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Gradient cracking method for researching compound cracking process

A compound and compound technology, applied in the field of compound analysis, can solve problems such as complex products, unfavorable compound cracking process, etc.

Active Publication Date: 2012-02-01
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pyrolysis products at higher temperatures often include the pyrolysis products at previous temperatures, and the products are complex, which is not conducive to the study of the pyrolysis process of compounds

Method used

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  • Gradient cracking method for researching compound cracking process
  • Gradient cracking method for researching compound cracking process
  • Gradient cracking method for researching compound cracking process

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] Example 1 Cracking of chlorogenic acid

[0022] Weigh about 10 mg of chlorogenic acid (purity >99%) into an alumina crucible, and raise the temperature from 30 °C to 900 °C at a heating rate of 5 °C / min under a nitrogen flow rate of 40 mL / min. The thermogravimetric analyzer records the weight loss curve of chlorogenic acid, and after a differential, the differential thermogravimetric curve is obtained. like figure 1 Shown:

[0023] It can be seen from the weight loss curve and differential thermogravimetric curve that the cracking of chlorogenic acid can be divided into five stages. The first stage is 30-120°C; the second stage is 120-190°C; the third stage is 190-260°C; the fourth stage is 260-500°C; the fifth stage is 500-900°C.

[0024] Weigh about 2 mg of sample into the quartz sample tube of the pyrolysis device, and perform isothermal cracking at 120, 190, 260, 500, and 900° C. for 20 minutes at each temperature point. Here, choosing the highest temperature ...

example 2

[0029] Example 2 Cracking of quinic acid

[0030] Weigh about 10 mg of quinic acid (purity >99%) into an alumina crucible, and raise the temperature from 30 °C to 900 °C at a heating rate of 5 °C / min under a nitrogen flow rate of 40 mL / min. The thermogravimetric analyzer records the weight loss curve of chlorogenic acid, and after a differential, the differential thermogravimetric curve is obtained. like image 3 Shown:

[0031] It can be seen from the weight loss curve and differential thermogravimetric curve that the cracking of chlorogenic acid can be divided into four stages. The first stage is 30-150°C; the second stage is 150-220°C; the third stage is 220-400°C; the fourth stage is 400-900°C.

[0032] Weigh about 2 mg of sample into the quartz sample tube of the pyrolysis device, and perform isothermal cracking at 150, 220, 400, and 900° C. for 20 minutes at each temperature point. The cleavage products of each stage were separated and analyzed by GC / MS.

[0033] ...

example 3

[0037] Cracking of example 3 rutin

[0038] Weigh about 10 mg of rutin (purity >98%) into an alumina crucible, and raise the temperature from 30 °C to 900 °C at a heating rate of 5 °C / min under a nitrogen flow rate of 40 mL / min. The thermogravimetric analyzer records the weight loss curve of chlorogenic acid, and after a differential, the differential thermogravimetric curve is obtained. like Figure 5 Shown:

[0039] It can be seen from the weight loss curve and differential thermogravimetric curve that the cracking of rutin can be divided into four stages. The first stage is 30-180°C; the second stage is 180-366°C; the third stage is 366-600°C; the fourth stage is 600-900°C.

[0040] Weigh about 2 mg of sample into the quartz sample tube of the pyrolysis device, and perform isothermal cracking at 180, 366, 600, and 900° C. for 20 minutes at each temperature point. The cleavage products of each stage were separated and analyzed by GC / MS.

[0041] GC / MS conditions:

[...

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Abstract

The invention relates to a gradient cracking method for researching a compound cracking process, which is characterized by comprising the following steps of: firstly, carrying out thermogravimetric analysis on a compound, and determining the main cracking stage of the compound according to a thermogravimetric curve and a thermogravimetric differential curve; then carrying out segmented cracking on the compound, and analyzing by using a gas chromatography-mass spectrometry to obtain the cracking process of each cracking stage of the target compound. The invention has the advantages that different cracking stages are distinguished, the gradient cracking is carried out by stages, and the cracking products at each stage are analyzed and researched, thereby avoiding the problem that the cracking process of the compound is difficult to analyze because the products at each cracking stage are mixed in the current common cracking method.

Description

technical field [0001] The invention relates to a compound analysis method, in particular to a gradient cracking method for studying the cracking process of a compound. The method first uses thermogravimetric analysis to identify the main reaction stages in the cracking process of the compound. Secondly, pyrolysis-gas chromatography-mass spectrometry (Py-GC / MS) was used to crack the compound step by step, and the cracking products of each stage were analyzed to realize the whole process analysis of the compound cracking process. Background technique [0002] Pyrolysis technology is a method that uses the thermal instability of materials to decompose materials through thermochemical action. Thermal cracking can simulate the actual combustion cracking process, and is widely used in the research of biomass cracking, cigarette smoking process, polymer cracking, etc. It can not only be used to study the composition of cracking products, cracking behavior rules, and predict combu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N5/04G01N30/02
Inventor 郭吉兆宛克花谢复炜张晓兵王洪波
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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