CN110057792A - A kind of Fluoride Analysis based on fluorescence graphene quantum dot - Google Patents
A kind of Fluoride Analysis based on fluorescence graphene quantum dot Download PDFInfo
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- CN110057792A CN110057792A CN201910196257.1A CN201910196257A CN110057792A CN 110057792 A CN110057792 A CN 110057792A CN 201910196257 A CN201910196257 A CN 201910196257A CN 110057792 A CN110057792 A CN 110057792A
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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
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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
- G01N21/62—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"
- G01N2021/6432—Quenching
Abstract
The invention discloses a kind of Fluoride Analysis based on fluorescence graphene quantum dot, steps are as follows: (1) citric acid, ethylenediamine and phenyl boric acid is dissolved in ultrapure water, heating heating；Water dilutes to obtain B, N-GQDs solution；(2) by B, N-GQDs solution, Hg2+The fluorescence intensity F of each mixed solution fluorescence spectrum is surveyed in the fluorine ion aqueous solution of deionized water solution and serial various concentration, mixing；Using fluorinion concentration as abscissa, using corresponding fluorescence recovery rate as ordinate, linear fit must detect fluorine ion standard curve；(3) by B, N-GQDs solution, Hg2+Deionized water solution and fluorine ion aqueous solution to be measured mix to obtain mixed liquor to be measured；(4) mixed liquor fluorescence spectrum to be measured is measured, fluorescence recovery rate R is calculated, standard curve is substituted into, obtains fluorinion concentration in mixed liquor to be measured.Raw material of the present invention be easy to get it is inexpensive, detection quickly, easy to operate, detection range is wide, and Monitoring lower-cut is low.
Description
Technical field
The invention belongs to technical field of chemical detection, are related to a kind of fluorine ion detection side based on fluorescence graphene quantum dot
Method.
Background technique
In various anion, ionic radius minimum and the strongest fluorine ion (F of electronegativity-) because of its unique chemical property
And it is concerned.Physiologically, fluorine ion is the important composition element of tooth and bone, with human life activity and tissue generation
A variety of diseases can be induced by thanking to closely related, abnormal fluorinion concentration, such as tooth and bone fluorine poisoning, stomach and kidney trouble, very
Extremely it can not work independently and live；In the environment, it is irrigated with fluorinated water metallurgy, uses fluorine-containing articles for daily use (toothpaste, battery and sky
Adjust), can all soil and groundwater be made to be contaminated.Therefore, either still exist in medical diagnosis on disease to the quantitative detection of fluorine ion
All there is important practical significance in terms of environmental protection.With traditional detection method (flame atomic absorption spectrometry, inductive coupling
Plasma Mass Spectrometry, electrochemical process, colorimetric analysis) it compares, fluorescence sense technology is concerned because of its unique performance,
Including easy to operate, detection is quick and low in cost.
A kind of fluorescent nano material as novel and unique --- graphene quantum dot (Graphene quantum dots,
GQDs), compared with organic fluorescent dye, optical property is stablized, and can be applied to long-term cell imaging and cell marking field；
It compared with semiconductor-quantum-point, is free of poisonous and hazardous metallic element (cadmium, lead, arsenic etc.), there is excellent biocompatibility,
It can be applied to the fields such as bio-sensing and analysis detection.Therefore, graphene quantum dot can be used as organic fluorescent dye and semiconductor
The substitute of quantum dot.
Currently, there has been no the reports of the Fluoride Analysis based on fluorescence graphene quantum dot.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide it is a kind of based on the fluorine of fluorescence graphene quantum dot from
Sub- detection method.
