CN109709183A - It is a kind of to exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion - Google Patents
It is a kind of to exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion Download PDFInfo
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- CN109709183A CN109709183A CN201811652068.2A CN201811652068A CN109709183A CN 109709183 A CN109709183 A CN 109709183A CN 201811652068 A CN201811652068 A CN 201811652068A CN 109709183 A CN109709183 A CN 109709183A
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Abstract
It is a kind of to exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion, it is related to heavy metal analysis technical field.By in compound film electrode built in shell, and the acetate buffer solution of pH=5 is added in shell, makes acetate buffer solution that compound film electrode be completely covered；Under conditions of temperature is 25 ± 0.1 DEG C, to environment water, oxidation peak current value in recording curve.The beneficial effects of the present invention are: the configuration of the present invention is simple, it is easy to use, by being detected in compound film electrode built in shell to environment water, and compound film electrode is CNTs/poly (β-CD) electrode, the advantages of conductive height of the electrode, large specific surface area, and contain many hydroxyls, it is easy and heavy metal combines, it is easy to detect the enrichment of heavy metal, detection error is small.
Description
Technical field
The present invention relates to heavy metal analysis technical fields, and in particular to generates when a kind of exclusion detection contents of many kinds of heavy metal ion
The new method interfered with each other.
Background technique
Heavy metal described in terms of the environmental pollution, is actually primarily referred to as the metals such as mercury, cadmium, lead, chromium, arsenic or eka-gold
Belong to, also refers to the general heavy metal with certain toxicity, such as copper, zinc, nickel, cobalt, tin.Heavy metal can be enriched in vivo, and
Enter human body by channels such as atmosphere, drinking water and foods, is caused including carcinogenic, teratogenesis and mutagenesis etc. to human health
Serious harm.Currently, common heavy metal detection method have it is ultraviolet can spectrophotometry (UV), atomic absorption method (AAS), former
Sub- fluorescence method (AFS), inductively coupled plasma body method (ICP), X fluorescence spectrum (XRF), Inductively coupled plasma-mass spectrometry
(ICP-MS) etc., though they have the advantages that respective, also generally existing equipment price is expensive, and instrument maintenance expense is larger, answers
The disadvantages of narrow with face, and when detecting, usually due to containing detection device for multi metallic elements in environment water, there are a heavy metal species
The case where to the interference of another heavy metal analysis.Accordingly it is desirable to production when can have a kind of exclusion detection contents of many kinds of heavy metal ion
The raw new method interfered with each other, to reduce the error of testing result.
Summary of the invention
The purpose of the present invention is being directed to defect described above, phase is generated when a kind of exclusion detection contents of many kinds of heavy metal ion is provided
The new method mutually interfered, this method is simple and convenient, and testing result error is small.
The purpose of the present invention is what is be achieved by the following technical programs.
It is a kind of to exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion, which is characterized in that successively to include
Following steps: (1) taking a U-shaped shell, and shell side upper end is provided with aperture；
(2) in compound film electrode built in shell, and the electrode is connect by the aperture of shell side with outer end power supply；
(3) acetate buffer solution of pH=5 is added in shell, makes acetate buffer solution that compound film electrode be completely covered；
(4) liquid to be detected is added, under conditions of temperature is 25 ± 0.1 DEG C, is stood after a certain period of time in -1 V preenrichment
20 s observe the linear scan curve from -0.3 V of V ~ -1, oxidation peak current value in recording curve.
