CN102507713A - Electrochemical stripping voltammetry for continuously measuring arsenic, stibonium and lead in mine groundwater - Google Patents
Electrochemical stripping voltammetry for continuously measuring arsenic, stibonium and lead in mine groundwater Download PDFInfo
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- CN102507713A CN102507713A CN2011103494851A CN201110349485A CN102507713A CN 102507713 A CN102507713 A CN 102507713A CN 2011103494851 A CN2011103494851 A CN 2011103494851A CN 201110349485 A CN201110349485 A CN 201110349485A CN 102507713 A CN102507713 A CN 102507713A
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Abstract
The invention discloses an electrochemical stripping voltammetry for continuously measuring arsenic, stibonium and lead in mine groundwater, which utilizes a gold electrode as a working electrode and measures the concentrations of arsenic, stibonium and lead in a test sample solution by an electrochemical method; the method comprises the following steps of: pre-treating the gold electrode, firstly polarizing the electrode, and activating the electrode in a circular voltammetry; varying the potential of the gold electrode toward a negative potential direction, simultaneously depositing arsenic and stibonium on the surface of the gold electrode under the same potential, and measuring the total concentration of arsenic and stibonium by potential dissolution; and then, changing the deposition potential, singly depositing the stibonium, measuring the stibonium concentration by the potential stripping, and obtaining the arsenic concentration according to a difference value; firstly depositing the arsenic and lead on the gold electrode under the same potential, scanning the gold electrode toward the positive potential direction, separating out the arsenic and lead electrically deposited on the surface of the gold electrode under different potentials, and respectively measuring the concentrations of the arsenic and lead. The method provided by the invention has the advantages of continuously measuring the concentrations of arsenic, stibonium and lead in the same solution in a convenient and sensitive manner.
Description
Technical field
The present invention relates to a kind of method of surveying arsenic in the water, antimony, lead content, especially to the tie-in method of mine arsenic from underwater, antimony, lead content.
Background technology
Heavy metal pollution is one of environmentally hazardous greatest problem.Arsenic, lead, antimony are the important analysis projects of environmental monitoring.Arsenic is a kind ofly to enter into human body through potable water and food easily, in human body, causes arsenic poisoning behind the savings, and a kind of extremely harmful element that can cause death.Arsenic generally is present in water body and the soil with sodium arsenite, arsenic trioxide, natrium arsenicum form at occurring in nature, and trivalent arsenic is stronger than pentavalent arsenic toxicity, and inorganic arsenic chemicals is stronger than organoarsenium compound toxicity.Lead is a kind of of quantity maximum in the heavy metal pollution, also is to one of the most serious metal of mankind's harm, can poison nervous system and hemopoietic system, causes spasm, hyponea, anaemia etc.Antimony can combine with sulfydryl in human body, and the activity of inhibition succinic oxidase etc. is destroyed ionic equilibrium in the cell, makes potassium deficiency in the cell, causes that internal metabolism is disorderly, causes multisystem, many organ injuries.Poisonous element as arsenic, lead, antimony, water pollution prevent that its content benchmark is below the 0.1ppm (100ppb) in the law regulation discharge water.For this reason, need a kind of easy and detection method that precision is good, can detect the concentration of arsenic, lead, antimony in discharge water and the mine water.The electrochemical method that detects arsenic, lead, antimony separately more has report, but in a kind of electrolyte solution, uses gold electrode METHOD FOR CONTINUOUS DETERMINATION arsenic, lead, antimony concentration also not to appear in the newspapers.
Summary of the invention
The purpose of this invention is to provide a kind of galvanochemistry stripping volt-ampere method that is used for mine arsenic from underwater, antimony and plumbous tie-in, this method can the easy arsenic of continuous detecting delicately, antimony and plumbous concentration.
