Preparation method and preparation device for solution for quantitative analysis

Abstract

To eliminate the time and effort for measuring and managing the volume of a solution to be analyzed to be introduced to an analyzer in performing quantitative analysis of a component with an unknown concentration in a sample by using a calibration curve, thereby performing accurate analysis.SOLUTION: In performing quantitative analysis of an unknown component included in a sample by using a calibration curve, a preparation device performs, by using the same absorption tube, introducing an absorbent absorbing gas into the absorption tube and causing the absorbent to absorb sample gas generated by decomposing the sample including the unknown component by heat to prepare a solution to be analyzed for the sample, and preparing a calibration curve solution, injects a diluted solution to the solution to be analyzed in the absorption tube and the calibration curve solution in the absorption tube to obtain constant-volume solutions, and introduces the solutions to an analyzer to perform analysis.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a method and apparatus for preparing an analyte solution containing a calibration curve solution to be introduced into an apparatus for detecting an unknown component, the unknown component being contained in a sample and having an unknown concentration, using a calibration curve of an ion chromatograph or other analyzer to quantitatively analyze the unknown component. [Background technology]

[0002] In the quantitative analysis of sulfur and halogens in a sample using ion chromatography (hereinafter referred to as "IC"), the sample is heated and decomposed, and the gasified components to be analyzed are collected in an absorbing liquid. The absorbing liquid that has absorbed the sample gas is then introduced into an IC analyzer as the solution to be analyzed.

[0003] A known sample processing device recovers the components to be analyzed in a sample as a pretreatment and introduces the recovered components into an IC analyzer. The sample processing device is equipped with a sample heating device that heats and decomposes the sample to produce a sample gas, an absorption tube that contains an absorption liquid that absorbs the sample gas and is configured so that the sample gas introduced from the sample heating device can come into contact with the absorption liquid, and a diluent supplying device that injects a diluent into the absorption tube (see, for example, Patent Document 1). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2011-237316 A Summary of the Invention [Problem to be solved by the invention]

[0005] When quantitative analysis of a sample is performed in an IC analyzer using the sample processing device having the above-mentioned configuration, the analysis can be performed, for example, through the following process. First, a calibration curve solution is prepared from a calibration curve stock solution whose concentration is known in advance, and this is introduced into the IC analyzer to perform IC measurement. Next, a calibration curve solution is prepared from the calibration curve stock solution at a different concentration from the above, and this is introduced into an IC analyzer to perform IC measurement, and a calibration curve is created from the solution concentration and peak area. Next, an unknown sample of unknown concentration is placed into the sample processing device of the above configuration, and is heated and decomposed in the sample heating device to generate sample gas. The generated sample gas is absorbed into an absorption liquid contained in an absorption tube, and a dilution liquid is injected into the absorption tube to make it a fixed amount, which is then introduced into an IC analysis device to perform IC measurement. Then, the peak area of ​​the unknown sample is determined by IC measurement, the unknown sample is thermally decomposed using the calibration curve created above, and the amount of the target component recovered in the sample gas is determined using the amount of sample introduced and the amount of the component detected. A quantitative analysis of the sample is then performed through this process.

[0006] In the quantitative analysis of samples as described above, it is necessary to accurately grasp the final volume of the absorbing liquid that has absorbed the sample gas and is introduced into the IC analyzer. For this purpose, it is time-consuming to precisely measure and manage the volume of the absorbing liquid that has absorbed the sample gas, and the process of grasping the final volume of the absorbing liquid is very difficult. Furthermore, in a device that automatically introduces the calibration solution and absorbing solution into an IC analyzer, a mechanism is required to switch between the nozzle that serves as the introduction flow path for the calibration solution and the nozzle that serves as the introduction flow path for the absorbing solution, which poses the problem that it is not possible to simplify the device structure.

