CN110376267A - A method of detection p-nitrophenol - Google Patents
A method of detection p-nitrophenol Download PDFInfo
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- CN110376267A CN110376267A CN201910751831.5A CN201910751831A CN110376267A CN 110376267 A CN110376267 A CN 110376267A CN 201910751831 A CN201910751831 A CN 201910751831A CN 110376267 A CN110376267 A CN 110376267A
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Abstract
The invention discloses a kind of methods for detecting p-nitrophenol, are working electrode by glass-carbon electrode, and saturated calomel electrode is reference electrode, and platinum filament is to be put into the phosphate buffer solution containing pH=6.0,1.00 × 10 to the three-electrode system of electrode‑4The Cu of mol/L2+With 1.00 × 10‑3In the Pidolidone polymeric solution of mol/L, in -0.4~2.6V potential range, 20s is stood, with distilled water flushing electrode surface, is dried with the scanning speed of 140mV/s using 12 circle of cyclic voltammetry scanning；With modified electrode obtained above, in the potential range of -1.1~0V, the time of repose of 44s under the scanning speed of 300mV/s, uses p-nitrophenol of the cyclic voltammetry using the phosphate buffer solution of pH=2.0 as supporting electrolyte.The result shows that the reduction peak current of p-nitrophenol and its concentration are 5.00 × 10‑6~8.00 × 10‑4It is in good linear relationship within the scope of mol/L, detection is limited to 3.00 × 10‑6mol/L.The present invention can be used for the quick detection of p-nitrophenol, have the features such as accuracy is high, sensitivity is big, and selectivity is good, easy to operate.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a method of detection p-nitrophenol.
Background technique
P-nitrophenol is a kind of organic synthesis raw material, can be used as medicine intermediate, prepares phenacetin, flutters hot breath
The analgesic-antipyretic such as pain；As pesticide intermediate, the organophosphorus insecticides such as pesticide 1605, parathion and parathion-methyl are prepared；
As dyestuff and photosensitive material intermediate, the dyestuffs and photographic developer etc. such as sulphur grass-green, reversion indigo plant are prepared.In addition, right
Nitrophenol is also used as mould inhibitor, monochromatic pH indicator and the standard solution of titrimetry of leather etc..So
P-nitrophenol has consequence and effect in industrial production and life.But p-nitrophenol is being widely used
While also bring pollution and harm to environment and human body, be mainly reflected in the following aspects: p-nitrophenol is heated meeting
Decompose to give off toxic nitrogen oxide flue gas；There is strong impulse effect to skin, can be absorbed by skin and respiratory tract, when serious
It makes one to have difficulty in breathing；It can cause methemoglobinemia, increase body temperature, is larger to the injury of liver kidney；It can make nervous centralis
Excitement is suppressed, and is played the role of carcinogenic；P-nitrophenol is a kind of toxic pollutant, p-nitrophenol main source in water
In chemical industry, the production waste water of pharmaceutical industry.It is reported that the p-nitrophenol containing 1mg/L will be given in drinking water or other food
The health even life of people poses a serious threat.So accurately detecting that the content of p-nitrophenol in solution gives birth to raising
The safety of environment living and guarantee people are of great significance.
At present detection solution in content of p-nitrophenol common method have spectrophotometry, fluorimetry, chromatography,
Titration and capillary electrophoresis etc..But these method reagent consumptions are big, and detection limit is higher, and consuming time is long, uses instrument
Device is expensive, and analysis cost is high, is not able to satisfy the requirement that scene is quick, accurately detects.Therefore, it is quite necessary to establish a kind of operation
Simply, fast, at low cost, high sensitivity the method for finding speed.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide it is a kind of detect p-nitrophenol method,
The detection method is selectively good, and high sensitivity, reproducibility is excellent, and method is reliable, so as to more simple and efficient detection to nitre
Base phenol provides faster and better measuring means for industrial production, life and environmental monitoring.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A method of detection p-nitrophenol, the various parameters that this method is related to are optimal values, rather than particular value,
Specific step is as follows:
S1: it prepares Copper-cladding Aluminum Bar L-glutamic acid modified electrode: being working electrode by glass-carbon electrode, saturated calomel electrode is ginseng
Than electrode, platinum filament is to be put into the phosphate buffer solution containing pH=6.0,1.00 × 10 to the three-electrode system of electrode-4mol/L
Cu2+With 1.00 × 10-3In the polymeric solution of the Pidolidone of mol/L, in -0.4~2.6V potential range, 20s is stood,
It, with distilled water flushing electrode surface, is arrived after drying with the scanning speed of 140mV/s using 12 circle of cyclic voltammetry scanning
The Copper-cladding Aluminum Bar L-glutamic acid modified electrode prepared under optimum condition；
S2: measurement p-nitrophenol: with modified electrode obtained above, in the potential range of -1.1~0V, the standing of 44s
Time under the scanning speed of 300mV/s, uses cyclic voltammetry using the phosphate buffer solution of pH=2.0 as supporting
The p-nitrophenyl phenol solution of electrolyte.
