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Method for simultaneously determining PAHs (polycyclic aromatic hydrocarbons) and n-alkanes in atmosphere particulates

A technology for atmospheric particles and n-alkanes, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as long time and cumbersome operation process, achieve low detection limit, good separation effect, and improve utilization rate

Inactive Publication Date: 2018-10-19
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the standard, Soxhlet extraction needs to be refluxed for 18 hours, the operation process is cumbersome, the time is long, and a large amount of high-purity organic solvent needs to be added as the extractant, which is not suitable for the rapid and accurate analysis of PAHs in a large number of environmental samples.

Method used

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  • Method for simultaneously determining PAHs (polycyclic aromatic hydrocarbons) and n-alkanes in atmosphere particulates
  • Method for simultaneously determining PAHs (polycyclic aromatic hydrocarbons) and n-alkanes in atmosphere particulates
  • Method for simultaneously determining PAHs (polycyclic aromatic hydrocarbons) and n-alkanes in atmosphere particulates

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1. The mensuration of PAHs in atmospheric particulate matter (microwave digestion pretreatment)

[0023] (1) Sample collection: use a large flow sampler (KB-1000 type, Qingdao Jinshida Electronic Technology Co., Ltd.) to 1.05m 3 / min traffic collection PM 2.5Samples 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 should start. A...

Embodiment 2

[0026] Embodiment 2. The mensuration of PAHs in atmospheric particulate matter (accelerated dissolution extraction pretreatment)

[0027] (1) Sample collection: The sample collection method is the same as in Example 1.

[0028] (2) Sample purification: Cut 1 / 8 filter membrane into pieces with ceramic scissors, put it into an accelerated solvent extraction apparatus, add 20ml of n-hexane / acetone mixed solution (1:3, v / v) to start extraction. The corresponding conditions are: temperature 140°C, pressure 1500Psi, static extraction time 10min, rinsing volume 60% of cell volume, nitrogen purging 60s, static extraction times 2 times. After the extraction, the extraction tank was washed with 5 mL of n-hexane, and the extract was filtered in a suction filter flask with a 0.45 μm PTEF filter membrane, and then transferred to a round bottom flask for rotary evaporation. Use a rotary evaporator to control the temperature below 45°C and concentrate to below 5.0mL, add 10ml of n-hexane, c...

Embodiment 3

[0030] Embodiment 3: the mensuration of n-alkanes in atmospheric particulate matter

[0031] (1) The sample collection method is the same as in Example 1;

[0032] (2) Sample purification: Cut 1 / 8 filter membrane into pieces with ceramic scissors, put it into a microwave extraction tank, add 20ml of n-hexane / acetone mixed solution (1:3, v / v), and place it in a microwave extraction apparatus , while adding 100ng deuterium tetradecane (d 50 ) internal standard to determine the sample recovery. Raise the temperature to 100°C, keep it for 30 minutes, and cool to room temperature after the digestion is completed. The extraction tank was washed with 5 ml of n-hexane, and the extract was filtered in a suction filter flask with a 0.45 μm PTEF filter membrane, and then transferred to a round bottom flask for rotary evaporation. Use a rotary evaporator to control the temperature below 45°C and concentrate to below 5.0ml, add 5-10ml of n-hexane, continue to concentrate until nearly dr...

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Abstract

The invention provides a method for simultaneously determining PAHs (polycyclic aromatic hydrocarbons) and n-alkanes in atmosphere particulates. The method comprises the following steps of collectingof a sample, purifying of the sample, and determining of the sample; GC-MS (gas chromatography-mass spectrometer) is used for determining, and a chromatographic column is a capillary chromatographic column with weak polarity, the MS adopts an EI (electromagnetic interference) source and MRM (multi-reaction mode) mode, the electron energy is 70eV, and the temperature of an ion source is 230 DEG C;in the heating procedure during PAHs determination, the initial column temperature is maintained at 40 DEG C for 2min, and is heated to 100 DEG C at the rate of 10 DEG C / min, the temperature of 100 DEG C is maintained for 1min, then the temperature is heated to 250 DEG C at the rate of 20 DEG C / min, and the temperature of 250 DEG C is maintained for 3min; in the heating procedure during n-alkanesdetermination, the initial column temperature is maintained at 50 DEG C for 2min, and is heated to 300 DEG C at the rate of 5 DEG C / min, and the temperature of 300 DEG C is maintained for 20min.

Description

technical field [0001] The invention relates to the detection of organic compounds in atmospheric or waste gas particulate matter, in particular to a method for simultaneously detecting polycyclic aromatic hydrocarbons and normal alkanes in atmospheric waste gas particulate matter. Background technique [0002] The aromatic compounds polycyclic aromatic hydrocarbons (PAHs) and aliphatic n-alkanes (n-alkanes) in the atmospheric gas phase and particle phase are all products from the incomplete combustion of carbon-containing fuels, among which PAHs compounds have carcinogenic and teratogenic properties, and are normal Alkanes also have some impact on the environment. Particulate matter PAHs and n-alkanes come from a wide range of sources, such as the combustion of fossil fuels such as coal and oil, the combustion of biomass such as straw and wood, garbage incineration, industrial smoke, and leakage of petrochemical products, which may be released by human activities. Atmosphe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 叶招莲顾远罗世鹏毕承路马帅帅
Owner JIANGSU UNIV OF TECH
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