[0007] In view of the problems associated with the conventional technology, the present invention aims to eliminate the need to measure and manage the volume of the solution to be analyzed introduced into an analytical device when quantitatively analyzing components contained in a sample using a calibration curve, and to enable automatic, highly accurate quantitative analysis. [Means for solving the problem]

[0008] In order to solve the above problems, the present invention provides a method for preparing an analyte solution to be introduced into an apparatus for detecting an unknown component in a sample using a calibration curve, the method comprising the steps of: preparing a solution to be analyzed of the sample by placing an absorbing liquid for absorbing gas in an absorption tube and allowing the sample containing the unknown component to be thermally decomposed and the generated sample gas to be absorbed in the absorbing liquid; Using the same absorption tube as above, prepare a calibration curve solution by pouring a solution of known concentration into the absorption tube; A method for preparing a solution for quantitative analysis, comprising the steps of: In the above-mentioned preparation method, the present invention is characterized in that a diluent is placed in an absorption tube to prepare the sample solution to be analyzed and the calibration curve solution. The diluent can be injected into the absorption tube up to the level detected by a liquid level sensor provided in the absorption tube, or a predetermined amount of the diluent can be injected into the absorption tube using a metering pump.

[0009] FIG. 1 shows an outline of a process for preparing a solution according to the preparation method of the present invention. The present invention uses a preparation processing system that includes a mechanism (device) for burning and thermally decomposing a sample to generate a sample gas, and an absorption tube, to prepare a solution to be analyzed. As shown in the figure, an unknown sample with an unknown concentration is decomposed by heating to generate a sample gas, which is then absorbed in an absorption liquid placed in an absorption tube, and a dilution liquid is added to quantitatively analyze the unknown components, preparing a solution for use in analyzing the unknown components. The calibration curve solution for preparing the calibration curve is prepared by using the same absorption tube as above, placing a solution of known concentration whose components and concentrations are known, and adding a diluent to make a quantitative amount. The solution to be analyzed prepared in the absorption tube is automatically or manually introduced from the absorption tube into an analyzer, where the components contained in the solution are analyzed. The prepared solution may be transferred from the absorption tube into a separate container, which is then transported to a storage location, where the prepared solution is stored until it is analyzed by the analyzer. The injection of the absorbing solution or the solution of known concentration into the absorbing tube may be performed automatically or manually using a pump for delivering the solution. The injection of the diluting solution may also be performed automatically or manually. When the diluting solution is delivered to the absorbing tube using a pump, if a liquid level sensor is provided in the absorbing tube to detect the total liquid amount in the tube, the amount of the solution prepared in the absorbing tube can be kept constant without checking the amount of the diluting solution delivered to the absorbing tube. On the other hand, when the diluting solution is delivered to the absorbing tube using a metering pump, the final amount of the solution prepared in the absorbing tube can be calculated from the amount of the absorbing solution put into the absorbing tube and the amount of the diluting solution delivered from the metering pump. In this way, a sample containing a component with an unknown concentration is thermally decomposed, and the absorbent solution of the sample obtained by absorbing the gas generated by the thermal decomposition and the calibration curve solution obtained from the solution of known concentration are prepared using the same absorption tube. This eliminates the need to burn a sample of known concentration in order to create a calibration curve. Furthermore, if a mechanism for automatically pumping the various solutions to be injected into the absorption tube and a mechanism or mechanism for detecting the amount of solution injected into the absorption tube are provided, the time required to adjust and check the final amounts of the absorption solution and the calibration curve solution can be eliminated, and the analysis can be performed quickly.

[0010] The present invention also provides a solution preparation device for quantitative analysis, which prepares an analyte solution to be introduced into an apparatus for detecting an unknown component in a sample using a calibration curve, comprising: an absorption tube in which the solution is prepared; a sample heating means for thermally decomposing the sample containing the unknown component to generate a sample gas; A diluent injection means for injecting a diluent into the absorption tube; a known concentration solution injection means for injecting a known concentration solution into the absorption tube; a function of absorbing the sample gas generated by the sample heating means into an absorbing liquid placed in the absorption tube and preparing an analyte solution of the sample by injecting a diluent into the absorption tube; The present invention is characterized by having a function of injecting a solution of known concentration into the absorption tube and a dilution solution to prepare a calibration curve solution. The apparatus having the above-mentioned configuration may further be configured such that the absorption tube is provided with a liquid level sensor. Furthermore, the device for detecting an unknown component can be provided with a function for automatically introducing the solution prepared in the absorption tube. In this case, the device for detecting the unknown component may be, for example, an ion chromatograph.

