Thermal pressure measuring device and thermal pressure measuring method

JP2026166467APending Publication Date: 2026-10-14YOKOGAWA ELECTRIC CORP
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Patent Information

Application Number
JP2025059424
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2025-03-31
Publication Date
2026-10-14

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【0007】 本発明によれば、シンプルな構造で熱分析の効率を向上させることができる。

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Abstract

Its simple structure improves the efficiency of thermal analysis. [Solution] The thermal pressure measuring device 100 includes at least one sealable sealed container 1, either a heater 11 that heats the sealed container 1 to vaporize volatile components or a cooler 13 that cools the sealed container 1 to condense volatile components, or both, a heating thermometer 12 and / or a cooling thermometer 14 for measuring the temperature of the sealed container 1, a transfer pump 2 for creating a vacuum in the sealed container 1, a pressure gauge 5 for measuring the pressure inside the sealed container 1, a memory, and a processor connected to the memory. The processor performs identification of volatile components based on changes in the temperature and pressure inside the sealed container 1 containing the volatile components.
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Description

Technical Field

[0001] The present invention relates to a thermal pressure measurement device and a thermal pressure measurement method.

Background Art

[0002] Thermal analysis refers to a series of techniques for measuring a certain physical property of a substance as a function of temperature while varying the temperature of the substance according to a predetermined program. For example, thermogravimetry, which is one of the representative thermal analysis techniques, is a technique for measuring a change in weight when a sample is heated or cooled at a constant rate or held at a constant temperature. As techniques for component analysis of substances, mass spectrometry of gas components (Patent Document 1), analysis using a gas chromatograph in a sealed container (Patent Document 2), gas spectroscopic analysis (Patent Document 3), and the like have been proposed.

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Patent Document 2

Patent Document 3

Summary of the Invention

Problems to be Solved by the Invention

[0004] However, since thermogravimetry uses a precision balance, its structure is complicated. In addition, thermogravimetry may have a large measurement error due to the influence of gas flow, weight, and the like.

[0005] One aspect of the present invention improves the efficiency of thermal analysis with a simple structure.

Means for Solving the Problems

[0006] A thermal pressure measuring device relating to one aspect includes at least one sealable container, either a heater that heats the container to vaporize volatile components or a cooler that cools the container to condense the volatile components, or both, a thermometer for measuring the temperature of the container, an exhaust unit for creating a vacuum in the container, a pressure gauge for measuring the pressure inside the container, a memory, and a processor connected to the memory. The processor performs identification of the volatile components based on changes in the temperature and pressure inside the container containing the volatile components. [Effects of the Invention]

[0007] According to the present invention, the efficiency of thermal analysis can be improved with a simple structure. [Brief explanation of the drawing]

[0008] [Figure 1] This is a block diagram of a thermal pressure measuring device according to the first embodiment. [Figure 2] This figure shows the correlation between temperature and pressure of a substance containing multiple volatile components. [Figure 3] This figure shows the process for identifying volatile components. [Figure 4] This is a phase diagram of H2O. [Figure 5] This is a simplified diagram of a configuration used for thermal pressure measurement. [Figure 6] This is a phase diagram of the volatile components of a mixture of H2O, CO2, and NH3. [Figure 7] This is a flowchart of the separation process of specific volatile components using a heating process with a thermal pressure measuring device according to the first embodiment. [Figure 8] This is a flowchart of the separation process of specific volatile components using a cooling process with a thermal pressure measuring device according to the first embodiment. [Figure 9] This is a block diagram of a thermal pressure measuring device according to the second embodiment. [Figure 10] This is a block diagram of a thermal pressure measuring device according to the third embodiment. [Figure 11] This is a hardware configuration diagram of the analysis control device. [Modes for carrying out the invention]

[0009] Embodiments of the thermal pressure measuring device and thermal pressure measuring method will be described below with reference to the drawings. The same elements are denoted by the same reference numerals, and redundant explanations are omitted as appropriate. Furthermore, each embodiment can be combined as appropriate within the bounds of consistency.

[0010] Thermal analysis is used in various fields as a method for evaluating the physical properties of materials in relation to temperature. There are several techniques for thermal analysis depending on the physical properties to be detected. Commonly used thermal analysis techniques include differential thermal analysis, which detects the temperature difference with a reference material; differential scanning calorimetry, which detects the heat flow difference with a reference material; thermogravimetric analysis, which detects weight changes; thermomechanical analysis, which detects dimensional changes; and dynamic viscoelasticity, which detects the elastic modulus.

[0011] Differential scanning calorimetry (DSC) allows for the study of reactions and thermal histories, as well as the measurement of specific heat capacity, including transitions such as melting, glass transition, and crystallization. However, while DSC can measure sublimation, evaporation, and thermal decomposition, it is rarely performed due to the lack of quantitative accuracy caused by changes in sample volume during decomposition, and the possibility of sensor corrosion from decomposition gases.

[0012] Thermomechanical analysis primarily measures phenomena involving shape changes, such as thermal expansion, thermal contraction, glass transition, hardening reactions, and thermal history. However, while thermomechanical analysis can also detect melting and crystallization, which involve shape changes, melting can sometimes lead to adhesion to the probe, making proper analysis difficult.

[0013] Dynamic viscoelasticity measurements primarily capture phenomena associated with intramolecular motion and structural changes, and are used to examine glass transitions, crystallization, reactions, and thermal history. However, while dynamic viscoelasticity measurements can measure the initial state of melting, they become difficult to perform as melting progresses and the sample loses its shape, making proper analysis challenging.

[0014] On the other hand, in thermogravimetry, phenomena that exhibit weight changes due to sublimation, evaporation, thermal decomposition, dehydration, and the like are the subjects of analysis. In addition, phenomena in which weight changes occur accompanying reactions are also the measurement targets in thermogravimetry. Furthermore, with a simultaneous measurement apparatus for differential thermal analysis and thermogravimetry, many phenomena other than specific heat capacity are added as measurement targets.

[0015] Thermogravimetry is classified into types such as top-loading type, horizontal type, and suspension type depending on the difference in the positional relationship between the balance mechanism section and the sample section. For example, suspension-type thermogravimetry is regarded as a structure advantageous for high-sensitivity measurement. A thermogravimetry apparatus that performs suspension-type thermogravimetry operates based on the following principle as an example. When a sample suspended from one end of a balance beam into a heating furnace is heated according to a control program and a weight change occurs, the balance beam tilts. Then, when a photoelectric conversion element detects the tilt of the balance beam, an electric current flows through a feedback coil to generate an electromagnetic force, thereby returning the balance beam to the horizontal position. The current value at this time is recorded as the weight change. As the sample temperature, a signal from a thermocouple disposed in the vicinity of the sample is recorded. The thermogravimetry apparatus further includes a computer for heating control and data processing, a flow meter for controlling the flow rate of atmospheric gas during measurement, and the like.

[0016] In this way, the thermogravimetry apparatus can calculate the content ratio of volatile gas components relative to the total weight of the sample. In addition, the thermogravimetry apparatus can analyze gases having different volatilization temperatures. However, the thermogravimetry apparatus has several problems as described below. Since the thermogravimetry apparatus uses a precision balance, its structure is complicated. In addition, the thermogravimetry apparatus employs an open-tube configuration because the precision balance cannot be heated, and thus a carrier of an inert gas such as nitrogen is required to prevent the sample from being oxidized. For this reason, the thermogravimetry apparatus may cause errors in weight measurement due to buoyancy or the like generated from the gas flow. Furthermore, since the weight measurement sensitivity of the thermogravimetry apparatus is affected by gravity, measurement errors increase in locations with low gravity. Moreover, in the case of a substance whose triple point or boiling point is at a low temperature, the thermogravimetry apparatus must complete sublimation and vaporization at a low temperature, which takes time for the analysis process.

[0017] Thus, from the standpoint of the complexity of the device, measurement errors, and the time required for analysis processing, thermogravimetric devices are unsuitable for thermal analysis in conditions such as weightlessness. Therefore, a thermal pressure measuring device that enables efficient thermal analysis by performing thermal pressure measurements with a simple configuration will be described below.

[0018] (First Embodiment) (Overall structure) Figure 1 is a block diagram of a thermal pressure measuring device according to the first embodiment. The thermal pressure measuring device 100 is a device that performs thermal pressure analysis, including the identification of volatile components contained in a sample to be measured and the quantitative determination of each volatile component. Here, the identification of volatile components refers to, for example, the identification of the type of substance of the volatile component. Furthermore, the quantitative determination of volatile components refers to, for example, the calculation of the amount of substance of the volatile component.

[0019] The volatile components contained in the sample vaporize at high temperatures. Therefore, the thermal pressure measuring device 100 can perform two types of thermal pressure measurements for the identification and quantification of volatile components: a heating process measurement, which measures the pressure of the vaporized volatile components by raising the temperature of the sample, and a cooling process measurement, which measures the pressure of components other than the condensed volatile components by lowering the temperature of the sample.

[0020] The thermal pressure measuring device 100 includes a sealed container 1, a transfer pump 2, a storage cell 3, a recovery cell 4, a pressure gauge 5, a heater 11, a heating thermometer 12, a cooler 13, a cooling thermometer 14, valves 21-29, and an analysis control device 300.

[0021] The sealed container 1 is a sample chamber for storing the sample. The sample contains one or more types of volatile components, such as H2O, CO2, CH4, H2S, NH3, SO2, C2H4, or CH3OH.

[0022] The sealed container 1 is a container that can be sealed. In preparation for thermal pressure measurement, the sealed container 1 is evacuated by an exhaust valve to make it clean. A transfer pump 2 can be used as the exhaust valve. As a result, the sealed container 1 is free from residual gas that could cause measurement errors. In addition, the measurement room in which the sealed container 1 is placed is also evacuated and the pressure is reduced to 1 mPa or less.

[0023] The sealed container 1 is an example of a "container." That is, the thermal pressure measuring device 100 has a sealed container 1 which is at least one sealable container. The exhaust unit then creates a vacuum in the sealed container 1. By creating a vacuum in the sealed container 1, the exhaust unit removes any residual gas inside the sealed container 1.

