CN113324955B - Method for detecting copper ions in aqueous solution by perovskite quantum dots - Google Patents
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- 229910052799 carbon Inorganic materials 0.000 description 1
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- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention discloses a method for passing copper ions (Cu)2+) Phase transfer technology for realizing perovskite CsPbX3(X = Cl, Br, I) quantum dot for detecting copper ions in aqueous solution. Cu2+The phase transfer technology is that strong organic ligand is added into quantum dot solution to selectively remove Cu in the aqueous solution to be detected2+Ions are transferred from the water into the quantum dot solution to form copper complexes, which in turn quench the fluorescence of perovskite quantum dots (PeQDs). The specific operation is as follows: dissolving newly prepared PeQDs and oleylamine (OAm) in cyclohexane or toluene to form a solution of PeQDs-OAm; mixing the solution of PeQDs-OAm with Cu2+Mixing the ionic water solution for 60s, OAm optionally mixing Cu2+From the aqueous phase to the organic phase. OAm-Cu formed at the interface of two phases2+The complex quenches the fluorescence of the PeQDs. Through the phase transfer technology, the invention realizes that the perovskite quantum dots directly detect the copper ions in the aqueous solution. Linear Range of PeQDs fluorescent probes (10)‑6‑10‑2 M) wide, short response time (1 min), for Cu2+The selectivity of (A) is good.
Description
Technical Field
The invention relates to the technical field of metal ion detection, in particular to a novel method for detecting copper ions in an aqueous solution by perovskite quantum dots through a copper ion phase transfer technology.
Background
Heavy metal ion contamination poses a great hazard to the life activities of living organisms, such as excessive copper ions (Cu) in the human body2+) Accumulation can lead to nausea, vomiting, diarrhea, stomachache, and the like. World Health Organization (WHO) specifies Cu in drinking water2+The safety value of (a) was 30 μ M. Therefore, a simple and rapid method was developed for detecting Cu in drinking water2+The concentration is very important. Several methods have been developed for detecting Cu2+Such as atomic absorption spectrometry, spectrophotometric analysis, liquid chromatography, electrochemical methods, fluorimetric methods, and the like.
The fluorescence-based detection method has the advantages of short detection time, low cost, easy use, high sensitivity, strong selectivity and the like. Several fluorescent sensors have been developed including quantum dots, organic dyes, silicon nanoparticles, carbon dots, noble metal nanoparticles, and the like. For example, Guxiangfeng and the like invent carbon nanodots modified by organic amine surface as fluorescent probes for detecting Cu2+(CN201611100198.6). The invention discloses a gold-copper nano-cluster fluorescent probe (CN201810241848.1) for detecting copper ions, and the like. Liu Sen et al invented a boron-nitrogen co-doped fluorescent carbon quantum dot for preparing a copper ion sensor (CN 201910367696.4). Among them, semiconductor Quantum Dots (QDs) have many unique photophysical properties, and thus they have significant advantages as fluorescent probes for heavy metal ion sensing.
Recently, CsPbX of perovskite structure3(X = Cl, Br and I) QDs are attracting great attention due to their excellent photoluminescence characteristics. Quantum dots have not only a wide range of applications in the display field and solar cells, but also for chemical sensing. Reported, CsPbX3QDs can be used as fluorescent probe for detecting Cu in grease with high sensitivity2+（Advanced Materials2017, 29.1700150), the material can also be used for trace detection of Cu in organic phase2+And peroxide content in edible oils (A), (B), (C), (D, E, and D)Journal of Materials Chemistry C, 2018, 6, 4793-4799). With O3And H2Perovskite-type QDs gas sensors in which S is the detection target have also been developed: (Analytical Chemistry, 2019, 91, 14183-14187；Nanoscale Advances, 2019, 1, 2699-2706). The polymer coating technology is adopted, and the all-inorganic perovskite type QDs are used for detecting biological molecules and metal ions (Analytical Chemistry, 2019, 91, 15915-15921). Clearly, these efforts selectively avoid their direct use in aqueous solutions due to the instability of perovskite quantum dots in water. Ma et al prepared stable PEA in water2PbI4Perovskite Nanocrystals (NCs) and their use for detecting Cu in aqueous environments2+（Chemical Communications, 2018, 54, 5784-5787.). Recently, Xuwen et al reported stable Cs3Bi2Br9：Eu3+Preparation of NCs and use for Cu in Water2+And low PL efficiency may limit its applications (a)ACS Sustainable Chemistry & Engineering, 2019, 7, 8397-8404）。
Disclosure of Invention
Aiming at the existing copper ions in the prior artThe invention provides a method for preparing a Cu-doped perovskite quantum dot with low sub-selectivity, narrow linear range and poor stability of perovskite quantum dots in aqueous solution2+Phase transfer technology for realizing application of perovskite quantum dots as fluorescent probes to Cu in aqueous solution2+The method of (1). Cu2+The phase transfer technology is that strong organic ligand is added into cyclohexane solution of quantum dots to selectively and selectively add Cu in aqueous solution to be detected2 +The ions are transferred from the water to cyclohexane to form copper complexes. The complex can effectively quench the fluorescence of perovskite quantum dots (PeQDs). As described in the examples, freshly prepared PeQDs and oleylamine (OAm) were first dissolved in cyclohexane, and the solution of PeQDs (OAm) was then mixed with Cu2+The aqueous solutions are mixed. Mixing for 1min on a vortex mixer, oleylamine in cyclohexane can capture Cu from water due to strong coordination of amine-rich ligands with metal ions2+OAm-Cu is formed at the cyclohexane/water interface2+And (3) a complex. These Cu2+The complex can diffuse rapidly into cyclohexane, eventually quenching the fluorescence of the PeQDs. Therefore, PeQDs can be used as fluorescent probes for Cu in aqueous solution2+Detection of (3).