[0011] For example, a process of introducing an unknown component contained in a sample into an IC analyzer using the solution preparation device of the present invention and quantitatively analyzing the component is carried out as follows. First, put a known concentration solution and a dilution solution into an absorption tube to prepare a calibration solution, then introduce the prepared solution into an IC analyzer to perform IC measurement. Specifically, a predetermined amount (e.g., 1 mL) of a solution of known concentration with a predetermined concentration (e.g., 10 ppm) is injected into the absorption tube from the known concentration solution injection means. Next, a dilution solution is injected into the absorption tube up to the liquid level sensor to make a constant volume (X mL), and this is introduced into the IC analyzer as a calibration solution to perform IC measurement. Next, the known concentration solution (10 ppm) is injected into the absorption tube from the known concentration solution injection means in a different volume (e.g., 2 mL), and the dilution solution is injected up to the liquid level sensor to make it a constant volume (X mL). This is introduced into the IC analyzer as the calibration solution and an IC measurement is performed, and a calibration curve is created from the previous measurement and the results of this measurement. A predetermined amount (e.g., 5 mL) of absorbing liquid is placed in the same absorption tube as above, and a sample with unknown components is heated and decomposed by a sample heating means to generate a sample gas, which is then absorbed in the absorbing liquid. Next, a diluting liquid is injected into the absorption tube up to the liquid level sensor to make it a constant volume (X mL), and this is then introduced into an IC analyzer to perform IC measurement. The concentration of the unknown sample is determined from the measurement results and the calibration curve prepared earlier. Effect of the Invention

[0012] According to the method for preparing a solution for quantitative analysis of the present invention, the absorption solution of the sample obtained by absorbing the gas generated by the thermal decomposition of a sample containing an unknown component and the calibration curve solution obtained from a solution of known concentration are prepared using the same absorption tube, which can eliminate the need to burn a sample of known concentration to generate an absorption solution of known concentration in order to create a calibration curve. In addition, it is possible to eliminate the need to adjust and check the final volume of the absorption solution, and the analysis can be performed quickly. Furthermore, according to the solution treatment device of the present invention, in measurements using this device, it is possible to calculate the concentration and amount of a target component in an unknown sample even if the amount of liquid up to the liquid level sensor installed in the absorption tube is unknown. This eliminates the need for measuring and managing the amount of liquid to obtain a quantitative amount of the analyte solution, which was previously time-consuming and tedious, and makes it possible to automatically perform highly accurate quantitative analysis regardless of whether the unknown sample is a liquid or a solid. [Brief description of the drawings]

[0013] [Figure 1] FIG. 1 is a diagram showing an overview of a process for preparing a solution according to a solution preparation method of the present invention. [Diagram 2] 1 is a diagram showing a schematic configuration of an embodiment of a solution preparation device of the present invention. [Diagram 3] FIG. 3 is a diagram showing a schematic configuration of the absorption tube in FIG. 2. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0014] Hereinafter, a preferred embodiment of the solution preparation device of the present invention will be described with reference to the drawings. FIG. 1 shows the schematic configuration of an apparatus for quantitatively analyzing unknown components contained in a sample using an IC analyzer, in which reference numeral 1 denotes the IC analyzer and reference numeral 2 denotes a solution preparation apparatus of the present invention for preparing an analyte solution including a calibration curve solution to be introduced into the IC analyzer.

[0015] The IC analyzer 1 is a well-known device that separates ions and polar molecules in a solution to be analyzed using ion exchange resin and analyzes anions and cations by detecting the electrical conductivity or absorbance of the solution, and is composed of a pump, a separation column (measuring tube) in a thermostatic bath, a detector, etc. Alternatively, a suppressor for reducing background is further provided between the separation column and the detector. A sample introduction valve 11 is disposed in a solution extraction pipe 71 extending from a solution containing tube (to be described later) to the IC analyzer 1 .

[0016] The solution preparation device 2 is configured to include an absorption tube 3 in which a solution to be analyzed is stored and which sends the solution to be analyzed to the IC analysis device 1, a sample heating means 4 which heats and decomposes the sample to generate a sample gas, a dilution liquid injection means 5 which injects a dilution liquid into the absorption tube 3, and a known concentration solution injection means 6 which injects a solution of known components and concentrations into the absorption tube 3.