[0024] For example, after the sealed container 1 is evacuated and the pressure gauge 5 has been adjusted, the sample is introduced into the container. If the sample is a gas, the sealed container 1 is evacuated before the sample is introduced. If the sample is a solid, the sealed container 1 may be evacuated after the sample has been introduced.

[0025] The heater 11 is placed, for example, inside the sealed container 1. The heater 11 heats part or all of the sealed container 1 to vaporize the volatile components contained in the sample stored in the sealed container 1. The heater 11 can be, for example, an optical heating device using an optical heating method such as laser light or an infrared lamp, a resistance heating device using a resistance heating method such as a resistance heater, or a Peltier element. In this way, the heater 11 heats the sealed container 1 to vaporize the volatile components.

[0026] The heating thermometer 12 can be, for example, an optical thermometer such as a bolometer. The heating thermometer 12 measures the temperature of the sealed container 1 when it is heated by the heater 11.

[0027] The cooler 13 is placed, for example, inside the sealed container 1. The cooler 13 cools the sealed container 1, causing the vaporized volatile components stored in the sealed container 1 to condense into a liquid or solid. The cooler 13 can be, for example, a cooling device using liquid nitrogen, liquid oxygen and liquid helium, a GM refrigerator, or a Peltier element. In this way, the cooler 13 cools the sealed container 1 and condenses the volatile components. Here, the heater 11 and the cooler 13 can be temperature-controlled, for example, in the range of 300K to 40K.

[0028] The cooling thermometer 14 can be, for example, a silicon diode or a platinum resistance thermometer. The cooling thermometer 14 measures the temperature of the sealed container 1 when it is cooled by the cooler 13.

[0029] In this embodiment, the thermal pressure measuring device 100 is equipped with both a heater 11 and a heating thermometer 12, and a cooler 13 and a cooling thermometer 14, in order to measure thermal pressure during both the heating process and the cooling process. However, to measure the heating process, the thermal pressure measuring device 100 only needs to be equipped with the heater 11 and the heating thermometer 12. To measure the cooling process, the thermal pressure measuring device 100 only needs to be equipped with the cooler 13 and the cooling thermometer 14.

[0030] Here, the heating thermometer 12 and the cooling thermometer 14 are examples of "thermometers." That is, the thermometers measure the temperature of the sealed container 1. The thermometers also include either or both of the heating thermometer 12, which measures the temperature of the sealed container 1 when it is heated by the heater 11, or the cooling thermometer 14, which measures the temperature of the sealed container 1 when it is cooled by the cooler 13, depending on the installation of the heater 11 or the cooler 13.

[0031] In this embodiment, one heater 11 and one cooler 13 are placed in the sealed container 1. However, the invention is not limited to this configuration, and multiple heaters 11 and coolers 13, or multiple units of either one, may be placed in the container.

[0032] Since the pressure gauge 5 measures the total pressure of the mixed gas inside the sealed container 1, it is preferable that its measurement sensitivity is not affected by the type of gas. Furthermore, it is preferable that the pressure gauge 5 can measure absolute pressures from 1 Pa to 100 kPa with high resolution.

[0033] The pressure gauge 5 is a highly sensitive, high-resolution absolute pressure sensor, and for example, a Si vibration type absolute pressure sensor can be used. The Si vibration type absolute pressure sensor uses a Si oscillator mounted on a diaphragm as the detection element and has a vacuum reference chamber inside the sensor chip. The Si vibration type absolute pressure sensor has high resolution and can measure pressure with a resolution of 1 mPa or less, enabling the detection and quantitative measurement of smaller samples and minute components. By zero-point calibration in a high vacuum, the Si vibration type absolute pressure sensor can measure down to a vacuum level of about 0.01 Pa, allowing for the measurement of minute pressure changes in thermal pressure measurements.

[0034] For example, if a Si vibration type absolute pressure sensor is used as the pressure gauge 5, the pressure gauge 5 can have a measurement accuracy of ±2 Pa, a measurement resolution of 1 mPa or less, and a sampling period of 100 msec. In this case, the pressure gauge 5 that measures the pressure in the sealed container 1 can measure changes in vacuum degree from 1 kPa to 0.1 Pa with high reproducibility and high resolution, regardless of the type of volatile component, and can detect minute pressure changes due to phase changes of the gas. Furthermore, since pressure measurement can be achieved with a small pressure sensor, the pressure gauge 5, the entire device can be made smaller and lighter.

[0035] The pressure gauge 5 is zeroed in preparation for thermal pressure analysis. Then, the path to which the pressure gauge 5 is connected is evacuated by the exhaust section until no pressure rise occurs in the pressure gauge 5 for more than one minute with the valve 21 closed. A transfer pump 2 can be used for this exhaust section.

[0036] The pressure gauge 5 measures the pressure inside the sealed container 1. A high-resolution vibration-type absolute pressure sensor can also be used for the pressure gauge 5.

[0037] The storage cell 3 is a container for temporarily storing vaporized volatile components. In this embodiment, one storage cell 3 is provided. The storage cell 3 is controlled to an appropriate temperature so that the volatile components inside remain in a gaseous state.

[0038] The recovery cell 4 is a container for recovering vaporized volatile components. The recovery cell 4 is detachable from the pipe through which the vaporized volatile components are supplied. Multiple recovery cells 4 exist. In this embodiment, one recovery cell 4 can be connected to the pipe through which the vaporized volatile components are supplied, and by changing the recovery cell 4 connected to the pipe, different types of volatile components can be recovered in different recovery cells 4. The recovery cell 4 is an example of a "detachable predetermined container".

[0039] The transfer pump 2 can be, for example, a vacuum pump. Alternatively, a vacuum space can be used as the transfer pump 2. The transfer pump 2 exhausts or transfers vaporized volatile components. For example, the transfer pump 2 can transfer vaporized volatile components from inside the sealed container 1 to the storage cell 3 or the recovery cell 4.

[0040] This transfer pump 2 is an example of a "transfer device." In other words, the transfer pump 2, which is a transfer device, transfers the vaporized volatile components inside the sealed container 1 to another container.

[0041] In this embodiment, one end of the transfer pump 2 is connected to the discharge port of the sealed container 1 by a pipe. Valves 21 and 22 are provided on the pipe connecting the transfer pump 2 and the sealed container 1. Valve 21 is, for example, a stop valve that opens and closes the discharge port of the sealed container 1. Valve 22 branches off from the pipe connecting the sealed container 1 and the transfer pump 2, and extends a pipe that connects to the second opening of the storage cell 3 and the pipe connecting the transfer pump 2 and the recovery cell 4. Valve 22 switches between a connection state that connects the sealed container 1 and the transfer pump 2, and a connection state that connects the pipes extending from valve 22 other than the pipe extending to the transfer pump 2 and the pipe extending to the sealed space with the pipe extending to the transfer pump 2.

[0042] Furthermore, the other end of the transfer pump 2 is connected to a pipe that connects to the external discharge port 30, the storage cell 3, and the recovery cell 4. A valve 23 is provided on the other end of the transfer pump 2. The valve 23 is connected to the pipe extending to the external discharge port 30 and to the pipe that connects to the storage cell 3 and the recovery cell 4. The valve 23 switches the connection destination of the transfer pump 2 to either the external discharge port 30 or the pipe that connects to the storage cell 3 and the recovery cell 4.

[0043] Furthermore, the pipe extending from valve 23 to storage cell 3 and recovery cell 4 branches into a pipe leading to storage cell 3 and a pipe leading to recovery cell 4. The pipe that branches off from valve 23 and leads to storage cell 3 is connected to the first opening of storage cell 3. Here, the opening connected to the pipe that branches off from the pipe connecting the transfer pump 2 of storage cell 3 and recovery cell 4 is called the first opening of storage cell 3. The opening on the side of storage cell 3 that is connected to valve 22 is called the second opening of storage cell 3.

[0044] A valve 24 is provided at the first opening of the storage cell 3. The valve 24 opens and closes the first opening of the storage cell 3. A valve 28 is provided at the second opening of the storage cell 3. The valve 28 opens and closes the second opening of the storage cell 3.

[0045] Furthermore, a pipe extending from valve 23 and branching off to the recovery cell 4 is connected to the intake port of the recovery cell 4. A valve 27 is provided at the intake port of the recovery cell 4. Valve 27 opens and closes the intake port of the recovery cell 4. When attaching or detaching the recovery cell 4, the intake port of the recovery cell 4 is closed by valve 27.

[0046] Furthermore, the pipe extending from valve 23 towards storage cell 3 branches off, and the pipe leading to recovery cell 4 branches off again at two points along the way. One of the branched pipes bypasses storage cell 3 and connects to valve 22. Valve 25 is provided on this branched pipe. Valve 25 opens and closes the section where the bypass pipe for storage cell 3 connects to the pipe connecting the transfer pump 2 and recovery cell 4. Hereafter, the pipe connecting valve 25 and valve 22, which does not go through the transfer pump 2, will be referred to as the bypass pipe. This branched pipe also branches off again on its way to valve 22, and the branched pipe connects to the second opening of storage cell 3.

[0047] Furthermore, one of the pipes that branches off from the pipe leading to the recovery cell 4 after the pipe extending from valve 23 towards the storage cell 3 branches off is connected to the suction port of the sealed container 1. A valve 26 is provided on the other branched pipe. Valve 26 opens and closes the portion of the other branched pipe that connects to the pipe connecting the transfer pump 2 and the recovery cell 4. A valve 29 is also provided at the suction port of the sealed container 1. Valve 29 opens and closes the suction port of the sealed container 1.

[0048] (Analysis control device) The analysis control device 300 controls the transfer pump 2, valves 21-29, heater 11, and cooler 13 to heat or cool the sealed container 1, and performs thermal pressure measurement of volatile components contained in the sample based on the temperature and pressure changes inside the sealed container 1. The analysis control device 300 has a control unit 301 and an analysis unit 302. The control unit 301 and the analysis unit 302 are implemented, for example, by a processor mounted on the analysis control device 300.

