specific configuration of the solution presentation unit 46 in the present embodiment will be described later. The problem presented by the solution presentation unit 46 and the solution are sent to the monitor 47. The solution presentation unit 46 corresponds to the solution presentation unit in the present invention.

  In addition, it is not necessary to newly measure and acquire measurement data as a basis of analysis by the photometry unit 30, and a new analysis parameter is set by the analysis parameter setting unit 41 and calculation processing is performed. In this case, the problem and the solution presented by the solution presentation unit 46 are also sent to the analysis parameter setting unit 41. Then, the analysis parameter setting unit 41 selects and resets a new analysis parameter from the current problem and the solution. Then, the analysis parameter reset by the analysis parameter setting unit 41 is sent to the analysis result deriving unit 42, and the analysis result deriving unit 42 obtains the measurement data based on the analysis parameter reset by the analysis parameter setting unit 41. Recalculate and obtain new analysis results without newly measuring and acquiring.

  The monitor 47 displays the current problem and the solution presented by the solution presentation unit 46. The current problem and solution displayed on the monitor 47 in this embodiment will be described later. The monitor 47 corresponds to the display means in this invention.

  Next, the analysis processing method according to the present embodiment will be described with reference to the flowchart of FIG. 2 and the explanatory diagrams of FIGS. FIG. 2 is a flowchart of an analysis processing method according to the present embodiment, FIG. 3 is an explanatory diagram of a calibration curve, FIGS. 4 to 7 are explanatory diagrams of profiles, and FIG. FIG. 9 is an explanatory diagram of information that associates past problems that are rejected when the analysis result is negative and a solution to the problem with each other. FIG. 10 is an explanatory diagram related to the display of the present problem and solution presented, and FIG. 11 is an explanatory diagram related to a display for setting a new analysis parameter.

(Step S1) Acquisition of Measurement Data First, in order to obtain an analysis result, the photometry unit 30 obtains measurement data as a basis for analysis. This measurement data is obtained as the intensity corresponding to the light for each of a plurality of wavelengths that are two-dimensionally developed and split by the diffraction grating G or the like.

(Step S2) Analysis Parameter Setting The element and wavelength to be analyzed are set as analysis parameters. For example, when the element to be quantitatively analyzed is aluminum (Al), the Al to be analyzed is set and the value assumed for the wavelength of Al is set. Based on the set input data, the analysis parameter setting unit 41 sets an analysis parameter and sends it to the analysis result deriving unit 42. This step S2 corresponds to the analysis condition setting step in the present invention. In this embodiment, the measurement data is acquired in step S1, and then the analysis parameter is set in step S2. However, after setting the analysis parameter in step S2, the measurement data is acquired in step S1, and the next step S3 is performed. Analysis may be performed at

(Step S3) Analysis Based on the analysis parameters set by the analysis parameter setting unit 41 and the measurement data measured by the photometry unit 30, the analysis result deriving unit 42 calculates light intensity to concentration. In this analysis, for example, a calibration curve based on the measurement of a sample having a known concentration shown in FIG. 3 and a profile shown in FIG. 4 are created, and the analysis is performed based on the created calibration curve and profile. Alternatively, a profile is created, and analysis is performed based on the created profile or a calibration curve created in advance.

  The element has a specific sensitivity for each wavelength. In the calibration curve, the horizontal axis represents the concentration (Al concentration in FIG. 3), and the vertical axis represents the intensity corresponding to the concentration (Al intensity I in FIG. 3). When the element Al is set and a wavelength of a certain predetermined value is set, a graph of a calibration curve according to the set element Al and the set wavelength of the predetermined value (see FIG. 3) Then, based on the intensity measured by the photometry unit 30, the Al concentration is obtained.

In the profile, the horizontal axis represents the wavelength (the actual wavelength of Al in FIG. 4), and the vertical axis represents the intensity corresponding to the wavelength (the Al intensity I in FIG. 4). The wavelength λ ₁ where the intensity is at a peak is the actual wavelength. By the way, there is a case where a unique intensity is superimposed on the profile of FIG. 4 as a background from a gas (for example, argon (Ar)) that generates plasma or an element contained in a large amount in a sample. Also, the intensity of the background may change depending on the wavelength. The slope of the change with respect to this wavelength is d in FIG. In these cases, “background correction” is performed for correction based on the background value BG and the gradient d, which are superimposed intensities. The profile after the background correction is a graph as shown in FIG.