[0017] The absorption tube 3 is made of a light-transmitting material such as glass and has an internal volume of 10 to 100 cm 3 The absorption tube 3 is a cylindrical container of about 100 mm in diameter. As described later, in the process of heating the sample with the sample heating means 4 and recovering the sample gas, an absorbing liquid that absorbs the sample gas is contained in the absorption tube 3. The absorbing liquid may be, for example, a hydrogen peroxide solution with a concentration of 0.001 to 1%, a dilute alkaline solution, or water. The absorbing liquid is injected into the absorption tube by a solution delivery pump (not shown). The absorbing liquid may also be injected manually.

[0018] The upper end of the absorption tube 3 is sealed with a lid to prevent the solution to be analyzed from scattering, and the solution extraction tube 71 and a known concentration solution injection tube 79 connected to the known concentration solution injection means 6 are inserted into this lid. A gas inlet pipe 75 is connected to the outer periphery of the absorption tube 3, and the sample gas generated by the sample heating means 4 described later is introduced from the gas inlet pipe 75 into the tube and absorbed by the absorbing liquid contained in the absorption tube 3. The diluent delivered from the diluent injection means 5 is also injected into the absorption tube 3 from the gas inlet pipe 75. The used absorbing liquid and washing water in the absorption tube 3 are discharged from a drain pipe 77 to the outside of the tube.

[0019] The sample heating means 4 includes an outer tube 41 capable of supplying oxygen and capable of being heated from the outer periphery by the heating means 12, an inner tube 43 capable of supplying a carrier gas and inserted into the outer tube 41 from its base end, and a boat 44 for supplying samples inserted into the inner tube 43 from its base end. In the sample heating means 4, the outer tube 41 and the inner tube 43 form a reaction tube. Usually, the outer tube 41, the inner tube 43, and the boat 44 are made of quartz.

[0020] A cylindrical electric furnace of about 0.7 to 1.5 kW is usually used as the heating means 42 for heating the outer tube 41 and the inner tube 43, which are reaction tubes. In other words, the outer tube 41 is inserted into the cylinder of the electric furnace. An oxygen introduction tube 72 for supplying oxygen to the outer tube is connected to the base end of the outer tube 41, and although not shown, the oxygen introduction tube 72 extends from an oxygen container and is provided with a flow rate controller on the way. In addition, a sample gas extraction tube 74 for extracting the sample gas obtained by thermal decomposition is provided at the tip of the outer tube 41, and this sample gas extraction tube 74 is connected to the gas blowing tube 75. Usually, the tip side of the inside of the outer tube 41 is filled with quartz cotton for stabilizing combustion (not shown).

[0021] The inner tube 43 is a conduit for guiding the sample gas generated by the thermal decomposition of the sample to the outer tube 41, and its tip opening (the end on the left side in FIG. 2) is inserted into the outer tube 41 at a position corresponding to the approximate center of the length in order to promote the combustion of the generated gas. The base end side of the inner tube 43, i.e., the part not inserted into the outer tube 41 (about half the length on the right side in FIG. 2) is exposed to the outside from the base end of the outer tube 41. A carrier gas introduction tube 73 for supplying a carrier gas such as argon is connected to the base end of the inner tube 43, and although not shown, the carrier gas introduction tube 73 extends from a carrier gas container and is provided with a flow rate controller on the way. In addition, a sample introduction port 45 is provided at the part of the inner tube 43 exposed from the outer tube 41, and the sample introduction port 45 has a structure in which the outer circumference of the opening provided in the inner tube 43 is covered with a casing with a lid.

[0022] The boat 44 for supplying samples is a small dish that carries a sample and moves back and forth between the sample inlet 45 and the vicinity of the tip of the inner tube 43 inside the inner tube 43, and is formed, for example, in the shape of a shallow, flat, elongated box. The boat 44 is provided at the tip of an operating rod that moves back and forth by the boat controller 46. Specifically, a short-axis cylindrical metal piece that fits loosely into the inner periphery of the inner tube 43 is attached to the base end of the operating rod, and a moving rod is arranged on the outer periphery of the inner tube 43, which is made of a ring-shaped magnet or electromagnet that fits loosely into the inner tube and moves linearly by a driving mechanism (e.g., a driving mechanism composed of a servo motor and a rack mechanism) of the boat controller 46, and the operating rod moves inside the inner tube 43 following the moving movement.

