JP2020091139A - Emission analyzer - Google Patents

Abstract

To provide an emission analyzer that can prevent an error in an analytic result that may occur depending on a shape of a solid sample.SOLUTION: A composition information acquisition processor 51 acquires composition information of a component in a solid sample by comparing a detection intensity of each wavelength of a detector 43 with an analytical curve. A standard determination processor 52 determines a corresponding standard from among a plurality of preset standards based on the composition information acquired by the composition information acquisition processor 51. A display processor 53 displays a setting screen when the standard is determined by the standard determination processor 52. A shape setting receiving unit 54 receives a setting of a shape of the solid sample on the setting screen. A correction processor 55 corrects the analytical curve according to the shape of the solid sample whose setting is received by the shape setting receiving unit 54.SELECTED DRAWING: Figure 2

Description

The present invention relates to an optical emission analyzer for discharging a solid sample and analyzing emission.

The emission analyzer is provided with, for example, an electrode, and the solid sample is placed so as to face the electrode. When a solid sample is analyzed, a discharge is generated between the solid sample and the electrodes, and the light generated by the discharge is dispersed in a spectroscope. Then, the separated light of each wavelength is received by the detector, so that the composition information of the components contained in the solid sample is analyzed based on the detected intensity of each wavelength (see, for example, Patent Document 1 below). ).

A general solid sample has a cylindrical shape. An opening smaller than the circular end surface of the solid sample is formed at the installation position of the solid sample, and the solid sample is installed so as to close the opening. As a result, the end surface of the solid sample and the electrode face each other across the opening, and discharge can be performed between them.

Japanese Patent No. 5077212

However, the solid sample is not limited to the cylindrical shape as described above, but may have other shapes such as a pin shape and a small shape. These pin-shaped and small-sized solid samples have an end surface area smaller than the opening area, and the solid sample cannot be installed so as to block the opening. In such a case, the end portion of the solid sample is held by a holding member formed of a material that does not discharge, and the solid sample is set at the setting position together with the holding member.

As described above, even when the shapes of the solid samples are different, it is possible to perform the analysis using the same emission analysis device. However, there is a problem that an error occurs in the analysis result depending on the shape of the solid sample.

The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an emission analysis device capable of preventing an error in an analysis result depending on the shape of a solid sample.

(1) An emission analysis device according to the present invention is an emission analysis device for discharging a solid sample and analyzing emission, comprising a spectroscope, a detector, a composition information acquisition processing unit, and a standard determination processing unit. A display processing unit, a shape setting reception unit, and a correction processing unit. The spectroscope disperses the light generated from the solid sample. The detector receives the light of each wavelength split by the spectroscope. The composition information acquisition processing unit acquires the composition information of the components in the solid sample by comparing the detection intensity of each wavelength in the detector with a calibration curve. The standard determination processing unit determines a corresponding standard from a plurality of preset standards based on the composition information acquired by the composition information acquisition processing unit. The display processing unit displays a setting screen when the standard determination processing unit determines the standard. The shape setting reception unit receives the setting of the shape of the solid sample on the setting screen. The correction processing unit corrects the calibration curve according to the shape of the solid sample whose setting has been received by the shape setting reception unit.

According to such a configuration, the calibration curve is corrected according to the shape of the solid sample whose setting has been accepted by the shape setting accepting unit, and therefore the composition information of the components in the solid sample is obtained using the corrected calibration curve. It is possible to obtain the standard and determine the applicable standard based on the composition information. This makes it possible to prevent an error from being generated in the analysis result depending on the shape of the solid sample.

(2) The shape setting reception unit may receive a setting from shape candidates including at least two of a cylindrical shape, a pin shape, and a small shape.

According to such a configuration, the shape of the solid sample can be set from the shape candidates including at least two of the cylindrical shape, the pin shape, and the small shape, and the calibration curve can be appropriately corrected according to the shape. ..

According to the present invention, since the calibration curve is corrected according to the shape of the solid sample whose setting has been received by the shape setting reception unit, the composition information of the components in the solid sample is acquired using the corrected calibration curve. By determining the applicable standard based on the composition information, it is possible to prevent an error from being generated in the analysis result depending on the shape of the solid sample.

