CN106290543B - The method for detecting resorcinol concentration in solution - Google Patents
The method for detecting resorcinol concentration in solution Download PDFInfo
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- CN106290543B CN106290543B CN201610838856.5A CN201610838856A CN106290543B CN 106290543 B CN106290543 B CN 106290543B CN 201610838856 A CN201610838856 A CN 201610838856A CN 106290543 B CN106290543 B CN 106290543B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention discloses a kind of methods of resorcinol concentration in detection solution, the resorcinol in solution to be measured is detected by cyclic voltammetry using three-electrode system, the concentration of resorcinol in solution to be measured is obtained according to the linear equation of resorcinol, for working electrode in three-electrode system through amination graphene quantum dot moditied processing, the working electrode is glass-carbon electrode.The present invention have it is easy to operate, detection quickly, high sensitivity, the highly sensitive identification of resorcinol in mixing sample solution can be carried out.
Description
Technical field
The present invention relates to resorcinol detection technique fields.It is more particularly related to which a kind of being based on amino fossil
The method that the electrochemical sensing of black alkene quantum dot modification detects resorcinol concentration in solution using cyclic voltammetry.
Background technology
Resorcinol is a kind of important industrial chemicals, mainly as organic intermediate, for medicine, food, dyestuff, modeling
The industry such as material, rubber.Resorcinol is also a kind of environmental contaminants simultaneously, has moderate toxicity, can stimulate skin, mucous membrane, can
It is absorbed rapidly by skin, generates ferrihemoglobin and cause cyanosis, lethargic sleep and fatal kidney injury, and in natural conditions
Under be difficult to degrade, have larger harm to human body and environment, environmental contaminants be classified as by multiple national environmental protection tissues.Therefore, right
It carries out quick, accurate, trace analysis detection and has a very important significance.Currently, the method for measuring resorcinol mainly has
Spectrophotometry, high performance liquid chromatography, thin-layered chromatography, Micellar Electrokinetic Chromatography and capillary electrophoresis etc., these technologies
Although big using the expensive equipment, reagent consumption than wide, used and analysis time is longer, cannot meet it is live quickly
The demand of detection.Resorcinol has electro-chemical activity, is oxidized easily, therefore can electrochemically be detected.Mostly
Number electricity analytical method has many advantages, such as that time saving, at low cost, selectivity is good, high sensitivity, response is fast, instrument is simple.
Graphene quantum dot, as a kind of novel quantum dot, other than the performance excellent with graphene, also because of it
Apparent quantum confined effect and dimensional effect have shown some novel features.Such as it is 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.
Invention content
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide one kind detecting isophthalic two based on amination graphene quanta dot modified electrode
The method of phenol concentration, have it is easy to operate, detection quickly, high sensitivity, the height of resorcinol in mixing sample solution can be carried out
Sensitive identification.
In order to realize these purposes and other advantages according to the present invention, it is dense to provide resorcinol in a kind of detection solution
The method of degree is detected the resorcinol in solution to be measured by cyclic voltammetry using three-electrode system, according to isophthalic
The linear equation of diphenol obtains the concentration of resorcinol in solution to be measured, and the working electrode in three-electrode system is through amino graphite
Alkene quantum dot moditied processing, the working electrode are glass-carbon electrode.
Preferably, in the described detection solution resorcinol concentration method, at amination graphene quantum dot modification
It is as follows to manage concrete operations：Working electrode is immersed containing in 2mg/mL amination graphene quantum dot solutions, cyclic voltammetric is utilized
It is taken out after method scanning, is placed in infrared drying oven and dries,
Wherein, sweep parameter is：Initial potential 0V, maximum potential 1V, minimum point 0V, final current potential 0V, sweep speed
0.1V/s, scanning times 100 times, sensitivity 10-4A/V, stand-by period 2s.
Preferably, the method for detecting resorcinol concentration in solution, it is further comprising the steps of：
Step 1: preparing the standard solution containing various concentration resorcinol, using PBS buffer solutions as solvent, wherein PBS
The pH of buffer solution is 7.4, and the concentration of a concentration of 0.1mol/L, resorcinol are 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, modified after working electrode build three-electrode system, using following
Ring voltammetry is detected the every part of standard solution prepared in step 1, obtains the cyclic voltammetry curve of every part of standard solution,
And the peak value of current strength in the cyclic voltammetry curve of every part of standard solution is recorded respectively；
Step 3: with the peak value of the corresponding current strength of the cyclic voltammetry curve of the every part of standard solution obtained in step 2
The difference of the peak value of the current strength of standard solution when 0 μm ol/L a concentration of with resorcinol is marked as ordinate with every part
A concentration of abscissa of quasi- solution draws standard curve and calculates linear equation；
Step 4: being detected to the solution to be measured containing unknown concentration resorcinol using cyclic voltammetry, waited for
The cyclic voltammetry curve of solution is surveyed, the peak value of the corresponding current strength of the cyclic voltammetry curve of solution to be measured and resorcinol is dense
Degree is that the difference of the peak value of the current strength of the standard solution of 0mol/L substitutes into the linear equation obtained in step 3, is calculated
To the concentration of resorcinol in solution to be measured.
