Thermal analysis and quantitative analysis accuracy verification method and system

Abstract

The invention discloses a thermal analysis and quantitative analysis accuracy verification method and system, and relates to the technical field of thermal analysis, and the method comprises the following steps: respectively carrying out instrument calibration and instrument temperature calibration on a synchronous thermal analyzer based on a preset verification regulation and a preset standard substance; repeatedly testing the initial melting temperature of the to-be-tested sample for multiple times based on the synchronous thermal analyzer to obtain a test result; obtaining a first uncertainty component introduced based on a preset standard substance, determining a second uncertainty component introduced based on a test result, and calculating the extended uncertainty of the synchronous thermal analyzer for thermal analysis and quantitative analysis; and based on the expansion uncertainty, verifying the accuracy of thermal analysis and quantitative analysis of the synchronous thermal analyzer. The technical problems that in the prior art, due to the fact that a unified quality control process and a traceability analysis method are lacked, measurement repeatability is poor, accuracy is low, and traceability cannot be well conducted on measurement results are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of thermal analysis, and in particular to a method and system for verifying the accuracy of quantitative analysis in thermal analysis. Background Art

[0002] Thermal analysis is a kind of technology that measures the relationship between a certain physical property of a substance and temperature or time under certain programmed temperature control and certain atmosphere (or vacuum) conditions. It can not only be used to study various transformations (such as glass transition, solid-phase transition, etc.) and reactions (such as oxidation, decomposition, reduction, etc.) of substances, but also be used to determine the composition of substances, judge the types of substances, measure thermal property parameters (such as coefficient of thermal expansion, specific heat capacity, thermal diffusivity), etc. A thermogravimetric analyzer (TG) is an instrument that uses thermogravimetry to detect the relationship between the mass of a substance and temperature or time. A differential scanning calorimeter (DSC) is an instrument that measures the relationship between the heat flow rate or heating power (difference) input to the test sample and the reference sample and temperature (or time) under programmed temperature control and a certain atmosphere. A simultaneous thermal analyzer (STA) combines the functions of TG and DSC, and can simultaneously obtain thermogravimetry (TG) and differential scanning calorimetry (DSC) information in one measurement. Compared with single tests, the simultaneous thermal analyzer can eliminate the influence of factors such as weighing accuracy, sample uniformity, and temperature correspondence, and the curve correspondence is better. In addition, the simultaneous thermal analyzer can comprehensively judge the specific physical and chemical processes based on the changes in thermal effects and mass. For example, thermal effects such as melting and crystallization correspond to unchanged mass; thermal effects such as decomposition and oxidation correspond to decreases and increases in mass, etc. When calculating the heat enthalpy, the phase change heat and reaction heat can be accurately calculated based on the current actual mass of the sample (obtained by real-time monitoring), which is widely used in the melting point detection and analysis in the field of thermodynamics research, and is also often used in the research of chemical reference substances, etc.

[0003] In actual tests, the accuracy of thermal analysis measurement results mainly comes from the deviation of test results caused by systematic errors and random errors. The former is obtained by comparing the measured value with the standard value, and can be reduced by measures such as the instrument use environment, instrument performance determination, standard method selection, and standard substance traceability. The latter is obtained by comparing the measured value with the measured average value, and can be controlled by measures such as sample uniformity and atmosphere stability. Systematic errors and random errors run through the quality control of the entire test process. However, due to the lack of a unified quality control process and traceability analysis method at present, it leads to poor measurement repeatability, low accuracy, and inability to trace the measurement results well. Summary of the Invention

[0004] In order to solve the technical problems existing in the prior art, such as poor measurement repeatability, low accuracy, and inability to trace the measurement results well due to the lack of a unified quality control process and traceability analysis method, an embodiment of the present invention provides a method and system for verifying the accuracy of thermal analysis quantitative analysis. The technical solutions are as follows:

