CN110849852A - Method for detecting heavy metal ions based on fluorescent perovskite nanocrystals - Google Patents
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Abstract
A method for detecting heavy metal ions based on fluorescent perovskite nanocrystals relates to the field of heavy metal ion detection, and adopts a liquid-liquid extraction method and utilizes CsPbBr3The organic solution extracts the heavy metal ion aqueous solution, and the heavy metal ions are extracted into the organic phase for detection. Due to CsPbBr3And the fluorescent material is not in direct contact with the water phase, so that the fluorescence is not quenched. Thereby well solving the problem of CsPbBr3Poor water corrosion resistance and limited application in aqueous solution. The method has the advantages of mild conditions, simple and convenient operation and higher sensitivity, and can realize the qualitative detection of the heavy metal ions in the aqueous solution.
Description
Technical Field
The invention relates to the field of heavy metal ion detection, in particular to a method for detecting heavy metal ions based on a fluorescent perovskite nanocrystal.
Background
Perovskite was originally referred to as the yellow, brown or black inorganic mineral perovskite titanate (CaTiO) found in russian Wularshan under the name of russian mineralogist Lev Perovski3) Now referring to a broad class of materials having the same structure. The metal halide perovskite is characterized by the chemical formula ABX3Comprising organic-inorganic halide perovskites, organic halide perovskites CH3NH3PbX3(X = Cl, Br, I) and all-inorganic halide perovskites, CsPbX3In the past few years, all-inorganic halide perovskite nanocrystals have received much attention due to their excellent optical and optoelectronic properties, and have become a new star in the field of nanomaterials. Meanwhile, perovskite has more attention due to long charge carrier life, high photoluminescence quantum yield and high efficiency, and becomes one of the most popular topics in current Photovoltaic (PV) research. However, the ionic property of halide perovskite causes instability in polar solvent, especially poor water corrosion resistance, and greatly limits CsPbBr3In practice, many researchers have been working on improving their stability and quantum yield. HU et al successfully prepared monodisperse CsPbBr by water-triggered and sol-gel method3Janus nanoparticles, which have high water erosion resistance and good stability but have not yet been put to practical use; parobek et al prepared CsPbBr with high quantum yield by doping Mn3Nanocrystals, but its drawback is still poor resistance to water etching, which gives CsPbBr3Presents challenges for practical application. Thus, study of CsPbBr3The optical property of the optical fiber is applied to actual analysis and detection, and has certain research significance and research value.
Heavy metals including gold, silver, copper, iron, mercury, lead, cadmium, etc. are accumulated in the human body to a certain extent, and chronic poisoning may be caused. However, heavy metals in terms of environmental pollution mainly refer to heavy elements with significant biological toxicity, such as mercury (mercury), cadmium, lead, chromium, and metalloid arsenic. Heavy metals are very difficult to biodegrade, but can be concentrated hundreds of times under the action of biological amplification of a food chain, and finally enter a human body, and can generate strong interaction with proteins, enzymes and the like in the human body to make the proteins, the enzymes and the like lose activity, and can also be accumulated in certain organs of the human body to cause chronic poisoning. At the present stage, numerous analysis and detection methods for heavy metal ions are available and mature in application, but few simple, visual and rapid methods for simultaneously detecting various heavy metal ions are reported, and few methods for detecting heavy metal ions by using fluorescent perovskite as a fluorescent probe are available.
In the prior art, a plurality of methods for detecting heavy metal ions exist, but the common detection method for the heavy metal ions cannot realize the simultaneous extraction and fluorescence detection of a plurality of heavy metal ions. CsPbBr3Although useful for the detection of metal ions, CsPbBr3The stability and the water erosion resistance of the fluorescent material are poor, and the fluorescence of the fluorescent material is rapidly quenched when the fluorescent material is contacted with water. So that the heavy metal ions in the aqueous solution can not be detected, and the application of the heavy metal ions in the actual analysis and detection is greatly limited.
