CN107121466A - A kind of working electrode of charcoal nitrogen composite modification detects the electrochemical method of micro heavy - Google Patents
A kind of working electrode of charcoal nitrogen composite modification detects the electrochemical method of micro heavy Download PDFInfo
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- CN107121466A CN107121466A CN201611119336.5A CN201611119336A CN107121466A CN 107121466 A CN107121466 A CN 107121466A CN 201611119336 A CN201611119336 A CN 201611119336A CN 107121466 A CN107121466 A CN 107121466A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The present invention relates to the electrochemical method that a kind of working electrode of charcoal nitrogen composite modification detects micro heavy, belong to the association areas such as food, health, environmental monitoring.The present invention utilizes g C3N4The working electrode of/C composite modification, quantitative analysis measure is carried out by anodic stripping voltammetry to micro and trace arsenic and heavy metal ion.Electrode modification process is simple, and sensitivity for analysis is high, and test performance is stable, can quick detection is micro and trace arsenic and heavy metal ion, have very strong popularizing application prospect.
Description
Technical field
The present invention relates to the electrochemical analysis detection field such as food, health, environment, more particularly to a kind of charcoal nitrogen composite wood
The working electrode of material modification detects the electrochemical method of micro heavy.
Background technology
Heavy metal pollution is directly detrimental to health, and causes environmental quality to deteriorate, wherein especially lead, mercury, cadmium, chromium,
Five kinds of harm such as arsenic are maximum.Electrochemical Detection heavy metal element is relative to atomic absorption spectrography (AAS), atomic fluorescence method, UV, visible light
It is simple with equipment for AAS, x ray fluorescence spectrometry, inductively coupled plasma mass spectrometry, it is easy to operate,
The advantages of sensitivity is high, there is important application value in fields such as food, health, environment.
Graphite phase carbon nitride（g-C3N4）The atomic layer formed by C-N covalent bonds, then layer by layer stacking and formed.This material
Originally material is mainly used as kollag, the photochemical catalyst without metal is used as first within 2008, since then as chemistry and material
Etc. the study hotspot of various fields, strong interest is received.g-C3N4Preparation process it is comparatively fairly simple, can pass through
Such as, the material such as dicyanodiamine, melamine, thiocarbamide high-temperature polycondensation just can be obtained some materials.With the high g-C of nitrogen content3N4With
The carbon materials such as CNT, graphene are assembled, and be can be very good to play the Electronic Performance of regulation carbon material and are improved material
Catalytic activity.This material shows superior catalytic performance on oxygen reduction reaction.
This patent is with g-C3N4/ C composite detects micro and trace arsenic and heavy metal member to modify working electrode analysis
Element, material therefor is cheap and easy to get, modification simple and fast, and sensitivity is high, and performance is stable, there is very strong popularizing application prospect.
The content of the invention
The purpose of the present invention is directed to during current electrochemical method detection micro heavy, the reality of working electrode selection
Using the deficiency existed, there is provided the electrochemical method that a kind of working electrode of charcoal nitrogen composite modification detects micro heavy on border
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of working electrode of charcoal nitrogen composite modification detects the electrochemical method of micro heavy, including the working electrode
For g-C3N4The modification of/C composite, preparation method is as follows:
g-C3N4Melamine or urea etc. are dissolved in water, are then proportionally added into by the preparation process of/C composite, mode one
The carbon materials such as graphite, carbon black, activated carbon, are sufficiently mixed, and calcine solid material addition Muffle furnace at a certain temperature after drying
Obtain g-C3N4/ C composite.Mode two, by the carbon material such as melamine or urea and graphite, carbon black, activated carbon in proportion
Mixed grinding, then obtain g-C by high-temperature calcination3N4/ C composite.Mode three, by g-C3N4With graphite, carbon black, activity
Mixed grinding obtains g-C to the carbon materials such as charcoal in proportion3N4/ C composite.
A certain amount of g-C3N4/ C composite is added to ultrasonic disperse, sealing preserve in ethanol, isopropanol or water equal solvent
It is standby.Take certain volume to be tested after being added drop-wise to glassy carbon electrode surface after polishing, drying at room temperature, continue dropwise addition micro
Working electrode surface after nafion to modification, or bismuth ion is added in solion to be measured, it can improve determinand
The detection range of matter.The electrode system of described electrochemical detection method includes two electrodes or three-electrode system.
Described electrochemical analysis method includes Differential Pulse Stripping Voltammetry, square wave Stripping Voltammetry using stripping voltammetry
The correlation techniques such as method, Linear Sweep Stripping Voltammetric.
Described detection range is micro heavy.Wherein, the preferred lead of heavy metal, chromium, mercury, cadmium, copper, zinc, arsenic.
Compared with prior art, the advantage of the invention is that：
1st, working electrode coating material abundance, urea, melamine and the graphite in charcoal nitrogen material source, carbon black, activity
The materials such as charcoal are common cheap and easy to get.Charcoal nitrogen can prepare composite with carbon material by three kinds of modes.