[0005] On the one hand, a method for verifying the accuracy of thermal analysis quantitative analysis is provided. The method includes: calibrating the instrument of the synchronous thermal analyzer based on a preset verification regulation; calibrating the instrument temperature of the synchronous thermal analyzer based on a preset reference material to form a temperature calibration curve; repeatedly testing the initial melting temperature of the sample to be tested by the synchronous thermal analyzer for multiple times, and correcting based on the temperature calibration curve to obtain a test result; obtaining a first uncertainty component introduced by the preset reference material, and determining a second uncertainty component introduced by the test result; calculating the expanded uncertainty of the synchronous thermal analyzer for thermal analysis quantitative analysis based on the first uncertainty component and the second uncertainty component; verifying the accuracy of the synchronous thermal analyzer for thermal analysis quantitative analysis based on the expanded uncertainty.

[0006] Optionally, the preset verification regulation includes a verification regulation for a thermogravimetric analyzer, a verification regulation for a differential scanning calorimeter, a verification regulation for a thermogravimetric analyzer, and a verification regulation for a differential scanning thermal analyzer.

[0007] Optionally, after calibrating the instrument of the synchronous thermal analyzer based on the preset verification regulation, the method further includes: determining the calibration parameters of the synchronous thermal analyzer; determining whether the synchronous thermal analyzer meets the preset standard based on the calibration parameters and the preset verification regulation.

[0008] Optionally, calculating the expanded uncertainty of the synchronous thermal analyzer for thermal analysis quantitative analysis based on the first uncertainty component and the second uncertainty component includes: substituting the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty of the synchronous thermal analyzer for thermal analysis quantitative analysis; wherein, the preset expanded uncertainty calculation formula includes:

[0009]

[0010] In the formula, u c (ΔT) is the expanded uncertainty, u(T e ) is the first uncertainty component, u(T s ) is the second uncertainty component, and are sensitivity coefficients.

[0011] On the other hand, a thermal analysis quantitative analysis accuracy verification system is also provided. The thermal analysis quantitative analysis accuracy verification system is used to implement the thermal analysis quantitative analysis accuracy verification method provided by the present invention, and includes: a first calibration module, a second calibration module, a test module, a determination module, a calculation module and a verification module; wherein, the first calibration module is used to calibrate the synchronous thermal analyzer based on a preset verification procedure; the second calibration module is used to calibrate the instrument temperature of the synchronous thermal analyzer based on a preset reference material to form a temperature calibration curve; the test module is used to repeatedly test the initial melting temperature of the sample to be tested based on the synchronous thermal analyzer and correct it based on the temperature calibration curve to obtain a test result; the determination module is used to obtain a first uncertainty component introduced based on the preset reference material and determine a second uncertainty component introduced based on the test result; the calculation module is used to calculate the expanded uncertainty of the synchronous thermal analyzer for thermal analysis quantitative analysis based on the first uncertainty component and the second uncertainty component; the verification module is used to verify the accuracy of the synchronous thermal analyzer for thermal analysis quantitative analysis based on the expanded uncertainty.

[0012] Optionally, the preset verification procedure includes a thermogravimetric analyzer verification procedure, a differential scanning calorimeter verification procedure, a thermogravimetric analyzer verification procedure and a differential scanning thermal analyzer verification procedure.

[0013] Optionally, the first calibration module is further used to: determine the calibration parameters of the synchronous thermal analyzer; and determine whether the synchronous thermal analyzer meets the preset standards based on the calibration parameters and the preset verification procedure.

[0014] Optionally, the calculation module is further used to: substitute the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty of the synchronous thermal analyzer for thermal analysis quantitative analysis; wherein, the preset expanded uncertainty calculation formula includes:

[0015]

[0016] In the formula, u c (ΔT) is the expanded uncertainty, u(T e ) is the first uncertainty component, u(T s ) is the second uncertainty component, and are sensitivity coefficients.