The compound film electrode is CNTs/poly (β-CD) electrode, is made by following methods:
(1) pretreatment of glassy carbon electrode
Polishing powder (the Al of suitable 30 nm is sprinkled on chamois leather2O3), a few drop deionized waters are then added dropwise, with glass-carbon electrode side
Edge stirs evenly, and pinches glass-carbon electrode vertically afterwards, uniformly firmly, at the uniform velocity draws circle, is then cleaned with deionized water, ear washing bulb is blown
It is dry, nitric acid is dripped in glassy carbon electrode surface, is cleaned after static 10 ~ 15 s with deionized water, then in ethanol water, nitre
20 s of ultrasound are distinguished in aqueous acid, deionized water, ear washing bulb drying is spare；
The glass-carbon electrode handled well is put into 5 mM K3Fe(CN)6、0.2 M KNO3In solution, with electrochemical workstation, use
Three-electrode system, reference electrode select saturated calomel electrode (SCE), select carbon-point to electrode, working electrode selects glass-carbon electrode
(GCE) (3 mm of diameter), using cyclic voltammetry, the scanning in the scanning range of 0 ~ 0.5 V；If redox peaks potential difference
Within 64 mV or so, 80 mV, 0.2 M H is changed to2SO4It is activated in solution, the scanning in -0.2 ~ 1.4V, until circulation volt
Antu repeats；
(2) processing of carbon nanotube
1) electronic balance weighs 5.0 g hydroxylated multi-walled carbon nanotubes, takes the HCL of 100 mL, 0.4 M with graduated cylinder, MWCNT and
HCL solution mixes, 5 h of mechanical stirring after ultrasonic oscillation；
2) in the H of 100 mL2SO4And HNO3Ultrasonic 5 hours in mixed solution (concentration ratio is 3:1), then magnetic agitation 10 are small
When；
3) carbon nanotube and mixed acid solution are filtered by vacuum, and are washed with deionized water to neutrality, and dry 24 h are placed in drying box；
4) take the processed carbon nanotube of 5 mg that deionized water is added to be settled to 10 mL, ultrasound is uniform to solution, spare；
(3) preparation of poly (β-CD) electrode
At room temperature, accurate measuring the good concentration of configured in advance be 0.1 M, pH value be 6 50 mL of phosphate buffer solution,
0.125 mM beta-cyclodextrin is added, ultrasound takes out placement after obtaining within 20 minutes uniform mixed solution after stirring to all dissolutions
It is spare；The same step of three-electrode system (1), scanning range are -1 ~ 2 V, and sweeping speed is 100 mV/s；Poly- β-is obtained after deposition
Cyclodextrin electrode is rinsed well rear spare with deionization；
(4) preparation of CNTs electrode
Taking 6 μ L concentration with liquid-transfering gun is that the MWCNTs of 0.5 mg/mL drops to the surface glass-carbon electrode (GCE), is placed under ultraviolet lamp,
It takes out to obtain CNTs electrode after drying, dries up spare after being rinsed with deionization, sample is named as CNTs electrode；
(5) preparation of CNTs/ poly (β-CD) electrode
CNTs electrode is taken to be put into the cyclodextrin PBS mixed solution prepared (concentration and step (3) are same)；Three-electrode system is same
Step (1) carries out electropolymerization using cyclic voltammetric, and scanning range is -1 ~ 2 V, and sweeping speed is 50 mV/s；After deposition
It to CNTs/poly (β-CD) electrode, is rinsed well with deionization rear spare, obtains CNTs/poly (β-CD) electrode.
The beneficial effects of the present invention are: the configuration of the present invention is simple, easy to use, by compound film electrode built in shell come
Environment water is detected, and compound film electrode is CNTs/ poly (β-CD) electrode, the conductive height of the electrode compares table
The big advantage of area, and contain many hydroxyls, it is easy and heavy metal combines, be easy to detect the enrichment of heavy metal, detection error is small.
Specific embodiment
In order to further illustrate the present invention, following serial specific embodiment is provided, but the present invention is not specific real by these
Apply the limitation of example, any understanding person skilled in art to few modifications of the invention will can achieve it is similar as a result, this
A little changes are also contained among the present invention.
Embodiment 1.
It is a kind of to exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion, which is characterized in that successively to include
Following steps: (1) taking a U-shaped shell, and shell side upper end is provided with aperture；
(2) in compound film electrode built in shell, and the electrode is connect by the aperture of shell side with outer end power supply；
(3) acetate buffer solution of pH=5 is added in shell, makes acetate buffer solution that compound film electrode be completely covered；
(4) liquid to be detected is added, under conditions of temperature is 25 ± 0.1 DEG C, is stood after a certain period of time in -1 V preenrichment
20 s observe the linear scan curve from -0.3 V of V ~ -1, oxidation peak current value in recording curve.
