CN103196985A - Method for measuring p-nitrophenol in water system - Google Patents
Method for measuring p-nitrophenol in water system Download PDFInfo
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- CN103196985A CN103196985A CN2013101500221A CN201310150022A CN103196985A CN 103196985 A CN103196985 A CN 103196985A CN 2013101500221 A CN2013101500221 A CN 2013101500221A CN 201310150022 A CN201310150022 A CN 201310150022A CN 103196985 A CN103196985 A CN 103196985A
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Abstract
The invention discloses a method for measuring p-nitrophenol in a water system, relates to a method for measuring p-nitrophenol, and aims at solving the problems that the limit of detection is high, the operation is complex, the instruments are expensive and the cost is high in the conventional method for measuring the p-nitrophenol. The method comprises the following steps of: 1, preparing a purified carbon electrode, 1, preparing a modified carbon electrode, 3, preparing an alkali p-nitrophenol solution, and 4, measuring. The method adopts the electrochemical oxidation reduction of the p-nitrophenol on an electrode modified by a graphene/nano copper composite material to measure the p-nitrophenol in the water system, the carbon electrode has good multi-circulation stability in the process of measuring the p-nitrophenol, and the electrode material can be repeatedly reused with low consumption. The method is applied to measurement on p-nitrophenol in the water system.
Description
Technical field
The present invention relates to the assay method of p-nitrophenol.
Background technology
P-nitrophenol is widely used in fine chemistry industry industries such as explosive, dyestuff, medicine intermediate as important chemical material, but it has strong carcinogenesis, it is a kind of biodegradable material that is difficult to, application widely causes producing a large amount of contaminated wastewater environment, and people have carried out a large amount of research to its assay method.For example, spectrophotometer method, the detection limit for height of this method; Chromatography, the expensive cost of complex operation and instrument is too high, makes the mensuration of p-nitrophenol in the aqueous systems can not widespread usage.
Summary of the invention
There is the detection limit for height in the method that the present invention will solve present mensuration p-nitrophenol, the high problem of the expensive cost of complex operation and instrument, and the assay method of p-nitrophenol in a kind of aqueous systems that provides.
The assay method of p-nitrophenol in a kind of aqueous systems, specifically finish according to following steps:
One, carbon electrode is immersed in the red fuming nitric acid (RFNA), keep 20h～30h, polish off the surface that thickness is 1mm～1.2mm with abrasive paper for metallograph again, the aluminium oxide mud of putting into particle diameter then and be 0.05 μ m is polished to smooth surface, controlling ultrasonic frequency under the normal temperature condition then in distilled water is 40KHz～60KHz, keeps 10min～20min, replaces supersound washing with acetone and absolute ethyl alcohol again, drying obtains the carbon electrode of purifying;
Two, Graphene/nanometer carbon/carbon-copper composite material being evenly spread to volumetric concentration is in 5%～6% the Nafion solution, obtain dispersion liquid, get 0.05mL～0.1mL dispersion liquid and be added to the carbon electrodes of the purifying that step 1 obtains, vacuum drying 3h～4h under normal temperature condition obtains modified graphite electrode again;
Three, NaOH is added in the p-nitrophenyl phenol solution, obtain alkaline p-nitrophenyl phenol solution;
Four, the alkaline p-nitrophenyl phenol solution that step 3 is obtained is packed in the electrolytic cell, the modified graphite electrode that step 2 is obtained, mercuric oxide electrode and platinum electrode insert in the p-nitrophenyl phenol solution again, feed pure nitrogen gas then, keep 30min～40min, hermetic electrolyte pond again, connect electrochemical workstation, setting sweep interval is-0.6V～1.2V, sweep speed is 100mV/s, measure electric current, finish the assay method of p-nitrophenol in the aqueous systems, wherein modified graphite electrode is working electrode, mercuric oxide electrode is contrast electrode, and platinum electrode is to electrode.
The present invention utilizes nitro-phenolic compound electrochemical redox in electrolytic cell to have the rule of certain conversion, adopts liquid phase reduction, and Graphene/nanometer carbon/carbon-copper composite material as electrode material, is measured p-nitrophenol in the aqueous systems.The present invention has method and has simply, quick, characteristics such as detection limit is low.
