CN102590320B - Electrochemical method for detecting trace trivalent inorganic arsenic by using mercaptoethylamine modified electrode - Google Patents
Electrochemical method for detecting trace trivalent inorganic arsenic by using mercaptoethylamine modified electrode Download PDFInfo
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- CN102590320B CN102590320B CN201210024585.1A CN201210024585A CN102590320B CN 102590320 B CN102590320 B CN 102590320B CN 201210024585 A CN201210024585 A CN 201210024585A CN 102590320 B CN102590320 B CN 102590320B
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Abstract
The invention discloses an electrochemical method for detecting trace trivalent inorganic arsenic by using a mercaptoethylamine modified electrode, and relates to the field of electrochemical detection. The method solves the problems of complex process, long detection time, poor reproducibility and poor interference resistance of the conventional electrochemical methods for detecting the trivalent arsenic. According to the method, the mercaptoethylamine modified gold electrode serving as a working electrode, silver-silver chloride serving as a reference electrode and platinum serving as a counter electrode form a three-electrode system; and constant potential deposition is performed by applying a voltage through differential pulse voltammetry, dissolved oxidation reaction of arsenic is performed on the surface of the mercaptoethylamine modified gold electrode, and the trivalent arsenic is detected in a phosphate buffer solution. The electrode preparation method is simple, an electrochemical polarization process under high potential is avoided, the sensitivity and the reproducibility of the sensing detection are improved, and the problem of interference of copper ions is solved; and the detection time is short, the detection limit can reach 0.02mugL<-1>, and the method can be used for detecting the arsenic in a practical sample.
Description
Technical field
The present invention relates to the Electrochemical Detection field, be specifically related to the electrochemical method of mercaptoethylmaine modified electrode for detection of trace trivalent inorganic arsenic.
Background technology
Water pollution is one of main environmental pollution, the heavy metal of environmental pollution aspect indication mainly refers to the significant mercury of bio-toxicity, cadmium, plumbous, chromium, thallium and heavy metal arsenic, heavy metal in environment can pass through food chain enrichment in vivo, a plurality of systems to body cause damage, the toxicity of element arsenic is extremely low, and the compound of arsenic all has severe toxicity, the trivalent arsenic compound is stronger than other arsenic compound toxicity, as intake surpasses excretion, will be the liver of human body, kidney, lung, spleen, accumulate at the positions such as uterus, enzyme system in cell is combined, the biological agent of enzyme is suppressed to lose activity, thereby cause poisoning, arsenic also has carcinogenesis in addition, therefore set up highly sensitive, the inorganic trivalent arsenic ion measurement of trace method accurately, significant to safeguarding the aspects such as Environmental security and human health.
Stripping voltammetry, as the arsenious electrochemical method of a kind of detection be widely used, mainly exists two problems, the poor reproducibility of measurement result and the copper ion serious interference to measurement result in the mensuration process.Existing patent " non-eletricity enriching is also measured the electrochemical method of trace trivalent inorganic arsenic in the aqueous systems " patent No. is CN101349673A, though can effectively solve the above problems, but the preparation process of electrode relates to the steps such as activation polarization and electronation, make electrode preparation method comparatively loaded down with trivial details, the non-eletricity enriching process need 15min taked in testing process in addition, make the testing process time consuming time long, and sensitivity is relatively low.
Summary of the invention
The objective of the invention is existing to detect that arsenious electrochemical method process is complicated, detection time is long in order to solve, the problem of poor reproducibility and poor anti jamming capability, and the mercaptoethylmaine modified electrode provided is for detection of the electrochemical method of trace trivalent inorganic arsenic.
The mercaptoethylmaine modified electrode is for detection of the electrochemical method of trace trivalent inorganic arsenic, and the method realizes as follows:
Step 1: gold electrode is polished to " minute surface " with the chamois leather that adds 1.0 μ m and 0.3 μ m aluminium oxide suspension respectively, after ethanol, intermediate water ultrasonic cleaning, standby;
Step 2: the gold electrode of the processing that step 1 is obtained is put into mercaptoethylmaine solution, and immersion, drip washing obtain the gold electrode that mercaptoethylmaine is modified;
Step 3: the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode, silver-silver chloride is contrast electrode, in the electrochemical investigating pond of platinum for the 5mL phosphate buffer that common insertion contains variable concentrations arsenic to electrode, each electrode is connected on electrochemical workstation, electrochemical workstation is connected with computing machine, select Differential Pulse Voltammetry in the technology option of electrochemical workstation, be set to-0.8V of potential range is to 0.3V, the operation electrochemical workstation is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, by its electrochemical response of computer monitoring,
Step 4: after detection, at former phosphate, detect in solution, each electrode is connected on electrochemical workstation, select current-time curvel in the technology option of electrochemical workstation, current potential is set to 0.4V, operation 30s, the operation electrochemical workstation is scanned, the arsenic on end of scan rear electrode surface can be oxidized to trivalent arsenic desorption fully, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond, with intermediate water, rinses well;
Step 5: adopt the Origin mapping, draw the oxidation peak current curve of arsenic.