Disclosure of Invention
The invention aims to provide a method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, which has mild conditions and simple and convenient operation, and overcomes the defects of CsPbBr3The problem that heavy metal ions in the aqueous solution can not be detected is solved, and CsPbBr is widened3The range of application of (1).
The embodiment of the invention is realized by the following steps:
a method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, comprising:
mixing a detection reagent with a solution to be detected, oscillating, standing for layering, and separating liquid to obtain an organic layer; observing and/or measuring the fluorescence intensity of the organic layer under an ultraviolet lamp;
wherein the detection reagent is CsPbBr3The nano crystal is prepared by dissolving the nano crystal in an organic solvent; the solution to be tested is an aqueous solution of heavy metal ions.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a fluorescent perovskite nanocrystal-based detection methodThe method for measuring heavy metal ions adopts a liquid-liquid extraction method and utilizes CsPbBr3The organic solution extracts the heavy metal ion aqueous solution, and the heavy metal ions are extracted into the organic phase for detection. Due to CsPbBr3And the fluorescent material is not in direct contact with the water phase, so that the fluorescence is not quenched. Thereby well solving the problem of CsPbBr3Poor water corrosion resistance and limited application in aqueous solution. The method has the advantages of mild conditions, simple and convenient operation and higher sensitivity, and can realize the qualitative detection of the heavy metal ions in the aqueous solution.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph showing a comparison of fluorescence intensity at 533nm in the experimental examples of the present invention;
FIG. 2 is a graph showing the comparison of fluorescence intensities in the range of 500 to 600nm according to the experimental examples of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for detecting heavy metal ions based on the fluorescent perovskite nanocrystals of the embodiment of the present invention is specifically described below.
The embodiment of the invention provides a method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, which comprises the following steps:
mixing a detection reagent with a solution to be detected, oscillating, standing for layering, and separating liquid to obtain an organic layer; and (3) observing and/or measuring the fluorescence intensity of the organic layer under an ultraviolet lamp.
Wherein the detection reagent is CsPbBr3The nano crystal is prepared by dissolving the nano crystal in an organic solvent; the solution to be tested is an aqueous solution of heavy metal ions.
Further, the organic solvent includes at least one of dichloromethane, chloroform, ethyl acetate and diethyl ether. The organic solvent can extract heavy metal ions in the solution to be detected into an organic phase, and the heavy metal ions and CsPbBr are extracted by the organic solvent3The combination of the nano crystals generates fluorescence change, thereby realizing the detection of metal ions in the water phase. Preferably, the organic solvent comprises at least one of dichloromethane and chloroform; preferably, the organic solvent comprises dichloromethane. The inventor finds out through creative work that when dichloromethane is used for extraction, the extraction effect is good, and CsPbBr can be effectively prevented3The fluorescence quenching of the nano crystal has lower detection limit for various heavy metal ions.
CsPbBr in detection reagent3The molar concentration of the nano-crystal is 0.5-5.75 mmol/L. The inventors found that CsPbBr was used in3When the concentration of the nano crystal is low, the detection result is not obvious, and the judgment of the result is influenced. And in CsPbBr3CsPbBr at higher nanocrystal concentrations3The nanocrystals are not easily dissolved and can affect the observation of the detection result. The inventor creatively finds that the detection effect on the heavy metal ions is better in the concentration range.
The detection method provided by the embodiment of the invention can be used for detecting various heavy metal ions, and the applicable heavy metal ions comprise Ag+、Cd2+、Co2+、Cr3+、Fe3+And Hg2+At least one of (1). Preferably, the concentration of heavy metal ions in the solution to be tested is > 0.3. mu.M. Within the concentration range, the change of fluorescence is obvious, and the detection result is accurate.
Further, the volume ratio of the detection reagent to the solution to be detected is 1: 0.5 to 1.5. The mixing detection effect is better according to the proportion. In actual operation, the detection reagent and the solution to be detected are mixed, fully oscillated and then kept stand for 1-5 min, so that the mixed solution is layered, and the detection accuracy is improved.
