CN110320256A - A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for measuring micro lead in water - Google Patents
A kind of highly integrated electrode of bismuth film and the preparation method and application thereof for measuring micro lead in water Download PDFInfo
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Abstract
The present invention provides a kind of highly integrated electrodes of bismuth film for measuring micro lead in water and preparation method thereof and the application in Electrochemical Detection.The electrode includes: electrode basement, buffer layer, layer, skin and conversion zone, and electrode uses three-electrode system, and wherein bismuth film is electroplated in working electrode, and to electrode platinum plating, reference electrode plates silver-silver chloride.Electrode is prepared the following steps are included: pre-processing to electrode of the substrate；The pretreated electrode of the substrate is put into plating bismuth solution, bismuth film electrode is made in plating.Maximum sensitivity of the present invention can reach 1ppm, detection time is short, step is simple, high sensitivity, it is at low cost, the quick detection that micro lead in water body can be achieved solves the micro lead detection for needing specific place, large-scale instrument, pre-treatment step, and small hand-held instrument and electrochemical workstation can be cooperated to use.
Description
Technical field
The invention belongs to field of electrochemical detection, and in particular to a kind of preparation method of bismuth film electrode, and its it is micro- in water
Measure the application in the quick detection of lead element.
Background technique
Lead element is typical heavy metal element, smaller to environmental hazard in the state of naturally occurring, but with industry
The development of change becomes one of the main source of environmental pollution using lead element as the heavy metal of representative.Into in water body and soil
Lead element be enriched in higher organism by the amplification of biology, significant damage caused to human body, it is serious very
To will lead to death.
The exceeded of lead element is one of great public safety problem of social concerns at present, and the exceeded water body of lead element is easy
Cause people and animal poisoning, lead element is related to nervous system, hemopoietic system to the toxic action of human body and animal, may go out
The symptoms such as existing instability of gait, neck muscle ballism, while also influencing whether the growth and development of humans and animals.Therefore, quickly measurement
Lead element in water body is social safety field urgent problem to be solved, especially pollution sources, drinking water, scene of the accident etc. no
It is the major demands of today's society with the instant detection under detection environment.
The conventional method of detection heavy metal mainly has atomic absorption spectrography (AAS), atomic emission spectrometry, spectrophotometric at present
Method, chromatography, Neutron activation analysiss, biological tracing method and electrochemical methods.Atomic absorption method or glimmering is generally used at present
Light spectrum hair precisely detects lead element, and both methods is required using large-scale instrument, and while expensive, detecting step is multiple
It is miscellaneous, it takes a long time, testing cost is higher, cannot achieve the quick detection to lead element micro in water body.
Electrochemical methods possess simple, quick, portable, sensitive feature, have in terms of quickly detection lead element only
Special advantage, however traditional electrochemical credit mostly uses greatly mercury film electrode perhaps, be easy to cause environment dirty while having larger toxicity
Dye problem, it is therefore desirable to a kind of electrode material of safety non-pollution, and the industrialization of respective electrode Yu fast test examination instrument can be promoted.
Patent CN102135518B discloses a kind of detecting electrode and preparation method thereof for trace lead in drinking water, should
Nafion- carbon nanotube mixing dressing agent is covered on electrode working electrode reaction zone, by by the carbon nanometer after oxidation processes
Pipe is scattered in the ethanol solution of Nafion, and is added dropwise in obtaining detecting electrode on the electrode working zone being completed, and is detected
Limit is lower than 0.01mg/L, and detection time is lower than 5min.But this method higher cost, complex process, in detection accuracy and sound
Also and not up to top standard is answered in speed, industrialization is not suitable for, is unfavorable for the mating research and development of the fast test examination instrument of micro lead in water.
In conclusion there are requirement particular detection environment, needing large-scale instrument for the detection of micro lead in water body at present
Device needs the problems such as pre-treatment step, therefore this patent problem to be solved is to provide one kind with highly sensitive, high stable
Property, low cost, the detecting electrode that small hand-held instrument and electrochemical workstation can be cooperated.
