CN100567974C - Measure the method for three kinds of isomerss of nitrophenols simultaneously - Google Patents
Measure the method for three kinds of isomerss of nitrophenols simultaneously Download PDFInfo
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- CN100567974C CN100567974C CNB2007100387423A CN200710038742A CN100567974C CN 100567974 C CN100567974 C CN 100567974C CN B2007100387423 A CNB2007100387423 A CN B2007100387423A CN 200710038742 A CN200710038742 A CN 200710038742A CN 100567974 C CN100567974 C CN 100567974C
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Abstract
The present invention relates to a kind of method of utilizing carboxylated multi-walled carbon nano-tubes modified electrode to measure three kinds of isomerss of basic phenol simultaneously, belong to organic chemistry isomers analysis determining technology field.It is as follows that the present invention measures process: at first glass-carbon electrode is applied dressing agent, dressing agent is dissolved in N for the carboxylated multiple-wall carbon nanotube of crossing through nitric acid treatment, the concentration that the mixed solution of dinethylformamide is made into is 0.1mg/ml, it is applied to the glass-carbon electrode surface, after the infrared lamp oven dry, promptly gets carboxylated receiving of carbon pipe modified electrode; Utilize this electrode and CHI660B galvanochemistry comprehensive tester then, be 0.4 at current potential～-the 0.9V scope in, electrode is carried out cyclic voltammetry scan in three kinds of isomers mixed solutions of nitrophenols, sweep velocity is 50mV/s, get differential linearity scanning volt-ampere curve one time, and obtain the concentration and the peak current graph of relation of each nitrophenols, obtain the typical curve equation simultaneously; With measured I
PValue is this equation of substitution respectively, can calculate the concentration of each nitrophenols.
Description
Technical field
The present invention relates to a kind ofly utilize carboxylated multi-walled carbon nano-tubes modified electrode to measure the method for three kinds of isomerss of nitrophenols simultaneously, belong to organic chemistry isomers analysis determining technology field.
Background technology
Phenolic compound is second largest class environmental contaminants; it is the common material in the industrial waste water; and the toxicity of nitrophenols is bigger, and wherein dinitrophenol is decided to be priority pollutant by the U.S. environment protection council, and therefore the separation detection for them becomes one of important topic of environmental analysis research.At present the separation determination main method for the nitrophenols isomers has: Flow Injection Analysis, spectrophotometric method combine with chemometrics method, liquid chromatography, the chromatography of ions and Capillary Electrophoresis etc.More than the assay method of several nitrophenols isomerss be not easy to carry, cost an arm and a leg, be not suitable in the environment water monitoring in real time, on-line determination.
Adopt electrochemical method, close by the nitrophenols isomers in three's character, be that oxidation peak current potential or reduction peak current potential are all very approaching and be difficult to realize measuring respectively.Therefore, must adopt the innovative approach of a kind of novelty on the galvanochemistry, three kinds of isomerss of paranitrophenol are measured simultaneously.
Summary of the invention
Thereby the purpose of this invention is to provide a kind of carboxylic carbon nano-tube modified electrode that utilizes and improve nitrophenols is measured three kinds of isomerss of nitrophenols simultaneously at the redox reaction employing electrochemical method of electrode surface method.
A kind of method of measuring three kinds of isomerss of nitrophenols simultaneously of the present invention is characterized in that having following mensuration process and step:
A, preparation hydroxylation carbon nano tube modified electrode: on common glass-carbon electrode matrix, apply the carboxylic carbon nano-tube dressing agent; The preparation method of this dressing agent is the carboxylated multi-walled carbon nano-tubes that 1mg is crossed through nitric acid treatment, joins the N of 10mL, and in the dinethylformamide, sonicated makes its even dispersion half an hour, obtains the black mixed solution of 0.1mg/mL, is dressing agent; The above-mentioned finely dispersed dressing agent of 10 μ l dripped be coated on the glass-carbon electrode matrix surface that cleans up, with infrared lamp oven dry 1 hour, behind distilled water flushing, promptly get again and test required carboxylic carbon nano-tube modified electrode subsequently;
B, make the typical curve of nitrophenols isomerism body measurement:
(1) in electrolytic cell, as working electrode, contrast electrode is that saturated calomel electrode, auxiliary electrode are the platinized platinum electrode with the carboxylic carbon nano-tube modified electrode; Experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Current potential 0.4～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; With m-nitrophenol, the concentration of its phenol of nitre is separately fixed at 4 * 10
-4Mol/L, and the concentration of change ortho-nitrophenol, along with the increase of ortho-nitrophenol concentration, reduction peak current increases, and gets ortho-nitrophenol linear relationship curve I
P=0.9306C+0.6479, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9964; Electric current I