2nd, micro nafion is properly added on the working electrode prepared, or is fitted in the solution of material to be detected
As a certain amount of Bi of addition3+, detection range and minimum detection limit can be improved.
3rd, Electrochemical Test Procedure is simple, and the testing time is short, and test limit is low, can be achieved to detect while multiple element.Energy
Enough solve the actual application problem of electrochemical method quick detection micro heavy.
Embodiment
Below by embodiment, the invention will be further described：
Embodiment 1
It is prepared by working electrode：
Melamine and carbon black etc. are mixed according to certain mass ratio, are fully ground after 600 DEG C of calcinings, 3 as a child, cooling
To room temperature.The absolute ethyl alcohol of certain volume is added, ultrasonic disperse ultrasound 40 minutes is sealed standby.Every time using preceding 20 points of ultrasound
Clock, the hanging drop that 6 uL are 15 ug is extracted with microsyringe and is added to glassy carbon electrode surface after polishing, is stored at room temperature after drying
2 uL Du Pont's coating solution is added dropwise（The nafion solution of DuPont 5%）To electrode surface.Add Bi3+Ion and lead ion to be measured
When mol ratio is 20, g-C3N4During the working electrode detection lead of/C composite modification, concentration and the dissolution peak current line of lead ion
Sexual intercourse is good, and detection limit is low.
Embodiment 2
It is prepared by working electrode：Carbon black is added in aqueous solution of urea, ultrasonic dissolution, after 80 DEG C of dryings, is put into Muffle furnace.550
DEG C calcining 3 hours, cooling naturally cool to room temperature.Take 15 ug g-C3N4The aqueous isopropanol drop coating of/C composite to polishing
On glass-carbon electrode afterwards, continue to be added dropwise the 2 uL nafion solution of DuPont 5% to electrode surface, it is stand-by after natural drying.
Electrochemical Detection uses Differential Pulse Stripping Voltammetry, and arrange parameter is as follows：Accumulating potential -0.8V, enrichment time
700s, cushioning liquid is acetic acid/sodium acetate solution of PH=4.5.
Add Bi3+When ion is 20 with lead ion mol ratio to be measured, the working electrode of carbon black modification is in detection heavy metal lead
When, the concentration and dissolution peak current of lead ion are linear, and detection limit is low.
Embodiment 3
It is prepared by working electrode：
G-C is obtained by urea and graphite mixed grinding in proportion, then by high-temperature calcination3N4/ C composite.15 ug g-
C3N4On glass-carbon electrode after the aqueous isopropanol drop coating to polishing of/C composite, continue that 2 uL DuPont 5% is added dropwise
Nafion solution is stand-by after natural drying to electrode surface.
Electrochemical Detection uses Differential Pulse Stripping Voltammetry, and arrange parameter is as follows：Accumulating potential -0.8V, enrichment time
700s, cushioning liquid is acetic acid/sodium acetate solution of PH=4.5.
Add Bi3+When ion is 20 with lead ion mol ratio to be measured, the working electrode of carbon black modification is in detection heavy metal lead
When, the concentration and dissolution peak current of lead ion are linear, and detection limit is low.
Embodiment 4
It is prepared by working electrode：
By g-C3N4Mixed grinding obtains g-C in proportion with activated carbon3N4/ C composite.15 ug g-C3N4/ C composite
On glass-carbon electrode after the ethanol solution drop coating to polishing of carbon black, continue to be added dropwise the 2 uL nafion solution of DuPont 5% to electric
Pole surface, it is stand-by after natural drying.
Electrochemical Detection uses Differential Pulse Stripping Voltammetry, and arrange parameter is as follows：Accumulating potential -1.0V, enrichment time
700s, cushioning liquid is acetic acid/sodium acetate solution of PH=4.5.
Add Bi3+When ion is 20 with chromium ion mol ratio to be measured, the working electrode of carbon black modification is in detection heavy metal lead
When, the concentration and dissolution peak current of chromium ion are linear, and detection limit is low.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (7)
1. a kind of working electrode of charcoal nitrogen composite modification detects the electrochemical method of micro heavy, it is characterised in that work
The decorative material of electrode is g-C3N4/ C composite, the preparation method of the working electrode is as follows:
g-C3N4The preparation of/C composite can take 3 kinds of modes：First, melamine or urea etc. are dissolved in into water, then by than
Example adds the carbon materials such as graphite, carbon black, activated carbon, is sufficiently mixed, and solid material is added into Muffle furnace in certain temperature after drying
Lower calcining obtains g-C3N4/ C composite；Second, the carbon materials such as melamine or urea and graphite, carbon black, activated carbon are pressed
Ratio mixed grinding, then obtain g-C by high-temperature calcination3N4/ C composite；Third, by g-C3N4With graphite, carbon black, work
Mixed grinding obtains g-C to the carbon materials such as property charcoal in proportion3N4/ C composite；A certain amount of g-C3N4/ C composite is added
The ultrasonic disperse into ethanol, isopropanol or water equal solvent, sealing preserve is standby；Certain volume is taken to be added drop-wise to glass-carbon electrode after polishing
Surface, drying at room temperature.
