CN104614421B - A kind of electrochemical method for detecting 2,4,6 trichlorophenol, 2,4,6,-Ts - Google Patents
A kind of electrochemical method for detecting 2,4,6 trichlorophenol, 2,4,6,-Ts Download PDFInfo
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- CN104614421B CN104614421B CN201510020921.9A CN201510020921A CN104614421B CN 104614421 B CN104614421 B CN 104614421B CN 201510020921 A CN201510020921 A CN 201510020921A CN 104614421 B CN104614421 B CN 104614421B
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Abstract
The present invention relates to 2,4,6 trichlorophenol, 2,4,6,-T analysis determining technology fields, it is more particularly to a kind of to prepare sulfydryl beta cyclodextrin and golden nanometer particle modification ITO electrode and with 2 in its quantitative determination aqueous systems using self-assembly method, the electrochemical method of 4,6 trichlorophenol, 2,4,6 ,-T contents.Modified electrode makes easier, and material price is cheap, good stability, nontoxic, free from environmental pollution, and this assay method effectively reduces the interference of coexisting substances, and selectivity is good, and sensitivity is high.
Description
Technical field
The present invention relates to 2,4,6- trichlorophenol, 2,4,6,-Ts（2,4,6-TCP）Analysis determining technology field, it is more particularly to a kind of to survey
Determine the electrochemical method of 2,4,6-TCP contents in aqueous systems.
Background technology
With extensive use of the chlorinated organics in industrial and agricultural production, thus the secondary polystream phenol for bearing is in the environment
Quantity it is growing day by day, most of chlorophenol toxicity is big, is difficult to be decomposed or biodegradable, and chemical stability is high, is insoluble in water, holds
Easily it is enriched with the grease of organism by food chain.It will be further appreciated that, even if these materials are also right in trace level
There is teratogenesis, carcinogenic, mutagenic threat in human health.2,4,6-TCP is the larger material of chlorophenol Poisoning, can be used as sterilization
Agent, preservative, defoliant.In organic synthesis, used in paper mill, printing industry more.The inspection of 2,4,6-TCP in environmental sample
The main difficulty source of survey to there is natural background complicated, concentration is extremely low and interfering material more than.Therefore, how to set up to biological and
Environmental matrices is efficient, reliable and more and more concerned with cost-benefit qualitative and quantitative analysis technology.With science and technology
The means and instrument of the various detection polystream phenols of development are come out one after another, detection means conventional at present have chromatography, spectroscopic methodology,
Chemical sensor etc..
1st, chromatography：Main analysis method has gas chromatography, gas chromatography-mass spectrography, high performance liquid chromatography.It is logical
Cross and control a series of chromatographic condition and realize that polystream phenol is separated and qualitative fixed with mass spectrum or Sample Pretreatment Technique combination
Amount detection.Because gas chromatography, gas chromatography-mass spectrography and high performance liquid chromatography have quick, high-resolution, high selection
Property the advantages of, these methods be increasingly becoming analysis determine trace polystream phenol measuring technology in Main Means.In polystream
In phenol traditional analysis, chromatography and its GC-MS occupy critical role.But chromatography exist equipment requirement it is high, operation
Formality is complicated, need to be not easy in non-laboratory, large-scale popularization and application through the limitation such as training of professional.
2nd, spectroscopic methodology：The technology of spectrographic determination polystream phenol mainly includes：Infrared method, ultraviolet spectrophotometry, Raman
Spectroscopic methodology etc..Infrared method is that the selective absorbing of the electromagnetic radiation of infrared light district is carried out structural analysis and determined using material
Property and a kind of method of quantitative analysis.The molecule of measured matter absorbs and its molecular vibration, rotation frequency under infrared radiation, only
The consistent infrared spectrum of rate.Infrared spectrum is dissected, qualitative analysis can be carried out to material.Existed in compound molecule
Many atomic groups, after each atomic group is excited, can all produce eigen vibration, and its vibration frequency is also necessarily reflected in INFRARED ABSORPTION light
In spectrum.Accordingly can various atomic groups in authenticating compound, can also carry out quantitative analysis.Ultraviolet spectrophotometry is according to measured object
The method that trap of the matter in the certain wave strong point or a wavelength range of ultraviolet light carries out qualitative and quantitative analysis to the material.