PUnit be μ A;
(2) in electrolytic cell, as working electrode, contrast electrode is a saturated calomel electrode with the carboxylic carbon nano-tube modified electrode, and auxiliary electrode is the platinized platinum electrode; Experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Current potential 0.4～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; The concentration of ortho-nitrophenol, paranitrophenol is separately fixed at 4 * 10
-4Mol/L, and the concentration of change m-nitrophenol, along with the increase of m-nitrophenol concentration, reduction peak current increases, and gets m-nitrophenol linear relationship curve I
P=0.5976C+2.4071, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9972; Electric current I
PUnit be μ A;
(3) separate in the pond at electrode, as working electrode, contrast electrode is a saturated calomel electrode with the carboxylic carbon nano-tube modified electrode, and auxiliary electrode is the platinized platinum electrode, experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached software for calculation is made for collection of experiment data and processing; Be 0.4 at current potential～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and following collection volt-ampere scanning two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; The concentration of ortho-nitrophenol, m-nitrophenol is separately fixed at 4 * 10
-4Mol/L, and the concentration of change paranitrophenol, along with the increase of paranitrophenol concentration, reduction peak current increases, and gets paranitrophenol linear relationship curve I
P=0.6202C+0.4630, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9965; Electric current I
PUnit be μ A;
C, its phenol isomers mixed solution sample of nitre is measured:
In conjunction with above-mentioned typical curve, the nitrophenols isomers mixed solution sample of unknown concentration is measured, calculate the concentration of each isomeride; Ortho-nitrophenol, m-nitrophenol, paranitrophenol three component mixed solutions with unknown concentration are placed in the electrolytic cell, and as working electrode, contrast electrode is that saturated calomel electrode, auxiliary electrode are the platinized platinum electrode with the carboxylic carbon nano-tube modified electrode; Test is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Be 0.4 at current potential～-electrode being contained in the 0.9V scope and carrying out cyclic voltammetry scan two circles in the solution of ortho-nitrophenol, a nitro, paranitrophenol with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; Record the I of different isomerss respectively at different characteristic voltage belt place
PValue; With measured I
PIn the typical curve equation of the above-mentioned gained of value difference substitution, calculate ortho-nitrophenol, m-nitrophenol, paranitrophenol concentration separately.
The present invention has utilized a kind of carboxylated multi-walled carbon nano-tubes modified electrode, is used as detecting the chemical sensor of nitrophenols isomers in the water with it.The inventive method has following advantage:
(1), adopt the carboxylated direct modified glassy carbon electrode of multi-walled carbon nano-tubes, distinguish the isomeride characteristic peak with it, need not compound other compounds, comparatively simple and efficient with the electrode method of modifying.
(2), measure highly sensitively, adopt the first order derivative technology to reduce the background interference signal, can further improve signal response.
(3), can carry out the while electrochemical gaging by three kinds of isomerss of paranitrophenol.
(4), this method is that the selective determination of a series of isomerss and even three-dimensional enantiomorph has improved new thinking.
Description of drawings
Fig. 1 is that carbon nano tube modified electrode is schemed the linear sweep one subdifferential volt-ampere (V-I) of variable concentrations ortho-nitrophenol in the inventive method.Medium solution is acid, and sweep velocity is 50mV/S, and m-nitrophenol, paranitrophenol are separately fixed at 4 * 10
-4Mol/L changes the concentration of adjacent its phenol of nitre; The concentration of ortho-nitrophenol is: 1-0,2-2 * 10
-4Mol/L, 3-4 * 10
-4Mol/L, 4-6 * 10
-4Mol/L, 5-8 * 10
-4Mol/L, 6-10 * 10
-4Mol/L; Horizontal ordinate is E/Vvs.SCE (saturated calomel electrode), and ordinate is I/ μ A.
Fig. 2 is the standard pass of concentration and peak current when carbon nano tube modified electrode detects ortho-nitrophenol in the inventive method
It is curve map.Among the figure, horizontal ordinate is ortho-nitrophenol concentration (mol/L), and ordinate is electric current I/μ A.
Embodiment
Embodiment 1
1, at first prepares hydroxylation multi-walled carbon nano-tubes modified electrode: on common glass-carbon electrode matrix, apply the carboxylic carbon nano-tube dressing agent; The preparation method of this dressing agent: with the carboxylated multi-walled carbon nano-tubes that 1mg crosses through nitric acid treatment, join the N of 10ml, in the dinethylformamide, sonicated makes its even dispersion half an hour, obtains the black mixed solution of 1mg/10ml, is dressing agent; The above-mentioned finely dispersed dressing agent of 10ul dripped be coated on the glass-carbon electrode matrix surface that cleans up, with infrared lamp oven dry 1 hour, behind distilled water flushing, promptly get again and test required carboxylic carbon nano-tube modified electrode subsequently; The diameter of carbon nano-tube is 20～40nm.