Preferably, in the described detection solution resorcinol concentration method, the reference electrode in three-electrode system is
Ag/AgCl electrodes, auxiliary electrode are platinum electrode.
Preferably, in the described detection solution resorcinol concentration method, utilize cyclic voltammetric in the step 2
Method detection the condition of scanning be：Initial potential -0.4V terminates current potential 0.8V, sweep speed 0.05V/s, current potential amplification 0.001V,
Stand-by period 2s, sensitivity 10-4A/V。
Preferably, the method for detecting resorcinol concentration in solution, working electrode is through amination graphene amount
Pretreatment is first passed through before son point moditied processing：Use granularity for 1.0 μm, 0.3 μm and 0.05 μ successively on polishing cloth working electrode
The polishing powder of m is polished, and is then cleaned with ultra-pure water.
Preferably, in the described detection solution resorcinol concentration method, after working electrode is preprocessed, amino
Following processing are first passed through before graphite alkene quantum dot moditied processing：
The electrolyte containing 10mM zirconium oxychlorides and 0.3M potassium chloride is first prepared with magnetized water, by pretreated work electricity
One layer of nano oxidized zirconium layer of electro-deposition in electrolyte is immersed in pole；
Metal and stone and propolis will be planted again, and grinds cross 200 mesh and sieve to obtain and plant metal and stone powder and bee glue powder respectively, will plant metal and stone powder and gas
Phase white carbon, bee glue powder and magnetized water are 2 according to mass ratio:2:1:1000 mixing, dispersion liquid is obtained through ultrasonic disperse, takes L points of 10 μ
Dispersion liquid drop coating is on the working electrode that electro-deposition has nano oxidized zirconium layer, drying.
The present invention includes at least following advantageous effect：
1) amination graphene quanta dot modified electrode electron transport rate provided by the invention is fast, and stability is good, prepares
Simply, easy to operate, detection process is simple and convenient, and high sensitivity, detection limit are low, it can be achieved that mixing resorcinol in sample solution
Quick detection；
2) nano zirconium dioxide has good thermo-chemical stability, pyroconductivity, nano zircite layer surface active sites
Point is more, and conductive capability is strong, can amplify electric signal, can enhance the conductivity of amination graphene quantum dot layer in detection process；It plants
Dispersion liquid made from metal and stone powder, gas-phase silica and bee glue powder can increase the specific surface area of working electrode, between being not only enriched with
Benzenediol and quickening electron transport rate, improve the detection sensitivity of resorcinol；
3) method of the invention is simple, and condition is easy to control, has good sensitivity, convenience, working electrode is convenient for life
Production, and in the detection of resorcinol, have a good application prospect, there is fast response time, high sensitivity, method simplicity etc.
Advantage.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Description of the drawings
Fig. 1 is the cyclic voltammetry curve figure of the resorcinol standard solution of various concentration in the embodiment of the present invention 1；
Fig. 2 is the canonical plotting of resorcinol in the embodiment of the present invention 1.
Specific implementation mode
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained.
Embodiment 1：
A kind of method of resorcinol concentration in detection solution, using three-electrode system by cyclic voltammetry to be measured molten
Resorcinol in liquid is detected, and the concentration of resorcinol in solution to be measured is obtained according to the linear equation of resorcinol, and three
For working electrode in electrode system through amination graphene quantum dot moditied processing, the working electrode is glass-carbon electrode.
The method of resorcinol concentration, amination graphene quantum dot moditied processing concrete operations in the detection solution
It is as follows：Working electrode is immersed containing in 2mg/mL amination graphene quantum dot solutions, is taken after being scanned using cyclic voltammetry
Go out, be placed in infrared drying oven and dry,
Wherein, sweep parameter is：Initial potential 0V, maximum potential 1V, minimum point 0V, final current potential 0V, sweep speed
0.1V/s, scanning times 100 times, sensitivity 10-4A/V, stand-by period 2s.