[0049] The analysis unit 302 is connected to the pressure gauge 5, the heater 11, the heating thermometer 12, the cooler 13, and the cooling thermometer 14. The analysis unit 302 acquires information on the temperature and pressure inside the sealed container 1, measured by the thermometer 12 or 14 and the pressure gauge 5, when part or all of the sealed container 1 is heated or cooled by the heater 11 or the cooler 13. The analysis unit 302 then acquires the changes in the temperature and pressure inside the sealed container 1 due to heating or cooling part or all of the container by the heater 11 or the cooler 13 from the information measured by the thermometer 12 or 14 and the pressure gauge 5. The analysis unit 302 then measures the vapor pressure curve from the change curve showing the changes in temperature and pressure inside the sealed container 1.

[0050] In the heating process measurement, the analysis unit 302 instructs the control unit 301 to heat the inside of the sealed container 1. Next, the analysis unit 302 heats the solid sample placed inside the sealed container 1 at a predetermined heating rate and records the pressure change inside the sealed container 1.

[0051] When volatile components vaporize, the pressure inside the sealed container 1 changes significantly. Therefore, the analysis unit 302 can determine that vaporization of some volatile components has begun due to the large change in pressure inside the sealed container 1. The analysis unit 302 further increases the temperature inside the sealed container 1, and once the pressure change stabilizes, it determines that the vaporization of some volatile components has ceased.

[0052] The analysis unit 302 then obtains the measurement result of the pressure change in the sealed container 1 under those conditions from the pressure gauge 5. This allows the analysis unit 302 to calculate the total amount of vaporized volatile components.

[0053] Furthermore, since the heating process is a sublimation phenomenon at very low temperatures, the amount of volatilization is small, and it takes a very long time for all volatile components to vaporize. As a result, the heating rate is extremely slow, requiring long-term measurements. Therefore, in heating process measurements, the rate of pressure change is very slow, and it may be difficult for the thermal pressure measuring device 100 to accurately grasp the pressure change.

[0054] During the cooling process measurement, the analysis unit 302 obtains the pressure measurement result of the sealed container 1 when all the volatile components contained in the sample have vaporized from the pressure gauge 5. This allows the analysis unit 302 to calculate the total amount of vaporized volatile components.

[0055] Next, the analysis unit 302 instructs the control unit 301 to cool the vaporized volatile components inside the sealed container 1. Then, the analysis unit 302 cools the inside of the sealed container 1 at a predetermined cooling rate and records the pressure change inside the sealed container 1.

[0056] When volatile components condense, the pressure inside the sealed container 1 changes significantly. Therefore, the analysis unit 302 can determine that the condensation of some volatile components has begun due to the large change in pressure inside the sealed container 1. The analysis unit 302 further lowers the temperature inside the sealed container 1, and once the pressure change stabilizes, it determines that the condensation of volatile components has ceased.

[0057] The analysis unit 302 then obtains the measurement result of the pressure change in the sealed container 1 in that state from the pressure gauge 5. This allows the analysis unit 302 to calculate the total amount of aggregated volatile components.

[0058] Furthermore, the condensation process occurs rapidly because vaporized volatile components come into contact with a cooled surface and are cooled, causing them to liquefy or solidify. As a result, pressure changes occur in a relatively short time, allowing the thermal pressure measuring device 100 to perform measurements quickly.

[0059] Here, the analysis unit 302 performs thermal pressure analysis based on the information obtained from the heating process measurement or the cooling process measurement to identify each volatile component and calculate the amount of substance. For example, in the heating process measurement, the sample is heated in the sealed container 1 and the volatile components vaporize, so the pressure inside the sealed container 1 rises from a vacuum state due to the accumulation of vaporized volatile components. In this case, the total pressure inside the sealed container 1 is the sum of the partial pressures of each vaporized volatile component. Each volatile component vaporizes according to its own unique phase change characteristics based on its vapor pressure characteristics. Therefore, when the heating temperature of the sample is slowly increased at a constant rate, the pressure inside the sealed container 1 shows a pressure change where the phase change characteristics of each volatile component overlap. Thus, the analysis unit 302 identifies the volatile components vaporized in the sealed container 1 from the temperature and pressure changes due to heating. The analysis unit 302 also calculates the molar ratio of each volatile component from the pressure change.

[0060] Furthermore, during the cooling process measurement, if volatile components that have cooled and reached their dew point inside the sealed container 1 condense, the volume of the condensed volatile components decreases, and therefore the pressure inside the sealed container 1 decreases. In this case, the total pressure inside the sealed container 1 is the sum of the partial pressures of each remaining volatile component. The condensed volatile components liquefy or solidify due to their unique phase change characteristics that depend on temperature and pressure. Therefore, when the sealed container 1 is cooled slowly at a constant temperature, the pressure inside the sealed container 1 changes significantly before and after the volatile components condense. The analysis unit 302 then identifies the liquefied or solidified volatile components that fill the inside of the sealed container 1 from the temperature and pressure changes due to cooling. The analysis unit 302 also calculates the molar ratio of each volatile component from the pressure change. Hereafter, the phase change characteristics that depend on temperature and pressure will simply be referred to as "phase change characteristics".

[0061] Here, we will explain the unique phase change characteristics of each volatile component. Figure 2 is a diagram showing the temperature and pressure correlation of a substance containing multiple volatile components. Figure 2 shows two graphs 101 and 102. Graph 101 shows pressure on the vertical axis and temperature on the horizontal axis. Graph 102 shows the temperature dependence of pressure on the vertical axis and temperature on the horizontal axis. The analysis data can be obtained, for example, by continuously measuring the absolute pressure inside the sealed container 1 with the finest precision and accuracy possible using a pressure gauge 5, which is a highly sensitive and accurate absolute pressure sensor, and simultaneously measuring the internal temperature with a heating thermometer 12 or a cooling thermometer 14.

[0062] The analysis unit 302 detects the temperature at which a large pressure change occurs inside the sealed container 1. For example, the analysis unit 302 obtains the amount of pressure change in graph 102 by differentiating the pressure change obtained in graph 101 with respect to temperature. The analysis unit 302 can then set the peak of the amount of pressure change in graph 102 to the temperatures T1, T2, and T3, or T1', T2', and T3', which correspond to the heating process and the cooling process, respectively, at which the pressure change in graph 101 is large. A large pressure change indicates that a phase change, such as vaporization of volatile components, or liquefaction or solidification due to condensation, is occurring at that point. That is, a phase change of volatile components is occurring in the regions 111 to 113 corresponding to temperatures T1 and T1', T2 and T2', and T3 and T3', respectively. Temperatures T1, T2, and T3 are the temperatures at which vaporization begins. Temperatures T1', T2', and T3' are the temperatures at which condensation occurs. The phase change characteristics of a particular volatile component closely match the vapor pressure curve of that specific volatile component that vaporizes or condenses at that temperature. Therefore, the analysis unit 302 can identify the volatile component by comparing the phase change characteristics with the vapor pressure curves of various substances.

[0063] The relationship between changes in temperature and pressure inside sealed container 1, phase change characteristics, and vapor pressure curve, as well as identification and quantitative processing using changes in temperature and pressure inside sealed container 1, will be further explained. Since an ideal gas follows the law of state P=nRT / V, the pressure and temperature change linearly through absolute temperature 0. Here, n is the number of moles, R is the gas constant, and V is the volume of sealed container 1. In graph 101, the lines 114-116 show the changes in the volatile components of the gaseous state.

[0064] On the other hand, when volatile components vaporize or condense, the pressure inside the sealed container 1 in the range where vaporization or condensation occurs undergoes temperature and pressure changes corresponding to the vapor pressure curve. Figure 3 is a diagram showing the process of identifying volatile components. For example, the analysis unit 302 obtains a curve 201 showing the relationship between temperature and pressure in Figure 3 as the phase change characteristic in region 113 of graph 101. Here, the analysis unit 302 has a database 202 containing, for example, vapor pressure curves 221 of various substances. Since the vapor pressure curve 221 is a change specific to gas molecules, the analysis unit 302 compares the curve 201 with each vapor pressure curve 221 included in the database 202 to identify a vapor pressure curve 221 that closely matches the curve 201. Then, the analysis unit 302 identifies the volatile component that underwent a phase change in region 113 by identifying the substance with the matching vapor pressure curve 221 as a volatile component.

[0065] Furthermore, the analysis unit 302 can determine the number of moles n of condensed volatile gas molecules from the pressure changes shown in graph 102 as n = VΔP / RT. Since the volatile components have been identified, the analysis unit 302 can then calculate the total weight w of the volatile gas molecules from their molecular weight M as w = nM.

[0066] In this case, when multiple gases are mixed, the analysis unit 302 will show a stepwise change in pressure as the temperature changes, and similarly, it is possible to identify and quantify each volatile component. For example, Graph 102 shows an example where three types of volatile components are mixed, in which case the analysis unit 302 is able to identify each of the three volatile components and quantify them by calculating the amount of substance.

[0067] For example, if the phase change characteristics in region 111 closely match the vapor pressure curve of gas A, the analysis unit 302 determines that the volatile component that underwent a phase change at temperature T1 is gas A. Similarly, if the phase change characteristics in region 112 closely match the vapor pressure curve of gas B, the analysis unit 302 determines that the volatile component that underwent a phase change at temperature T2 is gas B. Furthermore, if the phase change characteristics in region 113 closely match the vapor pressure curve of gas C, the analysis unit 302 determines that the volatile component that underwent a phase change at temperature T3 is gas C. The analysis unit 302 may also use temperatures T1', T2', and T3' to identify volatile gases.

[0068] Furthermore, the identification process performed by the analysis unit 302 will be explained in detail. Figure 4 is a phase diagram of H2O. In Figure 4, the vertical axis shows pressure and the horizontal axis shows temperature. Referring to Figure 4, the operation when the volatile component is a single component will be explained using the case of H2O as an example. The vapor pressure curve 121 is shown in the phase diagram of Figure 4.

[0069] Based on the phase diagram in Figure 4, the analysis unit 302 obtains the pressure Ps, which is the lower limit of the measurement pressure for H2O, the temperature Ts, at which the saturated water vapor pressure reaches pressure Ps, the temperature Tj, and the pressure Pj at which all the ice volatilizes, when the temperature is changed from 50K to 300K. Here, the range of (temperature Ts, pressure Ps) to (temperature Tj, pressure Pj) of the vapor pressure curve 121 is the region in which H2O undergoes a phase change from gas to solid, and corresponds to the phase change characteristics of H2O inside the sealed container 1 measured by the analysis unit 302.

