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Method for detecting benzopyrene in environmental water sample

A detection method and water sample technology, which is applied in the field of analytical chemistry, can solve the problems of great influence on the enrichment efficiency, endanger the health of experimenters, consume a large amount of organic reagents, etc., and achieve the effect of small harm, low detection limit and high sensitivity

Inactive Publication Date: 2015-07-01
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional liquid-liquid extraction (LLE) method is cumbersome and time-consuming, consumes a lot of organic reagents, pollutes the environment, and endangers the health of experimenters
Solid-phase extraction (SPE) is relatively simple to operate, and the amount of reagents is small, but multi-step operation is required, the enrichment efficiency is greatly affected by the speed of water sample passing through the column, the sample pretreatment time is long, and the cost of commercial columns is high

Method used

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  • Method for detecting benzopyrene in environmental water sample
  • Method for detecting benzopyrene in environmental water sample
  • Method for detecting benzopyrene in environmental water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Determination of benzo(a)pyrene in river water

[0027] 1. N-hexanoic acid modified magnetic nano-Fe 3 o 4 Preparation of solid phase extractant

[0028] Weigh 3.92g (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O, 2.70g FeCl 3 ·6H 2 O, after dissolving with 50mL deionized water, transfer it to a 250mL three-neck flask, under nitrogen protection, mechanically stir (1000rpm) and heat in a water bath to 80°C, then add 5mL acetone solution containing 100μL n-hexanoic acid, continue After stirring for 5 minutes, add 7 mL of concentrated ammonia water, and then slowly add 1 g of n-hexanoic acid within 1 minute. After the mixed solution continues to react for 30 minutes, after cooling to room temperature naturally, the product is collected with an external magnetic field and the reaction solution is discarded. The product is deionized with methanol (methanol and The volume ratio of deionized water is 1:1) and washed 5 times to obtain n-hexanoic acid modified magnetic nano...

Embodiment 2

[0031] Example 2: Determination of benzo(a)pyrene in lake water

[0032] 1. N-decanoic acid modified magnetic nano Fe 3 o 4 Preparation of solid phase extractant

[0033] Weigh 1.49g FeCl 2 4H 2 O, 2.03g FeCl 3 9H 2O, after dissolving with 50mL deionized water, transfer it to a 250mL three-necked bottle, under the protection of nitrogen, mechanically stir (speed: 800rpm) and heat to 70°C in a water bath, then add 5mL acetone solution containing 100mg n-decanoic acid, After continuing to stir for 10 minutes, add 10 mL of concentrated ammonia water, and slowly add 0.8 g of n-decanoic acid within 1 minute. After the mixed solution continues to react for 30 minutes, after cooling to room temperature naturally, the product is collected with an external magnetic field and the reaction solution is discarded. The product is washed with methanol deionized water ( The volume ratio of methanol and deionized water is 1:1) and washed 4 times to obtain n-decanoic acid-modified magne...

Embodiment 3

[0035] Example 3: Determination of benzo(a)pyrene in groundwater

[0036] 1. Undecanoic acid modified magnetic nano Fe 3 o 4 Preparation of solid phase extractant

[0037] Weigh 1.96g (NH 4 ) 2 Fe(SO 4 ) 2 ·6H 2 O, 2.81 g Fe 2 (SO 4 ) 3 9H 2 O, dissolved in 50mL deionized water, transferred to a 250mL three-neck bottle, under nitrogen protection, mechanically stirred (rotating speed: 700rpm) and heated to 60°C in a water bath, then added 5mL methanol solution containing 90mg undecanoic acid, After continuing to stir for 8 minutes, add 5 mL of concentrated ammonia water, and slowly add 0.4 g of undecanoic acid within 1 minute. After the mixed solution continues to react for 30 minutes, after naturally cooling to room temperature, the product is collected with an external magnetic field and the reaction solution is discarded. The product is washed with methanol deionized water ( The volume ratio of methanol and deionized water is 1:1) and washed 3 times to obtain un...

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Abstract

The invention discloses a method for detecting benzopyrene in an environmental water sample. According to the method, alkyl carboxylic acid modified magnetic nano Fe3O4 is utilized to extract polycyclic aromatic hydrocarbon in the environmental water sample, and high performance liquid chromatography / a fluorescence detector is combined for content measurement; the modified magnetic nano Fe3O4 has large specific surface area, good dispersibility in aqueous solution, good selectivity for polycyclic aromatic hydrocarbon, and can reach high enrichment factor after elution of an eluent, and the detection sensitivity can be improved greatly; compared with the traditional sample pretreatment method, according to the pretreatment method, the cost is low and the operation is simple; and besides, the use of organic solvent is reduced greatly, the pretreatment time is shortened, and the magnetic nano Fe3O4 can be utilized repeatedly, is environmentally friendly, and has wide application prospect.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to an alkyl carboxylic acid modified magnetic nano-Fe 3 o 4 It is a solid phase extraction method for the detection of benzo(a)pyrene in environmental water samples. Background technique [0002] Benzo(a)pyrene is a class of persistent organic pollutants with "carcinogenic, teratogenic, and mutagenic" effects. Benzo(a)pyrene in the environment mainly comes from incomplete combustion of carbon-containing compounds. They are commonly found in In various water bodies, it is therefore the priority monitoring object of environmental water in various countries. For example, the US Environmental Protection Agency lists 16 polycyclic aromatic hydrocarbons as priority monitoring organic pollutants, including benzo(a)pyrene. Due to the low content of benzo(a)pyrene in water, pretreatment for separation and enrichment of water samples is usually required before analysis. The traditional ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨亚玲廖文龙
Owner KUNMING UNIV OF SCI & TECH
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