Program, information processing method, and thermal analysis device

Abstract

[Problem] To provide a program or the like that enables accurate determination of specific heat in a temperature-modulated DSC. [Solution] According to one aspect of the present invention, provided is a program for causing a computer to execute the following steps: an acquisition step for acquiring a temperature change of a sample measured by a heating test in which the heating temperature of the sample is increased while being periodically changed, an initial weight of the sample during the heating test, and a representative value of weight change amounts of the sample during the heating test; a specific heat calculation step for calculating the specific heat of the sample by formula (1), wherein cp is the specific heat, Cp is the heat capacity of the sample calculated from the temperature change, W0 is the initial weight, and TG is the representative value. (1): cp = Cp / (W0 + TG)

Description

Program, information processing method, and thermal analysis apparatus

[0001] This invention relates to a program, an information processing method, and a thermal analysis apparatus.

[0002] Patent Document 1 discloses a method for determining the heat capacity of a sample by temperature-modulated DSC (differential scanning calorimetry) in which the heating temperature is periodically changed and increased.

[0003] Patent No. 2909950

[0004] The specific heat of a substance can be determined by dividing its heat capacity by its weight. However, in the aforementioned heating test, the temperature of the sample also changes unpredictably in accordance with temperature modulation. Therefore, for example, dividing the heat capacity obtained in the heating test by the initial weight of the sample does not yield an accurate specific heat.

[0005] In view of the above circumstances, the present invention provides a program, etc., that can accurately determine specific heat in a temperature-modulated DSC.

[0006] According to one aspect of the present invention, a program causes a computer to perform the following steps: In the acquisition step, the program acquires the temperature change of a sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test; In the specific heat calculation step, the program calculates the specific heat of the sample using the following formula (1), where c ｐ This is the specific heat, C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ The program provides the initial weight and TG as a representative value. ｐ = C ｐ / (W ０ +TG) ... (1)

[0007] With this configuration, the specific heat is calculated using the heat capacity obtained based on the temperature change measured during the heating test, and the weight change of the test, also measured during the heating test. Therefore, the specific heat can be determined with high accuracy in a temperature-modulated DSC.

[0008] This is a schematic diagram of the thermal analysis apparatus 10 according to this embodiment. This is a schematic diagram of the weight measurement mechanism of the detection unit 4. This is a schematic diagram of the temperature difference measurement mechanism (heat flow measurement mechanism) of the detection unit 4. This is a diagram showing the hardware configuration of the control device 6. This is a block diagram showing the functions realized by the control device 6 (processor 63). This is a graph showing an example of heating temperature control of the heating furnace 2. This is a flowchart showing an example of specific heat calculation processing by the control device 6 (processor 63).

[0009] Embodiments of the present invention will be described below with reference to the drawings. The various features shown in the embodiments below can be combined with each other.

[0010] Incidentally, the program for realizing the software appearing in one embodiment may be provided as a computer-readable non-transitor-readable medium, or it may be provided so that it can be downloaded from an external server, or it may be provided so that the program is launched on an external computer and its functions are realized on a client terminal (so-called cloud computing).

[0011] Furthermore, in various information processing according to one embodiment, an input and an output corresponding to the input can be realized. Here, as long as an output is obtained as a result of the input, the form of the information referenced in such information processing (hereinafter referred to as "reference information") is not limited. The reference information may be, for example, rule-based information such as a database, a lookup table, or a predetermined function (including a decision formula such as a regression equation constructed by a statistical method), or a pre-trained model that has learned the correlation between input and output in advance, or a generative AI such as a large-scale language model or visual language model that can output a desired result by inputting a prompt.

[0012] Furthermore, in one embodiment, "part" may include, for example, hardware resources implemented by a circuit in a broad sense, and the information processing of software that can be specifically realized by these hardware resources. Also, in one embodiment, various types of information are handled, and this information can be represented, for example, by the physical values ​​of signal values ​​representing voltage and current, the high or low values ​​of signal values ​​as a set of binary bits composed of 0s or 1s, or by quantum superposition (so-called qubits), and communication and calculations can be performed on a circuit in a broad sense.