The phosphate buffer solution is by Na3PO4、NaH2PO4、Na2HPO4Composition or K3PO4、KH2PO4、K2HPO4Group
At each material concentration is 0.1moL/L, H3PO4Adjusting pH is 2.0 or NaOH adjusting pH is 6.0.
Testing result show p-nitrophenol reduction peak current and its concentration 5.00 × 10-6~8.00 × 10- 4It is in good linear relationship within the scope of mol/L, detection is limited to 3.00 × 10-6mol/L。
Beneficial effects of the present invention:
1) Copper-cladding Aluminum Bar L-glutamic acid modified electrode of the present invention has the wider range of linearity and lower detection limit, is sweeping
It retouches in current potential -1.1~section 0V, 1.00 × 10-4Mol/L p-nitrophenol occurs on Copper-cladding Aluminum Bar L-glutamic acid modified electrode
Strong reduction peak, spike potential Epa=-0.672V, peak current Ipc=-6.461 × 10-4A, illustrate copper and Pidolidone polymerization after to right
Nitrophenol has stronger adsorption capacity and preferable accumulation ability, greatly strengthens the responding ability to p-nitrophenol, spirit
Sensitivity and selectivity are significantly improved, and detection effect is more preferable.
2) the method for the present invention is able to achieve the on-site test of p-nitrophenol, and selectivity is good, and high sensitivity, reproducibility is excellent, side
Method is reliable, and finding speed is fast, low in cost, and amount of reagent is small, and required detection device is simple and convenient, so as to more simple and efficient
Detection p-nitrophenol, faster and better measuring means is provided for industrial production, life and environmental monitoring.
Detailed description of the invention
Fig. 1 is the cyclic voltammogram of the Copper-cladding Aluminum Bar L-glutamic acid modified electrode prepared under optimum condition；
Fig. 2 is 1.00 × 10-4Cyclic voltammetry curve of the mol/L p-nitrophenol on Different electrodes.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
Embodiment 1 prepares Copper-cladding Aluminum Bar L-glutamic acid modified electrode
It is working electrode by glass-carbon electrode, saturated calomel electrode is reference electrode, and platinum filament is the three-electrode system to electrode
Being put into the phosphate buffer solution containing pH=6.0, (phosphate buffer solution is by Na3PO4、NaH2PO4、Na2HPO4Composition,
NaOH adjust pH be 6.0), 1.00 × 10-4The Cu of mol/L2+With 1.00 × 10-3In the polymeric solution of the Pidolidone of mol/L,
In -0.4~2.6V potential range, 20s is stood, is used with the scanning speed of 140mV/s using 12 circle of cyclic voltammetry scanning
Distilled water flushing electrode surface, to get to the Copper-cladding Aluminum Bar L-glutamic acid modified electrode prepared under optimum condition after drying.
Fig. 1 is cyclic voltammetric peace curve (1~12 expression that Copper-cladding Aluminum Bar L-glutamic acid modified electrode is prepared under optimum condition
1~12 circle of scanning): it is seen that in the first lap of polymerization, there is a copper peak in 0.1V or so；As number is enclosed in scanning
Increase, electric current is gradually steady, and polymerization curve tends to be overlapped, and illustrates the progress with polymerization reaction, the polymer thin of electrode surface
Film is gradually complete, and polymerization, deposition velocity slow down, and tends towards stability.
Embodiment 2 directly measures 1.00 × 10-4Mol/L p-nitrophenol
The Copper-cladding Aluminum Bar L-glutamic acid modified electrode that will be prepared by embodiment 1, the phosphate-buffered for being put into pH=2.0 are molten
(phosphate buffer solution is by Na in liquid3PO4、NaH2PO4、Na2HPO4Composition, each material concentration is 0.1moL/L, H3PO4It adjusts
Saving pH is 2.0), in -1.1~0V potential range, to use cyclic voltammetry with 300mV/ after standing 44s as supporting electrolyte
The scanning speed of s to contain 1.00 × 10-4The p-nitrophenyl phenol solution of mol/L is scanned measurement, then measures respectively a series of
P-nitrophenyl phenol solution containing known concentration draws standard curve.
According to standard curve, acquiring p-nitrophenol concentration using reduction peak current is 1.008 × 10-4Mol/L is and true
The relative standard deviation of value is 0.8%.
