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Quantitative detecting method of trace amount phosphine gas and enriching apparatus thereof

A phosphine, nitrogen and phosphorus detector technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of easy qualitative and quantitative, less miscellaneous peaks, and short peak time

Inactive Publication Date: 2008-10-08
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the defects of various existing analysis methods, the present invention provides a method capable of accurately and quickly measuring trace amounts of phosphine gas in the natural environment. The present invention refits the detection equipment online by designing the detection process, and adopts a secondary online The rapid enrichment of cold trap combined with gas chromatography-NPD method realizes the rapid enrichment and accurate measurement of phosphine on-line temperature control

Method used

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  • Quantitative detecting method of trace amount phosphine gas and enriching apparatus thereof
  • Quantitative detecting method of trace amount phosphine gas and enriching apparatus thereof
  • Quantitative detecting method of trace amount phosphine gas and enriching apparatus thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The method was used to determine the concentration of phosphine in air samples collected from a paddy field in Yangzhou City, Jiangsu Province.

[0041] A. Preparation of gas samples to be tested

[0042] A certain amount of atmospheric samples were collected before sunlight exposure. After the samples were collected, they were stored away from light in a sealed air bag (the inner layer was Tedlar, and the outer layer was light-proof aluminum foil) that did not absorb and absorb gases, and the analysis was completed within one week. .

[0043] B. The cooling and enrichment of phosphine gas and the establishment of GC / NPD detection device

[0044] Phosphine gas cooling enrichment and GC / NPD detection device as attached figure 1 shown.

[0045] Test and enrichment device: Agilent 4890D gas chromatograph 8, nitrogen and phosphorus detector (NPD), PLOTQ capillary column as chromatographic column 7 (25m×0.32mm) and cold trap (1.2m×0.53mm, No. 1 cold trap column 9 0.8m * ...

Embodiment 2

[0070] Atmospheric samples collected from swamps were used to determine the concentration of phosphine by this method.

[0071] A. The preparation of the gas sample to be measured is the same as in Example 1.

[0072] B. The cooling and enrichment of phosphine gas and the establishment of GC / NPD detection device

[0073] Phosphine gas cooling enrichment and GC / NPD detection device as attached figure 1 shown.

[0074] Test and enrichment device: Agilent 4890D gas chromatograph, nitrogen and phosphorus detector (NPD), Crosslinked 5% PhMe Silicone capillary column as chromatographic column (25m×0.32mm), Al 2 o 3 / Na 2 SO 4 Capillary column as cold trap column (0.8m×0.53mm, No. 1 cold trap; 0.6m×0.32mm, No. 2 cold trap), solid NaOH particle preparation adsorbed on porous carrier as pre-drying absorbent, six-way sample injection Valve, two 2L thermos cups (as a cold trap), liquid nitrogen for cooling, and lifting platform.

[0075] Chromatographic conditions: column temperat...

Embodiment 3

[0085] The sludge and biogas samples collected from the sewage treatment plant were determined by this method for the concentration of phosphine.

[0086] A. Preparation of gas samples to be tested The collection of biogas samples is the same as in Example 1, and the gas samples released from the sludge samples after alkali digestion are injected.

[0087] B. The cooling and enrichment of phosphine gas and the establishment of GC / NPD detection device

[0088] Phosphine gas cooling enrichment and GC / NPD detection device as attached figure 1 shown.

[0089] Test and enrichment device: Agilent 4890D gas chromatograph, nitrogen and phosphorus detector (NPD), PLOT-Al 2 o 3 / Na 2 SO 4 Capillary column as chromatographic column (25m×0.32mm), PLOT-Q capillary column as cold trap column (1.0m×0.53mm, No. 1 cold trap; 0.6m×0.32mm, No. 2 cold trap), adsorbed on the porous carrier The solid NaOH granular preparation is used as a pre-drying absorbent, a six-way sampling valve, two 2L...

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Abstract

The invention discloses a quantitative detecting method and a gathering device for measuring phosphine gas. The gathering device comprises a sampler, the sampler is connected with a cold trap column through a six-way valve, a first cold trap column is connected with a second cold trap column, the cold trap column is communicated with a chromatographic column. The detecting method is that the gas which is released after the sorption state phosphine is cleared up in a fixed method, then sampling according to a fixed operation, the sampling gas which is eliminated the acid gases and vapor through a NaOH absorption tube is entered into the gas chromatograph after gathering and removing impurities through the switching of the six-way valve in the two front column cold trap, reading the response signal of the nitrogen-phosphorus detector to integral, at last work out the concentration of the phosphine in the practical sample through comparing the area of the peak area of the sample and the phosphine standard gas chromatography. The invention has high sensitivity and low detecting limit, the time of appearing peak in gas chromatography is short, and the peak shape is distinctness, which is easy to determine the nature and the quantity and makes the detection rapid and simple.

Description

technical field [0001] The invention relates to a quantitative detection method and enrichment device for trace phosphine gas in natural environment. Background technique [0002] Phosphorus is one of the most important elements in the earth's crust, and it participates in or controls many biogeochemical cycle processes that occur in the biosphere. Due to the difficulty in the reduction process of phosphate and the difficulty in the analysis and quantification of trace phosphine, in the past, the study of the biogeochemical cycle of phosphorus was limited to two forms, solid and liquid, and gaseous phosphine (PH 3 ) does not exist in nature. With the development of analytical technology, phosphine in the environment has been detected one after another, and phosphine is finally confirmed as a trace gas ubiquitous in the environment, which is adsorbed in a free-gaseous phosphine and matrix State (matrix-bound phosphine) form exists in the environment. Phosphine is the carri...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/02
Inventor 耿金菊王晓蓉牛晓君韩圣慧丁丽丽任洪强洪宇宁
Owner NANJING UNIV
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