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Preparation method of high-fluorescent fluorescence carbon quantum dots and application of high-fluorescent fluorescence carbon quantum dots in Cr (VI) detection

A technology of carbon quantum dots and fluorescent performance, which is applied in the preparation and application of fluorescent sensors with high fluorescent performance, can solve the problems of limited use and inconvenience, and achieve low cost, simple and convenient operation, high detection sensitivity and stability Effect

Inactive Publication Date: 2018-05-29
DALIAN POLYTECHNIC UNIVERSITY
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  • Abstract
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Problems solved by technology

[0002] In the prior art, chromium is a widely used industrial material. Over the past few decades, industry and other anthropogenic processes have continuously released heavy metal ions into the environment. Cr(VI) is a toxic The World Health Organization has proposed a guideline limit of 0.05 mg / L for Cr in drinking water to detect Cr(VI) in order to monitor and reduce the risk of excessive Cr(VI) intake, especially in beverages and The risk in food is very important. In recent years, many analytical techniques have been successfully developed for the determination of Cr(VI) in different sample matrices, such as spectrophotometry, spectrofluorometry, flame atomic absorption spectrometry, inductively coupled plasma Bulk mass spectrometry, diffuse reflectance-Fourier transform infrared spectroscopy, etc., however, most of these methods are inconvenient due to the need for expensive equipment and complex pretreatments, limiting their use in rapid detection, and therefore, are highly desirable for development. A simple, sensitive, selective and low-cost method for Cr(VI) detection; fluorescent carbon quantum dots are a new type of carbon nanomaterials, due to their unique physical and chemical properties, such as low cost, simple synthesis route, Better biocompatibility, lower toxicity, high light and chemical stability, tunable excitation and emission spectra, these excellent properties make CD as a very potential nanosensor and has been successfully used in pH, Fluorescent detection of metal ions and biomacromolecular substances, however, still has several shortcomings that limit the further application of fluorescent carbon quantum dots. Ligand charge transfer) requires an intermolecular interaction between the chemical sensor and the target molecule, thus making the method complex and time-consuming, thus limiting practical applications. On the other hand, the quantum yield is a key indicator of fluorescent materials and is An important fundamental property that determines whether luminescent materials can be used in practical applications. The low quantum yield leads to low sensitivity in the detection system, which is one of the obstacles that prevent fluorescent carbon quantum dots from being used as fluorescent sensors. In order to overcome these shortcomings, high Quantum Yield of Fluorescent Carbon Quantum Dots and the Design of Fluorescence Measurement Systems Based on Alternative Mechanisms In the inner filter effect, since changes in absorbance are transformed exponentially into changes in fluorescence intensity, the sensitivity of this method is enhanced and can be compared with other mechanisms, based on The fluorescence measurement system of fluorescent carbon quantum dots with internal filter effect has been successfully developed. At the same time, doping is an effective method to improve the quantum yield. For example, B, N, S and P can improve the emission properties of carbon quantum dots. Among them, N doping Therefore, it is of great significance to develop fluorescent carbon quantum dots with high fluorescence performance for the detection of Cr(VI).

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  • Preparation method of high-fluorescent fluorescence carbon quantum dots and application of high-fluorescent fluorescence carbon quantum dots in Cr (VI) detection
  • Preparation method of high-fluorescent fluorescence carbon quantum dots and application of high-fluorescent fluorescence carbon quantum dots in Cr (VI) detection
  • Preparation method of high-fluorescent fluorescence carbon quantum dots and application of high-fluorescent fluorescence carbon quantum dots in Cr (VI) detection

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Embodiment 1

[0031]Example 1. Preparation of carbon nanofluorescent probes: Dissolve citric acid (0.35 g) and glycine (0.35 g) in 7 mL of water, and then transfer the solution to a poly(tetrafluoroethylene)-lined autoclave at 190 After heating in an oven at ℃ for 48 hours and naturally cooling to room temperature, a dark brown suspension containing fluorescent carbon quantum dots was obtained. After centrifuging at 4000 rpm for 10 minutes to remove large particles, a D101 macroporous adsorption resin column was used, and water was used as a wash. The crude product was deliquified and purified, and the fluorescent carbon quantum dots were concentrated by a vacuum rotary evaporator, and then freeze-dried to obtain purified fluorescent carbon quantum dots as a white powder. figure 1 ) can detect fluorescent carbon nanoparticles with good particle dispersion and an average particle size of 2.5 nm, which can be detected by fluorescence spectroscopy, ultraviolet spectroscopy (such as figure 2 )...

