CN113340866B - Method for detecting sulfite ions based on yellow fluorescent carbon quantum dots - Google Patents
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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"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
Abstract
The invention relates to a method for detecting sulfite ions based on yellow fluorescent carbon quantum dots, which specifically comprises the following steps: (1) Dissolving Y-CQDs in pH buffer solution, diluting to constant volume to obtain blank sample solution, stirring, standing, performing fluorescence test, and recording fluorescence intensity as F 0 (ii) a (2) Dissolving multiple equal mass parts of Y-CQDs in multiple equal volume parts of pH buffer solution, and adding SO-containing solution with different volumes 3 2‑ Diluting standard solution of standard substance to constant volume to obtain a series of standard sample solutions, stirring, standing, and performing fluorescence test to obtain a series of fluorescence intensities F n Separately calculate F n /F 0 Value, then F is obtained n /F 0 And SO 3 2‑ A functional relationship between concentrations; (3) Dissolving Y-CQDs in SO-containing solution to be detected 3 2‑ Performing fluorescence test on the polluted water sample to obtain F, and calculating according to the functional relationship to obtain SO in the polluted water sample 3 2‑ The concentration of (c). Compared with the prior art, the invention obviously improves SO 3 2‑ The sensitivity and accuracy of detection expand the application of the carbon quantum dots in the field of optical sensing.
Description
Technical Field
The invention relates to the field of fluorescent nano materials, in particular to a method for detecting sulfite ions based on yellow fluorescent carbon quantum dots.
Background
Sulfur dioxide (SO) due to the combustion of fossil fuels worldwide 2 ) Have been classified as the major atmospheric pollutants. SO in atmosphere 2 Will lead to the formation of acid rain, and sulfur dioxide is extremely highEasily dissolved in water, and after entering water body, sulfite (SO) is often used 3 2- ) The sulfite and the bisulfite exist in water in a dynamic balance manner, has certain toxic action on fishes and aquatic organisms in the water, can quickly consume dissolved oxygen in the water to deteriorate the water quality, can realize mutual conversion between the sulfite and sulfur with different forms in a water body, can convert the sulfite into sulfur dioxide, and then enters the atmosphere through gas-liquid exchange, thereby causing serious harm to the environment and human health, and has more and more evidences that the sulfite and the bisulfite exist in the water in a dynamic balance manner, SO that the sulfite and the bisulfite have certain toxic action on the fishes and aquatic organisms in the water, and the sulfite can quickly consume the dissolved oxygen in the water to deteriorate the water quality 2 Can cause a variety of diseases including respiratory, nervous, cardiovascular and even lung cancer. Therefore, the concentration of sulfite in water is an important indicator of the relevant environmental problems, for sulfur dioxide derivatives (SO) 3 2- ) Efficient detection of (a) is highly desirable.
Currently, the detection of sulfite comprises an iodometry, a colorimetry, a distillation-alkali titration method, an ion chromatography method and the like, but the iodometry, the colorimetry and the distillation-alkali titration method are long in time consumption and low in precision, and the ion chromatography method needs frequent replacement of a chromatographic column and also causes the problem of low analysis efficiency.
Disclosure of Invention
The invention aims to provide a method for detecting sulfite ions based on yellow fluorescent carbon quantum dots.
The purpose of the invention is realized by the following technical scheme:
a method for detecting sulfite ions based on yellow fluorescent carbon quantum dots, the method comprising the steps of:
(1) Dissolving Y-CQDs in pH buffer solution, diluting to constant volume to obtain blank sample solution, stirring, standing, performing fluorescence test, and recording fluorescence intensity as F 0 ；
(2) Dissolving multiple equal mass parts of Y-CQDs in multiple equal volume parts of pH buffer solution, and adding SO-containing solution with different volumes 3 2- Diluting standard solution of standard substance to constant volume to obtain a series of standard sample solutions, stirring, standing, and performing fluorescence testThe series of fluorescence intensities obtained was recorded as F n Separately calculate F n /F 0 Value, then F is obtained n /F 0 And SO 3 2- A functional relationship between concentrations;
(3) Dissolving Y-CQDs in SO-containing solution to be detected 3 2- Performing fluorescence test on the polluted water sample to obtain F, and calculating according to the functional relation obtained in the step (2) to obtain SO in the polluted water sample 3 2- The concentration of (c).
