JP3648887B2 - Analysis equipment - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention spectroscopically analyzes light generated from a sample by discharge or laser light irradiation, or analyzes a solid sample by aerosolization by laser light irradiation and then ICP or ICP mass analysis, while using a calibration sample instead of the sample. The present invention relates to an analyzer for performing an analysis operation to calibrate an analysis.
[0002]
[Prior art]
In general, in an analysis apparatus, it is necessary to routinely perform a calibration operation, that is, an operation for correcting a deviation occurring between a relative scale and an absolute value of a measuring instrument inside the apparatus. In such a calibration operation, an analysis is performed using a calibration sample (standard sample) whose standard analysis value is known in advance, and the above-described deviation is made based on the error between the analysis result and the standard analysis value. It is to be corrected.
[0003]
The calibration operation is performed multiple times on the calibration sample and then the average of the analysis results is obtained, or the analysis results are greatly different from other analysis results. After eliminating certain analysis results, the average of the remaining analysis results is obtained to obtain calibration data.
[0004]
Furthermore, a plurality of calibration samples corresponding to the analysis target are selected, calibration operations are performed on these calibration samples, and calibration data is collected respectively, and calibration is performed based on these calibration data. ing.
[0005]
On the other hand, an analyzer such as a spark emission analyzer or a laser emission analyzer that spectrally analyzes light generated from a sample by discharge or laser light irradiation, or an analyzer that analyzes a solid sample by aerosolization by laser light irradiation and then performs ICP or ICP mass analysis As shown in FIG. 3, it is avoided that analytical flaws 21 such as discharge holes occur on the surface (hereinafter referred to as analysis surface 20a) of the sample to be analyzed (the calibration sample 20 is illustrated in FIG. 3). In other words, it is impossible to reanalyze the portion of the analysis surface 20a where the analysis flaw 21 occurs. Therefore, it is necessary to change the analysis location on the analysis surface 20a for each analysis. Furthermore, if there is no analysis possible location on the analysis surface 20a, the analysis surface 20a is polished and updated until the analysis flaw 21 disappears. Pre-processing needs to be performed. In FIG. 3, reference numeral 22 is a remaining analyzable portion on the analysis surface 20 a. In addition, in the columnar calibration sample 20 illustrated in FIG. 3, the analysis surface 20a can be analyzed eight times, and has a total of eight possible analysis locations. This is a state where the number of remaining analyses is four.
[0006]
As described above, an analysis device such as a spark emission analysis device or a laser emission analysis device that spectrally analyzes light generated from a sample by discharge or laser light irradiation, or a solid sample is aerosolized by laser light irradiation and then ICP or ICP mass analysis is performed. In the analyzer, the calibration operation must be performed including the pre-processing described above, which is troublesome. Therefore, there are conventional analyzers that automate calibration operations including preprocessing.
[0007]
This analyzer includes a calibration sample storage unit, a preprocessing unit, an analysis unit, and a calibration analysis execution unit, and at the start of calibration analysis, the calibration analysis execution unit performs the following control. That is, the calibration sample is taken out from the calibration sample storage unit, preprocessed by the preprocessing unit, the processed calibration sample is analyzed by the analysis unit, and then the analyzed calibration sample is returned to the calibration sample storage unit.
[0008]
[Problems to be solved by the invention]
However, in the conventional analyzer that automates the calibration operation, there is a problem that the calibration sample is consumed very much and the working time is prolonged. This will be described below.
[0009]
As described above, in order to perform a calibration operation, it is necessary to perform a plurality of analyzes on each calibration sample 20. However, the number of times that each calibration sample 20 can be analyzed with respect to the analysis surface 20a is determined according to the size of the sample outer shape (area of the analysis surface 20a). For this reason, on the analysis surface 20a on which the analysis for calibration has already been performed, the allowable number of analyzes may not satisfy the number of analyzes required for the next calibration analysis, and if that happens, the analysis for calibration cannot be performed. End up.
[0010]
In order to eliminate such an inconvenience, in the conventional analysis apparatus in which the calibration is automated, the calibration sample 20 is pre-processed, that is, the analysis surface 20a is polished every time the calibration operation is performed. . However, this eliminates the inconvenience that the analysis for calibration cannot be performed, but the consumption of the calibration sample 20 becomes severe. Many of the calibration samples 20 are expensive, and the calibration sample 20 is exhausted by automation of calibration, which increases the running cost of the analyzer.
[0011]
Further, the polishing of the analysis surface 20a performed as pre-processing is an operation that requires a certain amount of time, and as described above, the calibration analysis needs to be performed on the plurality of calibration samples 20. For this reason, in a conventional analyzer that must be pre-processed for each calibration analysis, the time required for the analysis has been prolonged.