Summary of the invention
The object of the present invention is to provide a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water.
The highly integrated electrode matrix surface of bismuth film provided by the invention is equipped with buffer layer；, electrode matrix surface or buffer layer table
Face is equipped with layer and skin；Conductive layer surface is equipped with conversion zone.Buffer layer is at least two formation in Ti, W, Mo
Alloy-layer；Layer is layers of copper；Skin is layer gold.Buffer layer thickness is 5~50 μm；Layer with a thickness of 35~
40μm；Skin is with a thickness of 0.5~3.0 μm.
The highly integrated electrode of bismuth film provided by the invention uses three-electrode system, respectively working electrode, reference electrode with it is right
Electrode.Wherein working electrode plates bismuth film, and reference electrode plates silver-silver chloride, to electrode platinum plating.Three electrodes are generally aligned in the same plane, work
Make electrode and to the distance of electrode between 50~100 μm.
The highly integrated electrode of bismuth film takes the coplanar system of three electrodes, and fixed interelectrode distance is smaller, reduces concentration polarization,
Effectively improve electrode detection accuracy.
The highly integrated electrode of bismuth film is interdigital electrode, and interdigital electrode detection zone is as working electrode and USB port conducting shell
It is connected, ink box dam is equipped with around interdigital electrode detection zone, prevents testing liquid from overflowing electrode detection region.
The highly integrated electrode of bismuth film can be used cooperatively with small handheld instrument, directly be carried out in any environment to water body
Immediately detection, and can directly be connect with the USB interface of electrochemical workstation, instantaneous transmission data.
The present invention carries out the modification of bismuth film on FR-4 interdigital electrode surface using preplating bismuth embrane method, and detects aqueous solution with this
In micro lead element, compared with the electrode of prior art preparation, bismuth film electrode prepared by the present invention possess lower processing cost,
More environmentally friendly friendly process and higher sensitivity.
It is a further object of the present invention to provide a kind of for measuring the preparation method of the bismuth film electrode of micro lead in water.
The technical solution that the preparation of bismuth film electrode of the invention is taken includes the following steps:
S1: electrode of the substrate is pre-processed；
S2: pretreated electrode of the substrate is put into plating bismuth solution, bismuth film electrode is made in plating.
The electrode of the substrate that the present invention uses is high molecular polymer or ceramic interdigital electrode, it is contemplated that electrode performance at
This, selects FR-4 interdigital electrode as electrode of the substrate, and Modified Bismuth film is electroplated in electrode of the substrate, and traditional mercury film is substituted with this
Electrode prepares environmental-friendly type electrode.
In step S1 of the present invention, electrode of the substrate pretreatment the following steps are included:
(1) electrode of the substrate is placed in ethanol solution, is cleaned by ultrasonic 30min；
(2) processed electrode of the substrate is put into the ammonium persulfate mixed solution of 10% sulfuric acid solution and 10g/L, is impregnated
30~60s is washed with deionized water.
It is electrode surface oil removal treatment that electrode of the substrate, which is placed in ethanol solution and is cleaned by ultrasonic, and electrode is avoided before plating
The greasy dirt on surface interferes；Electrode of the substrate after oil removing is impregnated in sulfuric acid solution, can remove surface rusty stain and oxide,
It prepares for bismuth film is electroplated in next step.
The present invention prepares bismuth film electrode using preplating bismuth embrane method, the electrochemical parameter and bismuth when can be electroplated by changing from
The concentration adjustment plating bismuth effect of son.
In step S2 of the present invention, the solution composition of plating are as follows: bismuth nitrate 0.2mol/L, lithium bromide 0.5mol/L, nitric acid
0.5mol/L, hydrogen chloride 0.5mol/L, sodium chloride 0.5mol/L, citric acid 20g/L, ethylenediamine tetra-acetic acid 10g/L.