[0023] In order to supply sufficient water vapor to the inner tube 43, the sample heating means 4 is provided with a water supply pipe 76 connected to a water supply means, which is connected to the outer periphery of the inner tube 43 at a position corresponding to the base end of the outer jacket tube 41, so that water can be supplied from the outside, and with a water vapor generating section having a jacket structure that generates water vapor using residual heat from the heating means 42. A water vapor introduction hole (not shown) is provided in the wall surface corresponding to the upper surface side of the horizontally disposed inner tube 43, and the water vapor generated in the water vapor generating section is introduced to the reaction region of the inner tube 43 through this hole.

[0024] The diluent injection means 5 is a means for injecting water, which is a diluent, into the solution containing tube 3, and the diluent delivered from the diluent injection means 5 is injected into the absorption tube 3 through the diluent delivery tube 78 and the gas blowing tube 75. A pump for delivering the diluent can be used as the diluent injection means 5. For example, the diluent may be delivered to the absorption tube 3 using a metering pump such as a syringe pump.

[0025] The known concentration solution injection means 6 is a means for injecting a known sample solution whose components and concentrations are known into the absorption tube 3, and the known concentration solution is injected into the solution containing tube 3 through a known concentration solution injection tube 79. As the known concentration solution injection means 6, a syringe pump or the like capable of injecting any amount into the absorption tube 3 can be used. The known concentration solution is a solution in which a known amount of the component to be measured is dissolved, and can be a commercially available standard solution, a certified substance, or a solution prepared by appropriately mixing substances.

[0026] As shown in FIG. 3, the liquid level sensors 8, 8 provided in the absorption tube 3 can be composed of, for example, a light source such as a light-emitting diode or a semiconductor laser, and a photosensor including a light-receiving element such as a photodiode or an optical array that detects the intensity of the light from the light source that has passed through the solution containing tube 3. Although not shown, an amplifier for amplifying the output signal of the liquid level sensor 8, 8, a signal converter for digitizing the output signal, and a calculation processing means for processing the obtained digital signal constitute a liquid level detection means for the absorption column 2. The calculation processing means is provided in a control device (not shown) described later.

[0027] In the solution preparation device 2 of this embodiment, the dilution liquid injection means 5 and the known concentration solution injection means 6 are composed of water pumps, and the dilution liquid and the known concentration solution are automatically injected into the absorption tube 3. The absorption liquid is also automatically injected from the suction liquid reservoir by a water pump (not shown) into the absorption tube 3. The solution to be analyzed prepared in the absorption tube 3 is also automatically introduced into the IC device 1 by a water pump (not shown).

[0028] The operation of each of the components constituting the solution preparation apparatus 2, including the sample heating means 4, diluent injection means 5, known concentration solution injection means 6, valves such as the gate valve, and liquid level sensors 8, 8, is controlled by a control device consisting of a computer equipped with a predetermined program, and is configured to perform functions of preparing a solution for quantitative analysis, such as a function of absorbing the sample gas generated by the sample heating means 2 into the absorption liquid placed in the absorption tube 3 and injecting a diluent into the absorption tube 3 to prepare an analyte solution of the sample, and a function of injecting a known concentration solution and a diluent into the absorption tube 3 to prepare a calibration curve solution. That is, in the process of preparing an analyte solution by thermally decomposing a sample of unknown components, the injection of absorbing liquid into the absorption tube and the thermal decomposition of the sample are carried out automatically under the control of the control device, and the sample gas generated by thermal decomposition is absorbed into the absorbing liquid. Next, diluent is injected into the absorption tube 3 from the diluent injection means 5, and when the solution in the absorption tube 3 reaches the liquid level sensors 8,8, the control device stops the operation of the diluent injection means 5 based on the signal from the liquid level sensors 8,8, and the volume of the analyte solution prepared in the absorption tube 3 is kept constant. In the process of preparing a calibration curve solution from a solution of known concentration, the known concentration solution is injected into the absorption tube 3 from the known concentration solution injection means 6 under the control of the control device, and when the injection amount reaches a predetermined amount, the control device stops the solution injection operation of the known concentration solution injection means 6. Next, the control device operates the diluent injection means 5 to inject the diluent into the absorption tube 3, and when the solution in the absorption tube 3 reaches the liquid level sensors 8, 8, the control device stops the operation of the diluent injection means 5 based on the signal from the liquid level sensors 8, 8, and the calibration curve solution prepared to a predetermined concentration in the absorption tube 3 is kept at a constant volume. The solution to be analyzed and the calibration curve solution, which have been adjusted to a constant volume in the absorption tube 3, are introduced into the IC analyzer 1 by operating a water pump (not shown) by the control device, and IC measurement is performed.