The invention has the beneficial effects as follows:
1, to measure in the water quality method of p-nitrophenol simple in the present invention, operation easily, weak point consuming time, detection limit lower (p-nitrophenol concentration is lower than 0.01mol/L and also can detects).
2, the present invention utilizes p-nitrophenol in the electrochemical redox behavior determination aqueous systems of p-nitrophenol on the electrode of Graphene/nanometer carbon/carbon-copper composite material modified, have good many cyclical stabilities in the process of this carbon electrode mensuration p-nitrophenol, this electrode material can be recycled, low-loss.
The present invention is used for measuring the aqueous systems p-nitrophenol.
Description of drawings
Fig. 1 is the redox curve map that embodiment one measures p-nitrophenol;
Fig. 2 follows the redox curve map for embodiment one measures many groups of p-nitrophenol, and wherein curve 1 be cyclic oxidation first time virgin curve also;
Fig. 3 embodiment two measures the redox curve of p-nitrophenol.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the assay method of p-nitrophenol in a kind of aqueous systems of present embodiment, specifically finish according to following steps:
One, carbon electrode is immersed in the red fuming nitric acid (RFNA), keep 20h～30h, polish off the surface that thickness is 1mm～1.2mm with abrasive paper for metallograph again, the aluminium oxide mud of putting into particle diameter then and be 0.05 μ m is polished to smooth surface, controlling ultrasonic frequency under the normal temperature condition then in distilled water is 40KHz～60KHz, keeps 10min～20min, replaces supersound washing with acetone and absolute ethyl alcohol again, drying obtains the carbon electrode of purifying;
Two, Graphene/nanometer carbon/carbon-copper composite material being evenly spread to volumetric concentration is in 5%～6% the Nafion solution, obtain dispersion liquid, get 0.05mL～0.1mL dispersion liquid and be added to the carbon electrodes of the purifying that step 1 obtains, vacuum drying 3h～4h under normal temperature condition obtains modified graphite electrode again;
Three, NaOH is added in the p-nitrophenyl phenol solution, obtain alkaline p-nitrophenyl phenol solution;
Four, the alkaline p-nitrophenyl phenol solution that step 3 is obtained is packed in the electrolytic cell, the modified graphite electrode that step 2 is obtained, mercuric oxide electrode and platinum electrode insert in the p-nitrophenyl phenol solution again, feed pure nitrogen gas then, keep 30min～40min, hermetic electrolyte pond again, connect electrochemical workstation, setting sweep interval is-0.6V～1.2V, sweep speed is 100mV/s, measure electric current, finish the assay method of p-nitrophenol in the aqueous systems, wherein modified graphite electrode is working electrode, mercuric oxide electrode is contrast electrode, and platinum electrode is to electrode.
The method that present embodiment is measured p-nitrophenol in the water quality is simple, operation easily, and weak point consuming time, detection limit is lower.
Present embodiment is utilized p-nitrophenol in the electrochemical redox behavior determination aqueous systems of p-nitrophenol on the electrode of Graphene/nanometer carbon/carbon-copper composite material modified, have good many cyclical stabilities in the process of this carbon electrode mensuration p-nitrophenol, this electrode material can be recycled, low-loss.
Embodiment two: what present embodiment and embodiment one were different is: the control ultrasonic frequency is 45KHz～55KHz in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the mass ratio of nanometer copper and Graphene is 2.5～5: 1 in Graphene in the step 2/nanometer carbon/carbon-copper composite material.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: the quality of Graphene in the step 2/nanometer carbon/carbon-copper composite material and the volume ratio of Nafion solution are 0.05g: 1.0mL.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: the concentration of NaOH is 0.1mol/L～2.0mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.Other is identical with embodiment one.