Technical solution of the present invention is summarized as follows:
A kind of Fluoride Analysis based on fluorescence graphene quantum dot, includes the following steps:
(1) in proportion, 1g citric acid, 0.3g ethylenediamine and 0.1g phenyl boric acid are dissolved in 10ml ultrapure water, stirring is equal
It is even to obtain solution 1；By solution 1,160~240 DEG C of heating are risen to 5 DEG C/min heating rate and react 3~7h；It is cooled to room temperature,
Obtain dark brown B, N-GQDs original solution；The B is diluted with ultrapure water, N-GQDs original solution, obtaining mass fraction is 0.0005%
~0.001% B, N-GQDs solution；
(2) by the B, N-GQDs solution, concentration is the Hg of 5~20 μm of ol/L2+Deionized water solution and concentration range 0 and
A series of fluorine ion aqueous solution of various concentrations of 0.01-20mmol/L, mixes for 0.375:1:1 respectively by volume, measurement
The fluorescence intensity F of the fluorescence spectrum of each mixed solution；Using fluorinion concentration as abscissa, it is with corresponding fluorescence recovery rate
Ordinate carries out linear fit, obtains the standard curve of detection fluorine ion；
(3) by the B, N-GQDs solution, concentration is the Hg of 5~20 μm of ol/L2+Deionized water solution and fluorine ion water to be measured
Solution is 0.375:1:1 mixing by volume, obtains mixed liquor to be measured；
(4) fluorescence spectrum of mixed liquor to be measured is measured, and calculates fluorescence recovery rate R, the standard for substituting into detection fluorine ion is bent
In line, the concentration of fluorine ion in mixed liquor to be measured is obtained；R=(F-F0)/F0, wherein F0For in ultrapure water alternative steps (2)
Fluorine ion aqueous solution, the fluorescence intensity of the fluorescence spectrum of the mixed solution measured.
Measure the parameter of fluorescence spectrum are as follows: excitation wavelength 350nm, exciting slit 2.5nm；Launch wavelength is 450nm,
Transmite slit is 5nm.
Advantages of the present invention:
Raw material be easy to get it is inexpensive, detection quickly, easy to operate, detection range is wide, and Monitoring lower-cut is low.
Detailed description of the invention
Fig. 1 is the fluorescence spectrum of 1 step of embodiment (2) each mixed solution.From bottom to up, every curve respectively represents dense
Degree is the F of 0,0.25,0.50,0.75,1.0,2.0,3.0,4.0,5.0,6.0,7.0,8.0,9.0,10.0mmol/L-Ion with
B, N-GQDs solution and Hg2+Fluorescence spectrum after deionized water solution immixture.
Fig. 2 is the standard curve that 1 step of embodiment (2) detects fluorine ion.
Fig. 3 is the fluorescence spectrum of 2 step of embodiment (2) each mixed solution.From bottom to up, every curve respectively represents dense
Degree is the fluorine ion and B of 0,2.0,5.0,7.0,10.0,12.0,15.0,17.0,20.0mmol/L, N-GQDs solution and Hg2+From
Fluorescence spectrum after sub- aqueous solution immixture.
Fig. 4 is the standard curve that 2 step of embodiment (2) detects fluorine ion.
Fig. 5 is the fluorescence spectrum of 3 step of embodiment (2) each mixed solution.From bottom to up, every curve respectively represents dense
Degree is the fluorine ion and B of 0,0.01,0.25,0.50,0.75,1.0,2.0,3.0,4.0mmol/L, N-GQDs solution and Hg2+From
Fluorescence spectrum after sub- aqueous solution immixture.
Fig. 6 is the standard curve that 3 step of embodiment (2) detects fluorine ion.
Specific embodiment
The embodiment of the present invention is only used to illustrate the technical scheme of the present invention and not to limit it, although referring to preferred embodiment to this
Invention is described in detail, those skilled in the art should understand that, technical solution of the present invention can be repaired
Change or equivalent replacement should all cover and want in right of the invention without departing from the spirit and scope of the technical solution of the present invention
It asks in range.