[0012]
[Means for Solving the Problems]
In order to solve the above-described problems, the present invention has the following configuration. That is, spectroscopic analysis of light generated from a sample by discharge or laser light irradiation, or analysis of ICP or ICP mass after a solid sample is aerosolized by laser light irradiation, while using the calibration sample instead of the sample The calibration sample storage unit that stores the calibration sample, the pre-processing unit that polishes the analysis surface of the calibration sample and updates the analysis surface, and the sample and the calibration sample. An analysis unit that performs the analysis operation; an analysis possible number management unit that stores the number of remaining analysis possible times of the analysis surface obtained by subtracting the number of analysis times of the analysis surface from the number of analysis possible times of the analysis surface of the calibration sample; At the start of calibration analysis, the number of remaining analysis possible times on the analysis surface of the calibration sample stored in the analysis possible number management unit is called, and the called number of remaining analysis times satisfies the number of analysis required for calibration. If not, a pre-processing command is output. On the other hand, if the number of available remaining analyzes satisfies the number of analyzes required for calibration analysis, a judgment unit that outputs a calibration analysis command and the calibration analysis command receives the calibration analysis command. from the sample storage portion removed calibration sample, while analyzing the analyzable site analysis surface of the calibration sample analyzer, when receiving the pre-processing instructions, analyzed by pre-processing unit retrieves the calibration sample from the calibration sample storage unit An analysis execution unit that performs surface update processing and analyzes the processed calibration sample by the analysis unit.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, an embodiment of the present invention will be described in detail with reference to the drawings. FIG. 1 is a diagram showing a schematic configuration of an analyzer according to an embodiment of the present invention. This analyzer 1 is an emission analyzer that spectroscopically analyzes light generated from a sample by spark discharge, and includes a calibration sample storage unit 2, a preprocessing unit 3, an analysis unit 4, an analyzable number management unit 5, and the like. The determination unit 6, the analysis execution unit 7, and the monitor 8 are provided.
[0014]
The calibration sample storage unit 2 stores a calibration sample (not shown) used for calibration analysis. The pre-processing unit 3 polishes the analysis surface of the calibration sample and updates the analysis surface. The analysis unit 4 generates a spark discharge for the sample and the calibration sample, and spectrally analyzes light generated from the sample or the calibration sample by this discharge. The analysis possible number management unit 5 calculates the remaining analysis possible number of times on the analysis surface by subtracting the analysis number of the analysis surface from the analysis possible number of times on the analysis surface of the calibration sample, and stores the data. When the calibration analysis is started, the determination unit 6 calls the remaining analysis possible number of the analysis surface of the calibration sample stored in the analysis possible number management unit 5, and the called remaining analysis possible number does not satisfy the analysis number necessary for calibration. In this case, the preprocessing instruction F is output, while the calibration analysis instruction C is output when the called remaining analysis possible number satisfies the number of analysis necessary for the calibration analysis. The analysis execution unit 7 includes a handling robot 9 for carrying out and carrying in a calibration sample stored in the calibration sample storage unit 2 , and a handling robot 9 and a preprocessing unit based on a calibration analysis command C, a preprocessing command F, and the like. 3 and an analysis control unit 10 for controlling the operation of the analysis unit 4. The monitor 8 displays the number of analyzes necessary for calibration and the calibration sample stored in the calibration sample management unit 2 and the analysis data of the calibration sample corresponding to the stock table number of the calibration sample management unit 2. Yes.
[0015]
An example of analysis data displayed on the monitor screen 8a of the monitor 8 will be described with reference to FIG. On the monitor screen 8a, for example,
-Number of analyzes D1 required for calibration operation,
Stock table number D2 (identification number of the area where each calibration sample is stored in the calibration sample storage unit 2),
-Number of analyzable times D3 (the number of analyzable times for each analytical surface, which is determined by the size (area) of the calibration sample),
・ Number of already analyzed D4 (number of analyzes already performed on the current analysis surface),
・ Remaining analysis possible count D5 (= analysis possible count D3−already analyzed count D4),
To be shown, and is displayed in a table form that associates each data D 3 D5 stock table number D 2.
[0016]
Next, the calibration operation by the analyzer 1 will be described. Each calibration sample 20 (illustrated in FIG. 3) is stored in each calibration sample storage unit 2 in advance, and the number of analyzes D ₁ required for the calibration operation and the calibration sample stored in each stock table of the calibration sample storage unit 2 are stored. The initial data such as the data (substance name and the number of analyzable times D ₃ ) is registered in the analyzable number of times management unit 5. Registration is performed via an input device (not shown).
