CN106323931A - Method for quickly synthesizing carbon dots in microwave manner by using yeast bacteria as a main carbon source and using carbon dots to detect pH of solution - Google Patents
Method for quickly synthesizing carbon dots in microwave manner by using yeast bacteria as a main carbon source and using carbon dots to detect pH of solution Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical application, and particularly relates to a method for quickly synthesizing a carbon dot solution in a microwave manner by using yeast bacteria as a main carbon source and using the carbon dot solution to detect pH of a solution. The method for detecting the pH value of the solution comprises the following step: synthesizing the carbon dot solution by using the yeast bacteria as the main carbon source, using ethylenediamine as an auxiliary carbon source and using water as dispersion liquid under the condition of microwave heating to obtain the carbon dot solution with a fluorescence characteristic. Synthesized carbon dots have the fluorescence characteristic, the maximum excitation wavelength is 390 nm, and the maximum transmitting wavelength is 460 nm; and after the carbon dot solution react with solutions with different pH, the fluorescence intensity value of the carbon dot solution and pH of the solutions are in linear relation as follows: F= 354.66-19.00 pH, and the linear range of detection is 1.83-11.86.
Description
Technical field
The invention belongs to Chemical activator technical field, be specifically related to one with yeast antibacterial for main carbon source ethylenediamine for auxiliary
Carbon source, synthesizes carbon point solution under microwave heating condition;Utilize carbon point solution and the fluorescent value of solution after the solution reaction of different pH
Difference, can detect the pH of solution.
Background technology
Fluorescent carbon point is one of carbon nanomaterial the most popular after fullerene, CNT and Graphene.This kind is received
Rice material overcomes some shortcoming of tradition quantum dot, not only has excellent optical property and small size property, and has
Good biocompatibility, it is easy to accomplish surface-functionalized, biochemical sensitive, imaging analysis, environment measuring, photocatalysis technology,
The field such as metal ion detection and pharmaceutical carrier has good application potential.Synthetic method includes electrochemical process, and hydro-thermal method is micro-
Ripple method, ultrasonic method etc..At present, it is achieved being uniformly synthesized carbon point still has certain difficulty.It is contemplated that utilize the most uniform
Yeast antibacterial is carbon source, to synthesize uniformity more preferable carbon point.
People utilize electrochemical process pH value determination in early days, but owing to the impedance of traditional glass electrode is high, cracky and not
Preferably it is used for the mensuration of pH in fluorine-containing solution, and has " sodium error " in high alkalinity environment, make electrochemistry run in pH value is measured
A lot of problems.Therefore, people continually develop new pH measuring method in recent years.The present invention is that fluorescence is visited based on newly synthesized carbon point
Pin, the method establishing detection pH value of solution.The features such as this method has simple to operate, detection range width.
Summary of the invention
The main object of the present invention is the synthesis for existing carbon point and the detection technique of pH value of solution and method is shown
Some defects come, propose one and utilize volume uniform yeast antibacterial to be main carbon source, in conjunction with the preparation of microwave method synthetic technology all
Carbon point that even property is good the detection for pH value of solution.The method has the features such as simple to operate, pH detection range width.
For realizing the object of the invention, the technical solution used in the present invention is:
A kind of with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point the method for the detection for pH value of solution, its step is such as
Under:
(1) with yeast antibacterial as main carbon source, ethylenediamine is auxiliary carbon source, the yeast separated first is scattered in ethylenediamine molten
Liquid obtains mixed solution, then by mixed solution microwave heating treatment, after reaction, is the carbon thick solution of point with water dissolution, through from
The heart, filtration etc. obtain final carbon point solution after processing;
(2) determine carbon point solution fluorescence intensity level (I F ) and the pH value of solution between quantitative relationship;
(3) according to the relation between pH value and the fluorescent value of carbon point solution of solution, the pH value of solution to be measured can be detected.
In step (2) carbon point solution fluorescence intensity level (I F ) and the pH value of solution between quantitative relationship be:I F =
354.66-19.00 pH (correlation coefficientr=0.9964)。
The concentration of described ethylenediamine is 3.0 mol/L.
Described in step (1), it is middle high fire by the firepower of mixed solution microwave heating treatment.
Described in step (1), it is 25 min by the mixed solution microwave heating treatment time.
Described in step (1), first the carbon the obtained thick solution of point is respectively placed in centrifuge tube and carries out high speed centrifugation separation, then
The supernatant obtained is carried out filtration under diminished pressure process, finally obtains the carbon point solution that brown color is transparent.
Described in step (1), the centrifugal speed to the centrifugal treating of the carbon thick solution of point is 10000 revs/min, time centrifugal
Between be 15 minutes.
Described detected pH value of solution is in the range of 1.83-11.86.
The carbon point mean diameter of described synthesis is 3.8 nm.