In above-mentioned steps 2, the concentration of mercaptoethylmaine solution is 10mM;
In above-mentioned steps 2, soak time is 1 hour;
In above-mentioned steps 3, phosphatic concentration is 0.1M;
In above-mentioned steps 3, arsenious concentration sensing range is 0.2 μ gL
-1-300 μ gL
-1.
Above-mentioned mercaptoethylmaine modified electrode is for detection of the electrochemical method of trace trivalent inorganic arsenic, if also contain noisy copper ion in phosphate buffered solution, detecting step 1 and step 2 are constant, and other step is as follows:
Step 3: the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode, and silver-silver chloride is contrast electrode, and platinum is for being added with 50 μ gL to common insertion of electrode
-1in the electrochemical investigating pond of the 0.1M phosphate buffer of arsenic, each electrode is connected on electrochemical workstation used, electrochemical workstation is connected with computing machine, select Differential Pulse Voltammetry in the technology option of electrochemical workstation, be set to-0.8V of potential range is to 0.3V, the operation electrochemical workstation is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation redox reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, by its electrochemical response of computer monitoring;
Step 4: adopt the Origin mapping, draw the oxidation peak current curve of arsenic;
Step 5: detect complete, at former 50 μ gL
-1the 0.1M phosphate of arsenic detects in solution, each electrode is connected on electrochemical workstation, select current-time curvel in the technology option of electrochemical workstation, current potential is set to 0.4V, operation 30s, the operation electrochemical workstation is scanned, and the arsenic on end of scan rear electrode surface can be fully by desorption, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond, rinse well with intermediate water;
Step 6: at former 50 μ gL
-1the 0.1M phosphate of arsenic detects in solution, adds 50 μ gL
-1copper ion, be connected to each electrode on electrochemical workstation, repeats above-mentioned steps 3,4 and 5, investigates copper ion under condition of different pH and arsenic is detected to the impact of disturbing.
Beneficial effect:
(1) electrode preparation method of the present invention is simple, avoided the activation polarization process under the noble potential, by simple immersion, just can realize, not only effectively solved the problem that naked gold electrode easily pollutes, and having improved sensitivity and the reappearance of this sensing detection, experiment shows: the reproducible relative standard deviation of 6 arsenic of continuous sweep is 1.39%;
(2) method antijamming capability of the present invention is strong, and experiment shows: in the phosphate buffer solution of pH 7, the gold electrode that utilizes mercaptoethylmaine to modify, can effectively separate with the oxidation-reduction potential of metallic copper, gets rid of the interference of copper ion in water;
(3) method of the present invention is short detection time, adopts constant potential enrichment 100s, and detection limit can reach 0.02 μ gL
-1, lower than drinking water standard, can be accurately for the arsenious detection of actual sample;
(4) method of the present invention can be used for arsenious detection in actual sample, and the recovery is in the 98.25%-106.79% scope.
The accompanying drawing explanation
The schematic diagram that Fig. 1 is the three-electrode electro Chemical system;
Fig. 2 is mercaptoethylmaine modified electrode differentiated pulse Stripping Voltammetry curve in the arsenious phosphate buffer solution (pH 7) of variable concentrations, the linear relationship curve that illustration is oxidation peak current and trivalent arsenic concentration;
Fig. 3 is that the mercaptoethylmaine modified electrode is containing 100 μ gL
-1in the phosphate buffer solution of arsenic (pH 7), the Stripping Voltammetry response diagram of 6 arsenic of continuous sweep;
A in Fig. 4 is 50 μ gL
-1under the copper ion existence condition, enrichment 50 μ gL
-1the phosphate buffer solution differentiated pulse voltammogram of pH 1 of arsenic, in figure, B is 50 μ gL
-1under the copper ion existence condition, enrichment 50 μ gL
-1the phosphate buffer solution differentiated pulse voltammogram of pH 7 of arsenic;
In figure: 1, magnetic stirring apparatus, 2, magnetic stir bar, 3, working electrode, 4, contrast electrode, 5, to electrode, 6, electrochemical workstation, 7, computing machine, 8, electrochemical investigating pond.
