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Method for determining semi-volatile organic compounds in soil based on temperature programmed sampling-gas chromatography-mass spectrometry

A semi-volatile, temperature-programmed technology, applied in the detection field, can solve the problems of single quadrupole mass spectrometer with limited anti-interference ability, large difference in physical and chemical properties, and reduced work efficiency, so as to improve anti-matrix interference ability, high degree of automation, The effect of improving compatibility

Pending Publication Date: 2022-05-13
TIANJIN VOCATIONAL INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, the reason is that there are many types of semi-volatile organic compounds, and the physical and chemical properties vary greatly, so it is difficult to unify the instrument analysis conditions.
On the other hand, the reason is that the soil matrix is ​​complex, and the anti-interference ability of single quadrupole mass spectrometry is limited. Sample purification treatment can help improve the accuracy of analysis results. However, different types of semi-volatile organic compounds often require different purification conditions. , will greatly reduce work efficiency

Method used

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  • Method for determining semi-volatile organic compounds in soil based on temperature programmed sampling-gas chromatography-mass spectrometry
  • Method for determining semi-volatile organic compounds in soil based on temperature programmed sampling-gas chromatography-mass spectrometry
  • Method for determining semi-volatile organic compounds in soil based on temperature programmed sampling-gas chromatography-mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Preparation of standard working solution

[0029] Use 2000mg / L mixed standard solution of 64 semi-volatile organic compounds and 2000mg / L mixed standard solution of 6 substitutes, prepare a high-concentration mixed standard solution with chromatographically pure acetone as an intermediate solution, and then dilute it with acetone to form a 1-5 level standard Working solution, the working solution concentration range is shown in Table 1.

[0030] The gas chromatographic conditions: separate with DB-5MS UI quartz capillary column (30m*0.25mm*0.25μm), carrier gas is helium, splitless injection, flow rate 1.0mL / min, initial temperature 40°C, keep for 5min , raised to 110°C at 8°C / min and kept for 2 minutes, raised to 150°C at 10°C / min and kept for 5 minutes, raised to 300°C at 10°C / min and kept for 5 minutes.

[0031] Detection of the standard solution and drawing of the standard curve: Accurately pipette 1uL of the prepared 1-5 grade standard working solution above and...

Embodiment 2

[0054] Weigh 20g of natural air-dried soil sample into a conical flask, the exact value is 0.0001mg, add 5g of diatomaceous earth and mix evenly, transfer to a fast solvent extraction pool, extract with dichloromethane: acetone (1:1), the extraction condition is temperature 100°C, pressure 1500psi, let stand for 8min, wash 60% of the volume, and circulate twice. The extract is concentrated to about 5mL by rotary evaporation, and transferred to a 10mL volumetric flask. The 4mL mixed solution is washed twice in the flask. 10 mL was analyzed by gas chromatography tandem mass spectrometer.

[0055] Table 4. Content of semi-volatile organic compounds

[0056]

[0057]

[0058] Calculation of phenol results: phenol equation Y=-83222+26847.2*X, the peak area is 1206786, the phenol content is 48.05ng / mL calculated from the curve, and the sample weight is 20g, so the test result=C*V / m / 1000=48.05 *10 / 20 / 1000 = 0.024 mg / kg. Among them: C is the concentration of each compound calc...

Embodiment 3

[0060] Weigh 20g of natural air-dried soil sample in a conical flask, accurate to 0.0001mg, add 5g of diatomaceous earth and mix evenly, transfer to a fast solvent extraction pool, extract with dichloromethane: acetone (1:1), the extraction condition is temperature 100°C, pressure 1500psi, let stand for 8min, wash 60% of the volume, and circulate twice. The extract is concentrated to about 5mL by rotary evaporation, and transferred to a 10mL volumetric flask. The 4mL mixed solution is washed twice in the flask. 10 mL was analyzed by gas chromatography tandem mass spectrometer.

[0061] Table 5. Content of semi-volatile organic compounds

[0062]

[0063]

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Abstract

The invention discloses a method for determining semi-volatile organic compounds in soil based on temperature programmed sampling-gas chromatography-mass spectrometry, which comprises the following steps: step 1, preparing a high-concentration mixed standard solution as an intermediate solution by using the semi-volatile organic compounds and / or semi-volatile organic compound substitutes and utilizing chromatographically pure acetone, diluting into a 1-5 grade standard working solution; 2, setting gas chromatography conditions and mass spectrometry conditions, detecting a standard solution, drawing a standard curve, and screening parent ions, daughter ions and corresponding collision energy; 3, extracting semi-volatile organic compounds in the soil by using a rapid solvent extraction method, and fixing the volume to obtain a test sample; and step 4, under the gas chromatography condition and the mass spectrum condition, injecting the test sample into a gas chromatography tandem mass spectrometer for analysis, and calculating the content of each semi-volatile organic compound. According to the method, the compatibility of various semi-volatile compounds is improved, the matrix interference resistance is improved, the detection speed is high, and the accuracy is high.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for measuring semi-volatile organic compounds in soil based on programmed temperature sampling-gas chromatography. Background technique [0002] Semi-volatile organic compounds widely exist in the natural environment, including anilines, N-nitrosoamines, nitrobenzenes, phenols, chlorobenzenes, polycyclic aromatic hydrocarbons, phthalates, alkyl ethers, etc., and Through sedimentation, precipitation, adsorption and other processes, it finally gathers in the soil, causing serious pollution to the soil. These compounds are harmful to humans and animals to varying degrees. For example, N-nitroso compounds have carcinogenic effects and can induce gene mutations; chlorobenzenes have carcinogenic and mutagenic effects and are enriched in the biological chain and endanger human health and the environment. Ecosystem; phthalates interfere with human and animal endocrine and har...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 王欣陈硕祖晓冬李霞
Owner TIANJIN VOCATIONAL INST
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