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Efficient collection and rapid mass spectrometry method for organic compounds in atmosphere

A technology for organic compound and mass spectrometry analysis, which is applied in the field of efficient collection of organic compounds in the atmosphere and rapid mass spectrometry analysis. The effect of controllable quantity, high analytical sensitivity and low price

Pending Publication Date: 2022-02-11
XI'AN PETROLEUM UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the sampling efficiency can be improved by using the above thin films, these thin films are composed of polymer backbone, which is easy to decompose siloxane or background interference
At the same time, after the atmospheric samples are collected, the analysis of semi-volatile compounds needs to go through the processes of organic solvent extraction, purification, chromatographic separation / mass spectrometry detection, etc. The operation process is cumbersome, which is not conducive to rapid analysis
More importantly, when organic solvents are used to extract the organic compounds collected on the surface of the organic filter membrane, the filter membrane is prone to swelling or even dissolution

Method used

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  • Efficient collection and rapid mass spectrometry method for organic compounds in atmosphere
  • Efficient collection and rapid mass spectrometry method for organic compounds in atmosphere
  • Efficient collection and rapid mass spectrometry method for organic compounds in atmosphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] refer to figure 1 , the steps of this embodiment include:

[0031] Step 1. Accurately weigh 0.5g of silicon dioxide with a particle size of 10μm and 0.05g of corn starch and dissolve them in 100mL of deionized water. After ultrasonic emulsification for 20 minutes, heat it to boiling and keep it for 0.5 minutes; Load it in a vacuum filtration device containing blank filter paper, carry out suction filtration and coating, after the aqueous solution completely permeates the filter paper, wash with 10mL of absolute ethanol, and then dry it in a fume hood to obtain silica adsorbent-loaded paper matrix (such as figure 2 A).

[0032] Step 2, the prepared paper matrix is ​​used as an atmospheric sampling filter, placed in a high negative pressure ambient air particle sampler (the resistance to overcome is 20kPa when the maximum load is 50L / min), and the organic compounds and aerosol particles in the atmosphere are collected. The sampling flow rate is 30L / min. After the samp...

Embodiment 2

[0036] The preparation method was the same as in Example 1, except that 0.1g-0.9g of commercially purchased silica with a particle size of 10 μm was accurately weighed for the preparation of silica-loaded paper substrates, the collection of organic compounds in the atmosphere, and mass spectrometry analysis.

[0037] Performance comparison: By comparing the performance of paper substrates loaded with different amounts of silica, it can be found that when the surface of the paper substrate does not contain any silica, its enrichment efficiency for siloxane compounds (m / z 536, 610 and 684) in the atmosphere lower ( Figure 4 A); when 0.1g of silica is loaded on the surface of the paper substrate, its enrichment efficiency is significantly improved ( Figure 4 B); when the loaded amount of silicon dioxide reached 0.3g, its enrichment efficiency to the siloxane compound in the air gradually increased ( Figure 4 C); when the loaded amount of silicon dioxide was further increased ...

Embodiment 3

[0039] The preparation method is the same as in Example 1, except that 0.5 g of commercially purchased silica with a particle size of 1 μm-80 μm is accurately weighed for the preparation of silica-loaded paper substrates, the collection of organic compounds in the atmosphere, and mass spectrometry analysis.

[0040] Performance comparison: By comparing the performance of silica paper substrates loaded with different particle sizes, it can be found that when the particle size of silica is between 1 μm and 80 μm, its enrichment efficiency for siloxane compounds in the atmosphere is basically similar ( Figure 5 ). Nevertheless, during the sampling process, it was found that when the particle size of silica was small, the back pressure of the sampler was large (>20kPa, close to the limit value of the instrument), and the sampling volume was small; When the sample volume becomes stable, the backpressure drop of the sampler is about -13kPa; when the particle size of silica is furth...

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Abstract

The invention relates to an efficient collection and rapid mass spectrometry method for organic compounds in atmosphere, which comprises the following steps: firstly, a certain amount of inorganic solid adsorbent with the particle size of 10-20 [mu] m and binder starch in an aqueous solution are weighted, and ultrasonic treatment, heating, vacuum filtration, coating and the like are performed to prepare an adsorbent-loaded paper substrate; the prepared paper substrate is placed in a high negative pressure environment air particulate matter sampler, organic compounds and aerosol particles in the atmosphere are collected at the flow speed of 10 L / min to 40 L / min, and the sampling time ranges from 0.5 h to 6 h; and after the sampling is finished, a paper substrate containing a sample is sheared into a triangle, an elution solvent and spray voltage are loaded, and mass spectrum real-time analysis is performed. The adsorbent-loaded paper substrate and the preparation method have the advantages that the operation is simple, the adsorbent loading capacity is controllable, the adsorption capacity is high, and the price is low; the atmospheric sample collection process does not need equipment improvement, the sampling is simple, and the organic compound enrichment efficiency is high; and the whole mass spectrometry process has the characteristics of no need of sample pretreatment, high analysis sensitivity and the like, and can meet the requirements of rapid analysis of organic compounds and aerosol particles in the atmosphere.

Description

technical field [0001] The invention belongs to the technical field of analysis of organic compounds in the environment, and in particular relates to a method for efficient collection and rapid mass spectrometry analysis of organic compounds in the atmosphere. [0002] technical background [0003] While the rapid development of industrialization has brought great material wealth to human beings, it has also caused serious harm to the environment, among which organic pollutants are particularly prominent. In order to effectively evaluate the distribution of different organic pollutants in the environment, people have successively developed a variety of detection techniques such as chromatography, spectroscopy, mass spectrometry, and NMR for the detection and analysis of related substances. Among these methods, gas chromatography-mass spectrometry is considered to be the most effective method for detecting VOCs in the environment today. However, before using the above method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/24
CPCG01N27/62G01N1/2273
Inventor 张智平郑亚君行高选
Owner XI'AN PETROLEUM UNIVERSITY
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