[0017] On the other hand, an electronic device is also provided, including: a memory, a processor, and a computer program stored on the memory and executable on the processor, where when the processor executes the computer program, the method provided by the present invention is implemented.

[0018] On the other hand, a computer-readable storage medium is also provided, in which program code is stored, and the program code can be called by a processor to execute the method provided by the present invention.

[0019] An embodiment of the present invention provides a method and system for verifying the accuracy of thermal analysis quantitative analysis. By establishing a full-process quality control mode for test processes such as the stability confirmation of a synchronous thermal analyzer, the selection of standard test methods, and the traceability of reference materials, and based on the test process of reference materials, uncertainty analysis is carried out, which ensures the effectiveness of data in the thermal analysis process and alleviates the technical problems in the prior art, such as poor measurement repeatability, low accuracy, and inability to trace the measurement results well due to the lack of a unified quality control process and traceability analysis method. Description of the Drawings

[0020] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for description in the embodiments. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0021] Figure 1 is a flowchart of a method for verifying the accuracy of thermal analysis quantitative analysis provided by an embodiment of the present invention;

[0022] Figure 2 is a schematic diagram of a temperature calibration curve provided by an embodiment of the present invention;

[0023] Figure 3 is a TG-DSC curve graph of the first test on the initial melting temperature of a sample to be tested provided by an embodiment of the present invention;

[0024] Figure 4 is a TG-DSC curve graph of the second test on the initial melting temperature of a sample to be tested provided by an embodiment of the present invention;

[0025] Figure 5 is a TG-DSC curve graph of the third test on the initial melting temperature of a sample to be tested provided by an embodiment of the present invention;

[0026] Figure 6 is a schematic diagram of a system for verifying the accuracy of thermal analysis quantitative analysis provided by an embodiment of the present invention;

[0027] Figure 7 It is a schematic diagram of an electronic device provided by an embodiment of the present invention. Specific embodiments

[0028] The following will describe the technical solutions in the present invention with reference to the accompanying drawings.

[0029] In the embodiments of the present invention, words such as "exemplarily" and "for example" are used to represent examples, illustrations or explanations. Any embodiment or design solution described as an "example" in the present invention should not be construed as being more preferred or more advantageous than other embodiments or design solutions. Exactly speaking, the use of the word "example" is intended to present concepts in a specific way. In addition, in the embodiments of the present invention, the meaning expressed by "and / or" can be both, or either one of the two can be selected.

[0030] To make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following will be described in detail with reference to the accompanying drawings and specific embodiments.

[0031] Figure 1 It is a flowchart of a method for verifying the accuracy of quantitative thermal analysis according to an embodiment of the present invention. As Figure 1 shown, the method specifically includes the following steps:

[0032] Step S102, calibrate the instrument of the synchronous thermal analyzer based on a preset verification procedure.

[0033] In an optional embodiment provided by the embodiments of the present invention, the preset verification procedure includes a verification procedure for a thermogravimetric analyzer, a verification procedure for a differential scanning calorimeter, a verification procedure for a thermogravimetric analyzer, and a verification procedure for a differential scanning thermal analyzer.

[0034] Step S104, calibrate the instrument temperature of the synchronous thermal analyzer based on a preset reference material to form a temperature calibration curve.

[0035] Step S106, perform multiple repeated tests on the initial melting temperature of the sample to be tested based on the synchronous thermal analyzer, and correct based on the temperature calibration curve to obtain a test result.

[0036] Step S108, obtain a first uncertainty component introduced based on a preset reference material, and determine a second uncertainty component introduced based on the test result.

[0037] Specifically, the first uncertainty component is directly determined by the traceability information on the certificate of the preset reference material, and the second uncertainty component is determined by the standard deviation of the measurement results of multiple repeated tests.

[0038] Step S110: Calculate the expanded uncertainty for quantitative thermal analysis of the synchronous thermal analyzer based on the first uncertainty component and the second uncertainty component.