For realizing above-mentioned purpose, the present invention takes following design proposal:
A kind of galvanochemistry stripping volt-ampere method that is used for mine arsenic from underwater, antimony and plumbous tie-in directly uses gold electrode to be working electrode, measures arsenic, antimony, lead concentration in the sample solution with electrochemical means, and it may further comprise the steps:
A) gold electrode is carried out pre-service, first polarized electrode is used the cyclic voltammetry activated electrode then;
B) adopted for two steps realized to the arsenic in the sample solution, antimony and plumbous tie-in:
One of them step is to the arsenic in the sample solution, antimony tie-in; The current potential of the gold electrode of above-mentioned steps in a) is changed to the negative potential direction; Letting arsenic, antimony be deposited on simultaneously on the above-mentioned gold electrode surfaces earlier under the identical current potential, the total concentration of arsenic and antimony is measured in the current potential stripping; And then the change sedimentation potential, depositing antimony separately, the concentration of antimony is surveyed in the current potential stripping, obtains the concentration of arsenic according to difference;
Another step is to the arsenic in the sample solution, plumbous tie-in; Under same current potential; Make arsenic earlier, plumbous on the gold electrode of above-mentioned steps in a), deposit; To the above-mentioned gold electrode of positive potential scanning direction, electro-deposition is separated out under different potential at the arsenic on the above-mentioned gold electrode surfaces, lead, measure arsenic and plumbous concentration respectively;
In above-mentioned two steps, a selection pacing wherein goes out arsenic concentration and gets final product.
In the galvanochemistry stripping volt-ampere method of described arsenic, antimony and plumbous tie-in, the pre-service of gold electrode comprise respectively+2V ,-0.35V polarized electrode 10s, then from-10～15 activated electrodes of 0.3V to 1.6V cyclic voltammetry scan.
In the galvanochemistry stripping volt-ampere method of described arsenic, antimony and plumbous tie-in, in to the arsenic in the sample solution, antimony tie-in, the sedimentation potential of surveying its total concentration is-0.3V; The sedimentation potential of surveying antimony separately is 0.1V.
In the galvanochemistry stripping volt-ampere method of described arsenic, antimony and plumbous tie-in, in the arsenic in the sample solution, plumbous tie-in, sedimentation potential is-0.3V.
In the galvanochemistry stripping volt-ampere method of described arsenic, antimony and plumbous tie-in, the concentration of supporting electrolyte is 1M H in sample solution
2SO
4+ 0.1M HCl.
In the galvanochemistry stripping volt-ampere method of described arsenic, antimony and plumbous tie-in, in sample solution, add reductive agent hydrazine hydrochloride, vitamin C or Na2SO3; Be preferably Na2SO3.
The present invention is that a kind of direct gold electrode that uses is working electrode, and the method with arsenic, antimony and lead concentration in the electrochemical means mensuration sample solution can be used for the phreatic monitoring in mine.
Advantage of the present invention is: it can high precision and the continuous in high sensitivity concentration that in same solution, detects arsenic, antimony, lead with easy operation.
Description of drawings
Fig. 1 is arsenic in the continuous coverage water sample in one embodiment of the invention, plumbous galvanochemistry stripping voltammogram.
Fig. 2 is the galvanochemistry stripping voltammogram of arsenic, antimony in the continuous coverage water sample in one embodiment of the invention.
Fig. 3 is that the inventive method and ICP method are measured arsenic (As) in the water sample, plumbous (Pb), antimony (Sb) content results table.
Embodiment
It is the concentration of arsenic in the three-electrode system METHOD FOR CONTINUOUS DETERMINATION sample solution of working electrode, lead, antimony that the electrochemical method of arsenic of the present invention, antimony and plumbous tie-in is to use gold electrode, it is characterized in that possessing following operation: the pretreatment process of gold electrode; The reduction operation of arsenic and antimony; The electro-deposition operation of gold electrode surfaces is arrived in arsenic, lead, antimony electro-deposition; To positive potential scanning direction gold electrode, and make the operation of separating out that arsenic, lead, the antimony of above-mentioned gold electrode surfaces electro-deposition parses in said sample solution.
It at first is that gold electrode is carried out the mechanical buffing pre-service that the present invention measures in the method for arsenic in the sample solution, antimony, lead concentration, and polarized electrode is used the cyclic voltammetry activated electrode then again.Through mechanical buffing and two steps of activation polarization activation, to compare with the only mechanical treatment of routine, gold electrode surfaces is cleaner, and activity is higher, more helps the electro-deposition of arsenic, lead, antimony, and uses more conveniently, is convenient to robotization control.The polarized electrode pre-service of gold electrode comprise respectively+2V ,-0.35V polarized electrode 10s, then from-10～15 activated electrodes of 0.3V to 1.6V cyclic voltammetry scan.