Further, as shown in FIG. 6, there may be two or more peaks in the profile. In this case, one of the two or more existing peaks corresponds to the wavelength of the element to be analyzed (Al in FIG. 6), and the remaining peaks are elements close to the wavelength of the element to be analyzed (“ Corresponding to the wavelength of “interfering element” or “coexisting element”). Therefore, a profile relating to the interfering element is created as shown in FIG. 7, and the concentration of the interfering element is obtained at another wavelength λ ₃ , whereby the interfering element in the profile of the wavelength λ ₂ superimposed on FIG. The spectrum is estimated and “inter-element correction” is performed by subtracting and correcting the spectrum from FIG.

  Based on these calibration curves and profiles, the concentration of the element to be analyzed is obtained for analysis. The analysis result deriving unit 42 sends these analysis results to the analysis result determining unit 44. This step S3 corresponds to the analysis step in this invention.

(Step S4) Analysis Result Determination On the other hand, the first information storage unit 43 stores determination criteria for determining the quality of measurement data that is the basis of analysis, for example, as shown in FIG.

  Specifically, the judgment criteria are divided into three patterns, the pattern judged from the hardware status of the detector and other devices, the pattern judged from the measurement data profile from the mathematical point of view, and the known spectrum of each element It can be divided from the state of empirical patterns accumulated empirically. In each determination criterion item, a determination point, a state for determining pass / fail for the point, and a reference value are registered.

  For example, “there is an overflowing element” in the problem in FIG. 8 is when the detection capability of the detector of the photometry unit 30 (for example, a photodiode of a CCD or a charge-voltage converter) is exceeded. That is, based on the performance of the detector, it is determined whether or not the intensity overflows in the current analysis result. The judgment criterion in FIG. 8 is “intensity upper limit A or more due to detector performance”. A is an overflow threshold (predetermined value). This criterion is an example of a pattern determined from the hardware state of a device such as a detector.

  For example, the problem in FIG. 8 is that “the correct value of the intensity of the analytical element cannot be obtained with respect to the background and spectral interference” is subject to analysis due to the background due to the gas generating the plasma and interference due to the spectral. This is when the strength of the element decreases. A predetermined value is determined in advance from past values, and if it is less than the predetermined value, it is determined that a correct value cannot be obtained. The criterion in FIG. 8 is “the strength of the analytical element is I or less”. I is the predetermined value described above. This criterion is an example of a pattern determined from a mathematical viewpoint from the profile of measurement data.

  For example, “the background varies” in the problem in FIG. 8 is when the intensity varies strongly in the vicinity of the peak due to the background in FIG. At this time, the intensity variation overlaps the measured intensity. The background is presumed to be flat to some extent. Originally, it would be desirable to obtain the background value BG at the peak, but when the fluctuation is not flat, the peak cannot be measured. Get the value BG. Therefore, if the background value BG has only an influence below the predetermined value with respect to the accuracy of the determined intensity, there is no background fluctuation, but if there is an influence above the predetermined value, the background fluctuates. As described above, background correction is performed. That is, it is determined whether the intensity is insufficient or appropriate for the background value BG. The criterion in FIG. 8 is “background gradient is d or more”.

  For example, in the problem in FIG. 8, “there is spectral interference from coexisting elements” means that the peak of the coexisting element, that is, the interfering element is in the vicinity of the peak of the element to be analyzed, and the intensity of the element wavelength to be analyzed ( Or the concentration). From the profile in FIG. 6, when the intensity (or concentration) of the interfering element with respect to the intensity (or concentration) of the element wavelength to be analyzed is equal to or greater than a predetermined value, it is determined that there is an influence of interference. The criterion in FIG. 8 is “the analysis value of the interfering element is A or more” (where A is a predetermined value). This criterion is an example of a pattern that is empirically accumulated from a known spectrum state of each element.

  For example, “sample concentration is inappropriate” in the problem in FIG. 8 is when the concentration is not within the calibration range in FIG. For example, it is determined whether or not the upper and lower concentration ranges of the created calibration curve are exceeded. The criterion in FIG. 8 is “analysis value is out of confidence range of calibration curve”.

  For example, in the problem in FIG. 8, “high concentration element Na may have an influence on the analysis value” means that when the sample contains seawater, sodium (Na) as the main component of seawater It is when it is influenced by. At this time, the plasma state changes due to the influence of Na, and the sensitivity is affected. It is determined whether or not it is affected by Na based on past analysis results (for example, data relating to the concentration of high concentration element Na). The criterion in FIG. 8 is “the concentration of the high concentration element Na is C or more”. C is a predetermined value related to density.

  In the present analysis result performed in the analysis of step S3, the analysis result determination unit 44 determines the quality of these analysis results. Then, the quality of the current analysis result is sent to the solution presentation unit 46. This step S4 corresponds to the analysis result determination step in the present invention.