[0070] Therefore, the analysis unit 302 calculates a measurement curve 122 showing the phase change characteristics of H2O from the measurement results of the pressure gauge 5 and the heating thermometer 12 or cooling thermometer 14, in the range of (temperature Ts, pressure Ps) to (temperature Tj, pressure Pj). Then, by comparing the obtained measurement curve 122 with the range of (temperature Ts, pressure Ps) to (temperature Tj, pressure Pj) of the vapor pressure curve 121 of H2O, the analysis unit 302 can identify that the volatile component is H2O and calculate the amount of volatile component H2O that volatilizes. Furthermore, the analysis unit 302 can calculate the amount of volatile H2O molars from the volume, temperature, and pressure Pj of the sealed container 1.

[0071] Next, we will describe the thermal pressure measurement using the analytical control device 300 when multiple volatile components are contained in the sample. For example, suppose that volatile components #1, #2, and #3 are contained in the sample, and the volatile molar amounts of each component are C1, C2, and C3. Also, the partial pressures Pn of each volatile component #1, #2, and #3 are given by Pn = k × Cn × T / T0 × (22.4 / V). Here, n is 1, 2, or 3. Also, k is a constant. Also, T0 is the reference temperature. Furthermore, T is the temperature of the sealed container 1. In this case, the pressure P inside the sealed container 1 is P = P1 + P2 + P3.

[0072] Under conditions where a gas follows the ideal gas law, when the temperature T is changed from 50K to 300K, the pressure P changes proportionally with the temperature, and the pressure P changes significantly at the temperature at which volatile components vaporize or condense. Therefore, the analysis unit 302 can detect deviations from the ideal gas law by precisely measuring the pressure P.

[0073] Here, since condensation reactions are more likely to occur than sublimation reactions, we will explain using the cooling process measurement as an example. When volatile components are cooled, the change in pressure P becomes suddenly large at the temperature at which condensation occurs. When the volatile components are condensed and liquefied or solidified at that temperature, the condensed volatile components are almost completely eliminated from the residual gas.

[0074] Therefore, the analysis unit 302 records the pressure change of volatile components due to aggregation simultaneously with the temperature, thereby obtaining the phase change characteristics of the volatile components at temperature and pressure. The analysis unit 302 identifies and quantifies the volatile components by comparing the obtained phase change characteristics with the vapor pressure curve. In multi-component systems containing multiple volatile components in the sample, the analysis unit 302 repeatedly causes the control unit 301 to perform aggregation of the volatile components by changing the temperature, thereby identifying each of the multiple volatile components and quantifying them by calculating the amount of substance.

[0075] Next, we will describe a specific example of thermal pressure measurement using the analytical control device 300 when the sample contains multiple volatile components. Figure 5 is a simplified configuration diagram for thermal pressure measurement. Here, we will explain using the example of measuring the cooling process in a three-component system of CO2, H2O, and NH3.

[0076] For example, a mixture of H2O, CO2, and NH3 is poured into the sealed container 1 using the inlet A2. The sealed container 1 is cooled while its temperature is measured by the cooling thermometer 14. In Figure 5, the sealed container 1 is placed in a constant temperature bath 15. Alternatively, the sealed container 1 may be cooled by thermal contact with a temperature-controlled heat bath.

[0077] Figure 6 is a phase diagram of the volatile components of a mixture of H2O, CO2, and NH3. In Figure 6, the vertical axis represents pressure and the horizontal axis represents temperature. Graph 131 is the vapor pressure curve for H2O. Graph 132 is the vapor pressure curve for CO2. Graph 133 is the vapor pressure curve for NH3.

[0078] As shown in Figure 6, in the temperature range of 50K to 300K, graphs 131 to 133 all change exponentially due to phase change in the range of 1Pa to 100Pa W. On the other hand, the volatile components contained in the residual gas in the sealed container 1 change as a linear function of temperature according to the ideal gas law. Therefore, the analysis unit 302 can identify H2O, NH3, and CO2 by comparing the change in the slope of the phase change characteristics of each volatile component obtained from the measurement results with graphs 131 to 133 in Figure 6. Furthermore, the analysis unit 302 can calculate the amount of each substance of H2O, NH3, and CO2 and perform quantitative analysis of each.

[0079] Thus, the analysis unit 302, implemented by the processor, identifies the volatile components based on changes in temperature and pressure inside the sealed container 1 containing the volatile components. The analysis unit 302 also quantifies the volatile components present in the sealed container 1 based on changes in temperature and pressure inside the sealed container 1.

[0080] Furthermore, in the heating process measurement, the analysis unit 302 heats the sample stored in the sealed container 1 using the heater 11. Then, the analysis unit 302 identifies the volatile components contained in the sample based on the temperature rise inside the sealed container 1 measured by the heating thermometer 12 and the pressure rise inside the sealed container 1 measured by the pressure gauge 5.

[0081] Furthermore, during the cooling process measurement, the analysis unit 302 uses the cooler 13 to lower the temperature of the volatile components that have been released from the sample by vaporization and stored in the sealed container 1. The analysis unit 302 then identifies the volatile components contained in the sample based on the temperature drop inside the sealed container 1 measured by the cooling thermometer 14 and the pressure drop inside the sealed container 1 measured by the pressure gauge 5.

[0082] Furthermore, the analysis unit 302 compares data on the temperature and pressure changes inside the sealed container 1 with the vapor pressure curve of the substance to identify the volatile components.

[0083] It is fundamentally difficult to identify all volatile components solely by vapor pressure differences. Therefore, in the case of mixed gases where volatile components are difficult to identify, the thermal pressure measuring device 100 may use other methods such as molecular size analysis or adsorption in combination to reliably achieve analysis of volatile components. For example, the thermal pressure measuring device 100 performs a separation and extraction process that includes a heating process and a cooling process. For example, if only a specific volatile component inside the sealed container 1 is in a gaseous state, the thermal pressure measuring device 100 recovers the volatile component in the recovery cell 4 through the cooling process. Alternatively, if only a specific volatile component inside the sealed container 1 is in a solid or liquid state, the thermal pressure measuring device 100 vaporizes the volatile component through the heating process and recovers it in the recovery cell 4. In this way, the thermal pressure measuring device 100 also performs a heating process and a cooling process in the separation and extraction process. Since the thermal pressure measuring device 100 can recover volatile components that are difficult to identify by thermal pressure measurement in the recovery cell 4, other analytical methods can be easily implemented.

[0084] (Separation and extraction of volatile components) Next, the operation sequence of the transfer pump 2 and valves 21-20 related to the separation and extraction of vaporized volatile components inside the sealed container 1 will be described. The control unit 301 controls the transfer pump 2, valves 21-29, heater 11, and cooler 13 based on instructions from the analysis unit 302. For example, during the heating process, the control unit 301 controls the heater 11 to heat the sealed container 1, which is a sealed space, and vaporize the volatile components contained in the sample stored in the sealed container 1. During the cooling process, the control unit 301 controls the cooler 13 to cool the sealed container 1, which is a sealed space, and condense the vaporized volatile components inside the sealed container 1, causing them to liquefy or solidify.

[0085] Furthermore, the control unit 301 controls the opening and closing of valves 21 to 29 during the heating and cooling processes to switch the pipe connections. After switching the pipe connections, the control unit 301 causes the vaporized volatile components to be discharged or transferred through the transfer pump 2.

[0086] For example, when the control unit 301 discharges vaporized volatile components from inside the sealed container 1 through the external outlet 30 using the transfer pump 2, it controls valves 21 to 29 as follows: Valve 21 is opened, opening the outlet of the sealed container 1. Valve 22 connects the sealed container 1 to the transfer pump 2. Valve 23 is switched so that the transfer pump 2 is connected to the external outlet 30.

[0087] Furthermore, when the control unit 301 transfers the vaporized volatile components inside the sealed container 1 to the storage cell 3 using the transfer pump 2, it controls valves 21 to 29 as follows: Valve 21 is opened, opening the outlet of the sealed container 1. Valve 22 connects the sealed container 1 to the transfer pump 2. Valve 23 connects the transfer pump 2 to the pipe leading to the storage cell 3. Valve 24 is opened, opening the first opening of the storage cell 3. Valves 25 to 29 are closed.

[0088] Furthermore, when the control unit 301 transfers the vaporized volatile components inside the sealed container 1 to the recovery cell 4 using the transfer pump 2, it controls valves 21 to 29 as follows: Valve 21 is opened, opening the outlet of the sealed container 1. Valve 22 connects the sealed container 1 to the transfer pump 2. Valve 23 connects the transfer pump 2 to the pipe leading to the recovery cell 4. Valve 27 is opened, opening the suction port of the recovery cell 4. Valves 24 to 26, 28 and 29 are closed.

[0089] Furthermore, when the control unit 301 transfers the vaporized volatile components inside the storage cell 3 to the sealed container 1 using the transfer pump 2, it controls valves 21 to 29 as follows: Valve 22 connects the transfer pump 2 to the pipe that connects to the second opening of the storage cell 3. Valve 28 is opened, opening the second opening of the storage cell 3. Valve 26 is opened, connecting the pipe extending from the transfer pump 2 to the pipe that connects to the suction port of the sealed container 1. Valve 29 is opened, opening the suction port of the sealed container 1. Valves 21, 24, 25 and 27 are closed.

[0090] Furthermore, when the control unit 301 transfers vaporized volatile components from inside the storage cell 3 to the recovery cell 4 using the transfer pump 2, it controls valves 21 to 29 as follows: Valve 22 connects the transfer pump 2 to the pipe that connects to the second opening of the storage cell 3. Valve 28 is opened, opening the second opening of the storage cell 3. Valve 27 is opened, opening the suction port of the recovery cell 4. Valves 21, 23, 24, 25, 26 and 29 are closed.

[0091] Furthermore, when purging residual gas inside the sealed container 1, the control unit 301 controls valves 21 to 29 as follows: Valve 21 is opened, opening the outlet of the sealed container 1. Valve 22 is connected to the pipe that connects the transfer pump 2 to the outlet of the sealed container 1. Valve 23 is connected to the transfer pump 2 to the external outlet 30. Valves 24 to 29 are closed.