[0039] Specifically, step S110 further includes the following steps: Substitute the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty for quantitative thermal analysis of the synchronous thermal analyzer; wherein, the preset expanded uncertainty calculation formula includes:

[0040]

[0041] In the formula, u c (ΔT) is the expanded uncertainty, u(T e ) is the first uncertainty component, u(T s ) is the second uncertainty component, and are sensitivity coefficients.

[0042] Step S112: Verify the accuracy of quantitative thermal analysis of the synchronous thermal analyzer based on the expanded uncertainty.

[0043] Specifically, after step S102, the method provided by the embodiment of the present invention further includes:

[0044] Determine the calibration parameters of the synchronous thermal analyzer;

[0045] Based on the calibration parameters and a preset verification regulation, determine whether the synchronous thermal analyzer meets the preset standard.

[0046] Taking the synchronous thermal analyzer model STA449F3 as an example, the embodiment of the present invention illustrates the application process of the method provided by the embodiment of the present invention. Among them, the standard substances selected for calibration and verification of the synchronous thermal analyzer include In, Pb, and Zn, and the metal Zn with high purity (>99%) is selected as the sample to be measured.

[0047] (1) Instrument calibration: Compile an instrument calibration procedure with reference to the "Verification Regulation of Thermogravimetric Analyzers" (JJG1135-2017) and the "Verification Regulation of Differential Scanning Calorimeters" (JJG936-2012), and perform instrument calibration before the experiment to ensure that the instrument performance is in good condition. The relevant calibration parameters are used to guide the uncertainty analysis of the experimental results.

[0048] (2) Instrument temperature calibration: Temperature calibration refers to the deviation between the temperature measured by the thermocouple and the actual temperature of the sample. Using the method of testing the melting points of standard metals, select three standard substances, In, Sn, and Pb, and perform instrument temperature calibration according to the instrument temperature correction procedure used (STA instrument correction, cPH60-STA-04) to form a temperature calibration curve, asFigure 2 As shown, the calibration of the melting point temperature for actual testing.

[0049] (3) Sample testing: According to the standard methods of General Rules for Thermal Analysis - Part 1: General Principles (JY / T 0589·1 - 2020) and General Rules for Thermal Analysis Methods - Part 5: Thermogravimetry - Differential Scanning Calorimetry (JY / T 0589·5 - 2020), the initial melting temperature of the sample to be tested is repeatedly tested three times. Figure 3 is a TG - DSC curve graph for the first test of the initial melting temperature of the sample to be tested provided according to an embodiment of the present invention, Figure 4 is a TG - DSC curve graph for the second test of the initial melting temperature of the sample to be tested provided according to an embodiment of the present invention, Figure 5 is a TG - DSC curve graph for the third test of the initial melting temperature of the sample to be tested provided according to an embodiment of the present invention. As Figures 3 - 5 shown, the melting temperature values obtained from the three measurements are 420.8 °C, 420.6 °C, and 420.6 °C respectively.

[0050] (4) Traceability analysis of experimental results:

[0051] (a) Evaluation of temperature indication uncertainty:

[0052] According to the verification regulation of differential scanning calorimeter JJG 936 - 2012, the temperature indication error of the instrument is:

[0053] ΔT = T e - T s (1)

[0054] In the formula, ΔT - the indication error of temperature;

[0055] T e —the transition temperature of the reference material measured by the instrument (°C);

[0056] T s —the standard value of the reference material (°C).

[0057] According to formula (1) and the law of propagation of uncertainty, the variance and sensitivity coefficient can be expressed as:

[0058]

[0059] As can be seen from the above, the main factors affecting the uncertainty evaluation are two aspects: the uncertainty component u(T s )(i.e., the first uncertainty component) introduced by the reference material and the uncertainty component u(T e )(i.e., the second uncertainty component) introduced by the measurement repeatability of the instrument.

