CN109916948B - Calorimeter and testing method thereof - Google Patents
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- CN109916948B CN109916948B CN201910228450.9A CN201910228450A CN109916948B CN 109916948 B CN109916948 B CN 109916948B CN 201910228450 A CN201910228450 A CN 201910228450A CN 109916948 B CN109916948 B CN 109916948B
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- 238000012360 testing method Methods 0.000 title claims abstract description 74
- 238000007789 sealing Methods 0.000 claims abstract description 37
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- 238000001514 detection method Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
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Abstract
The invention discloses a calorimeter and a testing method thereof, wherein the calorimeter comprises: an insulated sealed box, a heater, and a data recording computing system; the bottom of the heat-insulating sealing box is provided with a plurality of knobs, and the knobs are used for fixing the sample containers; each sample container is provided with a thermocouple, and the thermocouple passes through the heat insulation sealing box and is connected with the data recording and calculating system; the data record computing system is connected with the heater; the heater is connected with the heat-insulating sealing box. The calorimeter provided by the invention has low cost, a plurality of calorimeters can be configured according to the requirements, and queuing is not needed; and multiple groups can be tested simultaneously, so that the working efficiency is effectively improved; further, the invention adopts the average value to represent the actual temperature of the heat conducting medium in the test process, thereby improving the test accuracy.
Description
Technical Field
The invention relates to the technical field of thermal analysis, in particular to a calorimeter and a testing method thereof.
Background
Currently, a well-known test tool for glass transition temperature, specific heat and latent heat of materials is a Differential Scanning Calorimeter (DSC). Because the calorimeter is high in price, each scientific research institute only purchases one piece of equipment, queuing is needed, the equipment is used for a long time, the detection period is prolonged, the working progress is affected, and the equipment can only test one sample at a time, so that the working efficiency is low; meanwhile, carrier gas, a crucible, a heating rate, sample quantity and the like can influence a DSC curve in the test process, so that the reproducibility of data is poor, and the test accuracy is influenced.
Therefore, how to improve the working efficiency and the accuracy of the test results are urgent to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a calorimeter and a testing method thereof, which have low cost, can be configured into a plurality of sets according to requirements without queuing and waiting, can test a plurality of sets at the same time, and effectively improve the working efficiency; meanwhile, the average value is adopted to represent the actual temperature of the heat conducting medium in the test process, so that the accuracy of a test result is improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a calorimeter, comprising: an insulated sealed box, a heater, and a data recording computing system;
the bottom of the heat-insulating sealing box is provided with a plurality of knobs, and the knobs are used for fixing the sample containers; each sample container is provided with a thermocouple, and the thermocouple passes through the heat insulation sealing box and is connected with the data recording and calculating system;
the data record computing system is connected with the heater;
the heater is connected with the heat-insulating sealing box.
Furthermore, the maximum mass/volume of the heat-conducting medium is calculated in advance according to the size of the heat-insulating sealing box and the number of the sample containers before the heat-conducting medium is injected into the heater, so that the heat-conducting medium cannot enter the sample containers, and the test sample is effectively prevented from being polluted by the heat-conducting medium.
Preferably, the wall material of the heat-insulating sealing box is made of hollow hard plastic, a heat-insulating plate is stuck on the inner side of the wall material, and heat-insulating anticorrosive paint is coated on the inner side of the heat-insulating plate.
Preferably, the heat-insulating board is made of extruded polystyrene foam board.
Preferably, the heater is connected with the heat insulation sealing box through a pipeline, and an electromagnetic valve is arranged on the pipeline.
Preferably, the heater is provided with an opening for injecting the heat-conducting medium.
Preferably, a liquid outlet is arranged at the bottom of the heat-insulating sealing box.
Preferably, a thermocouple is connected to the data logging computing system and extends into the heater.
Preferably, the position of the sample container is selected according to the number of test samples; and the average temperature according to the rest of thermocouple test is taken as the actual temperature of the heat conducting medium.