The carbon point of described synthesis has fluorescent characteristic, and maximum excitation wavelength is 390 nm, and maximum emission wavelength is 460
nm。
Accompanying drawing explanation
Fig. 1 is the fluorescence spectrum figure of carbon point solution prepared by the embodiment of the present invention.
Fig. 2 is the TEM figure of carbon point solution prepared by the embodiment of the present invention.
Fig. 3 be carbon point solution prepared by the embodiment of the present invention TEM in grain size distribution.
Fig. 4 is that (1-11 is molten for the fluorescence intensity change figure of the carbon point solution different pH solution of detection prepared by the embodiment of the present invention
The pH of liquid is respectively 1.83,2.91,3.71,4.70,5.72,6.80,7.87,8.81,9.84,10.81,11.86).
Specific embodiment:
Following example are intended to further illustrate the present invention rather than limitation of the invention further.
(1) cultivation of yeast antibacterial and extraction
The composition of culture medium: glucose 20.0 g, distilled water 1000 mL.
Accurately weigh the glucose of 20.0 g, be added in the beaker containing 900 mL distilled water, be allowed to Glass rod stirring
Fully dissolve, be settled to 1000 mL.Measure 20 mL glucose solutions in triangular flask, add tampon, wrap up with kraft paper.To treat
The glucose solution of sterilizing puts into autoclave, in 121 ° of C sterilizing 20 min.Sterilized glucose solution is placed in aseptic work
In station, open ultraviolet lamp sterilization 2 h.In strict accordance with sterility requirements, by Angel high activity dried yeast (the Angel ferment of 0.020 g
Female limited company) it is inoculated in glucose solution, last 37 ° of C cultivate 24 h.
Take the yeast of one bottle of above-mentioned cultivation, be sub-packed in the centrifuge tube of 45 mL, with the speed of 10000 revs/min from
The heart 10 minutes;Taking precipitation after centrifugal end, now yeast is deposited in bottom centrifuge tube in solid form;By each centrifuge tube
In yeast ethylenediamine solution with 1.0 mL, 3.0 mol/L respectively mix.
(2) preparation of carbon point
Take 12 above-mentioned centrifuge tubes, solution therein transferred in the conical flask of 250 mL, then toward conical flask add 8 mL,
The ethylenediamine solution of 3.0 mol/L, is 20 mL to final volume.Conical flask being transferred in microwave oven, middle high fire, microwave adds
Heat 25 min.Reaction takes out conical flask after terminating, and with 10 mL water dissolutioies, gained solution is the carbon thick solution of point.By the carbon thick solution of point
First with 10000 revs/min, centrifugal 15 minutes, take supernatant, then be filtrated to get carbon with the filter membrane vacuum decompression of aperture 0.2 μm
Point solution.As it is shown in figure 1, maximum excitation wavelength is 390 nm, maximum emission wavelength is 460 nm.And the pattern etc. of carbon point is entered
Go TEM sign, as in figure 2 it is shown, the carbon point good dispersion of synthesis, and the most uniform.Particle diameter distribution results (such as Fig. 3) shows carbon
Point size 3.82 nm is in left and right.
(3) the preparation condition optimization of carbon point
Inquire into the impact on synthesis carbon point of the concentration of ethylenediamine, volume, microwave heating time and firepower, mainly to synthesis
The fluorescence intensity impact of carbon point solution is investigated.
The fluorescence intensity of carbon point solution is had an impact by the concentration of ethylenediamine, and the concentration having inquired into ethylenediamine is respectively 1.0
Fluorescence intensity to the carbon point solution of synthesis when mol/L, 3.0 mol/L, 5.0 mol/L, 8.0 mol/L, 10.0 mol/L
Impact.When the concentration of ethylenediamine is 3.0 mol/L, 5.0 mol/L, the fluorescence of carbon point solution is relatively strong, and when ethylenediamine concentration is
During 3.0 mol/L, the fluorescence of carbon point solution is the strongest, and final preferred concentration is 3.0 mol/L.
The fluorescence intensity of carbon point solution is had an impact by the volume of ethylenediamine, inquired into the volume of ethylenediamine be respectively 10 mL,
15 mL, 20 mL, 25 mL, 30 mL, the 35 mL impact on the fluorescence intensity of the carbon point solution of synthesis.Volume when ethylenediamine
When being 20 mL, 25 mL, the fluorescence of carbon point solution is relatively strong, and when the volume of ethylenediamine is 20 mL, and the fluorescence of carbon point solution is
By force, final preferred volume is 20 mL.