[0013] Furthermore, a circuit in a broad sense is a circuit realized by combining at least an appropriate combination of circuits, circuits, processors, and memory. The processor may be a general-purpose processor or a dedicated circuit. In other words, this includes application-specific integrated circuits (ASICs), programmable logic devices (for example, simple programmable logic devices (SPLDs), complex programmable logic devices (CPLDs), and field programmable gate arrays (FPGAs)), etc.

[0014] <Thermal analyzer 10> Figure 1 is a schematic diagram of the thermal analyzer 10 according to this embodiment. The thermal analyzer 10 is a device that measures the thermal behavior of a sample when the sample is heated (for example, thermogravimetric analysis (TG), differential scanning calorimetry (DSC), simultaneous thermogravimetric and differential scanning calorimetry analysis (TG-DSC), etc.). The thermal analyzer 10 comprises a measuring device 1 and a control device 6 (an example of an information processing device).

[0015] The measuring device 1 is configured to heat the sample and measure the weight and temperature (heat flow) of the sample. Specifically, the measuring device 1 includes a heating furnace 2, a first sample holder 3A, a second sample holder 3B, and a detection unit 4.

[0016] <Furnace 2> Furnace 2 is configured to simultaneously heat the sample to be analyzed for thermal analysis (the object to be measured) (hereinafter referred to as the "sample to be measured") and a standard sample whose thermal behavior (change in state due to temperature change) is known. Furnace 2 is, for example, a resistance-type heating furnace equipped with a protective tube and a heater.

[0017] The protective tube is a cylindrical tube with an internal space for housing the sample to be measured and the standard sample. In the thermal analyzer 10 shown in Figure 1, the protective tube is positioned with its central axis aligned horizontally. The heater is a cylindrical member configured to heat the inside of the protective tube. Specifically, the heater is configured to heat the protective tube by passing current through a heating element located on the outside of the protective tube. The heating furnace 2 may be an electric furnace other than a resistance heating furnace, an infrared heating furnace, or the like.

[0018] <First sample holder 3A and second sample holder 3B> The first sample holder 3A is configured to hold a container containing the sample to be measured. The second sample holder 3B is configured to hold a container containing a standard sample. The first sample holder 3A and the second sample holder 3B are each located inside the heating furnace 2.

[0019] The first sample holder 3A is held in the heating furnace 2 by the first balance beam 41A of the detection unit 4, which will be described later, and the second sample holder 3B is held in the heating furnace 2 by the second balance beam 41B of the detection unit 4.

[0020] <Detection Unit 4> The detection unit 4 shown in Figure 1 is configured to detect the thermal behavior of the sample being heated in the heating furnace 2. Specifically, the detection unit 4 is configured to detect at least one of the following: the weight of the sample to be measured and the standard sample, and the temperature difference between the sample to be measured and the standard sample (heat flow rate between the sample to be measured and the standard sample).

[0021] For example, when the thermal analyzer 10 is used for TG, the detection unit 4 detects the weight of each of the measurement target sample and the standard sample (that is, the weight difference between the measurement target sample and the standard sample). Further, for example, when the thermal analyzer 10 is used for DSC, the detection unit 4 detects the temperature difference between the measurement target sample and the standard sample. Furthermore, for example, when the thermal analyzer 10 is used for TG-DSC, the detection unit 4 detects both the weight of each of the measurement target sample and the standard sample, and the temperature difference between the measurement target sample and the standard sample.

[0022] The detection unit 4 includes a first balance beam 41A, a second balance beam 41B, a weight detection device 42, a first thermocouple 43A, a second thermocouple 43B, and a temperature detection device 44. According to such a configuration, it is possible to construct the thermal analyzer 10 that can easily and reliably improve the accuracy of thermal analysis data related to weight and temperature difference.