A method of testing a calorimeter comprising the steps of:
1) Selecting the position of the sample container according to the number of the test samples;
2) Preparing a test sample, and standing the test sample at room temperature;
3) According to the property of the test sample, determining a required test temperature range, further selecting a corresponding heat conducting medium, weighing, pouring into a heater, starting the heater, setting the temperature, and starting a data recording and calculating system;
4) When the heat conducting medium is heated to a set temperature, the heat conducting medium is introduced into an adiabatic sealing box, when the temperature change in the adiabatic sealing box is stable, a stationary test sample with known mass is placed into a sample container, a thermocouple is inserted, the adiabatic sealing box is closed, a data recording computing system starts to work, and data are recorded;
5) And obtaining an experimental result according to the data recorded by the data recording and calculating system.
Compared with the prior art, the calorimeter and the testing method provided by the invention have the advantages that the integral structure is simple, the key components are the heat insulation sealing box, the thermocouple, the heater and the data recording and calculating system, the cost of the components is low, the manufacturing cost is about twenty thousands, and the advantage is obvious compared with the millions of prices of calorimeter products of Germany, relaxation resistance, american TA and other companies. And because the cost is low, each unit can be configured to be multiple according to the requirement, queuing is not needed, work is not delayed, and the working efficiency can be effectively improved.
Moreover, the calorimeter provided by the invention can test a plurality of groups of test samples at the same time, thereby greatly improving the working efficiency. Meanwhile, the average value is adopted to represent the actual temperature of the heat conducting medium in the test process, so that the accuracy of a test result is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a calorimeter according to the present invention;
FIG. 2 is a schematic diagram of a calorimeter according to the present invention;
FIG. 3 is a schematic representation of the temperature versus time curve of the test provided by the present invention.
In the figure:
1. the device comprises an adiabatic sealing box 2, a heater 3, a data recording and calculating system 4, a knob 5, a sample container 6, a thermocouple 7, an electromagnetic valve 8, an opening 9 and a liquid outlet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1 and 2, an embodiment of the present invention discloses a calorimeter, comprising: an insulated sealed box 1, a heater 2 and a data recording computing system 3;
a plurality of knobs 4 are distributed at the bottom of the heat-insulating sealing box 1, and the knobs 4 are used for fixing a sample container 5; each sample container 5 is provided with a thermocouple 6, and the thermocouple 6 passes through the heat insulation sealing box 1 and is connected with the data recording and calculating system 3; the data record computing system 3 is connected with the heater 2; the heater 2 is connected with the heat-insulating sealed box 1.
The knob is a common screw knob, and the bottom of the sample container is correspondingly provided with screw threads matched with the screw knob. During the test, the excess sample containers can be unscrewed or a corresponding number of sample containers can be screwed according to the experimental requirements.
The calorimeter provided by the invention has a simple integral structure, key components are an insulation sealing box, a thermocouple, a heater and a data recording and calculating system, the cost of the components is low, the manufacturing cost is about twenty thousands, compared with the price of millions of calorimeter products of Germany, fast, american TA and other companies, the calorimeter has obvious advantages, and due to the low cost, each unit can be provided with a plurality of units according to the requirements, the queuing is not needed, the work is not delayed, and the working efficiency is improved. Moreover, the calorimeter provided by the invention can test a plurality of groups of test samples at the same time, thereby greatly improving the working efficiency.
In addition, the calorimeter provided by the invention avoids the influence of factors such as heating rate, carrier gas, crucible, sample quantity and the like, improves the experimental accuracy, increases the requirement on the sample quality to gram level, and has the advantages that the thermal effect is theoretically amplified by 1000 times, and the result is more visual.
In specific implementation, a thermocouple with an accuracy of 0.1 ℃ can be used; a round opening is formed in the top of the heat-insulating sealing box, a thermocouple can penetrate through the round opening to be connected with a data recording and calculating system, and heat preservation and heat insulation treatment is carried out at the round opening. The data recording and calculating system records the change of the temperature of the thermocouple at any time, and the time interval can be set to be 2 seconds when the thermocouple is applied to a specific application.
The test container is used for containing a test sample in an experiment, and is made of a material with high heat conductivity coefficient.