The fluorescence intensity of carbon point solution is had an impact by the quantity of antibacterial.The amount of antibacterial is represented with the volume of inoculum
Impact on the fluorescence intensity of carbon point solution.Probed into the volume of culture fluid be respectively 20 mL, 40 mL, 60 mL, 80 mL,
100 mL impact on the fluorescence intensity of the carbon point solution of synthesis.When the volume of culture fluid is 60 mL, 80 mL, carbon point solution
Fluorescence relatively strong, and when the volume of culture fluid is 60 mL, the fluorescence of carbon point solution is the strongest, the volume of final preferably culture fluid
It is 60 mL.
The fluorescence intensity of carbon point solution is had an impact by microwave firepower.Probed into microwave firepower be respectively in low fire, moderate heat, in
Impact on the fluorescence intensity of synthesis carbon point solution when Gao Huo, high fire.When microwave firepower is moderate heat, middle high fire, carbon point solution
Fluorescence relatively strong, and when microwave firepower is middle high fire, the fluorescence of carbon point solution is the strongest, and final preferably microwave firepower is middle height
Fire.
The fluorescence intensity of carbon point solution is had an impact by microwave heating time.Probe into microwave heating time and be respectively 10
The impact of fluorescence intensity on synthesis carbon point solution when min, 15min, 20 min, 25 min, 30 min.Work as microwave heating time
When being 20 min, 25 min, the fluorescence of carbon point solution is relatively strong, and when microwave heating time is 25min, the fluorescence of carbon point solution
The strongest, the final preferably microwave time is 25 min.
(4) the carbon point detection parameter to pH value of solution
Take the centrifuge tube of 11 2.0 mL, put on respectively A, B, C, D, E, F, G, H, I, J, No. K, to A-K prop up in centrifuge tube add
1.6 mL diluted the carbon point solution of 50 times in advance, then were sequentially added into the Britton-of 400 L differences pH in A-K centrifuge tube
Robinson buffer solution, pH value is respectively 1.83,2.91,3.71,4.70,5.72,6.80,7.87,8.81,9.84,
10.81、11.86.After question response 30 min, the solution in each centrifuge tube is tested successively in spectrofluorophotometer, note
Record carbon point fluorescence spectrum value in the presence of different BR buffer solution, result is shown in Fig. 4, fluorescence intensity level (I F ) and the pH value of solution
Between quantitative relationship be:I F =354.66-19.00 pH (r=0.9964)。
Also, it should be noted the specific embodiment of the present invention is used only to exemplary illustration, and limit never in any form
Determining protection scope of the present invention, the person skilled of this area can be improved according to more above-mentioned explanations or be changed, but
All these improvements and changes all should belong to the protection domain of the claims in the present invention.
Claims (10)
1., with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point a method for the detection for pH value of solution, its feature exists
In following steps:
(1) with yeast antibacterial as main carbon source, ethylenediamine is auxiliary carbon source, the yeast separated first is scattered in ethylenediamine molten
Liquid obtains mixed solution, then by mixed solution microwave heating treatment, after reaction, is the carbon thick solution of point with water dissolution, through from
The heart, filtration etc. obtain final carbon point solution after processing;
(2) determine carbon point solution fluorescence intensity level (I F ) and the pH value of solution between quantitative relationship;
(3) according to the relation between pH value and the fluorescent value of carbon point solution of solution, the pH value of solution to be measured can be detected.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: in step (2) carbon point solution fluorescence intensity level (I F ) and the pH value of solution between quantitative relationship
For:I F =354.66-19.00 pH (r=0.9964)。
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: the concentration of ethylenediamine is 3.0 mol/L.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: the described firepower by mixed solution microwave heating treatment of step (1) is middle high fire.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: step (1) is described is 25 min by the mixed solution microwave heating treatment time.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: in step (1), first the carbon the obtained thick solution of point is respectively placed in centrifuge tube and carries out high speed centrifugation
Separate, then the supernatant obtained is carried out filtration under diminished pressure process, finally obtain the carbon point solution that brown color is transparent.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: in step (1), the centrifugal speed to the centrifugal treating of the carbon thick solution of point is 10000 revs/min, from
The heart time is 15 minutes.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: pH value of solution can be detected in the range of 1.83-11.86.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the detection of pH value of solution
Method, it is characterised in that: the carbon point mean diameter of synthesis is 3.8 nm.
The most according to claim 1 with yeast antibacterial for main carbon source microwave Fast back-projection algorithm carbon point and for the inspection of pH value of solution
The method surveyed, it is characterised in that: the carbon point of synthesis has fluorescent characteristic, and maximum excitation wavelength is 390 nm, maximum emission wavelength
It is 460 nm.
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CN108083257A (en) * | 2017-12-28 | 2018-05-29 | 湖南科技大学 | A kind of method that fluorescent carbon point is prepared using chloroplaset as carbon source |
CN108195816A (en) * | 2018-02-05 | 2018-06-22 | 湖南科技大学 | The method that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots |
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