Embodiment:
The present invention will be further described for 1-4 and embodiment by reference to the accompanying drawings.
Step 1: adopt as shown in Figure 1 in the three-electrode electro Chemical system, gold electrode is polished to " minute surface " with the chamois leather that adds 1.0 μ m and 0.3 μ m aluminium oxide suspension respectively, after ethanol, intermediate water ultrasonic cleaning, standby;
Step 2: the gold electrode of the processing that step 1 is obtained is put into 10mM mercaptoethylmaine solution, soaks 1 hour, and the effect by the Au-S key is fixed on gold electrode surfaces by mercaptoethylmaine, then electrode is used to intermediate water drip washing, obtains the gold electrode that mercaptoethylmaine is modified;
Step 3: will put a magnetic stir bar 2 in electrochemical investigating pond 8, be placed on magnetic stirring apparatus 1, the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode 3, and silver-silver chloride is contrast electrode 4, and platinum is for to electrode 5, common insertion contains respectively 0.2 μ gL
-1, 0.5 μ gL
-1, 1.5 μ gL
-1, 3.0 μ gL
-1, 5.0 μ gL
-1, 8 μ gL
-1, 12 μ gL
-1, 20 μ gL
-1, 40 μ gL
-1, 70 μ gL
-1, 150 μ gL
-1, 200 μ gL
-1, 250 μ gL
-1with 300 μ gL
-1in the electrochemical investigating pond 8 of the 5mL0.1M phosphate buffer of arsenic (PH is 7), each electrode is connected on electrochemical workstation used 6, electrochemical workstation 6 is connected with computing machine 7, select Differential Pulse Voltammetry in the technology option of electrochemical workstation, be set to-0.8V of potential range is to 0.3V, operation electrochemical workstation 6 is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, by computing machine 7 its electrochemical responses of monitoring,
Step 4: after each concentration detects, at former 0.1M phosphate, detect in solution, each electrode is connected on electrochemical workstation 6, select current-time curvel in the technology option of electrochemical workstation 6, current potential is set to 0.4V, operation 30s, operation electrochemical workstation 6 is scanned, the arsenic on end of scan rear electrode surface can be oxidized to trivalent arsenic desorption fully, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond 8, with intermediate water, rinses well;
Step 5: adopt the Origin mapping, draw the oxidation peak current curve of arsenic.
Fig. 2 is mercaptoethylmaine modified electrode differentiated pulse Stripping Voltammetry curve in the arsenious phosphate buffer solution (pH 7) of variable concentrations, the linear relationship curve that illustration is oxidation peak current and trivalent arsenic concentration, as can be seen from the figure, the gold electrode that mercaptoethylmaine is modified is at 0.2-300 μ gL
-1in scope, linear, detect and be limited to 0.02 μ gL
-1, lower than the content standard of Arsenic in Drinking Water, can be for detection of arsenious content in actual sample.
Step 1: adopt as shown in Figure 1 in the three-electrode electro Chemical system, gold electrode is polished to " minute surface " with the chamois leather that adds 1.0 μ m and 0.3 μ m aluminium oxide suspension respectively, after ethanol, intermediate water ultrasonic cleaning, standby;
Step 2: the gold electrode of the processing that step 1 is obtained is put into 10mM mercaptoethylmaine solution, soaks 1 hour, and the effect by the Au-S key is fixed on gold electrode surfaces by mercaptoethylmaine, then electrode is used to intermediate water drip washing, obtains the gold electrode that mercaptoethylmaine is modified;
Step 3: by putting a magnetic stir bar 2 in electrochemical investigating pond 8, be placed on magnetic stirring apparatus 1, the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode 3, and silver-silver chloride is contrast electrode 4, and platinum is for containing 100 μ gL to common insertion of electrode 5
-1in the electrochemical investigating pond 8 of the 5mL0.1M phosphate buffer of arsenic (PH is 7), each electrode is connected on electrochemical workstation used 6, electrochemical workstation 6 is connected with computing machine 7, select Differential Pulse Voltammetry in the technology option of electrochemical workstation, be set to-0.8V of potential range is to 0.3V, operation electrochemical workstation 6 is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, by computing machine 7 its electrochemical responses of monitoring,
Step 4: detect complete, at the former 100 μ gL that contain
-1the 0.1M phosphate of arsenic detects in solution, each electrode is connected on electrochemical workstation 6, select current-time curvel in the technology option of electrochemical workstation 6, current potential is set to 0.4V, operation 30s, operation electrochemical workstation 6 is scanned, and the arsenic on end of scan rear electrode surface can be oxidized to trivalent arsenic desorption fully, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond 8, rinse well with intermediate water;
Step 5: adopt the Origin mapping, draw the oxidation peak current curve of arsenic.