In step S2 of the present invention, electroplating time is 120s~300s, and preferably 180s, current density is 1.3~1.5ASD,
Preferably 1.4ASD.
It is a further object of the present invention to provide a kind of for measuring answering for the preparation method of the bismuth film electrode of micro lead in water
Use method.
For the present invention using the micro lead in Voltammetry water body, detection mechanism is as follows:
(1) enriching step, Pb2+It is reduced to form lead bismuth alloy；
(2) lead is reoxidized and in rework solution: Pb (Bi) → Pb2++2e-.In this step, the amount of lead element is by making
It is determined with sensitive electrochemical techniques, such as linear voltammetric scan method (LSV), differential pulse voltammetry (DPV) or square wave volt-ampere
Method (SWV) etc..
The present invention measures electrode detection curve using stripping voltammetry (ASV).
Electro-chemical test of the invention is carried out in three-electrode system, and wherein bismuth film electrode is working electrode, and platinum electrode is
To electrode, silver-silver chloride electrode is reference electrode, and test solution is the 0.1M NaAc_HAc buffer solution that pH is 3.5.
Electro-chemical test of the invention uses stripping voltammetry, and scanning current potential is -0.9V~-0.2V, and scanning speed is
100mV/s, electro-chemical test environment maintain 25 ± 2 DEG C of room temperature.
The highly integrated electrode of bismuth film prepared by the present invention can accurately measure the micro lead in water body.
The highly integrated electrode of bismuth film prepared by the present invention can be matched with small handheld instrument, before without preceding processing
It puts and quickly detection is carried out immediately to the micro lead in water body.
The highly integrated electrode of bismuth film prepared by the present invention can be directly connected with electrochemical workstation by USB interface, be realized real
When data association.
The highly integrated electrode of bismuth film prepared by the present invention is right to when the range of linearity of micro lead in water body is 1.0~20 μM
Answering sensitivity is 1ppm.
The beneficial effects of the present invention are:
(1) present invention uses the coplanar system of three electrodes, by reducing interelectrode fixed range, greatly reduces concentration polarization
Change, to improve the accuracy of electrode detection.
(2) present invention has abandoned traditional mercury film electrode, simple process, cost using bismuth film electrode as working electrode
It is lower, to more environment-friendly.
(3) the highly integrated electrode of bismuth film of the invention can cooperate with small handheld instrument, and micro lead is in realization water body
When quickly detect, be not necessarily to precondition and large-scale instrument, environmental requirement, realize the quick instant detection of lead element, can be used for
The multiple fields such as food safety, environmental monitoring, geology detecting.
Detailed description of the invention
Invention is described further using attached drawing, but the embodiments in the accompanying drawings do not constitute any limitation to the present invention,
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to the following drawings
Its attached drawing.
Fig. 1 is the highly integrated electrode of bismuth film obtained in FR-4 electrode surface plating bismuth film.
Fig. 2 is the detection of (a) common bismuth film electrode bismuth film interdigital electrode coplanar with (b) three electrode under equal conditions
Stripping Voltammetry curve can be compared.
Fig. 3 is lead element measurement Stripping Voltammetry curve of the highly integrated electrode of bismuth film in 0.1M Acetic acid-sodium acetate solution.
Fig. 4 is that the highly integrated electrode of bismuth film lies prostrate the dissolution of the lead element of various concentration in 0.1M Acetic acid-sodium acetate solution
Pacify curve.
Fig. 5 is the stability test of the highly integrated electrode of bismuth film.
Fig. 6 is the standard Stripping Voltammetry curve of micro lead in the highly integrated determination of electrode water body of bismuth film.
Fig. 7 be electroplating time be 10min when bismuth film electrode.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
It is a kind of for measuring the preparation method of the highly integrated electrode of bismuth film of micro lead in water, specifically includes the following steps:
S1: electrode of the substrate is pre-processed；
S2: pretreated electrode of the substrate is put into plating bismuth solution, bismuth film electrode is made in plating.
