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Gravitational thermal analysis method and device for heating sample by microwave

A technology of thermogravimetric analysis and microwave heating furnace, which is applied in the preparation of test samples and weighing by removing certain components, which can solve the problems of small sample usage, unsatisfactory heating methods, and small thermal conductivity. , to achieve the effect of convenient installation and maintenance, solving temperature measurement problems, and accurate measurement

Inactive Publication Date: 2009-03-11
SHANDONG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

At the same time, for larger materials, especially porous media containing a large amount of aggregates and pores, the thermal conductivity is very small, and conventional heating methods cannot meet the requirements, and the amount of samples used is too small to represent the actual situation well. , the traditional thermogravimetric analysis method cannot meet the above requirements

Method used

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  • Gravitational thermal analysis method and device for heating sample by microwave
  • Gravitational thermal analysis method and device for heating sample by microwave

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Effect test

Embodiment 1

[0021] Embodiment 1: This method heats the sample with microwaves, and the microwave input power is continuously adjustable between 0-3KW. The microwave input power can be set to a fixed value, or it can be set to be linked with the temperature measurement system; The stainless steel wall is condensed, and a heating resistance wire is installed outside the stainless steel furnace wall to maintain the temperature of the stainless steel wall between 350-400°C. The quality of the sample is measured online with a mass sensor; the weighing range of the mass sensor is 0-300g, and the resolution is 0.01g. The position of the quartz hanging basket in the furnace can be realized by changing the length of the heat-resistant wire, and samples with a diameter of <40mm can be placed. The temperature of the sample is measured online with an infrared thermometer or a thermocouple; the heating atmosphere is an air atmosphere, and the required gas is stored in a gas cylinder 26 . Different ga...

Embodiment 2

[0029] Embodiment 2: method and device are identical with embodiment 1, and difference is, carry out thermogravimetric analysis to different sample, need to adjust the heating atmosphere in furnace 36, be further explanation with heating atmosphere as oxygen atmosphere below: adjust oxygen cylinder Pipeline flowmeter 24 reaches the maximum opening, open the switch of oxygen cylinder 26, adjust the regulating valve 25 to the appropriate opening, flush the furnace for about 5 minutes, and after the air in the furnace is exhausted, adjust the regulating valve 25 so that the flowmeter 24 reads to The flow rate required for heating is sufficient, and the heating atmosphere is adjusted.

[0030] A thermocouple 4 is installed on the furnace wall at the lower part of the furnace 36 to measure the atmosphere temperature and display it through the atmosphere temperature display 18 . The heating atmosphere and flow in the furnace 36 are prepared and regulated through the air inlet 3, the...

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Abstract

The invention discloses a microwave thermogravimetric analysis (TGA) method and a device, wherein, the device comprises four parts, namely, a microwave oven, a mass measurement system, a temperature measurement system and an atmosphere adjustment system. The microwave input power can be set to a fixed value and also can set to be linked with the temperature measurement system. The mass measurement system monitors the mass variation of a test sample in real time; the temperature measurement system utilizes an infrared thermometer and a thermocouple to monitor the temperature of the test sample and the hearth in real time. The atmosphere heating can be achieved by the atmosphere adjustment system and the heating atmosphere can be air atmosphere, inert atmosphere, oxidizing atmosphere or reducing atmosphere. The device provided by the invention has the advantages of simple structure, high degree of automation and convenient operation, the invention can obtain the relation among mass, time / mass, and temperature of multiple test samples under different atmospheres in the process of microwave heating, and realizes microwave thermogravimetric analysis of the test samples with larger mass or volume.

Description

technical field [0001] The invention relates to a thermogravimetric analysis method and a device for thermogravimetric analysis using the method. Background technique [0002] Thermogravimetric analysis is an important method to study material properties and reaction laws. At present, thermogravimetric analysis usually uses a small amount of sample, and heats the sample by electric heating, which is an external heating method; uses a thermocouple to measure the temperature of the atmosphere around the sample to represent the temperature of the sample, and studies the temperature of the sample at a specific temperature. Or mass-time relationship or mass-temperature relationship under temperature programming. Since the amount of sample used is very small, and the temperature of the atmosphere around the sample is used instead of the sample temperature, it is questionable whether the conclusions obtained are applicable to the actual situation. [0003] Microwave heating has t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04G01N1/44
Inventor 马春元赵希强宋占龙王涛李龙之
Owner SHANDONG UNIV
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