CN106932449A - The preparation method of electrochemical sensor and its application in plumbum ion concentration is detected - Google Patents
The preparation method of electrochemical sensor and its application in plumbum ion concentration is detected Download PDFInfo
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- CN106932449A CN106932449A CN201710134968.7A CN201710134968A CN106932449A CN 106932449 A CN106932449 A CN 106932449A CN 201710134968 A CN201710134968 A CN 201710134968A CN 106932449 A CN106932449 A CN 106932449A
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Abstract
The preparation method of electrochemical sensor and its application in plumbum ion concentration is detected, are related to the preparing technical field of electrochemical sensor.Under ultrasound condition, redox graphene is scattered in N N-dimethylformamides, obtains the DMF solution of redox graphene；The DMF solution drop coating of redox graphene, in being freezed under 4 DEG C of environment temperatures, is obtained final product into the electrochemical sensor for detecting lead ion in clean glassy carbon electrode surface again.By making Pb2+After the heavy metal solution of concentration and the linear relationship chart of peak point current, re-test goes out Pb in heavy metal solution to be measured2+Concentration.The inventive method equipment is available Conventional electrochemical pond, and method is simple, easy to operate, and has used current-time curvel to be enriched with so that substantially increasing detection limit.
Description
Technical field
The present invention relates to the preparing technical field of electrochemical sensor.
Background technology
Pb2+ Belong to one of main source of heavy metal pollution, have greatly danger safely to the life and health of environment and the mankind
Evil property.Lead can not be biodegradable, conversely but can be under the biological magnification of food chain, and thousands of hundred times of enrichment is most laggard
Enter human body.There is strong interaction in lead, them is lost activity, it is also possible in human body in people's physical efficiency and protein and enzyme etc.
Some organs in accumulate, cause slow poisoning, damage hematopoiesis and cardiovascular system, nervous system and kidney.
At present, Pb is detected2+ Method mainly have Atomic absorption, atomic emissions, inductively coupled plasma mass spectrometry, this
There is complicated sample pre-treatments, expensive instrument, poisonous solvent and need by people's ability of special training in a little methods
The defects such as operation.
The content of the invention
The present invention seeks to propose a kind of convenient detection lead ion（Pb2+）Electrochemical sensor preparation method.
The present invention is comprised the following steps：
1）Under ultrasound condition, redox graphene is scattered in N-N dimethylformamides（DMF）In, obtain reduction-oxidation
The DMF solution of Graphene；
2）By the DMF solution drop coating of redox graphene in clean glassy carbon electrode surface, in being freezed under 4 DEG C of environment temperatures,
Obtain final product the electrochemical sensor for detecting lead ion.
Electrochemistry electrochemical sensor due to instrument material benefit, sample relatively should not be complicated pre-treatment, the spy such as simple to operate
Point, receives more and more attention, and research shows, Electrochemical Stripping voltammetry is one powerful can detect lot of trace weight
The technology of metal, particularly after the combination of preconcentration steps and advanced electrochemical measurement analyte, due to oxygen reduction fossil
The superior electric conductivity of black alkene and chemical stability, therefore redox graphene is fixed on glass-carbon electrode to Pb2 +Inspection
Survey has very important significance.
Present invention employs redox graphene, using its superior electric conductivity, chemical stability and larger ratio
Surface area, so that more efficient electrochemical sensor interface is constructed, additionally, N-N dimethylformamides（DMF）Parcel reduction-oxidation
Graphene, can effectively prevent it from being come off from the surface of electrode, and the stability of device is passed to improve.Can make electrode under 4 DEG C of environment temperatures
It is just lyophilized in 24 hours, and locate to preserve for a long time in the present context.
Further, the concentration of redox graphene of the present invention be 5 mg/ml, can make redox graphene compared with
It is scattered in DMF well, and makes the response of peak current maximum.
Additionally, the invention allows for above electrochemical sensor to Pb2+ Detection in application process.
