CN104614421A - Electrochemical method for detecting 2,4,6-trichlorophenol - Google Patents
Electrochemical method for detecting 2,4,6-trichlorophenol Download PDFInfo
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- CN104614421A CN104614421A CN201510020921.9A CN201510020921A CN104614421A CN 104614421 A CN104614421 A CN 104614421A CN 201510020921 A CN201510020921 A CN 201510020921A CN 104614421 A CN104614421 A CN 104614421A
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Abstract
The invention relates to the technical field of assay determination of 2,4,6-trichlorophenol, in particular to an electrochemical method for quantitatively detecting the content of 2,4,6-trichlorophenol in a water system by using an HS-beta-CD/AuNPs/ITO modified electrode prepared with a self-assembly method. The modified electrode is simpler to manufacture, the material is low in price, good in stability, non-toxic and environment-friendly, and the detection method effectively reduces interference of coexisting substances and is good in selectivity and high in sensitivity.
Description
Technical field
The present invention relates to 2,4,6-trichlorophenol (2,4,6-TCP) analysis determining technology field, particularly relate to one to utilize self-assembly method to prepare mercapto group-beta-cyclodextrin (HS-β-CD) and golden nanometer particle (AuNPs) to modify ITO electrode and for the electrochemical method of 2,4,6-TCP content in quantitative measurement aqueous systems.
Background technology
Along with the widespread use of chlorinated organics in industrial and agricultural production, the secondary polystream phenol quantity in the environment born grows with each passing day thus, and most of chlorophenol toxicity is large, not easily be decomposed or biodegradation, chemical stability is high, is insoluble in water, easily by food chain enrichment in the grease of biosome.It will be further appreciated that, even if these materials also exist teratogenesis, carcinogenic, mutagenic threat to human health in trace level.2,4,6-TCP is the material that chlorophenol Poisoning is larger, can be used as germifuge, antiseptic, defoliant.In organic synthesis, in paper mill, printing industry use more.In environmental sample 2,4,6-TCP detection main difficulty source there is natural background complexity, concentration is extremely low and interfering material is many.Therefore, how to set up biological and environmental matrices efficient, reliable and to have cost-benefit qualitative and quantitative analysis technology more and more concerned.
Means and the instrument of the various detection polystream of the development along with science and technology phenol are come out one after another, and detection means conventional at present has chromatography, spectroscopic methodology, chemical sensor etc.
1, chromatography: main analytical approach has vapor-phase chromatography, gas chromatography-mass spectrography, high performance liquid chromatography.By controlling a series of chromatographic condition and realizing being separated of polystream phenol and qualitative and quantitative detection with mass spectrum or Sample Pretreatment Technique coupling.Due to vapor-phase chromatography, gas chromatography-mass spectrography and high performance liquid chromatography have fast, the advantage such as high resolving power, high selectivity, these methods become the Main Means analyzed and measure in trace polystream phenol measuring technology gradually.In polystream phenol traditional analysis, chromatography and coupling technique thereof occupy critical role.But chromatography exists that equipment requirement is high, operating performance is complicated, need through the limitations such as the training of professional be not easy to non-laboratory, apply on a large scale.
2, spectroscopic methodology: the technology of spectrographic determination polystream phenol mainly comprises: infrared method, ultraviolet spectrophotometry, Raman spectroscopy etc.Infrared method utilizes material to the selective absorbing of the electromagnetic radiation in infrared light district to carry out a kind of method of structure analysis and qualitative and quantitative analysis.The molecule of measured matter, under infrared radiation, only absorbs the infrared spectrum consistent with its molecular vibration, rotational frequency.Infrared spectrum is dissected, qualitative analysis can be carried out to material.There is many atomic groups in compound molecule, after each atomic group is excited, all can produce eigen vibration, its vibration frequency also must be reflected on infrared absorption spectrum.Accordingly can various atomic group in authenticating compound, also can carry out quantitative test.Ultraviolet spectrophotometry is the method for according to the absorbance log of measured matter in the certain wave strong point or a wavelength range of ultraviolet light, this material being carried out to qualitative and quantitative analysis.Raman spectrum analysis method is the Raman scattering effect found based on India scientist C.V. Raman (Raman), molecular vibration, rotation aspect information are obtained to scattering spectrum analyze different from incident light frequency, and is applied to a kind of analytical approach of molecular structure research.Raman spectrum has quick detection, simple to operate, highly sensitive, repeatable and undamaged advantage of carrying out qualitative and quantitative analysis, but the introducing of be easy to be affected such as loose look area, optical system parameter and some non-detection things all can cause measuring error.