The principle for detecting p-nitrophenol is as follows:
Fig. 2 is 1.00 × 10-4Cyclic voltammetry curve of the p-nitrophenol of mol/L on Different electrodes: can be with from figure
Find out, in scanning current potential -1.1~section 0V, p-nitrophenol not appearance on glass-carbon electrode (curve 1) shows glass carbon electricity
Extremely there is no catalytic action to p-nitrophenol；Occur apparent reduction peak, peak electricity on Pidolidone modified electrode (curve 2)
Position Epa=-0.617V, peak current Ipc=-3.747 × 10-4A shows that Pidolidone modified electrode has preferably p-nitrophenol
Response；Occur stronger reduction peak, spike potential E on Copper-cladding Aluminum Bar L-glutamic acid modified electrode (curve 3)pa=-0.672V,
Peak current Ipc=-6.461 × 10-4A shows that peak shape is more preferable, and peak current is bigger, i.e., to nitro after copper and Pidolidone polymerization
Phenol has stronger adsorption capacity and preferable accumulation ability, greatly strengthens the responding ability to p-nitrophenol, sensitivity
It is significantly improved.Therefore, Copper-cladding Aluminum Bar L-glutamic acid modified electrode is higher to the selectivity of p-nitrophenol and sensitivity, inspection
It is more preferable to survey effect.
The p-nitrophenol of 3 Standard Addition Method for Determination unknown concentration of embodiment
According to 2 condition of embodiment, the Copper-cladding Aluminum Bar L-glutamic acid modified electrode prepared by embodiment 1 is placed in containing not
Know in concentration p-nitrophenyl phenol solution and measure, 1.00 × 10 are added in the solution-4After mol/L p-nitrophenol, measure again.
Test result shows that the concentration of p-nitrophenol in unknown sample is 2.42 × 10-5Mol/L, standard addition method are surveyed
Obtaining the rate of recovery is 99.23%.
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.
Claims (3)
1. a kind of method for detecting p-nitrophenol, it is characterised in that: Copper-cladding Aluminum Bar L-glutamic acid modified electrode is used, in pH=
2.0 phosphate buffer solution, the potential range of -1.1~0V, the time of repose of 44s, under the scanning speed of 300mV/s, identification
With detection p-nitrophenol；
The Copper-cladding Aluminum Bar L-glutamic acid modified electrode preparation method: using glass-carbon electrode as working electrode, saturated calomel electrode is
Reference electrode, platinum filament be to electrode construct three-electrode system, and be put into the phosphate buffer solution containing pH=6.0,1.00 ×
10-4The Cu of mol/L2+With 1.00 × 10-3It is quiet in -0.4~2.6V potential range in the Pidolidone polymeric solution of mol/L
20s is set, with the scanning speed of 140mV/s, using 12 circle of cyclic voltammetry scanning, with distilled water flushing electrode surface, after drying
Obtain Copper-cladding Aluminum Bar L-glutamic acid modified electrode.
2. a kind of method for detecting p-nitrophenol according to claim 1, which is characterized in that the phosphate-buffered is molten
Liquid is by Na3PO4、NaH2PO4、Na2HPO4Composition or K3PO4、KH2PO4、K2HPO4Composition, each material concentration is 0.1moL/L,
H3PO4Adjusting pH is 2.0 or NaOH adjusting pH is 6.0.
3. a kind of method for detecting p-nitrophenol according to claim 1, which is characterized in that the reduction of p-nitrophenol
Peak current and its concentration are 5.00 × 10-6~8.00 × 10-4It is in good linear relationship within the scope of mol/L, detection is limited to 3.00
×10-6mol/L。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112903776A (en) * | 2021-01-27 | 2021-06-04 | 齐鲁工业大学 | Preparation of spirobifluorenyl microporous polymer membrane modified electrode, obtained product and application |
| CN113624700A (en) * | 2021-07-27 | 2021-11-09 | 北京农业质量标准与检测技术研究中心 | Method for detecting p-nitrophenol |
Citations (2)
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| CN103196985A (en) * | 2013-04-26 | 2013-07-10 | 黑龙江大学 | Method for measuring p-nitrophenol in water system |
| CN107643331A (en) * | 2017-09-06 | 2018-01-30 | 山西大学 | A kind of electrode face finish material and its preparation method and application |
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| CN103196985A (en) * | 2013-04-26 | 2013-07-10 | 黑龙江大学 | Method for measuring p-nitrophenol in water system |
| CN107643331A (en) * | 2017-09-06 | 2018-01-30 | 山西大学 | A kind of electrode face finish material and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112903776A (en) * | 2021-01-27 | 2021-06-04 | 齐鲁工业大学 | Preparation of spirobifluorenyl microporous polymer membrane modified electrode, obtained product and application |
| CN113624700A (en) * | 2021-07-27 | 2021-11-09 | 北京农业质量标准与检测技术研究中心 | Method for detecting p-nitrophenol |
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