Embodiment six: what present embodiment was different with one of embodiment one to five is: the concentration of NaOH is 0.2mol/L～1.8mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the concentration of NaOH is 0.5mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to six is: the concentration of NaOH is 1.5mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.Other is identical with one of embodiment one to six.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
The assay method of p-nitrophenol in a kind of aqueous systems of present embodiment, specifically finish according to following steps:
One, carbon electrode is immersed in the red fuming nitric acid (RFNA), keep 24h, polish off the surface that thickness is 1mm with abrasive paper for metallograph again, the aluminium oxide mud of putting into particle diameter then and be 0.05 μ m is polished to smooth surface, controlling ultrasonic frequency under the normal temperature condition then in distilled water is 50KHz, keeps 10min, replaces supersound washing with acetone and absolute ethyl alcohol again, drying obtains the carbon electrode of purifying;
Two, Graphene/nanometer carbon/carbon-copper composite material being evenly spread to volumetric concentration is in 5% the Nafion solution, obtain dispersion liquid, get the 0.1mL dispersion liquid and be added to the carbon electrodes of the purifying that step 1 obtains, vacuum drying 3h under normal temperature condition obtains modified graphite electrode again;
Three, NaOH is added in the p-nitrophenyl phenol solution, obtain alkaline p-nitrophenyl phenol solution;
Four, the alkaline p-nitrophenyl phenol solution that step 3 is obtained is packed in the electrolytic cell, the modified graphite electrode that step 2 is obtained, mercuric oxide electrode and platinum electrode insert in the p-nitrophenyl phenol solution again, feed pure nitrogen gas then, keep 30min, hermetic electrolyte pond again, connect electrochemical workstation, setting sweep interval is-0.6V～1.2V, sweep speed is 100mV/s, measure electric current, finish the assay method of p-nitrophenol in the aqueous systems, wherein modified graphite electrode is working electrode, mercuric oxide electrode is contrast electrode, and platinum electrode is to electrode.
The concentration of p-nitrophenyl phenol solution is 0.01mol/L in the present embodiment, and the mass ratio of nanometer copper and Graphene is 5: 1 in Graphene in the step 2/nanometer carbon/carbon-copper composite material, and the concentration of NaOH is 0.5mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.
The redox curve map of present embodiment mensuration p-nitrophenol as shown in Figure 1; Present embodiment is measured many groups of p-nitrophenol and is followed the redox curve map as shown in Figure 2, and wherein curve 1 be cyclic oxidation first time virgin curve also;
Embodiment two:
The assay method of p-nitrophenol in a kind of aqueous systems of present embodiment, specifically finish according to following steps:
One, carbon electrode is immersed in the red fuming nitric acid (RFNA), keep 24h, polish off the surface that thickness is 1mm with abrasive paper for metallograph again, the aluminium oxide mud of putting into particle diameter then and be 0.05 μ m is polished to smooth surface, controlling ultrasonic frequency under the normal temperature condition then in distilled water is 50KHz, keeps 10min, replaces supersound washing with acetone and absolute ethyl alcohol again, drying obtains the carbon electrode of purifying;
Two, Graphene/nanometer carbon/carbon-copper composite material being evenly spread to volumetric concentration is in 5% the Nafion solution, obtain dispersion liquid, get the 0.1mL dispersion liquid and be added to the carbon electrodes of the purifying that step 1 obtains, vacuum drying 3h under normal temperature condition obtains modified graphite electrode again;
Three, NaOH is added in the p-nitrophenyl phenol solution, obtain alkaline p-nitrophenyl phenol solution;
Four, the alkaline p-nitrophenyl phenol solution that step 3 is obtained is packed in the electrolytic cell, the modified graphite electrode that step 2 is obtained, mercuric oxide electrode and platinum electrode insert in the p-nitrophenyl phenol solution again, feed pure nitrogen gas then, keep 30min, hermetic electrolyte pond again, connect electrochemical workstation, setting sweep interval is-0.6V～1.2V, sweep speed is 100mV/s, measure electric current, finish the assay method of p-nitrophenol in the aqueous systems, wherein modified graphite electrode is working electrode, mercuric oxide electrode is contrast electrode, and platinum electrode is to electrode.