Embodiment 1
A kind of Fluoride Analysis based on fluorescence graphene quantum dot, includes the following steps:
(1) 1g citric acid, 0.3g ethylenediamine and 0.1g phenyl boric acid are dissolved in 10ml ultrapure water, are uniformly mixing to obtain molten
Liquid 1；By solution 1,200 DEG C of heating reaction 5h are risen to 5 DEG C/min heating rate；It is cooled to room temperature, obtains dark brown B, N-
GQDs original solution；The B is diluted with ultrapure water, N-GQDs original solution obtains the B that mass fraction is 0.0008%, N-GQDs solution；
(2) by the B, N-GQDs solution, concentration is the Hg of 10 μm of ol/L2+Ion (mercuric nitrate) aqueous solution and concentration range
A series of various concentrations of 0 and 0.25-10mmol/L fluorine ion (sodium fluoride) aqueous solution (specially 0,0.25,0.50,
0.75,1.0,2.0,3.0,4.0,5.0,6.0,7.0,8.0,9.0,10.0mmol/L), it is by volume 0.375:1:1 difference
Mixing, measures the fluorescence intensity F of the fluorescence spectrum (see Fig. 1) of each mixed solution；Using fluorinion concentration as abscissa, with opposite
The fluorescence recovery rate answered is ordinate, carries out linear fit, obtains detection F-The standard curve of ion, (see Fig. 2)；
(3) by the B, N-GQDs solution, concentration is the Hg of 10 μm of ol/L2+Deionized water solution and fluorine ion aqueous solution to be measured
(sodium fluoride aqueous solution that concentration is 1.5mmol/L) is 0.375:1:1 mixing by volume, obtains mixed liquor to be measured；
(4) fluorescence spectrum of mixed liquor to be measured is measured, and calculates fluorescence recovery rate R=0.12180, substitutes into detection fluorine ion
Standard curve (Fig. 2) in, obtain fluorine ion in mixed liquor to be measured concentration be 1.536mmol/L；
It is that the present invention measures the result is that 1.536mmol/L, relative error 2.4%, with its known concentration 1.5mmol/L phase
Difference can be ignored, and illustrate that measurement result of the present invention is sensitive, accurate.
R=(F-F0)/F0=0.05141 [M]+0.04282, R2=0.9940, the range of linearity is 0.25~7.0mM, detection
Lower limit is 0.180mM.Wherein F0For with the F in ultrapure water alternative steps (2)-Deionized water solution, the fluorescence of the mixed solution measured
The fluorescence intensity of spectrum.M in formula is F-The concentration of ion.
Measure the parameter of fluorescence spectrum are as follows: excitation wavelength 350nm, exciting slit 2.5nm；Launch wavelength is 450nm,
Transmite slit is 5nm.
Embodiment 2
A kind of Fluoride Analysis based on fluorescence graphene quantum dot, includes the following steps:
(1) 1g citric acid, 0.3g ethylenediamine and 0.1g phenyl boric acid are dissolved in 10ml ultrapure water, are uniformly mixing to obtain molten
Liquid 1；By solution 1,160 DEG C of heating reaction 7h are risen to 5 DEG C/min heating rate；It is cooled to room temperature, obtains dark brown B, N-
GQDs original solution；The B is diluted with ultrapure water, N-GQDs original solution obtains the B that mass fraction is 0.0005%, N-GQDs solution；
(2) by the B, N-GQDs solution, concentration is the Hg of 20 μm of ol/L2+Ion (mercuric nitrate) aqueous solution and concentration range
In a series of F of various concentrations of 0 and 2-20mmol/L-Ion (sodium fluoride) aqueous solution (0,2.0,5.0,7.0,10.0,
12.0,15.0,17.0,20.0mmol/L), it is mixed respectively for 0.375:1:1 by volume, measures the fluorescence of each mixed solution
The fluorescence intensity F of spectrum (see Fig. 3)；With F-Ion concentration is abscissa, using corresponding fluorescence recovery rate as ordinate, is carried out
Linear fit obtains detection F-The standard curve of ion, (see Fig. 4)；
(3) by the B, N-GQDs solution, concentration is the Hg of 20 μm of ol/L2+Deionized water solution and F to be measured-Deionized water solution
(sodium fluoride aqueous solution that concentration is 10.0mmol/L) is 0.375:1:1 mixing by volume, obtains mixed liquor to be measured；
(4) fluorescence spectrum of mixed liquor to be measured is measured, and calculates fluorescence recovery rate R=0.17937, substitutes into detection F-Ion
Standard curve in, obtain F in mixed liquor to be measured-The concentration of ion is 9.974mmol/L；
It is that the present invention measures the result is that 9.974mmol/L, relative error 0.26%, with its known concentration 10.0mmol/L
Difference can be ignored, and illustrate that measurement result of the present invention is sensitive, accurate.