It is the schematic which showed the structural example of the optical emission analyzer which concerns on one Embodiment of this invention. FIG. 2 is a block diagram showing an example of an electrical configuration of the emission analysis device of FIG. 1. 7 is a flowchart showing an example of processing by the control unit at the time of determination analysis. It is the figure which showed an example of a calibration curve. It is sectional drawing which showed an example of the other shape of a sample, and has shown the state which the sample was mounted in the sample mounting base shown in FIG.

1. Overall Configuration of Emission Analysis Device FIG. 1 is a schematic diagram showing an example of the configuration of an emission analysis device according to an embodiment of the present invention. This optical emission analyzer is equipped with a sample mounting table 1 and an electrode 2. A discharge chamber 11 is formed inside the sample mounting table 1, and the tip of the electrode 2 faces the discharge chamber 11. An opening 12 is formed in the wall surface of the discharge chamber 11 at a position facing the tip of the electrode 2. The solid sample 3 to be analyzed is placed on the sample placing table 1 so as to close the opening 12, and the surface thereof faces the tip of the electrode 2 with a space therebetween.

At the time of analysis, a voltage is applied to the electrode 2 to cause discharge between the surface of the sample 3 and the tip of the electrode 2. The light generated in the discharge chamber 11 at the time of discharge passes through the condenser lens 13 and is guided to the measurement unit 4. The measurement unit 4 is formed in a hollow shape by forming a measurement chamber 41 therein, and a spectroscope 42 and a detector 43 are provided in the measurement chamber 41.

The light generated by discharging the sample 3 enters the measurement chamber 41 and is dispersed by the spectroscope 42. The detector 43 is provided with a plurality of light receiving elements 431, and the light of each wavelength split by the spectroscope 42 is received by each light receiving element 431, so that the wavelength specific to the element contained in the sample 3 is obtained. A bright line spectrum having a peak is obtained.

A gas supply passage 14 and a gas discharge passage 15 that communicate the inside and the outside of the discharge chamber 11 are formed in the sample mounting table 1. At the time of analysis, the inert gas supplied from the gas supply passage 14 into the discharge chamber 11 overflows from the gas discharge passage 15, so that the discharge chamber 11 is filled with the inert gas. In this way, by expelling the air in the discharge chamber 11 with the inert gas, it is possible to prevent the components in the air from adversely affecting the analysis result. As the inert gas introduced into the discharge chamber 11, for example, argon gas or the like is used, but it is also possible to use a gas other than the argon gas.

2. Electrical Configuration of Emission Spectrometer FIG. 2 is a block diagram showing an example of the electrical configuration of the emission spectroscope of FIG. In addition to the configuration described above, this emission analysis device is provided with, for example, a control unit 5, a display unit 6, an operation unit 7, a storage unit 8 and the like. The control unit 5 is configured to include, for example, a CPU (Central Processing Unit), and the composition information acquisition processing unit 51, the standard determination processing unit 52, the display processing unit 53, the shape setting reception unit by the CPU executing a program. 54 and the correction processing unit 55.

The display unit 6 is composed of, for example, a liquid crystal display, and can display various information on the display screen. The operation unit 7 is composed of, for example, a keyboard and a mouse, and a user can perform an input operation. The storage unit 8 includes, for example, a hard disk and a RAM (Random Access Memory). A calibration curve data storage unit 81, a standard data storage unit 82, and the like are assigned to the storage area of the storage unit 8.

The calibration curve data storage unit 81 stores calibration curve data representing the relationship between the detection intensity of each light receiving element 431 of the detector 43 and the element content rate. That is, the calibration curve data represents the relationship between the detection intensity of each wavelength detected by each light receiving element 431 and the content rate of the element having a peak at that wavelength.

The standard data storage unit 82 stores, as standard data, a plurality of standard data preset as a specific composition. The standard may be a standardized standard such as the Japanese Industrial Standard (JIS), or may be a standard set arbitrarily.

The composition information acquisition processing unit 51 performs processing for acquiring the composition information of the components in the sample 3 by comparing the detection intensity of each wavelength in the detector 43 with the calibration curve. Specifically, the detection intensity of each light receiving element 431 of the detector 43 is compared with the calibration curve data stored in the calibration curve data storage unit 81 to calculate the content rate of the element corresponding to each wavelength. To be done. Thereby, the element contained in the sample 3 and the content rate of the element are acquired as composition information.

