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Fluorescent sensor for measuring picric acid content and preparation method thereof

A picric acid and chemical sensor technology, applied in the field of fluorescence sensor, can solve the problems of high detection limit of spectrophotometry, shortened service life of chromatographic column, many operation steps, etc., and achieves the effects of online measurement, simple structure and easy synthesis

Inactive Publication Date: 2012-12-19
JIANGSU RADIO & TV UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection limit of spectrophotometry is relatively high, but there are more operation steps
Liquid chromatography requires extraction and concentration, and the operation is relatively cumbersome. Gas chromatography analyzes the aqueous solution of picric acid. Moisture will shorten the service life of the chromatographic column, and seriously cause the chromatographic column to fail.

Method used

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  • Fluorescent sensor for measuring picric acid content and preparation method thereof
  • Fluorescent sensor for measuring picric acid content and preparation method thereof
  • Fluorescent sensor for measuring picric acid content and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Synthetic steps of allyl tetraiodofluorescein The synthetic route in the reference (Anal. Chim. Acta, 1997: V342 207-213), the specific steps are as follows:

[0017] Sodium tetraiodofluorescein (compound A) and bromopropene (compound B) with a molar ratio of 1:3 were stirred in N,N-dimethylformamide at 80°C for 3 hours to fully react, After the reaction was completed, the N,N-dimethylformamide was removed by rotary evaporation, and the obtained solid was dissolved in water, and 0.2mol l -1 The hydrochloric acid was adjusted to acidity, resulting in a red precipitate, which was filtered, dried, and recrystallized from ethanol. A tetraiodofluorescein derivative (compound C) with a terminal double bond was obtained with a yield of 65%, MS: (M+H) + 877.

[0018]

[0019] The nitro group on the aromatic ring in picric acid is a strong electron-withdrawing group, which forms a fluorescent complex with tetraiodofluorescein, resulting in the fluorescence quenching of tetr...

Embodiment 2

[0021] The preparation and determination of the fluorescent sensor include the following steps:

[0022] 1. Silanization of glass slides: Soak quartz glass slides (diameter 12.5mm) in chromic acid lotion for 40 minutes, then soak them in 3% hydrofluoric acid for 30 minutes, and then rinse them with distilled water so that they are no longer stained. There is 3% hydrofluoric acid, then add 10% hydrogen peroxide and soak for 30 minutes. Then rinse with distilled water. Measure 0.2ml propyl methacrylate with a dry pipette, 2ml 0.2mol l -1 The acetic acid-sodium acetate buffer solution with a pH of 3.6 was mixed with 8 ml of distilled water, and stirred for 10 minutes to completely dissolve the propyl methacrylate to prepare a silylation solution. The slides were immersed in this solution for 2-3 hours, then washed with distilled water, and dried at room temperature for later use.

[0023] 2. Preparation of the optode film: Dissolve 15 mg of allyl tetraiodofluorescein in 0.2 ml...

Embodiment 3

[0025] Embodiment 3: Determination of correction equation

[0026] Different concentrations of picric acid solution (0mol l -1 , 1×10 -7 mol l -1 , 1×10 -6 mol l -1 ,1×10 -5 mol l -1 ,1×10 -4 moll -1 ,1×10 -3 mol l -1 ,1×10 -2 mol l -1 ,0.5×10 -1 moll -1 , 1×10 -1 moll -1 ) are respectively input into the flow cell by the peristaltic pump at a speed of 1.3ml / min, and a stable fluorescence intensity (I) can be obtained after the optode membrane and the solution reach equilibrium. Use Sigmaplot software for straight line fitting, when the picric acid concentration is 1×10 -7 ~0.5×10-1 mol l -1 When between, there is a good linear relationship between -lnC and fluorescence intensity, such as image 3 As shown, the correction equation obtained is: I=7.43(-ln C)+353.05(R=0.9940). The concentration of picric acid is 1×10 -7 ~0.5×10 -1 mol l -1 Between, it can be used as a sensor to measure the quantitative relationship of picric acid.

[0027] Put the sample o...

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Abstract

The invention discloses a fluorescent sensor for measuring the picric acid content. A fluorescent carrier in a film substrate monomer is an allyl four iodine fluorescein. 15mg of fluorescent carrier allyl four iodine fluorescein is dissolved in 0.2ml of N, N-dimethylformamide for sufficient dissolution, 200mg of acrylamide, 0.4ml of hydroxyethyl methylacrylate, 0.15ml of cross-linking agent triethoxy trimethyl acrylate and 0.2ml of triethanolamine are added, finally 0.25ml of 1-oxhydryl cyclohexyl phenyl ketone is added for even mixing; and a solution is removed to drop on a Teflon plate, a quartz slide subjected to silanization is covered on the Teflon plate, an ultraviolet lamp is used for irradiating for 20 minutes, and drying is carried out at a room temperature. The sensor has the advantages of simple preparation, good stability, short response time, good reproducibility and the like, and can continuously and timely measure the picric acid content on line.

Description

technical field [0001] The invention relates to a fluorescent sensor, in particular to a fluorescent sensor for measuring picric acid content and a preparation method thereof. Background technique [0002] Picric acid, scientific name 2,4,6-trinitrophenol, belongs to nitrophenol compounds, is light yellow crystalline solid, odorless, bitter taste. It is mainly used in the manufacture of explosives, fungicides and fungicides in agriculture, fungicides and astringents in medical treatment, etc. It is harmful to eyes, skin, respiratory tract and digestive tract. If it is inhaled, it can cause symptoms such as headache, dizziness, nausea, vomiting, loss of appetite, diarrhea and fever, and damage red blood cells, causing hemorrhagic nephritis, hepatitis and jaundice. As a strong oxidant, it can react violently with combustibles and reducing agents to cause combustion and explosion. Can corrode metals, and the resulting metal salts are extremely sensitive to shock or heat. If ...

Claims

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Application Information

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IPC IPC(8): G01N21/64
Inventor 秦品珠唐荣韩承辉牛承岗干方群
Owner JIANGSU RADIO & TV UNIV
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