CN106248769A - The method of hydroquinone concentration in detection solution - Google Patents
The method of hydroquinone concentration in detection solution Download PDFInfo
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- CN106248769A CN106248769A CN201610837518.XA CN201610837518A CN106248769A CN 106248769 A CN106248769 A CN 106248769A CN 201610837518 A CN201610837518 A CN 201610837518A CN 106248769 A CN106248769 A CN 106248769A
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Abstract
The invention discloses and a kind of detect the method for hydroquinone concentration in solution, three-electrode system is used by cyclic voltammetry, the hydroquinone in solution to be measured to be detected, linear equation according to hydroquinone obtains the concentration of hydroquinone in solution to be measured, working electrode in three-electrode system processes through amination modified by graphene quantum dot, and described working electrode is glass-carbon electrode.The present invention have simple to operate, detect quick, highly sensitive, the highly sensitive identification of hydroquinone in biased sample solution can be carried out.
Description
Technical field
The present invention relates to hydroquinone detection technique field.It is more particularly related to one is based on amino fossil
The electrochemical sensing that ink alkene quantum dot is modified utilizes the method for hydroquinone concentration in cyclic voltammetry detection solution.
Background technology
Hydroquinone is a kind of very important phenolic compound, is widely used in photograph aobvious in daily production and life
Shadow agent, synthetic dyestuffs, polymerization inhibitor, inhibitor, rubber antioxidant and food antioxidant etc., have bigger toxicity, to skin to human body
Skin, eyes, mucosa have stimulation, and are difficult under field conditions (factors) degrade, and human body and environment are had bigger harm, by many
Individual national environmental protection tissue is classified as environmental contaminants.Therefore, it is carried out quick, accurate, trace analysis detection and have particularly significant
Meaning.At present, the method measuring hydroquinone mainly has spectrophotography, high performance liquid chromatography, thin layer chromatography, micelle
Electrokinetic chromatography and high performance capillary electrophoresis etc., although these technology Application comparison are extensive, but the expensive equipment used, reagent consumption
Amount is big and analysis time is longer, it is impossible to meet the demand of field quick detection.Hydroquinone has electro-chemical activity, easily by oxygen
Change, therefore can electrochemically detect.Most of electricity analytical methods have save time, low cost, selectivity are good, sensitivity
The advantages such as height, response is fast, instrument is simple.
Graphene quantum dot, as a kind of novel quantum dot, in addition to having the performance that Graphene is excellent, also because of it
Significantly quantum confined effect and dimensional effect, shown the feature of some novelties.The most excellent fluorescence property, good
The special physicochemical properties such as biocompatibility, low cytotoxicity, chemical inertness, all these advantageous properties make Graphene
Quantum dot is expected in bio-imaging, medicament transport, metal ion or bioprobe, photoelectric device, energy storage device and photocatalysis etc.
Field is with a wide range of applications.
Summary of the invention
It is an object of the invention to solve at least the above, and the advantage that at least will be described later is provided.
It is a still further object of the present invention to provide a kind of amination modified by graphene quantum dot electrode detection hydroquinone
Method, have simple to operate, detect quick, highly sensitive, the highly sensitive identification of hydroquinone in biased sample solution can be carried out.
In order to realize according to object of the present invention and further advantage, it is provided that in a kind of detection solution, hydroquinone is dense
The method of degree, uses three-electrode system to be detected the hydroquinone in solution to be measured by cyclic voltammetry, according to benzene
The linear equation of diphenol obtains the concentration of hydroquinone in solution to be measured, and the working electrode in three-electrode system is through amination graphite
Alkene quantum dot moditied processing, described working electrode is glass-carbon electrode.
