Method for rapidly and efficiently 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 unobtainable, enhanced aggregation fluorescence, high detection limit, etc., and achieve the effects of less sample consumption, high optical transparency and high sensitivity

Active Publication Date: 2019-12-03
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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  • Method for rapidly and efficiently detecting trace p-phenylenediamine
  • Method for rapidly and efficiently detecting trace p-phenylenediamine
  • Method for rapidly and efficiently detecting trace p-phenylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Effect of P-Phenylenediamine Concentration on Fluorescence Intensity of Solid Phase Fluorescence Detection Membrane

[0039] A detection method for p-phenylenediamine is characterized in that it comprises the following steps:

[0040] Step 1: dissolving cotton cellulose to prepare a cellulose solution with a mass concentration of 5%;

[0041] Step 2: after degassing the cellulose solution prepared in step 1, casting the film on the substrate, washing after solidification to obtain a regenerated cellulose gel film;

[0042] Step 3: put the regenerated cellulose gel film obtained in step 2 into 1 g / L sodium periodate aqueous solution and oxidize it at room temperature for 6 hours to obtain a dialdehyde cellulose gel film;

[0043]Step 4: the dialdehyde fiber membrane obtained in (3) is placed in different concentrations of p-phenylenediamine solutions (0, 10, 20, 40, 50, 60, 80, 100, 200, 400, 500, 600, 800 , 1000 μg / L) to react to obtain a cellulose film enri...

Embodiment 2

[0046] Example 2 Effect of Salicylaldehyde Concentration on Fluorescent Intensity of Solid-Phase Fluorescence Detection Membrane

[0047] The concentration of p-phenylenediamine solution was fixed at 250 μg / L, and the effect of salicylaldehyde concentration on the fluorescence intensity of solid-phase fluorescence detection membrane was studied. Specific operation: Put dialdehyde cellulose membranes of the same size into 6 groups of 250 μg / L p-phenylenediamine solutions respectively, react in a water bath at 25°C for 1 hour, take them out and wash them. Then put the film in the concentration of 0%, 0.01%, 0.05%, 0.1%, 0.5%, 1% salicylaldehyde solution to react for 10min, wash with water, and dry in an oven at 50°C, and then test the excitation of each system at 370nm Fluorescence spectra at wavelengths. The results showed that as the concentration of salicylaldehyde increased, the fluorescence intensity of the solid-phase fluorescence detection membrane first increased and th...

Embodiment 3

[0048] Example 3 The influence of the concentration of aldehyde groups in the oxide film on the fluorescence intensity of the solid-phase fluorescence detection film

[0049] Dialdehyde cellulose films with different aldehyde content (0, 50, 100, 200, 300, 400 μmol / g) were obtained by changing the concentration of sodium periodate solution and oxidation time. Afterwards, the obtained dialdehyde cellulose membranes were respectively placed in 6 groups of p-phenylenediamine solutions with a concentration of 250 μg / L, reacted in a water bath at 25° C. for 1 hour, and then removed and washed. Then, the p-phenylenediamine-enriched film was reacted in 0.5% salicylaldehyde solution for 10 minutes, washed with water, and dried in an oven at 50°C, and then the fluorescence spectrum of each system at an excitation wavelength of 370nm was tested. The results showed that the higher the aldehyde group content of dialdehyde cellulose, the greater the fluorescence intensity of the solid-phas...

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Abstract

The invention discloses a method for rapidly and efficiently detecting trace p-phenylenediamine. The method specifically comprises the following steps of dissolving cotton cellulose to prepare a regenerated cellulose membrane; selectively oxidizing hydroxyls on the regenerated cellulose membrane into aldehyde groups by adopting sodium periodate; and carrying out a two-step Schiff base reaction toprepare a solid-phase fluorescence detection membrane of each system for emitting yellow fluorescence, wherein the solid-phase fluorescence detection membrane is used for qualitative analysis and quantitative detection of the phenylenediamine. The method has the advantages of simplicity and quickness, high sensitivity and good selectivity.

Description

technical field [0001] The invention relates to an analysis and detection method for p-phenylenediamine, in particular to a method for detecting trace p-phenylenediamine by using solid-phase surface fluorescence spectroscopy. Background technique [0002] P-phenylenediamine is an important organic chemical raw material, widely used in the production of dyes, pigments, hair dyes, rubber antioxidants, etc. It can penetrate into the human body through inhalation, ingestion or skin, causing serious damage to the liver, blood system, nervous system, etc. It also has potential carcinogenic and mutagenic effects, and is an important environmental pollutant. [0003] At present, the methods for detecting p-phenylenediamine mainly include ultraviolet-visible spectrophotometry, gas chromatography (GC), high-phase liquid chromatography, liquid chromatography-mass spectrometry (GC-MS), and electrophoresis. Some of these methods have low sensitivity, some have expensive instruments, and...

Claims

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Application Information

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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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