Because arsenic, antimony chemical property are very approaching, their stripping current potential basically identical is difficult to distinguish, and adopts control sedimentation potential method in the present invention, realizes METHOD FOR CONTINUOUS DETERMINATION arsenic antimony concentration.In addition,, in electrolyte solution, need add a certain amount of reductive agent, prevent the oxidation of arsenic antimony and reduce high valence state ion, in the present invention relatively reductive agent hydrazine hydrochloride, vitamin C and Na because the arsenic antimony of pentavalent does not have electrochemical activity
2S0
3, draw sodium sulphite Na
2S0
3Be comparatively desirable reductive agent, its concentration is controlled in 10～20 times of scopes of institute's test specimens ion concentration.
According to the present invention, when utilizing electrochemical reaction to detect the concentration of arsenic, lead, antimony, through the pre-service gold electrode; The control sedimentation potential; With easy operation and device, can high precision and high sensitivity, and have good reproduction property ground continuous detecting arsenic, lead and antimony and measure its concentration.Wherein, when specifically measuring, can realize the arsenic in the sample solution, antimony and plumbous tie-in through two steps:
One of them step is to the arsenic in the sample solution, antimony tie-in; The current potential of pretreated gold electrode is changed to the negative potential direction; Let arsenic, antimony be deposited on simultaneously on the above-mentioned gold electrode surfaces earlier in (sedimentation potential be-about 0.3V) under the identical current potential, the total concentration of arsenic and antimony is measured in the current potential stripping; And then the change sedimentation potential, sedimentation potential is 0.1V, deposits antimony separately, the concentration of antimony is surveyed in the current potential stripping, obtains the concentration of arsenic according to difference;
Another step is to the arsenic in the sample solution, plumbous tie-in; Under same current potential; Arsenic, lead are deposited on pretreated gold electrode,, electro-deposition is separated out at the arsenic on the above-mentioned gold electrode surfaces, lead under different potential to the above-mentioned gold electrode of positive potential scanning direction; Sedimentation potential is-0.3V to measure arsenic and plumbous concentration respectively;
In above-mentioned two steps, all can in each step, can both measure the concentration of arsenic, so going out arsenic concentration, a selection pacing wherein gets final product.
In sample solution, can add supporting electrolyte, the concentration of this supporting electrolyte is 1M H
2SO
4+ 0.1M HCl.
Below, further specify of the present invention with reference to specific embodiment.
Embodiment 1
1) pre-service of gold electrode
Al with 0.05mm
2O
3About two minutes, gold electrode is thoroughly cleaned with secondary water in the polishing back to burnishing powder at mechanical grinding gold electrode on the polishing paper; Electrochemical oxidation and reduction gold thereupon, with chronoamperometry respectively 2V ,-0.35V polarized electrode 10s, again at 0.5 M H
2SO
4Middle scan round activated electrode 10 circle (sweep limit :-300～1600mV, sweep speeds: 4V/s); At last at 0.5 M H
2SO
4The middle gold electrode of crossing with the cyclic voltammetry characterization process (sweep limit :-300～1600mV, sweep speed: 0.1V/s), used in the experiment is platinum electrode to electrode, and contrast electrode is a saturated calomel electrode;
2) concentration of METHOD FOR CONTINUOUS DETERMINATION arsenic, lead and antimony:
A) concentration of METHOD FOR CONTINUOUS DETERMINATION As (III), Pb (II) solution
Use NaAsO2, Pb (NO
3)
2Be standard substance, prepare As (III), Pb (II) solution of variable concentrations, and it is measured.At first, preparation end liquid.In the end liquid, select for use redistilled water, add H as solvent
2SO
4Making its concentration is 1M, and it is 0.1M that interpolation HCl makes its concentration, adds Na
2S0
3Making its concentration is 1mg/l.Then, with NaAsO
2, Pb (NO
3)
2Join in the end liquid, be mixed with As (III), Pb (II) WS as measuring;
In the mensuration system, selecting the gold electrode of handling for use is working electrode, and saturated calomel electrode is a contrast electrode, and platinum electrode is to electrode.Then, employing can effectively detect the linear sweep stripping voltammetry of micro constitutent, originally adds negative potential, and As, Pb electro-deposition to positive potential scanning direction current potential, measure the current value of this moment after on the electrode;
Condition determination is following:
Electro-deposition current potential-0.3V, electrodeposition time 180s (stirring 180s);
Rest potential-0.3V, rest time 30s;
Sweep speed 100mV/s, sweep limit-0.3V～0.4V;
The result is as shown in Figure 1.