2, make the typical curve of nitrophenols isomerism body measurement:
(1) in electrolytic cell, as working electrode, contrast electrode is that saturated calomel electrode, auxiliary electrode are the platinized platinum electrode with the carboxylic carbon nano-tube modified electrode; Experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Current potential 0.4～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 5mV/S; With m-nitrophenol, the concentration of its phenol of nitre is separately fixed at 4 * 10
-4Mol/L, and the concentration of change ortho-nitrophenol; Its concentration is respectively: 1-0,2-2 * 10
-4Mol/L, 3-4 * 10
-4Mol/L, 4-6 * 10
-4Mol/L, 5-8 * 10
-4Mol/L, 6-10 * 10
-4Mol/L; Obtain linear sweep one subdifferential volt-ampere (V-I) figure of ortho-nitrophenol; Referring to Fig. 1, wherein horizontal ordinate is E/Vvs.SCE (mercurous chloride electrode), and ordinate is I/ μ A.Along with concentration increases, the reduction peak power supply also increases.Be converted to ortho-nitrophenol linear relationship curve then, promptly the equation of typical curve is I
P=0.9306C+0.6479, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9964.
Referring to Fig. 2, Fig. 2 is ortho-nitrophenol concentration and peak current linear relationship curve map, and wherein horizontal ordinate is ortho-nitrophenol concentration (mol/L), and ordinate is electric current (I/ μ A).
(2) employing can obtain m-nitrophenol linear relationship curve with the step of above-mentioned same method, and promptly the typical curve equation is I
P=0.5976C+2.4071, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9972.(its curve map is similar to the former, is omitted)
(3) adopt with above-mentioned same method and step, can obtain paranitrophenol linear relationship curve, promptly the typical curve equation is I
P=0.6202C+0.4630, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9965.(its curve map is similar to the former, is omitted)
3, its phenol isomers mixed solution sample of nitre is measured:
(1) at first identify the sensitivity or the relative error of this assay method: preparation ortho-nitrophenol, m-nitrophenol, paranitrophenol three concentration of component are respectively 1.0 * 10
-4Mol/L, 3.0 * 10
-4Mol/L, 1.0 * 10
-4The mixed solution of mol/L; In electrolytic cell, as working electrode, contrast electrode is saturated calomel electrode (SCE) with the carboxylic carbon nano-tube modified electrode, and auxiliary electrode is the platinized platinum electrode, experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing.Be 0.4 at current potential～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode; Carry out linear sweep afterwards, sweep velocity is 50mV/S, the I that records respectively at different characteristic spike potential place
PValue is respectively in the typical curve equation of the above-mentioned gained of substitution, calculates ortho-nitrophenol, m-nitrophenol, paranitrophenol concentration and is respectively 1.01,3.05,0.96 * 10
-4Mol/L, measuring the recovery is 101.0%, 101.7%, 96%, all within the error allowed band.
(2) the nitrophenols isomers mixed solution sample of unknown concentration is measured: utilize above-mentioned typical curve equation, adopt and above-mentioned same method and step, ortho-nitrophenol, m-nitrophenol, the paranitrophenol mixed solution of unknown concentration are measured.On the different characteristic spike potential on the linear sweep voltammogram, promptly ortho-nitrophenol is about-0.18V, and m-nitrophenol is about 0.05V, and paranitrophenol is located about 0.25V, records I separately
PValue, and in the typical curve equation with the above-mentioned gained of its difference substitution, calculate the concentration of ortho-nitrophenol, m-nitrophenol, paranitrophenol.