(Step S5) Is there a problem?
If there is a problem that the analysis result is negative, the process proceeds to the next step S6. If the analysis result is good, the series of analysis processing ends.

  For example, if the strength overflows in the current analysis result, it is determined that there is a problem (no). If the intensity of the element to be analyzed decreases due to the background due to the gas that generates plasma or interference due to spectroscopy, it is determined that there is a problem (no) if it is below a predetermined value. If the background gradient exceeds a predetermined value, it is determined that there is a problem (no). If the peak of the interfering element is in the vicinity of the peak of the element to be analyzed and the analytical value of the interfering element is not less than a predetermined value, it is determined that there is a problem (no). If it is outside the concentration range in the calibration curve, it is determined that there is a problem (no). If the influence of Na is too great, it is determined that there is a problem (no).

(Step S6) Presentation of Problem and Solution On the other hand, in the second information storage unit 45, information (table that correlates past problems that are rejected when the analysis result is negative and solutions to the problems are associated with each other. ) Is stored as shown in FIG. 9, for example.

  For example, the problem in Figure 9 is “There is an overflowing element. ], The sensitivity may be too high at the set wavelength and the intensity may overflow. In this case, it is not necessary to newly measure and acquire the measurement data in step S1, and the analysis wavelength setting unit 41 resets the analysis wavelength with lower sensitivity as the analysis parameter, and the analysis result of this time is the analysis result. This can be solved by performing recalculation in the derivation unit 42. Therefore, the solution shown in Fig. 9 may be solved by adding a less sensitive analysis wavelength. Recalculation is possible without re-measurement. The system selects the analysis wavelength. "There is an overflowing element." ] Is stored in the second information storage unit 45 in advance.

  Also for other problems, solutions to the problem are associated with each other and stored in advance in the second information storage unit 45 as a table in FIG.

  Note that “Sample concentration is inappropriate.” In the case of “”, it is necessary to remeasure in step S1. The system estimates the calibration curve concentration. “The sample concentration is inappropriate. ] Is stored in the second information storage unit 45 in advance.

  These associated problems and solutions are read from the second information storage unit 45, and the problem presentation unit 46 presents the problems of the analysis result this time and the solutions for the problem. The solution presentation unit 46 sends the information to the monitor 47, and the monitor 47 displays the presented current problem and the solution as shown in FIG. 10, for example. This step S6 corresponds to the solution presentation step and the display step in the present invention.

(Step S7) Solved by recalculation?
When solving by recalculation, for example, as shown in Fig. 9 and Fig. 10, the problem is "There is an overflowing element. If the solution is solved by resetting the analysis wavelength with lower sensitivity as the analysis parameter and performing recalculation, the process proceeds to the next step S8. If the problem cannot be solved even by recalculation, the process returns to the acquisition of measurement data in step S1.

(Step S8) Analytical parameter resetting When solving by recalculation, that is, there is no need to newly measure and acquire measurement data in step S1, and the analysis result is good by setting a new analytical parameter and performing the analysis. In this case, a new analysis parameter is selected and reset from the current problem and the solution presented by the solution presentation unit 46.

  For example, there is a problem “There is an overflowing element on the monitor 47 in FIG. ”And a solution“ There is a possibility to solve by adding a less sensitive analysis wavelength. Recalculation is possible without re-measurement. The system selects the analysis wavelength. Is displayed. In addition to this, the sample name and the element to be analyzed (cadmium (Cd) in the case of FIG. 10) are displayed, and the wavelength set in step S2 is displayed. Further, as shown in FIG. 10, a “solve” button is provided at the right end portion of the monitor, and this button is constituted by a touch panel. By depressing this button and selecting a solution method, an analysis parameter corresponding to the solution method is newly set. In the case of FIG. 10, the analysis parameter setting unit 41 resets an analysis wavelength with lower sensitivity as an analysis parameter.

  When resetting by the analysis parameter setting unit 41, for example, the additional wavelength is displayed on the monitor 47 in FIG. 11, and “Cancel” for canceling the resetting and “OK” button for resetting are displayed. To do. These buttons are also constituted by a touch panel. A new analysis parameter is reset by pressing the “OK” button. In the case of FIG. 11, a wavelength with lower sensitivity is set as an additional wavelength, and the additional wavelength is set as a new analysis parameter.

  Thus, the problem and the solution presented by the solution presentation unit 46 are sent to the analysis parameter setting unit 41, and when the “OK” button is pressed, the analysis parameter setting unit 41 causes the current problem and solution. Select a new analysis parameter from the method and reset it. Then, the analysis parameter reset by the analysis parameter setting unit 41 is sent to the analysis result deriving unit 42. This step S8 corresponds to the analysis condition resetting step in the present invention.