[0060] (b) Calculation of the uncertainty of the main factors:

[0061] (1) Uncertainty component introduced by the reference material: It can be obtained from the reference material certificate that the standard melting temperature of the reference material Zn is 420.67 °C, the coverage factor k = 2, and the expanded uncertainty is 0.60 °C (the reference material with the maximum uncertainty). Therefore, the standard uncertainty is 0.30 °C, that is, = 0.30 °C.

[0062] (2) Uncertainty component introduced by the measurement repeatability of the instrument: Measure the melting temperature of the reference material Zn (GBW(E)130185), repeat the measurement 5 times, and the test experimental data are shown in Table 1. The average value is 420.46 °C, and the standard deviation is 0.30 °C. The number of measurements of the sample to be tested is 3 times, then = 0.17 °C.

[0063] Table 1 Uncertainty component introduced by the measurement repeatability of the instrument

[0064]

[0065]

[0066] Table 2 Summary table of uncertainty components of temperature indication error

[0067]

[0068] (c) Combined and expanded uncertainty:

[0069] Combine the above uncertainty components to obtain:

[0070]

[0071] Take the coverage factor k = 2, and the expanded uncertainty is:

[0072] U(ΔT) = k·u c (ΔT) = 2 × 0.34 °C = 0.68 °C

[0073] The average melting temperature of the sample to be tested is 420.7 °C, the expanded uncertainty is 0.68 °C, and the coverage factor K = 2.

[0074] From the above results, it can be seen that the synchronous thermal analyzer can perform thermal analysis tests in a wide range (-150 °C to 1600 °C). By establishing a full-process quality control mode for the test process from the stability confirmation of the instrument, the selection of standard test methods, and the traceability of reference materials, taking the experiment of "determination of the initial melting temperature of unknown substances" as an example, test values with small errors are obtained, and uncertainty analysis is carried out to ensure the validity of the data and verify the accuracy of the experimental data under this mode.

[0075] The embodiments of the present invention also provide a full-process quality control mode, including:

[0076] (1) Laboratory environment:

[0077] Before the experiment, ensure that the laboratory environment meets the specified operating conditions of the instrument. The specified environmental temperature for this instrument is 15 - 28°C, and the humidity is <85% (RH) (for specific instruments, please refer to the regulations on the instrument's operating environmental conditions). Place the instrument on a stable laboratory bench and adjust it to a horizontal state. Avoid touching the test bench during the experiment to eliminate vibration interference.

[0078] (2) Selection of standard methods:

[0079] The statistics of thermal analysis standard methods are shown in Table 3. Combining the test indicators of the present invention and the performance indicators of the instrument, select General Principles of Thermal Analysis - Part 1: General Rules (JY / T 0589·1 - 2020) and Thermogravimetry - Differential Thermal Analysis and Thermogravimetry - Differential Scanning Calorimetry (JY / T 0589·5 - 2020) as the standard methods of the present invention.

[0080] Table 3 Statistics of Thermal Analysis Standard Methods

[0081]

[0082] (3) Instrument performance:

[0083] Currently, the verification regulations for thermal analyzers mainly include Verification Regulation of Thermogravimetric Analyzer (WJ 2292 - 1995), Verification Regulation of Differential Scanning Calorimeter (WJ 2290 - 1995), Verification Regulation of Thermal Analyzer (JJG 014 - 1996), Verification Regulation of Thermogravimetric Analyzer (JJG 1135 - 2017), and Verification Regulation of Differential Scanning Calorimeter (JJG 936 - 2012), etc. Combining the test requirements, the performance of the used instrument, and the technical index requirements of the selected standard method, finally select 4 verification indicators including temperature repeatability, temperature indication error, melting point repeatability, and melting point indication error. After the instrument is verified by metrology, the indicators meet the standard requirements. The verification results are shown in the following table:

[0084] Table 4 Instrument Verification Results

[0085]

[0086]

[0087] (4) Selection of reference materials:

[0088] Select national certified reference materials to meet traceability. The temperature range of the standard sample should cover the melting temperature of the substance to be measured, and the melting temperature point is preferably at the median of the temperature range of the reference material.

