A fast and efficient method for detecting trace p-phenylenediamine

A high-efficiency technology for p-phenylenediamine, applied in the field of analysis and detection of p-phenylenediamine, can solve the problems of high detection limit, inability to obtain, enhanced aggregation fluorescence, etc., and achieves high mechanical strength, easy chemical modification, and high optical transparency. Effect

Active Publication Date: 2021-08-03
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Disadvantages of Document 1: First, the conventional liquid phase fluorescence analysis method is still used for the detection of p-phenylenediamine in the prior art, and the detection limit is relatively high
Second, the detection principle of the existing technology is to use salicylaldehyde and p-phenylenediamine to synthesize bis salicylaldehyde-p-phenylenediamine Schiff base, which has the phenomenon of aggregation fluorescence enhancement
In fact, the determination of the oxidant in this link cannot be obtained without creative work by those skilled in the art

Method used

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  • A fast and efficient method for detecting trace p-phenylenediamine
  • A fast and efficient method for detecting trace p-phenylenediamine
  • A fast and efficient method for detecting trace p-phenylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Effect of phenylenediamine concentration on fluorescence intensity of solid phase fluorescence

[0039] A method of detecting phenylenediamine, a base is, including the following steps:

[0040] Step 1: The cellulose solution of cotton cellulose is prepared from 5% mass concentration;

[0041] Step 2: After depulating the cellulose solution obtained by step 1, the substrate flow is derived into a film, and the regenerative cellulose gel film is obtained after solidification;

[0042] Step 3: Putting the regenerated cellulose gel film obtained by step 2 into a 1 g / L of the sodium serotonate solution at room temperature for 6 h, resulting in an aldehydecellulose gel film;

[0043]Step 4: Place the dialdehyde fibers obtained in (3) in different concentrations of phenylenediamine (0, 10, 20, 40, 50, 60, 80, 100, 200, 400, 500, 600, 800) , 1000 μg / L) reaction, to obtain a cellulose film enriched to benzylamine;

[0044] Step 5: Immersing the cellulose membrane of t...

Embodiment 2

[0046] Example 2 Effect of salicyldehyde concentration on fluorescence intensity of solid phase fluorescence

[0047] The concentration of the phenylenediamine solution was 250 μg / L, and the effect of hydrosarian concentration on the fluorescence intensity of solid phase fluorescence was detected. Specific operation: The same diehydecellulosic membrane is placed in a 6 group 250 μg / L in a phenylenediamine solution, and the washed washed after a water bath at a water bath at 25 ° C. The film was then placed in a concentration of 0%, 0.01%, 0.05%, 0.1%, 0.5%, and 1% of the hydrarseofaldehyde solution, washed, and dried in a 50 ° C oven, and then tested each system in 370 nm excitation. Fluorescence spectrum under wavelength. The results show that as the concentration of hydrosalyceal is increased, the fluorescence intensity of the solid phase fluorescence detection film will be slowed down.

Embodiment 3

[0048] Example 3 Effect of oxide aldehyde group concentration on fluorescence intensity of solid phase fluorescence

[0049] Differential aldehyde cellulosic membranes differ from aldehyde content (0, 50, 200, 200, 300, 400 μmol / g) by changing the concentration of sodium the sodium diodate. Thereafter, the resulting dialdehyde film was placed in a p-phenylenediamine solution having a concentration of 250 μg / L, respectively, after 1 h, respectively, after 1 h, washed 1 h, respectively, washed at 25 ° C. The membrane of the enriched phenylenediamine was then placed in a hydrogen solution of 0.5%, washed 10 min, washed, and dried in a 50 ° C oven, and then tested fluorescence spectrum of each system at 370 nm excited wavelength. The results showed that the higher the aldehyde basal amount of diehyde cellulose, the greater the fluorescence intensity of the solid phase fluorescence detection film.

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Abstract

A method for quickly and efficiently detecting trace p-phenylenediamine, specifically, dissolving cotton cellulose to prepare a regenerated cellulose film, using sodium periodate to selectively oxidize the hydroxyl groups on the regenerated cellulose film to aldehyde groups, and then pass The two-step Schiff base reaction prepares solid-phase fluorescence detection membranes of various systems emitting yellow fluorescence, which are used for qualitative analysis and quantitative detection of p-phenylenediamine. The invention has the advantages of simplicity, rapidity, high sensitivity and good selectivity.

Description

Technical field [0001] The present invention relates to an analysis detection method of phenylenediamine, and more particularly to a method of detecting trace amounts of phenylenediamine using a solid phase surface fluorescence spectroscopy. Background technique [0002] Phenylenediamine is an important organic chemical raw material, which is widely used in the production of dyes, pigments, hair dye, rubber anti-aging agents. It can penetrate the human body by inhalation, incoming or skin, causing serious damage to the liver, blood system, nervous system, etc., and potential carcinogenic, mutation, etc. is an important environmental pollutant. [0003] At present, the method for detecting phenylenediamine mainly has ultraviolet-visible spectrophotometry, gas chromatography (GC), high phase liquid chromatography, liquid chromatography - mass spectrometry (GC-MS), electrophoresis, and the like. These methods have low sensitivity, and some instruments are expensive, and some pretrec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
CPCG01N21/6402
Inventor 张胜利刘伯芳张思略胡代燕周祚万裴彥博
Owner SOUTHWEST JIAOTONG UNIV
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