Method for separation and enrichment of trace phthalates in pyridine ionic liquid two-phase system

A technology of dibutyl phthalate and aqueous two-phase system, which is applied in the preparation of test samples and other directions, can solve the problems of poor stability, difficulty in popularization, low sensitivity, etc., and achieves small relative standard deviation and high determination recovery rate. , the effect of a wide linear range

Inactive Publication Date: 2015-10-21
CHANGAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the shortcomings of existing PAEs detection methods such as low sensitivity, poor stability, high cost, long cycle, difficult popularization and environmental pollution, the purpose of the present invention is to provide a pyridine-based ionic liquid two-phase system for separation, A New Method for Enrichment of Trace PAEs in the Environment

Method used

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  • Method for separation and enrichment of trace phthalates in pyridine ionic liquid two-phase system
  • Method for separation and enrichment of trace phthalates in pyridine ionic liquid two-phase system
  • Method for separation and enrichment of trace phthalates in pyridine ionic liquid two-phase system

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Experimental program
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Effect test

Embodiment 1

[0039] Take 39 g of [EPy]Br ionic liquid, place it in a 60 ml Erlenmeyer flask, add 10.89 g of C 4 o 6 h 4 KNa, add 2 ml dibutyl phthalate standard solution and 10 ml distilled water, mix well. At 25 °C and pH 5.0, vibrate and extract in a constant temperature oscillator for 2.5 h and then let it stand still. After the phase separation is clear, measure the concentration of residual dibutyl phthalate in the water phase, from the dibutyl phthalate in the water phase before and after extraction. The content of dibutyl formate calculates the extraction rate of dibutyl phthalate to be 94.67%.

Embodiment 2

[0041] Take 49 g of [EPy]Br ionic liquid, place it in a 60 ml Erlenmeyer flask, add 10.15 g of C 4 o 6 h 4 KNa, add 2 ml dibutyl phthalate standard solution and 10 ml distilled water, mix well. At 15 °C and pH 5.4, vibrate and extract in a constant temperature oscillator for 3 h and then let it stand still. After the phase separation is clear, measure the concentration of residual dibutyl phthalate in the water phase, from the dibutyl phthalate in the water phase before and after extraction. The content of dibutyl formate calculates the extraction rate of dibutyl phthalate to be 95.53%.

Embodiment 3

[0043] Take 39 g of [EPy]Br ionic liquid, place it in a 60 ml Erlenmeyer flask, add 7.96 g of C 4 o 6 h 4KNa, add 2 ml dibutyl phthalate standard solution and 10 ml distilled water, mix thoroughly. Under the conditions of 15 ℃ and pH 5.9, shake and extract in a constant temperature oscillator for 2.5 h and then let it stand still. After the phase separation is clear, the ionic liquid and the water phase are separated, and 39 g of [EPy]Br ionic liquid is added to the water phase , after repeating this three times, measure the concentration of residual dibutyl phthalate in the water phase, calculate the extraction rate of dibutyl phthalate from the content of dibutyl phthalate in the water phase before and after extraction to be 95.98 %.

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Abstract

The invention discloses a new method for separating and enriching trace phthalates in the environment by using a pyridine type ionic liquid aqueous two-phase system. The method comprises the following steps of: evenly mixing 39-49 g of brominated N-ethylpyridine ionic liquid with 7.96-10.89 g of sodium potassium tartrate salt, thereby obtaining an aqueous two-phase extraction system; adding the aqueous two-phase extraction system to 2 ml of to-be-tested dibutyl phthalate aqueous solution, and then carrying out oscillating extraction once to three times in a constant-temperature oscillator under the conditions of a temperature in the range from 15 to 25 DEG C and a pH value in the range from 5.0 to 5.9, wherein the time of extraction each time is 2.5-3 hours; and then standing for phase separation after extraction. The extraction rate of the method for dibutyl phthalate is capable of reaching 98.9%. The method has the characteristics of wide linear range, low detection limit, low relative standard deviation and high yield in sample measurement. Besides, the method is capable of meeting the state requirements for detection of residual phthalates, is quite simple to operate, and is suitable for quantitative analysis of trace and ultra-trace phthalates in the environment.

Description

technical field [0001] The invention belongs to the environmental protection technology field of environmental engineering and analytical chemistry, and specifically relates to a new method for separating and enriching trace / ultra-trace phthalates in the environment of a pyridine-based ionic liquid two-phase system. Simple and accurate. Background technique [0002] Phthalic acid esters (Phthalic Acid Esters, PAEs), also known as phthalates, are an important class of environmental endocrine disruptors, which are characterized by environmental persistence, bioaccumulation, high toxicity, and long-distance migration ability. It is used as a plasticizer (softener) for plastics, a pesticide carrier, and raw materials for the production of insect repellents, clothing, cosmetics, lubricants, etc. Among them, plastic plasticizers are used in the largest amount. PAEs generally exist in high molecular polymers in a physical combination. Over time, free PAEs will slowly seep out of m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/34G01N1/40
Inventor 李宇亮卢筱佳张梦诗苏杭刘倩石江林
Owner CHANGAN UNIV
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