The concentration of p-nitrophenyl phenol solution is 0.01mol/L in the present embodiment, and the mass ratio of nanometer copper and Graphene is 5: 1 in Graphene in the step 2/nanometer carbon/carbon-copper composite material, and the concentration of NaOH is 1.5mol/L in the step 3 neutral and alkali p-nitrophenyl phenol solution.
The redox curve map of present embodiment mensuration p-nitrophenol as shown in Figure 3.
As can be seen from the figure the present invention utilizes p-nitrophenol in the electrochemical redox behavior determination aqueous systems of p-nitrophenol on the electrode of Graphene/nanometer carbon/carbon-copper composite material modified, have good many cyclical stabilities in the process of this carbon electrode mensuration p-nitrophenol, this electrode material can be recycled, low-loss.
Claims (8)
1. the assay method of p-nitrophenol in the aqueous systems is characterized in that the assay method of p-nitrophenol in a kind of aqueous systems, specifically finishes according to following steps:
One, carbon electrode is immersed in the red fuming nitric acid (RFNA), keep 20h～30h, polish off the surface that thickness is 1mm～1.2mm with abrasive paper for metallograph again, the aluminium oxide mud of putting into particle diameter then and be 0.05 μ m is polished to smooth surface, controlling ultrasonic frequency under the normal temperature condition then in distilled water is 40KHz～60KHz, keeps 10min～20min, replaces supersound washing with acetone and absolute ethyl alcohol again, drying obtains the carbon electrode of purifying;
Two, Graphene/nanometer carbon/carbon-copper composite material being evenly spread to volumetric concentration is in 5%～6% the Nafion solution, obtain dispersion liquid, get 0.05mL～0.1mL dispersion liquid and be added to the carbon electrodes of the purifying that step 1 obtains, vacuum drying 3h～4h under normal temperature condition obtains modified graphite electrode again;
Three, NaOH is added in the p-nitrophenyl phenol solution, obtain alkaline p-nitrophenyl phenol solution;
Four, the alkaline p-nitrophenyl phenol solution that step 3 is obtained is packed in the electrolytic cell, the modified graphite electrode that step 2 is obtained, mercuric oxide electrode and platinum electrode insert in the p-nitrophenyl phenol solution again, feed pure nitrogen gas then, keep 30min～40min, hermetic electrolyte pond again, connect electrochemical workstation, setting sweep interval is-0.6V～1.2V, sweep speed is 100mV/s, measure electric current, finish the assay method of p-nitrophenol in the aqueous systems, wherein modified graphite electrode is working electrode, mercuric oxide electrode is contrast electrode, and platinum electrode is to electrode.
2. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 1 is characterized in that the control ultrasonic frequency is 45KHz～55KHz in the step 1.
3. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 1 is characterized in that the mass ratio of nanometer copper and Graphene is 2.5～5: 1 in Graphene in the step 2/nanometer carbon/carbon-copper composite material.
4. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 1 is characterized in that the quality of Graphene in the step 2/nanometer carbon/carbon-copper composite material and the volume ratio of Nafion solution are 0.05g: 1.0mL.
5. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 1 is characterized in that the concentration of NaOH in the step 3 neutral and alkali p-nitrophenyl phenol solution is 0.1mol/L～2.0mol/L.
6. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 5 is characterized in that the concentration of NaOH in the step 3 neutral and alkali p-nitrophenyl phenol solution is 0.2mol/L～1.8mol/L.
7. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 6 is characterized in that the concentration of NaOH in the step 3 neutral and alkali p-nitrophenyl phenol solution is 0.5mol/L.
8. the assay method of p-nitrophenol in a kind of aqueous systems according to claim 6 is characterized in that the concentration of NaOH in the step 3 neutral and alkali p-nitrophenyl phenol solution is 1.5mol/L.
