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Method for detecting trace phosphine gas in water sample by gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method

A gas chromatography, phosphine technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of high detection limit, detection limit fails to meet the requirements of trace phosphine detection, phosphine gas collection, storage and The enrichment technology has not yet passed the test and other problems, achieving the effect of obvious peak shape, short peak time and convenient analysis

Inactive Publication Date: 2012-03-28
NANJING UNIV
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Problems solved by technology

[0006] However, due to the low content of phosphine in the natural environment, the detection limit of conventional methods is too high. At the same time, the collection, storage and enrichment technology of phosphine gas has not yet passed the test. Quantitative determination of phosphine
The domestic determination of phosphine mainly adopts molybdate colorimetry, gas chromatography and Fourier transform infrared analyzer. The detectors used are different, but the detection limit cannot meet the detection requirements of trace phosphine.
[0007] Patent document CN101281178A discloses a quantitative detection method and enrichment device of trace phosphine gas, but does not disclose the extraction and calculation method of dissolved phosphine gas in water samples. On this basis, the present invention discloses A method for detecting trace phosphine gas in water samples by gas chromatography combined with two cold trap enrichment methods before the column, especially the improvement points are the establishment of a two-phase equilibrium method for extracting phosphine gas and dissolved phosphorus in water Calculation method of phosphine, the calculation method of phosphine content in this invention

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  • Method for detecting trace phosphine gas in water sample by gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method
  • Method for detecting trace phosphine gas in water sample by gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method
  • Method for detecting trace phosphine gas in water sample by gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method

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Experimental program
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Effect test

Embodiment 1

[0128] In a scientific research project, water samples were collected from the Yellow Sea coast of Yancheng, Jiangsu, and the concentration of phosphine in the water samples was determined by this method.

[0129] Experimental instruments and reagents:

[0130] Agilent 4890D gas chromatograph, equipped with thermal ion nitrogen phosphorus detector (NPD), chromatographic column is the capillary column that adopts Crosslinked 5%Ph Me Silicone (25m * 0.2mm * 0.33 μ m film thickness, Hewlett Packard); valve; two 2L thermos cups (as a cold trap); liquid nitrogen (refrigeration laboratory of Nanjing University); standard PH3 gas (Nanjing Special Gas Factory).

[0131] Chromatographic conditions: column temperature 40°C; detector temperature 220°C (280°C); carrier gas (nitrogen) flow rate 2mL / min; air flow rate 120mL / min; hydrogen flow rate 3-45mL / min; 30mL / min; the activation voltage of the detector is controlled at about 450mV, and the activation signal is about 23.

[0132] Accu...

Embodiment 2

[0140] In a scientific research project, water samples collected from the Jiangsu section of the Yangtze River were collected by this method to determine the concentration of phosphine in the water samples.

[0141] Experimental instruments and reagents:

[0142] Agilent 4890D gas chromatograph, equipped with thermal ion nitrogen phosphorus detector (NPD), chromatographic column is the capillary column that adopts Crosslinked 5%Ph Me Silicone (25m * 0.2mm * 0.33 μ m film thickness, Hewlett Packard); valve; two 2L thermos cups (as a cold trap); liquid nitrogen (refrigeration laboratory of Nanjing University); standard PH3 gas (Nanjing Special Gas Factory).

[0143] Chromatographic conditions: column temperature 40°C; detector temperature 220°C (280°C); carrier gas (nitrogen) flow rate 2mL / min; air flow rate 120mL / min; hydrogen flow rate 3-45mL / min; 30mL / min; the activation voltage of the detector is controlled at about 450mV, and the activation signal is about 23.

[0144] Ac...

Embodiment 3

[0152] In a scientific research project, water samples from Taihu Lake in Jiangsu Province were collected, and the concentration of phosphine in water samples was determined by this method.

[0153] Experimental instruments and reagents:

[0154] Agilent 4890D gas chromatograph, equipped with thermal ion nitrogen phosphorus detector (NPD), chromatographic column is the capillary column that adopts Crosslinked 5%Ph Me Silicone (25m * 0.2mm * 0.33 μ m film thickness, Hewlett Packard); valve; two 2L thermos cups (as a cold trap); liquid nitrogen (refrigeration laboratory of Nanjing University); standard PH3 gas (Nanjing Special Gas Factory).

[0155] Chromatographic conditions: column temperature 40°C; detector temperature 220°C (280°C); carrier gas (nitrogen) flow rate 2mL / min; air flow rate 120mL / min; hydrogen flow rate 3-45mL / min; 30mL / min; the activation voltage of the detector is controlled at about 450mV, and the activation signal is about 23.

[0156] Accurately draw 30m...

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Abstract

The invention provides a method for detecting trace phosphine gas in a water sample by a gas chromatograph (GC)-cooperating pre-column twice cold trap enrichment method, and aims to overcome the shortcomings of the existing various measurement methods. The method mainly comprises the following steps of: (1) cooling and enriching the phosphine gas and establishing a GC / NPD (nitrogen phosphorous detector) detection device; (2) extracting and dissolving the phosphine gas in lake water by a gas-liquid two-phase phase equilibrium method, and preparing a gas sample to be detected; (3) preprocessingthe gas sample; (4) extracting a certain volume of the gas sample into a gas absorption tube; (5) performing primary enrichment of the processed gas sample in a cold trap I, and removing the impuritygas with a relatively low boiling point; (6) heating the cold trap I so that the gas enters a cold trap II for secondary enrichment; (7) detecting the final enrichment product by a nitrogen phosphorous detector in a gas chromatograph through a chromatographic column; and (8) converting the measured area of a characteristic peak of the phosphine according to a certain formula to obtain the concentration of the phosphine in the water sample to be detected.

Description

technical field [0001] The invention belongs to the field of environmental monitoring, and particularly relates to a method for detecting trace phosphine gas in water samples by gas chromatography combined with two cold trap enrichment methods before a column. Background technique [0002] Phosphorus is the limiting factor for algal blooms in water bodies. With the development of our country's social economy, the amount of phosphorus discharged into natural water bodies in our country is increasing day by day, resulting in serious eutrophication. At present, the wastewater phosphorus removal methods adopted in my country include chemical phosphorus removal, biological phosphorus removal, etc., all of which produce a large amount of sludge, and the treatment of sludge requires high cost, so the study of phosphorus removal methods with low sludge output has become the current research hotspots. [0003] Phosphine is also a poisonous and carcinogenic active gas. Inhalation of ...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/02
Inventor 耿金菊任洪强牛晓君王晓蓉
Owner NANJING UNIV
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