[0017]
After performing such an initial setting operation, a calibration sample 20 corresponding to a sample to be actually analyzed is selected, and data such as the selected calibration sample name is input to the analysis control unit 10 via an input device (not shown). To do. Then, the analysis control unit 10 inquires of the determination unit 6 about the analysis state of the analysis surface 20a of the designated calibration sample 20. Upon receiving the inquiry, the determination unit 6 calls the management data of the stock table D ₂ corresponding to the designated calibration sample 20. Furthermore, in the called management data, if the remaining analysis possible count D ₅ satisfies the analysis count D ₁ necessary for calibration in the called management data, the analysis for calibration is performed on the current analysis surface 20 a of the calibration sample 20. Therefore, the calibration command C is output to the analysis control unit 10. On the other hand, if the remaining analysis possible count D ₅ does not satisfy the analysis count D ₁ necessary for calibration in the called management data, it is impossible to perform calibration analysis on the current analysis surface 20 a of the calibration sample 20. Therefore, it is determined that preprocessing is necessary, and a preprocessing command F is output to the analysis control unit 10.
[0018]
Upon receiving the calibration command C, the analysis control unit 10 transmits a calibration control signal S1 to the handling robot 9 and the analysis unit 4. The handling robot 9 and the analysis unit 4 that have received the calibration control signal S1 perform the following operations. That is, the handling robot 9 first takes out the designated calibration sample 20 from the calibration sample storage unit 2 and transports it to the analysis unit 4.
[0019]
The analysis unit 4 into which the calibration sample 20 is carried in performs an analysis operation (a spark discharge is generated between the calibration sample 20 and the sample 20 that remains on the analysis surface 20a of the calibration sample 20). The operation is performed for spectroscopic analysis of the light generated from (1), and calibration data is collected. At this time, the analysis operation is repeated for the number of analyzes necessary for calibration.
[0020]
When the collection of the calibration data is completed, the handling robot 9 takes out the analyzed calibration sample 20 from the analysis unit 4 and transports it to the calibration sample storage unit 2. The calibration sample storage unit 2 stores the loaded calibration sample 20 in a corresponding storage area.
[0021]
In this way, when the analysis operation for calibration is completed, the analysis control unit 10 outputs a first data update command E to the analysis possible number management unit 5. Upon receiving the first data update instruction E, the analysis possible number management unit 5 stores each data of the already analyzed number of times D ₄ and the remaining number of possible analyses D ₅ of the stock table number corresponding to the calibration sample 20 that has been analyzed for calibration. Update. For example, the data is updated as follows. That is, the update data already analyzed the number D ₄ is carried out by adding the data of the number of analyzes D ₁ required calibration data already analyzed times D ₄ which is stored. Updating data of the remaining analyzable number of times D ₅ from the storage to have analyzable number D ₃ data is performed by subtracting the data already analyzed times D ₄ which updated. Such data update is an example of an update method and may be another update method. In this way, since each of D _{1 to} D ₅ including the updated data is displayed on the monitor 8, the operator can accurately grasp the state of the calibration sample 20.
[0022]
On the other hand, the analysis control unit 10 that has received the preprocessing instruction F transmits a preprocessing control signal S2 to the handling robot 9, the preprocessing unit 3, and the analysis unit 4. The handling robot 9, the preprocessing unit 3, and the analysis unit 4 that have received the preprocessing control signal S2 perform the following operations. That is, the handling robot 9 first takes out the designated calibration sample 20 from the calibration sample storage unit 2 and transports it to the preprocessing unit 3. The preprocessing unit 3 into which the calibration sample 20 has been carried out performs preprocessing, that is, processing for polishing and updating the analysis surface 20a of the calibration sample 20 until the analysis flaw 21 disappears.
[0023]
When the preprocessing is completed in the preprocessing unit 3, the handling robot 9 takes out the preprocessed calibration sample 20 from the preprocessing unit 3 and transports it to the analysis unit 4. The analysis unit 4 into which the processed calibration sample 20 has been loaded has the analysis possible part 22 remaining on the analysis surface 20a of the processed calibration sample 20 (in the case of the processed calibration sample 20, all the analysis possible parts are included). Analytical operation (operation that generates a spark discharge with the sample and spectroscopically analyzes light generated from the sample by the discharge) is performed to collect calibration data. At this time, the analysis operation is repeated for the number of analyzes necessary for calibration.
[0024]
When the collection of the calibration data is completed, the handling robot 9 takes out the analyzed calibration sample 20 from the analysis unit 4 and transports it to the calibration sample storage unit 2. The calibration sample storage unit 2 stores the loaded calibration sample 20 in a corresponding storage area.