3, chemical sensor: along with the development of science and technology, chemical sensor has greater advance in environmental monitoring.Immunosensor is good because of selectivity in recent years, is highly sensitively more and more paid attention to, and main method has enzyme linked immunosorbent assay, radioimmunology, dissociating strengthens lanthanide fluoro immuno assay method etc.Although immunization is the organic method of detection electrically inactive conventional at present, also have some unvanquishable shortcomings, such as antibody is cultivated costly, can only certain material of specific detection.It is a class easier in various detection method that electrochemical method detects, and has higher sensitivity and selectivity, is particularly suitable for in-situ enrichment and mensuration, by the modification to electrode interface, be suitable for the analysis requirement in complex matrices.Electrochemical analysis in recent years has obtained and has applied more widely in environmental analysis, but is used for the mensuration of electroactive material.And polystream phenol is difficult to directly occur redox reaction on general electrode, so the mensuration of polystream phenol is the difficult problem in electrochemical analysis in aqueous systems always.Electrochemica biological sensor is one of effective way addressed this problem, but there is the defect that sensing interface modification is loaded down with trivial details, condition is harsher.Catalytic oxidation reduction is another solution route.But electrical catalyze reduction technology ground zero, is also in the laboratory exploratory stage, there is a lot of weak point, need solve further.Select suitable electrode material, reduce noble metal use amount, improving current efficiency etc. is the very important problem faced in practical application.
Summary of the invention
Object of the present invention is exactly the electrochemical method providing a kind of detection 2,4,6-TCP for above-mentioned shortcoming, utilizes self-assembly method to prepare HS-β-CD and AuNPs and modifies ITO electrode.On the one hand, HS-β-CD can optionally with various organic, and inorganic and biological guest molecule forms stable Host-guest inclusion complex, has higher molecular selectivity and the accumulation ability to object.On the other hand, AuNPs has larger specific surface area, good electro catalytic activity and electron transmission ability.To be there is the new material of AuNPs and HS-β-CD property simultaneously after AuNPs is by HS-β-CD functionalization.Polystream phenol in solution produces obvious electrochemical signals under the cooperative effect of AuNPs and HS-β-CD, and along with the increase of polystream phenol concentration, corresponding peak current increases, and can be used to the content of target polystream phenol in dosing solution thus.Utilize self-assembly method to prepare HS-β-CD and AuNPs and modify ITO electrode, its electrode fabrication is easier, and material price is cheap, and good stability is nontoxic, free from environmental pollution, and this assay method effectively reduces the interference of coexisting substances, and selectivity is good, highly sensitive.
Technical scheme of the present invention is: a kind of electrochemical method detecting 2,4,6-TCP, utilizes self-assembly method to prepare HS-β-CD and AuNPs and modifies ITO electrode and with 2,4,6-TCP content in its quantitative measurement aqueous systems.
Utilize self-assembly method to make modified electrode, the steps include: to take 0.04 g HAuCl
44H
2o joins in 100 mL ultrapure waters and is heated to boiling, then pipettes the trisodium citrate of 10 mL 38.8 mmol/L, is joined in above-mentioned solution, continue to add hot reflux 15 min and obtain claret solution; By HS-β-CD and AuNPs with the mixed in molar ratio of 2:1, at room temperature continue stirring 24 h, centrifugally obtain HS-β-CD/AuNPs, wash 3 times respectively with ethanol and ultrapure water, vacuum drying 4 h at 60 DEG C; The ITO of 1.5 × 5.0 cm is immersed in methyl alcohol the K of 0.5 mol/L after ultrasonic 10 min
2cO
3in solution, the volume ratio of 1 h(methyl alcohol and ultrapure water is 2:1), a large amount of ultrapure water, nitrogen drying obtains the ITO of surface hydroxylation; Subsequently the above-mentioned ITO handled well is immersed in containing 10
-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take out electrode and use a large amount of ultrapure water after dry 48 h at 120 DEG C; Finally the ITO with phenyl-phosphonic acid is immersed in 10
-4dry up with nitrogen after 24 h in the HS-β-CD/AuNPs solution of mol/L and obtain self-assembling electrode HS-β-CD/AuNPs/SAM/ITO.
With modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode, utilizes differential pulse voltammetry to carry out electrochemical measurement to 2,4,6-TCP.