Further, electrode of the substrate used in process made above is high score sub-electrode, preferably FR-4 electrode.
Further, in step S1, electrode of the substrate pretreatment the following steps are included:
(1) electrode of the substrate is placed in ethanol solution, is cleaned by ultrasonic 30min；
(2) electrode of the substrate for crossing aforementioned processing is put into the ammonium persulfate mixed solution of 10% sulfuric acid solution and 10g/L,
30~60s is impregnated, is washed with deionized water.
Further, in step S2, the solution composition of bismuth is electroplated are as follows: bismuth nitrate 0.2mol/L, lithium bromide 0.5mol/L, nitric acid
0.5mol/L, hydrogen chloride 0.5mol/L, sodium chloride 0.5mol/L, citric acid 20g/L, ethylenediamine tetra-acetic acid 10g/L.
Further, in step S2, electroplating time is 120s~300s, and current density is 1.3~1.5ASD；Preferably, it walks
In rapid S2, electroplating time 180s, current density 1.4ASD.
The contents of the present invention are described in further detail below by way of specific embodiment.
Embodiment 1
The preparation of the highly integrated electrode of bismuth film:
The coplanar interdigital electrode of tri- electrode of FR-4 is placed in ethanol solution, puts it into 10% sulfuric acid after being cleaned by ultrasonic 30min
In the ammonium persulfate mixed solution of solution and 10g/L, 60s is impregnated, is washed with deionized water spare.By pretreated FR-4 electricity
Pole is put into plating bismuth solution, and the interdigital detection zone as working electrode is electroplated, and bismuth film electrode is made, and electroplating solution group becomes nitre
Sour bismuth 0.2mol/L, lithium bromide 0.5mol/L, nitric acid 0.5mol/L, hydrogen chloride 0.5mol/L, sodium chloride 0.5mol/L, citric acid
20g/L, ethylenediamine tetra-acetic acid 10g/L, electroplating time 180s, current density 1.4ASD take out electrode after plating, use
Deionized water is rinsed three times, and the highly integrated electrode of bismuth film is obtained.
It is to electrode with platinum, silver-silver chloride is reference electrode, and bismuth film electrode is working electrode, and it is 3.5 that test solution, which is pH,
0.1M NaAc_HAc buffer solution, scanning current potential be -0.9V~-0.2V, scanning speed 100mV/s, electro-chemical test
Environment carries out stripping voltammetry test under conditions of maintaining 25 ± 2 DEG C of room temperature.
Embodiment 2
Detection of the highly integrated electrode of bismuth film to micro lead in water:
The highly integrated electrode of bismuth film is prepared according to the step of embodiment 1, and is put into 0.1M NaAc_HAc buffer solution
(pH3.5) in, and 50mg/L lead ion solution is added, tests its Stripping Voltammetry curve graph and is compared with plain buffer, obtained
Test result such as attached drawing 3.Visible lead ion has apparent oxidation peak on the highly integrated electrode of bismuth film in figure, according to test result,
It can be concluded that the highly integrated electrode of bismuth film of the invention can be used for the measurement of micro lead in water body.
Embodiment 3
Quantitative test of the highly integrated electrode of bismuth film to micro lead in water:
The highly integrated electrode of bismuth film is prepared according to the step of embodiment 1, and is put into 0.1M NaAc_HAc buffer solution
(pH3.5) in, and lead at different concentrations solion is added, tests its Stripping Voltammetry curve graph, obtain test result such as attached drawing 4.
The oxidation peak of visible lead ion is lifted as plumbum ion concentration increases in figure, and oxidation current also increases, according to test
As a result, it can be concluded that the highly integrated electrode of bismuth film of the invention can be within the scope of a certain concentration for the micro lead in water body
Carry out the metastable measurement of essence.