[0092] Furthermore, when purging residual gas inside the storage cell 3, the control unit 301 controls valves 21 to 29 as follows: Valve 28 is opened, opening the second opening of the storage cell 3. Valve 22 is connected to the pipe connecting the transfer pump 2 to the second opening of the storage cell 3. Valve 23 is connected to the transfer pump 2 to the external outlet 30. Valves 21, 24 to 27 and 29 are closed.

[0093] Furthermore, when purging residual gas inside the recovery cell 4, the control unit 301 controls valves 21 to 29 as follows: Valve 27 is opened, opening the intake port of the recovery cell 4. Valve 22 connects the transfer pump 2 to the bypass pipe. Valve 25 is opened, connecting the bypass pipe to the pipe leading to the recovery cell 4. Valve 23 connects the transfer pump 2 to the external discharge port 30. Valves 21, 24, 26, 28 and 29 are closed.

[0094] Furthermore, when purging the pipe on the side of the transfer pump 2 that connects to the sealed container 1, the control unit 301 controls valves 21 to 29 as follows: Valve 22 connects the transfer pump 2 to the bypass pipe. Valve 25 is opened and connects the bypass pipe to the pipe connected to valve 26. Valve 26 is opened and connects the bypass pipe to the pipe connected to the suction port of the sealed container 1. Valve 23 connects the transfer pump 2 to the external discharge port 30. Valves 21, 24 and 27 to 29 are closed.

[0095] Furthermore, when purging the pipe connected to valve 23 of the transfer pump 2, the control unit 301 controls valves 21 to 29 as follows: Valve 22 connects the transfer pump 2 to the bypass pipe. Valve 25 is opened and connects the bypass pipe to the pipe connected to valve 26. Valve 23 connects the pipe on the opposite side of the transfer pump 2 to the external discharge port 30. Valves 21, 24 and 26 to 29 are closed.

[0096] Note that the control of valves 21-29 shown here is just one example, and the control unit 301 can control each of valves 21-29 according to the purpose.

[0097] Here, the separation and extraction of specific volatile components during the heating process by the control unit 301 will be explained. Here, it is assumed that the control unit 301 appropriately controls the transfer pump 2 and opens and closes valves 21 to 29 according to the process to be executed, so the explanation of the control of the transfer pump 2 and the opening and closing of valves 21 to 29 will be omitted.

[0098] The control unit 301 controls the heater 11 to gradually heat the sample stored in the sealed container 1, thereby vaporizing the volatile components contained in the sample.

[0099] Subsequently, if the pressure inside the sealed container 1 changes significantly, the control unit 301, upon receiving instructions from the analysis unit 302, maintains the temperature at that time. This allows the control unit 301 to extract some of the volatile components contained in the sample. After the significant change in pressure inside the sealed container 1 subsides, the control unit 301, upon receiving instructions from the analysis unit 302, transfers the vaporized volatile components inside the sealed container 1 to the recovery cell 4 using the transfer pump 2, thereby separating and recovering some of the volatile components in the recovery cell 4.

[0100] Next, the control unit 301 controls the heater 11 to restart the temperature rise inside the sealed container 1, and repeats the vaporization of volatile components contained in the sample and their collection into the recovery cells 4 in order of increasing vaporization temperature. Each time volatile components are collected, a new recovery cell 4 is attached. In this way, the control unit 301 can collect each volatile component contained in the sample into a different recovery cell 4.

[0101] Next, the separation and extraction of specific volatile components during the cooling process by the control unit 301 will be described. Here again, the control unit 301 appropriately controls the transfer pump 2 and opens and closes the valves 21 to 29 according to the process being executed, so the explanations of the control of the transfer pump 2 and the opening and closing of the valves 21 to 29 will be omitted.

[0102] The control unit 301 controls the heater 11 to heat the sealed container 1 and vaporize all the volatile components contained in the sample. Subsequently, the control unit 301 controls the cooler 13 to cool the sealed container 1 and condense some of the vaporized volatile components present inside the sealed container 1.

[0103] When the pressure inside the sealed container 1 changes significantly, the control unit 301 receives instructions from the analysis unit 302 and maintains the temperature at that time. This allows the control unit 301 to solidify or liquefy some of the volatile components contained in the sample and extract them.

[0104] Next, the control unit 301 separates some of the condensed volatile components from the residual gas by transferring the residual gas inside the sealed container 1 to the storage cell 3 using the transfer pump 2. Then, the control unit 301 controls the heater 11 to vaporize some of the condensed volatile components remaining in the sealed container 1. After that, the control unit 301 separates some of the volatile components from the vaporized volatile components inside the sealed container 1 to the recovery cell 4 using the transfer pump 2 and recovers them in a specific recovery cell 4.

[0105] Next, the control unit 301 uses the transfer pump 2 to transfer the residual gas inside the storage cell 3 back to the sealed container 1. Then, the control unit 301 repeats the aggregation, separation, vaporization, and recovery of the volatile components contained in the sample into the recovery cell 4, in order of decreasing aggregation temperature. The recovery cell 4 is replaced with a new recovery cell 4 each time volatile components are recovered. In this way, the control unit 301 can recover each volatile component contained in the sample into a different recovery cell 4.

[0106] Figure 7 is a flowchart of the separation process of specific volatile components using the heating process by the thermal pressure measuring device according to the first embodiment. Next, referring to Figure 7, the flow of the separation process of specific volatile components using the heating process by the thermal pressure measuring device 100 according to this embodiment will be explained. Here, preliminary preparations such as vacuuming the measurement area of ​​the sealed container 1 and pressure gauge 5, adjusting the pressure gauge 5, injecting the sample into the sealed container 1, and sealing the sealed container 1 have already been completed. The control unit 301 controls the transfer pump 2, heater 11, cooler 13, and valves 21-29 based on instructions from the analysis unit 302, but the instructions from the analysis unit 302 may be omitted here. Here, as an example, temperatures T1, T2, and T3 shown in Figure 2 will be explained as threshold temperatures. The analysis unit 302 has temperature T1 as the initial threshold temperature and changes the threshold temperature in the order of temperature T1, temperature T2, and temperature T3.

[0107] The control unit 301 controls the cooler 13 to cool the inside of the sealed container 1 and condense all the volatile components present inside the sealed container 1 (step S1).

[0108] Next, the control unit 301 controls the heater 11 to heat the inside of the sealed container 1 (step S2).

[0109] When the analysis unit 302 confirms from the measurement results of the heating thermometer 12 that the temperature inside the sealed container 1 has reached the threshold temperature, it instructs the control unit 301 to maintain the temperature. Upon receiving the instruction from the analysis unit 302, the control unit 301 maintains the temperature inside the sealed container 1 at the threshold temperature (step S3).

[0110] Next, the analysis unit 302 confirms that the vaporization of volatile components that vaporize at the current threshold temperature is complete (step S4).

[0111] Once the vaporization of the volatile components that vaporize at the current threshold temperature is complete, the control unit 301 controls the transfer pump 2 and valves 21-29 to transfer the vaporized volatile components inside the sealed container 1 to the recovery cell 4 (step S5). This allows the control unit 301 to separate and extract the vaporized volatile components.

[0112] Next, the analysis unit 302 determines whether the temperature inside the sealed container 1 is below temperature T3 (step S6).

[0113] If the temperature inside the sealed container 1 is below temperature T3 (step S6: affirmative), the analysis unit 302 changes the temperature threshold to the next threshold (step S7). For example, if the current temperature threshold is T1, the analysis unit 302 changes the temperature threshold to T2, and if the current temperature threshold is T2, it changes the temperature threshold to T3. After that, the separation process for specific volatile components returns to step S2.

[0114] Conversely, if the temperature inside the sealed container 1 is higher than temperature T3 (step S6: negative), the analysis unit 302 terminates the separation process for specific volatile components.

[0115] Figure 8 is a flowchart of the separation process of specific volatile components using a cooling process by the thermal pressure measuring device according to the first embodiment. Next, referring to Figure 8, the flow of the separation process of specific volatile components using a cooling process by the thermal pressure measuring device 100 according to this embodiment will be explained. Here, too, preliminary preparations such as vacuuming the measurement area of ​​the sealed container 1 and pressure gauge 5, adjusting the pressure gauge 5, injecting the sample into the sealed container 1, and sealing the sealed container 1 have already been completed. The control unit 301 controls the transfer pump 2, heater 11, cooler 13, and valves 21-29 in response to instructions from the analysis unit 302, but the instructions from the analysis unit 302 may be omitted here. Here, as an example, temperatures T1', T2', and T3' shown in Figure 2 will be explained as threshold temperatures. The analysis unit 302 has temperature T3' as the initial threshold temperature and changes the threshold temperature in the order of temperature T3', temperature T2', and temperature T1'.

[0116] The control unit 301 controls the heater 11 to heat the inside of the sealed container 1 and vaporize all the volatile components contained in the sample (step S11).

[0117] Next, the control unit 301 controls the cooler 13 to cool the inside of the sealed container 1 (step S12).

[0118] When the analysis unit 302 confirms from the measurement results of the cooling thermometer 14 that the temperature inside the sealed container 1 has reached the threshold temperature, it instructs the control unit 301 to maintain the temperature. Upon receiving the instruction from the analysis unit 302, the control unit 301 maintains the temperature inside the sealed container 1 at the threshold temperature (step S13).

[0119] Next, the analysis unit 302 confirms the completion of aggregation of volatile components that aggregate at the current threshold temperature (step S14).

[0120] When the condensation of volatile components that condense at the current threshold temperature is complete, the control unit 301 controls the transfer pump 2 and valves 21-29 to transfer the residual gas inside the sealed container 1 to the storage cell 3 (step S15).

[0121] Subsequently, the control unit 301 controls the heater 11 to heat the inside of the sealed container 1 and vaporize the condensed volatile components (step S16).

[0122] After all the aggregated volatile components have been vaporized, the control unit 301 controls the transfer pump 2 and valves 21-29 to transfer the vaporized volatile components inside the sealed container 1 to the recovery cell 4 (step S17). This allows the control unit 301 to separate and extract the aggregated volatile components.

[0123] Next, the analysis unit 302 determines whether the temperature inside the sealed container 1 is above or below temperature T1' (step S18).

[0124] If the temperature inside the sealed container 1 is above temperature T1' (step S18: affirmative), the control unit 301 controls the transfer pump 2 and valves 21-29 to transfer the residual gas from the storage cell 3 to the sealed container 1 (step S19).