Optionally, the organic layer obtained from the extraction was observed under an ultraviolet lamp of 365 nm. The detection reagent appears yellow under 365nm ultraviolet light, but appears green after the heavy metal ions are combined. According to the change of the color, whether the aqueous solution contains heavy metal ions can be judged. In addition, the fluorescence intensity of the organic layer at 533nm was measured. CsPbBr3The emission spectrum of the nano crystal is the maximum emission wavelength at 533nm, and the obtained result is more accurate by comparing the fluorescence intensity change at the wavelength before and after the extraction of the detection reagent.
Further, CsPbBr adopted in the embodiment of the invention3The nanocrystals were prepared as follows. It includes:
s1, mixing oleylamine with HBr in an inert atmosphere, and reacting at 120-150 ℃ for 1-5 h to obtain an HBr mixture;
s2, under the inert atmosphere, adding Cs2Co3Mixing PbO, 1-octadecene, oleic acid and the HBr mixture, and reacting for 30-60 min at 120-160 ℃.
Specifically, it can be prepared as follows.
S1, 10mL OLA and 1.28mL HBr are added into a 25mL round-bottom flask, the solidification reaction mixture is vacuumized, heated at 120 ℃ for 2h under the protection of N2, the reaction temperature is raised to 150 ℃, and the heating reaction is continued for 0.5 h.
S2, adding 0.1mmol of Cs2Co3, 0.2mmol of PbO, 10mL of 1-octadecene, 1mLOA and N2 into a 50mL three-neck flask, heating at 120 ℃ for 30min, raising the temperature to 160 ℃, adding 0.7-0.9 mL of OLA-HBr, continuing to react for 5min, stopping heating, adding 20mL of N-hexane after the temperature is reduced to room temperature, centrifuging at 6000rpm for 5min, discarding supernatant, washing precipitate with absolute ethyl alcohol, drying at 80 ℃, and storing in dark place.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This example provides a method for detecting Ag in an aqueous solution based on fluorescent perovskite nanocrystals+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Ag+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 2
The embodiment provides a method for detecting Cd in aqueous solution based on fluorescent perovskite nanocrystals2+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Cd2+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 3
This example provides a method for detecting Co in an aqueous solution based on fluorescent perovskite nanocrystals2+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Co2+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 4
The embodiment provides a method for detecting Cr in an aqueous solution based on fluorescent perovskite nanocrystals3+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 muL of 10 mmol/L Cr3+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 5
This example provides a method for detecting Fe in an aqueous solution based on fluorescent perovskite nanocrystals3+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Fe3+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 6
The embodiment provides a method for detecting Hg in an aqueous solution based on fluorescent perovskite nanocrystals2+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Hg2+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 2 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 7
This example provides a method for detecting Ag in an aqueous solution based on fluorescent perovskite nanocrystals+The method of (1), comprising:
s1, weighing 0.01 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Ag+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 1mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 8
This example provides a method for detecting Ag in an aqueous solution based on fluorescent perovskite nanocrystals+The method of (1), comprising:
s1, weighing 0.01 g CsPbBr3And (3) adding 30 mL of dichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 muL of 1 mmol/L Ag+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 1mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 9
This example provides a method for detecting Ag in an aqueous solution based on fluorescent perovskite nanocrystals+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding 30 mL of trichloromethane into the nanocrystal in a 50mL centrifuge tube to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Ag+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 1mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Example 10
This example provides a method for detecting Ag in an aqueous solution based on fluorescent perovskite nanocrystals+The method of (1), comprising:
s1, weighing 0.1 g CsPbBr3And (3) adding the nanocrystal into a 50mL centrifuge tube, and adding 30 mL ethyl acetate to obtain the detection reagent.
S2, adding 2 mL of ultrapure water into a 5mL centrifuge tube, and then adding 2 mu L of 10 mmol/L Ag+And (5) water solution to obtain the solution to be detected.
And S3, mixing the solution to be detected prepared in the S2 with 4 mL of detection reagent, fully shaking, standing for 1 min, and taking the lower organic phase to measure the fluorescence emission spectrum.
