CN108226119A - A kind of method using carbon quantum dot phosphorescence detection ferric ion concentration - Google Patents
A kind of method using carbon quantum dot phosphorescence detection ferric ion concentration Download PDFInfo
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- CN108226119A CN108226119A CN201810036957.XA CN201810036957A CN108226119A CN 108226119 A CN108226119 A CN 108226119A CN 201810036957 A CN201810036957 A CN 201810036957A CN 108226119 A CN108226119 A CN 108226119A
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- 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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Abstract
The present invention relates to a kind of methods using carbon quantum dot phosphorescence detection ferric ion concentration, include the following steps：The ferric ion standard solution of multiple and different concentration is prepared, is separately added into carbon quantum dot and cyanuric acid, is uniformly mixed；Acquired solution is respectively put into sepectrophotofluorometer, phosphorescence intensity value is recorded under phosphorescence pattern, and draw linear regression curves；Solution to be measured is detected according to the method described above, gained phosphorescence intensity data are brought into and are substituted into the regression curve, obtain the ferric ion concentration of solution to be measured.Operation is simple for method provided by the invention, compared to the interference that fluorescence detection method can eliminate background fluorescence and particle scattering light in solution, has higher signal-to-noise ratio and accuracy of detection.
Description
Technical field
The invention belongs to metal ion detection field more particularly to carbon quantum dot phosphorescence in ferric ion detection
Using.
Background technology
Iron ion is that life entity carries out one of necessary ion of vital movement, is the main matter to sustain life, is to participate in
The transport of oxygen, the formation of muscle, life energy invertase the important meals ion that hemachrome enzyme is formed one by one.Iron ion is in life
Content can excessively cause iron ion to be poisoned in life body, so as to cause diseases such as hemochrome deposition, dysfunction of liver and diabetes.Cause
The normal operation of this body that sustains life, it is necessary to ensure iron concentration within limits.
Carbon quantum dot is expected to substitute organic dyestuff and mostly containing a huge sum of money so that stability is good, toxicity is low, is easy to the advantages such as functionalization
The semiconductor-quantum-point of category has very big application prospect in fields such as cell imaging, biochemical analysis.At present for current carbon quantum
Most of point ion detection is using its fluorescent characteristic, and few people are detected using the phosphorescence of carbon quantum dot.Compared to glimmering
Light detection, phosphorescence have a longer life expectancy and background fluorescence and particle in solution therefore can be eliminated with larger Stokes shift dissipates
The interference of light is penetrated, in the detection with higher signal-to-noise ratio and accuracy of detection.
Invention content
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of application carbon quantum dot phosphorescence detection three
The method of valency iron concentration, this method has higher sensitivity and preferable selectivity, and the preparation method of raw material is simple
It is easy.
Specifically, method provided by the invention includes the following steps：
(1) the ferric ion standard solution of multiple and different concentration is prepared, is separately added into carbon quantum dot and cyanuric acid,
After mixing, multiple compound suspensions of carbon quantum dot-standard items are obtained；
(2) the compound suspension of carbon quantum dot-standard items is respectively put into sepectrophotofluorometer, in phosphorescence pattern
It is lower record phosphorescence intensity value, and using phosphorescence intensity value decline percentage as ordinate, it is dense with the ferric ion of standard solution
It spends and draws linear regression curves for abscissa；
(3) solution to be measured is taken, the compound suspension of carbon quantum dot-product to be tested is prepared according to step (1) the method, according to step
Suddenly (2) the method measures phosphorescence intensity value decline percentage, substitutes into the regression curve, obtains the ferric iron of solution to be measured
Ion concentration.
The mass ratio of step (1) the of the present invention carbon quantum dot and cyanuric acid is 1:800~1200.In practical behaviour
When making, 0.05~0.2mg of carbon quantum dot is added in every milliliter of standard solution.
The concentration of the ferric ion standard solution of multiple and different concentration of the present invention is in the range of 0~1.5mM；It is excellent
The concentration for selecting the standard solution is respectively：0th, 0.1mM, 0.2mM, 0.3mM, 0.4mM, 0.5mM and 0.8mM.
Carbon quantum dot of the present invention preferably uses hydro-thermal method at 250~300 DEG C using citric acid and urea as raw material
Synthesis obtains.For the present invention by largely putting into practice discovery, the carbon quantum dot being prepared using the above method is dense to ferric ion
The detection of degree has higher sensitivity and accuracy.
Specifically, the carbon quantum dot is prepared with the following method：By citric acid and urea with mass ratio 5:1~
1:4 mix in water, and gained mixed solution is positioned in hydrothermal reaction kettle, and 8~16 hours are reacted at 250~300 DEG C,
To obtain the final product.In order to improve detection sensitivity and accuracy, the preparation method of the carbon quantum dot further includes：By products therefrom carry out from
Heart processing, removal precipitation, takes supernatant liquor, freeze-dried, obtains black carbon quantum dot powder.