[0125] Next, the analysis unit 302 changes the temperature threshold to the next threshold (step S20). For example, if the current temperature threshold is T3', the analysis unit 302 changes the temperature threshold to T2', and if the current temperature threshold is T2', it changes the temperature threshold to T1'. After that, the separation process for specific volatile components returns to step S12.

[0126] Conversely, if the temperature inside the sealed container 1 is lower than temperature T1' (step S18: negative), the analysis unit 302 terminates the separation process for specific volatile components.

[0127] In addition to the methods described above, there are other methods for separating specific volatile components. For example, the thermal pressure measuring device 100 can separate specific volatile components by maintaining a temperature for a certain period of time at a temperature where the pressure changes significantly.

[0128] (effect) As described above, the thermal pressure measuring device 100 according to this embodiment heats or cools the volatile components contained in the sample to cause a change of state, such as vaporization, liquefaction, or solidification, for each volatile component. The thermal pressure measuring device 100 then identifies the type of each volatile component based on the phase changes in temperature and pressure that occur when the change of state for each volatile component occurs. Furthermore, the thermal pressure measuring device 100 calculates the molar ratio of each volatile component and performs quantitative analysis based on the pressure at which the change of state for each volatile component is completed.

[0129] The thermal pressure measuring device 100 can determine the ratio of each volatile component by measuring thermal pressure. Furthermore, by calculating the total weight before and after measurement, the thermal pressure measuring device 100 can determine the quantitative value of a specific volatile component from the ratio of each volatile component, and can calculate the content of each volatile component relative to the total weight of all volatile components contained in the sample.

[0130] Furthermore, in the case of the thermal pressure measuring device 100, when measuring during the heating process, if the measurement starts from a low temperature, it is difficult to separate and extract volatile components, resulting in a slow sublimation rate, a long time required, and difficulty in determining the end point. In contrast, in the case of measuring during the cooling process, the thermal pressure measuring device 100 cools from a temperature at which all volatile components can vaporize, and separates and extracts the volatile components by liquefying or solidifying them through coagulation. In other words, by performing measurement during the cooling process, the thermal pressure measuring device 100 can easily perform thermal pressure measurement in a shorter time.

[0131] Furthermore, unlike fractional distillation performed under atmospheric pressure, the thermal pressure measuring device 100 cannot perform fractional distillation in a sealed container 1 as a continuous process, but it can efficiently measure thermal pressure by using multiple cells. Also, when condensation occurs inside the sealed container 1, pressure changes are significant below 10 kPa. Therefore, the thermal pressure measuring device 100 uses a high-resolution vibration-type absolute pressure sensor as the pressure gauge 5, enabling pressure measurement that is independent of the type of volatile component.

[0132] Furthermore, while thermal gravity measurement utilizes gravitational acceleration, the thermal pressure measuring device 100 does not use gravitational acceleration, thus enabling thermal pressure measurement independent of the magnitude of gravitational acceleration. The thermal pressure measuring device 100 also measures thermal pressure by measuring the pressure inside the sealed container 1. Since the pressure change is larger as the volume of the sealed container 1 decreases, the thermal pressure measuring device 100 is suitable for miniaturization. Also, because the pressure measurement is performed within the sealed container 1, the thermal pressure measuring device 100 does not require an inert gas such as N2 and is not affected by errors due to gas flow. Additionally, since the thermal pressure measuring device 100 analyzes volatile components inside the sealed container 1, thermal pressure measurement can be performed without using gases for dilution. Furthermore, the thermal pressure measuring device 100 has very few moving parts and a simple mechanism, resulting in improved robustness. Moreover, if the vapor pressure curve of the volatile components is known in advance, the thermal pressure measuring device 100 can identify multiple gases simply by measuring the temperature change in the pressure of the volatile components inside the sealed container 1. Furthermore, the thermal pressure measuring device 100 can separate and extract specific volatile components. Therefore, measurements can be performed using laser gas analyzers, Q-MASS (Quadrupole Mass Spectrometer), GCMS (Gas Chromatograph Mass Spectrometer), etc., with the separated and extracted volatile components. The thermal pressure measuring device 100 allows for even more detailed analysis by comparing the measurement results. Moreover, the thermal pressure measuring device 100 can be realized with a pressure gauge 5, a heater 11, a heating thermometer 12, a cooler 13, and a cooling thermometer 14, and does not require a complex mechanism, making it easy to combine with other measurement methods. As described above, the thermal pressure measuring device 100 can improve the efficiency of thermal analysis.

[0133] Furthermore, techniques that utilize phase changes due to heat and pressure include distillation and fractional distillation. These techniques take advantage of the difference in liquefaction temperatures of mixed gases caused by temperature changes under atmospheric pressure. When performing fractional distillation under atmospheric pressure, the target gas can be liquefied by cooling it to a temperature below its boiling point where liquefaction begins.

[0134] For example, let's explain distillation using petroleum refining as an example. Oil contains components with different liquefaction temperatures depending on the length of their carbon chains, and these are classified into naphtha, kerosene, diesel fuel, heavy diesel fuel, and heavy oil. Crude oil is heated to over 350°C in a furnace at the front of the distillation column and vaporized. Then, the vaporized crude oil is introduced into the distillation column, and as the gas cools, it is sequentially liquefied and separated and extracted. This process is carried out under atmospheric pressure, so the liquefaction temperature is below the boiling point. Therefore, if the boiling point of each component is known, separation is possible.

[0135] In contrast, the thermal pressure measuring device 100 according to this embodiment cools and condenses or heats and vaporizes volatile components inside the sealed container 1. Therefore, the technology that utilizes the phase change due to thermal pressure as described above presents the following problems. Firstly, the temperature at which the volatile components condense changes due to the pressure change of the volatile components caused by the temperature drop during cooling, making it difficult to use a fixed temperature such as the boiling point. Secondly, because a sealed container 1 is used, it is difficult to separate and extract the residual gas and condensed volatile components by methods such as distillation as described above. Furthermore, because a sealed container 1 is used, continuous processing such as in a distillation column is difficult when a large number of volatile components are present.

[0136] Due to the problems described above, for example, it is difficult to use a technique that utilizes phase change due to thermal pressure in the thermal pressure measurement performed by the thermal pressure measuring device 100 according to this embodiment. Therefore, the thermal pressure measuring device 100 according to this embodiment makes it possible to improve the efficiency of thermal analysis by using the thermal pressure measurement method described in this embodiment.

[0137] (Second Embodiment) Figure 9 is a block diagram of a thermal pressure measuring device according to the second embodiment. In this embodiment, the thermal pressure measuring device 100 transfers the vaporized volatile components to another sealed container 50 and condenses the volatile components in the sealed container 50. In the following description, the operation of each part, which is the same as in the first embodiment, may be omitted. Here, as an example, the case in which volatile components are separated using a cooling process will be described.

[0138] The thermal pressure measuring device 100 includes a sealed container 1, a transfer pump 2, a storage cell 3, a recovery cell 4, a pressure gauge 5, a heater 11, a heating thermometer 12, a cooler 13, a cooling thermometer 14, valves 21-25, 27 and 28, and an analysis control device 300. Furthermore, the thermal pressure measuring device 100 includes valves 31 and 32, a sealed container 50, and a pressure gauge 60.

[0139] The sealed container 50 includes a heater 501, a heating thermometer 502, a cooler 503, and a cooling thermometer 504. The sealed container 50 is a container that can be sealed.

[0140] The sealed container 50 has a first opening connected to a pipe branching off from the pipe connecting the valve 23 and the recovery cell 4. The sealed container 50 also has a second opening, from which a pipe extends, connected to a bypass pipe. Here, the opening of the sealed container 50 connected to the pipe branching off from the pipe connecting the transfer pump 2 and the recovery cell 4 is referred to as the first opening of the sealed container 50. The opening of the sealed container 50 connected to the bypass pipe is referred to as the second opening of the sealed container 50.

[0141] Valve 31 is provided at the first opening of the sealed container 50. Valve 31 opens and closes the first opening of the sealed container 50. Valve 32 is provided at the second opening of the sealed container 50. Valve 32 opens and closes the second opening of the sealed container 50.

[0142] The heater 501 heats part or all of the sealed container 50. The cooler 503 cools part or all of the sealed container 50. The heater 501 and cooler 503 can adjust the internal temperature of the sealed container 50, for example, within a range of 300K to 40K. The heating thermometer 502 measures the temperature of the sealed container 50 when it is heated by the heater 501. The cooling thermometer 504 measures the temperature of the sealed container 50 when it is cooled by the cooler 503.

[0143] The pressure gauge 60 is an absolute pressure gauge. The pressure gauge 60 measures the pressure inside the sealed container 50.

[0144] The control unit 301 of the analysis control device 300 performs the following volatile component separation process. The control unit 301 controls the heater 11 to heat the sealed container 1 and vaporize all the volatile components contained in the sample. The control unit 301 controls the transfer pump 2, valves 21-25, 27, 28, 31 and 32 to transfer the vaporized volatile components from the sealed container 1 to the sealed container 50.

[0145] Next, the control unit 301 controls the cooler 503 to cool the inside of the sealed container 50, causing some of the volatile components to condense and either liquefy or solidify. When the volatile components condense and the pressure inside the sealed container 50 changes significantly, the control unit 301 maintains the temperature inside the sealed container 50 at that time, in accordance with the temperature maintenance instruction from the analysis unit 302.

[0146] Subsequently, the control unit 301 controls the transfer pump 2, valves 21-25, 27, 28, 31, and 32 to transfer the residual gas from the sealed container 50 to the storage cell 3. This allows the control unit 301 to separate the volatile components that have condensed inside the sealed container 50.

[0147] Next, the control unit 301 closes the valve 31 to seal the sealed container 50 and controls the heater 501 to vaporize the condensed volatile components inside the sealed container 50. Subsequently, the control unit 301 controls the transfer pump 2, valves 21-25, 27, 28, 31 and 32 to transfer the vaporized volatile components inside the sealed container 50 to the recovery cell 4.