Embodiment 4
The stability test of the highly integrated electrode of bismuth film:
The highly integrated electrode of bismuth film is prepared according to the step of embodiment 1, and is put into 0.1M NaAc_HAc buffer solution
(pH3.5) in, and a certain amount of lead ion solution is added and carries out Stripping Voltammetry test, and continues 3000s, scanning voltage is -0.9V
~-0.2V obtains test result such as attached drawing 5.According to test result, it can be deduced that conclusion: the highly integrated electrode of bismuth film of the invention
In the case where continuous work, there is no obvious decaying for reactivity, are suitable for long-term measurement, stability with higher.
Embodiment 5
The standard curve determination of micro lead in the highly integrated electrode detection water of bismuth film:
The highly integrated electrode of bismuth film is prepared according to the step of embodiment 1, and is put into 0.1M NaAc_HAc buffer solution
(pH3.5) in, its Stripping Voltammetry curve in various concentration lead ion is tested, plumbum ion concentration range is 1.0~50mg/L,
Scanning voltage is -0.9V~-0.2V, and scanning speed 100mV/s obtains test result attached drawing 6.According to the meter of standard curve
It calculates, it can be deduced that the conclusion: (R within the scope of 1.0~20mg/L concentration gradient2=0.982), the highly integrated electrode of bismuth film of the invention
Detection sensitivity can reach 1ppm.
Comparative example
The preparation of common bismuth film electrode:
FR-4 single electrode is placed in ethanol solution, its back side glue is sealed after being cleaned by ultrasonic 30min, reserves front electroplating region
Domain is put into the ammonium persulfate mixed solution of 10% sulfuric acid solution and 10g/L, is impregnated 60s, is washed with deionized water spare.
It is to electrode with platinum, silver-silver chloride is reference electrode, and bismuth film electrode is working electrode, and it is 3.5 that test solution, which is pH,
0.1M NaAc_HAc buffer solution, scanning current potential be -0.9V~-0.2V, scanning speed 100mV/s, electro-chemical test
Environment carries out stripping voltammetry test under conditions of maintaining 25 ± 2 DEG C of room temperature.
The coplanar highly integrated interdigital electrode of bismuth film of three electrodes made from common bismuth film electrode made from comparative example and embodiment 1 is gathered around
There is the working electrode of identical size and area, two kinds of electrodes are placed in 0.1M NaAc_HAc buffer solution, adds same dense
The lead ion solution of degree carries out the Stripping Voltammetry test that both sides measure the comparison of lead element ability, obtains test result such as attached drawing 2.
It is seen that the dissolution peak peak type of the coplanar bismuth film interdigital electrode of three electrode of Fig. 2 (b) is more prominent, and Fig. 2 (a) is common
The dissolution peak of bismuth film electrode is comparatively gentle, it may be said that the interdigitation bismuth film height collection of three-electrode structure prepared by bright embodiment 1
It is sensitiveer at response of the electrode for lead ion, in terms of measuring plumbum ion concentration advantageously.
Phenetic analysis
Attached drawing 1 is the schematic diagram of the highly integrated electrode of bismuth film prepared in embodiment 1.Electrode uses three-electrode system, including
Working electrode, reference electrode and to electrode.Wherein working electrode plates bismuth film, and reference electrode plates silver-silver chloride, to electrode platinum plating,
Three electrode runs parallels are integrated, and electrode ports are adapted to USB interface in the same plane, can directly be connect with electrochemical workstation,
It realizes detection immediately and transmitting detection data, can also be used cooperatively with small handheld instrument, realize not examined environment limit
The instant quick detection of system.