B) concentration of METHOD FOR CONTINUOUS DETERMINATION As (III), Sb (III) solution
Use NaAsO
2, the Sb powder is a standard substance, prepares As (III), Sb (III) solution of variable concentrations, and it is measured.At first, preparation end liquid.In the end liquid, select for use redistilled water, add H as solvent
2SO
4Making its concentration is 1M, and it is 0.1M that interpolation HCl makes its concentration, adds Na
2S0
3Making its concentration is 1mg/l.Then, the As for preparing (III), Sb (III) are joined in the end liquid, be modulated into As (III), Pb (II) WS as measuring;
In the mensuration system, selecting the gold electrode of handling for use is working electrode, and saturated calomel electrode is a contrast electrode, and platinum electrode is to electrode.Then, employing can effectively detect the linear sweep stripping voltammetry of micro constitutent, originally adds negative potential-0.3V, and As, Sb electro-deposition to positive potential scanning direction current potential, measure the current value of this moment after on the electrode, and be the total concentration signal of arsenic antimony this moment; Change then that to add negative potential be sedimentation potential 0.1V, have only the Sb electro-deposition this moment on electrode, to positive potential scanning direction current potential, measures the current value of this moment, and be the concentration signal of antimony this moment; Ask its difference, can realize the METHOD FOR CONTINUOUS DETERMINATION of arsenic antimony;
Condition determination is following:
Electro-deposition current potential-0.3V or 0.1V, electrodeposition time 180s (stirring 180s);
Rest potential-0.3V, rest time 30s;
Sweep speed 100mV/s, sweep limit-0.3V～0.4V;
The result is as shown in Figure 2 (wherein: a: sedimentation potential 0.1v; B: sedimentation potential-0.3v).
Embodiment 2
Arsenic in the sampling of ground water of mine, lead and antimony are measured
Get mine sampling of ground water 50ml and add H
2SO
4, HCl and Na
2S0
3, H in the solution
2SO
4Concentration is that 1M, HCl concentration are 0.1M, Na
2S0
3Concentration is 1mg/l.Be heated to little boiling 10 minutes, be cooled to room temperature.
The concentration of METHOD FOR CONTINUOUS DETERMINATION As (III), Pb (II) solution
In the mensuration process, selecting the gold electrode of handling for use is working electrode, and saturated calomel electrode is a contrast electrode, and platinum electrode is to electrode.Condition determination is following:
Electro-deposition current potential-0.3V, electrodeposition time 180s (stirring 180s);
Rest potential-0.3V, rest time 30s;
Sweep speed 100mV/s, sweep limit-0.3V-0.4V;
The concentration determination condition of METHOD FOR CONTINUOUS DETERMINATION As (III), Sb (III) solution is following:
Electro-deposition current potential-0.3V or 0.1V,, electrodeposition time 180s (stirring 180s);
Rest potential-0.3V, rest time 30s;
Sweep speed 100mV/s, sweep limit-0.3V～0.4V;
Add negative potential-0.3V, As, Sb electro-deposition to positive potential scanning direction current potential, measure the current value of this moment after on the electrode, and be the total concentration signal of arsenic antimony this moment; Change then that to add negative potential be sedimentation potential 0.1V, have only the Sb electro-deposition this moment on electrode, to positive potential scanning direction current potential, measures the current value of this moment, and be the concentration signal of antimony this moment; Ask its difference, can realize the METHOD FOR CONTINUOUS DETERMINATION of arsenic antimony.
With said method the arsenic in the water sample of mine (As), plumbous (Pb), antimony (Sb) assay result are seen table 1, adopt inductively coupled plasma emission (ICP) atomic absorption spectrum to measure simultaneously.Result in the table 1 shows this method and aas determination basically identical as a result.
Above-mentioned each embodiment can not depart from the scope of the present invention down in addition some variations, thus above explanation comprises and accompanying drawing shown in structure should be regarded as exemplary, but not in order to limit the protection domain that the present invention applies for a patent.
