Secondary cold trap enrichment and GC-FID (Gas Chromatography-Flame Ionization Detector) combining device and method for detecting trace hydrogen phosphide

A GC-FID and secondary cold trap technology, applied in the field of phosphine detection, can solve the problems of low phosphine content and late start of phosphine research, achieve economical price, reduce operation difficulty and economic cost, and operate convenient effect

Inactive Publication Date: 2014-08-27
SOUTH CHINA UNIV OF TECH
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  • Claims
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Problems solved by technology

[0004] The content of phosphine in the natural environment is very low, and it can hardly be detected by the molybdenum blue colorimetric metho

Method used

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  • Secondary cold trap enrichment and GC-FID (Gas Chromatography-Flame Ionization Detector) combining device and method for detecting trace hydrogen phosphide
  • Secondary cold trap enrichment and GC-FID (Gas Chromatography-Flame Ionization Detector) combining device and method for detecting trace hydrogen phosphide
  • Secondary cold trap enrichment and GC-FID (Gas Chromatography-Flame Ionization Detector) combining device and method for detecting trace hydrogen phosphide

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Embodiment 1

[0020] Such as figure 1 As shown, a kind of secondary cold trap enrichment combined with GC-FID device for detecting trace amounts of phosphine in this embodiment includes a cold trap secondary enrichment system and a GC-FID analysis system. The trap secondary enrichment system is composed of a sample sampling device 1, a six-way valve 2, a primary cold trap 3 and a secondary cold trap 4, and a temperature online detector 5 is set in the primary cold trap and the secondary cold trap; the GC- The FID analysis system consists of a gas phase sampler 6, a chromatographic column 7, a flame ionization detector (FID) 8 and a carrier gas system 9 of the GC-FID analysis system. Sample injection device, port ② is the exhaust gas discharge port, port ③ is connected to the inlet of the secondary cold trap, port ④ is connected to the carrier gas system of the GC-FID analysis system, port ⑤ is connected to the outlet of the primary cold trap, port ⑥ The inlet of the primary cold trap is co...

Embodiment 2

[0024] A secondary cold trap enrichment and GC-FID combined device for detecting trace amounts of phosphine in this embodiment includes a cold trap secondary enrichment system and a GC-FID analysis system, and the cold trap secondary enrichment The system consists of a sample sampling device, a six-way valve, a primary cold trap and a secondary cold trap. A Pt100 thermal resistance temperature detector is installed in the primary cold trap and the secondary cold trap. The length of the primary cold trap and the secondary cold trap is 100cm , 0.53mm in diameter, filled with Al 2 o 3 -Na 2 SO 4 The enrichment capillary column and the cold trap cup are composed of the capillary column placed in the cold trap cup, liquid nitrogen is poured into the cold trap cup, the cold trap cup is placed on the lifting platform, and the liquid nitrogen liquid in the cold trap cup is adjusted by the lifting platform The distance between the surface and the capillary column is used to realize ...

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Abstract

The invention belongs to the technical field of detection of hydrogen phosphide and discloses secondary cold trap enrichment and GC-FID (Gas Chromatography-Flame Ionization Detector) combining device and method for detecting trace hydrogen phosphide. A gas loading system of the secondary cold trap enrichment and GC-FID combining device is connected with a six-way valve of a cold trap secondary enrichment system; an outlet of a secondary cold trap is connected to a gas-phase sample feeding device of a GC-FID analyzing system through a capillary tube. The detection conditions of a method for detecting the trace hydrogen phosphide by using the combining device are as follows: the gas loading flow is 1.5mL/min; the trap enrichment temperature is -90 DEG C; the chromatographic column separation temperature is 90 DEG C; the temperature of a flame ionization detector is 220 DEG C. The device and the method disclosed by the invention are used for detecting the trace hydrogen phosphide and have the advantages of good repeatability and stability and high detection precision.

Description

technical field [0001] The invention belongs to the technical field of phosphine detection, and in particular relates to a secondary cold trap enrichment and GC-FID combined device and method for detecting trace phosphine. Background technique [0002] Phosphine (PH 3 ) is an important reduced form of phosphorus in the natural environment, and this view has been generally accepted. Since Devai et al first detected the presence of phosphine in the volatiles of sewage plants in 1988, more and more researchers have participated in the research of phosphine related fields. The study of phosphine not only has important geochemical significance for understanding the cycle of phosphorus in nature, but also provides a new solution direction for the increasingly serious problem of water eutrophication. [0003] Phosphine quantitative and qualitative analysis methods mainly include molybdenum blue colorimetry and gas chromatography. The former is complicated to operate, takes a lon...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/32
Inventor 牛晓君魏爱书
Owner SOUTH CHINA UNIV OF TECH
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