Test examples
The fluorescence emission spectra of the organic phase and the detection reagent (Blank) extracted in examples 1 to 6 were measured, and the fluorescence intensities at 533nm were compared, and the results are shown in fig. 1 and 2.
As can be seen from FIGS. 1 and 2, the method provided in embodiments 1 to 6 of the present invention can be used for Ag in an aqueous solution+、Cd2+、Co2+、Cr3+、Fe3+And Hg2+All respond to enhance CsPbBr3The fluorescence of the nanocrystal at 533nm achieves the aim of detecting heavy metal ions. Especially for Ag+The detection is most sensitive, and the obtained fluorescence intensity is strongest.
In summary, the embodiment of the present invention provides a method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, which employs a liquid-liquid extraction method and utilizes CsPbBr3The organic solution extracts the heavy metal ion aqueous solution, and the heavy metal ions are extracted into the organic phase for detection. Due to CsPbBr3And the fluorescent material is not in direct contact with the water phase, so that the fluorescence is not quenched. Thereby well solving the problem of CsPbBr3Poor water corrosion resistance and limited application in aqueous solution. The method has the advantages of mild conditions, simple and convenient operation and higher sensitivity, and can realize the qualitative detection of the heavy metal ions in the aqueous solution.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for detecting heavy metal ions based on fluorescent perovskite nanocrystals is characterized by comprising the following steps:
mixing a detection reagent with a solution to be detected, oscillating, standing for layering, and separating liquid to obtain an organic layer; observing and/or measuring the fluorescence intensity of the organic layer under an ultraviolet lamp;
wherein the detection reagent is CsPbBr3The nano crystal is prepared by dissolving the nano crystal in an organic solvent; the solution to be detected is an aqueous solution of heavy metal ions.
2. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals of claim 1, wherein the organic solvent comprises at least one of dichloromethane, chloroform, ethyl acetate and diethyl ether; preferably, the organic solvent comprises at least one of dichloromethane and chloroform; preferably, the organic solvent comprises dichloromethane.
3. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals of claim 2, wherein the CsPbBr is added to the detection reagent3The molar concentration of the nano-crystal is 0.5-5.75 mmol/L.
4. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals according to claim 1, wherein the heavy metal ions comprise Ag+、Cd2+、Co2+、Cr3+、Fe3+And Hg2+At least one of (1).
5. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, according to claim 4, wherein the concentration of the heavy metal ions in the solution to be detected is > 0.3 μ M.
6. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, as claimed in claim 1, wherein the volume ratio of the detection reagent to the solution to be detected is 1: 0.5 to 1.5.
7. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals, as claimed in claim 1, wherein the detection reagent is mixed with the solution to be detected, and after sufficient oscillation, the mixture is allowed to stand for 1-5 min to allow the mixed solution to be layered.
8. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals according to claim 1, wherein the organic layer is observed under a 365nm ultraviolet lamp.
9. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals of claim 1, wherein the fluorescence intensity of the organic layer at 533nm is measured.
10. The method for detecting heavy metal ions based on fluorescent perovskite nanocrystals of claim 1, wherein CsPbBr is added3The preparation method of the nano crystal comprises the following steps:
mixing oleylamine and HBr in an inert atmosphere, and reacting at 120-150 ℃ for 1-5 h to obtain an HBr mixture;
under inert atmosphere, adding Cs2Co3Mixing PbO, 1-octadecene, oleic acid and the HBr mixture, and reacting for 30-60 min at 120-160 ℃.
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| CN111999271A (en) * | 2020-08-12 | 2020-11-27 | 嘉兴学院 | Cs4PbX6Application of perovskite nano material in detection of water content in nonpolar solvent |
| CN113267477A (en) * | 2021-05-14 | 2021-08-17 | 云南大学 | Method for visually detecting and quantitatively detecting mercury ions in aqueous solution by using water-soluble bromine-iodine-cesium-lead-perovskite |
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