In the steps (1), (2) and (3), the fluorescent carbon quantum dots are prepared by the following steps: p-phenylenediamine and tetraethylene glycol are used as raw materials, and the mass ratio is 1:20, adding absolute ethyl alcohol, performing ultrasonic dissolution, putting the solution into a 100mL stainless steel autoclave (model YZPR-100 ML), and reacting for 12 hours at 180 ℃; then the Y-CQDs are obtained by separation steps including filtration, column chromatography and the like.
In the steps (1) and (2), the pH buffer solution is composed of Na with the concentration of 0.2M 2 HPO 4 The solution and citric acid solution with the concentration of 0.1M.
In the steps (1) and (2), the pH of the pH buffer solution is 3 to 7, preferably 6.
In the steps (1) and (2), when the concentration of Y-CQDs in the blank sample solution and the standard sample solution is 0.167 multiplied by 10 -3 In mg/mL, SO in the standard sample solution in step (2) and step (II) 3 2- The concentration of (b) is 20-300. Mu.M, specifically 20. Mu.M, 40. Mu.M, 60. Mu.M, 80. Mu.M, 100. Mu.M, 130. Mu.M, 160. Mu.M, 190. Mu.M, 220. Mu.M, 250. Mu.M, 280. Mu.M, 300. Mu.M.
In step (2), SO 3 2- The standard substance adopts Na 2 SO 3 。
In the steps (1), (2) and (3), the fluorescence test conditions are as follows: lambda ex ＝380-420nm，λ em ＝540-560nm。
In step (2), F n /F 0 And SO 3 2- Is F n /F 0 ＝(6.62496±0.34003)+(0.08275±0.00205)×n[SO 3 2- ]Wherein n [ SO ] 3 2- ]Unit of (2)Is in. Mu.M.
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots, the method comprising the steps of:
dissolving Y-CQDs in a pH buffer solution, diluting and fixing the volume to obtain a blank sample solution, stirring and standing the blank sample solution, and then carrying out ultraviolet visible absorbance test, wherein the absorbance is recorded as A 0 ；
(II) taking a plurality of equal mass parts of Y-CQDs to respectively dissolve the Y-CQDs in a plurality of equal volume parts of pH buffer solutions, and then adding SO-containing buffer solutions with different volumes 3 2- Diluting standard solution of standard substance, diluting to desired volume to obtain a series of standard sample solutions, stirring, standing, and testing ultraviolet and visible absorbance to obtain a series of absorbances A n Separately calculate A n /A 0 Value, then obtain A n /A 0 And SO 3 2- A functional relationship between concentrations;
(III) dissolving Y-CQDs in SO-containing solution to be detected 3 2- Carrying out ultraviolet and visible absorbance test on the polluted water sample to obtain A, and calculating according to the functional relation obtained in the step (II) to obtain SO in the polluted water sample 3 2- The concentration of (c).
In the steps (I), (II) and (III), the fluorescent carbon quantum dots are prepared by adopting the following steps: p-phenylenediamine and tetraethylene glycol are used as raw materials, and the mass ratio is 1:20, adding absolute ethyl alcohol, dissolving by ultrasonic wave, putting the solution into a 100mL stainless steel autoclave (model YZPR-100 ML), and reacting for 12 hours at 180 ℃; then the Y-CQDs are obtained by separation steps including filtration, column chromatography and the like.
In the steps (I) and (II), the pH buffer solution is prepared from Na with the concentration of 0.2M 2 HPO 4 The solution and citric acid solution with the concentration of 0.1M.
In steps (I) and (II), the pH of the pH buffer solution is 3 to 7, preferably 6.
In the steps (I) and (II), the concentration of Y-CQDs in the blank sample solution and the standard sample solution is 0.167 multiplied by 10 - 3 mg/mL, step (2) and step (II), SO in Standard sample solution 3 2- In a concentration of20-300. Mu.M, specifically 20. Mu.M, 40. Mu.M, 60. Mu.M, 80. Mu.M, 100. Mu.M, 130. Mu.M, 160. Mu.M, 190. Mu.M, 220. Mu.M, 250. Mu.M, 280. Mu.M, 300. Mu.M.