R=(F-F0)/F0=0.01822 [M]+0.00236, R2=0.9870, the range of linearity is 2.0~20.0mmol/L,
Monitoring lower-cut is 0.177mmol/L.Wherein F0For with the F in ultrapure water alternative steps (2)-Deionized water solution, the mixing measured are molten
The fluorescence intensity of the fluorescence spectrum of liquid；M is F in formula-The concentration of ion.
Measure the parameter of fluorescence spectrum are as follows: excitation wavelength 350nm, exciting slit 2.5nm；Launch wavelength is 450nm,
Transmite slit is 5nm.
Embodiment 3
A kind of Fluoride Analysis based on fluorescence graphene quantum dot, includes the following steps:
(1) 1g citric acid, 0.3g ethylenediamine and 0.1g phenyl boric acid are dissolved in 10ml ultrapure water, are uniformly mixing to obtain molten
Liquid 1；By solution 1,240 DEG C of heating reaction 3h are risen to 5 DEG C/min heating rate；It is cooled to room temperature, obtains dark brown B, N-
GQDs original solution；The B is diluted with ultrapure water, N-GQDs original solution obtains the B that mass fraction is 0.001%, N-GQDs solution；
(2) by the B, N-GQDs solution, concentration is the Hg of 5 μm of ol/L2+Ion (mercuric nitrate) aqueous solution and concentration range
In a series of F of various concentrations of 0 and 0.01-4mmol/L-Deionized water solution (0,0.01,0.25,0.50,0.75,1.0,
2.0,3.0,4.0mmol/L), mixed respectively for 0.375:1:1 by volume, measure each mixed solution fluorescence spectrum (see
Fluorescence intensity F Fig. 5)；With F-Ion concentration is abscissa, using corresponding fluorescence recovery rate as ordinate, carries out Linear Quasi
It closes, obtains detection F-The standard curve of ion, (see Fig. 6)；
(3) by the B, N-GQDs solution, concentration is the Hg of 5 μm of ol/L2+Deionized water solution and F to be measured-Deionized water solution
(sodium fluoride aqueous solution that concentration is 0.50mmol/L) is 0.375:1:1 mixing by volume, obtains mixed liquor to be measured；
(4) fluorescence spectrum of mixed liquor to be measured is measured, and calculates fluorescence recovery rate R=0.12316, substitutes into detection F-Ion
Standard curve in, obtain F in mixed liquor to be measured-The concentration of ion is 0.5274mmol/L；
It is that the present invention measures the result is that 0.5274mmol/L, relative error 5.48%, with its known concentration 0.50mmol/
L difference can be ignored, and illustrate that measurement result of the present invention is sensitive, accurate.
R=(F-F0)/F0=0.19289 [M]+0.02143, R2=0.9925, the range of linearity is 0.01~1.0mmol/L,
Monitoring lower-cut is 0.0618mmol/L.Wherein F0For with the F in ultrapure water alternative steps (2)-Deionized water solution, the mixing measured
The fluorescence intensity of the fluorescence spectrum of solution, formula M are F-The concentration of ion.
Measure the parameter of fluorescence spectrum are as follows: excitation wavelength 350nm, exciting slit 2.5nm；Launch wavelength is 450nm,
Transmite slit is 5nm.
The present invention is prepared for the nitrogen co-doped stone of boron using citric acid, ethylenediamine and phenyl boric acid as raw material, by one step hydro thermal method
Black alkene quantum dot (Boron-nitrogen co-doped graphene quantum dots, B, N-GQDs).As addition F-From
Son is added to B, N-GQDs-Hg2+In fluorescent quenching system, due to F-And Hg2+Stronger combination, makes Hg between ion2+From
Son is restored in B, the fluorescence of N-GQDs surface desorption, quenching.According to fluorescence recovery extent and F-Pass between ion concentration
Unknown F detects in system-The concentration of ion.