In detection method of the present invention, the compound suspension of carbon quantum dot-standard items or carbon quantum dot-product to be tested are being prepared
During compound suspension, 5~30min is mixed in a manner of physical agitation after preferably adding in the carbon quantum dot in the solution, adds in three
30~100min is blended in a manner of physical agitation again after paracyanogen acid, obtains compound suspension.
The present invention be using phosphorescence intensity value decline percentage as ordinate, using the ferric ion concentration of standard solution as
Abscissa draws linear regression curves.Wherein, the phosphorescence declines percentage=(initial phosphor intensity value-terminal phosphorescence is strong
Angle value)/initial phosphor intensity value, the time of the terminal is to add in the time being uniformly mixed after cyanuric acid.In practical operation
In, 30~100min is blended in a manner of physical agitation again to add in after cyanuric acid, the time that the blending terminates.
During the drafting regression curve, linear segment therein should be chosen and be fitted and obtain fitting formula, be computed,
The present invention can reach 32uM to the detection limit of ferric ion.
Present invention finds between the phosphorescence intensity changing value of carbon quantum dot Complex Probes and the concentration of ferric ion
In good linear relationship, using the phosphorescence of carbon quantum dot to being detected with ferric ion concentration.Since phosphorescence has
Longer service life and larger Stokes shift, therefore the interference of background fluorescence and particle scattering light in solution can be eliminated, it can
To avoid the interference of autofluorescence and scattering light；And the phenomenon that phosphorescence relative to fluorescence is a kind of more rare, therefore detect
When selectivity be further enhanced.And the present invention can reach 32uM to the detection limit of ferric ion.In addition, carbon quantum
The phosphorescence of point is difficult to obtain, and the present invention carries out phosphorescence detection using simple, environmental-friendly carbon quantum is prepared, and provides a kind of letter
Single easy, cheap detection method.
Description of the drawings
Fig. 1 is influence of the different ions to phosphorescence intensity in embodiment 1.
Fig. 2 is phosphorescence intensity in embodiment 2 with the change curve of fluorescence emission wavelengths.
Fig. 3 is phosphorescence intensity decreasing ratio in embodiment 2 with the variation relation of iron concentration.
Fig. 4 is the transmission electron microscope picture of 3 gained carbon quantum dot of embodiment.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
Following embodiment cannot be used for limiting the scope of the invention for illustrating the present invention.In present embodiment
Involved raw material is commercially available, and without purification processes.
Embodiment 1
A kind of fluorescence quantum for being used to detect ferric ion concentration is present embodiments provided, is prepared by the following method
It forms：
(1) folic acid of 1g citric acids and the urea of 1g is dissolved in the deionized water of 25ml, obtains mixed solution；
(2) (1) obtained mixed solution is placed in the polytetrafluoroethylene (PTFE) autoclave of 50ml, it is anti-at 250 DEG C
It answers 10 hours, obtains carbon quantum initial soln；
(3) it is 9500rpm in rotating speed by (2) initial soln, centrifugation time is 20 minutes, removes black precipitate, takes upper strata
Brown color clear liquid freeze-dried 72 hours, obtains black carbon quantum dot powder.The carbon quantum dot is made into 100ug/ml's
Carbon quantum dot solution, it is spare.
The present embodiment is further provided detects Fe using above-mentioned carbon quantum dot powder3+The method of concentration, specially：
(1) it is separately added into carbon quantum dot solution described in lml into 7 quartzy fluorescence cuvettes；
(2) with liquid-transfering gun respectively by concentration 0, the Fe of 0.1mM, 0.2mM, 0.3mM, 0.4mM, 0.5mM and 0.8mM3+It instills
In the above-mentioned cuvette equipped with carbon quantum dot solution, mix 15 minutes, obtain mixed solution；
(3) mixed solution is separately added into 0.1g cyanuric acids, mixes 1h, then put it into fluorescence spectrophotometry
Phosphorescence is detected in meter.
It is respectively Na that if it, which is solion in step (2),+、Ca2+、Cu2+、K+、Al3+、Cu2+、Mg2+、Ag+And Z2 +When, concentration is 0.3mM, can obtain selective figure of the phosphorescence to different ions.Influence result of the different ions to phosphorescence intensity
As shown in Figure 1.