In order to further optimize the technical scheme, the wall material of the heat-insulating sealing box 1 is made of hollow hard plastic, a heat-insulating plate is stuck on the inner side of the heat-insulating sealing box, and heat-insulating anti-corrosion paint is coated on the inner side of the heat-insulating plate. Preferably, the material of the heat-insulating plate is extruded polystyrene foam plate.
In order to further optimize the technical scheme, the heater 2 is connected with the heat-insulating sealing box 1 through a pipeline, and a solenoid valve 7 is arranged on the pipeline. In concrete implementation, the two ends of the pipeline are filled with heat-insulating cotton and are subjected to heat insulation treatment; an electromagnetic valve 7 is arranged in the pipeline, and the switch of the pipeline is controlled through the electromagnetic valve 7.
In order to further optimize the above solution, the heater 2 is provided with openings 8 for injecting a heat-conducting medium. The liquid level of the heat conducting medium introduced into the heat insulating sealed box 1 is equal to the upper edge of the test container after the test container is placed in the heat insulating sealed box 1, so that the test sample is effectively prevented from being polluted by the heat conducting medium. The heating range of the heater can be set to be 0-300 ℃, and the temperature is kept constant after the set temperature is reached. The heat transfer medium is composed of substances of known heat capacity and boiling point, such as: water, glycerol, and the like.
It should be noted here that the heater may be connected to the heat-insulating seal box by a communicating vessel principle, and in a specific arrangement, the height of the heater may be set to be higher than that of the heat-insulating seal box, or the heater and the heat-insulating seal box may be set at the same level, so that a power device (e.g., a pump) is added to the pipeline to ensure that the heat-conducting medium in the heater can smoothly flow into the heat-insulating seal box.
Meanwhile, the maximum mass/volume of the heat transfer medium required is calculated in advance according to the size of the heat insulating sealing case and the number of sample containers before injecting the heat transfer medium into the heater.
For example: when the number of the test samples is 1, only 1 sample container is adopted, the maximum mass/volume of the heat-conducting medium required is the length of the heat-insulating sealing box, the width of the heat-insulating sealing box, the height of the sample container and the volume of the sample container, and the height of the heat-insulating sealing box and the volume of the sample container can be measured in advance.
Further by way of example: when 2 test samples are used, 2 sample containers are used, and the maximum mass/volume of the heat transfer medium required is the length of the heat-insulating sealed box, the width of the heat transfer medium, the height of the sample containers minus the volume of the 2 sample containers, and so on.
In order to further optimize the technical scheme, the bottom of the heat-insulating sealing box 1 is provided with a liquid outlet 9 for discharging and recycling the heat-conducting medium after experiments.
In order to further optimize the technical scheme, the data recording and calculating system 3 draws out a thermocouple 6, and the thermocouple 6 stretches into the heater 2, and the thermocouple is used for detecting whether the temperature of the heat conducting medium in the heater reaches the set temperature.
To further optimise the above technical solution, the position of the sample container 5 is selected according to the number of test samples; and the average temperature according to the rest of the thermocouple 6 test is taken as the actual temperature of the heat conducting medium.
Specific examples are:
the sample containers are numbered 5-1 to 5-5 in sequence from left to right, and the thermocouples are numbered 6-1 to 6-5 in sequence from left to right respectively.
When the number of the test samples is 1, placing the test samples in sample containers No. 5-3, taking down sample containers No. 5-1, 5-2, 5-4 and 5-5, and determining the average temperature of thermocouples 6-1,6-2,6-4 and 6-5 as the actual temperature of the heat conducting medium; when the number of the test samples is 2, placing the test samples in sample containers No. 5-2 and No. 5-4, taking down sample containers No. 5-1, no. 5-3 and No. 5-5, and determining the average temperatures of thermocouples 6-1,6-3 and 6-5 as the actual temperature of the heat conducting medium; when the number of the test samples is 3, placing the test samples in sample containers 5-2, 5-3 and 5-4, taking down sample containers 5-1 and 5-5, and determining the average temperature of thermocouples 6-1 and 6-5 as the actual temperature of the heat conducting medium; when the number of the test samples is 4, placing the test samples in sample containers 5-1, 5-2, 5-4 and 5-5, taking down sample containers 5-3, and determining the average temperature of the thermocouple 6-3 as the actual temperature of the heat conducting medium; the actual temperature of the heat conducting medium in the test process can be represented to the greatest extent, and the accuracy of the test result is greatly improved.