[0148] Furthermore, if residual gas is stored in the storage cell 3, the control unit 301 controls the transfer pump 2, valves 21-25, 27, 28, 31 and 32 to transfer the residual gas stored in the storage cell 3 to the sealed container 50. Subsequently, the control unit 301 repeats the process of coagulation and separation of volatile components in the sealed container 50 described above until there is no residual gas left in the storage cell 3. In this case, the recovery cell 4 is replaced each time volatile components are recovered from the sealed container 50. At this point, the control unit 301 may control the transfer pump 2, valves 21-25, 27, 28, 31 and 32 to discharge the residual gas stored in the storage cell 3 to the external outlet 30, thereby ending the process of separating volatile components.

[0149] The analysis unit 302 acquires measurement results from the pressure gauge 5, heating thermometer 12, cooling thermometer 14, heating thermometer 502 and cooling thermometer 504, and pressure gauge 60. The analysis unit 302 notifies the control unit 301 of the measurement results from the pressure gauge 5, heating thermometer 12, cooling thermometer 14, heating thermometer 502 and cooling thermometer 504, and pressure gauge 60. The analysis unit 302 can also instruct the control unit 301 to heat or cool the inside of the sealed container 1. Furthermore, the analysis unit 302 can instruct the control unit 301 to control the transfer pump 2 and valves 21-25, 27, 28, 31 and 32.

[0150] The above explanation used the cooling process as an example, but in the case of the heating process, for example, the thermal pressure measuring device 100 can raise the temperature inside the sealed container 1 and transfer the volatile components to the recovery cell 4 in the order in which they vaporize, thereby sequentially separating the volatile components after vaporization.

[0151] Furthermore, in this embodiment, the thermal pressure measuring device 100 separates the volatile components by transferring the vaporized volatile components between the sealed container 50 and the storage cell 3, but it is not limited to this. For example, the thermal pressure measuring device 100 may separate the volatile components by transferring the vaporized volatile components between the sealed container 1 and the sealed container 50.

[0152] Here, sealed container 1 is an example of a "first sealed container." Also, sealed container 50 is an example of a "second sealed container." The analysis unit 302, implemented by the processor, uses a transfer pump 2, which is a transfer device, to transfer the volatile components stored in the first sealed container to the second sealed container and perform separation of the volatile components.

[0153] (effect) As described above, the thermal pressure measuring device 100 according to this embodiment performs thermal pressure measurement using two sealed containers 1 and 50 that can be heated and cooled. This makes it possible to measure the thermal pressure of volatile components in the sample while removing all components other than volatile components, thereby enabling more accurate thermal pressure measurement.

[0154] (Third embodiment) Figure 10 is a block diagram of a thermal pressure measuring device according to the third embodiment. In this embodiment, the thermal pressure measuring device 100 uses a plurality of sealed containers 51 to 53 that can be heated and cooled in addition to the sealed container 1 to perform thermal pressure measurement. In this embodiment, the case of three sealed containers 51 to 53 will be described, but the number of sealed containers 51 to 53 may be two or four or more. In the following description, the operation of each part, as in the first embodiment, may be omitted. Here, as an example, the case in which volatile components are separated using a cooling process will be described.

[0155] The thermal pressure measuring device 100 includes a sealed container 1, a transfer pump 2, a recovery cell 4, a pressure gauge 5, a heater 11, a heating thermometer 12, a cooler 13, a cooling thermometer 14, valves 21-23, 25 and 27, and an analysis control device 300. Furthermore, the thermal pressure measuring device 100 includes valves 41-46, sealed containers 51-53 and pressure gauges 61-63.

[0156] Sealed container 51 includes a heater 511, a heating thermometer 512, a cooler 513, and a cooling thermometer 514. Sealed container 52 includes a heater 521, a heating thermometer 522, a cooler 523, and a cooling thermometer 524. Sealed container 53 includes a heater 531, a heating thermometer 532, a cooler 533, and a cooling thermometer 534. Sealed containers 51 to 53 are airtight containers.

[0157] The sealed containers 51-53 have their first openings connected to pipes branching off from the pipe connecting valve 23 and recovery cell 4. Additionally, the pipes extending from the second openings of the sealed containers 51-53 are connected to the pipe connecting valve 22 and valve 25. Here, for each of the sealed containers 51-53, the opening connected to the pipe branching off from the pipe connecting transfer pump 2 and recovery cell 4 is referred to as the first opening. Furthermore, the openings on the side of the sealed containers 51-53 that connect to the bypass pipe are referred to as the second openings.

[0158] Valve 41 is provided at the first opening of the sealed container 51. Valve 41 opens and closes the first opening of the sealed container 51. Valve 44 is provided at the second opening of the sealed container 51. Valve 44 opens and closes the second opening of the sealed container 51. Valve 42 is provided at the first opening of the sealed container 52. Valve 42 opens and closes the first opening of the sealed container 52. Valve 45 is provided at the second opening of the sealed container 52. Valve 45 opens and closes the second opening of the sealed container 52. Valve 43 is provided at the first opening of the sealed container 53. Valve 43 opens and closes the first opening of the sealed container 53. Valve 46 is provided at the second opening of the sealed container 53. Valve 46 opens and closes the second opening of the sealed container 53.

[0159] The heater 511 heats part or all of the sealed container 51. The cooler 513 cools part or all of the sealed container 51. The heater 511 and cooler 513 can adjust the temperature of the sealed container 51, for example, within a range of 300K to 40K. The heating thermometer 512 measures the temperature of the sealed container 51 when it is heated by the heater 511. The cooling thermometer 514 measures the temperature of the sealed container 51 when it is cooled by the cooler 513.

[0160] The heater 521 heats part or all of the sealed container 52. The cooler 523 cools part or all of the sealed container 52. The heater 521 and cooler 523 can adjust the temperature of the sealed container 52 within a range of, for example, 300K to 40K. The heating thermometer 522 measures the temperature of the sealed container 52 when it is heated by the heater 521. The cooling thermometer 524 measures the temperature of the sealed container 52 when it is cooled by the cooler 523.

[0161] The heater 531 heats part or all of the sealed container 53. The cooler 533 cools part or all of the sealed container 53. The heater 531 and cooler 533 can adjust the temperature of the sealed container 51 within a range of, for example, 300K to 40K. The heating thermometer 532 measures the temperature of the sealed container 53 when it is heated by the heater 531. The cooling thermometer 534 measures the temperature of the sealed container 53 when it is cooled by the cooler 533.

[0162] Pressure gauges 61-63 are absolute pressure gauges. Pressure gauge 61 measures the pressure inside sealed container 51. Pressure gauge 62 measures the pressure inside sealed container 52. Pressure gauge 63 measures the pressure inside sealed container 53.

[0163] The control unit 301 of the analysis control device 300 performs the following volatile component separation process. The control unit 301 controls the heater 11 to heat the sealed container 1 and vaporize all the volatile components contained in the sample. Next, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27 and 41-46 to transfer the vaporized volatile components from the sealed container 1 to the sealed container 51.

[0164] Next, the control unit 301 controls the cooler 513 to cool the inside of the sealed container 51, causing some of the volatile components to condense and liquefy or solidify. When the pressure inside the sealed container 51 changes significantly due to the condensation and liquefaction or solidification of the volatile components, the control unit 301, upon receiving instructions from the analysis unit 302, maintains the temperature inside the sealed container 51 at that time.

[0165] Subsequently, once the condensation of volatile components at that temperature is complete, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27, and 41-46 to transfer the residual gas from the sealed container 51 to the sealed container 52. This allows the control unit 301 to separate the volatile components that have condensed inside the sealed container 51.

[0166] Next, the control unit 301 closes the valve 41 to seal the sealed container 51 and controls the heater 511 to vaporize the condensed volatile components inside the sealed container 51. After that, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27 and 41-46 to transfer the vaporized volatile components inside the sealed container 51 to the recovery cell 4.

[0167] In parallel with the processing of the condensed volatile components inside the sealed container 51, the control unit 301 controls the cooler 523 to cool the inside of the sealed container 52, causing some of the volatile components to condense and liquefy or solidify. When the volatile components condense and the pressure inside the sealed container 52 changes significantly, the control unit 301 maintains the temperature inside the sealed container 52 at that time, in accordance with the temperature maintenance instruction from the analysis unit 302.

[0168] Subsequently, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27, and 41-46 to transfer the residual gas from the sealed container 52 to the sealed container 53. This allows the control unit 301 to separate the volatile components that have condensed inside the sealed container 52.

[0169] Next, the control unit 301 closes the valve 42 to seal the sealed container 52 and controls the heater 521 to vaporize the condensed volatile components inside the sealed container 52. After that, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27 and 41-46 to transfer the vaporized volatile components inside the sealed container 52 to the recovery cell 4.

[0170] In parallel with the processing of the condensed volatile components inside the sealed container 52, the control unit 301 controls the cooler 533 to cool the inside of the sealed container 53, causing some of the volatile components to condense and liquefy or solidify. When the volatile components condense and the pressure inside the sealed container 53 changes significantly, the control unit 301 maintains the temperature inside the sealed container 53 at that time, in accordance with the temperature maintenance instruction from the analysis unit 302.

[0171] Subsequently, the control unit 301 controls the transfer pump 2, valves 21-23, 25, 27, and 41-46 to transfer the residual gas from the sealed container 53 to another empty sealed container 51 or 52. This allows the control unit 301 to separate the volatile components that have condensed inside the sealed container 53.

[0172] The control unit 301 repeatedly separates the volatile components using the sealed containers 51-53 until no volatile components remain after aggregation. When no volatile components remain after aggregation, the control unit 301 vaporizes the aggregated volatile components and transfers them to the recovery cell 4, thereby ending the separation of the volatile components. However, if the separation of volatile components is terminated midway, the control unit 301 transfers the vaporized volatile components at the time of termination to the external discharge port 30 for discharge.

[0173] The analysis unit 302 acquires measurement results from pressure gauges 5 and 61-63, heating thermometers 12, 512, 522, and 532, and cooling thermometers 14, 514, 524, and 534. The analysis unit 302 notifies the control unit 301 of the measurement results acquired from pressure gauges 5 and 61-63, heating thermometers 12, 512, 522, and 532, and cooling thermometers 14, 514, 524, and 534. The analysis unit 302 can also instruct the control unit 301 to heat or cool the inside of the sealed container 1. Furthermore, the analysis unit 302 can instruct the control unit 301 to control the transfer pump 2, valves 21-23, 25, 27, and 41-46.