The compound film electrode is CNTs/poly (β-CD) electrode, is made by following methods:
(1) pretreatment of glassy carbon electrode
Polishing powder (the Al of suitable 30 nm is sprinkled on chamois leather2O3), a few drop deionized waters are then added dropwise, with glass-carbon electrode side
Edge stirs evenly, and pinches glass-carbon electrode vertically afterwards, uniformly firmly, at the uniform velocity draws circle, is then cleaned with deionized water, ear washing bulb is blown
It is dry, nitric acid is dripped in glassy carbon electrode surface, is cleaned after static 10 ~ 15 s with deionized water, then in ethanol water, nitre
20 s of ultrasound are distinguished in aqueous acid, deionized water, ear washing bulb drying is spare；
The glass-carbon electrode handled well is put into 5 mM K3Fe(CN)6、0.2 M KNO3In solution, with electrochemical workstation, use
Three-electrode system, reference electrode select saturated calomel electrode (SCE), select carbon-point to electrode, working electrode selects glass-carbon electrode
(GCE) (3 mm of diameter), using cyclic voltammetry, the scanning in the scanning range of 0 ~ 0.5 V；If redox peaks potential difference
Within 64 mV or so, 80 mV, 0.2 M H is changed to2SO4It is activated in solution, the scanning in -0.2 ~ 1.4V, until circulation volt
Antu repeats；
(2) processing of carbon nanotube
1) electronic balance weighs 5.0 g hydroxylated multi-walled carbon nanotubes, takes the HCL of 100 mL, 0.4 M with graduated cylinder, MWCNT and
HCL solution mixes, 5 h of mechanical stirring after ultrasonic oscillation；
2) in the H of 100 mL2SO4And HNO3Ultrasonic 5 hours in mixed solution (concentration ratio is 3:1), then magnetic agitation 10 are small
When；
3) carbon nanotube and mixed acid solution are filtered by vacuum, and are washed with deionized water to neutrality, and dry 24 h are placed in drying box；
4) take the processed carbon nanotube of 5 mg that deionized water is added to be settled to 10 mL, ultrasound is uniform to solution, spare；
(3) preparation of poly (β-CD) electrode
At room temperature, accurate measuring the good concentration of configured in advance be 0.1 M, pH value be 6 50 mL of phosphate buffer solution,
0.125 mM beta-cyclodextrin is added, ultrasound takes out placement after obtaining within 20 minutes uniform mixed solution after stirring to all dissolutions
It is spare；The same step of three-electrode system (1), scanning range are -1 ~ 2 V, and sweeping speed is 100 mV/s；Poly- β-is obtained after deposition
Cyclodextrin electrode is rinsed well rear spare with deionization；
(4) preparation of CNTs electrode
Taking 6 μ L concentration with liquid-transfering gun is that the MWCNTs of 0.5 mg/mL drops to the surface glass-carbon electrode (GCE), is placed under ultraviolet lamp,
It takes out to obtain CNTs electrode after drying, dries up spare after being rinsed with deionization, sample is named as CNTs electrode；
(5) preparation of CNTs/ poly (β-CD) electrode
CNTs electrode is taken to be put into the cyclodextrin PBS mixed solution prepared (concentration and step (3) are same)；Three-electrode system is same
Step (1) carries out electropolymerization using cyclic voltammetric, and scanning range is -1 ~ 2 V, and sweeping speed is 50 mV/s；After deposition
It to CNTs/poly (β-CD) electrode, is rinsed well with deionization rear spare, obtains CNTs/poly (β-CD) electrode.
It is very big to can be seen that peak current at the beginning from record result, is to keep peak electric because CNTs electric conductivity is fine on electrode
Stream is very high, but with the progress of electropolymerization, electrode surface constantly has polymer generation, and polymer relative molecular weight is big, electric conductivity
It is poor, cause conductivity of composite material to reduce, peak current reduces.Later because electroactive material increases, peak current starts slightly
Degree increases, and later as electroactive material is continuously increased, electrode surface material thickeies, and electric conductivity reduces, and peak current tends to be steady
It is fixed.
Claims (2)
1. a kind of exclude to generate the new method interfered with each other when detection contents of many kinds of heavy metal ion, which is characterized in that successively comprising such as
Lower step: (1) taking a U-shaped shell, and shell side upper end is provided with aperture；
(2) in compound film electrode built in shell, and the electrode is connect by the aperture of shell side with outer end power supply；
(3) acetate buffer solution of pH=5 is added in shell, makes acetate buffer solution that compound film electrode be completely covered；
(4) liquid to be detected is added, under conditions of temperature is 25 ± 0.1 DEG C, is stood after a certain period of time in -1 V preenrichment
20 s observe the linear scan curve from -0.3 V of V ~ -1, oxidation peak current value in recording curve.
