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Thermal analyzer for material pyrolysis behavior and flowing carrier gas-single-drop microextraction combined device and using method thereof

A thermal analyzer and material technology, which is applied in thermal analysis of materials, measuring devices, and analytical materials, etc., can solve the problems of difficulty in collecting escaping components from thermal analyzers, and difficulty in qualitative and semi-quantitative analysis of mixtures for escaping components. To achieve the effect of good extraction effect, convenient operation and simple device

Active Publication Date: 2011-05-04
HONGTA TOBACCO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is also to overcome the problem of qualitative and semi-quantitative difficulty in analyzing the mixture of escaped components of existing thermal analyzers, and combine the escaped components extracted by single droplet microextraction with gas chromatography, liquid chromatography and other gas analysis methods Separation analysis identification for detailed characterization of the pyrolysis behavior of substances
[0005] The purpose of the present invention is to overcome the problem of difficulty in collecting the escaped components of existing thermal analyzers, and provide a combined device for thermal analyzers and flowing carrier gas-single droplet micro-extraction

Method used

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  • Thermal analyzer for material pyrolysis behavior and flowing carrier gas-single-drop microextraction combined device and using method thereof
  • Thermal analyzer for material pyrolysis behavior and flowing carrier gas-single-drop microextraction combined device and using method thereof
  • Thermal analyzer for material pyrolysis behavior and flowing carrier gas-single-drop microextraction combined device and using method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Using thermogravimetry-flowing carrier gas-single droplet microextraction device combined with gas chromatography-mass spectrometry to analyze the pyrolysis behavior of lutein

[0045] 1. Before the experiment, keep the thermogravimetric in the air atmosphere at 600°C for 10 minutes to remove impurities in the furnace. Accurately weigh 5.00±0.05mg of lutein and put it into a thermogravimetric platinum crucible. The heating program is The sensitivity of the thermobalance is 1 μg, the temperature control range of the furnace body is from room temperature to 1000 ° C, the carrier gas is air, the empty crucible is used as a reference object, and the flow rate of the carrier gas is 400 mL / min.

[0046] 2. The obtained thermal analysis data are as follows: figure 2 , combined with the thermogravimetric analysis data, the whole pyrolysis process is divided into 16 continuous temperature segments according to the temperature difference, using such as figure 1 Th...

Embodiment 2

[0050] Example 2: Using thermogravimetry-flowing carrier gas-single droplet microextraction device combined with gas chromatography-mass spectrometry to analyze the pyrolysis behavior of caffeic acid

[0051] 1. Accurately weigh 10.0±0.05mg of caffeic acid sample into a thermogravimetric platinum crucible. The analysis conditions are: the heating program is (keep for 10 minutes). The carrier gas is high-purity nitrogen with a flow rate of 400 mL / min.

[0052] 2. The obtained thermal analysis data are as follows: Figure 5 , caffeic acid begins to lose mass at 160°C and ends at 360°C. The temperature range from 160°C to 360°C is evenly divided into 10 continuous temperature segments, and 10 extraction samples are obtained. , combined with thermogravimetric analysis data, using such as figure 1 The shown thermal analyzer and flowing carrier gas-single droplet micro-extraction device extract caffeic acid release products step by step.

[0053] 3. Select ethanol as the extra...

Embodiment 3

[0055] Example 3: Analysis of formaldehyde produced by glucose pyrolysis using thermogravimetry-flowing carrier gas-single droplet microextraction combined device

[0056] 1. Accurately weigh 10.0±0.05mg of glucose sample into a thermogravimetric platinum crucible. The analysis conditions are: (keep for 10 minutes). The carrier gas is air with a flow rate of 200mL / min.

[0057] 2. The obtained thermal analysis data are as follows: Figure 7 , combined with thermogravimetric analysis data, the entire glucose pyrolysis process was performed from 200 °C to 500 °C for single droplet microextraction.

[0058] 3. Select the reaction solvent with formaldehyde characteristics: 2,4-dinitrophenylhydrazine derivatization reagent is used as the extraction solvent, and the droplet volume is kept at about 10 μL. The result of 4min extraction and sampling under the condition of thermogravimetric without adding sample was used as the blank control sample.

[0059] 4. The obtained extr...

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Abstract

The invention discloses a thermal analyzer and flowing carrier gas-single-drop microextraction combined device and a using method thereof. A material is thermally decomposed to release a gas in a thermal analyzer, the component gas passes through a metal adapter, is vertically discharged upwards through an air vent at the upper end of an adapter under the driving of flowing carrier gas, and is extracted by single drop above the air vent, and escaping components are enriched and concentrated during extraction. The invention has the characteristics that: 1, sample pretreatment technology of single-drop microextraction integrating rapidness, efficiency, low cost and low solvent consumption is applied to analysis of the escaping components of the thermal analyzer under the driving of the carrier gas; 2, the sample pretreatment is performed by the combined device, and by combining other analyzers, giving the information of the escaping components of the thermal analyzer and combining thermal analysis data, material thermal degradation can be comprehensively characterized; and 3, the thermal analyzer and flowing carrier gas-single-drop microextraction combined device has good extractioneffect, and is simple, convenient to operate, and conveniently combined with the other analyzers.

Description

technical field [0001] The invention belongs to the field of pretreatment of analytical chemical samples, and in particular relates to a thermal analyzer and a flow carrier gas-single droplet microextraction combined device and method for analyzing thermal analysis data in the pyrolysis process of substances and combining the extraction, condensation, and extraction of escaped products. Enrichment, concentration. Background technique [0002] Thermal analysis technology is a type of technology that measures the relationship between the physical properties of a substance and the temperature at a programmed temperature. These physical properties include mass, temperature difference, expansion coefficient, magnetic force, etc. Such techniques are important detection tools in material development and quality control. With the advancement of technology, it is necessary to combine thermal analyzers with other analytical instruments to analyze the escaped components, and combine ...

Claims

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Application Information

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IPC IPC(8): G01N25/00G01N30/08
Inventor 杨柳杨继吴亿勤孟昭宇朱文辉高韬
Owner HONGTA TOBACCO GRP
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