Fig. 3 is that the mercaptoethylmaine modified electrode is containing 100 μ gL
-1in the phosphate buffer solution of arsenic (pH 7), the Stripping Voltammetry response diagram of 6 arsenic of continuous sweep, as can be seen from the figure, the gold electrode that mercaptoethylmaine is modified has good reappearance, and relative standard deviation is 1.39%.
Method of the present invention can be used for arsenious detection in actual sample, as shown in table 1, and the recovery, can be for the arsenious detection of actual sample in the 98.25%-106.79% scope.
Table 1
Step 1: adopt as shown in Figure 1 in the three-electrode electro Chemical system, gold electrode is polished to " minute surface " with the chamois leather that adds 1.0 μ m and 0.3 μ m aluminium oxide suspension respectively, after ethanol, intermediate water ultrasonic cleaning, standby;
Step 2: the gold electrode of the processing that step 1 is obtained is put into 10mM mercaptoethylmaine solution, soaks 1 hour, and the effect by the Au-S key is fixed on gold electrode surfaces by mercaptoethylmaine, then electrode is used to intermediate water drip washing, obtains the gold electrode that mercaptoethylmaine is modified;
Step 3: by putting a magnetic stir bar 2 in electrochemical investigating pond 8, be placed on magnetic stirring apparatus 1, the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode 3, and silver-silver chloride is contrast electrode 4, and platinum is for inserting containing adding 50 μ gL electrode 5 is common
-1in the electrochemical investigating pond 8 of the 0.1M phosphate buffer of arsenic (the pH value is 7), each electrode is connected on electrochemical workstation used 6, electrochemical workstation 6 is connected with computing machine 7, select Differential Pulse Voltammetry in the technology option of electrochemical workstation, be set to-0.8V of potential range is to 0.3V, operation electrochemical workstation 6 is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, by computing machine 7 its electrochemical responses of monitoring.
Step 4: adopt the Origin mapping, draw the oxidation peak current curve of arsenic;
Step 5: detect complete, at former 50 μ gL
-1the 0.1M phosphate of arsenic detects in solution, each electrode is connected on electrochemical workstation, select current-time curvel in the technology option of electrochemical workstation, current potential is set to 0.4V, operation 30s, the operation electrochemical workstation is scanned, and the arsenic on end of scan rear electrode surface can be fully by desorption, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond, rinse well with intermediate water;
Step 6: at former 50 μ gL
-1the 0.1M phosphate of arsenic detects in solution, adds 50 μ gL
-1copper ion, be connected to each electrode on electrochemical workstation, repeats above-mentioned steps 3,4 and 5, investigates copper ion under condition of different pH and arsenic is detected to the impact of disturbing.
Fig. 4 has provided copper ion under the condition of different pH and arsenic has been detected to the impact of disturbing, and A is 50 μ gL
-1under the copper ion existence condition (solid line), enrichment 50 μ gL
-1the phosphate buffer solution differentiated pulse voltammogram of pH 1 of arsenic, figure B is 50 μ gL
-1under the copper ion existence condition (solid line), enrichment 50 μ gL
-1the phosphate buffer solution differentiated pulse voltammogram of pH 7 of arsenic; Wherein dotted line is to only have arsenic to have the differentiated pulse voltammogram in situation, as seen from Figure 4, increase along with pH, arsenious current potential is negative to be moved, in the phosphate buffer solution of pH 7, the gold electrode that utilizes mercaptoethylmaine to modify, can effectively separate with the oxidation-reduction potential of metallic copper, the poor Δ E=360mV of spike potential, this character can be used for getting rid of the interference of common copper ion in water.
