Detection method of phthalates and degradation products in environmental water samples

A technology of phthalic acid monoester and phthalic acid, which is applied in the field of water environment quality detection and analysis, can solve the problems of difficult treatment, secondary pollution of the environment, complex matrix, etc., and achieve large enrichment multiples and high extraction efficiency , the effect of using less

Inactive Publication Date: 2018-06-01
JIANGSU UNIV
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The n-octane-water partition coefficient logP and acidity coefficient pKa of PAEs and their degradation products MPEs are quite different, the matrix in the water body is complex, and the pretreatment such as purification and enrichment is difficult
[0004] The existing pretreatment methods for detecting phthalates, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), need to use a large amount of toxic organic solvents, which damage the health of analysts and easily cause secondary pollution to the environment. Secondary pollution; solid phase microextraction (SPME) is subject to many restrictions in practical application due to the limited service life of the extraction fiber, which is easy to break and may have residues during the analysis process

Method used

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  • Detection method of phthalates and degradation products in environmental water samples
  • Detection method of phthalates and degradation products in environmental water samples
  • Detection method of phthalates and degradation products in environmental water samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Standard solution adopts national standard substance preparation, selects diethyl phthalate, di-n-butyl phthalate, bis(2- There are 6 kinds of ethylhexyl) ester, monoethyl phthalate, monobutyl phthalate, and mono(2-ethylhexyl) phthalate. First prepare a 1g / L stock solution with methanol, take 100μl each of the six standard stock solutions in a 10mL volumetric flask, dilute to 10ml with methanol, and prepare a mixed standard solution. The concentration of each target pollutant is 10mg / L. L.

[0029] In order to verify the separation effect of high performance liquid chromatography, the above mixed standard solution was taken for HPLC analysis. The liquid chromatograph used in the test is the Breeze2 liquid chromatographic system of Waters Company in the United States, 1525 binary pump, 2707 automatic sampler, 2489 ultraviolet / visible detector; Eclipse XDB-C18 liquid chromatographic separation column, 150mm × 4.6mm, granular Diameter 5μm; column temperature 30℃; injecti...

Embodiment 2

[0031]Standard solution adopts national standard substance preparation, selects diethyl phthalate, di-n-butyl phthalate, bis(2- There are 6 kinds of ethylhexyl) ester, monoethyl phthalate, monobutyl phthalate, and mono(2-ethylhexyl) phthalate. First prepare a 1g / L stock solution with methanol, take 100μl each of the six standard stock solutions in a 10mL volumetric flask, dilute to 10ml with methanol, and prepare a mixed standard solution. The concentration of each target pollutant is 10mg / L. L.

[0032] In order to obtain the standard curve of the six target pollutants, the above 10 mg / L mixed standard solution was diluted with ultrapure water into a series of simulated polluted water samples (0.1-100 μg / L) with different concentrations.

[0033] Take a 12cm-long polypropylene hollow fiber (inner diameter 280 μm, wall thickness 50 μm, pore diameter 0.1 μm, porosity 60%), place it in acetone for ultrasonic cleaning to remove surface impurities, and dry it for later use; mm, ...

Embodiment 3

[0041] The established method was used to enrich and detect phthalates and their degradation products in two kinds of environmental water samples, namely tap water in the laboratory and river water in the Zhenjiang section of the Beijing-Hangzhou Grand Canal.

[0042] Take a 12cm-long polypropylene hollow fiber (inner diameter 280 μm, wall thickness 50 μm, pore diameter 0.1 μm, porosity 60%), place it in acetone for ultrasonic cleaning to remove surface impurities, and dry it for later use; mm, length 8mm, syringe volume 0.5mL) inject ultrapure water (adjust the pH value to 10 with NaOH) as the receiving phase into the cavity of the hollow fiber; Hexafluorophosphate, 1-hexyl-3-methylimidazolium hexafluorophosphate, and 1-octyl-3-methylimidazolium hexafluorophosphate are mixed in a volume ratio of 1:1:1), and ultrasonically oscillated for 30 Seconds, a liquid film is formed in the micropores of the hollow fiber membrane wall; the ionic liquid remaining on the surface of the fib...

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Abstract

The invention discloses a method for detecting phthalate compounds and degradation products thereof in an environmental water sample, and belongs to the field of water environment quality detection and analysis. According to the polarity of a substance to be detected, the ratio of ionic liquid is optimized, through the capillary force, the ionic liquid is filled into pores of hollow fiber membrane wall to form a liquid membrane, the pH value of sample and acceptor is adjusted to a proper range, and the acceptor is encapsulated in the cavity of the hollow fiber membrane to produce an extraction apparatus. The extraction apparatus is placed in a sample, and thus a two phase (water / organic solvent) system or a three phase (water / organic solvent / water) system is formed. After enrichment, purification, and methanol elution, HPLC (high performance liquid chromatography) is used to analyze the target pollutant concentration. The method can be used to detect the phthalate plasticizer in the environment, provides data for environmental behavior analysis of phthalate plasticizer, evaluates the quality of environmental water, and has the advantages of rapidness, reliability, simple operation, and environment-friendliness.

Description

technical field [0001] The invention relates to a method for detecting phthalate plasticizers in environmental water samples, in particular to a method for enriching and detecting phthalates in environmental water samples using a hollow fiber-supported ionic liquid liquid-phase microextraction method. The invention discloses a method for formate ester compounds and degradation products thereof, belonging to the field of detection and analysis of water environment quality. Background technique [0002] Phthalate esters (PAEs), as one of the most commonly used plasticizers, are mainly used in the polyvinyl chloride processing industry, and can also be used as pesticide carriers, cosmetics, lubricants, detergents, and paints. Raw materials, even alternatives to palm oil, are illegally added to food. Since such compounds are only connected to the plastic matrix through hydrogen bonds or van der Waals forces, and are not polymerized into the polymer carbon chain of the plastic, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/062
Inventor 朱方徐超孙国茂薛永来杜道林
Owner JIANGSU UNIV
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