Quantitative detection method of pentachlorophenol in soil

A quantitative detection method, the technology of pentachlorophenol, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex derivatization process, high polarity of pentachlorophenol, low vapor pressure, etc., and achieve low toxicity and stable recovery rate , the effect of less reagent

Inactive Publication Date: 2010-01-20
INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the high polarity and low vapor pressure of pentachlorophenol make the determination of gas chromatography still have certain restrictions, and some monitoring methods and the determination method of pentachlorophenol in water standards are mostly determined by derivatization gas chromatography (Zhang Hongyu, Zhang Jie , Huang Xiuhua. Direct determination of three chlorophenols in wastewater by solid phase microextraction / GC. Journal of Analytical Science, 2002, 18(5): 421-423; Wang Xin, Fang Ruibin, Zhu Ronggang. Determination of drinking water by SPME combined with GC / ECD Chlorophenols. Yunnan Chemical Industry, 2001, 28(3): 23-25; Huang Xiuhua, Sun Yuli. Determination of phenolic compounds in water by gas chromatography. China Water Supply and Drainage, 2000, 16(3): 52-53)
The derivatization process is complicated, and consumes a lot of reagents and is highly toxic

Method used

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  • Quantitative detection method of pentachlorophenol in soil
  • Quantitative detection method of pentachlorophenol in soil
  • Quantitative detection method of pentachlorophenol in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: Extraction and purification of PCP in soil

[0038] 1) Extraction of PCP

[0039] Accurately weigh 2.0 g of the soil sample and place it in a 30 mL centrifuge tube, add 2 mL of sulfuric acid with a concentration of 6 mol / L, add 10 mL of acetonitrile and shake and mix on a vortex mixer, then add 2 mL of n-hexane, and shake and mix evenly. Shake on a shaker for 30 minutes, ultrasonic at 40°C for 1 hour, centrifuge at 5000 r / min for 5 minutes, and wait for purification.

[0040] 2) Purification of the extract

[0041] Weigh 20mg ODSC 18 1. Put 200mg of anhydrous magnesium sulfate in a 15mL centrifuge tube, and vortex to mix. Take 2 mL of the extract to be purified, add it into the mixed purification system, mix on a vortex for 2 min, and centrifuge at 9000 r / min for 5 min. Take 1 mL of the supernatant and pass it through a 0.45 μm filter membrane for determination on the machine.

Embodiment 2

[0042] Embodiment 2: the selection of high performance liquid chromatography (HPLC) condition of the present invention and working curve

[0043] The standard solutions were prepared with chromatographic standard substances from DR. Ehrenstorfer Company in Germany, and they were respectively prepared into methanol standard series and matrix standard series. Assay by HPLC.

[0044] 1) HPLC determination conditions

[0045] Chromatographic column: Agilent5 m SB-C 18 Reversed-phase column, 4.6×250mm;

[0046] Mobile phase: 85% methanol + 15% water containing 0.1% glacial acetic acid, using isocratic elution for 10 minutes. The flow rate is 1.0mL / min;

[0047] Injection volume: injection volume 10L;

[0048] Column temperature: 35°C;

[0049] Detector: ultraviolet detector (DAD), detection wavelength 225nm.

[0050] 2) Selection of working curve

[0051] The substrate solution is prepared from soil through the above-mentioned pretreatment method. Prepare standard concentr...

Embodiment 3

[0052] Embodiment 3: the minimum detection limit and the linear range of the detection method of the present invention

[0053] Prepare the standard concentration with matrix solution as 0.0500mg / L, 0.100mg / L, 0.200mg / L, 0.500mg / L, 1.00mg / L, 2.00mg / L, 5.00mg / L, 10.0mg / L, 20.0mg / L The PCP standard series of L was measured on the machine. Get standard curve y=7.53x+1.28, R=0.9995, R 2 =0.9991, the linear range is 0.1-20mg / L.

[0054] According to the optimized pre-treatment and instrument conditions, continuously measure 7 same low-concentration spiked samples, using the formula MDL=S×t (n-1，1-a＝0.99) , to calculate the detection limit of the method. Among them, MDL is the detection limit of the method, t is the value when the confidence level is 99%, and the degree of freedom is n-1, and S is the standard deviation of the concentration of n spiked determinations. Obtained through table lookup and calculation, S=0.45g / g, t=3.14, n=7, and MDL=1.413g / g obtained by substitution...

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Abstract

The invention discloses a quantitative detection method of pentachlorophenol in the soil, which belongs to the field of analysis and detection of compounds. The quantitative detection method comprises the following steps: a) regulating the pH value of a soil sample to be detected, and precipitating the pentachlorophenol in molecular form; b) adding an extraction agent and n-hexane into the sample, and extracting the pentachlorophenol into the extraction agent; c) adding an absorbent into an extract and purifying the extract; and d) detecting the pentachlorophenol in the extract by liquid phase chromatography. The method can be used for quantitative detection of content of the pentachlorophenol in the soil as the standard method and be characterized by rapidness, simplicity, good universality, small toxicity, simple operation, good reproducibility, low detection limit and the like.

Description

technical field [0001] The invention relates to pentachlorophenol, in particular to a quantitative detection method for pentachlorophenol in soil. The method combines oscillating ultrasound with QuEChERS technology to quickly and accurately quantitatively detect pentachlorophenol, which belongs to the field of compound analysis and detection. Background technique [0002] Pentachlorophenol (PCP) is a toxic and refractory organic compound, which is formed by replacing five hydrogen atoms on the benzene ring of phenol with five chlorine atoms. As an organochlorine pesticide, pentachlorophenol is widely used as fungicide, molluscicide, algicide, insecticide and herbicide, and wood preservative. Due to its persistent and refractory nature in the environment and potential threats to human health, it has been included in the priority control of environmental governance by the US Environmental Protection Agency (US EPA), the European Commission (European Commission), China Environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 王亚男牛书涛董一威贺小蔚汪聪慧
Owner INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI
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