[0089] Table 5 Standard Substance Statistical Table

[0090]

[0091] (5) Traceability analysis:

[0092] ① Identify sources of uncertainty: Comprehensively consider various factors that may affect the test results, including the accuracy of measuring equipment, environmental conditions, the skills and experience of operators, the limitations of measurement methods, etc.

[0093] ② Quantify uncertainty components: Analyze each identified source of uncertainty through methods such as experimental data, calibration certificates, technical specifications, or empirical estimates, and quantify the magnitude of the uncertainty it may cause.

[0094] ③ Calculate the combined uncertainty: According to the law of propagation of uncertainty, combine each uncertainty component to obtain the total uncertainty of the test result.

[0095] ④ Evaluate the impact of uncertainty: Analyze the degree of influence of uncertainty on the test result and determine whether it is within an acceptable range.

[0096] ⑤ Report uncertainty: Clearly and accurately state the evaluation results of uncertainty in the test report, including the value of uncertainty and the coverage factor, etc.

[0097] Figure 6 is a schematic diagram of a system for verifying the accuracy of thermal analysis quantitative analysis provided by an embodiment of the present invention. This system is used to implement the method for verifying the accuracy of thermal analysis quantitative analysis provided by an embodiment of the present invention. As Figure 6 shown, the system includes: a first calibration module 10, a second calibration module 20, a test module 30, a determination module 40, a calculation module 50, and a verification module 60.

[0098] Specifically, the first calibration module 10 is used to calibrate the synchronous thermal analyzer based on a preset verification procedure;

[0099] The second calibration module 20 is used to calibrate the instrument temperature of the synchronous thermal analyzer based on a preset standard substance to form a temperature calibration curve;

[0100] The test module 30 is used to repeatedly test the initial melting temperature of the sample to be tested based on the synchronous thermal analyzer and correct it based on the temperature calibration curve to obtain the test result;

[0101] The determination module 40 is used to obtain the first uncertainty component introduced based on a preset standard substance and determine the second uncertainty component introduced based on the test result;

[0102] A calculation module 50 is configured to calculate the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis based on the first uncertainty component and the second uncertainty component.

[0103] A verification module 60 is configured to verify the accuracy of the synchronous thermal analyzer for quantitative thermal analysis based on the expanded uncertainty.

[0104] Specifically, the preset verification procedures include the verification procedures for thermogravimetric analyzers, differential scanning calorimeters, thermogravimetric analyzers, and differential scanning thermal analyzers.

[0105] Specifically, the first calibration module 10 is further configured to:

[0106] Determine the calibration parameters of the synchronous thermal analyzer;

[0107] Based on the calibration parameters and the preset verification procedures, determine whether the synchronous thermal analyzer meets the preset standards.

[0108] Specifically, the calculation module 50 is further configured to: substitute the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis; wherein, the preset expanded uncertainty calculation formula includes:

[0109]

[0110] In the formula, u c (ΔT) is the expanded uncertainty, u(T e ) is the first uncertainty component, u(T s ) is the second uncertainty component, and are sensitivity coefficients.

[0111] The present invention also provides an electronic device, as Figure 7 shown, including: a memory 701, a processor 702, and a computer program stored on the memory 701 and executable on the processor. When the processor 702 executes the computer program, the method provided by the present invention is implemented.

[0112] The present invention also provides a computer-readable storage medium. The computer-readable storage medium stores program codes, and the program codes can be called by a processor to execute the method provided by the present invention.