[0023] Figure 2 is a schematic diagram of a weight measurement mechanism included in the detection unit 4. The first balance beam 41A supports the first sample holder 3A and constitutes a balance mechanism for detecting the weight of the measurement target sample held by the first sample holder 3A. Specifically, the first sample holder 3A is attached to one end of the first balance beam 41A. Further, the other end of the first balance beam 41A is disposed inside the weight detection device 42. Furthermore, the first balance beam 41A is supported by a fulcrum 411 so as to be swingable in the vertical direction about the fulcrum 411.

[0024] Although illustration is omitted, the second balance beam 41B has the same configuration as the first balance beam 41A. That is, the second balance beam 41B supports the second sample holder 3B and constitutes a balance mechanism for detecting the weight of the standard sample held by the second sample holder 3B. Specifically, the second sample holder 3B is attached to one end of the second balance beam 41B. Further, the other end of the second balance beam 41B is disposed inside the weight detection device 42. Furthermore, the second balance beam 41B is supported by a fulcrum 411 so as to be swingable in the vertical direction about the fulcrum 411.

[0025] The weight detection device 42 is a device configured to detect the respective weights of a measurement target sample and a standard sample. The weight detection device 42 detects the weight of the measurement target sample from the inclination of the first balance beam 41A, and detects the weight of the standard sample from the inclination of the second balance beam 41B.

[0026] Specifically, the weight detection device 42 has an optical sensor that detects the position (deflection amount) of the respective end portions (for example, a shutter 412 attached to the end portion) of the first balance beam 41A and the second balance beam 41B. The optical sensor includes, for example, a light source 421 and a light receiving element 422 arranged to sandwich the balance beam in the horizontal direction. The optical sensor detects the position of the end portion of the balance beam based on a change in the amount of light emitted from the light source 421 received by the light receiving element 422. The light receiving element 422 includes, for example, a first element arranged above a reference position and a second element arranged below the reference position.

[0027] The weight detection device 42 converts the amount of light received by the light receiving element 422 into the weight of the measurement target sample or the standard sample, for example, according to the following procedure. That is, the weight detection device 42 uses a PID control circuit 423 to supply current to a drive coil 424 connected to the balance beam to swing the balance beam such that the output difference between the first element and the second element of the light receiving element 422 becomes zero (in other words, such that the end portion of the balance beam is at an initial position (horizontal state)). Subsequently, the weight detection device 42 uses an arithmetic circuit 425 to calculate the amount of weight change of the measurement target sample or the standard sample from the current value supplied to the drive coil 424 for making the output difference between the first element and the second element of the light receiving element 422 zero. Note that the relationship between the current value and the amount of weight change is obtained in advance.

[0028] FIG. 3 is a schematic diagram of a temperature difference measurement mechanism (heat flow measurement mechanism) included in the detection unit 4. The first thermocouple 43A is a pair of metal wires of different types connected to the first sample holder 3A. The second thermocouple 43B is a pair of metal wires of different types connected to the second sample holder 3B. The first thermocouple 43A and the second thermocouple 43B are each electrically connected to a power compensation circuit 444 of a temperature detection device 44 described later.

[0029] The first thermocouple 43A is held by the first balance beam 41A (see Figure 1). Specifically, the first thermocouple 43A is inserted into the interior of the first balance beam 41A. The second thermocouple 43B is held by the second balance beam 41B. Specifically, the second thermocouple 43B is inserted into the interior of the second balance beam 41B.

[0030] The temperature detection device 44 is configured to detect the heat flow generated in the sample being measured by energy compensation. The temperature detection device 44 in Figure 4A includes a first compensation heater 443A, a second compensation heater 443B, and a power compensation circuit 444.

[0031] The first compensation heater 443A and the second compensation heater 443B are configured to heat the sample under measurement and the standard sample separately, respectively. The power compensation circuit 444 adjusts the amount of power supplied to the first compensation heater 443A and the second compensation heater 443B so that there is no difference between the temperature of the sample under measurement obtained by the first thermocouple 43A and the temperature of the standard sample obtained by the second thermocouple 43B. Based on the difference between the amount of power supplied to the first compensation heater 443A and the amount of power supplied to the second compensation heater 443B, the power compensation circuit 444 outputs the heat flow rate in the sample under measurement.