Raman spectrum analysis method is the Raman scattering effect found based on India scientist C.V. Ramans (Raman), pair and incident light
The different scattering spectrum of frequency is analyzed to obtain molecular vibration, rotation aspect information, and is applied to molecular structure research
A kind of analysis method.Raman spectrum has quick detection, simple to operate, sensitivity high, repeatable and undamaged is determined
The advantage of property quantitative analysis, but be highly susceptible to influence such as dissipate drawing for color area, optical system parameter and some non-detection things
Entering can all cause measurement error.
3rd, chemical sensor：With the development of science and technology, chemical sensor has greater advance in terms of environmental monitoring.
In recent years immunosensor because selectivity it is good, sensitivity is high more and more to be paid attention to, and main method has Enzyme-linked Immunosorbent Assay
Method, radioimmunology, dissociation enhancing lanthanide fluoro immuno assay method etc..Immunization is despite detection electrically inactive conventional at present
The method of organic matter, but also have some unvanquishable shortcomings, such as antibody culture is costly, can only specific detection certain
Material.Electrochemical method detection is an easier class in various detection methods, with sensitivity higher and selectivity, especially
It is suitable for in-situ enrichment and measure, by the modification to electrode interface, suitably the analysis requirement in complex matrices.In recent years send a telegram here
Chemical analysis has obtained wide application in environmental analysis, but is used for the measure of electroactive material.And polystream phenol exists
It is difficult to directly redox reaction on general electrode, so the measure of polystream phenol is always electrochemical analysis in aqueous systems
In problem.Electrochemica biological sensor is one of the effective way for solving this problem, but there is sensing interface modified
The defect that journey is cumbersome, condition is harsher.Electrocatalytic oxidation reduction is another solution route.But electro-catalysis reduction technique ground zero,
Also in the laboratory exploratory stage, many weak points are there are, need to further solved.Suitable electrode material is selected, is reduced
Noble metal usage amount, it is the critically important problem faced in practical application to improve current efficiency etc..
The content of the invention
The purpose of the present invention provides a kind of electrochemical method of detection 2,4,6-TCP aiming at disadvantages mentioned above, utilizes
Self-assembly method prepares HS- β-CD and AuNPs modification ITO electrode.On the one hand, the nothing organic with various that HS- β-CD can be selective
Machine and biological guest molecule form the Host-guest inclusion complex stablized, with molecule higher selectively and to the enrichment energy of object
Power.On the other hand, AuNPs has larger specific surface area, good electro catalytic activity and electron transmission ability.When AuNPs quilts
To there is the new material of AuNPs and HS- β-CD properties simultaneously after HS- β-CD functionalization.Polystream phenol in solution
Obvious electrochemical signals are produced under the cooperative effect of AuNPs and HS- β-CD, with the increase of polystream phenol concentration, accordingly
Peak current increase, thus can be used to the content of target polystream phenol in dosing solution.Using self-assembly method prepare HS- β-
CD and AuNPs modification ITO electrodes, its electrode fabrication is easier, and material price is cheap, good stability, nontoxic, free from environmental pollution,
And this assay method effectively reduces the interference of coexisting substances, selectivity is good, and sensitivity is high.
The technical scheme is that：The electrochemical method of one kind detection 2,4,6-TCP, it is characterised in that specific steps
For：Weigh 0.04 g HAuCl4·4H2O is heated to boiling in being added to 100 mL ultra-pure waters, then pipettes 10 mL 38.8
The trisodium citrate of mmol/L, in adding it to above-mentioned solution, continues to be heated to reflux 15 min to obtain claret solution；Will
HS- β-CD and AuNPs are with 2：1 mixed in molar ratio, continues to stir 24 h at room temperature, and centrifugation obtains HS- β-CD/AuNPs, uses
Ethanol and ultra-pure water are washed 3 times respectively, and 4 h are vacuum dried at 60 DEG C；By the ITO of 1.5 × 5.0 cm in methyl alcohol ultrasound 10
The K of 0.5 mol/L is immersed in after min2CO31 h in solution, a large amount of ultrapure waters, nitrogen is dried to obtain surface hydroxylation
ITO electrode；Then the above-mentioned ITO electrode handled well is immersed in and contains 10-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take
Go out after electrode dries 48 h at 120 DEG C and obtain the ITO electrode with phenyl-phosphonic acid with a large amount of ultrapure waters（It is denoted as SAM/
ITO electrode）, SAM/ITO electrodes are finally immersed in 10-4Blown with nitrogen after 24 h in the HS- β-CD/AuNPs solution of mol/L
It is dry to obtain self-assembling electrode HS- β-CD/AuNPs/SAM/ITO.It is work electricity with modified electrode HS- β-CD/AuNPs/SAM/ITO
Pole, Ag/AgCl electrodes are reference electrode, and platinum electrode is, to electrode, electrification to be carried out using differential pulse voltammetry to 2,4,6-TCP
Learn measurement.