A kind of electrochemical method detecting 2,4,6-TCP, concrete steps are:
(1) in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Getting a certain amount of 2,4,6-TCP solution with microsyringe joins in electrolytic cell, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, and record differential pulse voltammetry voltammogram, measures peak point current
i p1; According to said method, add 2,4,6-TCP standard solution of variable concentrations, corresponding peak point current can be obtained
i p, peak point current
i ppresent good linear relationship with the concentration of 2,4,6-TCP, the range of linearity is 3.0 × 10
-9– 2.8 × 10
-8mol/L, linear equation is
i p=-0.3889+0.2426
c,
cbe concentration, unit is nmol/L,
i pbe peak point current, unit is μ A, linearly dependent coefficient
r 2=0.9982, detect and be limited to 1.0 × 10
-9mol/L;
(2) in conjunction with above-mentioned linear relationship, to unknown concentration 2,4,6-TCP sample measures, and calculates 2, and 4,6-TCP concentration: in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Add a certain amount of solution to be measured, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, record differential pulse voltammetry voltammogram, obtains peak point current
i p, will
i pbring above-mentioned equation into, the concentration calculating in liquid to be measured 2,4,6-TCP can be asked.
Beneficial effect of the present invention is: a kind of electrochemical method detecting 2,4,6-TCP, utilizes self-assembly method to prepare HS-β-CD and AuNPs and modifies ITO electrode.Polystream phenol in solution produces obvious electrochemical signals under the cooperative effect of AuNPs and HS-β-CD, and along with the increase of polystream phenol concentration, corresponding peak current increases, and can be used to the content of target polystream phenol in dosing solution thus.
Utilize self-assembly method to prepare HS-β-CD and AuNPs and modify ITO electrode, its electrode fabrication is easier, and material price is cheap, and good stability is nontoxic, free from environmental pollution; Utilize the Host-guest Recognition ability of HS-β-CD and the electro catalytic activity of AuNPs and electron transmission ability, improve selectivity and electrochemical activity, by HS-β-CD and the Host-guest Recognition effect of the phenyl ring of the phenyl-phosphonic acid of electrode surface, HS-β-CD/AuNPs is self-assembled to electrode surface, be made into Electrochemical Modification electrode.Employing differential pulse voltammetry scans, and to data processing, effectively reduces the interference of coexisting substances, further increases selectivity and the sensitivity of detection.
The method does not need the steps such as cultivation under specific condition and sample pre-treatments, and detection speed is fast, operation operation; The detection limit of this method to 2,4,6-TCP is relatively low, has higher practical value, and under the cooperative effect of HS-β-CD and AuNPs, effectively reduce the interference of coexisting substances, selectivity is good, highly sensitive.
accompanying drawing illustrates:
Figure 1 shows that the cyclic voltammogram of 2,4,6-TCP in naked ITO electrode and the ITO electrode (HS-β-CD/AuNPs/SAM/ITO electrode) after modifying.
Figure 2 shows that 2,4,6-TCP of variable concentrations differential pulse voltammetry voltammograms on modified electrode.
Figure 3 shows that peak current difference of the present invention and lg
clinear relationship chart.
Wherein, the concentration representing 2,4,6-TCP respectively by the oxidation peak figure of a to h in Fig. 2 is 0,3.0 × 10
-9, 8.0 × 10
-9, 1.2 × 10
-8, 1.6 × 10
-8, 2.0 × 10
-8, 2.4 × 10
-8, 2.8 × 10
-8mol/L;
1-ITO electrode, 2-HS-β-CD/AuNPs/SAM/ITO electrode.
embodiment:
In order to understand the present invention better, describe technical scheme of the present invention in detail with instantiation below, but the present invention is not limited thereto.
Embodiment 1
A kind of electrochemical method detecting 2,4,6-TCP, utilizes self-assembly method to prepare HS-β-CD and AuNPs and modifies ITO electrode and with 2,4,6-TCP content in its quantitative measurement aqueous systems.