The method of resorcinol concentration, further comprising the steps of in the detection solution：
Step 1: preparing the standard solution containing various concentration resorcinol, using PBS buffer solutions as solvent, wherein PBS
The pH of buffer solution is 7.4, and the concentration of a concentration of 0.1mol/L, resorcinol are 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, modified after working electrode build three-electrode system, using following
Ring voltammetry is detected the every part of standard solution prepared in step 1, obtains the cyclic voltammetry curve of every part of standard solution,
And the peak value of current strength in the cyclic voltammetry curve of every part of standard solution is recorded respectively；
Step 3: with the peak value of the corresponding current strength of the cyclic voltammetry curve of the every part of standard solution obtained in step 2
The difference of the peak value of the current strength of standard solution when 0 μm ol/L a concentration of with resorcinol is marked as ordinate with every part
A concentration of abscissa of quasi- solution draws standard curve and calculates linear equation；
Step 4: being detected to the solution to be measured containing unknown concentration resorcinol using cyclic voltammetry, waited for
The cyclic voltammetry curve of solution is surveyed, the peak value of the corresponding current strength of the cyclic voltammetry curve of solution to be measured and resorcinol is dense
Degree is that the difference of the peak value of the current strength of the standard solution of 0mol/L substitutes into the linear equation obtained in step 3, is calculated
To the concentration of resorcinol in solution to be measured.
The method of resorcinol concentration in the described detection solution, the reference electrode in three-electrode system is Ag/AgCl electricity
Pole, auxiliary electrode are platinum electrode.
The method of resorcinol concentration in the described detection solution, sweeping using cyclic voltammetry detection in the step 2
The condition of retouching is：Initial potential -0.4V terminates current potential 0.8V, sweep speed 0.05V/s, current potential amplification 0.001V, stand-by period
2s, sensitivity 10-4A/V。
The method of resorcinol concentration in the described detection solution, working electrode through amination graphene quantum dot modification at
Pretreatment is first passed through before reason：The polishing powder for being successively 1.0 μm, 0.3 μm and 0.05 μm with granularity on polishing cloth by working electrode
Polishing, is then cleaned with ultra-pure water.
The cyclic voltammetric that the resorcinol standard solution of various concentration shown in FIG. 1 is obtained according to the method for embodiment 1 is bent
Line chart, the wherein concentration of resorcinol are carried out according to for 0mol/L standard solution (i.e. PBS buffer solutions) through above-mentioned cyclic voltammetry
Measurement obtains cyclic voltammetry curve a, and the concentration of resorcinol is followed successively by 1.0 × 10-5mol/L、5×10-5mol/L、1×10- 4mol/L、2×10-4The standard solution of mol/L be measured through above-mentioned cyclic voltammetry obtain successively cyclic voltammetry curve b, c,
D, e, it can be seen that the corresponding current strength of solution to be measured enhances with the increase of the concentration of resorcinol, Fig. 2 is according to step 3
The obtained canonical plotting of resorcinol of method, Y-axis is the difference of current strength peak value, and unit is μ A, and X-axis is isophthalic two
The concentration of standard solution of phenol, unit are μM that current strength and resorcinol concentration have good linear relationship, R2=0.9992.
Embodiment 2：
On the basis of embodiment 1, the method for resorcinol concentration, working electrode are preprocessed in the detection solution
Later, following processing are first passed through before amination graphene quantum dot moditied processing：
The electrolyte containing 10mM zirconium oxychlorides and 0.3M potassium chloride is first prepared with magnetized water, 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 -1.1V~
It is cleaned with ultra-pure water after depositing 8-10 circles under+0.7V；
Metal and stone and propolis will be planted again, and grinds cross 200 mesh and sieve to obtain and plant metal and stone powder and bee glue powder respectively, will plant metal and stone powder and gas
Phase white carbon, bee glue powder and magnetized water are 2 according to mass ratio:2:1:1000 mixing, dispersion liquid is obtained through ultrasonic disperse, takes L points of 10 μ
Dispersion liquid drop coating is on the working electrode that electro-deposition has nano oxidized zirconium layer, drying.