The electrochemical method of one kind detection 2,4,6-TCP, concretely comprises the following steps：
（1）In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS- β-CD/AuNPs/SAM/
ITO is working electrode, and Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is comprehensively surveyed in CHI842C electrochemistry
Carried out on examination instrument, its attached computer software is made for the collection and treatment of experimental data；Taken with microsyringe a certain amount of
2,4,6-TCP solution are added in electrolytic cell, and differential pulse scanning is carried out in 0.0~0.8 V potential ranges, and record shows poor arteries and veins
Voltammogram is rushed, peak point current is measuredI p1；According to said method, 2,4,6-TCP standard liquids of various concentrations are added, you can obtain corresponding
Peak point currentI p, peak point currentI pWith 2,4,6-TCP concentration is presented good linear relationship, and the range of linearity is 3.0 × 10-9 – 2.8×10-8 Mol/L, linear equation isI p = -0.3889 + 0.2426c,cIt is concentration, unit is nmol/L,I pIt is
Peak point current, unit is μ A, linearly dependent coefficientR 2 =0.9982, detection is limited to 1.0 × 10-9 mol/L；
（2）With reference to above-mentioned linear relationship, the 2 of unknown concentration, 4,6-TCP samples are measured, calculate 2,4,6-TCP
Concentration：In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, it is with modified electrode HS- β-CD/AuNPs/SAM/ITO
Working electrode, Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is on CHI842C Electrochemical Comprehensive Testers
Carry out, its attached computer software is made for the collection and treatment of experimental data；A certain amount of solution to be measured is added, 0.0~
Differential pulse scanning is carried out in 0.8 V potential ranges, differential pulse voltammetry voltammogram is recorded, peak point current is obtainedI p, willI pSubstitute into above-mentioned
Equation, can seek the concentration for calculating in prepare liquid 2,4,6-TCP.
Beneficial effects of the present invention are：The electrochemical method of one kind detection 2,4,6-TCP, HS- is prepared using self-assembly method
β-CD and AuNPs modification ITO electrodes.Polystream phenol in solution is produced significantly under the cooperative effect of AuNPs and HS- β-CD
Electrochemical signals, with the increase of polystream phenol concentration, thus corresponding peak current increase can be used to mesh in dosing solution
Mark the content of polystream phenol.
HS- β-CD and AuNPs modification ITO electrode are prepared using self-assembly method, its electrode fabrication is easier, and material price is low
Honest and clean, good stability is nontoxic, free from environmental pollution；Using the Host-guest Recognition ability of HS- β-CD and the electro catalytic activity of AuNPs and
Electron transmission ability, improves selectivity and electro-chemical activity, by HS- β-CD and the master of the phenyl ring of the phenyl-phosphonic acid of electrode surface
HS- β-CD/AuNPs are self-assembled to electrode surface by object recognition reaction, are fabricated to Electrochemical Modification electrode.Using differential pulse voltammetry
Scanning, and to data processing, effectively reduces the interference of coexisting substances, further increases the selectivity of detection and sensitive
Degree.
The method does not need the steps such as culture and the sample pre-treatments under specific condition, and detection speed is fast, operation operation；This
Method is to 2, and 4,6-TCP detection limit is relatively low, with practical value higher, in the cooperative effect of HS- β-CD and AuNPs
Under, the interference of coexisting substances is effectively reduced, selectivity is good, and sensitivity is high.
Brief description of the drawings：
Fig. 1 show ITO electrodes of the 2,4,6-TCP after naked ITO electrode and modification（HS-β-CD/AuNPs/SAM/ITO
Electrode）On cyclic voltammogram.
Fig. 2 show differential pulse voltammetry voltammograms of the 2,4,6-TCP of various concentrations on modified electrode.
Fig. 3 show peak current difference of the present invention and lgcLinear relationship chart.
Wherein, the concentration for 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 electrodes, 2- HS- β-CD/AuNPs/SAM/ITO electrodes.
Specific embodiment：
For a better understanding of the present invention, technical scheme is described in detail with instantiation below, but originally
Invention is not limited thereto.
Embodiment 1
A kind of electrochemical method of detection 2,4,6-TCP.