(Step S9) Recalculation of Analysis Result The analysis result deriving unit 42 recalculates based on the analysis parameter reset by the analysis parameter setting unit 41. This step S9 corresponds to a recalculation process in the present invention.

(Step S10) Re-derivation of analysis result Then, a new analysis result is obtained from the recalculation. This step S10 corresponds to the analysis result re-derivation step in the present invention.

  According to the analysis apparatus 1 according to the above-described embodiment, when performing a predetermined analysis (high-frequency plasma issuance analysis in this embodiment) based on the analysis parameter (analysis condition) set by the analysis parameter setting unit 41, The analysis result determination unit 44 determines the quality of the current analysis result based on the determination criteria for determining the quality of the measurement data that is the basis of the analysis stored in the first information storage unit 43. Therefore, even an analyst with little analysis experience can easily determine the quality of the analysis result. Then, the solution presentation unit 46 presents a solution to the problem of the current analysis result based on the past problem and solution information associated with each other stored in the second information storage unit 45. Therefore, even an analyst with little analysis experience can easily find a problem that is not acceptable.

  In this example, it is not necessary to newly measure and acquire measurement data that is the basis of analysis, and when the analysis result is good by setting a new analysis parameter and performing analysis, a solution is presented. The new analysis conditions described above are selected from the current problems and solutions presented by the unit 46, and the current analysis results are recalculated based on the new analysis conditions. Each means of the analysis processing control unit 40 is configured so as to obtain a new analysis result without newly measuring and acquiring. With this configuration, when the analysis result is good by setting a new analysis parameter and performing the analysis, a new analysis result is obtained without newly measuring and acquiring measurement data. be able to. Then, the obtained new analysis result is good.

  Further, in this embodiment, the monitor 47 that displays the current problem and the solution can be provided so that the analyst can easily view the display of the problem and the solution.

  Further, since the echelle-type high-frequency plasma emission analysis as in this embodiment is provided with a multi-channel type detector such as a CCD camera or a line sensor, it is possible to simultaneously acquire measurement data in a batch. . In the case of the simultaneous analysis type represented by the analysis using such an echelle spectroscope, measurement data is also acquired for other wavelengths of the target peak at the same time. Spectral interference information used for inter-element correction can be obtained by using the recalculation to improve the analysis result or by comparing with data at other wavelengths. Thus, it is useful to apply to simultaneous analysis type high frequency plasma emission analysis.

  The present invention is not limited to the above-described embodiment, and can be modified as follows.

  (1) In the above-described embodiments, the echelle type high-frequency plasma emission analysis has been described as an example. However, a simultaneous analysis type high-frequency plasma emission analysis other than the echelle type may be used. In addition to the simultaneous analysis type high frequency plasma emission analysis, a sequential type high frequency plasma emission analysis may be used. Furthermore, the analysis is not particularly limited as long as it is an analysis other than the high-frequency plasma emission analysis, and an analysis parameter is set and a predetermined analysis is performed based on the analysis parameter. For example, a chromatographic analyzer for analyzing a compound produced in a resin particle by placing a resin particle for solid phase reaction in a reaction vessel, injecting a reagent or a solvent into the reaction vessel to advance the solid phase reaction. This invention can also be applied. In addition, the present invention can also be applied to an analysis device such as a thermal analysis calorimeter, a radiation foreign matter detection device that detects, for example, foreign matter in food with radiation, a viscosity distribution measurement device, and an odor identification device.

  (2) To execute the above-described embodiment, an analysis processing program for executing steps S1 to S10 or an analysis processing storage medium storing a program for executing steps S1 to S10 may be used. In the case of an analysis processing program, such a program is downloaded (acquired) to the analysis apparatus via a telecommunication line (for example, RS-232C standard cable or LAN (Local Area Network) cable), and the program is downloaded by a personal computer. What is necessary is just to make the comprised analysis process control part 40 perform. In the case of an analysis processing storage medium, the above-described analysis processing program is stored in advance in a storage medium such as a ROM or RAM, and the program stored in the storage medium is read by the analysis processing control unit 40. Just execute.

  (3) In the above-described embodiment, when it is not necessary to newly measure and acquire measurement data and the analysis result is good by performing analysis by setting a new analysis condition, a new analysis parameter is obtained. However, it is not always necessary to have the functions of resetting and recalculation.

