CN110161009B - Application of tin dioxide quantum dots in detection of heavy metal ions in sewage and detection method - Google Patents
Application of tin dioxide quantum dots in detection of heavy metal ions in sewage and detection method Download PDFInfo
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- CN110161009B CN110161009B CN201910569874.1A CN201910569874A CN110161009B CN 110161009 B CN110161009 B CN 110161009B CN 201910569874 A CN201910569874 A CN 201910569874A CN 110161009 B CN110161009 B CN 110161009B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
Abstract
The invention discloses an application and a detection method of tin dioxide quantum dots for detecting heavy metal ions in sewage, wherein the tin dioxide quantum dots have the advantages of no toxicity, good chemical stability, low cost, wide excitation spectrum and narrow emission spectrum, and are used as fluorescent probes for detecting the heavy metal ions in the sewage. The invention also provides a method for detecting heavy metal ions in sewage by the tin dioxide quantum dots, which comprises the steps of firstly establishing a quantitative standard curve between the fluorescence intensity variation of each heavy metal ion and the concentration of each heavy metal, wherein the more the data of the standard library is, the higher the detection accuracy is, then mixing the tin dioxide quantum dot standard solution and the solution to be detected at normal temperature, measuring and calculating the fluorescence intensity variation of the tin dioxide quantum dot standard solution before and after reaction, and finding the concentration of the heavy metal ion corresponding to the fluorescence intensity variation by using the quantitative standard curve.
Description
Technical Field
The invention relates to the technical field of fluorescent materials, in particular to application of tin dioxide quantum dots to detection of heavy metal ions in sewage and a detection method.
Background
Pollution has become a serious concern worldwide, and heavy metals discharged from industrial wastewater may come from metal plating equipment, metal surface treatment, chemical, fertilizer and cardboard factory production. These heavy metal ions pose a significant threat to the environment and public health due to their non-biodegradability and strong toxicity to plants, animals and humans. Therefore, there is an urgent need to develop a simple and sensitive method for detecting heavy metal ions in water.
Quantum dots are an important low-dimensional semiconductor material, and the size of each of the three dimensions is not larger than twice the exciton bohr radius of the corresponding semiconductor material. Quantum dots are generally spherical or spheroidal, often with diameters between 2-20 nm. Common quantum dots are composed of IV, II-VI, IV-VI or III-V elements. Quantum dots are nano-scale semiconductors that fluoresce at a specific frequency by applying a certain electric field or light pressure to the nano-semiconductor material.
Several techniques for detecting heavy metal ions are available, such as atomic absorption spectroscopy, inductively coupled plasma mass spectrometry, and fluorescence spectroscopy. However, these methods have high requirements on operators, high detection cost and complex treatment process. The quantum dot is a semiconductor nanocrystal particle, has a wide excitation spectrum and a narrow emission spectrum, is high in chemical stability and light stability, and long in fluorescence life, and due to the characteristics, the quantum dot receives more and more attention, and the application of the quantum dot serving as a fluorescence probe in the field of analytical chemistry becomes a hot spot, including the application of the quantum dot in detecting heavy metal ions in water.
Several quantum dots have been successfully synthesized, such as CdS, CdTe, ZnS quantum dots and their composites. However, some of them contain toxic elements.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an application and a detection method for detecting heavy metal ions in sewage by using tin dioxide quantum dots, namely tin dioxide (SnO)2) The quantum dot is an environment-friendly semiconductor and has the advantages of no toxicity, good chemical stability and low cost.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the tin dioxide quantum dots are applied to detection of heavy metal ions in sewage, specifically, the detected heavy metals are copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium or bismuth, and the particle size of the tin dioxide quantum dots is preferably 2 nm-10 nm.
The invention also provides a method for detecting heavy metal ions in sewage by using the tin dioxide quantum dots, which is characterized by comprising the following steps:
step S1: preparing a tin dioxide quantum dot standard solution with a certain concentration, and measuring the fluorescence intensity of the tin dioxide quantum dot standard solution;
step S2: preparing heavy metal ion solutions with different concentrations, respectively adding the heavy metal ion solutions into the tin dioxide quantum dot standard solution prepared in the step S1, respectively measuring fluorescence intensity of each solution after reaction, and drawing a quantitative standard curve between the fluorescence intensity variation before and after the addition of the heavy metal ion solution and the concentration of the heavy metal ion;
step S3: and (4) adding the liquid to be detected into the standard solution of the tin dioxide quantum dots prepared in the step (S1), measuring the fluorescence intensity after reaction, calculating the fluorescence intensity variation before and after the addition of the liquid to be detected, and finding the concentration of the heavy metal ions corresponding to the fluorescence intensity variation in the quantitative standard curve prepared in the step (S2).
Preferably, the heavy metal is copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium or bismuth.
Preferably, in the step S1, the method for preparing the tin dioxide quantum dot standard solution includes: dissolving a certain amount of stannous chloride and thiourea in deionized water, and magnetically stirring at normal temperature to obtain a stannic oxide quantum dot solution.