Embodiment 2
A kind of fluorescence quantum for being used to detect ferric ion concentration is present embodiments provided, is prepared by the following method
It forms：
(1) folic acid of 1g citric acids and the urea of 0.5g is dissolved in the deionized water of 25ml, obtains mixed solution；
(2) (1) obtained mixed solution is placed in the polytetrafluoroethylene (PTFE) autoclave of 50ml, it is anti-at 250 DEG C
It answers 10 hours, obtains carbon quantum initial soln；
(3) it is 9500rpm in rotating speed by (2) initial soln, centrifugation time is 20 minutes, removes black precipitate, takes upper strata
Brown color clear liquid freeze-dried 72 hours, obtains black carbon quantum dot powder.The carbon quantum dot is made into 100ug/ml's
Carbon quantum dot solution, it is spare.
The present embodiment is further provided detects Fe using above-mentioned carbon quantum dot powder3+The method of concentration, specially：
(1) it is separately added into carbon quantum dot solution described in lml into 7 quartzy fluorescence cuvettes；
(2) with liquid-transfering gun respectively by concentration 0, the Fe of 0.1mM, 0.2mM, 0.3mM, 0.4mM, 0.5mM and 0.8mM3+It instills
In the above-mentioned cuvette equipped with carbon quantum dot solution, mix 15 minutes, obtain mixed solution；
(3) mixed solution is separately added into 0.1g cyanuric acids, mixes 1h, then put it into fluorescence spectrophotometry
Phosphorescence is detected in meter, the compound suspension phosphorescence intensity of carbon quantum dot is drawn and declines change curve of the percentage with iron concentration,
Linear segment therein is chosen to be fitted and obtain fitting formula, and calculate the lowest detection limit, specially 32uM.
Phosphorescence intensity is as shown in Figure 2 with the change curve of fluorescence emission wavelengths in the present embodiment；Phosphorescence intensity decreasing ratio
It is as shown in Figure 3 with the variation relation and regression curve of iron concentration.
Embodiment 3
A kind of fluorescence quantum for being used to detect ferric ion concentration is present embodiments provided, is prepared by the following method
It forms：
(1) folic acid of 1g citric acids and the urea of 0.5g is dissolved in the deionized water of 25ml, obtains mixed solution；
(2) (1) obtained mixed solution is placed in the polytetrafluoroethylene (PTFE) autoclave of 50ml, it is anti-at 250 DEG C
It answers 16 hours, obtains carbon quantum initial soln；
(3) it is 9500rpm in rotating speed by (2) initial soln, centrifugation time is 20 minutes, removes black precipitate, takes upper strata
Brown color clear liquid freeze-dried 72 hours, obtains black carbon quantum dot powder.The transmission electricity of carbon quantum dot obtained by the present embodiment
Mirror figure is as shown in Figure 4.
The carbon quantum dot is made into the carbon quantum dot solution of 100ug/ml, it is spare.
The present embodiment is further provided detects Fe using above-mentioned carbon quantum dot powder3+The method of concentration, specially：
(1) it is separately added into carbon quantum dot solution described in lml into 7 quartzy fluorescence cuvettes；
(2) with liquid-transfering gun respectively by concentration 0, the Fe of 0.1mM, 0.2mM, 0.3mM, 0.4mM, 0.5mM and 0.8mM3+It instills
In the above-mentioned cuvette equipped with carbon quantum dot solution, mix 15 minutes, obtain mixed solution；
(3) mixed solution is separately added into 0.1g cyanuric acids, mixes 1h, then put it into fluorescence spectrophotometry
Phosphorescence is detected in meter.
Embodiment 4
This comparative example provides a kind of fluorescence quantum for being used to detect ferric ion concentration, prepares by the following method
It forms：
(1) urea of 1g citric acids and 0.5g is dissolved in the deionized water of 25ml, obtains mixed solution；
(2) (1) obtained mixed solution is placed in the polytetrafluoroethylene (PTFE) autoclave of 50ml, it is anti-at 180 DEG C
It answers 5 hours, obtains carbon quantum initial soln；
(3) it is 9500rpm in rotating speed by (2) initial soln, centrifugation time is 20 minutes, removes black precipitate, takes upper strata
Brown color clear liquid freeze-dried 72 hours, obtains black carbon quantum dot powder.
Using above-mentioned carbon quantum dot, Fe is detected using 2 the method for embodiment3+Concentration, the results showed that, utilize this kind of carbon amounts
Son point can not obtain phosphorescence and Fe3+Linear relationship, it is impossible to obtain regression curve.
Although above having used general explanation, specific embodiment and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (9)
- A kind of 1. method using carbon quantum dot phosphorescence detection ferric ion concentration, which is characterized in that include the following steps：(1) the ferric ion standard solution of multiple and different concentration is prepared, is separately added into carbon quantum dot and cyanuric acid, is mixed After uniformly, multiple compound suspensions of carbon quantum dot-standard items are obtained；(2) the compound suspension of carbon quantum dot-standard items is respectively put into sepectrophotofluorometer, remembered under phosphorescence pattern Record phosphorescence intensity value, and using phosphorescence intensity value decline percentage as ordinate, using the ferric ion concentration of standard solution as Abscissa draws linear regression curves；(3) solution to be measured is taken, the compound suspension of carbon quantum dot-product to be tested is prepared according to step (1) the method, according to step (2) the method measures phosphorescence intensity value and declines percentage, substitutes into the regression curve, obtain the ferric iron of solution to be measured from Sub- concentration.