In step (II), SO 3 2- The standard substance adopts Na 2 SO 3 。
In the steps (I), (II) and (III), the ultraviolet visible absorbance test conditions are as follows: lambda [ alpha ] Absorption of ＝560-565nm。
In step (II), A n /A 0 And SO 3 2- Is A n /A 0 ＝(0.6882±0.00665)+(-0.00177±4.01727E-5)×n[SO 3 2- ]Wherein n [ SO ] 3 2- ]The unit of (d) is μ M.
By virtue of excellent characteristics of the carbon quantum dots, such as good light stability, low production cost, simple preparation process, good biocompatibility, non-toxicity and the like, the carbon quantum dots are widely applied to aspects of drug transportation, biological probes, biological imaging, fluorescent probes, photocatalysis and the like by researchers in various fields in recent years, and particularly in the field of fluorescent probes, the carbon quantum dots are widely applied to detection of various ions and organic molecules and can be used as fluorescent detection probes for detection due to the characteristics of non-toxicity, small particle size, excellent optical characteristics and the like.
Compared with the prior art, the invention has the following advantages:
(1) Y-CQDs as a novel zero-dimensional carbon nano material with a large amount of-NH on the surface of the carbon core 2 A fluorescent group such as-COOH, etc., has good fluorescent characteristics when SO is used 3 2- Upon collision with Y-CQDs, the functional group on the surface of Y-CQDs is easily bound to SO 3 2- Oxidation-reduction reaction is carried out to form non-radiative transition, and further the fluorescence of the carbon point is changed; the yellow carbon quantum dots are aligned to SO compared to other fluorescent probes 3 2- The quantitative detection has higher sensitivity and linear relation, and the linear correlation coefficient can reach more than 0.99.
(2) The detection means can perform fluorescence detection by means of a fluorescence spectrometer and can perform absorbance detection by means of an ultraviolet spectrophotometer.
(3) Compared with other traditional detection methods which comprise a reduction method, a polarographic spectrophotometry method, a flow injection method, a chemiluminescence method, an ion chromatography method and the like and are carried out by virtue of laboratory instruments, the detection technology does not need high instrument cost, complex operation steps and complex sample preparation processes; in addition, the yellow carbon quantum dot can be further expanded to be made into a film material, and the change of the color of the material can be obviously perceived by naked eyes of people, so that the yellow carbon quantum dot is applied to field real-time detection.
Drawings
FIG. 1 is a diagram showing SO detection based on Y-CQDs in example 1 3 2- Working principle diagram of (1);
FIG. 2 is a fluorescence spectrum of a standard sample solution and a blank sample solution for each series of concentrations in example 1;
FIG. 3 shows fluorescence intensity and SO in example 1 3 2- A linear plot of concentration;
FIG. 4 is detection of SO based on Y-CQDs in example 3 3 2- Working principle diagram of (1);
FIG. 5 is the UV absorption spectra of the standard sample solution and the blank sample solution of example 3 at various concentrations;
FIG. 6 is the absorbance and SO in example 3 3 2- A linear plot of concentration;
FIG. 7 is a diagram showing the standard sample solution and the blank sample solution of example 1 under the irradiation of an ultraviolet lamp at various concentrations;
FIG. 8 is a diagram showing the sample solutions of the standard sample and the blank sample at various concentrations in example 1 under sunlight;
FIG. 9 is a transmission electron microscope photograph of Y-CQDs.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots comprises the following steps:
(1) Dissolving Y-CQDs in pH buffer solution, and diluting to desired volumeAdding the mixture into a blank sample solution, stirring and standing the mixture, and then carrying out fluorescence test, wherein the fluorescence intensity is recorded as F 0 The fluorescent carbon quantum dot is prepared by the following steps: adding p-phenylenediamine and tetraethylene glycol as raw materials into absolute ethyl alcohol, performing ultrasonic dissolution, placing the solution into a stainless steel high-pressure kettle, reacting at 180 ℃ for 12h, and performing separation to obtain Y-CQDs (the same as below), wherein the pH buffer solution is Na with the concentration of 0.2M 2 HPO 4 The solution and 0.1M citric acid solution (the same below), pH of pH buffer solution is 3-7 (the same below), and lambda is ex ＝380-420nm，λ em =540-560nm (same below);
(2) Dissolving multiple equal mass parts of Y-CQDs in multiple equal volume parts of pH buffer solution, and adding SO-containing solution with different volumes 3 2- Diluting standard solution of standard substance to constant volume to obtain a series of standard sample solutions, stirring, standing, and performing fluorescence test to obtain a series of fluorescence intensities F n Separately calculate F n /F 0 Value, then F is obtained n /F 0 And SO 3 2- A functional relationship between concentrations;
(3) Dissolving Y-CQDs in SO-containing solution to be detected 3 2- Performing fluorescence test on the polluted water sample to obtain F, and calculating according to the functional relation obtained in the step (2) to obtain SO in the polluted water sample 3 2- The concentration of (c).