[0032] The temperature detection device 44 in Figure 4B is configured to detect the heat flow generated in a sample to be measured by the heat flux. The temperature detection device 44 in Figure 4B includes a heat-sensitive plate 445 and a heat quantity correction circuit 446.

[0033] The heat-sensing plate 445 is a component that integrates the first sample holder 3A and the second sample holder 3B. The heat quantity correction circuit 446 outputs the heat flow rate in the sample to be measured based on the difference in electromotive force between the first thermocouple 43A and the second thermocouple 43B, which are connected to the heat-sensing plate 445, respectively.

[0034] Such a temperature detection device 44 using heat flux is applied to a detection unit 4 configured such that a first sample holder 3A and a second sample holder 3B are supported by a single balance beam. In this configuration, errors occur in the weight of the detected sample due to the expansion of the balance beam caused by room temperature fluctuations, heating and cooling, etc. However, by performing a blank measurement of the holder in an empty state before measurement and subtracting that data, for example, the expansion error due to heating and cooling can be minimized.

[0035] <Control device 6> The control device 6 is configured to control the heating temperature of the heating furnace 2, acquire the detection results of the detection unit 4, and so on. In particular, the control device 6 is configured to calculate the measurement results of the measuring device 1 (detection unit 4).

[0036] Figure 4 shows the hardware configuration of the control device 6. The control device 6 comprises a communication bus 60, a communication unit 61, a storage unit 62, a processor 63, a display unit 64, and an input unit 65. The communication unit 61, storage unit 62, processor 63, display unit 64, and input unit 65 are electrically connected within the control device 6 via the communication bus 60.

[0037] <Communication Unit 61> The communication unit 61 preferably uses wired communication methods such as USB, IEEE 1394, Thunderbolt®, and wired LAN network communication, but may also include wireless LAN network communication, mobile communication such as 3G / LTE / 5G, and Bluetooth® communication as needed. In other words, the control device 6 may communicate various information from the outside via the communication unit 61 and the network.

[0038] <Storage Unit 62> The storage unit 62 stores various types of information as defined above. This can be implemented, for example, as a storage device such as a solid-state drive (SSD) that stores various programs related to the control device 6 executed by the processor 63, or as a memory such as a random-access memory (RAM) that stores temporarily necessary information (arguments, arrays, etc.) related to program calculations. The storage unit 62 stores various programs, variables, etc. related to the control device 6 executed by the processor 63.

[0039] <Processor 63> The processor 63 performs processing and control of the overall operation related to the control device 6. The processor 63 is, for example, a Central Processing Unit (CPU). The processor 63 realizes various functions related to the control device 6 by reading predetermined programs stored in the memory unit 62. In other words, the processor 63 can read programs and execute each functional unit. These will be described in more detail in the next section. Note that the processor 63 is not limited to being a single unit; the control device 6 may have multiple processors 63 for each of one or more functions.

[0040] <Display Unit 64> The display unit 64 displays a graphical user interface (GUI) screen that can be operated by the user. The display unit 64 may be included in the housing of the thermal analyzer 10 or it may be an external device. Specifically, the display unit 64 may be implemented as a display device such as a CRT display, liquid crystal display, organic EL display, or plasma display.

[0041] <Input Unit 65> The input unit 65 receives operation inputs made by the user. The operation inputs are transmitted to the processor 63 via the communication bus 60 as command signals. The processor 63 can perform predetermined controls and calculations based on the transmitted command signals as needed. The input unit 65 may be included in the housing of the thermal analysis apparatus 10 or it may be externally mounted. For example, the input unit 65 may be implemented as a touch panel integrated with the display unit 64. When the input unit 65 is implemented as a touch panel, the user can input tap operations, swipe operations, etc. to the input unit 65. Instead of a touch panel, the input unit 65 can be a switch button, mouse, trackpad, QWERTY keyboard, etc.