[0174] The above explanation used the cooling process as an example, but in the case of the heating process, for example, the thermal pressure measuring device 100 can raise the temperature inside the sealed container 1 and transfer the volatile components to the recovery cell 4 in the order in which they vaporize, thereby sequentially separating the volatile components after vaporization.

[0175] Here, the sealed containers 51-53 are examples of "three or more sealed containers." The analysis unit 302, implemented by the processor, uses the transfer pump 2, which is a transfer device, to transfer the volatile components between each of the three or more sealed containers 51-53, thereby performing the separation of the volatile components.

[0176] (effect) As described above, the thermal pressure measuring device 100 according to this embodiment uses a plurality of sealed containers 51 to 53 in addition to two sealed containers 1 that can be heated and cooled to perform thermal pressure measurements. As a result, the thermal pressure measuring device 100 can perform the processing of some vaporized volatile components, the processing of residual gas transfer, and the processing of heating and recovery of condensed volatile components in parallel, thereby further improving the efficiency of thermal analysis with a simple structure.

[0177] (system) Unless otherwise specified, the processing procedures, control procedures, specific names, and various data and parameters shown in the above documents and drawings may be changed at will.

[0178] Furthermore, the components of each illustrated device are functionally conceptual and do not necessarily need to be physically configured as shown. In other words, the specific forms of distribution and integration of each device are not limited to those shown. That is, all or part of them can be functionally or physically distributed and integrated in any unit according to various loads and usage conditions.

[0179] Furthermore, each processing function performed by each device may be implemented, in whole or in part, by a CPU (Central Processing Unit) and a program executed by that CPU, or by wired logic hardware.

[0180] (Hardware) Next, an example of the hardware configuration of the analysis control device 300 will be described. Figure 11 is a hardware configuration diagram of the analysis control device. As shown in Figure 11, the analysis control device 300 has a processor 91, memory 92, hard disk 93, and network interface 94. The processor 91 is connected to the memory 92, hard disk 93, and network interface 94 via a bus.

[0181] The network interface 94 is used for communication between the analysis control device 300 and other information processing devices.

[0182] The hard disk 93 is an auxiliary storage device. The hard disk 93 stores various programs, including programs for realizing the functions of the control unit 301 and the analysis unit 302.

[0183] The processor 91 reads various programs stored in the hard disk 93, loads them into the memory 92, and executes them. In this way, the processor 91 realizes the functions of the control unit 301 and the analysis unit 302.

[0184] Thus, the analysis control device 300 operates as an information processing device that executes various processing methods by reading and executing a program. Furthermore, the analysis control device 300 can also achieve the same functions as the embodiment described above by reading the program from the recording medium using a media reader and executing the read program. Note that the program referred to here is not limited to being executed by the analysis control device 300. For example, the present invention can be similarly applied when another computer or server executes the program, or when they cooperate to execute the program.

[0185] This program can be distributed via networks such as the Internet. Furthermore, this program can be recorded on computer-readable storage media such as hard disks, flexible disks (FDs), CD-ROMs, MO (Magneto-Optical disks), and DVDs (Digital Versatile Discs), and executed by reading the program from these media using a computer.

[0186] Some examples of the combinations of technical features that will be disclosed are listed below.

[0187] (1) At least one airtight container, A heater that heats the container to vaporize the volatile components, or a cooler that cools the container to condense the volatile components, or both of these, A thermometer for measuring the temperature of the container, The aforementioned container includes an exhaust section for creating a vacuum, A pressure gauge for measuring the pressure inside the container, Memory and A processor connected to the aforementioned memory, Equipped with, The processor performs identification of the volatile components based on changes in temperature and pressure inside the container storing the volatile components. Thermal pressure measuring device. (2) The thermal pressure measuring device according to (1), wherein the processor performs quantitative determination of volatile components present in the container based on changes in the temperature and pressure inside the container. (3) The thermal pressure measuring device according to (1) or (2), further comprising a transfer device for transferring the vaporized volatile components inside the container to another container. (4) The transfer device is a vacuum pump, The processor uses the vacuum pump to transfer the volatile components stored in the container to another container, thereby performing the separation of the volatile components. (3) The thermal pressure measuring device described above. (5) The container is a single sealed container, The processor uses the transfer device to transfer the volatile components stored in the sealed container to a detachable predetermined container, thereby performing the separation of the volatile components. (3) or (4) The thermal pressure measuring device described above. (6) The aforementioned containers are a first sealed container and a second sealed container, The processor uses the transfer device to transfer the volatile components stored in the first sealed container to the second sealed container, thereby performing the separation of the volatile components. (3) or (4) The thermal pressure measuring device described above. (7) The containers are three or more airtight containers, The processor uses the transfer device to transfer the volatile components between each of the three or more sealed containers to perform the separation of the volatile components. (3) or (4) The thermal pressure measuring device described above. (8) The thermal pressure measuring device according to any one of (1) to (7), wherein the thermometer includes either or both a heating thermometer for measuring the temperature of the container when it is heated by the heater or a cooling thermometer for measuring the temperature of the container when it is cooled by the cooler, depending on the installation of the heater or the cooler. (9) The heater is an optical heating device, a resistance heating device, or a Peltier element. The aforementioned heating thermometer is an optical thermometer. (8) The thermal pressure measuring device described above. (10) The cooler is a cooling device using liquid nitrogen, liquid oxygen, and liquid helium, a GM refrigerator, or a Peltier element. The cooling thermometer is a silicon diode or a platinum resistance thermometer. (8) and (9) The thermal pressure measuring device described above. (11) The pressure gauge is a high-resolution vibrating absolute pressure sensor, as described in any one of (1) to (10) of the thermal pressure measuring device. (12) The thermal pressure measuring device according to any one of (1) to (11), wherein the processor compares data on changes in temperature and pressure inside the container with the vapor pressure curve of the substance to identify the volatile components. (13) The exhaust section removes residual gas from inside the container by creating a vacuum in the container, as described in any one of (1) to (12). (14) At least one airtight container, A heater that heats the container to vaporize the volatile components, or a cooler that cools the container to condense the volatile components, or both of these, A thermometer for measuring the temperature of the container, The aforementioned container includes an exhaust section for creating a vacuum, A thermal pressure measurement method using a thermal pressure measuring device equipped with a pressure gauge for measuring the pressure inside the container, The aforementioned thermal pressure measuring device Based on the changes in temperature and pressure inside the container containing the volatile components, the volatile components are identified. Method for measuring thermal pressure. [Explanation of Symbols]

[0188] 1.50~53 Airtight container 2. Transfer pump 3 Storage Cells 4 Recovery Cells 5, 60~63 Pressure gauge 11,501,511,521,531 Heater 12,502,512,522,532 Heating thermometer 13,503,513,523,533 Cooler 14,504,514,524,534 Cooling thermometer 21-29, 31-32 valves 100 Thermal pressure measuring device 300 Analysis Control Device 301 Control Unit 302 Analysis Department

Claims

1. At least one airtight container, A heater that heats the container to vaporize the volatile components, or a cooler that cools the container to condense the volatile components, or both of these, A thermometer for measuring the temperature of the container, The aforementioned container includes an exhaust section for creating a vacuum, A pressure gauge for measuring the pressure inside the container, Memory and A processor connected to the aforementioned memory, Equipped with, The processor performs identification of the volatile components based on changes in temperature and pressure inside the container storing the volatile components. Thermal pressure measuring device.

2. The thermal pressure measuring device according to claim 1, wherein the processor performs quantitative analysis of volatile components present in the container based on changes in the temperature and pressure inside the container.

3. The thermal pressure measuring device according to claim 1, further comprising a transfer device for transferring the vaporized volatile components inside the container to another container.

4. The transfer device is a vacuum pump, The processor uses the vacuum pump to transfer the volatile components stored in the container to another container, thereby performing the separation of the volatile components. The thermal pressure measuring device according to claim 3.

5. The container is a single sealed container, The processor uses the transfer device to transfer the volatile components stored in the sealed container to a detachable predetermined container, thereby performing the separation of the volatile components. The thermal pressure measuring device according to claim 3.

6. The aforementioned containers are a first sealed container and a second sealed container, The processor uses the transfer device to transfer the volatile components stored in the first sealed container to the second sealed container, thereby performing the separation of the volatile components. The thermal pressure measuring device according to claim 3.

7. The containers are three or more airtight containers, The processor uses the transfer device to transfer the volatile components between each of the three or more sealed containers to perform the separation of the volatile components. The thermal pressure measuring device according to claim 3.

8. The thermal pressure measuring device according to claim 1, wherein the thermometer includes either a heating thermometer for measuring the temperature of the container when it is heated by the heater, or a cooling thermometer for measuring the temperature of the container when it is cooled by the cooler, depending on the installation of the heater or the cooler.

9. The heater is an optical heating device, a resistance heating device, or a Peltier element. The aforementioned heating thermometer is an optical thermometer. The thermal pressure measuring device according to claim 8.

10. The cooler is a cooling device using liquid nitrogen, liquid oxygen, and liquid helium, a GM refrigerator, or a Peltier element. The cooling thermometer is a silicon diode or a platinum resistance thermometer. The thermal pressure measuring device according to claim 8.

11. The thermal pressure measuring device according to claim 1, wherein the pressure gauge is a high-resolution vibrating absolute pressure sensor.

12. The thermal pressure measuring device according to claim 1, wherein the processor compares data on changes in temperature and pressure inside the container with a vapor pressure curve of the substance to identify the volatile components.

13. The thermal pressure measuring device according to claim 1, wherein the exhaust unit removes residual gas from inside the container by creating a vacuum in the container.

14. At least one airtight container, A heater that heats the container to vaporize the volatile components, or a cooler that cools the container to condense the volatile components, or both of these, A thermometer for measuring the temperature of the container, The aforementioned container includes an exhaust section for creating a vacuum, A thermal pressure measurement method using a thermal pressure measuring device equipped with a pressure gauge for measuring the pressure inside the container, The aforementioned thermal pressure measuring device Based on the changes in temperature and pressure inside the container containing the volatile components, the volatile components are identified. Method for measuring thermal pressure.

Citation Information

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