Attached drawing 2 is the common bismuth film of three electrodes of the preparation of embodiment 1 coplanar bismuth film interdigital electrode (b) and comparative example preparation
Comparison of the electrode (a) under identical conditions to the measurement ability of the lead ion in water body.As it can be seen that both having more bright in figure
Aobvious dissolution peak, can determine both have measurement water body in micro lead ability, wherein three electrodes it is coplanar bismuth film it is interdigital
The dissolution peak of electrode (b) is more prominent, and the dissolution peak of common bismuth film electrode (a) is comparatively gentle, illustrates bismuth of the invention
The highly integrated electrode of film possesses faster response speed and higher sensitivity.This is because present invention employs the coplanar bodies of three electrodes
Three electrode runs parallels are set to same plane and substantially reduce and fix interelectrode line space, greatly reduce concentration polarization by system
Change, improves the detection performance of electrode.The sensitivity of electrode and accurate also greatly improved in the interdigital structure of detecting electrode simultaneously
Property.
Attached drawing 3 is the highly integrated electrode of bismuth film of the preparation of embodiment 1 in 0.1M NaAc_HAc buffer solution (pH3.5)
The Stripping Voltammetry curve graph before and after 50mg/L lead ion solution, scanning speed 50mV/s is added.The oxygen of visible lead ion in figure
Change peak and be approximately located i -0.55V or so, lead ion shows oxidation spike potential very more outstanding than blank solution on the electrode, says
The bright highly integrated electrode of bismuth film of the invention can be used for the measurement of micro lead in water body.
Attached drawing 4 is 0.1M Acetic acid-sodium acetate of the highly integrated electrode of bismuth film in the lead ion containing various concentration of the preparation of embodiment 1
Stripping Voltammetry curve graph in buffer solution (pH3.5), scanning speed 50mV/s.It is visible as plumbum ion concentration increases in figure
Add, the oxidation peak positioned at -0.55V or so is gradually lifted, lead ion solution of the oxidation current in 10~80mg/L concentration ranges
In linearly increase with concentration, calculate (R according to linear2=0.997), detection sensitivity can reach 1ppm, illustrate the present invention
The highly integrated electrode of bismuth film can carry out the metastable measurement of essence for the micro lead in water body within the scope of a certain concentration.
Attached drawing 5 is the stability test of the highly integrated electrode of bismuth film prepared by embodiment 1, specifically in -0.9V~-0.2V
It is put under scanning voltage in 0.1M NaAc_HAc buffer solution (pH3.5), and a certain amount of lead ion solution is added and carries out
Stripping Voltammetry test, and continues 3000s, and records data according to scanning circle number scale, take respectively the 10th circle, the 50th circle, the 100th circle,
The scan image of 150th circle compares.In figure as it can be seen that as the increase of number, the extension of testing time, electrode dissolution are enclosed in scanning
Peak gradually becomes smaller, and peak current also gradually becomes smaller, but its amplitude of variation is little, and value illustrates bismuth film of the invention within 10%
For highly integrated electrode in the case where continuous work, there is no obvious decaying for reactivity, are suitable for long-term measurement, have higher
Stability.
Attached drawing 6 is the standard curve determination of micro lead in the highly integrated determination of electrode water body of bismuth film of the preparation of embodiment 1, specifically
It is to test its Stripping Voltammetry curve in various concentration lead ion in 0.1M NaAc_HAc buffer solution (pH3.5),
Plumbum ion concentration range is 1.0~50mg/L, and scanning voltage is -0.9V~-0.2V, scanning speed 100mV/s.Obtain difference
Peak current data under plumbum ion concentration are as follows:
And standard curve is drawn according to upper table data.It can be seen that plumbum ion concentration be 1.0~20mg/L and 10~
In the concentration range of 50mg/L, plumbum ion concentration and peak current possess linear relationship.It is calculated according to linear, in 1.0~20mg/L
(R within the scope of concentration gradient2=0.982), electrode detection sensitivity can reach 1ppm.
Attached drawing 7 is plating bismuth pole picture of the common bismuth film electrode of the preparation of comparative example 1 when electroplating time is 10min, bismuth
Film is integrally in silver color, is uniformly attached on electrode conducting layer.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the embodiments can also be by appropriately combined, formation those skilled in the art
The other embodiments that member is understood that.The technical detail being not described in detail in the present invention can pass through appointing in this field
One prior art is realized.Particularly, all technical characterstics being not described in detail can pass through any prior art reality in the present invention
It is existing.