2. a kind of working electrode of charcoal nitrogen composite modification according to claim 1 detects the electrochemistry of micro heavy
Method, it is characterised in that g-C3N4The working electrode of/C composite modification can be in two electrodes or three-electrode system.
3. a kind of working electrode of charcoal nitrogen composite modification according to claim 1 or 2 detects the electricity of micro heavy
Chemical method, it is characterised in that it is molten that electrochemical analysis method includes Differential Pulse Stripping Voltammetry, square wave using stripping voltammetry
Go out the correlation techniques such as voltammetry, Linear Sweep Stripping Voltammetric.
4. a kind of working electrode of charcoal nitrogen composite modification according to claim 1 or 3 detects the electricity of micro heavy
Chemical method, it is characterised in that the material of carbon material modification working electrode detection is micro and trace arsenic and heavy metal.
5. a kind of working electrode detection micro heavy of charcoal nitrogen composite modification according to claim 1,3 or 4
Electrochemical method, it is characterised in that the heavy metal of detection includes：Lead, chromium, mercury, cadmium, copper, zinc, arsenic.
6. a kind of working electrode of charcoal nitrogen composite modification according to claim 1,2,3,4 or 5 detects a micro huge sum of money
The electrochemical method of category, it is characterised in that the addition concentration of the bismuth ion of detection is：1×10-6 Mol/L~1 × 10-3 mol/L。
7. a kind of working electrode of charcoal nitrogen composite modification according to claim 1,2,3,4 or 5 detects a micro huge sum of money
The electrochemical method of category, it is characterised in that the nafion of detection（The nafion solution of DuPont 5%）Addition be：1~1000
UL/mL prepare liquids.
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| CN201611119336.5A CN107121466A (en) | 2016-12-08 | 2016-12-08 | A kind of working electrode of charcoal nitrogen composite modification detects the electrochemical method of micro heavy |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323465A (en) * | 2020-03-15 | 2020-06-23 | 郑程程 | Detection preparation and detection method for heavy metal ions for pediatrics |
| CN111725506A (en) * | 2020-06-01 | 2020-09-29 | 佛山科学技术学院 | Porous carbon/carbon nitride composite material and preparation method thereof |
| CN114917871A (en) * | 2022-06-21 | 2022-08-19 | 徐靖才 | Photocatalytic regenerated active carbon and preparation method thereof |
| US20230201811A1 (en) * | 2021-12-29 | 2023-06-29 | Suzhou University of Science and Technology | SYNTHESIS METHOD OF g-C3N4/C COMPOSITE MATERIAL BASED ON HOLLYHOCK STALK |
-
2016
- 2016-12-08 CN CN201611119336.5A patent/CN107121466A/en active Pending
Non-Patent Citations (5)
| Title |
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| DONGYUE LI ET AL.: "Simultaneous determination of Cd(II) and Pb(II) by differential pulse anodic stripping voltammetry based on graphite nanofibers–Nafion composite modified bismuth film electrode", 《TALANTA》 * |
| RAJESH MADHU ET AL.: "Eco-friendly synthesis of activated carbon from dead mango leaves for the ultrahigh sensitive detection of toxic heavy metal ions and energy storage applications", 《RSC ADVANCES》 * |
| STEFANO CINTI ET AL.: "Hg<sup>2+</sup> detection using a disposable and miniaturized screen-printed electrode modified with nanocomposite carbon black and gold nanoparticles", 《ENVIRON SCI POLLUT RES》 * |
| XIAOYUN CHEN ET AL.: "Nanonization of g-C<sub>3</sub>N<sub>4</sub> with the assistance of activated carbon for improved visible light photocatalysis", 《RSC ADVANCES》 * |
| 王栋萍 等: "氮化碳/碳纳米管复合材料的制备及其在铅离子检测中的应用", 《广东化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111323465A (en) * | 2020-03-15 | 2020-06-23 | 郑程程 | Detection preparation and detection method for heavy metal ions for pediatrics |
| CN111323465B (en) * | 2020-03-15 | 2020-10-13 | 青岛市妇女儿童医院 | Detection preparation and detection method for heavy metal ions for pediatrics |
| CN111725506A (en) * | 2020-06-01 | 2020-09-29 | 佛山科学技术学院 | Porous carbon/carbon nitride composite material and preparation method thereof |
| US20230201811A1 (en) * | 2021-12-29 | 2023-06-29 | Suzhou University of Science and Technology | SYNTHESIS METHOD OF g-C3N4/C COMPOSITE MATERIAL BASED ON HOLLYHOCK STALK |
| US11833491B2 (en) * | 2021-12-29 | 2023-12-05 | Suzhou University of Science and Technology | Synthesis method of g-C3N4/c composite material based on hollyhock stalk |
| CN114917871A (en) * | 2022-06-21 | 2022-08-19 | 徐靖才 | Photocatalytic regenerated active carbon and preparation method thereof |
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