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots comprises the following steps:
dissolving Y-CQDs in a pH buffer solution, diluting and fixing the volume to obtain a blank sample solution, stirring and standing, and then carrying out ultraviolet visible absorbance test, wherein the absorbance is recorded as A 0 The fluorescent carbon quantum dot is prepared by the following steps: adding p-phenylenediamine and tetraethylene glycol as raw materials into absolute ethyl alcohol, performing ultrasonic dissolution, placing the solution into a stainless steel autoclave, reacting at 180 ℃ for 12h, and then performing a separation step to obtain Y-CQDs (the same below), wherein the pH buffer solution is Na with the concentration of 0.2M 2 HPO 4 The solution and citric acid solution with concentration of 0.1M (the same below), pH of pH buffer solution is 3-7 (the same below),λ absorption of =560-565nm (same below);
(II) taking a plurality of equal mass parts of Y-CQDs to respectively dissolve the Y-CQDs in a plurality of equal volume parts of pH buffer solutions, and then adding SO-containing buffer solutions with different volumes 3 2- Diluting the standard solution of the standard substance to a constant volume to obtain a series of standard sample solutions, stirring and standing, and performing ultraviolet-visible absorbance test to obtain a series of absorbances A n Separately calculate A n /A 0 Value, then obtain A n /A 0 And SO 3 2- A functional relationship between concentrations;
(III) dissolving Y-CQDs in SO-containing solution to be detected 3 2- Carrying out ultraviolet and visible absorbance test on the polluted water sample to obtain A, and calculating according to the functional relation obtained in the step (II) to obtain SO in the polluted water sample 3 2- The concentration of (c).
Example 1
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots (Y-CQDs), wherein the Y-CQDs are used as fluorescent probes and prepared by the following steps: p-phenylenediamine and tetraethylene glycol are used as raw materials, and the mass ratio is 1:20, adding absolute ethyl alcohol, dissolving by ultrasonic wave, putting the solution into a 100mL stainless steel autoclave (YZPR-100 ML), and reacting for 12 hours at 180 ℃; then, separation steps such as filtration and column chromatography are carried out to obtain Y-CQDs, and a projection electron microscope image of the obtained Y-CQDs is shown in FIG. 9 (the scale bar of the image is 100nm, and the scale bar of the upper right small image is 5 nm).
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots (Y-CQDs), the method comprising the steps of, as shown in fig. 1:
(1) Preparing a Y-CQDs mother solution: weighing appropriate amount of Y-CQDs to be dissolved in deionized water to obtain the concentration of about 0.01 mg/mL -1 The mother liquor of Y-CQDs.
(2) preparing a pH buffer solution: using a certain proportion of Na 2 HPO 4 (0.2M) and citric acid (0.1M) were formulated as pH buffers at different pH to ensure that Y-CQDs were undergoing SO 3 2- The detection has the best acid-base environment.