The method comprises the following steps:
the method comprises the following steps: and (3) synthesizing a part of perovskite quantum dots, centrifuging, and dispersing the precipitate in cyclohexane to form a quantum dot solution.
Step two: preparing copper ion solutions with different concentrations.
Step three: and uniformly mixing the oleylamine-containing quantum dot solution and the copper ion solution by using a uniformly mixing instrument, and standing.
Step four: the upper quantum dot solution was aspirated and the fluorescence intensity was measured.
The concentration range of the quantum dot solution in the step one is 10-10 – 1mol/L。
The concentration range of the copper ion solution in the second step is 10-10–0.10mol/L。
The volume ratio of the oleylamine to the quantum dot solution added in the third step is 1: 4000-1: 2.
The volume ratio of the quantum dot solution to the copper ion aqueous solution in the third step is 10: 1-1: 10.
The mixing time in the third step should be within the range of 5 s-1 h.
The standing time after the uniform mixing in the third step is within the range of 5 s-4 h.
The beneficial effects of the invention are as follows.
1. According to the invention, by the metal ion phase transfer technology, the perovskite quantum dots are directly applied to the detection of copper ions in an aqueous solution.
2. The perovskite quantum dot in the invention is taken as a fluorescent probe to show a wide linear range (10)-6 M - 10-2M), short response time (1 min) and Cu2+Good selectivity of the catalyst.
3. The invention has the advantages of simple raw materials, simple reaction conditions, short reaction time, simple operation and high efficiency.
Drawings
FIG. 1 shows CsPbBr3Absorption and emission spectra of QDs.
FIG. 2 is a graph of the absorption spectra of different solutions.
FIG. 3 shows CsPbBr3Photoluminescence spectra of QDs solutions vs Cu2+Dependence on concentration.
FIG. 4 shows different metal ion pairs CsPbBr3Influence of the luminescence intensity of the solution.
Detailed Description
The following are non-limiting examples of the present invention, which are further described in conjunction with the accompanying drawings.
Example 1: CsPbBr3Preparation of QDs solution.
S1: 0.267 g of Cs2CO30.837 mL OA and 10mL octadecene were added to a 50 mL three-necked flask in N2Degassed for 10 minutes at ambient and then dried under vacuum at 120 ℃ for about 1 h. And introducing nitrogen, further heating the mixed solution to 150 ℃, keeping the temperature for 10min until cesium carbonate is completely dissolved, and cooling to room temperature. (preheating to 100 ℃ is required for use).
S2: 10mL of octadecene and 0.376 mmol of PbBr2Is put into a 50 mL three-neck flaskIn N2Stirring at room temperature for 10min under an atmosphere, and then stirring at 120 deg.CoAnd C, drying for about 1h in vacuum until no bubbles are generated. The nitrogen was switched and 1mL of oleic acid and 1mL of oleylamine were rapidly injected into the flask. Again at 120oAnd C, vacuum drying for about 1 h. When the solution becomes clear, N is turned on2Heating to 170 deg.CoC and rapidly inject 1mL cesium oleate precursor. After 5 seconds of reaction the ice-water bath was cooled to room temperature.
S3: the mixture was centrifuged at 10000rpm for 5 minutes, and the precipitate was dispersed in 20mL of cyclohexane. Then, 1mL of the solution was taken out and diluted to 40-fold, and CsPbBr was calculated3Has a concentration of 3.11X 10-4mol/L. The fluorescence intensity and absorption peak of the solution are measured, and the fluorescence spectrogram and the ultraviolet absorption chart are shown in figure 1.