Comprise the following steps：
1）Respectively will known at least three difference Pb2+The heavy metal solution of concentration is mixed in electrochemistry with hac buffer
Chi Zhong, the electrochemical sensor is placed in electrochemical cell, using constant potential enriched lead, obtains different Pb2+Under concentration conditions
The electrochemical sensor of enriched lead；
2）By variant Pb2+The electrochemical sensor of enriched lead is respectively placed in hac buffer under concentration conditions, using difference
Divide pulse voltammetry that corresponding peak point current is determined under the V of current potential -0.8~-0.1；
3）Make Pb2+The heavy metal solution of concentration and the linear relationship chart of peak point current；
4）By Pb to be measured2+The heavy metal solution of concentration is mixed in electrochemical cell with hac buffer, and the electrochemistry is passed
Sensor is placed in electrochemical cell, using constant potential enriched lead, obtains Pb to be measured2+The electrochemical sensing of enriched lead under concentration conditions
Device；By Pb to be measured2+The electrochemical sensor of enriched lead is placed in hac buffer under concentration conditions, using differential pulse voltammetry
Method measure under the V of current potential -0.8~-0.1 obtains peak point current；
From the Pb2+The Pb corresponding to peak point current is checked in the heavy metal solution of concentration and the linear relationship chart of peak point current2+
Concentration value is Pb in heavy metal solution to be measured2+Concentration value.
The inventive method equipment is available Conventional electrochemical pond, and method is simple, easy to operate, and has used current-vs-time
Curve is enriched with and causes to substantially increase detection limit.
In addition, during constant potential enriched lead of the present invention, accumulating potential is -1V, and enrichment time is 220s, and during the setting, Pb2+
Peak current it is maximum.
Brief description of the drawings
Fig. 1 is the peak current and Pb made using electrochemical sensor of the present invention2+ The linear relationship chart of concentration.
Specific embodiment
Below by embodiment, and with reference to accompanying drawing, technical scheme is described in further detail.
First, electrochemical sensor preparation process：
1st, 10.0 mg redox graphenes are taken to be scattered in the DMF that 2 mL, concentration are 0.5wt%, ultrasound to being completely dispersed,
It is the DMF solution of the redox graphene of 5mg/ml to obtain redox graphene content.
2nd, the DMF solution drop coating of 5 μ L redox graphenes is taken on clean glass-carbon electrode, is freezed under the conditions of 4 DEG C,
Obtain final product electrochemical sensor.
2nd, the application of electrochemical sensor：
1st, electrochemical sensor is fixed in electrochemical cell.
2nd, the hac buffer that 10mL, concentration are 0.1mol/L is pipetted（PH is 4.5）In electrochemical cell.
3rd, the Pb that will be prepared2+Content is that 0.05 μm of mL of the heavy metal solution of ol/L 10 is added in above-mentioned electrochemical cell, is adopted
It is enriched with current versus time curve method, accumulating potential is -1 V, enrichment time is 220 s.
4th, Pb will be enriched with2+ Above-mentioned glass-carbon electrode be placed in containing the hac buffer that 10 mL, pH are 4.5 blank electricity
Chemical bath.Using differential pulse voltammetry, determined under the V of current potential -0.8~-0.1, obtain peak current I1。
5th, above step 3,4 is repeated, by Pb in heavy metal solution2+Concentration be changed to 0.2 μm of ol/L, 0.3 μm of ol/ respectively
L、0.4 μmol/L、0.5μmol/L、0.6μmol/L、0.7μmol/L、0.9 μmol/L、1.0μmol/L、1.1 μmol/L、
1.2 μm of ol/L, will respectively obtain electric current I2、I3、I4、I5、I6、I7、I8、I9、I10、I11。
6th, peak current and Pb are made2+ The linear relationship chart of concentration, as shown in Figure 1.
3rd, contrast test and result：
In order to investigate the achieved reliability of the inventive method, the detection of Yangzhou Slender West Lake water sample has been carried out.Water sample is taken from thin west
The deep lake water in 0.5 meter of central underwater.
1st, the electrochemical sensor being first made is fixed in electrochemical cell.
2nd, 10 mL water samples to be measured are taken and hac buffer that 10 mL, concentration are 0.1 mol/L（PH is 4.5）Add
In electrochemical cell.It is enriched with using using current versus time curve method, accumulating potential is -1 V, enrichment time is 220 s.
The 3rd, electrochemical sensor after enrichment is placed in the blank electricity containing the hac buffer that 10 mL, pH are 4.5 again
Chemical bath.Using differential pulse voltammetry, determined under current potential -0.8~-0.1V, obtain peak current for 0.104 μ A.
4th, through the peak current and Pb of Fig. 12+ The linear relationship chart of concentration is checked in：Pb in water sample to be measured2+Content is 0.082 μ
mol/L.The content of the lead i.e. in the water of Slender West Lake is 0.082 μm of ol/L.
Take same sample and use National Standard Method（Atomic absorption method）It is measured, is as a result 0.085 μm of ol/L.