[0029] The process of quantitatively analyzing a sample containing an unknown component using the solution preparation apparatus 2 of this embodiment configured as described above is carried out, for example, as follows. First, a solution of known concentration is put into the absorption tube 3 to prepare a calibration curve solution, and the prepared solution is introduced into the IC analyzer 1 to perform IC measurement. Specifically, a predetermined amount of a solution of known concentration is injected into the absorption tube 3 from the known concentration solution injection means 6. Next, the diluent is injected into the absorption tube 3 from the diluent injection means 5 to the liquid level sensors 8, 8 to make a constant volume, and this is introduced into the IC analyzer 1 as a calibration curve solution to perform IC measurement. Although not shown, the absorption tube 3 is provided so that oxygen gas and argon gas can be supplied, and the injection of the solution of known concentration is performed with the supply of both gases temporarily stopped, and further, by supplying both gases into the absorption tube 3 after the diluent has been injected, the solution of known concentration and the diluent are mixed in the absorption tube 3. Next, a solution of known concentration is injected into the absorption tube 3 from the known concentration solution injection means 6 using a different amount of liquid from the above, and the diluent is injected from the diluent injection means 5 up to the liquid level sensors 8, 8 to make a constant volume. This is introduced into the IC analysis device 1 as a calibration curve solution and an IC measurement is performed, and a calibration curve is created from the previous measurement and the results of this measurement. A predetermined amount of absorbing liquid is placed in the absorption tube 3, and a sample of unknown concentration is heated and decomposed by the sample heating means 4 to generate a sample gas. The generated sample gas is absorbed in the absorbing liquid. Next, with the supply of the oxygen gas and argon gas stopped, diluent is injected from the diluent injection means 5 into the absorption tube 3 up to the liquid level sensors 8, 8 to make the volume constant. Then, the two gases are supplied into the absorption tube 3 to mix the solutions, and the solution is introduced into the IC analyzer 1 to perform IC measurement. The concentration of the unknown sample is determined from the measurement results and the calibration curve prepared earlier.

[0030] With the solution preparation apparatus configured in this manner, it is possible to calculate the concentration and amount of the target component in the unknown sample even if the amount of liquid up to the liquid level sensor provided in the absorption tube is unknown. This eliminates the need for measuring and managing the amount of liquid to obtain a quantitative amount of the analyte solution, which was previously time-consuming and tedious. It is therefore possible to automatically perform highly accurate quantitative analysis regardless of whether the unknown sample is a liquid or a solid. Furthermore, the following specific practical effects can be obtained. In other words, since the device has a function for automatically diluting a solution of known concentration, which is the original calibration curve solution, there is no need to prepare a calibration curve solution in advance. A dilution solution is added to the calibration solution and the absorption solution that has absorbed the sample gas of the sample containing the unknown component, and the volume is adjusted to a constant volume using a liquid level sensor installed in the same absorption tube, so there is no need to measure the liquid volume up to the liquid level sensor. In addition, the function of injecting the absorbing liquid into the absorption tube can also be used to prepare the calibration solution, so that the calibration solution can be prepared by adding the absorbing liquid that has absorbed the sample gas of the unknown sample to it, and the unknown sample solution to be analyzed and the calibration solution can be made to have the same composition and introduced into the IC analyzer for measurement. When creating a calibration curve, if the amount of calibration curve solution introduced into the IC analyzer is changed, there is a problem that the baseline changes when the amount of introduced solution is changed. In the solution preparation device of the above configuration, the amount of solution introduced into the IC analyzer is constant without changing, and only the solution concentration of the calibration curve solution is changed, so the baseline does not fluctuate and there is no risk of reducing the analysis accuracy. In addition, compared to creating a calibration curve by changing the amount of solution introduced into the IC analyzer, the dilution rate of the known concentration solution can be increased, so it is possible to create a calibration curve over a wide concentration range. Furthermore, when the method of preparing a test line solution in advance, performing an IC measurement, and then performing an IC measurement of the absorption liquid obtained by burning and absorbing an unknown sample is performed using an apparatus equipped with a mechanism for automatically introducing the solution into the IC measurement apparatus, a valve is required to switch between a nozzle that aspirates the calibration line solution and a nozzle that aspirates the analyte solution prepared by similarly aspirating the sample gas. However, with the solution preparation apparatus configured as shown in the figure, the calibration line solution and the analyte solution of the unknown sample are contained in the same absorption tube and can be introduced into the IC analysis apparatus separately, eliminating the need for a switching valve. EXAMPLES