Claims (8)
1. a galvanochemistry stripping volt-ampere method that is used for mine arsenic from underwater, antimony and plumbous tie-in directly uses gold electrode to be working electrode, measures arsenic, antimony, lead concentration in the sample solution with electrochemical means, it is characterized in that, may further comprise the steps:
A) gold electrode is carried out pre-service, polarized electrode is used the cyclic voltammetry activated electrode then again;
B) adopted for two steps realized to the arsenic in the sample solution, antimony and plumbous tie-in:
One of them step is to the arsenic in the sample solution, antimony tie-in; The current potential of the gold electrode of above-mentioned steps in a) is changed to the negative potential direction; Letting arsenic, antimony be deposited on simultaneously on the above-mentioned gold electrode surfaces earlier under the identical current potential, the total concentration of arsenic and antimony is measured in the current potential stripping; And then the change sedimentation potential, depositing antimony separately, the concentration of antimony is surveyed in the current potential stripping, obtains the concentration of arsenic according to difference;
Another step is to the arsenic in the sample solution, plumbous tie-in; Under same current potential; Make arsenic earlier, plumbous on the gold electrode of above-mentioned steps in a), deposit; To the above-mentioned gold electrode of positive potential scanning direction, electro-deposition is separated out under different potential at the arsenic on the above-mentioned gold electrode surfaces, lead, measure arsenic and plumbous concentration respectively;
In above-mentioned two steps, a selection pacing wherein goes out arsenic concentration and gets final product.
2. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in; It is characterized in that: the pre-service of gold electrode comprise respectively+2V ,-0.35V polarized electrode 10s, then from-10～15 activated electrodes of 0.3V to 1.6V cyclic voltammetry scan.
3. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in, it is characterized in that: in to the arsenic in the sample solution, antimony tie-in, the sedimentation potential of surveying its total concentration is-0.3V; The sedimentation potential of surveying antimony separately is 0.1V.
4. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in, it is characterized in that: in the arsenic in the sample solution, plumbous tie-in, sedimentation potential is-0.3V.
5. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in is characterized in that: in sample solution, add supporting electrolyte, the concentration of this supporting electrolyte is 1M H
2SO
4+ 0.1M HCl.
6. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in is characterized in that: in sample solution, add reductive agent hydrazine hydrochloride, vitamin C or sodium sulphite Na
2SO
3Be preferably sodium sulphite Na
2SO
3
7. the galvanochemistry stripping volt-ampere method of arsenic according to claim 6, antimony and plumbous tie-in is characterized in that: concentration of sodium sulfite is controlled in 10～20 times of scopes of institute's test specimens ion concentration.
8. the galvanochemistry stripping volt-ampere method of arsenic according to claim 1, antimony and plumbous tie-in is characterized in that: gold electrode is carried out the pre-service of mechanical buffing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408108A (en) * | 2013-07-26 | 2013-11-27 | 中国科学院生态环境研究中心 | Method for quickly removing pentavalent antimony pollutant in water by combining sodium sulfite and electrochemistry |
| CN108793515A (en) * | 2018-06-15 | 2018-11-13 | 甘肃省合作早子沟金矿有限责任公司 | A kind of method of Au-Sn deposit mountain processing underground gushing water qualified discharge |
| US10274451B2 (en) | 2015-02-18 | 2019-04-30 | Santa Clara University | Affordable electrochemical detection of environmental contaminants |
| CN111624243A (en) * | 2020-06-09 | 2020-09-04 | 中国科学院生态环境研究中心 | Core-shell structure electrode material for arsenic-antimony electrochemical detection |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408108A (en) * | 2013-07-26 | 2013-11-27 | 中国科学院生态环境研究中心 | Method for quickly removing pentavalent antimony pollutant in water by combining sodium sulfite and electrochemistry |
| CN103408108B (en) * | 2013-07-26 | 2014-09-10 | 中国科学院生态环境研究中心 | Method for quickly removing pentavalent antimony pollutant in water by combining sodium sulfite and electrochemistry |
| US10274451B2 (en) | 2015-02-18 | 2019-04-30 | Santa Clara University | Affordable electrochemical detection of environmental contaminants |
| CN108793515A (en) * | 2018-06-15 | 2018-11-13 | 甘肃省合作早子沟金矿有限责任公司 | A kind of method of Au-Sn deposit mountain processing underground gushing water qualified discharge |
| CN108793515B (en) * | 2018-06-15 | 2021-12-10 | 甘肃省合作早子沟金矿有限责任公司 | Method for treating underground gushing water of gold-antimony mine and discharging water up to standard |
| CN111624243A (en) * | 2020-06-09 | 2020-09-04 | 中国科学院生态环境研究中心 | Core-shell structure electrode material for arsenic-antimony electrochemical detection |
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