Preferably, the method for hydroquinone concentration in described detection solution, at amination modified by graphene quantum dot
Reason concrete operations are as follows: immerse working electrode containing in 2mg/mL amination graphene quantum dot solution, utilize cyclic voltammetric
Take out after method scanning, be placed in infrared drying oven drying,
Wherein, sweep parameter is: initial potential 0V, maximum potential 1V, minimum point position 0V, final current potential 0V, sweep speed
0.1V/s, scanning times 100 times, sensitivity 10-4A/V, waiting time are 2s.
Preferably, the method for hydroquinone concentration in described detection solution, further comprising the steps of:
Step one, the preparation standard solution containing variable concentrations hydroquinone, with PBS buffer solution as solvent, wherein PBS
The pH of buffer solution is 7.4, and concentration is 0.1mol/L, and the concentration of hydroquinone is followed successively by 1.0 × 10-5mol/L、5×10- 5mol/L、1×10-4mol/L、2×10-4mol/L；
Step 2, using reference electrode, auxiliary electrode and the working electrode after modifying to build three-electrode system, utilization follows
Every part of standard solution of preparation in step one is detected by ring voltammetry, obtains the cyclic voltammetry curve of every part of standard solution,
And record the peak value of current intensity in the cyclic voltammetry curve of every part of standard solution respectively；
Step 3, the peak value of current intensity corresponding to cyclic voltammetry curve of every part of standard solution to obtain in step 2
With the difference of the peak value of the current intensity that hydroquinone concentration is standard solution during 0 μm ol/L as vertical coordinate, with every part of mark
The concentration of quasi-solution is that abscissa is drawn standard curve and calculates linear equation；
Step 4, utilize cyclic voltammetry that the solution to be measured containing unknown concentration hydroquinone is detected, treated
Survey the cyclic voltammetry curve of solution, by dense with hydroquinone for the peak value of current intensity corresponding for the cyclic voltammetry curve of solution to be measured
The difference that degree is the peak value of the current intensity of the standard solution of 0mol/L substitutes in the linear equation obtained in step 3, calculates
The concentration of hydroquinone in solution to be measured.
Preferably, the method for hydroquinone concentration in described detection solution, reference electrode is Ag/AgCl electrode, auxiliary
Helping electrode is platinum electrode.
Preferably, in described detection solution, the method for hydroquinone concentration, utilizes cyclic voltammetric in described step 2
The condition of scanning of method detection is: initial potential-0.4V, termination current potential 0.8V, sweep speed 0.05V/s, current potential amplification 0.001V,
Waiting time 2s, sensitivity 10-4A/V。
Preferably, the method for hydroquinone concentration in described detection solution, working electrode is through amination Graphene amount
Pretreatment is first passed through: by granularity be 1.0 μm, 0.3 μm and 0.05 μ successively by working electrode on polishing cloth before son point moditied processing
The polishing powder polishing of m, then cleans with ultra-pure water.
Preferably, the method for hydroquinone concentration in described detection solution, after working electrode is preprocessed, amino
Following process is first passed through before functionalized graphene quantum dot moditied processing:
First with magnetic water preparation containing 10mM zirconium oxychloride and the electrolyte of 0.3M potassium chloride, by pretreated work electricity
One layer of nano oxidized zirconium layer of electro-deposition in electrolyte is immersed in pole；
Metal and stone will be planted again and propolis grinds respectively will be crossed 200 mesh sieves and must be planted metal and stone powder and propolis powder, metal and stone powder will be planted with remote
Infrared nanometer powder, propolis powder, magnetic water are 3:1:1:1000 mixing according to mass ratio, obtain dispersion liquid through ultrasonic disperse, take 10 μ L
Dispersant liquid drop is coated in electro-deposition to be had on the working electrode of nano oxidized zirconium layer, dries.