2. the new method interfered with each other is generated when a kind of exclusion detection contents of many kinds of heavy metal ion according to claim 1,
Be characterized in that: the compound film electrode is CNTs/poly (β-CD) electrode, is made by following methods:
(1) pretreatment of glassy carbon electrode
Polishing powder (the Al of suitable 30 nm is sprinkled on chamois leather2O3), a few drop deionized waters are then added dropwise, with glass-carbon electrode edge
It stirs evenly, pinches glass-carbon electrode vertically afterwards, uniformly firmly, at the uniform velocity draw circle, then cleaned with deionized water, ear washing bulb drying,
Nitric acid is dripped in glassy carbon electrode surface, is cleaned after static 10 ~ 15 s with deionized water, then in ethanol water, nitric acid
20 s of ultrasound are distinguished in aqueous solution, deionized water, ear washing bulb drying is spare；
The glass-carbon electrode handled well is put into 5 mM K3Fe(CN)6、0.2 M KNO3In solution, with electrochemical workstation, use
Three-electrode system, reference electrode select saturated calomel electrode (SCE), select carbon-point to electrode, working electrode selects glass-carbon electrode
(GCE) (3 mm of diameter), using cyclic voltammetry, the scanning in the scanning range of 0 ~ 0.5 V；If redox peaks potential difference
Within 64 mV or so, 80 mV, 0.2 M H is changed to2SO4It is activated in solution, the scanning in -0.2 ~ 1.4V, until circulation volt
Antu repeats；
(2) processing of carbon nanotube
1) electronic balance weighs 5.0 g hydroxylated multi-walled carbon nanotubes, takes the HCL of 100 mL, 0.4 M with graduated cylinder, MWCNT and
HCL solution mixes, 5 h of mechanical stirring after ultrasonic oscillation；
2) in the H of 100 mL2SO4And HNO3Ultrasonic 5 hours in mixed solution (concentration ratio is 3:1), then magnetic agitation 10 are small
When；
3) carbon nanotube and mixed acid solution are filtered by vacuum, and are washed with deionized water to neutrality, and dry 24 h are placed in drying box；
4) take the processed carbon nanotube of 5 mg that deionized water is added to be settled to 10 mL, ultrasound is uniform to solution, spare；
(3) preparation of poly (β-CD) electrode
At room temperature, accurate measuring the good concentration of configured in advance be 0.1 M, pH value be 6 50 mL of phosphate buffer solution,
0.125 mM beta-cyclodextrin is added, ultrasound takes out placement after obtaining within 20 minutes uniform mixed solution after stirring to all dissolutions
It is spare；The same step of three-electrode system (1), scanning range are -1 ~ 2 V, and sweeping speed is 100 mV/s；Poly- β-is obtained after deposition
Cyclodextrin electrode is rinsed well rear spare with deionization；
(4) preparation of CNTs electrode
Taking 6 μ L concentration with liquid-transfering gun is that the MWCNTs of 0.5 mg/mL drops to the surface glass-carbon electrode (GCE), is placed under ultraviolet lamp,
It takes out to obtain CNTs electrode after drying, dries up spare after being rinsed with deionization, sample is named as CNTs electrode；
(5) preparation of CNTs/ poly (β-CD) electrode
CNTs electrode is taken to be put into the cyclodextrin PBS mixed solution prepared (concentration and step (3) are same)；Three-electrode system is same
Step (1) carries out electropolymerization using cyclic voltammetric, and scanning range is -1 ~ 2 V, and sweeping speed is 50 mV/s；After deposition
It to CNTs/poly (β-CD) electrode, is rinsed well with deionization rear spare, obtains CNTs/poly (β-CD) electrode.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007045916A2 (en) * | 2005-10-21 | 2007-04-26 | Isis Innovation Limited | Electrochemical detection of arsenic |
| CN103884761A (en) * | 2012-12-20 | 2014-06-25 | 西北师范大学 | Method for simultaneously detecting three isomers of resorcinol by using MWNTs-IL/GCE electrochemical sensor |
| CN104280448A (en) * | 2014-10-17 | 2015-01-14 | 扬州大学 | Method for measuring concentration of lead ions in PM2.5 |
| CN105717174A (en) * | 2016-02-22 | 2016-06-29 | 山东省科学院新材料研究所 | Electrochemical detection method for detecting trace heavy metal ions in water with modified graphene oxide composite modified electrode |
-
2018
- 2018-12-31 CN CN201811652068.2A patent/CN109709183A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007045916A2 (en) * | 2005-10-21 | 2007-04-26 | Isis Innovation Limited | Electrochemical detection of arsenic |
| CN103884761A (en) * | 2012-12-20 | 2014-06-25 | 西北师范大学 | Method for simultaneously detecting three isomers of resorcinol by using MWNTs-IL/GCE electrochemical sensor |
| CN104280448A (en) * | 2014-10-17 | 2015-01-14 | 扬州大学 | Method for measuring concentration of lead ions in PM2.5 |
| CN105717174A (en) * | 2016-02-22 | 2016-06-29 | 山东省科学院新材料研究所 | Electrochemical detection method for detecting trace heavy metal ions in water with modified graphene oxide composite modified electrode |
Non-Patent Citations (1)
| Title |
|---|
| 张萌芽: "碳基复合物修饰电极的制备及其在重金属检测和甲醇催化氧化中的应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20190503 |