(3) Respectively take 50 μ L Y-CQDs stock, 200 μ L pH =6 pH buffer solution was added to a clean glass vial, followed by different volumes of Na 2 SO 3 Standard solution, diluted to 3mL in deionized water to make Na 2 SO 3 The final concentration range of (b) is 20 to 300. Mu.M (specifically, 20. Mu.M, 40. Mu.M, 60. Mu.M, 80. Mu.M, 100. Mu.M, 130. Mu.M, 160. Mu.M, 190. Mu.M, 220. Mu.M, 250. Mu.M, 280. Mu.M, 300. Mu.M), and the fluorescence test (. Lamda.M) is carried out by stirring and standing for a while ex ＝400nm，λ em =460 nm), the fluorescence spectrum is shown in FIG. 2 (the curves in the graph correspond to 0. Mu.M, 20. Mu.M, 40. Mu.M, 60. Mu.M, 80. Mu.M, 100. Mu.M, 130. Mu.M, 160. Mu.M, 190. Mu.M, 220. Mu.M, 250. Mu.M, 280. Mu.M and 300. Mu.M from bottom to top), and the fluorescence intensities are F, respectively 1 ＝2352、F 2 ＝2941、F 3 ＝3335、F 4 ＝4048、F 5 ＝4312、F 6 ＝4998、F 7 ＝5811、F 8 ＝6610、F 9 ＝7415、F 10 ＝8327、F 11 ＝8777，F 12 ＝8907。
(4) Add 50. Mu. L Y-CQDs stock, 200. Mu.L pH =6 buffer to a clean glass vial, dilute to a total volume of 3mL with deionized water, stir, stand for a short period, and perform fluorescence (lambda. Fluorescence test) ex ＝400nm，λ em =460 nm), the corresponding fluorescence spectrum is shown in fig. 2, and the fluorescence intensity is F 0 =2032, and a series of F's are calculated n /F 0 . A series of F will be obtained n /F 0 (as y value) and SO 3 2- The concentration (as the value of x) was plotted to obtain a linear relationship chart (the broken line in the graph is the joint line of each data, and the straight line is the fitted line), namely F, as shown in FIG. 3 n /F 0 ＝(6.62496±0.34003)+(0.08275±0.00205)×n[SO 3 2- ]Wherein n [ SO ] 3 2- ]Has the unit of mu M, the sum of squared residuals is 3.15451, pearson's r is 0.99724, R is 2 (COD)＝0.99449，R 2 (adjusted) =0.99387, demonstrate yellow carbon quantum dots to SO 3 2- The detection has good linear relation and sensitivity, and the linear correlation coefficient can reach 0.99387.
In addition, FIG. 7 and FIG. 8 are respectively a seriesThe full graph of the standard sample solution and the blank sample solution with column concentration under the irradiation of ultraviolet lamp and sunlight is shown in FIG. 7 (the leftmost end of FIG. 7 is a bottle containing Y-CQDs blank sample solution as a control, and Na is contained in other bottles 2 SO 3 The concentration of (A) increases from 20 to 300. Mu.M from the left and right), it can be visually observed that SO is added to the pH buffer solution containing Y-CQDs 3 2- After that, the solution fluorescence is converted from yellow light to blue light and with SO 3 2- The blue fluorescence becomes stronger and stronger, and the fluorescence intensity is enhanced. It can be visually observed from FIG. 8 (the leftmost end of FIG. 8 is a bottle containing a blank sample solution of Y-CQDs as a control, and Na in the other bottles 2 SO 3 The concentration of (A) increases from 20 to 300. Mu.M from the left and right), it can be visually observed that SO is added to the pH buffer solution containing Y-CQDs 3 2- After that, the solution becomes lighter in color, gradually transitioning from dark purple to light purple, and with SO 3 2- Increase, solution color until clear.
Example 2
In order to examine the SO shown in example 1 3 2- The actual performance of the detection mode is that a comparison experiment is carried out on an actual water sample (tap water); the operation is as follows: (1) Taking 20 μ L of mother liquor of Y-CQDs, 200 μ L of buffer solution with pH =6, adding a certain amount of SO 3 2- Putting the aqueous solution into a transparent small bottle, adding deionized water to make the total volume be 3mL, and preparing a series of SO 3 2- Stirring the standard solution at room temperature, standing, and then transferring the standard solution into a 4mL quartz cuvette for fluorescence test to obtain a linear equation shown in example 1; (2) Adding SO into tap water by adopting an external standard method 3 2- Three control experiments (with the concentrations of the added standard substances of 100, 300 and 500 mu M respectively) are carried out on the standard aqueous solution, three parallel samples are arranged in each group of experiments, the experimental operation steps are the same as (1), fluorescence emission intensity data are obtained and are substituted into the linear equation obtained in (1) (the step (1) can also be omitted, and the obtained data are directly substituted into the linear equation obtained in the example 1 for calculation), SO that the measured SO is calculated 3 2- The concentration values and results are shown in Table 1.