[0042] <Functional Configuration> Figure 5 is a block diagram showing the functions realized by the control device 6 (processor 63). Specifically, the control device 6 (processor 63) includes a reception unit 631, an acquisition unit 632, and a specific heat calculation unit 633.

[0043] <Reception Unit 631> The reception unit 631 is configured to receive inputs of various information, commands, etc., from the user. Specifically, the reception unit 631 receives inputs such as instructions to perform a measurement and measurement conditions. The reception unit 631 receives inputs from the user, for example, through the input unit 65 of the control device 6, or through external devices (information processing devices, input devices, etc.) connected to the control device 6.

[0044] <Acquisition Unit 632> The acquisition unit 632 is configured to acquire the measurement results from the measuring device 1. Specifically, the acquisition unit 632 is configured to acquire the temperature change of the sample to be measured measured by a heating test in which the heating temperature of the sample to be measured (heating temperature by the heating furnace 2) is periodically changed and increased in the measuring device 1, the initial weight of the sample to be measured in the heating test, and a representative value of the amount of weight change of the sample to be measured during the heating test.

[0045] Specifically, the acquisition unit 632 heats the sample to be measured and the standard sample in the heating furnace 2 while periodically changing the heating temperature of the furnace 2, and acquires the heat flow rate and weight of the sample to be measured during heating from the detection unit 4. The weight change amount of the sample to be measured is a value corrected using the weight change amount of the standard sample detected by the detection unit 4 (weight change amount with the drift of the thermal analyzer 10 canceled out).

[0046] Figure 6 is a graph showing an example of controlling the heating temperature of the heating furnace 2. As shown in Figure 6, the acquisition unit 632 changes the heating temperature of the heating furnace 2 according to a heating program (temperature control function: solid line in Figure 6) which superimposes a sinusoidal temperature modulation component (AC component) onto a constant-rate heating component (DC component: dashed line in Figure 6). The temperature modulation component is a sine function with respect to time, and the frequency, amplitude, and period of the temperature modulation component are constant.

[0047] "Temperature change of the sample to be measured" refers to information regarding the change in the temperature of the sample to be measured over time, as detected by the temperature detection device 44 of the detection unit 4. Specifically, the acquisition unit 632 acquires basic data as the temperature change of the sample to be measured, including the relationship between the heat flow rate of the sample to be measured and time (heat flow curve), and the relationship between the temperature of the sample to be measured and time (temperature rate). The basic data is data in which data caused by the AC component of the heating temperature and data caused by the DC component of the heating temperature are superimposed.

[0048] The "initial weight of the sample to be measured" is, for example, the weight detected by the weight detection device 42 of the detection unit 4 before heating by the heating furnace 2 begins for the sample to be measured, which is placed on the first sample holder 3A.

[0049] The "weight change of the object being measured" is the change in the weight of the object being measured over time, as detected by the weight detection device 42. Specifically, the weight change is the change (positive or negative value) from the initial weight at each point in time, and is zero at the start of measurement.

[0050] The "representative value of weight change" is, for example, the weight change at any point in time, the maximum, minimum, or average value of weight change at any multiple points in time, or the maximum, minimum, or average value of weight change within any range. The "any (multiple) points in time" may be a specific point in time set by the user (a specific point in time when the input is received by the reception unit 631), a predetermined point in time (a predetermined time has elapsed since the start of the test), or the point in time when a predetermined temperature is reached. The "arbitrary range" may be a specific range set by the user (a specific range when the input is received by the reception unit 631), a predetermined time range, a predetermined temperature range, or the entire period of the heating test (the entire range of the acquired weight curve). The "arbitrary range" may also be set in units of the period of the temperature modulation component (i.e., the temperature modulation period in the heating test).

[0051] In particular, the representative value of the weight change is preferably the average value of the weight change of the sample being measured over a predetermined period in the heating test. With this configuration, the noise-reduced average value is used as TG, which constitutes the denominator of equation (1) used by the specific heat calculation unit 633 described later, thereby improving the accuracy of the specific heat calculation.