Claims (10)
1. a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that the electrode matrix surface is equipped with
Buffer layer；The electrode matrix surface or the buffer-layer surface are equipped with layer and skin；The conductive layer surface
Equipped with conversion zone；The electrode matrix is any one of high molecular polymer or ceramics；The buffer layer is in Ti, W, Mo
At least two alloy-layers formed；The layer is layers of copper；The skin is layer gold；The buffer layer thickness is 5
~50 μm；The layer is with a thickness of 35~40 μm；The skin is with a thickness of 0.5~3.0 μm.
2. according to claim 1 a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that institute
Electrode is stated for working electrode, reference electrode and to the coplanar Integrated electrode of electrode, wherein the working electrode conversion zone is bismuth
Film, described is platinum to electrode reaction layer, and the reference electrode conversion zone is silver-silver chloride.
3. according to claim 1 a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that institute
Working electrode and the distance to electrode are stated between 50~100 μm.
4. according to claim 1 a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that institute
Stating electrode is interdigital electrode, is equipped with ink box dam around the interdigital electrode detection zone.
5. it is according to claim 1 a kind of for measuring the preparation method of the highly integrated electrode of bismuth film of micro lead in water,
It is characterized in that, comprising the following steps:
S1, electrode of the substrate is pre-processed；
S2: the pretreated electrode of the substrate is put into plating bismuth solution, bismuth film electrode is made in plating.
6. it is according to claim 5 a kind of for measuring the preparation method of the highly integrated electrode of bismuth film of micro lead in water,
Be characterized in that, in step S1, electrode of the substrate pretreatment the following steps are included:
(1) electrode of the substrate is placed in ethanol solution, is cleaned by ultrasonic 30min；
(2) the processed electrode of the substrate is put into the ammonium persulfate mixed solution of 10% sulfuric acid solution and 10g/L, is impregnated
30~60s is washed with deionized water.
7. it is according to claim 5 a kind of for measuring the preparation method of the highly integrated electrode of bismuth film of micro lead in water,
It is characterized in that, in step S2, the solution composition of the plating are as follows: bismuth nitrate 0.2mol/L, lithium bromide 0.5mol/L, nitric acid
0.5mol/L, hydrogen chloride 0.5mol/L, sodium chloride 0.5mol/L, citric acid 20g/L, ethylenediamine tetra-acetic acid 10g/L.
8. it is according to claim 5 a kind of for measuring the preparation method of the highly integrated electrode of bismuth film of micro lead in water,
It is characterized in that, in step S2, the electroplating time is 120s~300s, and current density is 1.3~1.5ASD.
9. according to claim 1 a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that institute
Stating bismuth film electrode can be used for detecting micro lead in water.
10. according to claim 1 a kind of for measuring the highly integrated electrode of bismuth film of micro lead in water, which is characterized in that
The bismuth film electrode is 1ppm to the detection sensitivity of micro lead in water.
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| CN113702456A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Bismuth film modified electrode for heavy metal detection and preparation method thereof |
| CN113702477A (en) * | 2021-04-30 | 2021-11-26 | 广州钰芯智能科技研究院有限公司 | Gold film modified electrode for heavy metal detection and preparation method thereof |
| CN113804627A (en) * | 2021-09-14 | 2021-12-17 | 广东中图半导体科技股份有限公司 | Semiconductor photoelectrochemical sensor and preparation method thereof |
| CN114002285A (en) * | 2021-10-19 | 2022-02-01 | 广州钰芯智能科技研究院有限公司 | Polyaniline-nano bismuth composite electrode for heavy metal detection and preparation method thereof |
| CN115047053A (en) * | 2022-04-13 | 2022-09-13 | 哈尔滨工业大学 | Preparation method of bismuth-containing screen-printed electrode and application of bismuth-containing screen-printed electrode in heavy metal ion detection |
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