[0031] The effectiveness of the method for preparing a solution for quantitative analysis of the present invention was confirmed by quantitatively analyzing a sample. An ethanol solution of (4-chloro-3-trifluoromethyl)phenylthiourea (F: 179.8 μg / mL, Cl: 111.8 μg / mL, S: 101.1 μg / mL) was used as a sample, and the fluorine, chlorine, and sulfur contents in the sample were analyzed by a combustion ion chromatography analyzer. We carried out IC analysis using the calibration curve solution prepared in the absorption tube of the solution preparation device of the above type, and a conventional IC analysis method using calibration curve solutions individually prepared by hand in a measuring flask, and confirmed the difference in the analysis results between these two analysis methods. Three solutions (samples) were prepared using each method and IC analysis was carried out. The results are shown in Table 1. As shown in Table 1, even when the analytical method of the present invention was used, analytical results equivalent to those of the conventional analytical method were obtained, confirming that the present invention can also perform analysis with the same level of accuracy as the conventional method.

[0032] [Table 1]

[0033] The configurations and configurations of the components of the solution preparation device described and illustrated above are merely examples, and the present invention is not limited to the configurations and configurations described and illustrated, but may have other appropriate configurations and configurations. The present invention can be applied as a method and device for preparing a solution for various analytical devices, including an ion chromatograph, that quantitatively analyzes unknown components contained in a sample using a calibration curve. [Explanation of symbols]

[0034] 1 IC analyzer, 2 solution preparation device, 3 absorption tube, 4 sample heating means, 5 dilution solution injection means, 6 known concentration solution injection means, 8 liquid level sensor

Claims

1. A method for preparing an analyte solution to be introduced into an apparatus for detecting an unknown component in a sample using a calibration curve, the method comprising the steps of: preparing a solution to be analyzed of the sample by placing an absorbing liquid for absorbing gas in an absorption tube and allowing the sample containing the unknown component to be thermally decomposed and the generated sample gas to be absorbed in the absorbing liquid; Using the same absorption tube as above, prepare a calibration curve solution by pouring a solution of known concentration into the absorption tube; A method for preparing a solution for quantitative analysis comprising the steps of:

2. 2. A method for preparing a solution for quantitative analysis according to claim 1, wherein the preparation of the sample solution to be analyzed and the preparation of the calibration curve solution are carried out by adding a diluting solution to the absorption tube.

3. 3. The method for preparing a solution for quantitative analysis according to claim 2, wherein the diluent is added to the absorption tube until the amount of the diluent is detected by a liquid level sensor provided in the absorption tube.

4. 3. The method for preparing a solution for quantitative analysis according to claim 2, wherein a fixed amount of the diluent is fed into the absorption tube by a metering pump.

5. 1. A solution preparation device for preparing an analyte solution to be introduced into an apparatus for detecting an unknown component in a sample for quantitative analysis of the unknown component using a calibration curve, comprising: an absorption tube in which the solution is prepared; a sample heating means for thermally decomposing the sample containing the unknown component to generate a sample gas; A diluent injection means for injecting a diluent into the absorption tube; a known concentration solution injection means for injecting a known concentration solution into the absorption tube; a function of absorbing the sample gas generated by the sample heating means into an absorbing liquid placed in the absorption tube and preparing an analyte solution of the sample by injecting a diluent into the absorption tube; A function of injecting a solution of known concentration into the absorption tube and a dilution solution to prepare a calibration curve solution; A solution preparation device for quantitative analysis comprising:

6. 6. The apparatus for preparing a solution for quantitative analysis according to claim 5, wherein the absorption tube is provided with a liquid level sensor.

7. 7. The device for preparing a solution for quantitative analysis according to claim 5, further comprising a function for automatically introducing the solution prepared in the absorption tube into a device for detecting an unknown component.

8. 8. The apparatus for preparing a solution for quantitative analysis according to claim 7, wherein the apparatus for detecting the unknown component is an ion chromatograph.

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