The standard determination processing unit 52 performs a process of determining a standard based on the composition information acquired by the composition information acquisition processing unit 51. Specifically, by comparing the obtained composition information with the standard data stored in the standard data storage unit 82, the composition information is selected from among a plurality of standards preset as standard data. Applicable standards are extracted.

The display processing unit 53 controls the display on the display unit 6. At the time of the judgment analysis for judging the standard of the composition information of the sample 3, the display processing unit 53 displays a setting screen for setting the judgment analysis on the display unit 6. In addition, when the standard of the composition information of the sample 3 is determined by the standard determination processing unit 52, the determination result is displayed on the display unit 6 by the display processing unit 53. The setting screen and the judgment result regarding the judgment analysis may be displayed on the display unit 6 on a common screen or on separate screens.

When the user operates the operation unit 7 to set the shape of the sample 3 on the determination analysis setting screen, the shape setting reception unit 54 receives the setting. As the shape of the sample 3, a plurality of types of shape candidates such as a cylindrical shape, a pin shape, and a small shape are predetermined, and an arbitrary shape can be selected from these shape candidates.

The cylindrical sample 3 has a shape having a circular end surface, the area of the end surface is larger than the opening 12 of the discharge chamber 11, and the sample 3 is mounted on the sample mounting table 1 so as to close the opening 12 with the end surface. .. The pin-shaped sample 3 is a rod-shaped sample 3 having an end surface area smaller than that of the columnar shape, and the end surface area is smaller than the opening 12 of the discharge chamber 11, so that the end surface cannot close the opening 12. Similar to the pin shape, the small-sized sample 3 has a smaller end surface area than the cylindrical shape, but has a shape different from the pin shape (for example, a bolt), and the opening 12 may be closed by the end surface. Can not. Therefore, when analyzing the pin-shaped or small-sized sample 3, by holding the sample 3 with the sample holding member, the opening 12 of the discharge chamber 11 is closed by the end face of the sample 3 and the end face of the sample holding member. Be done.

The user can set the shape of the sample 3 by performing an operation of selecting from a plurality of types of shapes using the operation unit 7. The shape of the sample 3 whose setting has been accepted by the shape setting accepting unit 54 is displayed on the determination analysis setting screen by the display processing unit 53. The shape candidates preferably include at least two of a cylindrical shape, a pin shape, and a small shape, but are not limited to these shapes.

The correction processing unit 55 performs a process of correcting the calibration curve data stored in the calibration curve data storage unit 81 according to the shape of the sample 3 whose setting has been accepted by the shape setting acceptance unit 54. That is, since the optimum calibration curve changes when the shape of the sample 3 is different, the correction processing unit 55 corrects the calibration curve data so that the optimum calibration curve is obtained according to the set shape of the sample 3. ..

3. Processing by control unit at the time of determination analysis FIG. 3 is a flowchart showing an example of processing by the control unit at the time of determination analysis. When performing the judgment analysis, first, the display processing unit 53 displays the judgment analysis setting screen on the display unit 6 (step S101). In this setting screen, the user can set the shape of the sample 3 by operating the operation unit 7, and can also set various conditions necessary for the judgment analysis.

When the shape of the sample 3 is set on the setting screen (Yes in step S102), the correction processing unit 55 corrects the calibration curve according to the set shape of the sample 3 (step S103). .. When the operation for starting the analysis is performed after the various settings are performed in this way (Yes in step S104), the analysis is started under the set conditions.

Specifically, the composition information acquisition processing unit 51 reads the calibration curve data from the calibration curve data storage unit 81 (step S105), and compares the calibration curve with the detection intensity of the detector 43, Composition information of the components in the sample 3 is acquired (step S106). Then, the standard determination processing unit 52 compares the obtained composition information with the standard data stored in the standard data storage unit 82, and determines the applicable standard from a plurality of preset standards ( Step S107). The determined standard of the component in the sample 3 is displayed on the display unit 6 as the determination result by the display processing unit 53 (step S108).