[0052] When the acquisition unit 632 acquires the average value of the weight change over a predetermined period as a representative value of the weight change, the predetermined period may be the temperature modulation period in the heating test. With this configuration, the value of TG that constitutes the denominator of equation (1) used by the specific heat calculation unit 633, which will be described later, becomes a value obtained by leveling the weight change of the sample being measured during the heating test with the temperature modulation period. Therefore, the accuracy of the specific heat calculation is improved. The temperature modulation period that is set as the predetermined period may be one period or multiple periods.

[0053] <Specific Heat Calculation Unit 633> The specific heat calculation unit 633 is configured to calculate the heat capacity and specific heat of the sample to be measured that underwent a heating test, based on the data (measurement results of the heating test) acquired by the acquisition unit 632.

[0054] Specifically, the specific heat calculation unit 633 is configured to calculate the specific heat of the sample to be measured by the following formula (1). In formula (1), c ｐ represents the specific heat of the sample to be measured [J / (g·K)], and C ｐ represents the heat capacity [J / K] of the sample calculated from the temperature change of the sample to be measured, and W ０ represents the initial weight [g] of the sample to be measured, and TG represents the representative value [g] of the weight change amount of the sample to be measured. c ｐ =C ｐ / (W ０ +TG) ┈ (1)

[0055] The specific heat calculation unit 633 calculates the heat capacity of the sample to be measured, for example, by the following formula (2). In formula (2), Φ Ａ represents the amplitude [W] of the heat flow of the sample to be measured caused by the alternating current component of the heating temperature of the heating furnace 2, and T Ａ represents the amplitude [K] of the temperature modulation component (sine wave) at the heating temperature of the heating furnace 2, ω is the temperature modulation frequency [Hz] in the heating test, and K(ω) is the calibration coefficient.

[0056] Specifically, the specific heat calculation unit 633 averages the heat flow rate (basic heat flow rate) and the temperature rate (basic temperature rate) included in the basic data acquired by the acquisition unit 632 respectively over one period of temperature modulation (the period of the temperature modulation component at the heating temperature of the heating furnace 2), thereby acquiring the total heat flow rate and the total temperature rate caused by the direct current component from which the alternating current component of the heating temperature has been removed. Next, the specific heat calculation unit 633 performs Fourier transform on the data obtained by subtracting the total heat flow rate and the total temperature rate from the basic heat flow rate and the basic temperature rate respectively, to obtain the respective amplitudes of the reversing heat flow rate and the reversing temperature rate caused by the alternating current component of the heating temperature. Further, the specific heat calculation unit 633 calculates the heat capacity of the sample to be measured from the amplitude ratio between the reversing heat flow rate and the reversing temperature rate (formula (2)). Subsequently, the specific heat calculation unit 633 acquires the reversing heat flow rate by multiplying the heat capacity by the average temperature rate derived from the basic data.

[0057] The reversing heat flow resulting from the alternating current component of the heating temperature mainly consists of the passive heat flow changes of the sample being measured, with active reactions (spontaneous reactions) of the sample being measured excluded.

[0058] When using the average value of the weight change of the sample being measured during the temperature modulation period in the heating test as TG in equation (1), TG is calculated by the following equation (3). In equation (3), tg(t) is the weight change at time t, t ｐ This is the modulation period.

[0059] Figure 7 is a flowchart showing an example of the specific heat calculation process by the control device 6 (processor 63). In this specific heat calculation process, first, the processor 63 causes the detection unit 4 to detect the initial weight of the sample to be measured and acquires the detected initial weight (step S110). Next, the processor 63 heats the sample to be measured and the standard sample with periodic fluctuations using the heating furnace 2, and causes the detection unit 4 to detect the temperature change (heat flow rate) and weight change value of the sample to be measured and acquires the detected temperature change and weight change value (step S120).