S4: as shown in FIG. 1, CsPbBr3The UV absorption spectrum of QDs solutions shows an absorption peak at about 500 nm, while the fluorescence spectrum shows a narrow green emission at 516 nm under 365nm light excitation.
Example 2: cu2+Validation of the transfer from the aqueous phase to the oil phase.
S1: 3mL of oleylamine-containing cyclohexane (cyclohexane) (OAm) was mixed with 3mL of 10-2And mixing the mol/L copper nitrate solution uniformly. After standing for 1 hour, the supernatant was recorded as (cyclohexane (OAm) Cu2+). 3mL of cyclohexane solution and 3mL of 10- 2mixing the mol/L copper ion solution evenly. After standing for 1 hour, the supernatant was taken out and designated as (CyclohexanecCu)2+). Determination of Cyclohexane (OAm) Cu2+、cyclohexane(OAm)、cyclohexaneCu2+The ultraviolet absorption spectrum of the solution is shown in figure 2.
S2: as shown in FIG. 2, Cyclohexanecu2+The solution showed a very weak absorption peak in the Ultraviolet (UV) region (blue curve). Cyclohexane (OAm) produces a strong absorption band in the UV region (green curve). Cyclohexane (OAm) Cu2+The new absorption band (red curve) generated in the range of 500-700 nm is Cu2+Due to the d-d transition of (a). This phenomenon indicates that Cu2+Ions can be transferred from water to cyclohexane by oleylamine complexation to form OA at the cyclohexane/water interfacem-Cu2+The complex was dissolved in cyclohexane.
Example 3: CsPbBr3QDs are used as fluorescent probes for the detection of copper ions.
S1: 3mL of CsPbBr containing 40. mu. LOAm3The solution was added to 3mL of copper nitrate solution, Cu2 +Respectively has a concentration of 0, 10-7、10-6、10-5、10-4、10-3、10-2mol/L. After mixing on a vortex mixer for 60 seconds, the mixed solution was allowed to stand for 1 hour. The upper solution was then aspirated for further measurement of the fluorescence spectrum, which is shown in FIG. 3.
S2: as shown in FIG. 3, CsPbBr3Fluorescence intensity of QDs is dependent on [ Cu ]2+]Increase from 0 to 10-2M decreases continuously.
Example 4: other ion pairs CsPbBr3Influence of QDs fluorescence intensity.
S1 operation is the same as in the step S1 of example 3, except that Cu2+Change of ionic solution to Na+，K+，Mg2+，Ca2+，Sr2+，Ba2+，Ni2+，Mn2+，Pb2+，Zn2+，Er3+，Yb3+Ionic solutions or pure water. All metal ions had a concentration of 10-3mol/L. The fluorescence spectrum is shown in FIG. 4.
S2: as shown in FIG. 4, the upper CsPbBr layer3The luminescence intensity of the QDs solution is limited by Cu only2+The solution of ions is quenched remarkably, and other metal ion solutions or pure water cannot quench CsPbBr remarkably3Luminescence of QDs solutions. Indicating probe solution to Cu in water2+The ions have high selectivity.
Claims (8)
1. CsPbBr3The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: synthesis of CsPbBr3Centrifuging after quantum dots, and dispersing the precipitate in a nonpolar solvent to prepare a quantum dot solution with a certain concentration;
step two: preparing copper ion aqueous solutions with different concentrations;
step three: uniformly mixing the oleylamine-containing quantum dot solution and the copper ion solution by using a mixing instrument, and standing;
step four: the upper quantum dot solution was aspirated and the fluorescence intensity was measured.
2. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the concentration range of the quantum dot solution in the step one is 10-10 – 1 mol/L。
3. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: in the first step, the nonpolar solvent is cyclohexane and toluene.
4. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the concentration range of the copper ion solution in the second step is 10-10 – 0.10 mol/L。
5. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the volume ratio of oleylamine to the quantum dot solution in the third step is in the range of 1: 4000-1: 2.
6. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the volume ratio of the quantum dot solution to the copper ion aqueous solution in the third step is 10: 1-1: 10.
7. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps:the mixing time in the third step should be within the range of 5 s-1 h.
8. The CsPbBr of claim 13The method for detecting the copper ions in the aqueous solution by using the quantum dots as the fluorescent probe is characterized by comprising the following steps: the standing time after the uniform mixing in the third step is within the range of 5 s-4 h.
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| Title |
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| All-inorganic CsPbBr3 perovskite quantum dots as a photoluminescent probe for ultrasensitive Cu2+ detection;Yongfeng Liu et al;《J. Mater. Chem. C》;20181231;第6卷;全文 * |
| Cesium Lead Halide Perovskite Quantum Dots as a Photoluminescence Probe for Metal Ions;Xuexi Sheng et al;《Adv. Mater.》;20171231;第29卷;全文 * |
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