- 2. according to the method described in claim 1, it is characterized in that, step (1) carbon quantum dot and the quality of cyanuric acid Than being 1:800~1200.
- 3. method according to claim 1 or 2, which is characterized in that carbon quantum dot 0.05 is added in every milliliter of standard solution ~0.2mg.
- 4. the method according to claim 1 or 3, which is characterized in that the ferric ion standard of the multiple various concentration The concentration of solution is in the range of 0~1.5mM；It is preferred that the concentration of the standard solution is respectively：0、0.1mM、0.2mM、 0.3mM, 0.4mM, 0.5mM and 0.8mM.
- 5. according to the method described in claim 1, it is characterized in that, the carbon quantum dot is to be adopted using citric acid and urea as raw material It is synthesized and obtained at 250~300 DEG C with hydro-thermal method.
- 6. according to the method described in claim 5, it is characterized in that, the carbon quantum dot is prepared with the following method：It will Citric acid and urea are with mass ratio 5:1~1:4 mix in water, gained mixed solution are positioned in hydrothermal reaction kettle, 250 At~300 DEG C react 8~16 hours to get.
- 7. according to the method described in claim 6, it is characterized in that, the preparation method of the carbon quantum dot further includes：By gained Product carries out centrifugal treating, and removal precipitation takes supernatant liquor, freeze-dried, obtains black carbon quantum dot powder.
- 8. according to the method described in claim 1~7 any one, which is characterized in that after the carbon quantum dot is added in solution 5~30min is mixed in a manner of physical agitation, adds in after cyanuric acid and 30~100min is blended with physical agitation again, is obtained compound outstanding Turbid.
- 9. the method according to claim 1 or 8, which is characterized in that the phosphorescence declines percentage=(initial phosphor intensity Value-terminal phosphorescence intensity value)/initial phosphor intensity value, time of the terminal be add in after cyanuric acid be uniformly mixed when Between.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2702418C1 (en) * | 2018-12-20 | 2019-10-08 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский национальный исследовательский университет информационных технологий, механики и оптики" (Университет ИТМО) | Luminescent sensor for concentration of heavy metal ions in water and method of using it |
| CN110713829A (en) * | 2019-10-26 | 2020-01-21 | 北京工业大学 | Preparation of orange carbon dots and p-Fe thereof3+Detection of (2) |
| CN110715915A (en) * | 2019-11-06 | 2020-01-21 | 东北师范大学 | Method for detecting ferric ions based on carbon quantum dots prepared from egg white |
| CN111334285A (en) * | 2020-04-08 | 2020-06-26 | 中国科学院长春光学精密机械与物理研究所 | Carbon nanodot composite material with cyanuric acid doped in carbon nanodots, preparation method and application |
| CN113376129A (en) * | 2021-03-26 | 2021-09-10 | 中科院苏州医工所郑州工程技术研究院 | Preparation method and application of carbon dot-based nano composite for detecting iron ions |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2702418C1 (en) * | 2018-12-20 | 2019-10-08 | федеральное государственное автономное образовательное учреждение высшего образования "Санкт-Петербургский национальный исследовательский университет информационных технологий, механики и оптики" (Университет ИТМО) | Luminescent sensor for concentration of heavy metal ions in water and method of using it |
| CN110713829A (en) * | 2019-10-26 | 2020-01-21 | 北京工业大学 | Preparation of orange carbon dots and p-Fe thereof3+Detection of (2) |
| CN110715915A (en) * | 2019-11-06 | 2020-01-21 | 东北师范大学 | Method for detecting ferric ions based on carbon quantum dots prepared from egg white |
| CN111334285A (en) * | 2020-04-08 | 2020-06-26 | 中国科学院长春光学精密机械与物理研究所 | Carbon nanodot composite material with cyanuric acid doped in carbon nanodots, preparation method and application |
| CN111334285B (en) * | 2020-04-08 | 2022-08-09 | 中国科学院长春光学精密机械与物理研究所 | Carbon nanodot composite material with cyanuric acid doped in carbon nanodots, preparation method and application |
| CN113376129A (en) * | 2021-03-26 | 2021-09-10 | 中科院苏州医工所郑州工程技术研究院 | Preparation method and application of carbon dot-based nano composite for detecting iron ions |
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Application publication date: 20180629 |