[0060] After acquiring the temperature change and weight change values, the processor 63 calculates the specific heat of the sample to be measured using the initial weight, temperature change, weight change value, modulation period, etc. (step S130). The processor 63 may calculate the specific heat after calculating the heat capacity of the sample to be measured, or it may calculate the specific heat directly without calculating the heat capacity. After calculating the specific heat, the processor 63 records the specific heat in the storage unit 62, etc., or outputs it to the display unit 64, etc. (step S140).

[0061] <Operation> According to the thermal analyzer 10, the specific heat is calculated using the heat capacity obtained based on the temperature change measured during the heating test and the weight change of the test, also measured during the heating test. Therefore, the specific heat can be determined with high accuracy using a temperature-modulated DSC.

[0062] Although embodiments of the present invention have been described above, the present invention is not limited thereto and can be modified as appropriate without departing from the technical spirit of the invention.

[0063] <Other> The above embodiment may also be an information processing method using an information processing device (control device 6). This information processing method includes the steps of obtaining the temperature change of a sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test, and the steps of calculating the specific heat of the sample by the following formula (1). In formula (1), c ｐ This is the specific heat of the sample, C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ is the initial weight of the sample, and TG is a representative value of the change in the sample's weight. ｐ = C ｐ / (W ０ +TG) ... (1)

[0064] Furthermore, the above embodiment may be a program that causes a computer to perform the following steps. In the acquisition step, the temperature change of the sample measured by a heating test in which the heating temperature of the sample is increased while periodically changing it, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test are acquired. In the specific heat calculation step, the specific heat of the sample is calculated by the following formula (1). In formula (1), c ｐ This is the specific heat of the sample, C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ is the initial weight of the sample, and TG is a representative value of the change in the sample's weight. ｐ is, c ｐ = C ｐ / (W ０ +TG) ... (1)

[0065] The information processing device and program described above do not necessarily have to be implemented as components of the thermal analysis apparatus 10 equipped with the measuring device 1. For example, the information processing device may be a device independent of the measuring device 1. In other words, the information processing device may be a device that acquires measurement data of an arbitrary sample (initial weight of the sample, temperature change, weight change value, modulation period of the heating test, etc.) and calculates the specific heat of the sample based on said measurement data. Similarly, the program may cause a computer independent of the measuring device 1 to perform information processing (each of the steps described above) for calculating the specific heat.

[0066] The product may be provided in any of the following embodiments.

[0067] (1) A program that causes a computer to perform the following steps, wherein in the acquisition step, the temperature change of the sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test are acquired, and in the specific heat calculation step, the specific heat of the sample is calculated by the following formula (1), where, in formula (1), c ｐ This is the specific heat, and C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ The program is defined as follows: is the initial weight, and TG is the representative value. ｐ = C ｐ / (W ０ +TG) ... (1)

[0068] With this configuration, the specific heat is calculated using the heat capacity obtained based on the temperature change measured during the heating test, and the weight change of the test, also measured during the heating test. Therefore, the specific heat can be determined with high accuracy in a temperature-modulated DSC.

[0069] (2) A program in which the representative value is the average value of the change in weight of the sample over a predetermined period in the heating test.

[0070] With this configuration, a noise-reduced average value is used as TG in the denominator of equation (1), thereby improving the accuracy of the specific heat calculation.

[0071] (3) A program in which the predetermined period is the temperature modulation period in the heating test, in the program described in (2) above.

[0072] With this configuration, the TG value in the denominator of equation (1) becomes the value obtained by averaging the weight change of the sample during the heating test with the temperature modulation period. Therefore, the accuracy of the specific heat calculation is improved.

[0073] (4) An information processing method using an information processing device, comprising the steps of obtaining the temperature change of a sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test, and calculating the specific heat of the sample by the following formula (1), wherein in formula (1), c ｐ This is the specific heat, and C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ An information processing method in which is the initial weight and TG is the representative value. ｐ = C ｐ / (W ０ +TG) ... (1)

[0074] With this configuration, the specific heat is calculated using the heat capacity, which is determined based on the temperature change measured during the heating test, and the weight change of the test, which is also measured during the heating test. Therefore, the specific heat can be determined with high accuracy in a temperature-modulated DSC.

