Enrichment-thermal desorption-chromatography separating unit

A chromatographic separation and separation device technology, which is applied in the field of gas sample rapid enrichment-thermal desorption-chromatographic separation device, can solve the problem of difficulty in taking into account analysis speed and separation efficiency, reducing the ability of a chromatographic column to resolve peaks, and the initial enrichment temperature. Long time and other problems, to achieve the effect of improving the thermal analysis speed, high temperature programming rate, and reducing the analysis cycle time

Inactive Publication Date: 2016-06-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] 1. Enrichment at room temperature has low enrichment efficiency for low boiling point components
[0006] 2. The heating rate of the heater is slow, the long-term desorption process and the transmission line of the thermal desorption component cause the peak broadening of the thermal desorption component, which reduces the resolution ability of the chromatographic column to the peak, making qualitative and quantitative difficulties
Therefore, commercialized devices all use secondary cold trap and secondary thermal analysis technology, which will lead to a long analysis period and increase the cost and complexity of the device
[0007] 3. After the thermal analysis is completed, the time for the high-temperature thermal analysis tube to cool naturally to the initial enrichment temperature is too long, resulting in a long analysis period, generally more than 10 minutes
[0008] 4. The analysis period of the conventional chromatographic analysis method is too long, generally more than 15 minutes, which is not conducive to rapid analysis; while ordinary fast gas chromatography is difficult to ensure sufficient analysis rate, resolution and peak capacity at the same time, resulting in difficulty in balancing analysis speed and separation efficiency

Method used

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  • Enrichment-thermal desorption-chromatography separating unit
  • Enrichment-thermal desorption-chromatography separating unit
  • Enrichment-thermal desorption-chromatography separating unit

Examples

Experimental program
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Embodiment 1

[0040] A kind of enrichment-thermal analysis-chromatographic separation device, such as figure 1 As shown, it consists of an enrichment thermal desorption device 100 , a sampling device 200 , a separation device 300 and a cooling source 104 .

[0041] The enrichment thermal desorption device 100 is composed of an adsorption tube 102 , a heating wire 103 , a first cooling cover 106 and a first cooling nozzle 105 . The adsorption tube 102 is a quartz tube with a main body diameter of 3 mm, which is filled with an adsorbent 101, which is a mixture of 5 mg of graphitized carbon black and 4 mg of Carbosieve SIII. The adsorption tube 102 is wound with a heating wire 103. The heating wire 103 is a Ni-Cr alloy with a wire diameter of 0.4 mm, a resistance of 10 ohms, and a heating rate of 40° C. / s. Both ends of the adsorption tube 102 are respectively connected to the sample source and the sampling device 200 ; the end of the adsorption tube 102 connected to the sampling device 200 ha...

Embodiment 2

[0049] The device as described in Embodiment 1, wherein the sampling device 200 is a three-way two-position solenoid valve.

Embodiment 3

[0051] The device as described in Example 1, wherein the adsorption tube 102 is a stainless steel tube with an inert inner wall, and the adsorbent 101 is 10 mg carbon molecular sieve TDX-1. The sampling device 200 and its connecting pipes are in room temperature environment. The device can realize rapid enrichment-thermal analysis-chromatographic separation of low-carbon hydrocarbons (such as ethane, ethylene, propane, etc.), and the entire analysis period is less than 2 minutes.

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Abstract

The invention provides an enrichment-thermal desorption-chromatography separating unit. The enrichment-thermal desorption-chromatography separating unit is composed of a rapid enrichment thermal desorption device, a sample introduction device, and a rapid separating device; the rapid enrichment thermal desorption device is used for realizing low temperature enrichment of target components in gas samples using an adsorption tube at the action of low temperature of carbon dioxide gas, and realizing rapid heating thermal desorption via a heating wire, wherein an adsorbent is arranged in the adsorption tube, and the adsorption tube is enwound by the heating wire; after enrichment and desorption, the target components are delivered into the rapid separating device via the sample introduction device; a low temperature carbon dioxide gas cooling chromatographic column is adopted in the rapid separating device, relatively low chromatographic column initial temperature and relatively high heating rate are achieved via combination of the low temperature carbon dioxide gas cooling chromatographic column with a rapid heating module, so that high separation effect, extremely high analysis speed, and high peak capacity are achieved. The enrichment-thermal desorption-chromatography separating unit is capable of realizing on-line enrichment, rapid desorption, and super rapid gas chromatography of trace components in gas samples.

Description

technical field [0001] The invention belongs to the field of analytical instruments, in particular to a gas sample rapid enrichment-thermal analysis-chromatographic separation device. Background technique [0002] The analysis of trace substances in gas samples is an important part of analytical chemistry and environmental analysis. Its main application fields include: 1) Monitoring of volatile organic compounds (Volatile Organic Compounds, referred to as VOCs) in the air; VOCs in the air are harmful to human health, and lead to photochemical pollution and odor problems, so online and fast , Highly sensitive detection is of great significance. 2) The detection of trace volatile organic compounds in exhaled breath has great guiding significance for early detection, early diagnosis and screening of diseases. 3) On-line detection of hazardous compounds in the working environment, which is an important guarantee for safe production. [0003] Due to the complex composition, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/16
Inventor 关亚风张杨刚吴大朋刘洪鹏孟虎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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