TABLE 1
Example 3
A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots (Y-CQDs), wherein the Y-CQDs are used as fluorescent probes and adopt the Y-CQDs prepared in example 1. The method comprises the following steps, as shown in fig. 4:
(1) Preparing a Y-CQDs mother solution: weighing appropriate amount of Y-CQDs, and dissolving in deionized water to obtain concentration of about 0.01 mg/mL -1 The mother liquor of Y-CQDs.
(2) preparing a pH buffer solution: using a certain proportion of Na 2 HPO 4 (0.2M) and citric acid (0.1M) were prepared as pH buffered solutions at different pH.
(3) 50 μ L Y-CQDs stock solution, 200 μ L pH =6 buffer solution was added to a clean glass vial separately, followed by different volumes of Na 2 SO 3 Standard solution, diluted to 3mL in deionized water to make Na 2 SO 3 The final concentration of (b) is in the range of 20 to 300. Mu.M (specifically, 20. Mu.M, 40. Mu.M, 60. Mu.M, 80. Mu.M, 100. Mu.M, 130. Mu.M, 160. Mu.M, 190. Mu.M, 220. Mu.M, 250. Mu.M, 280. Mu.M, 300. Mu.M), and the mixture is stirred and left to stand for a while, and subjected to ultraviolet-visible absorbance test (. Lamda.M) Absorption of =562 nm), corresponding ultraviolet absorption spectrum is shown in figure 5 (the curve in the figure corresponds to 0 μ M, 20 μ M, 40 μ M, 60 μ M, 80 μ M, 100 μ M, 130 μ M, 160 μ M, 190 μ M, 220 μ M, 250 μ M, 280 μ M, 300 μ M from top to bottom in sequence), absorbance is A respectively 1 ＝0.34、A 2 ＝0.31、A 3 ＝0.29、A 4 ＝0.27、A 5 ＝0.26、A 6 ＝0.24、A 7 ＝0.21、A 8 ＝0.18、A 9 ＝0.16、A 10 ＝0.12、A 11 ＝0.08、A 12 ＝0.07。
(4) 50 μ L Y-CQDs stock solution, 200 μ L pH =6 buffer solution was added to a clean glass vial, diluted to a total volume of 3mL with deionized water, left to stand with stirring for a while, and subjected to light absorption test (λ:. Lamda.) (for a while) Absorption of =562 nm), correspondingThe ultraviolet absorption spectrum is shown in FIG. 5, and the absorbance is A 0 =0.51, and a series of a's are calculated n /A 0 . A series A obtained n /A 0 (as y value) and SO 3 2- The concentrations (as x values) were plotted to obtain a linear relationship graph (broken line in the graph is a connecting line of each data, and straight line is a fitting line), A, as shown in FIG. 6 n /A 0 ＝(0.6882±0.00665)+(-0.00177±4.01727E-5)×n[SO 3 2- ]Wherein n [ SO ] 3 2- ]Has a unit of mu M, a sum of squared residuals of 0.00121, pearson's r of-0.9977 2 (COD)＝0.9954，R 2 (adjusted) =0.99489, demonstrate yellow carbon quantum dots to SO 3 2- The detection has good linear relation and sensitivity, and the linear correlation coefficient can reach 0.99489.