1 modified electrode makes, and the steps include: to take 0.04 g HAuCl
44H
2o joins in 100 mL ultrapure waters and is heated to boiling, then pipettes the trisodium citrate of 10 mL 38.8 mmol/L, is joined in above-mentioned solution, continue to add hot reflux 15 min and obtain claret solution; By HS-β-CD and AuNPs with the mixed in molar ratio of 2:1, at room temperature continue stirring 24 h, centrifugally obtain HS-β-CD/AuNPs, wash 3 times respectively with ethanol and ultrapure water, vacuum drying 4 h at 60 DEG C; The ITO of 1.5 × 5.0 cm is immersed in methyl alcohol the K of 0.5 mol/L after ultrasonic 10 min
2cO
3in solution, the volume ratio of 1 h(methyl alcohol and ultrapure water is 2:1), a large amount of ultrapure water, nitrogen drying obtains the ITO of surface hydroxylation; Subsequently the above-mentioned ITO handled well is immersed in containing 10
-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take out electrode and use a large amount of ultrapure water after dry 48 h at 120 DEG C; Finally the ITO with phenyl-phosphonic acid is immersed in 10
-4dry up with nitrogen after 24 h in the HS-β-CD/AuNPs solution of mol/L and obtain self-assembling electrode HS-β-CD/AuNPs/SAM/ITO.
2 utilize above-mentioned HS-β-CD/AuNPs/SAM/ITO modified electrode to measure in solution 2,4,6-TCP, and concrete steps are:
(1) in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Getting a certain amount of 2,4,6-TCP solution with microsyringe joins in electrolytic cell, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, and record differential pulse voltammetry voltammogram, measures peak point current
i p1; According to said method, add 2,4,6-TCP standard solution of variable concentrations, corresponding peak point current can be obtained
i p, peak point current
i ppresent good linear relationship with the concentration of 2,4,6-TCP, the range of linearity is 3.0 × 10
-9– 2.8 × 10
-8mol/L, linear equation is
i p=-0.3889+0.2426
c,
cbe concentration, unit is nmol/L,
i pbe peak point current, unit is μ A, linearly dependent coefficient
r 2=0.9982, detect and be limited to 1.0 × 10
-9mol/L;
(2) in conjunction with above-mentioned linear relationship, to unknown concentration 2,4,6-TCP sample measures, and calculates 2, and 4,6-TCP concentration: in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Add a certain amount of solution to be measured, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, record differential pulse voltammetry voltammogram, obtains peak point current
i p, will
i pbring above-mentioned equation into, the concentration calculating in liquid to be measured 2,4,6-TCP can be asked.
The present invention adopts self-assembly method to prepare HS-β-CD and AuNPs modification ITO electrode and detects 2,4,6-TCP.In solution 2,4,6-TCP produces obvious electrochemical signals under the cooperative effect of AuNPs and HS-β-CD, and along with the increase of 2,4,6-TCP concentration, corresponding peak current increases, and can be used to the content of in dosing solution 2,4,6-TCP thus.Utilize the Host-guest Recognition ability of HS-β-CD and the electro catalytic activity of AuNPs and electron transmission ability, improve selectivity and electrochemical activity, by HS-β-CD and the Host-guest Recognition effect of the phenyl ring of the phenyl-phosphonic acid of electrode surface, HS-β-CD/AuNPs is self-assembled to electrode surface, be made into Electrochemical Modification electrode.Employing differential pulse voltammetry scans, and effectively reduces the interference of coexisting substances, further increases selectivity and the sensitivity of detection.This modified electrode is simple for production, and material price is cheap, and electrode is easy to upgrade, and good stability is nontoxic, free from environmental pollution.This modified electrode achieves the Electrochemical Detection to having comparatively light current chemical activity organism 2,4,6-TCP, can greatly reduce 2,4,6-TCP sense cycle in environment, reduces testing cost.
Claims (4)
1. one kind is detected 2,4,6-trichlorophenol (2,4,6-TCP) electrochemical method, it is characterized in that utilizing self-assembly method to prepare mercapto group-beta-cyclodextrin (HS-β-CD) and golden nanometer particle (AuNPs) and modify ITO electrode and with in its quantitative measurement aqueous systems 2,4,6-TCP content.