1 modified electrode makes, and its step is：Weigh 0.04 g HAuCl4·4H2O adds in being added to 100 mL ultra-pure waters
Then heat pipette the trisodium citrate of the mmol/L of 10 mL 38.8 to seething with excitement, and adds it in above-mentioned solution, continues to heat
15 min that flow back obtain claret solution；By HS- β-CD and AuNPs with 2：1 mixed in molar ratio, continues to stir 24 at room temperature
H, centrifugation obtains HS- β-CD/AuNPs, is washed respectively 3 times with ethanol and ultra-pure water, and 4 h are vacuum dried at 60 DEG C；By 1.5 ×
The ITO of 5.0 cm is immersed in the K of 0.5 mol/L after ultrasonic 10 min in methyl alcohol2CO31 h in solution（Methyl alcohol and ultra-pure water
Volume ratio is 2:1）, a large amount of ultrapure waters, nitrogen is dried to obtain the ITO of surface hydroxylation；Then by the above-mentioned ITO for handling well
It is immersed in and contains 10-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take out after electrode dries 48 h at 120 DEG C and are surpassed with a large amount of
Pure water rinsing obtains the ITO electrode with phenyl-phosphonic acid（It is denoted as SAM/ITO electrodes）, SAM/ITO electrodes are finally immersed in 10-4
Dried 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, using in above-mentioned HS- β-CD/AuNPs/SAM/ITO modified electrodes measure solution 2,4,6-TCP, concretely comprise the following steps：
（1）In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS- β-CD/AuNPs/SAM/
ITO is working electrode, and Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is comprehensively surveyed in CHI842C electrochemistry
Carried out on examination instrument, its attached computer software is made for the collection and treatment of experimental data；Taken with microsyringe a certain amount of
2,4,6-TCP solution are added in electrolytic cell, and differential pulse scanning is carried out in 0.0~0.8 V potential ranges, and record shows poor arteries and veins
Voltammogram is rushed, peak point current is measuredI p1；According to said method, 2,4,6-TCP standard liquids of various concentrations are added, you can obtain corresponding
Peak point currentI p, peak point currentI pWith 2,4,6-TCP concentration is presented good linear relationship, and the range of linearity is 3.0 × 10-9 – 2.8×10-8 Mol/L, linear equation isI p = -0.3889 + 0.2426c,cIt is concentration, unit is nmol/L,I pIt is
Peak point current, unit is μ A, linearly dependent coefficientR 2 =0.9982, detection is limited to 1.0 × 10-9 mol/L；
（2）With reference to above-mentioned linear relationship, the 2 of unknown concentration, 4,6-TCP samples are measured, calculate 2,4,6-TCP
Concentration：In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, it is with modified electrode HS- β-CD/AuNPs/SAM/ITO
Working electrode, Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is on CHI842C Electrochemical Comprehensive Testers
Carry out, its attached computer software is made for the collection and treatment of experimental data；A certain amount of solution to be measured is added, 0.0~
Differential pulse scanning is carried out in 0.8 V potential ranges, differential pulse voltammetry voltammogram is recorded, peak point current is obtainedI p, willI pSubstitute into above-mentioned
Equation, can seek the concentration for calculating in prepare liquid 2,4,6-TCP.
The present invention prepares HS- β-CD and AuNPs modification ITO electrode and 2,4,6-TCP is detected using self-assembly method.It is molten
In liquid 2,4,6-TCP produce obvious electrochemical signals under the cooperative effect of AuNPs and HS- β-CD, with 2,4,6-TCP
The increase of concentration, corresponding peak current increase, thus can be used in dosing solution 2,4,6-TCP content.Using HS- β-
The Host-guest Recognition ability of CD and the electro catalytic activity of AuNPs and electron transmission ability, improve selectivity and electro-chemical activity, lead to
Cross HS- β-CD and HS- β-CD/AuNPs are self-assembled into electricity with the Host-guest Recognition effect of the phenyl ring of the phenyl-phosphonic acid of electrode surface
Pole surface, is fabricated to Electrochemical Modification electrode.Scanned using differential pulse voltammetry, effectively reduce the interference of coexisting substances, further
Improve selectivity and the sensitivity of detection.This modified electrode is simple for production, and material price is cheap, and electrode is easily updated, surely
It is qualitative good, it is nontoxic, it is free from environmental pollution.The modified electrode is realized to compared with light current chemism organic matter 2,4,6-TCP's
Electrochemical Detection, can greatly reduce 2,4,6-TCP detection cycle in environment, reduce testing cost.
