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O-phenylenediamine detection method based on nano-interface energy transferring

A technology of o-phenylenediamine and energy transfer, applied in the detection field, can solve the problems of low detection limit, cumbersome operation, high detection limit, etc., and achieve the effect of low detection cost, simple operation and low detection limit

Inactive Publication Date: 2015-12-30
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The spectrophotometric method uses silver ions to be reduced to nano-silver under certain conditions to realize the detection of o-phenylenediamine (LiNanetal., Colorimetric determination of ofo-phenylenediamine in water samples based on the formation of silver nanoparticles as a colorimetric probe, SpectrochimicaActaPartA2015 No. 140), this method is simple, fast, and low in cost, but the detection limit High, with a linear range of 1×10 -6 mol L -1 ~8×10 -5 mol L -1 High-performance liquid chromatography, gas chromatography and gas chromatography-mass spectrometry (Wan Baopo, pilot test research on the production process of white o-phenylenediamine, China Chemical Industry Trade 2012 No. 7) have high sensitivity and low detection limit advantages, but due to complex equipment and cumbersome determination process, it is not suitable for widespread promotion and rapid detection, and requires professional and technical personnel to operate; electrochemical methods use perovskite composite nanomaterials LaNiTiO 3 -Fe 3 o 4 Modified glassy carbon electrode to detect the response current of o-phenylenediamine (such as patent CN103543188A), when performing the measurement, an electrochemical workstation and a three-electrode system are required, and the operation is cumbersome

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  • O-phenylenediamine detection method based on nano-interface energy transferring

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Experimental program
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Embodiment 1

[0025] Embodiment 1: the preparation of gold nano

[0026] All glass instruments used in the preparation process were soaked in aqua regia (concentrated hydrochloric acid:concentrated nitric acid=3:1) for at least 5 hours, washed and dried for later use. In a flat bottom flask was added 39.2 mL of distilled water, 2% (w / v) HAuCl 4 Solution 0.82mL, mix well, place on a magnetic stirrer, heat and stir until boiling, then add 6.4mL, 38.8mmol·L -1 Sodium citrate solution, the color of the solution can be seen from yellow to black to wine red within 1min. After continuing to heat and stir for 15min, stop heating and continue to stir until the solution is cooled to room temperature. Filter it into a brown reagent bottle with a 0.22μm filter membrane to obtain nano-gold .

[0027] According to Lambert-Beer's law, when the molar absorptivity is 2.7×10 8 m -1 cm -1 , the concentration of the gold nanometer (AuNPs) solution was calculated to be 8.8nM using the absorbance at 520nm. ...

Embodiment 2

[0028] Example 2: Nanointerface Energy Transfer Donor Selection

[0029] In this example, four nano-interface energy transfer donors were tested: one anionic fluorescent dye (eosin B) and three cationic fluorescent dyes (rhodamine 6G, acridine orange, and saffron T). The final concentrations of the four nanointerfacial energy transfer donors were 2.50×10 -5 mol L -1 , 2.50×10 -7 mol L -1 , 1.25×10 -6 mol L -1 , 2.50×10 -5 mol L -1 . According to the quenching efficiency formula of AuNPs to organic fluorescent dyes: η=1-(F / F 0 ), where F, F 0 are the fluorescence intensities of the fluorescent molecules with and without the quencher under the optimal measurement conditions, respectively, and η is the quenching efficiency.

[0030]Calculated by the formula, the quenching efficiencies of AuNPs to rhodamine 6G, acridine orange, saffron T and eosin B are respectively: 96%, 57%, 55%, 60%. Rhodamine 6G has the best quenching effect, with a quenching efficiency of 96%. The ...

Embodiment 3

[0031] Embodiment 3: selectivity experiment

[0032] When the concentration of o-phenylenediamine is 6.0×10 -7 mol L -1 , the influence of possible interfering substances on the system was investigated, and when the relative deviation was not greater than ±10%, 6.0×10 -6 mol L -1 Cd 2+ , Ba 2+ , Ni 2+ , Pb 2+ , Cu 2+ , Zn 2+ , Cr 3+ ,P0 4 3- , CO 3 2- , PO 4 3- , SO 4 2- , Nitrobenzene, phenol, ethanol, glucose, tryptophan do not interfere.

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Abstract

The invention provides an o-phenylenediamine detection method based on nano-interface energy transferring. The o-phenylenediamine detection method comprises the following steps: (1) mixing a sodium citrate buffering solution, a gold nanoparticle solution and an energy transferring donor solution at a volume ratio of (2-7) to (2-6) to 1, and then adding an o-phenylenediamine standard working solution; (2) scanning the mixed solution on a fluorescence spectrophotometer and obtaining a mathematical model of o-phenylenediamine and fluorescence intensity F correlation by using a laser wavelength of 529nm. According to the o-phenylenediamine detection method, gold nanoparticles are used as a fluorescence energy transferring receptor, and preferable rhodamine 6G is used as a fluorescence energy transferring donor to establish an efficient nano-interface energy transferring system. The efficient nano-interface energy transferring system is used as the basis for developing a novel o-phenylenediamine detection method; the method can be used for accurately and sensitively detecting the content of o-phenylenediamine in water and the lowest detection limit is 4.5*10<-9>mol / L. A sample does not need a complicated pre-treatment process so that the consumed time is short; the detection cost is much lower than that of a traditional instrument detection method, the detection limit is low and the operation is simple.

Description

technical field [0001] The invention belongs to the detection field, and in particular relates to a method for detecting o-phenylenediamine by using fluorescence. Background technique [0002] O-phenylenediamine (o-phenylenediamine, OPD) is a white crystal, slightly soluble in cold water, soluble in hot water, easily soluble in ethanol, ether and chloroform, is a traditional fine chemical intermediate, mainly used in the production of pesticides, Dyes, drugs, and photosensitive materials, etc. OPD is an internationally recognized carcinogen, which is extremely harmful to the environment and human health. It is now listed as a blacklist of 14 types of environmental pollutants in my country. Acute exposure of the human body can damage the respiratory system, digestive system, liver, and even suffer from cancer. O-phenylenediamine can be absorbed through the skin, causing damage to the liver, and its use in daily necessities is strictly limited. The detection of trace or even...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 周斌张洁郑小莉王永生杨慧仙徐小娜薛金花杨胜园
Owner NANHUA UNIV