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Cited By (11)
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| CN103913504A (en) * | 2014-04-25 | 2014-07-09 | 黑龙江大学 | Method for measuring p-nitrophenol in water system by taking nano nickel supported carbon nanotube as 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 |
| CN104034772A (en) * | 2014-06-18 | 2014-09-10 | 许昌学院 | Preparation method and application of modification electrode |
| CN104090006A (en) * | 2014-07-25 | 2014-10-08 | 南通大学 | Polycarbazole/nitrogen-doped graphene modified electrode, preparation method and application of polycarbazole/nitrogen-doped graphene modified electrode |
| CN104267081A (en) * | 2014-10-10 | 2015-01-07 | 天津出入境检验检疫局工业产品安全技术中心 | Quantitative detection method of trace nitrophenol explosive |
| CN104458881A (en) * | 2014-11-10 | 2015-03-25 | 天津出入境检验检疫局工业产品安全技术中心 | Novel electrode material for detecting p-nitrophenol through modified electrode, preparation method of electrode material and detection of p-nitrophenol |
| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
| CN107290416A (en) * | 2017-06-02 | 2017-10-24 | 华中科技大学 | Detect light-initiated self energizing electrochemical sensor and its application of 4 nitrophenols |
| CN109613098A (en) * | 2018-07-13 | 2019-04-12 | 湖北民族学院 | The preparation method and application of automatically cleaning electrochemical sensor under a kind of visible light |
| CN110376267A (en) * | 2019-08-15 | 2019-10-25 | 蚌埠学院 | A method of detection p-nitrophenol |
| CN111289594A (en) * | 2020-03-27 | 2020-06-16 | 中南大学 | Lanthanum hydroxide-oxidized multi-walled carbon nanotube modified glassy carbon electrode and application thereof |
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Cited By (15)
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| CN103913504A (en) * | 2014-04-25 | 2014-07-09 | 黑龙江大学 | Method for measuring p-nitrophenol in water system by taking nano nickel supported carbon nanotube as 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 |
| CN104034772A (en) * | 2014-06-18 | 2014-09-10 | 许昌学院 | Preparation method and application of modification electrode |
| CN105548309A (en) * | 2014-07-25 | 2016-05-04 | 南通大学 | Application of polycarbazole / nitrogen-doped graphene modified electrode |
| CN104090006A (en) * | 2014-07-25 | 2014-10-08 | 南通大学 | Polycarbazole/nitrogen-doped graphene modified electrode, preparation method and application of polycarbazole/nitrogen-doped graphene modified electrode |
| CN105548309B (en) * | 2014-07-25 | 2017-12-22 | 南通大学 | The purposes of polycarbazole/nitrogen-doped graphene modified electrode |
| CN104267081A (en) * | 2014-10-10 | 2015-01-07 | 天津出入境检验检疫局工业产品安全技术中心 | Quantitative detection method of trace nitrophenol explosive |
| CN104267081B (en) * | 2014-10-10 | 2015-06-03 | 天津出入境检验检疫局工业产品安全技术中心 | Quantitative detection method of trace nitrophenol explosive |
| CN104458881A (en) * | 2014-11-10 | 2015-03-25 | 天津出入境检验检疫局工业产品安全技术中心 | Novel electrode material for detecting p-nitrophenol through modified electrode, preparation method of electrode material and detection of p-nitrophenol |
| CN104458881B (en) * | 2014-11-10 | 2015-10-28 | 天津出入境检验检疫局工业产品安全技术中心 | Modified electrode detects the new electrode materials of p-nitrophenol, preparation method and the detection to p-nitrophenol thereof |
| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
| CN107290416A (en) * | 2017-06-02 | 2017-10-24 | 华中科技大学 | Detect light-initiated self energizing electrochemical sensor and its application of 4 nitrophenols |
| CN109613098A (en) * | 2018-07-13 | 2019-04-12 | 湖北民族学院 | The preparation method and application of automatically cleaning electrochemical sensor under a kind of visible light |
| CN110376267A (en) * | 2019-08-15 | 2019-10-25 | 蚌埠学院 | A method of detection p-nitrophenol |
| CN111289594A (en) * | 2020-03-27 | 2020-06-16 | 中南大学 | Lanthanum hydroxide-oxidized multi-walled carbon nanotube modified glassy carbon electrode and application thereof |
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Application publication date: 20130710 |