The present invention at least includes following beneficial effect:
1) the amination modified by graphene quantum dot electrodic electron transfer rate that the present invention provides is fast, good stability, preparation
Simply, easy to operate, detection process is simple and convenient, highly sensitive, detection limit is low, can realize the fast of hydroquinone in testing sample
Speed detection；
2) nano zirconium dioxide has good thermo-chemical stability, pyroconductivity, nano oxidized zirconium layer Adsorption
Point is many, and conductive capability is strong, can amplify the signal of telecommunication, can strengthen the conductivity of amination graphene quantum dot layer during detecting；Plant
The dispersion liquid that metal and stone powder, propolis powder, far infrared nano powder prepare, can increase the specific surface area of working electrode, not only can be enriched with
Hydroquinone and accelerate electron transport rate, improve hydroquinone detection sensitivity；
The method of the present invention is simple, and condition is easy to control, has good sensitivity, convenience, and working electrode is easy to produce,
And in the detection of hydroquinone, have a good application prospect, there is fast response time, that highly sensitive, method is easy etc. is excellent
Point.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will be by this
Invention research and practice and be understood by the person skilled in the art.
Accompanying drawing explanation
Fig. 1 is the cyclic voltammetry curve figure of the hydroquinone standard solution of variable concentrations in embodiments of the invention 1；
Fig. 2 is the canonical plotting of hydroquinone in embodiments of the invention 1.
Detailed description of the invention
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to description literary composition
Word can be implemented according to this.
It should be noted that experimental technique described in following embodiment, if no special instructions, it is conventional method, institute
State reagent and material, if no special instructions, the most commercially obtain.
Embodiment 1:
A kind of detect the method for hydroquinone concentration in solution, use three-electrode system by cyclic voltammetry to be measured molten
Hydroquinone in liquid detects, and obtains the concentration of hydroquinone in solution to be measured according to the linear equation of hydroquinone, and three
Working electrode in electrode system processes through amination modified by graphene quantum dot, and described working electrode is glass-carbon electrode.
Wherein, the method for hydroquinone concentration in described detection solution, amination modified by graphene quantum dot processes tool
Gymnastics is made as follows: immerses working electrode containing in 2mg/mL amination graphene quantum dot solution, utilizes cyclic voltammetry to sweep
Taking out after retouching, be placed in infrared drying oven drying, wherein, sweep parameter is: initial potential 0V, maximum potential 1V, minimum point
Position 0V, final current potential 0V, sweep speed 0.1V/s, scanning times 100 times, sensitivity 10-4A/V, waiting time are 2s.Here
Cyclic voltammetry scanning is to be electrodeposited on working electrode by amination graphene quantum dot.
Wherein, the method for hydroquinone concentration in described detection solution, further comprising the steps of:
Step one, the preparation standard solution containing variable concentrations hydroquinone, with PBS buffer solution as solvent, wherein PBS
The pH of buffer solution is 7.4, and concentration is 0.1mol/L, and the concentration of hydroquinone is followed successively by 1.0 × 10-5mol/L、5×10- 5mol/L、1×10-4mol/L、2×10-4mol/L；
Step 2, using reference electrode, auxiliary electrode and the working electrode after modifying to build three-electrode system, utilization follows
Every part of standard solution of preparation in step one is detected by ring voltammetry, obtains the cyclic voltammetry curve of every part of standard solution,
And record the peak value of current intensity in the cyclic voltammetry curve of every part of standard solution respectively；
Step 3, the peak value of current intensity corresponding to cyclic voltammetry curve of every part of standard solution to obtain in step 2
With the difference of the peak value of the current intensity that hydroquinone concentration is standard solution during 0 μm ol/L as vertical coordinate, with every part of mark
The concentration of quasi-solution is that abscissa is drawn standard curve and calculates linear equation；
Step 4, utilize cyclic voltammetry that the solution to be measured containing unknown concentration hydroquinone is detected, treated
Survey the cyclic voltammetry curve of solution, by dense with hydroquinone for the peak value of current intensity corresponding for the cyclic voltammetry curve of solution to be measured
The difference that degree is the peak value of the current intensity of the standard solution of 0mol/L substitutes in the linear equation obtained in step 3, calculates
The concentration of hydroquinone in solution to be measured.