[0113] It should be understood that the memory in the embodiments of the present invention may be a volatile memory or a non-volatile memory, or may include both volatile and non-volatile memories. Among them, the non-volatile memory may be a read-only memory (ROM), a programmable read-only memory (PROM), an erasable programmable read-only memory (EPROM), an electrically erasable programmable read-only memory (EEPROM), or a flash memory. The volatile memory may be a random access memory (RAM), which is used as an external cache. By way of example but not limitation, many forms of random access memory (RAM) are available, such as static random access memory (SRAM), dynamic random access memory (DRAM), synchronous dynamic random access memory (SDRAM), double data rate synchronous dynamic random access memory (DDR SDRAM), enhanced synchronous dynamic random access memory (ESDRAM), synchlink dynamic random access memory (SLDRAM), and direct rambus random access memory (DR RAM).

[0114] The above embodiments can be implemented in whole or in part by software, hardware (such as circuits), firmware, or any combination thereof. When implemented using software, the above embodiments can be implemented in whole or in part in the form of a computer program product. The computer program product includes one or more computer instructions or computer programs. When the computer instructions or computer programs are loaded or executed on a computer, the processes or functions described in the embodiments of the present invention are generated in whole or in part. The computer can be a general-purpose computer, a special-purpose computer, a computer network, or other programmable devices. The computer instructions can be stored in a computer-readable storage medium, or transmitted from one computer-readable storage medium to another. For example, the computer instructions can be transmitted from one website, computer, server, or data center to another website, computer, server, or data center by wired (such as infrared, wireless, microwave, etc.) means. The computer-readable storage medium can be any available medium that can be accessed by a computer, or a data storage device such as a server or data center that contains one or more collections of available media. The available media can be magnetic media (such as floppy disks, hard disks, magnetic tapes), optical media (such as DVDs), or semiconductor media. The semiconductor media can be a solid-state drive.

[0115] It should be understood that in various embodiments of the present invention, the order numbers of the above processes do not mean the order of execution. The order of execution of each process should be determined by its function and internal logic, and should not constitute any limitation to the implementation process of the embodiments of the present invention.

[0116] Those of ordinary skill in the art can realize that the units and algorithm steps of each example described in combination with the embodiments disclosed herein can be implemented by electronic hardware, or a combination of computer software and electronic hardware. Whether these functions are executed in a hardware or software manner depends on the specific application and design constraints of the technical solution. Professional technicians can use different methods to implement the described functions for each specific application, but such implementation should not be considered to exceed the scope of the present invention.

[0117] Those skilled in the art can clearly understand that for the convenience and brevity of description, the specific working processes of the devices, apparatuses, and units described above can refer to the corresponding processes in the foregoing method embodiments, and will not be described herein again.

[0118] In several embodiments provided by the present invention, it should be understood that the disclosed devices, apparatuses, and methods can be implemented in other ways. For example, the apparatus embodiments described above are merely illustrative. For example, the division of the units is only a logical function division. In actual implementation, there may be other division methods. For example, multiple units or components can be combined or integrated into another device, or some features can be ignored or not executed. Another point is that the displayed or discussed couplings or direct couplings or communication connections to each other can be through some interfaces. The indirect couplings or communication connections of the devices or units can be in electrical, mechanical, or other forms.

[0119] The units described as separate components may or may not be physically separated. The components displayed as units may or may not be physical units, that is, they can be located in one place or distributed to multiple network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of this embodiment.

[0120] In addition, in each embodiment of the present invention, the functional units can be integrated in a processing unit, or each unit can exist physically alone, or two or more units can be integrated in one unit.

[0121] If the functions are implemented in the form of software function units and sold or used as independent products, they can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present invention, in essence, or the part that contributes to the prior art, or this part of the technical solution, can be embodied in the form of a software product. This computer software product is stored in a storage medium and includes several instructions to enable a computer device (which can be a personal computer, a server, or a network device, etc.) to execute all or part of the steps of the methods described in each embodiment of the present invention. The foregoing storage medium includes: various media such as USB flash drives, mobile hard disks, read-only memory (ROM), random access memory (RAM), magnetic disks, or optical discs that can store program codes.