2. one according to claim 1 detects the electrochemical method of 2,4,6-TCP, it is characterized in that, utilizes self-assembly method to make modified electrode, the steps include: to take 0.04 g HAuCl
44H
2o joins in 100 mL ultrapure waters and is heated to boiling, then pipettes the trisodium citrate of 10 mL 38.8 mmol/L, is joined in above-mentioned solution, continue to add hot reflux 15 min and obtain claret solution; By HS-β-CD and AuNPs with the mixed in molar ratio of 2:1, at room temperature continue stirring 24 h, centrifugally obtain HS-β-CD/AuNPs, wash 3 times respectively with ethanol and ultrapure water, vacuum drying 4 h at 60 DEG C; The ITO of 1.5 × 5.0 cm is immersed in methyl alcohol the K of 0.5 mol/L after ultrasonic 10 min
2cO
3in solution, the volume ratio of 1 h(methyl alcohol and ultrapure water is 2:1), a large amount of ultrapure water, nitrogen drying obtains the ITO of surface hydroxylation; Subsequently the above-mentioned ITO handled well is immersed in containing 10
-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take out electrode and use a large amount of ultrapure water after dry 48 h at 120 DEG C; Finally the ITO with phenyl-phosphonic acid is immersed in 10
-4dry up with nitrogen after 24 h in the HS-β-CD/AuNPs solution of mol/L and obtain self-assembling electrode HS-β-CD/AuNPs/SAM/ITO.
3. one according to claim 1 detects 2,4, the electrochemical method of 6-TCP, it is characterized in that, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, platinum electrode is to electrode, differential pulse voltammetry is utilized to carry out electrochemical measurement to 2,4,6-TCP.
4. the one according to the arbitrary claim of claim 1-3 detects the electrochemical method of 2,4,6-TCP, and it is characterized in that, concrete steps are:
(1) in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Getting a certain amount of 2,4,6-TCP solution with microsyringe joins in electrolytic cell, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, and record differential pulse voltammetry voltammogram, measures peak point current
i p1; According to said method, add 2,4,6-TCP standard solution of variable concentrations, corresponding peak point current can be obtained
i p, peak point current
i ppresent good linear relationship with the concentration of 2,4,6-TCP, the range of linearity is 3.0 × 10
-9– 2.8 × 10
-8mol/L, linear equation is
i p=-0.3889+0.2426
c,
cbe concentration, unit is nmol/L,
i pbe peak point current, unit is μ A, linearly dependent coefficient
r 2=0.9982, detect and be limited to 1.0 × 10
-9mol/L;
(2) in conjunction with above-mentioned linear relationship, to unknown concentration 2,4,6-TCP sample measures, and calculates 2, and 4,6-TCP concentration: in the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS-β-CD/AuNPs/SAM/ITO for working electrode, Ag/AgCl electrode is contrast electrode, and platinum electrode is to electrode; Experiment is carried out on CHI842C Electrochemical Comprehensive Tester, and its attached computer software is made for the acquisition and processing of experimental data; Add a certain amount of solution to be measured, in 0.0 ~ 0.8 V potential range, carry out differential pulse scanning, record differential pulse voltammetry voltammogram, obtains peak point current
i p, will
i pbring above-mentioned equation into, the concentration calculating in liquid to be measured 2,4,6-TCP can be asked.
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|---|---|---|---|
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Cited By (4)
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| CN105606670A (en) * | 2016-01-19 | 2016-05-25 | 济南大学 | Electrochemical method for detecting polycyclic aromatic hydrocarbons in high-sensitivity manner |
| CN108195920A (en) * | 2018-01-31 | 2018-06-22 | 大丰跃龙化学有限公司 | For detecting the preparation of the electrochemical sensor of 2,4,6- trichlorophenol, 2,4,6,-Ts and analysis method |
| CN108732218A (en) * | 2018-05-21 | 2018-11-02 | 江苏理工学院 | A kind of electrochemical sensor measuring 2,4,6- trichlorophenol, 2,4,6,-Ts and its preparation and application |
| CN109828013A (en) * | 2019-03-11 | 2019-05-31 | 哈尔滨理工大学 | Electrochemical cathode synthesize a kind of metal-organic framework materials and its in Electrochemical Detection water 2,4,6- trichlorophenol, 2,4,6,-T application |
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Cited By (5)
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| CN108195920A (en) * | 2018-01-31 | 2018-06-22 | 大丰跃龙化学有限公司 | For detecting the preparation of the electrochemical sensor of 2,4,6- trichlorophenol, 2,4,6,-Ts and analysis method |
| CN108732218A (en) * | 2018-05-21 | 2018-11-02 | 江苏理工学院 | A kind of electrochemical sensor measuring 2,4,6- trichlorophenol, 2,4,6,-Ts and its preparation and application |
| CN109828013A (en) * | 2019-03-11 | 2019-05-31 | 哈尔滨理工大学 | Electrochemical cathode synthesize a kind of metal-organic framework materials and its in Electrochemical Detection water 2,4,6- trichlorophenol, 2,4,6,-T application |
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| CN104614421B (en) | 2017-06-23 |
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