Infrared oven and GC-MS based method and infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes

An analysis method and infrared furnace technology, applied in the field of on-line analysis, can solve the problem of inability to use a large sample volume and so on

Inactive Publication Date: 2010-04-07
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method and device for on-line analysis of simulated smoking and smoking of cigarettes based on infrared furnace and GC-MS in view of the above-mentioned shortcomings that the existing pyrolysis on-line analysis technology cannot use a large sample amount

Method used

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  • Infrared oven and GC-MS based method and infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes
  • Infrared oven and GC-MS based method and infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes
  • Infrared oven and GC-MS based method and infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh a certain amount (0.1 to 2 grams) of shredded cigarette tobacco sample, put it into the quartz tube of the focusing infrared furnace, set the sample heating program of the temperature program controller (room temperature to 1000 ° C), adjust the flow rate of the carrier gas (nitrogen 0 ~ 500mL / min, oxygen 0~500mL / min), start to heat up; when the set sampling stage is reached, change the six-way valve to the sampling state, after the sampling is completed, change the six-way valve to the sampling state; Nitrogen cooling down to -100°C to -20°C; during sample injection, the temperature of the PTV inlet can be set to a temperature rise program to allow the sample to enter the GC / MS for analysis.

[0025] GC / MS measurement conditions:

[0026] Injection port temperature: 280°C; ionization method: EI; ion source temperature: 230°C; transfer line temperature: 280°C; split ratio: 10:1~100:1; carrier gas: helium, constant flow rate 0.8~1.5mL / min; chromatographic column...

Embodiment 2

[0029] Weigh 0.5g of cigarette shredded tobacco sample, put it into the quartz tube of the focusing infrared furnace, set the sample heating program of the temperature programming controller: the initial temperature is 200°C, stay for 5 minutes, raise the temperature to 800°C at 10°C / s, and adjust the flow rate of the carrier gas (nitrogen 200mL / min, oxygen 50mL / min), start to heat up. When the temperature in the infrared furnace reaches 300 degrees, change the six-way valve to the sampling state, and when it reaches 400 degrees, change the six-way valve to the sampling state; the PTV sample inlet should be cooled to -60°C with liquid nitrogen in the sampling state; , the temperature of the PTV injection port was raised to 280 degrees at 10 °C / min, and the sample entered the GC / MS for analysis.

[0030] GC / MS measurement conditions:

[0031] Inlet temperature: 280°C; ionization mode: EI; ion source temperature: 230°C; transfer line temperature: 280°C; split ratio: 30:1; carri...

example 3

[0034] Weigh 2 grams of cigarette shredded tobacco sample, put it into the quartz tube (quartz boat) of the focusing infrared furnace, adjust the carrier gas flow rate (nitrogen 500mL / min, oxygen 50mL / min), set the sample heating program of the temperature program controller: initial temperature 100°C, stay for 5 minutes, raise the temperature to 1000°C at 50°C / sec, and start to heat up. When the temperature in the infrared furnace reaches 700 degrees, change the six-way valve to the sampling state, and change the six-way valve to the sampling state when it reaches 900 degrees. The PTV inlet was cooled to -150°C with liquid nitrogen in the sampling state. During sample injection, the temperature of the PTV injection port is raised to 280°C at 720°C / min, and the sample enters the GC / MS for analysis.

[0035] GC / MS measurement conditions:

[0036]Inlet temperature: 280°C; ionization mode: EI; ion source temperature: 230°C; transfer line temperature: 280°C; split ratio: 200:1; ...

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Abstract

The invention provides an infrared oven and GC-MS based method and an infrared oven and GC-MS based device for on-line analysis of simulated combustion of cigarettes and is characterized in that the method comprises: a cigarette sample is put under a condition of inert gas or synthetic air to realize the control of the oxygen content in the cracking atmosphere by using a gas flowmeter; a focused infrared oven is used as a heating device for cracking cigarette, and under the control of a programmable temperature rise controller, the infrared oven can control the temperature change in the simulating process, realize quick temperature rise cracking of the gram-class cigarette samples and simulate temperature rise conditions of the combustion of cigarettes; the cracking products obtained at different time periods can be selectively delivered to a PTV sample injection opening by a six-way valve and condensed and enriched by liquid nitrogen, the enriched cracking products are separated by the gas chromatography GC and then delivered to the mass spectrometry for quantitative and qualitative analysis; and by simulating the conditions of the combustion of cigarettes, the cracking experiments of the gram-class cigarette samples at different temperature-rise speeds and with different oxygen contents are carried out.

Description

technical field [0001] The invention relates to an on-line analysis method and device which connect a focused infrared furnace, a six-way valve and a gas chromatography-mass spectrometry instrument. The device can realize pyrolysis of gram-level tobacco samples, simulate cigarette smoking conditions, and online gas chromatography-mass spectrometry analysis of smoking products. Background technique [0002] Cigarette smoke is mainly produced by distillation and pyrolysis of tobacco and its additives during the smoking process of cigarettes. Therefore, using pyrolysis technology to crack cigarette samples, simulate the smoking process of cigarettes, and analyze and evaluate the cracked products produced is a widely used experimental method for evaluating the source of smoke components and flavor transfer. The on-line pyrolysis analysis devices used in previous literatures are mainly commercial thermal crackers and gas chromatography-mass spectrometry. The heating rate of the...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/20G01N30/72G01N1/44
Inventor 郭吉兆张晓兵王洪波赵阁颜权平胡斌刘绍锋谢复炜
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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