[0122] As described above, the above are only specific implementation manners of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered by the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims

1. A method for verifying the accuracy of quantitative analysis in thermal analysis, characterized in that The method includes: Calibrating the synchronous thermal analyzer based on a preset verification procedure; Calibrating the instrument temperature of the synchronous thermal analyzer based on a preset reference material to form a temperature calibration curve; Repeatedly testing the initial melting temperature of the sample to be tested based on the synchronous thermal analyzer and correcting based on the temperature calibration curve to obtain a test result; Obtaining a first uncertainty component introduced based on the preset reference material and determining a second uncertainty component introduced based on the test result; Calculating the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis based on the first uncertainty component and the second uncertainty component; Verifying the accuracy of the synchronous thermal analyzer for quantitative thermal analysis based on the expanded uncertainty.

2. The method according to claim 1, wherein The preset verification procedure includes the verification procedures for thermogravimetric analyzers, differential scanning calorimeters, thermogravimetric analyzers, and differential scanning thermal analyzers.

3. The method according to claim 1, characterized in that, After calibrating the synchronous thermal analyzer based on the preset verification procedure, the method further includes: Determining the calibration parameters of the synchronous thermal analyzer; Determining whether the synchronous thermal analyzer meets the preset standards based on the calibration parameters and the preset verification procedure.

4. The method according to claim 1, wherein Calculating the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis based on the first uncertainty component and the second uncertainty component, including: Substituting the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis; wherein, the preset expanded uncertainty calculation formula includes: where u c (ΔT) is the expanded uncertainty, u(T e ) is the first uncertainty component, u(T s ) is the second uncertainty component, and are sensitivity coefficients.

5. A system for verifying the accuracy of quantitative thermal analysis, the system for verifying the accuracy of quantitative thermal analysis being used to implement the method for verifying the accuracy of quantitative thermal analysis according to any one of claims 1-5, characterized in that including: A first calibration module, a second calibration module, a testing module, a determination module, a calculation module, and a verification module; wherein, The first calibration module is used to calibrate the synchronous thermal analyzer based on a preset verification procedure; The second calibration module is used to calibrate the instrument temperature of the synchronous thermal analyzer based on a preset reference material to form a temperature calibration curve; The testing module is used to repeatedly test the initial melting temperature of the sample to be tested based on the synchronous thermal analyzer and correct based on the temperature calibration curve to obtain a test result; The determination module is used to obtain a first uncertainty component introduced based on the preset reference material and determine a second uncertainty component introduced based on the test result; The calculation module is used to calculate the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis based on the first uncertainty component and the second uncertainty component; The verification module is used to verify the accuracy of the synchronous thermal analyzer for quantitative thermal analysis based on the expanded uncertainty.

6. The system according to claim 5, wherein The preset verification procedure includes the verification procedures for thermogravimetric analyzers, differential scanning calorimeters, thermogravimetric analyzers, and differential scanning thermal analyzers.

7. The system according to claim 5, wherein The first calibration module is further used to: Determine the calibration parameters of the synchronous thermal analyzer; Determine whether the synchronous thermal analyzer meets the preset standards based on the calibration parameters and the preset verification procedure.

8. The system according to claim 5, characterized in that The calculation module is further configured to: substitute the first uncertainty component and the second uncertainty component into a preset expanded uncertainty calculation formula to calculate the expanded uncertainty of the synchronous thermal analyzer for quantitative thermal analysis; wherein, the preset expanded uncertainty calculation formula includes: where \(u\) c \((\Delta T)\) is the expanded uncertainty, \(u(T\) e ) is the first uncertainty component, \(u(T\) s ) is the second uncertainty component, and are sensitivity coefficients.

9. An electronic device, characterized in that, including: a memory, a processor, and a computer program stored on the memory and executable on the processor, wherein the processor implements the method according to any one of claims 1-4 when executing the computer program.

10. A computer-readable storage medium, characterized in that, The computer-readable storage medium stores program code, and the program code can be called by the processor to execute the method according to any one of claims 1 to 4.

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