Example 4
In order to examine the SO shown in example 3 3 2- The actual performance of the detection mode is that a comparison experiment is carried out on an actual water sample (tap water); the operation is as follows: (1) Taking 20 μ L of mother liquor of Y-CQDs, 200 μ L of buffer solution with pH =6, adding a certain amount of SO 3 2- Putting the aqueous solution into a transparent small bottle, adding deionized water to make the total volume be 3mL, and preparing a series of SO 3 2- Stirring the standard solution at room temperature, standing, and then transferring the standard solution into a 4mL cuvette for ultraviolet-visible absorbance test to obtain a linear equation shown in the embodiment 3; (2) Adding SO into tap water by adopting an external standard method 3 2- Performing three groups of control experiments (with the concentrations of the added standard substances of 100, 300 and 500 mu M respectively) on the standard aqueous solution, setting three parallel samples in each group of experiments, performing the same experimental operation steps as (1) to obtain ultraviolet-visible absorbance data, substituting the ultraviolet-visible absorbance data into the linear equation obtained in (1) (or omitting the step (1), and directly substituting the obtained data into the linear equation obtained in the example 3 for calculation), thereby calculating and determining SO 3 2- The concentration values and results are shown in Table 2.
TABLE 2
As can be seen from tables 1 and 2, the two methods of the present invention are for determining SO 3 2- Has good sensitivity in concentration and simple operation.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. A method for detecting sulfite ions based on yellow fluorescent carbon quantum dots is characterized by comprising the following steps:
(1) Dissolving Y-CQDs in pH buffer solution, diluting to constant volume to obtain blank sample solution, stirring, standing, performing fluorescence test, and recording fluorescence intensity as F 0 ；
(2) Dissolving multiple parts of equal mass Y-CQDs in multiple parts of equal volume pH buffer solution, and adding different volumes of SO-containing buffer solution 3 2- Diluting standard solution of standard substance to desired volume to obtain a series of standard sample solutions, stirring, standing, performing fluorescence test to obtain a series of fluorescence intensities F n Separately calculate F n /F 0 Value, then F is obtained n /F 0 And SO 3 2- A functional relationship between concentrations;
(3) Dissolving Y-CQDs in SO-containing solution to be detected 3 2- Performing fluorescence test on the polluted water sample to obtain F, and calculating according to the functional relation obtained in the step (2) to obtain SO in the polluted water sample 3 2- The concentration of (c);
under an ultraviolet lamp: adding SO to pH buffer solution containing Y-CQDs 3 2- After that, the solution fluorescence is converted from yellow light to blue light, and thenTo SO 3 2- The blue fluorescence becomes stronger and stronger, and the fluorescence intensity is enhanced;
under a fluorescent lamp: adding SO into pH buffer solution containing Y-CQDs 3 2- After that, the solution becomes lighter in color, gradually transitioning from dark purple to light purple, and with SO 3 2- Increase, solution color until clear;
in the steps (1), (2) and (3), the fluorescent carbon quantum dots are prepared by the following steps: p-phenylenediamine and tetraethylene glycol are taken as raw materials, added into absolute ethyl alcohol to be dissolved by ultrasonic, and then the solution is placed into a stainless steel high-pressure autoclave to react for 12 hours at 180 ℃; then obtaining Y-CQDs through a separation step.
2. The method for detecting sulfite ions based on yellow fluorescent carbon quantum dots according to claim 1, wherein in the steps (1) and (2), the pH buffer solution is composed of Na with the concentration of 0.2M 2 HPO 4 The solution and citric acid solution with the concentration of 0.1M.
3. The method for detecting sulfite ions based on yellow fluorescent carbon quantum dots according to claim 1, wherein in the steps (1) and (2), the pH of the pH buffer solution is 3-7.
4. The method for detecting sulfite ions based on yellow fluorescent carbon quantum dots according to claim 1, wherein in the steps (1) and (2), when the concentration of Y-CQDs in the blank sample solution and the standard sample solution is 0.167 x 10 - 3 mg/mL, step (2), SO in Standard sample solution 3 2- The concentration of (2) is 20-300. Mu.M.
5. The method for detecting sulfite ions based on yellow fluorescent carbon quantum dots according to claim 1, wherein in the steps (1), (2) and (3), the fluorescence test conditions are as follows: lambda [ alpha ] ex =380-420 nm，λ em =540-560 nm。
6. The method for detecting sulfite ions based on yellow fluorescent carbon quantum dots according to claim 1, wherein in the step (2), F n /F 0 And SO 3 2- Is F n /F 0 =(6.62496±0.34003)+(0.08275±0.00205)×n[SO 3 2- ]Wherein n [ SO ] 3 2- ]The unit of (d) is μ M.
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