[0075] (5) A thermal analyzer comprising a measuring device configured to heat a sample and measure the weight and temperature of the sample, and an information processing device configured to calculate the measurement results of the measuring device, wherein the information processing device has an acquisition unit configured to acquire the temperature change of the sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased in the measuring device, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test, and a specific heat calculation unit configured to calculate the specific heat of the sample by the following formula (1), in formula (1), c ｐThis is the specific heat, and C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ An information processing method in which is the initial weight and TG is the representative value. ｐ = C ｐ / (W ０ +TG) ... (1)

[0076] With this configuration, the specific heat is calculated using the heat capacity, which is determined based on the temperature change measured during the heating test, and the weight change of the test, which is also measured during the heating test. Therefore, the specific heat can be determined accurately in a temperature-modulated DSC. Of course, this is not always the case.

[0077] Finally, while various embodiments relating to this disclosure have been described, these are presented as examples only and are not intended to limit the scope of the invention. These novel embodiments can be implemented in a variety of other forms, and various omissions, substitutions, and modifications can be made without departing from the spirit of the invention. These embodiments and their variations are included in the scope and spirit of the invention, as well as in the claims and their equivalents.

[0078] 1: Measuring device, 2: Heating furnace, 3A: First sample holder, 3B: Second sample holder, 4: Detection unit, 41A: First balance beam, 41B: Second balance beam, 411: Pivot point, 412: Shutter, 42: Weight detection device, 421: Light source, 422: Photodetector, 423: PID control circuit, 424: Drive coil, 425: Calculation circuit, 43A: First thermocouple, 43B: Second Thermocouple, 44: Temperature detection device, 443A: First compensating heater, 443B: Second compensating heater, 444: Power compensation circuit, 445: Heat sensing plate, 446: Heat quantity correction circuit, 6: Control device, 60: Communication bus, 61: Communication unit, 62: Memory unit, 63: Processor, 631: Reception unit, 632: Acquisition unit, 633: Specific heat calculation unit, 64: Display unit, 65: Input unit, 10: Thermal analyzer

Claims

1. A program that causes a computer to perform the following steps: In the acquisition step, the temperature change of the sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test are acquired; In the specific heat calculation step, the specific heat of the sample is calculated by the following formula (1), where, in formula (1), c ｐ This is the specific heat, and C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ The program is defined as follows: is the initial weight, and TG is the representative value. ｐ = C ｐ / (W ０ +TG) ...(1) 2. The program according to claim 1, wherein the representative value is the average value of the weight change of the sample over a predetermined period in the heating test.

3. The program according to claim 2, wherein the predetermined period is the temperature modulation period in the heating test.

4. An information processing method using an information processing apparatus, comprising: a step of acquiring: a temperature change of the sample measured by a heating test in which a heating temperature of the sample is increased while being periodically changed; an initial weight of the sample in the heating test; and a representative value of a weight change amount of the sample during the heating test; and a step of calculating a specific heat of the sample by the following formula (1), wherein in formula (1), c ｐ is the specific heat, and C ｐ is a heat capacity of the sample calculated from the temperature change, W ０ is the initial weight, and TG is the representative value. c ｐ =C ｐ / (W ０ +TG) ... (1) 5. A thermal analyzer comprising: a measuring device configured to heat a sample and measure the weight and temperature of the sample; and an information processing device configured to calculate the measurement results of the measuring device, wherein the information processing device comprises: an acquisition unit configured to acquire the temperature change of the sample measured by a heating test in which the heating temperature of the sample is periodically changed and increased in the measuring device, the initial weight of the sample in the heating test, and a representative value of the amount of weight change of the sample during the heating test; and a specific heat calculation unit configured to calculate the specific heat of the sample by the following formula (1), where c ｐ This is the specific heat, and C ｐ This is the heat capacity of the sample calculated from the temperature change, W ０ An information processing method in which is the initial weight and TG is the representative value. ｐ = C ｐ / (W ０ +TG) ...(1)

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