In addition, the embodiment of the invention also discloses a testing method of the calorimeter, which comprises the following steps:
selecting the position of the sample container according to the number of the test samples;
preparing a test sample, and standing the test sample at room temperature; the mass is preferably densely packed in the sample container.
According to the property of the test sample, determining a required test temperature range, further selecting a corresponding heat conducting medium, weighing, pouring into a heater, starting the heater, setting the temperature, and starting a data recording and calculating system;
the above steps are preliminary preparation work in the experimental process, and the order of the above steps is not specified as long as the work is done when the experiment is formally performed.
When the heat-conducting medium is heated to the set temperature, the heat-conducting medium is introduced into the heat-insulating sealed box 1, and when the temperature change in the heat-insulating sealed box 1 is stable (i.e. the temperature drops to be linear, as shown by a curve T in FIG. 3) 1 T 2 ) When the test sample is in a state of being placed in a sample container 5, a thermocouple 6 is inserted, the heat insulation sealing box 1 is closed, the data recording and calculating system 3 starts working, and data are recorded;
the data record calculating system 3 obtains experimental results according to the recorded data.
Specifically, according to the test purpose, the parameters to be calculated are selected in the data recording and calculating system, the thermocouple number for calculating the average temperature of the heat conducting medium is input in the data recording and calculating system, and the acquired thermocouple data for calculating the parameters of the test sample and the corresponding time point are combined to give the result. For testing the specific heat of the phase change material, the temperature corresponding to the selected time point should be higher than the phase change temperature thereof.
Referring to fig. 3, taking a group of examples, a comparative thermal calculation is described, where the formula of the calculation is given:
c: specific heat, kJ/(kg ℃ C.) c of sample 0 Specific heat of heat-conducting medium (known), kJ/(kg ℃ C.)
m 0 : mass of heat-conducting medium, kg m 1 Test sampleQuality of product, kg
T 3 Heat-conducting medium t 1 Theoretical temperature of moment, °c T 4 Heat-conducting medium t 2 Theoretical temperature of moment, DEG C
T 5 Heat-conducting medium t 1 Actual temperature at time, T 6 Heat-conducting medium t 2 Actual temperature at time, C
T 7 Sample t 1 Actual temperature at time, T 8 Sample t 2 Actual temperature at moment, DEG C;
if multiple groups of experiments are performed, multiple primary equations can be built in the same way. Wherein the theoretical temperature can be determined by T 1 T 2 The linear dashed line fitted out results.
Referring to fig. 3, regarding latent heat calculation, the formula is also given here:
h latent heat of sample, kJ/kg c 0 Specific heat of heat-conducting medium (known), kJ/(kg ℃ C.)
m 0 : mass of heat-conducting medium, kg m 1 Test sample mass, kg
T 9 Heat-conducting medium t 3 Theoretical temperature of moment, °c T 10 Heat-conducting medium t 3 Actual temperature at time, C
T 11 Sample t 3 Actual temperature at moment, DEG C; if multiple groups of experiments are performed, multiple primary equations can be built in the same way. Likewise, the theoretical temperature can be seen in the dashed line portion of the graph.
