Method for analyzing volatile phenolic compounds in water based on ultrasonic-assisted in-situ bubbling and simultaneous derivation-dispersion liquid-liquid microextraction
An ultrasound-assisted, liquid-dispersed technology, applied in the direction of analysis of materials, material separation, measurement devices, etc., can solve the problems of solvent waste solubility, difficulty in phase separation of large-volume samples, unusable analysis, etc., and achieve the effect of reducing pollution
Pending Publication Date: 2020-06-09
ZHEJIANG UNIV OF TECH
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Problems solved by technology
However, when large-volume water samples are subjected to dispersion liquid-liquid microextraction technology, they will encounter the bottleneck of complete emulsification and difficult emulsification.
On the one hand, when the volume of the aqueous solution is enlarged, the amount of dispersant increases, resulting in a waste of solvent and a decrease in the solubility of the target analyte in the extractant. If the air-assisted method is used, the operation will be cumbersome and labor-intensive; on the other hand, Due to the limitation of the size of the centrifuge tube by the general laboratory centrifuge, it is difficult to separate the phase of large-volume samples through the laboratory centrifuge, so that the centrifugal demulsification method cannot be used for the analysis of large-volume water samples.
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Embodiment 1
[0031] Example 1: Extraction and Analysis of Volatile Phenolic Compounds in Water Samples
[0032] (1) Preparation of standard solution
[0033]Stock solution: Dissolve 8 kinds of volatile phenol mixed standard substances in methanol to obtain a concentration of 10.0 μg·mL -1 The mixed standard stock solution was stored at -4°C in the dark.
[0034] The standard curve working solution was obtained by serially diluting the stock solution with deionized water.
[0035] (2) Preparation of volatile phenol derivative standard reagent (preparation of volatile phenol acetate)
[0036] Pipette 1 mL of 8 kinds of volatile phenol stock solutions (10.0 μg·mL -1 ) in a 10mL brown volumetric flask, dilute to volume with acetonitrile (1.0μg·mL -1 ). After the solution is uniform and stable, pipette 0.50 mL into a 1 mL brown bottle, add 50.0 μL of pyridine, mix ultrasonically, add 0.10 mL of acetic anhydride, and heat at 80°C for 30 minutes to complete the reaction. Afterwards, it was ...
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Abstract
The invention discloses a method for analyzing volatile phenolic compounds in water based on ultrasonic-assisted in-situ bubbling and simultaneous derivation-dispersion liquid-liquid microextraction.The method comprises the following steps: mutually dissolving an extracting agent and acetic anhydride, injecting into a K2CO3-containing sample aqueous solution, carrying out ultrasonic treatment for15-75s, adding edible salt water to raise the liquid level, sucking an upper-layer organic phase, drying with anhydrous sodium sulfate, and injecting into GC-MS for analysis. According to the method,an in-situ generated carbon dioxide bubbling demulsification technology and a dispersion liquid-liquid microextraction technology are combined for the first time so that the problem that demulsification is performed by using centrifugation in a traditional dispersion liquid-liquid microextraction method is solved, and the method can be suitable for pretreatment operation of water samples with different volumes; an organic solvent with low density and low toxicity is used as an extracting agent so that the defect that halogenated alkane with the density greater than that of water is used as the extracting agent in the traditional dispersion liquid-liquid microextraction method is overcome, and the pollution to the environment is reduced. The method can be combined with reality to provide afavorable detection means for volatile phenolic compounds in the environment.
Description
technical field [0001] The invention relates to a method for analyzing residues of volatile phenolic compounds in water, in particular to a method for analyzing volatile phenolic compounds in water by ultrasonic-assisted in-situ generation of carbon dioxide gas bubbling and simultaneous derivation-dispersion liquid-liquid microextraction. Background technique [0002] Volatile phenols refer to chlorine atom-substituted, methyl-substituted and nitro-substituted phenolic compounds. Due to the high solubility and low vapor pressure of these compounds in water, they can enter the environment through water or atmospheric systems, and are considered to be the most important environmental pollutants in today's environment. one of the main pollutants in the Chlorophenols are widely used in agriculture, pharmaceuticals, dyeing, and petrochemical industries. At the same time, studies have shown that chlorophenols can also be used as precursors of dioxins and furans. Among them, penta...
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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/062G01N2030/065
Inventor 李祖光徐方祥聂晶李上
Owner ZHEJIANG UNIV OF TECH