Method for detecting phthalate substances in environmental sample

A technology for phthalic acid and environmental samples, which is applied in the field of chemical detection and can solve the problems of high cost and complicated processing

Inactive Publication Date: 2017-12-15
SHENYANG UNIV
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  • Method for detecting phthalate substances in environmental sample
  • Method for detecting phthalate substances in environmental sample

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Embodiment 1

[0016] PAEs determination in the soil sample of embodiment 1

[0017] 1. Extraction of PAEs from samples. Take the 100-mesh soil into conical flasks, 10g in each bottle, add dichloromethane in 3 times (10mL, 5mL, 5mL), extract with ultrasonic vibration for 15min under ice-bath conditions, let stand for 10min, and combine the extracts , passed through anhydrous sodium sulfate column, transferred to a chicken heart bottle, concentrated to near dryness with a rotary evaporator at 40°C, and then reconstituted with 1 mL of absolute ethanol, and each treatment was repeated three times. 2. Fluorescent reaction. Take 4 μL of the above absolute ethanol solution in a 10 mL colorimetric tube, dilute to the mark with 80% concentrated sulfuric acid, mix well, and let stand for 240 min to react. 3. Sample determination. The scanning parameters of the fluorescence spectrometer were set as: excitation wavelength / emission wavelength = 218 nm / 363 nm, photomultiplier tube voltage 700 V, exci...

Embodiment 2

[0020] DnBP recovery rate experiment in embodiment 2 water sample

[0021] 1. Take 25mL of the solution to be tested in a 60mL separatory funnel, add dichloromethane twice (5mL each time), shake manually for 3min (pay attention to outgassing), let it stand for 25min, extract the PAEs in the solution, combine the organic phase, and pass Anhydrous sodium sulfate column, transferred to a chicken heart bottle, evaporated to dryness and concentrated with a rotary evaporator at 40°C, and then reconstituted with 1 mL of absolute ethanol, and each treatment was repeated three times. 2. Fluorescent reaction. Take 4 μL of the above absolute ethanol solution in a 10 mL colorimetric tube, dilute to the mark with 80% concentrated sulfuric acid, mix well, and let stand for 240 min to react. 3. Sample determination. The scanning parameters of the fluorescence spectrometer were set as: excitation wavelength / emission wavelength = 218 nm / 363 nm, photomultiplier tube voltage 700 V, excitation...

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Abstract

The invention relates to a chemical substance detection method, and especially relates to a method for detecting phthalate substances in an environmental sample. The method comprises the following steps: extraction of PAEs from the environmental sample, a fluorescence reaction, sample determination, and drawing of a standard working curve. The standard working curve is obtained through the following steps: detecting the fluorescence intensity of a DnBP standard solution reaction system by a fluorospectrophotometer three times, averaging the obtained resuls, and linearly fitting the obtained average value and the corresponding DnBP concentration. The phthalate fluorescence analysis method has the advantages of simplicity in operation, fast analysis speed, and good precision, the detection limit is 8.2 * 10<-3> mg.L<-1>, the RSD of parallel samples is 5.6%, the recovery rate of DnBP in a soil sample is 95-120%, the recovery rate of the DnBP in a water sample is 90-115%, and the method can be used for detecting the total amount of the PAEs in the environmental sample, and has certain practical application values.

Description

technical field [0001] The invention relates to a method for detecting chemicals, in particular to a method for detecting phthalates in environmental samples. Background technique [0002] Phthalates (PAEs) are an important class of industrial raw materials. Because they are not volatile and have high tolerance to adverse environments such as severe cold and high temperature, they are widely used as plasticizers and added to plastic products. . However, PAEs and plastic matrix molecules do not form covalent bonds, but are connected by hydrogen bonds or van der Waals forces with lower bond energy, and are easy to migrate to the external environment. At present, PAEs can be detected in soil, water, atmosphere and even organisms. Studies have shown that PAEs have environmental estrogen effects, and can be concentrated, accumulated, and amplified along the food chain, and eventually endanger human health. The environmental pollution caused by them has attracted global attentio...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N21/01
CPCG01N21/6402G01N21/01
Inventor 李玉双李冰陈琳刘厶瑶侯永侠宋雪英
Owner SHENYANG UNIV
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