Preferably, the weight part ratio of the stannous chloride to the thiourea is 20-50: 1.
Preferably, the fluorescence intensity is measured using a fluorescence spectrophotometer.
Preferably, in the step S1, the concentration of the tin dioxide quantum dot standard solution is 1E-6mol/L to 1E-1 mol/L.
Preferably, the particle size of the tin dioxide quantum dots in the tin dioxide quantum dot standard solution is 2 nm-10 nm.
According to the technical scheme, the tin dioxide quantum dots have the advantages of no toxicity, good chemical stability, low cost, wide excitation spectrum and narrow emission spectrum, and are used as fluorescent probes for detecting heavy metal ions in sewage. The invention also provides a method for detecting heavy metal ions in sewage by the tin dioxide quantum dots, which comprises the steps of firstly establishing a quantitative standard curve between the fluorescence intensity variation of each heavy metal ion and the concentration of each heavy metal, wherein the more the data of the standard library is, the better the detection accuracy is, then mixing the tin dioxide quantum dot standard solution and the solution to be detected at normal temperature, measuring and calculating the fluorescence intensity variation of the tin dioxide quantum dot standard solution before and after reaction, and finding the concentration of the heavy metal ion corresponding to the fluorescence intensity variation by using the quantitative standard curve.
Drawings
FIG. 1 is SnO prepared by the present invention2The particle size distribution diagram of the quantum dots is shown, wherein the abscissa represents the particle size, the left ordinate represents the percentage of the quantum dots of each particle size in all the quantum dots, and the right ordinate represents the percentage of the total quantum dots of all the particle sizes before the particle size of the corresponding abscissa in all the quantum dots;
FIG. 2 is a high resolution Transmission Electron Microscopy (TEM) view of SnO prepared in accordance with the present invention2The morphology of the quantum dots;
FIG. 3 shows a method for producing a metal oxide from SnO2SnO obtained in aqueous solutions of quantum dots2XRD pattern of the powder;
FIG. 4 is a graph showing fluorescence intensities of tin dioxide solutions of different concentrations after being excited by light having a wavelength of 310nm in the present invention;
FIG. 5 is SnO in the present invention2Fluorescence spectrum after mixing quantum dots and heavy metal ions, wherein the peak value appears at the emission wavelength of 300nm to 310 nm.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
In the following detailed description of the embodiments of the present invention, in order to clearly illustrate the structure of the present invention and to facilitate explanation, the structure shown in the drawings is not drawn to a general scale and is partially enlarged, deformed and simplified, so that the present invention should not be construed as limited thereto.
The synthesis method of the stannic oxide quantum dot comprises the step of adding a certain amount of stannous chloride (SnCl)2·2H2O) and thiourea (CH)4N2S) dissolving the tin dioxide quantum dot in deionized water, and magnetically stirring at normal temperature to obtain a tin dioxide quantum dot solution. Stannous chloride provides the tin source, and thiourea is the catalyst and stabilizer.
In this example, 2.257g of stannous oxide (SnCl) was weighed out separately2·2H2O) and 0.077g of thiourea (CH)4N2S), dissolving in 50ml of deionized water, and stirring in a magnetic stirring device at about 25 ℃ for 24 hours in a water bath. SnCl2After hydrolytic oxidation, the aqueous SnO is obtained2A quantum dot solution. Wherein the concentration of the finally obtained stannic oxide quantum dot solution is 0.2 mol/l.
SnO analysis by dynamic light scattering2The particle size of the quantum dots is in the range of 2nm to 10nm, and the average particle size is 2.23nm, as shown in fig. 1, and it can be seen that the prepared quantum dots have uniform dispersibility in aqueous solutions.
The solution was dried to a powder, the morphology thereof was observed by transmission electron microscopy, with reference to fig. 2, with a regular rutile appearance, and subjected to X-ray diffraction, with reference to fig. 3.
The method for detecting the heavy metal ions in the polluted water by using the prepared tin dioxide quantum dots comprises the following steps:
s1: preparing a tin dioxide quantum dot standard solution with a certain concentration, and measuring the fluorescence intensity of the tin dioxide quantum dot standard solution by using a fluorescence spectrophotometer.
In order to find the concentration of the tin dioxide quantum dot solution with the optimal sensitivity, tin dioxide quantum dot solutions with different concentrations are prepared, and the fluorescence intensity is measured by using a fluorescence spectrophotometer, as shown in FIG. 4, preferably, the concentration of the tin dioxide quantum dot standard solution is 1E-6 mol/L-1E-1 mol/L.
In the embodiment, the concentration of the tin dioxide quantum dot solution with the strongest fluorescence is taken as the concentration of the standard solution, namely 1E-4.
