Detecting method of aromatic amine compound in water sample

A detection method and aromatic amine technology, applied in the field of analytical chemistry, can solve the problems of harmful human health, lower dispersion coefficient, lower sensitivity, etc., and achieve the effects of reducing environmental pollution, high sensitivity and low detection limit

Inactive Publication Date: 2012-01-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the use of a dispersant, the dispersion coefficient of the analyte in the extractant decreases, resulting in a decrease in sensitivity
In addition, the extractant and dispersant used in this experiment are all organic reagents, polluting the environment and harmful to human health

Method used

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  • Detecting method of aromatic amine compound in water sample
  • Detecting method of aromatic amine compound in water sample
  • Detecting method of aromatic amine compound in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The influence of embodiment 1 extractant kind

[0032] Adjust the pH value of the water sample to 13.0, add 50 μL [C4 MIM][PF 6 ] or [C 6 MIM][PF 6 ], and then at a speed of 2800 rpm, the mixture was vortexed for 2 min. Centrifuge at 3600rpm for 5min, and the ionic liquid phase is deposited at the bottom of the centrifuge tube. Remove the supernatant and add 380 μL of mobile phase to dissolve the ionic liquid phase. Take 3 μL of the diluted solution and inject it into an ultra-fast liquid chromatograph for analysis.

[0033] The effects of two ionic liquids on the peak areas of three aromatic amines are as follows: figure 1 As shown, [C 6 MIM][PF 6 ] is used as an extractant to obtain a peak area greater than that of [C 4 MIM][PF 6 ] as the peak area obtained when the extractant was used. This is because [C 4 MIM][PF 6 ] Solubility in water (1.88g / 100mL) is greater than [C 6 MIM][PF 6 ] solubility (0.75g / 100mL), so in the extraction process, [C 4 MIM][PF ...

Embodiment 2

[0034] The influence of embodiment 2 extractant volume (consumption)

[0035] Process is with embodiment 1. After the pH value of the water sample was adjusted to 13.0, 40 μL, 45 μL, 50 μL, 55 μL, 60 μL and 65 μL of [C 6 MIM][PF 6 ] was added to the water sample, and then the mixture was vortexed for 2 min at a speed of 2800 rpm. Centrifuge at 3600 rpm for 5 min.

[0036] The effect of different extractant volumes on the peak areas of the three aromatic amines is as follows: figure 2 shown, indicating that with [C 6 MIM][PF 6 ] volume increases, the peak area of ​​aromatic amines increases accordingly. But when [C 6 MIM][PF 6 ] When the volume exceeds 50 μL, the peak area gradually decreases. Therefore, the optimal extractant volume is 50-55 μL.

Embodiment 3

[0037] The influence of embodiment 3 vortex meter rotational speed

[0038] Process is with embodiment 1. Adjust the pH value of the water sample to 13.0, add 50 μL [C 6 MIM][PF 6 ], and then at 560rpm, 1120rpm, 1400rpm, 1960rpm, 2520rpm and 2800rpm, respectively, the mixture was vortexed for 2min. Centrifuge at 3600 rpm for 5 min.

[0039] The influence of different rotational speeds on the peak areas of the three aromatic amines is as follows: image 3 As shown, it shows that the peak areas of all aromatic amines increase correspondingly with the increase of rotational speed. Therefore, the optimum rotational speed of the vortex instrument is 2520-2800rpm.

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Abstract

The invention discloses a detecting method of an aromatic amine compound in a water sample, belonging to the technical field of analytical chemistry. The aromatic amine compound is p-chloroaniline, 1-naphthylamine and 4-aminobiphenyl. The detecting method comprises extraction and detection processes, ionic liquid [C6MIN][PF6]or[C4MIM][PF6] is used as an extracting agent, vortex oscillation is adopted to assist the ionic liquid in carrying out microextraction, an ultra fast liquid chromatograph is used for detecting, and a regressive curve equation is used for obtaining a detection result. The detecting method provided by the invention has high sensitivity, low detection limit and good degree of precision; a green reagent is used as the extracting agent, thus, using an organic reagent isavoided, and pollution to the environment is reduced; the detecting method has the characteristics of rapidness, stability and the like, and the time for detecting samples is greatly shortened; and the detecting method can be applied to the detection of the aromatic amine compounds in various water samples and has a certain social significance on protecting the environment and the health of humanbeings.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for rapidly extracting three aromatic amines in environmental water samples with eddy current-assisted ionic liquids, and then detecting them with an ultra-fast liquid chromatograph. Background technique [0002] Aromatic amine compounds are one of the important raw materials for the synthesis of epoxy resins and polyurethane polymer materials, and are widely used in industrial production such as rubber, plastics, pesticides, dyes, photography and pharmaceuticals. These compounds are highly toxic and potentially carcinogenic. With the discharge of industrial wastewater, they seep into the soil and enter the water system, bringing great safety hazards to people's lives. In 1970, the U.S. Environmental Protection Agency placed several toxic and potentially carcinogenic aromatic amine compounds on the Priority Control List. In order to protect huma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 宋大千孙颖孙秀敏吴丽威姜春竹王丽英高岩于希
Owner JILIN UNIV
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