Embodiment 2

[0032] Example 2, establishment of a standard curve between Cr(IV) concentration and fluorescence intensity: take the fluorescent carbon quantum dots in Example 1 and prepare a carbon nanoparticle solution with a concentration of 0.05 g / ml, and prepare 1 ml of each The carbon nanoparticle solution was used as the blank control group; another 15 centrifuge tubes were added with 1 ml of the prepared carbon nanoparticle solution, and then 5 ml of Cr(IV) were added to the 15 centrifuge tubes with concentrations of 5, 10, 20, respectively. 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 150, 200, 500, 1000 μM aqueous solution, after mixing thoroughly, the obtained carbon nanoparticles and the standard solution of Cr(IV) were allowed to stand for 1 min Finally, the fluorescence intensity F1 in the standard solution was detected by a fluorescence photometer whose detection wavelength range covers 280-700 nm. The detection conditions were that the excitation wavelength was 340 nm, the emiss...

Embodiment 3

[0033] Example 3, detection of actual samples: Take the fluorescent carbon quantum dots in Example 1, take tap water as a sample, and filter through a 0.22 μm membrane before analysis, the concentration of carbon dots is 0.05 mg / mL, take 1 ml of pure water Add 1 ml of the prepared carbon nanoparticle solution as a blank control group, and the measured fluorescence intensity is F 0 , Take 1 ml of tap water and mix it with 1 ml of carbon nanoparticles with a concentration of 0.05 mg / ml to detect the fluorescence intensity F1, according to the linear regression equation (F 0 -F 1 ) / F 0 = 0.00274x+ 0.01637, calculated as not detected.

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Abstract

The invention discloses a preparation method of high fluorescent fluorescence carbon quantum dots. The preparation method comprises the following specific steps: A, dissolving 0.1 to 10g of citric acid and 0.1 to 10g of glycine into 1 to 20mL of water; B, putting a high pressure reactor into a baking oven, heating for several hours under the condition of high temperature and then carrying out natural cooling to room temperature, thus obtaining dark brown suspension containing the fluorescence carbon quantum dots; C, centrifuging the obtained dark brown suspension to remove large particles, using the means of adsorption with macroporous resin, size exclusion chromatography gel or dialysis, purifying a coarse product by using water as eluant and purifying the fluorescence carbon quantum dots; D, concentrating the purified product by using a rotary evaporator at the temperature of 45 DEG C and carrying out freeze-drying to obtain purified fluorescence carbon quantum dots which are white powder. The preparation method of the high fluorescent fluorescence carbon quantum dots, disclosed by the invention, has the advantages of low cost, simple and controllable preparation process, simpleand convenient operation, high sensitivity and selectivity, intuitive detection results and capability of realizing quantitative detection; the obtained carbon quantum dots have the advantages of highquantum yield, long fluorescence life as well as higher detection sensitivity and stability.

Description

technical field [0001] The invention relates to the technical field of preparation and application of a fluorescence sensor with high fluorescence performance, in particular to a preparation method of a fluorescent carbon quantum dot with high fluorescence performance and its application in Cr(VI) detection. Background technique [0002] In the prior art, chromium is a widely used industrial material. Over the past few decades, industry and other anthropogenic processes have continuously released heavy metal ions into the environment. Cr(VI) is a toxic The World Health Organization has proposed a guideline limit of 0.05 mg / L for Cr in drinking water to detect Cr(VI) in order to monitor and reduce the risk of excessive Cr(VI) intake, especially in beverages and The risk in food is very important. In recent years, many analytical techniques have been successfully developed for the determination of Cr(VI) in different sample matrices, such as spectrophotometry, spectrofluoromet...

Claims

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Application Information

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IPC IPC(8): C01B32/15C09K11/65G01N21/64B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C01P2004/64C01P2006/60C09K11/65G01N21/643G01N2021/6432
Inventor 王海涛刘珊谭明乾程沙沙宋玉昆谢伊莎张丽娟那晓康
Owner DALIAN POLYTECHNIC UNIVERSITY
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