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A pulse heating and in-situ technology, applied in the field of analytical instruments, can solve problems such as reaction process distortion and detection distortion, and achieve high integration, minimized secondary reactions, and high performance
Pending Publication Date: 2022-06-24
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI +1
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Problems solved by technology
[0004] In view of the distortion of the reaction process caused by the slow temperature rise of the thermogravimetric unit in the current TG-MS coupling and the detection distortion caused by the secondary reaction of the product in the traditional sampling process, the purpose of the present invention is to develop a general pulse temperature rise wide range thermogravimetric and In situ gas sampling technology, research on new in situ sampler, optimization of coupling technology and combination of pulse heating thermogravimetry and gas analyzer
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[0032] It should be noted that the terms "first", "second" and the like in the description and claims of the present invention and the above drawings are used to distinguish similar objects, and are not necessarily used to describe a specific sequence or sequence. It is to be understood that the data so used may be interchanged under appropriate circumstances such that the embodiments of the invention described herein can be practiced in sequences other than those illustrated or described herein. In addition, the terms "comprising" and "having" and any variations thereof in the embodiments of the present invention are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to Those steps or elements that are expressly listed may instead include other steps or elements that are not expressly listed or are inherent to the process, method, product or apparatus.
[0033] I...
Embodiment 1
[0047] 1) Place the equipment on the test bench with a flat and level surface, and adjust the bottom adjusting stud to make the balance in a horizontal state.
[0048] 2) Turn on the regulated power supply, workstation, gas flow meter, and computer host in turn, and open the nitrogen bottle to make the pressure 0.5MP.
[0049] 3) Open the lifting device controlled by the data analysis unit 17 , take out the clean sample holder 6 and insert it vertically into the circular support frame channel from top to bottom, and place the clean empty sample crucible 7 on the sample holder 6 .
[0050] 4) Control the lifting device to open and close the furnace through the data analysis unit 17, adjust zero on the operation interface, and deduct the weight of the empty crucible.
[0051] 5) Write the reaction heating program, start the balance, and carry out the blank experiment.
[0052] 6) Weigh 30mg-50mg calcium oxalate with an electronic analytical balance.
[0053] 7) After the blank...
Embodiment 2
[0056] Replace the experimental sample with coal tar and repeat the relevant steps of Example 1.
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Abstract
The invention discloses pulse heating coupled in-situ sampling thermogravimetric-mass spectrometry equipment, which relates to the technical field of analytical instruments and comprises a mass measuring unit, a heating unit, an atmosphere adjusting unit, an in-situ sampling unit, a temperature control unit and a data analysis unit, the invention relates to a thermogravimetric mass spectrometer which realizes rapid temperature rise and control and undistorted capture of gas by using pulse temperature rise and high-temperature in-situ sampling technologies, and is used for more accurately measuring the relationship between the mass and the temperature of a substance. Wherein the heating unit realizes rapid heating and temperature control in a carbon thermal shock mode; the in-situ sampling unit realizes gas in-situ capture by a high-temperature in-situ sampler. The temperature rise rate of the thermogravimetry-mass spectrometry combined equipment can reach 105 K / s, rapid temperature rise and control and high-precision in-situ sampling can be achieved under the action of a high-temperature in-situ sampler, the application range of existing thermogravimetry is widened, and the thermogravimetry-mass spectrometry combined equipment has wide application and popularization prospects.
Description
technical field [0001] The invention relates to the technical field of analytical instruments, in particular to a pulsed temperature rise coupled in-situ sampling thermogravimetric-mass spectrometry equipment. Background technique [0002] Thermogravimetric mass spectrometry (TG-MS) consists of a thermogravimetric analyzer and a mass spectrometer. Among them, thermogravimetric analysis is a thermal analysis technique that uses a thermobalance to measure the relationship between mass and temperature under program-controlled temperature. It has the advantages of simple and rapid instrument operation, high sensitivity, and micro-quantification of samples. Mass spectrometry is to ionize and separate substances according to the mass-to-mix ratio of the examples, and then identify the composition of volatile substances by measuring the intensities of various ion spectrum peaks. components, and can be detected online. Thermogravimetric analysis combined with mass spectrometry tec...
Claims
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Application Information
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04G01N30/72
CPCG01N5/04G01N30/72
Inventor 袁浩然李德念赵悦张军阳济章陈勇
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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