Calculation of glass transition temperature:
the glass transition temperature can be calculated by solving the specific heat over a continuous time and plotting it. The midpoint of the specific heat rise curve is the glass transition temperature.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A calorimeter, comprising: an insulated sealed box, a heater, and a data recording computing system; the bottom of the heat-insulating sealing box is provided with a plurality of knobs, and the knobs are used for fixing the sample containers; each sample container is provided with a thermocouple, and the thermocouple passes through the heat insulation sealing box and is connected with the data recording and calculating system;
the data record computing system is connected with the heater;
the heater is connected with the heat-insulating sealing box;
the heater is connected with the heat insulation sealing box through a pipeline, and an electromagnetic valve is arranged on the pipeline;
an opening for injecting a heat conducting medium is formed in the heater; the liquid level of the heat conducting medium introduced into the heat insulation sealing box is equal to the upper edge of the test container after the test container is placed in the heat insulation sealing box;
the data recording computing system is connected with a thermocouple, and the thermocouple stretches into the heater;
selecting a position of the sample container according to the number of test samples; and the average temperature according to the rest of thermocouple test is taken as the actual temperature of the heat conducting medium.
2. The calorimeter of claim 1, wherein the wall material of the heat-insulating sealed box is made of hollow hard plastic, a heat-insulating plate is adhered to the inner side of the heat-insulating sealed box, and heat-insulating anticorrosive paint is coated on the inner side of the heat-insulating plate.
3. The calorimeter of claim 2, wherein the insulation board is an extruded polystyrene foam board.
4. The calorimeter of claim 1, wherein a drain port is provided in the bottom of the heat-insulating sealed box.
5. A method of testing a calorimeter, wherein a calorimeter of any one of claims 1-4 is used, the method comprising the steps of: 1) Selecting the position of the sample container according to the number of the test samples;
2) Preparing a test sample, standing the test sample at room temperature, and balancing the temperature;
3) According to the property of the test sample, determining a required test temperature range, further selecting a corresponding heat conducting medium, weighing, pouring into a heater, starting the heater, setting the temperature, and starting a data recording and calculating system;
4) When the heat conducting medium is heated to a set temperature, the heat conducting medium is introduced into an adiabatic sealing box, when the temperature change in the adiabatic sealing box is stable, a test sample with known quality and stable state is placed into a sample container, a thermocouple is inserted, the adiabatic sealing box is closed, a data recording computing system starts to work, and data are recorded;
5) And obtaining an experimental result according to the data recorded by the data recording and calculating system.
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| US4439048A (en) * | 1978-05-15 | 1984-03-27 | The Dow Chemical Company | Accelerating rate calorimeter and method of operation |
| CN101251502A (en) * | 2008-04-09 | 2008-08-27 | 东华大学 | Apparatus and method for measuring textile heat conduction, thermal diffusivity and volumetric heat capacity |
| CN101470088A (en) * | 2007-12-28 | 2009-07-01 | 中国航天科技集团公司第五研究院第五一〇研究所 | Test method for low-temperature thermal conductivity of fluid |
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| CN101871902A (en) * | 2010-05-24 | 2010-10-27 | 北京科技大学 | Test device and test method for limit heat-flow density of porous material for heat pipe |
| CN102004119A (en) * | 2010-11-04 | 2011-04-06 | 西北工业大学 | Method for measuring combustion heat value of boron powder |
| CN209784235U (en) * | 2019-03-25 | 2019-12-13 | 中冶建筑研究总院有限公司 | Calorimeter |
-
2019
- 2019-03-25 CN CN201910228450.9A patent/CN109916948B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4439048A (en) * | 1978-05-15 | 1984-03-27 | The Dow Chemical Company | Accelerating rate calorimeter and method of operation |
| CN101470088A (en) * | 2007-12-28 | 2009-07-01 | 中国航天科技集团公司第五研究院第五一〇研究所 | Test method for low-temperature thermal conductivity of fluid |
| CN101251502A (en) * | 2008-04-09 | 2008-08-27 | 东华大学 | Apparatus and method for measuring textile heat conduction, thermal diffusivity and volumetric heat capacity |
| CN101839873A (en) * | 2010-04-23 | 2010-09-22 | 中国建筑材料科学研究总院 | Testing device and testing method for thermal performance of phase-change temperature regulation building material |
| CN101871902A (en) * | 2010-05-24 | 2010-10-27 | 北京科技大学 | Test device and test method for limit heat-flow density of porous material for heat pipe |
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| CN209784235U (en) * | 2019-03-25 | 2019-12-13 | 中冶建筑研究总院有限公司 | Calorimeter |
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