Claims (6)
1. the mercaptoethylmaine modified electrode, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, the method realizes as follows:
Step 1: gold electrode is polished to " minute surface " after ethanol, intermediate water ultrasonic cleaning with the chamois leather that adds 1.0 μ m and 0.3 μ m aluminium oxide suspension respectively, standby;
Step 2: the gold electrode of the processing that step 1 is obtained is put into mercaptoethylmaine solution, and immersion, drip washing obtain the gold electrode (3) that mercaptoethylmaine is modified;
Step 3: the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode (3), silver-silver chloride is contrast electrode (4), in the electrochemical investigating pond (8) of platinum for the phosphate buffered solution that common insertion contains variable concentrations arsenic to electrode (5), each electrode is connected on electrochemical workstation (6), described electrochemical workstation (6) is connected with computing machine (7), select Differential Pulse Voltammetry in the technology option of electrochemical workstation (6), be set to-0.8V of potential range is to 0.3V, operation electrochemical workstation (6) is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, monitor its electrochemical response by computing machine (7),
Step 4: after each concentration detects, at former phosphate, detect in solution, each electrode is connected on electrochemical workstation (6), select current-time curvel in the technology option of electrochemical workstation (6), current potential is set to 0.4V, operation 30s, operation electrochemical workstation (6) is scanned, the arsenic on end of scan rear electrode surface can be oxidized to trivalent arsenic desorption fully, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond, rinse well with intermediate water;
Step 5: adopt the Origin mapping, draw the oxidation peak current curve of arsenic.
2. mercaptoethylmaine modified electrode as claimed in claim 1, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, in above-mentioned steps 2, the concentration of mercaptoethylmaine solution is 10mM.
3. mercaptoethylmaine modified electrode as claimed in claim 1, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, in above-mentioned steps 2, soak time is 1 hour;
4. mercaptoethylmaine modified electrode as claimed in claim 1, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, in above-mentioned steps 3, the concentration of phosphate buffered solution is 0.1M.
5. mercaptoethylmaine modified electrode as claimed in claim 1, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, the concentration sensing range of arsenic is 0.2 μ gL
-1-300 μ gL
-1.
6. mercaptoethylmaine modified electrode as claimed in claim 1, for detection of the electrochemical method of trace trivalent inorganic arsenic, is characterized in that, if also contain noisy copper ion in phosphate buffered solution, step 1 and step 2 are constant, and other step is as follows:
Step 3: the gold electrode that the mercaptoethylmaine that the step 2 of take obtains is modified is working electrode (3), and silver-silver chloride is contrast electrode (4), and platinum is for being added with 50 μ gL to common insertion of electrode (5)
-1in the electrochemical investigating pond (8) of the 0.1M phosphate buffer of arsenic, each electrode is connected on electrochemical workstation (6), described electrochemical workstation (6) is connected with computing machine (7), select Differential Pulse Voltammetry in the technology option of electrochemical workstation (6), be set to-0.8V of potential range is to 0.3V, operation electrochemical workstation (6) is scanned, under-0.8V current potential, deposit, deposit 100s under stirring condition, standing 10s, the gold electrode surfaces generation oxidation reaction that the arsenic of enrichment is modified at mercaptoethylmaine in scanning process, monitor its electrochemical response by computing machine (7),
Step 4: adopt the Origin mapping, draw the oxidation peak current curve of arsenic;
Step 5: detect complete, at the former 50 μ gL that contain
-1the 0.1M phosphate of arsenic detects in solution, each electrode is connected on electrochemical workstation (6), select current-time curvel in the technology option of electrochemical workstation (6), current potential is set to 0.4V, operation 30s, operation electrochemical workstation (6) is scanned, and the arsenic on end of scan rear electrode surface can be fully by desorption, after desorption, the mercaptoethylmaine modified electrode is taken out from electrochemical investigating pond, rinse well with intermediate water;
Step 6: at former 50 μ gL
-1the 0.1M phosphate of arsenic detects in solution, adds 50 μ gL
-1copper ion, be connected to electrochemical workstation (6) by each electrode upper, repeats above-mentioned steps 3,4 and 5, investigates copper ion under condition of different pH and arsenic is detected to the impact of disturbing.
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| CN108548860A (en) * | 2018-02-09 | 2018-09-18 | 南昌大学 | Trivalent arsenic electrochemical detection method based on trithiocyanuric acid/reduced graphene |
| CN108776076B (en) * | 2018-07-19 | 2021-05-11 | 上海理工大学 | Biological sensor |
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| JP4583937B2 (en) * | 2005-01-07 | 2010-11-17 | 積水化学工業株式会社 | Method for electrochemical measurement of arsenic ions |
| GB0509307D0 (en) * | 2005-05-06 | 2005-06-15 | Isis Innovation | Derivatised carbon |
| CN101349673B (en) * | 2008-09-04 | 2012-12-19 | 南京大学 | Electrochemical method for non-eletricity enriching and measuring trace amount tervalence inorganic arsenic in water system |
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