Claims (3)
1. it is a kind of to detect 2,4,6- trichlorophenol, 2,4,6,-Ts（2,4,6-TCP）Electrochemical method, it is characterised in that concretely comprise the following steps：Claim
Take 0.04 g HAuCl4·4H2O is heated to boiling in being added to 100 mL ultra-pure waters, then pipettes the mmol/L of 10 mL 38.8
Trisodium citrate, in adding it to above-mentioned solution, continue to be heated to reflux 15 min to obtain claret solution；By HS- β-CD
With AuNPs with 2：1 mixed in molar ratio, continues to stir 24 h at room temperature, and centrifugation obtains HS- β-CD/AuNPs, with ethanol and
Ultra-pure water is washed 3 times respectively, and 4 h are vacuum dried at 60 DEG C；By the ITO electrode of 1.5 × 5.0 cm in methyl alcohol ultrasound 10
The K of 0.5 mol/L is immersed in after min2CO31 h in solution, a large amount of ultrapure waters, nitrogen is dried to obtain surface hydroxylation
ITO electrode；Then the above-mentioned ITO electrode handled well is immersed in and contains 10-324 h in the phenyl-phosphonic acid aqueous solution of mol/L, take
Go out after electrode dries 48 h at 120 DEG C and obtain the ITO electrode with phenyl-phosphonic acid with a large amount of ultrapure waters（It is denoted as SAM/
ITO electrode）, SAM/ITO electrodes are finally immersed in 10-4Blown with nitrogen after 24 h in the HS- β-CD/AuNPs solution of mol/L
It is dry to obtain self-assembling electrode HS- β-CD/AuNPs/SAM/ITO.
2. one kind according to claim 1 detects 2,4,6-TCP electrochemical method, it is characterised in that with modified electrode
HS- β-CD/AuNPs/SAM/ITO are working electrode, and Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode, using difference
Pulse voltammetry carries out electrochemical measurement to 2,4,6-TCP.
3. the one kind according to claim 1-2 any claims detects 2,4,6-TCP electrochemical method, and its feature exists
In concretely comprising the following steps：
（1）In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS- β-CD/AuNPs/SAM/ITO
It is working electrode, Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is in CHI842C Electrochemical Comprehensive Testers
On carry out, its attached computer software is made for the collection and treatment of experimental data；A certain amount of 2,4 are taken with microsyringe,
6-TCP solution is added in electrolytic cell, and differential pulse scanning, record differential pulse voltammetry volt are carried out in 0.0~0.8 V potential ranges
Antu, measures peak point currentI p1；According to said method, 2,4,6-TCP standard liquids of various concentrations are added, you can obtain corresponding peak
Current valueI p, peak point currentI pWith 2,4,6-TCP concentration is presented good linear relationship, and the range of linearity is 3.0 × 10-9 –
2.8×10-8 Mol/L, linear equation isI p = -0.3889 + 0.2426c,cIt is concentration, unit is nmol/L,I pIt is peak electricity
Flow valuve, unit is μ A, linearly dependent coefficientR 2 =0.9982, detection is limited to 1.0 × 10-9 mol/L；
（2）With reference to above-mentioned linear relationship, the 2 of unknown concentration, 4,6-TCP samples are measured, calculate 2,4,6-TCP is dense
Degree：In the electrolytic cell of the PBS solution containing 10 mL pH 6.5, with modified electrode HS- β-CD/AuNPs/SAM/ITO as work
Make electrode, Ag/AgCl electrodes are reference electrode, and platinum electrode is to electrode；Experiment is enterprising in CHI842C Electrochemical Comprehensive Testers
OK, its attached computer software is made for the collection and treatment of experimental data；A certain amount of solution to be measured is added, 0.0~0.8
Differential pulse scanning is carried out in V potential ranges, differential pulse voltammetry voltammogram is recorded, peak point current is obtainedI p, willI pSubstitute into above-mentioned side
Journey, can seek the concentration for calculating in prepare liquid 2,4,6-TCP.
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| CN105606670B (en) * | 2016-01-19 | 2018-04-03 | 济南大学 | A kind of electrochemical method of highly sensitive detection polycyclic aromatic hydrocarbon |
| 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 |
| CN108732218B (en) * | 2018-05-21 | 2020-06-12 | 江苏理工学院 | Electrochemical sensor for measuring 2,4, 6-trichlorophenol and preparation and application thereof |
| CN109828013B (en) * | 2019-03-11 | 2021-04-09 | 哈尔滨理工大学 | Metal organic framework material synthesized by electrochemical cathode and application of metal organic framework material in electrochemical detection of 2,4, 6-trichlorophenol in water |
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