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Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5

A technology for quantitative detection of nitrobenzene, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of complex pre-treatment purification steps, easy false positives, background matrix interference, etc., to achieve fast and efficient collection and save analysis Cost, effect of fast extraction

Inactive Publication Date: 2014-03-05
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA +1
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Problems solved by technology

[0010] Aiming at the problems of background matrix interference, complex pretreatment and purification steps, and easy false positives in nitrobenzene compounds in current atmospheric particulate matter environmental samples, the present invention provides a method for quantitatively detecting six kinds of nitrobenzene compounds in atmospheric fine particle PM2.5 Compound method, established and optimized the detection method of 6 kinds of nitrobenzene compounds by secondary mass spectrometry (MS / MS), the optimized method has better selectivity and higher sensitivity than conventional detection method, this kind of two The advantages of advanced mass spectrometry detection technology in compound qualitative can meet the needs of rapid quantitative detection of 6 kinds of nitrobenzene compounds in ambient air particulate matter samples without complicated pretreatment, which greatly saves analysis time and cost

Method used

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  • Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5
  • Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5
  • Method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (A) target compound selects nitrobenzene compound;

[0044] (B) Sample collection: Use glass fiber filter membrane or quartz fiber filter membrane as sampling enrichment filter membrane, use air sampler with particle size segmentation to collect atmospheric particulate matter samples, and the sampling flow rate is 0.8-1.2m 3 / min, the collection time does not exceed 12h, and the collection air volume is 576~792m 3 ;

[0045] (C) Sample extraction: After cutting the filter membrane for collecting particulate matter samples, use the extraction solvent to continuously extract with a Soxhlet fat extractor. The extraction time is 12 hours. The extraction solvent is n-hexane and acetone in a volume ratio of 1:1 mixed solution;

[0046] (D) Concentration of the sample: Concentrate the extract after the sample extraction to 1 mL, blow it with nitrogen until it is nearly dry, and then use isooctane to make up the volume, and store the sample to be tested in a dark environment ...

Embodiment 2

[0052] (A) The target compound selects the o-dinitrobenzene compound, and the preparation concentration is 6 kinds of nitrobenzene standard substance solutions of 1000ug / mL, such as figure 2 shown in;

[0053] (B) Sample collection: Use glass fiber filter membrane or quartz fiber filter membrane as sampling enrichment filter membrane, use air sampler with particle size segmentation to collect atmospheric particulate matter samples, and the sampling flow rate is 0.8m 3 / min, the collection time does not exceed 12h, and the collection air volume is 576m 3 ;

[0054] (C) Sample extraction: After cutting the filter membrane for collecting particulate matter samples, use the extraction solvent to continuously extract with a Soxhlet fat extractor. The extraction time is 8 hours. The extraction solvent is n-hexane and acetone in a volume ratio of 1:1 mixed solution;

[0055] (D) Sample concentration: Concentrate the extract obtained after extraction to about 1mL, blow it with nit...

Embodiment 3

[0063] (A) target compound selects m-dinitrobenzene compound;

[0064] (B) Sample collection: Use glass fiber filter membrane or quartz fiber filter membrane as sampling enrichment filter membrane, use air sampler with particle size segmentation to collect atmospheric particulate matter samples, and the sampling flow rate is 1.2m 3 / min, the collection time does not exceed 24h, and the collected air volume is 792m 3 ;

[0065] (C) Sample extraction: After cutting the filter membrane for collecting particulate samples, use the extraction solvent to continuously extract with a Soxhlet fat extractor. The extraction time is 24 hours. The extraction solvent is n-hexane and dichloromethane in a volume ratio of 1 : 1 mixed solution;

[0066] (D) Sample concentration: Concentrate the extract obtained after extraction to about 0.5mL, blow it to near dryness with nitrogen, and then use isooctane to make up the volume, and store the sample to be tested in a dark environment at -20°C; ...

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Abstract

The invention provides a method for quantitatively detecting six kinds of nitrobenzene compounds in fine atmospheric particles PM2.5. The method comprises the following steps: acquiring a sample, extracting the sample, concentrating and purifying the sample and quantitatively detecting by adopting chromatography-tandem mass spectrometry. By optimizing parameters of secondary mass spectrometry conditions, the method is better in selectivity and higher in sensitivity on target compounds in comparison with an existing detection method reported in literature. According to the method, the disadvantage that the selectivity and the sensitivity of a conventional detector in the process of detecting the trace quantity of nitrobenzene compounds in a complex background matrix cannot be ensured at the same time is overcome by virtue of a gas chromatography / tandem mass spectrometry selective reaction monitoring technology, and the qualitative operation is accurate and reliable, so that the method has very remarkable advantages in comparison with conventional GC / ECDs (gas chromatography / election capture detectors), GC / NPDs (gas chromatography / nitrogen-phosphorus detector), GC / LRMS (gas chromatography / low resolution mass spectrometry) detectors or GC / HRMS (gas chromatography / high resolution mass spectrometry) detectors.

Description

technical field [0001] The present invention relates to a quantitative monitoring method for nitrobenzene compounds in atmospheric fine particles PM2.5, in particular to a method for quantitatively detecting six kinds of nitrobenzene compounds in atmospheric fine particles PM2.5, specifically, It is a method for rapid quantitative detection of 6 nitrobenzene compounds in atmospheric particulate matter PM2. . Background technique [0002] Nitrobenzene compounds are the general term for nitroaromatic compounds, and are intermediates in the synthesis of dyes, paints, plastics, explosives, pharmaceuticals and pesticides. Nitrobenzene pollutants in the environment mainly include nitrobenzene, nitrochlorobenzene, nitrotoluene, nitrophenol, nitroaniline and other substances. [0003] Most nitrobenzene compounds have the characteristics of stable chemical properties, high toxicity and bioaccumulation. They are highly toxic pollutants and have been included in the list of priority ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 赵欣丁宝国王晓宁周晓静曾瑶应蓉蓉冯艳红单艳红林玉锁张胜田龙涛王国庆
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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