  (4) In the embodiment described above, the display means represented by a monitor or the like is provided as an output means for outputting the present problems and solutions presented here, but it is a means for output printing (for example, a printer). May be. Alternatively, a monitor or printer may be externally attached to the analyzer, and the solution presentation unit in the analyzer may send output data to the external monitor or printer.

  (5) As described in the above-described embodiments, either the first information storage unit 43 or the second information storage unit 45, or the first information storage unit 43 and the second information storage unit 45 are updated with the latest information. The information may be rewritable. In the case of such a configuration, the storage units 43 and 45 use RAM instead of ROM. By configuring each of the memories 43 and 45 to be rewritable in this way, the analysis result determination unit 44 in the case of the first information storage unit 43 and the solution presentation unit 46 in the case of the second information storage unit 45 are updated. You can always refer to the information. In the case of the first information storage unit 43, it is possible to accurately determine the quality of the analysis result, and in the case of the second information storage unit 45, it is possible to accurately find the problem that is not acceptable.

It is a block diagram which shows the outline of the analyzer which concerns on an Example. It is a flowchart of the analysis processing method which concerns on an Example. It is explanatory drawing of a calibration curve. It is explanatory drawing of a profile. It is explanatory drawing of a profile. It is explanatory drawing of a profile. It is explanatory drawing of a profile. It is explanatory drawing of the criteria for judging the quality of the measurement data used as the basis of analysis. It is explanatory drawing of the information which linked | related the past problem which becomes no in the case of an analysis result, and the solution method with respect to the problem. It is explanatory drawing regarding the display of the present problem and the solution method which were shown. It is explanatory drawing regarding the display which sets a new analysis parameter.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Analysis apparatus 41 ... Analysis parameter setting part 43 ... 1st information storage part 44 ... Analysis result determination part 45 ... 2nd information storage part 46 ... Solution presentation part 47 ... Monitor

Claims (8)

  An analysis apparatus comprising analysis condition setting means for setting analysis conditions, and performing a predetermined analysis based on the analysis conditions set by the analysis condition setting means, for determining whether the measurement data that is the basis of the analysis is good or bad A first information storage means for preliminarily storing the judgment criteria, an analysis result judgment means for judging the quality of the current analysis result based on the judgment criteria stored in the first information storage means, and the analysis result is NO A second information storage means for storing information in advance by associating a past problem and a solution to the problem in advance, and the associated past problem stored in the second information storage means, and An analysis apparatus comprising: solution presentation means for presenting a solution to a problem of the current analysis result based on information on the solution.   The analysis apparatus according to claim 1, wherein it is not necessary to newly measure and acquire the measurement data, and when the analysis result is good by performing analysis by setting new analysis conditions, the solution From the current problem presented by the method presenting means and the solution, the new analysis condition is selected, the current analysis result is recalculated based on the new analysis condition, and the measurement data An analyzer characterized in that each means is configured so as to obtain a new analysis result without newly measuring and acquiring the value.   3. The analysis apparatus according to claim 1, further comprising display means for displaying the current problem and the solution presented by the solution presentation means.   4. The analyzer according to claim 1, wherein the first information storage means and / or the second information storage means are configured to be rewritable with the latest information. Analysis equipment.   5. The analyzer according to claim 1, wherein the predetermined analysis is an analysis in which measurement data serving as a basis of analysis is measured and the measurement data is collectively acquired. Analyzing device.   6. The analyzer according to claim 5, comprising a multi-channel type detector, and performing simultaneous analysis type high-frequency plasma emission analysis capable of simultaneously acquiring measurement data within a measurement wavelength range.   An analysis processing method for executing a series of analysis processes including an analysis process for performing a predetermined analysis based on a set analysis condition, the analysis condition setting process for setting the analysis condition, and setting in the analysis condition setting process An analysis process for performing a predetermined analysis based on the analysis conditions performed, an analysis result determination process for determining the quality of the current analysis result based on a determination criterion for determining the quality of measurement data that is the basis of analysis, In the case where the analysis result is NO, when the past problem that is rejected and the solution to the problem are associated with each other, the analysis result of this time is based on the information on the associated past problem and the solution An analysis processing method comprising: a solution presentation step for presenting a solution to the above problem. The analysis processing method according to claim 7, wherein it is not necessary to newly measure and acquire the measurement data, and when an analysis result is good by performing analysis by setting a new analysis condition, An analysis condition resetting step for selecting and resetting the new analysis condition from the current problem and the solution presented in the solution presentation step, and an analysis based on the new analysis condition An analysis processing method comprising: a recalculation step for recalculating a result; and an analysis result re-derivation step for obtaining a new analysis result without newly measuring and acquiring the measurement data.

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