Wherein, the method for hydroquinone concentration in described detection solution, reference electrode is Ag/AgCl electrode, auxiliary electricity
Extremely platinum electrode.
Wherein, in described detection solution, the method for hydroquinone concentration, utilizes cyclic voltammetry to examine in described step 2
The condition of scanning surveyed is: initial potential-0.4V, terminates current potential 0.8V, sweep speed 0.05V/s, current potential amplification 0.001V, waits
Time 2s, sensitivity 10-4A/V。
Wherein, the method for hydroquinone concentration in described detection solution, working electrode is through amination graphene quantum dot
Pretreatment is first passed through: by granularity be 1.0 μm, 0.3 μm and 0.05 μm successively by working electrode on polishing cloth before moditied processing
Polishing powder is polished, and then cleans with ultra-pure water.
The cyclic voltammetric that method according to embodiment 1 obtains the hydroquinone standard solution of the variable concentrations shown in Fig. 1 is bent
Line chart, wherein the concentration of hydroquinone is according to carrying out through above-mentioned cyclic voltammetry for 0mol/L standard solution (i.e. PBS buffer solution)
Mensuration obtains cyclic voltammetry curve a, and the concentration of hydroquinone is followed successively by 1.0 × 10-5mol/L、5×10-5mol/L、1×10- 4mol/L、2×10-4Mol/L is measured obtaining cyclic voltammetry curve b, c, d, e successively through above-mentioned cyclic voltammetry, can learn
The current intensity that solution to be measured is corresponding strengthens with the increase of the concentration of hydroquinone, and Fig. 2 is that the method according to step 3 obtains
The canonical plotting of hydroquinone, Y-axis is the difference of current intensity peak value, and unit is μ A, and X-axis is the titer of hydroquinone
Concentration, unit is μM, and current intensity and hydroquinone concentration have good linear relationship, R2=0.9836.
Embodiment 2:
On the basis of embodiment 1, the method for hydroquinone concentration in described detection solution, working electrode is preprocessed
Afterwards, following process is first passed through before the process of amination modified by graphene quantum dot:
First with magnetic water preparation containing 10mM zirconium oxychloride and the electrolyte of 0.3M potassium chloride, by pretreated work electricity
One layer of nano oxidized zirconium layer of electro-deposition in electrolyte is immersed in pole；Electro-deposition mentioned here i.e. with cyclic voltammetry at-1.1V～
Clean with ultra-pure water after depositing 8-10 circle under+0.7V；
Metal and stone will be planted again and propolis grinds respectively will be crossed 200 mesh sieves and must be planted metal and stone powder and propolis powder, metal and stone powder will be planted with remote
Infrared nanometer powder, propolis powder, magnetic water are 3:1:1:1000 mixing according to mass ratio, obtain dispersion liquid through ultrasonic disperse, take 10 μ L
Dispersant liquid drop is coated in electro-deposition to be had on the working electrode of nano oxidized zirconium layer, dries.
The method of the present embodiment 2 records current intensity has more preferably linear relationship, R with hydroquinone concentration2=0.9983.
Although embodiment of the present invention are disclosed as above, but it is not restricted in description and embodiment listed
Using, it can be applied to various applicable the field of the invention completely, for those skilled in the art, and can be easily
Realizing other amendment, therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details with shown here as the legend with description.
Claims (7)
1. detect a method for hydroquinone concentration in solution, use three-electrode system by cyclic voltammetry to solution to be measured
In hydroquinone detect, obtain the concentration of hydroquinone in solution to be measured according to the linear equation of hydroquinone, it is special
Levying and be, the working electrode in three-electrode system processes through amination modified by graphene quantum dot, and described working electrode is glass carbon
Electrode.
