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A kind of method using triphenylamine dye to detect sulfite

A technology of sulfite and triphenylamine, applied in measuring devices, analysis materials, material excitation analysis, etc., can solve the problems of continuous detection, large sample consumption, high detection cost, etc., achieve low detection limit, low detection cost, Simple operation effect

Active Publication Date: 2019-04-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a high detection limit up to ppb level, response within 10min, low detection cost and simple operation in view of the existing problems of high detection cost, complicated operation, large amount of samples and inability to continuously detect the existing technology. Selective and sensitive method for the detection of sulfite using triphenylamine dyes

Method used

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  • A kind of method using triphenylamine dye to detect sulfite
  • A kind of method using triphenylamine dye to detect sulfite
  • A kind of method using triphenylamine dye to detect sulfite

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Experimental program
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Effect test

Embodiment 1

[0027] 1. Preparation of triphenylamine dyes

[0028] Add 1.3655g (5mmol) 4‐(diphenylamine) benzaldehyde, 0.6608g (10mmol) malononitrile and an appropriate amount of triethylamine into a 100mL flask, and then add 50mL of absolute ethanol. After reacting at room temperature for 24 hours, the solvent was distilled off under reduced pressure, and the residual solid was purified with a silica gel column under the condition that the eluent composition was ethyl acetate:n-hexane=1:8 (v / v) to obtain 1.2521 g of a yellow solid. Yield 78%.

[0029] 2. Compound Characterization

[0030] 1 H NMR (400MHz, DMSO-d 6 )δ (ppm): 8.20 (s, 1H), 7.82 (d, J = 8.5Hz, 2H), 7.44 (t, J = 7.5Hz, 4H), 7.26 (dd, J = 19.7, 7.4Hz, 6H) , 6.83 (d, J=8.5Hz, 2H).

[0031] 13 C NMR (100MHz, DMSO-d 6)δ (ppm): 159.30, 152.89, 144.70, 133.07, 130.13, 126.77, 126.24, 122.58, 117.41, 115.37, 114.42, 73.73;

[0032] IR(v -1 , KBr): 3057, 2216, 1610, 1590, 1568, 1506, 1440, 1349, 1317, 1241, 1189, 830, 763, 6...

Embodiment 2

[0038] Detection of Sulfite Ion with Triphenylamine Dye

[0039] (1) Prepare a triphenylamine dye acetonitrile solution with a concentration of 25 mM, take 2 parts of 10 μL triphenylamine dye acetonitrile solution respectively, add distilled water to dilute to 10 mL, and obtain 2 parts of triphenylamine dye aqueous solution;

[0040] (2) preparation concentration is the sodium sulfite aqueous solution of 30mM, and concentration is the sodium bisulfate aqueous solution of 30mM;

[0041] (3) Add dropwise 0.1 mL of sodium sulfite aqueous solution and 0.1 mL of sodium bisulfate aqueous solution prepared in step (2) respectively in 2 parts of 10 mL of triphenylamine dye aqueous solution, after mixing evenly, observe the triphenylamine dye aqueous solution under 365 nm light excitation changes in fluorescence.

[0042] The results showed that the fluorescence of the triphenylamine dye aqueous solution was quenched after the sodium sulfite aqueous solution was added, and the fluores...

Embodiment 3

[0044] Detection of Sulfite Ion with Triphenylamine Dye

[0045] (1) Prepare a triphenylamine dye DMSO solution with a concentration of 30 mM, take 2 parts of 10 μL triphenylamine dye DMSO solution respectively, add distilled water to dilute to 10 mL, and obtain 2 parts of triphenylamine dye aqueous solution;

[0046] (2) preparation concentration is the sodium sulfite aqueous solution of 40mM, and concentration is the sodium dihydrogen phosphate aqueous solution of 60mM;

[0047] (3) Add dropwise 0.1 mL of sodium sulfite aqueous solution and 0.1 mL of sodium dihydrogen phosphate aqueous solution prepared in step (2) respectively to 2 parts of 10 mL of triphenylamine dye aqueous solution, and after mixing evenly, observe triphenylamine dye under 365 nm light excitation Fluorescence changes in aqueous solutions.

[0048] The results showed that the fluorescence of the triphenylamine dye aqueous solution was quenched after the sodium sulfite aqueous solution was added, and the ...

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Abstract

A method of detecting sulfite through applying triphenylamine dye is disclosed. The method includes (1) dissolving the triphenylamine dye into a hydrophilic organic solvent to prepare a triphenylamine dye stock solution, weighing a proper amount of the triphenylamine dye stock solution, and diluting with water to obtain an aqueous triphenylamine dye solution, and (2) adding dropwise a sample to be detected, and observing whether fluorescence of the aqueous triphenylamine dye solution quenches or not under excitation with light the wavelength of which is 365 nm, wherein the sample is determined to contain sulfite, cyanide or ferric ion if the fluorescence quenches, and whether the sample contains the sulfite or not is determined by further assistant distinguishing through a 1H NMR spectrum. The method is advantaged by high selectivity and sensitivity, capability of being hardly interfered by other anions, a low detection limit which can be a ppm level, rapid response that is within 10 min, a low detection cost, simple operation, and the like.

Description

technical field [0001] The invention relates to a triphenylamine compound, in particular to a method for detecting sulfite using a triphenylamine dye. Background technique [0002] Anions play an important role in environmental protection, industrial production and biological applications. Excessive sulfite and its oxidation products will produce side effects and acute symptoms, endangering human health. The detection methods of sulfite ion include atomic absorption spectrophotometry, flame photometry, electron probe microanalysis and ion selective electrode method, etc., which have problems such as high detection cost, complicated operation, large sample consumption and inability to continuously detect. Fluorescent probes have the advantages of high selectivity and sensitivity, low detection limit, rapid response, low detection cost and simple operation. Therefore, exploring fluorescent probes with high selectivity and sensitivity has aroused the interest of many research...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
CPCG01N21/643G01N2021/6432
Inventor 瞿金清杨小东刘瑞源
Owner SOUTH CHINA UNIV OF TECH