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Method for detecting n-alkanes in atmospheric particulates

A technology for atmospheric particulate matter and n-alkane, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of no relevant patents and methods for particle phase determination, difficulties in effective separation, extraction and determination, and complex components of atmospheric particulate matter. Reduced analysis cost, low detection limit, and high sensitivity

Inactive Publication Date: 2019-01-08
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex composition of atmospheric particulate matter, including thousands of organic compounds, and the concentration of each component is low, it brings certain difficulties to effective separation, extraction and determination
Regarding the determination of n-alkanes in the atmosphere, there are currently national occupational health standards for the determination of alkane compounds in the workplace air toxic substances (GBZ / T 160.38-2007), but there are no relevant patents and methods for the determination of the particulate phase

Method used

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  • Method for detecting n-alkanes in atmospheric particulates
  • Method for detecting n-alkanes in atmospheric particulates
  • Method for detecting n-alkanes in atmospheric particulates

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031] The mensuration of n-alkanes in the air particulate matter during the accelerated solvent extraction of embodiment 1

[0032] Particle sample collection: use a large flow sampler (KB-1000 type, Qingdao Jinshida Electronic Technology Co., Ltd.) to 1.05m 3 / min traffic collection PM 2.5 Samples were collected on a quartz filter (20.3×25.4cm, Whatman QM-A) for 20 hours. Before sampling, the quartz filter membrane was pre-placed in a muffle furnace and roasted at 500°C for 4h, placed in a constant temperature and humidity dryer (temperature 22°C, humidity 45%) to balance for 48h, weighed with a balance with an accuracy of 0.01mg, and then wrapped with aluminum foil Packaged and stored in a -20°C low-temperature freezer until analysis. Before on-site sampling, the flow rate of the sampler should be calibrated, the filter membrane clip and the adsorbent sleeve should be installed in sequence, connected to the sampler, the sampling flow rate should be adjusted, and sampling ...

Embodiment 2

[0036] The mensuration of n-alkanes in atmospheric particulate matter during microwave extraction of embodiment 2

[0037] Particulate matter sample collection and standard curve drawing are the same as in Example 1.

[0038] Sample separation: Cut the filter membrane into pieces and put it into a microwave extraction tank (polytetrafluoroethylene material), add 20ml of dichloromethane, and add 100ng of deuterium tetradecane (d 50 ) internal standard to determine the recovery rate of the sample, put it in a microwave digestion apparatus, raise the temperature to 100°C, keep it for 30min, and cool to room temperature after the extraction is completed. Filter the extract through a 0.45 μm PTEF filter membrane with a needle filter and pour it into a round-bottomed flask for rotary evaporation. The temperature of the rotary evaporator is controlled and concentrated to about 5.0ml in a water bath at 40°C. Add 5-10ml of n-hexane to continue concentrating When it is nearly dry, rins...

Embodiment 3

[0040] Determination of n-alkanes in atmospheric particulate matter during ultrasonic extraction of embodiment 3

[0041] The particle sample collection and standard determination methods are the same as in Example 1. The difference is that the GC-MS determination method after standard extraction is as follows: column temperature is 90°C, retain for 1min, heat up to 140°C at a speed of 20°C / min, hold for 5min, and then heat up to 300°C at a speed of 8°C / min. ℃, keep for 20min. The total ion chromatograms of the corresponding standard mixed samples are shown in Figure 5 .

[0042] After cutting the filter membrane into pieces, put it into an ultrasonic cleaner, add 20ml of extract solution three times for extraction, extract for 15-30min each time, and combine the extract solution. Filter the extract through a 0.45 μm PTEF filter membrane with a needle filter and pour it into a round-bottomed flask for rotary evaporation. The temperature of the rotary evaporator is controll...

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Abstract

The invention relates to a method for detecting n-alkanes in atmospheric particulates. The n-alkanes in a sample can be extracted by Soxhlet extraction, accelerated solvent extraction, microwave extraction or ultrasonic extraction and dissolved into an organic phase, the extract is filtered by a sampler and a PTFE filter to remove insoluble particles, the filtrate is concentrated by rotary evaporation, then the concentrate is transferred to a glass chromatography column for purification, n-alkanes are eluted with n-hexane, the eluate is reduced to be 1 ml or less than 1 ml by rotary evaporation and nitrogen blowing, n-hexane is added to a constant volume of 1.0 mL, and the content of the n-alkanes is measured by gas chromatography-mass spectrometry (GC-MS). The method has good resolution for the n-alkanes in the particulate sample, high sensitivity and low detection limit, and is suitable for rapidly detecting the n-alkanes in the atmospheric particulates.

Description

technical field [0001] The invention relates to the detection of organic compounds in atmospheric particulate matter, in particular to a method for detecting normal alkanes in atmospheric particulate matter. Background technique [0002] Atmospheric particulate matter plays a vital role in air quality, global climate, and human health. Studies have shown that 20-90% of fine particulate matter is organic matter. Normal alkanes (n-alkanes) are a class of aliphatic compounds and semi-volatile organic compounds that exist in both the gas phase and the particle phase. Normal alkanes in the particulate phase include isoprenoids, terpenes, steranes, and the like. The normal alkanes in the particle phase mainly come from the incomplete combustion of carbon-containing fuels and lubricating oil, which have a certain impact on the environment. Normal alkanes in atmospheric particulate matter include C 9 -C 40 , most of which are C 10 -C 15 . Due to the complex composition of at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 毕承路莫世荣叶招莲罗世鹏
Owner JIANGSU UNIV OF TECH