S2: making standard library data, preparing heavy metal ion solutions with different concentrations, wherein the heavy metal can be copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium or bismuth, respectively adding the heavy metal into the tin dioxide quantum dot standard solution prepared in the step S1, respectively measuring fluorescence intensity of each solution after reaction, and drawing a quantitative standard curve between the fluorescence intensity variation before and after the heavy metal ion solution is added and the concentration of the heavy metal ion. The more the data of the standard library, the closer the fitted quantitative standard curve is to the reality, and the more accurate the detection result is.
See fig. 5 with Cu2+，Pd2+，Cd2+，Ni2+And Fe3+For example, SnO2Fluorescence spectrum after mixing quantum dots and heavy metal ions, wherein the peak value appears at the emission wavelength of 300nm to 310 nm. Thus, the tin dioxide quantum dot pairs are Cu2+，Pd2 +，Cd2+，Ni2+And Fe3+The equiheavy metal ions have good fluorescence response, short response time and low detection limit.
S3: and (4) adding the liquid to be detected into the standard solution of the tin dioxide quantum dots prepared in the step (S1), measuring the fluorescence intensity after reaction, calculating the fluorescence intensity variation before and after the addition of the liquid to be detected, and finding the concentration of the heavy metal ions corresponding to the fluorescence intensity variation in the quantitative standard curve prepared in the step (S2). Heavy metal ions can cause the fluorescence intensity of the quantum dots to be weakened.
In this embodiment, the amount of change in fluorescence intensity is equal to the fluorescence intensity value measured after the reaction divided by the fluorescence intensity value measured before the reaction.
The method for detecting the heavy metal ions by the tin dioxide quantum dots has high sensitivity, the detection process is simple and rapid, no complex pretreatment is needed, and the characteristics enable the reagent to become a prospect reagent for detecting the heavy metal ions in water.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The application of the tin dioxide quantum dots in detection of heavy metal ions in sewage is characterized in that the heavy metals are copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium or bismuth, and the tin dioxide quantum dots are used as fluorescent probes for detection of the heavy metal ions in the sewage.
2. The use of claim 1, wherein the particle size of the tin dioxide quantum dots is 2nm to 10 nm.
3. A method for detecting heavy metal ions in sewage by using tin dioxide quantum dots is characterized by comprising the following steps:
step S1: preparing a tin dioxide quantum dot standard solution with a certain concentration, and measuring the fluorescence intensity of the tin dioxide quantum dot standard solution;
step S2: preparing heavy metal ion solutions with different concentrations, respectively adding the heavy metal ion solutions into the tin dioxide quantum dot standard solution prepared in the step S1, respectively measuring fluorescence intensity of each solution after reaction, and drawing a quantitative standard curve between the fluorescence intensity variation before and after the addition of the heavy metal ion solution and the concentration of the heavy metal ion, wherein the heavy metal is copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium or bismuth;
step S3: and (4) adding the liquid to be detected into the standard solution of the tin dioxide quantum dots prepared in the step (S1), measuring the fluorescence intensity after reaction, calculating the fluorescence intensity variation before and after the addition of the liquid to be detected, and finding the concentration of the heavy metal ions corresponding to the fluorescence intensity variation in the quantitative standard curve prepared in the step (S2).
4. The method as claimed in claim 3, wherein in step S1, the method for preparing the tin dioxide quantum dot standard solution is as follows: dissolving a certain amount of stannous chloride and thiourea in deionized water, and magnetically stirring at normal temperature to obtain a stannic oxide quantum dot solution.
5. The method according to claim 4, wherein the weight part ratio of stannous chloride to thiourea is 20-50: 1.
6. The method of claim 3, wherein the fluorescence intensity is measured using a fluorescence spectrophotometer.
7. The method according to claim 3, wherein in the step S1, the concentration of the tin dioxide quantum dot standard solution is 1E-6mol/L to 1E-1 mol/L.
8. The method according to claim 3, wherein the particle size of the tin dioxide quantum dots in the tin dioxide quantum dot standard solution is 2 nm-10 nm.
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| CN110726759A (en) * | 2019-10-31 | 2020-01-24 | 大连海事大学 | Preparation method of tin dioxide quantum dots, gas sensor and preparation method of gas sensor |
| CN110672575B (en) * | 2019-11-06 | 2021-12-07 | 湖北师范大学 | Be used for detecting Hg2+And Cu2+Ratiometric fluorescent sensor, and preparation method and application thereof |
| CN111847575A (en) * | 2020-07-24 | 2020-10-30 | 大连海事大学 | Method for removing octane-containing pollutants by using stannic oxide photocatalytic quantum dots and application thereof |
| CN113267476B (en) * | 2021-04-30 | 2022-11-25 | 大连海事大学 | Method for detecting sulfur content in marine fuel oil by using tin dioxide quantum dots |
| CN113049565A (en) * | 2021-04-30 | 2021-06-29 | 南京师范大学 | Bi3+Method for rapidly detecting concentration |
| CN113406018B (en) * | 2021-06-17 | 2024-02-09 | 大连海事大学 | Marine fuel oil sulfur content detector and detection method |
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