Claims (1)
1. method of measuring three kinds of isomerss of nitrophenols simultaneously is characterized in that having following mensuration process and step:
A, preparation hydroxylation carbon nano tube modified electrode: on common glass-carbon electrode matrix, apply the carboxylic carbon nano-tube dressing agent; The preparation method of this dressing agent is the carboxylated multi-walled carbon nano-tubes that 1mg is crossed through nitric acid treatment, joins the N of 10ml, and in the dinethylformamide, sonicated makes its even dispersion half an hour, obtains the black mixed solution of 0.1mg/mL, is dressing agent; The above-mentioned finely dispersed dressing agent of 10 μ l dripped be coated on the glass-carbon electrode matrix surface that cleans up, with infrared lamp oven dry 1 hour, behind distilled water flushing, promptly get again and test required carboxylic carbon nano-tube modified electrode subsequently;
B, make the typical curve of nitrophenols isomerism body measurement:
(1) in electrolytic cell, as working electrode, contrast electrode is that saturated calomel electrode, auxiliary electrode are the platinized platinum electrode with the carboxylic carbon nano-tube modified electrode; Experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Current potential 0.4～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; With m-nitrophenol, the concentration of its phenol of nitre is separately fixed at 4 * 10
-4Mol/L, and the concentration of change ortho-nitrophenol, along with the increase of ortho-nitrophenol concentration, reduction peak current increases, and gets ortho-nitrophenol linear relationship curve I
P=0.9306C+0.6479, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9964; Electric current I
PUnit be μ A;
(2) in electrolytic cell, as working electrode, contrast electrode is a saturated calomel electrode with the carboxylic carbon nano-tube modified electrode, and auxiliary electrode is the platinized platinum electrode; Experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Current potential 0.4～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and carrying out cyclic voltammetry scan two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; The concentration of ortho-nitrophenol, paranitrophenol is separately fixed at 4 * 10
-4Mol/L, and the concentration of change m-nitrophenol, along with the increase of m-nitrophenol concentration, reduction peak current increases, and gets m-nitrophenol linear relationship curve I
P=0.5976C+2.4071, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9972; Electric current I
PUnit be μ A;
(3) separate in the pond at electrode, as working electrode, contrast electrode is a saturated calomel electrode with the carboxylic carbon nano-tube modified electrode, and auxiliary electrode is the platinized platinum electrode, experiment is carried out on CHI660B galvanochemistry comprehensive tester, and its attached software for calculation is made for collection of experiment data and processing; Be 0.4 at current potential～-electrode contained in the 0.9V scope in the solution of ortho-nitrophenol, m-nitrophenol, paranitrophenol and following collection volt-ampere scanning two circles with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; The concentration of ortho-nitrophenol, m-nitrophenol is separately fixed at 4 * 10
-4Mol/L, and the concentration of change paranitrophenol, along with the increase of paranitrophenol concentration, reduction peak current increases, and gets paranitrophenol linear relationship curve I
P=0.6202C+0.4630, C are concentration, and unit is 10
-4Mol/L, linearly dependent coefficient r=0.9965; Electric current I
PUnit be μ A;
C, its phenol isomers mixed solution sample of nitre is measured:
In conjunction with above-mentioned typical curve, the nitrophenols isomers mixed solution sample of unknown concentration is measured, calculate the concentration of each isomeride; Ortho-nitrophenol, m-nitrophenol, paranitrophenol three component mixed solutions with unknown concentration are placed in the electrolytic cell, and as working electrode, contrast electrode is that saturated calomel electrode, auxiliary electrode are the platinized platinum electrode with the carboxylic carbon nano-tube modified electrode; Test is carried out on CHI660B galvanochemistry comprehensive tester, and its attached computer software is made for collection of experiment data and processing; Be 0.4 at current potential～-electrode being contained in the 0.9V scope and carrying out cyclic voltammetry scan two circles in the solution of ortho-nitrophenol, a nitro, paranitrophenol with activated electrode, carry out linear sweep afterwards, sweep velocity is 50mV/S; Record the I of different isomerss respectively at different characteristic voltage belt place
PValue; With measured I
PIn the typical curve equation of the above-mentioned gained of value difference substitution, calculate ortho-nitrophenol, m-nitrophenol, paranitrophenol concentration separately.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101963593B (en) * | 2010-09-14 | 2013-08-28 | 济南大学 | Beta-CD-SBA15 modified electrode and method for measuring nitrophenol isomerides |
| CN101949880B (en) * | 2010-09-14 | 2013-01-02 | 济南大学 | Functionalized mesoporous material modified electrode and method for measuring benzenediol isomerides |
| CN102128865A (en) * | 2010-11-28 | 2011-07-20 | 上海大学 | Method for detecting phenol compounds by using horseradish peroxidase-modified electrode |
| CN103926302A (en) * | 2014-04-25 | 2014-07-16 | 黑龙江大学 | Method for determining p-nitrophenol in water system by taking graphene-loaded nano-nickel as electrode |
| CN104280432B (en) * | 2014-10-10 | 2015-04-29 | 天津出入境检验检疫局工业产品安全技术中心 | Quantitative detection system for trace nitrophenol explosives |
| CN110865116A (en) * | 2019-11-25 | 2020-03-06 | 江西科技师范大学 | Electrochemical nano enzyme sensor for detecting 5-nitroguaiacol sodium |
| CN110988072B (en) * | 2019-12-20 | 2021-12-24 | 肇庆学院 | Single-walled carbon nanohorn @ hydroxylated multi-walled carbon nanotube electrochemical sensor and application thereof in detection of nitenpyram |
| CN114894878A (en) * | 2022-05-24 | 2022-08-12 | 福州大学 | Method for measuring concentration of inhibitor in acidic copper plating solution |
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