The method of the present embodiment 2, which measures current strength and resorcinol concentration, more preferably linear relationship, R2=0.9999.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (4)
1. a kind of method of resorcinol concentration in detection solution, which is characterized in that pass through cyclic voltammetric using three-electrode system
Method is detected the resorcinol in solution to be measured, and resorcinol in solution to be measured is obtained according to the linear equation of resorcinol
Concentration, for the working electrode in three-electrode system through amination graphene quantum dot moditied processing, the working electrode is glass carbon
Electrode；
Amination graphene quantum dot moditied processing concrete operations are as follows：Working electrode is immersed and contains 2mg/mL amino graphites
In alkene quantum dot solution, is taken out after being scanned using cyclic voltammetry, be placed in infrared drying oven and dry, wherein sweep parameter
For：Initial potential 0V, maximum potential 1V, minimum point 0V, final current potential 0V, sweep speed 0.1V/s, scanning times 100 times,
Sensitivity 10-4A/V, stand-by period 2s；
Working electrode before amination graphene quantum dot moditied processing through first passing through pretreatment：By working electrode on polishing cloth according to
The secondary polishing powder for being 1.0 μm, 0.3 μm and 0.05 μm with granularity is polished, and is then cleaned with ultra-pure water；
Following processing are first passed through after working electrode is preprocessed, before amination graphene quantum dot moditied processing：First with magnetic
Change water and prepare the electrolyte containing 10mM zirconium oxychlorides and 0.3M potassium chloride, pretreated working electrode is immersed in electrolyte
One layer of nano oxidized zirconium layer of electro-deposition；Metal and stone and propolis will be planted again, and grinds cross 200 mesh and sieve to obtain and plant metal and stone powder and bee glue powder respectively,
It is 2 according to mass ratio that metal and stone powder, which will be planted, with gas-phase silica, bee glue powder and magnetized water:2:1:1000 mixing, obtain through ultrasonic disperse
Dispersion liquid, taking 10 μ L dispersant liquid drops to be coated in electro-deposition has on the working electrode of nano oxidized zirconium layer, drying.
2. the method for detecting resorcinol concentration in solution as described in claim 1, which is characterized in that further include following step
Suddenly：
Step 1: the standard solution containing various concentration resorcinol is prepared, and using PBS buffer solutions as solvent, wherein PBS bufferings
The pH of solution is 7.4, and the concentration of a concentration of 0.1mol/L, resorcinol are 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, modified after working electrode build three-electrode system, utilize cycle volt
Peace method is detected the every part of standard solution prepared in step 1, obtains the cyclic voltammetry curve of every part of standard solution, and divide
The peak value of current strength in the cyclic voltammetry curve of every part of standard solution is not recorded；
Step 3: with the peak value of the corresponding current strength of the cyclic voltammetry curve of the every part of standard solution obtained in step 2 and
The difference of the peak value of the current strength of standard solution when a concentration of 0 μm of ol/L of benzenediol is molten with every part of standard as ordinate
A concentration of abscissa of liquid draws standard curve and calculates linear equation；
Step 4: being detected to the solution to be measured containing unknown concentration resorcinol using cyclic voltammetry, obtain to be measured molten
The cyclic voltammetry curve of liquid, the peak value of the corresponding current strength of the cyclic voltammetry curve of solution to be measured and resorcinol is a concentration of
The difference of the peak value of the current strength of the standard solution of 0mol/L substitutes into the linear equation obtained in step 3, is calculated and waits for
Survey the concentration of resorcinol in solution.
3. the method for detecting resorcinol concentration in solution as described in claim 1, which is characterized in that in three-electrode system
Reference electrode is Ag/AgCl electrodes, and auxiliary electrode is platinum electrode.
4. the method for detecting resorcinol concentration in solution as claimed in claim 2, which is characterized in that sharp in the step 2
With cyclic voltammetry detect the condition of scanning be：Initial potential -0.4V terminates current potential 0.8V, sweep speed 0.05V/s, current potential
Amplification 0.001V, stand-by period 2s, sensitivity 10-4A/V。
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Address after: 530001 Nanning Normal University, No. 175, Mingxiu East Road, Nanning City, Guangxi Zhuang Autonomous Region Patentee after: Nanning Normal University Address before: Mingxiu Road East of Nanning city the Guangxi Zhuang Autonomous Region 530001 Guangxi Teachers Education University No. 175 Patentee before: Guangxi Normal University |
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Effective date of registration: 20200117 Address after: No. 137, Xiaojiang resettlement area, Jiangnan team, Hongting street, Qinbei District, Qinzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Hengqin Testing Technology Co., Ltd Address before: 530001 Nanning Normal University, No. 175, Mingxiu East Road, Nanning City, Guangxi Zhuang Autonomous Region Patentee before: Nanning Normal University |