The result of two methods is compared, and relative error is that 3.5% error is smaller, and testing result is good.
And obviously facilitated using the inventive method, without complicated sample pre-treatments, it is to avoid expensive instrument input, keep away
The use of poisonous solvent is exempted from.
Claims (4)
1. the preparation method of electrochemical sensor, it is characterised in that comprise the following steps：
1）Under ultrasound condition, redox graphene is scattered in N-N dimethylformamides, obtains redox graphene
DMF solution；
2）By the DMF solution drop coating of redox graphene in clean glassy carbon electrode surface, in being freezed under 4 DEG C of environment temperatures,
Obtain final product the electrochemical sensor for detecting lead ion.
2. preparation method according to claim 1, it is characterised in that reduced in the DMF solution of the redox graphene
The concentration of graphene oxide is 5 mg/ml.
3. application of the electrochemical sensor that prepared by method as claimed in claim 1 in plumbum ion concentration is detected, its feature exists
In comprising the following steps：
1）Respectively will known at least three difference Pb2+The heavy metal solution of concentration is mixed in electrochemical cell with hac buffer
In, the electrochemical sensor is placed in electrochemical cell, using constant potential enriched lead, obtain different Pb2+It is rich under concentration conditions
Collect the electrochemical sensor of lead；
2）By variant Pb2+The electrochemical sensor of enriched lead is respectively placed in hac buffer under concentration conditions, using difference
Divide pulse voltammetry that corresponding peak point current is determined under the V of current potential -0.8~-0.1；
4）Make Pb2+The heavy metal solution of concentration and the linear relationship chart of peak point current；
5）By Pb to be measured2+The heavy metal solution of concentration is mixed in electrochemical cell with hac buffer, and the electrochemistry is passed
Sensor is placed in electrochemical cell, using constant potential enriched lead, obtains Pb to be measured2+The electrochemical sensing of enriched lead under concentration conditions
Device；By Pb to be measured2+The electrochemical sensor of enriched lead is placed in hac buffer under concentration conditions, using differential pulse voltammetry
Method measure under the V of current potential -0.8~-0.1 obtains peak point current；
From the Pb2+The Pb corresponding to peak point current is checked in the heavy metal solution of concentration and the linear relationship chart of peak point current2+
Concentration value is Pb in heavy metal solution to be measured2+Concentration value.
4. application according to claim 3, it is characterised in that：During using constant potential enriched lead, accumulating potential is -1 V, rich
The collection time is 220 s.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109254067A (en) * | 2018-09-21 | 2019-01-22 | 东华大学 | A kind of glass-carbon electrode and its preparation and application based on the modification of rhodamine b/ redox graphene |
| CN109612574A (en) * | 2018-12-04 | 2019-04-12 | 南京粒子声学科技有限公司 | A kind of preparation method of sound particle vibration velocity sensor |
| CN111751421A (en) * | 2020-07-14 | 2020-10-09 | 江西农业大学 | Electrochemical sensor for quickly and efficiently detecting lead ions |
| CN113466010A (en) * | 2021-07-09 | 2021-10-01 | 利晟（杭州）科技有限公司 | Water pollution detection system based on electrochemical sensor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109254067A (en) * | 2018-09-21 | 2019-01-22 | 东华大学 | A kind of glass-carbon electrode and its preparation and application based on the modification of rhodamine b/ redox graphene |
| CN109254067B (en) * | 2018-09-21 | 2020-08-11 | 东华大学 | Rhodamine b/reduced graphene oxide modified glassy carbon electrode and preparation and application thereof |
| CN109612574A (en) * | 2018-12-04 | 2019-04-12 | 南京粒子声学科技有限公司 | A kind of preparation method of sound particle vibration velocity sensor |
| CN109612574B (en) * | 2018-12-04 | 2020-09-15 | 南京粒子声学科技有限公司 | Preparation method of acoustic particle vibration velocity sensor |
| CN111751421A (en) * | 2020-07-14 | 2020-10-09 | 江西农业大学 | Electrochemical sensor for quickly and efficiently detecting lead ions |
| CN111751421B (en) * | 2020-07-14 | 2021-06-04 | 江西农业大学 | Electrochemical sensor for detecting lead ions |
| CN113466010A (en) * | 2021-07-09 | 2021-10-01 | 利晟（杭州）科技有限公司 | Water pollution detection system based on electrochemical sensor |
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Application publication date: 20170707 |