Claims (2)
1. a kind of Fluoride Analysis based on fluorescence graphene quantum dot, it is characterized in that including the following steps:
(1) in proportion, 1g citric acid, 0.3g ethylenediamine and 0.1g phenyl boric acid are dissolved in 10ml ultrapure water, are stirred evenly
To solution 1；By solution 1,160~240 DEG C of heating are risen to 5 DEG C/min heating rate and react 3~7h；It is cooled to room temperature, obtains
Dark brown B, N-GQDs original solution；Dilute the B with ultrapure water, N-GQDs original solution, obtain mass fraction be 0.0005%~
0.001% B, N-GQDs solution；
(2) by the B, N-GQDs solution, concentration is the Hg of 5~20 μm of ol/L2+Deionized water solution and concentration range 0 and
A series of fluorine ion aqueous solution of various concentrations of 0.01-20mmol/L, mixes for 0.375:1:1 respectively by volume, measurement
The fluorescence intensity F of the fluorescence spectrum of each mixed solution；Using fluorinion concentration as abscissa, it is with corresponding fluorescence recovery rate
Ordinate carries out linear fit, obtains the standard curve of detection fluorine ion；
(3) by the B, N-GQDs solution, concentration is the Hg of 5~20 μm of ol/L2+Deionized water solution and fluorine ion aqueous solution to be measured
It is mixed by volume for 0.375:1:1, obtains mixed liquor to be measured；
(4) fluorescence spectrum of mixed liquor to be measured is measured, and calculates fluorescence recovery rate R, is substituted into the standard curve of detection fluorine ion,
Obtain the concentration of fluorine ion in mixed liquor to be measured.
2. a kind of detection method of fluorine ion based on fluorescence graphene quantum dot according to claim 1, it is characterized in that
Measure the parameter of fluorescence spectrum are as follows: excitation wavelength 350nm, exciting slit 2.5nm；Launch wavelength is 450nm, transmite slit
For 5nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112675892A (en) * | 2020-12-27 | 2021-04-20 | 上海应用技术大学 | Hollow N, B-GQDs-CdS @ TiO2Nano catalyst and preparation method and application thereof |
| CN113916845A (en) * | 2020-07-10 | 2022-01-11 | Tcl科技集团股份有限公司 | Method for detecting polyhydroxy compound |
| CN114894757A (en) * | 2022-04-30 | 2022-08-12 | 桂林理工大学 | Method for detecting multiple heavy metal ions by using lead-doped PEG (polyethylene glycol) passivated graphene quantum dot fluorescent probe |
| CN114894757B (en) * | 2022-04-30 | 2024-05-17 | 桂林理工大学 | Method for detecting various heavy metal ions by using lead-doped PEG-passivated graphene quantum dot fluorescent probe |
-
2019
- 2019-03-15 CN CN201910196257.1A patent/CN110057792A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| PANXING YANG 等: "B,N-Co-doped graphene quantum dots as fluorescence sensor for detection of Hg2+ and F ions", 《ANALYTICAL METHODS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113916845A (en) * | 2020-07-10 | 2022-01-11 | Tcl科技集团股份有限公司 | Method for detecting polyhydroxy compound |
| CN112675892A (en) * | 2020-12-27 | 2021-04-20 | 上海应用技术大学 | Hollow N, B-GQDs-CdS @ TiO2Nano catalyst and preparation method and application thereof |
| CN112675892B (en) * | 2020-12-27 | 2022-07-05 | 上海应用技术大学 | Hollow N, B-GQDs-CdS @ TiO2Nano catalyst and preparation method and application thereof |
| CN114894757A (en) * | 2022-04-30 | 2022-08-12 | 桂林理工大学 | Method for detecting multiple heavy metal ions by using lead-doped PEG (polyethylene glycol) passivated graphene quantum dot fluorescent probe |
| CN114894757B (en) * | 2022-04-30 | 2024-05-17 | 桂林理工大学 | Method for detecting various heavy metal ions by using lead-doped PEG-passivated graphene quantum dot fluorescent probe |
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