2. the method for hydroquinone concentration in detection solution as claimed in claim 1, it is characterised in that amination Graphene amount
Son point moditied processing concrete operations are as follows: immersed by working electrode containing in 2mg/mL amination graphene quantum dot solution, sharp
Take out after scanning by cyclic voltammetry, be placed in infrared drying oven drying,
Wherein, sweep parameter is: initial potential 0V, maximum potential 1V, minimum point position 0V, final current potential 0V, sweep speed 0.1V/
S, scanning times 100 times, sensitivity 10-4A/V, waiting time are 2s.
3. the method for hydroquinone concentration in detection solution as claimed in claim 2, it is characterised in that also include following step
Rapid:
Step one, the preparation standard solution containing variable concentrations hydroquinone, with PBS buffer solution as solvent, wherein PBS buffering
The pH of solution is 7.4, and concentration is 0.1mol/L, and the concentration of hydroquinone is followed successively by 1.0 × 10-5mol/L、5×10-5mol/L、1
×10-4mol/L、2×10-4mol/L；
Step 2, use reference electrode, auxiliary electrode and the working electrode after modifying to build three-electrode system, utilize circulation volt
Every part of standard solution of preparation in step one is detected by peace method, obtains the cyclic voltammetry curve of every part of standard solution, and divides
Do not record the peak value of current intensity in the cyclic voltammetry curve of every part of standard solution；
Step 3, every part of standard solution to obtain in step 2 the peak value of current intensity corresponding to cyclic voltammetry curve with right
Benzodiazepines concentration be the difference of the peak value of the current intensity of standard solution during 0 μm ol/L as vertical coordinate, molten with every part of standard
The concentration of liquid is that abscissa is drawn standard curve and calculates linear equation；
Step 4, utilize cyclic voltammetry that the solution to be measured containing unknown concentration hydroquinone is detected, obtain to be measured molten
The cyclic voltammetry curve of liquid, by the peak value of current intensity corresponding for the cyclic voltammetry curve of solution to be measured with hydroquinone concentration be
The difference of the peak value of the current intensity of the standard solution of 0mol/L substitutes in the linear equation obtained in step 3, is calculated and treats
Survey the concentration of hydroquinone in solution.
4. the method for hydroquinone concentration in detection solution as claimed in claim 1, it is characterised in that reference electrode is Ag/
AgCl electrode, auxiliary electrode is platinum electrode.
5. the method for hydroquinone concentration in detection solution as claimed in claim 3, it is characterised in that profit in described step 2
By the condition of scanning of cyclic voltammetry detection it is: initial potential-0.4V, terminates current potential 0.8V, sweep speed 0.05V/s, current potential
Amplification 0.001V, waiting time 2s, sensitivity 10-4A/V。
6. the method for hydroquinone concentration in detection solution as claimed in claim 2, it is characterised in that working electrode is through amino
First pass through pretreatment before functionalized graphene quantum dot moditied processing: by working electrode on polishing cloth successively with granularity be 1.0 μm,
The polishing powder polishing of 0.3 μm and 0.05 μm, then cleans with ultra-pure water.
7. the method for hydroquinone concentration in detection solution as claimed in claim 6, it is characterised in that working electrode is through pre-place
After reason, amination modified by graphene quantum dot first pass through following process before processing:
First with magnetic water preparation containing 10mM zirconium oxychloride and the electrolyte of 0.3M potassium chloride, pretreated working electrode is soaked
Enter one layer of nano oxidized zirconium layer of electro-deposition in electrolyte；
Metal and stone will be planted again and propolis grinds respectively will be crossed 200 mesh sieves and must be planted metal and stone powder and propolis powder, metal and stone powder and far infrared will be planted
Nano powder, propolis powder, magnetic water are 3:1:1:1000 mixing according to mass ratio, obtain dispersion liquid through ultrasonic disperse, take 10 μ L dispersions
Drop-coated has on the working electrode of nano oxidized zirconium layer in electro-deposition, dries.
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