[0025]
In this way, when the preprocessing and calibration analysis operations are completed, the analysis control unit 10 outputs a second data update command G to the analysis possible number of times management unit 5. Upon receiving the second data update command G, the analysis possible number management unit 5 stores each data of the already analyzed number of times D ₄ and the number of remaining analysis possible times D ₅ of the stock table number corresponding to the calibration sample 20 that has been analyzed for calibration. Update. For example, the data is updated as follows. That is, the update data already analyzed the number D ₄ is, instead of the data already analyzed times D ₄ which is stored, by storing the data of the number of analyzes D ₁ required for calibration as already analyzed count data D ₄ Do. Updating data of the remaining analyzable number of times D ₅ from the storage to have analyzable number D ₃ data is performed by subtracting the data already analyzed times D ₄ which updated. Such data update is an example of an update method and may be another update method. In this way, since each of D _{1 to} D ₅ including the updated data is displayed on the monitor 8, the operator can accurately grasp the state of the calibration sample 20.
[0026]
Based on the calibration data collected as described above, a calibration operation is performed in a calibration calculation unit (not shown). Since the calibration operation itself is not different from the conventional method, its description is omitted.
[0027]
By the way, in the analyzer 1 configured as described above, it is necessary to grasp the position of the analyzable portion 22 remaining on the analysis surface 20 a of the calibration sample 20 and then carry it into the analysis unit 4. Otherwise, there is a possibility that the inconvenience of performing the analysis operation again on the formation site of the analysis flaw 21 may occur. For example, when the analyzed calibration sample 20 carried out from the analysis unit 4 is returned to the calibration sample storage unit 2, the handling robot 9 can control the calibration sample 20. The direction may be controlled as follows. In other words, the orientation of the calibration sample 20 is controlled so that the remaining analyzable portion 22 is at a predetermined angular position, and then the sample is carried into the calibration sample storage unit 2. Then, the next time the handling robot 9 takes out the calibration sample 20 from the calibration sample storage unit 12, it can accurately grasp the remaining analyzable portion, The inconvenience of performing the analysis operation again does not occur.
[0028]
In the above-described embodiment, the present invention is implemented in the spark emission analyzer. However, in the present invention, in addition to this, the arc emission analyzer, the laser emission analyzer, and further, the solid sample is aerosolized by laser light irradiation. Needless to say, the present invention can be applied to an analysis apparatus that needs to perform pre-processing such as polishing on a calibration sample and update the analysis surface, such as an analysis apparatus that performs ICP or ICP mass analysis.
[0029]
【The invention's effect】
As described above, according to the present invention, it is possible to efficiently use the analysis surface of the calibration sample for analysis, and accordingly, the consumption of the calibration sample is reduced, and the running cost of the analyzer can be suppressed.
[0030]
Further, since the calibration sample should be subjected to the minimum necessary pretreatment, the analysis time can be shortened accordingly.
[Brief description of the drawings]
FIG. 1 is a diagram showing a configuration of an analyzer according to an embodiment of the present invention.
FIG. 2 is a diagram illustrating a display example of a monitor of the analyzer according to the embodiment.
FIG. 3 is a perspective view showing a configuration of a calibration sample handled by the analyzer of the present invention.
[Explanation of symbols]
2 calibration sample storage unit 3 preprocessing unit 4 analysis unit 5 possible number of times management unit 6 determination unit 7 analysis execution unit 9 handling robot 10 analysis control unit 20 calibration sample 20a analysis surface 21 analysis flaw C calibration command F preprocessing command

Claims (1)

Spectral analysis of the light generated from the sample by discharge or laser light irradiation, or analysis of ICP or ICP mass after solidifying the solid sample by laser light irradiation, while performing the analysis operation using a calibration sample instead of the sample An analyzer for calibrating the analysis,
A calibration sample storage section for storing calibration samples;
A pre-processing unit that polishes the analysis surface of the calibration sample and updates the analysis surface;
An analysis unit for performing an analysis operation on the sample and the calibration sample;
An analysis possible number management unit for storing the number of remaining analysis possible times of the analysis surface obtained by subtracting the number of previous analysis of the analysis surface from the number of possible analysis times of the analysis surface of the calibration sample;
At the start of calibration analysis, call the remaining number of possible analysis on the analysis surface of the calibration sample stored in the analysis possible number management unit. If the called number of remaining analysis does not satisfy the number of analysis required for calibration, pre-processing A determination unit that outputs a calibration analysis command when the remaining number of available analysis calls satisfies the number of analysis required for calibration analysis,
When the calibration analysis command is received, the calibration sample is taken out from the calibration sample storage unit, and the analysis unit analyzes the analyzable portion of the analysis surface of the calibration sample. On the other hand, when the pretreatment command is received, the calibration sample storage unit performs calibration. An analysis apparatus comprising: an analysis execution unit configured to extract a sample, perform an analysis surface update process in a preprocessing unit, and analyze the processed calibration sample in the analysis unit.

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