4. Calibration Curve Correction Processing FIG. 4 is a diagram showing an example of the calibration curve. In FIG. 4, an example of a calibration curve represented by the following equation (1) is shown, in which the horizontal axis represents the element content C and the vertical axis represents the detection intensity I of the detector 43. Note that a, b, c, and d are coefficients.
C=aI ³ +bI ² +cI+d (1)

As described above, the calibration curve is represented by a cubic expression including the plurality of coefficients a, b, c, d. The correction processing unit 55 corrects the calibration curve according to the shape of the sample 3 by changing at least one of the coefficients a, b, c, d of the calibration curve represented by the above formula (1). .. However, the calibration curve is not limited to that represented by the cubic equation, and may be represented by the linear equation, the quadratic equation, or the quaternary equation or more.

The correction processing unit 55 corrects the calibration curve by sequentially performing a plurality of types of correction processing. The plurality of types of correction processing include so-called master curve correction. In the master curve correction, a standard sample for master curve correction containing a typical component contained in the sample 3 is measured, and correction is performed using a linear equation or a quadratic equation. In the present embodiment, this master curve correction is performed in different modes depending on the set shape of the sample 3. However, the correction processing other than the master curve correction may be performed in a different manner depending on the set shape of the sample 3.

5. Other Shape of Sample FIG. 5 is a cross-sectional view showing another example of the shape of the sample 3, and shows a state in which the sample 3 is mounted on the sample mounting table 1 shown in FIG. 5, the structure of the sample mounting table 1 is the same as that of FIG. 1, and thus the same structures as those of FIG.

In FIG. 5, the case where the sample 3 has a pin shape is shown. As shown in FIG. 5, one end of the pin-shaped sample 3 is held by the sample holding member 31, and the opening 12 of the discharge chamber 11 is closed by the end face of the sample 3 and the end face of the sample holding member 31. Although not shown, even when the sample 3 has a small shape, the sample 3 is mounted on the sample mounting table 1 while being held by the sample holding member.

6. Function and Effect (1) In the present embodiment, the calibration curve is corrected according to the shape of the sample 3 whose setting has been accepted by the shape setting accepting unit 54. Therefore, the corrected calibration curve is used to determine the components in the sample 3. It is possible to obtain the composition information and determine the applicable standard based on the composition information. As a result, it is possible to prevent an error from being generated in the analysis result depending on the shape of the sample 3.

(2) In particular, in the present embodiment, the shape of the sample 3 is set from the shape candidates including at least two of the cylindrical shape, the pin shape, and the small shape, and the calibration curve is appropriately corrected according to the shape. You can

7. Modified Example In the above embodiment, the configuration in which the spectroscope 42 and the detector 43 are provided in the measurement chamber 41 has been described. However, the configuration is not limited to such a configuration, and the detector 43 may be provided outside the measurement chamber 41, for example.

The configuration for generating light by discharging the sample 3 is not limited to the configuration shown in FIG. 1, and any other configuration can be adopted. In this case, an arbitrary aspect such as spark discharge, arc discharge, inductively coupled plasma (ICP) discharge can be adopted as the aspect of discharge.

1 sample mounting table 2 electrode 3 sample 4 measuring unit 5 control unit 6 display unit 7 operating unit 8 storage unit 31 sample holding member 41 measuring chamber 42 spectroscope 43 detector 51 composition information acquisition processing unit 52 standard determination processing unit 53 display processing Part 54 Shape setting accepting part 55 Correction processing part 81 Calibration curve data storage part 82 Standard data storage part 431 Light receiving element

Claims (2)

An emission analysis device for discharging a solid sample and analyzing emission, comprising:
A spectroscope for separating the light generated from the solid sample,
A detector that receives light of each wavelength dispersed by the spectroscope,
By comparing the detection intensity of each wavelength in the detector with a calibration curve, a composition information acquisition processing unit that acquires composition information of components in a solid sample,
Based on the composition information acquired by the composition information acquisition processing unit, a standard determination processing unit that determines a corresponding standard from a plurality of preset standards,
A display processing unit that displays a setting screen when the standard is determined by the standard determination processing unit;
On the setting screen, a shape setting receiving unit that receives the setting of the shape of the solid sample,
An emission analysis device, comprising: a correction processing unit that corrects the calibration curve according to the shape of the solid sample whose setting has been received by the shape setting reception unit. The emission analysis device according to claim 1, wherein the shape setting reception unit receives a setting from shape candidates including at least two of a cylindrical shape, a pin shape, and a small shape.

Images