CN109085227A - It is a kind of for the hydroxyapatite films electrode of detection of heavy metal ion, preparation method and applications - Google Patents

It is a kind of for the hydroxyapatite films electrode of detection of heavy metal ion, preparation method and applications Download PDF

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CN109085227A
CN109085227A CN201810693693.5A CN201810693693A CN109085227A CN 109085227 A CN109085227 A CN 109085227A CN 201810693693 A CN201810693693 A CN 201810693693A CN 109085227 A CN109085227 A CN 109085227A
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CN109085227B (en
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李子亨
孙明旭
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Jilin University
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    • 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
    • G01N27/28—Electrolytic cell components
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    • G01N27/333—Ion-selective electrodes or membranes
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N27/416—Systems
    • G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage

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Abstract

It is a kind of for the hydroxyapatite films electrode of detection of heavy metal ion, preparation method and applications, belong to thin-film material technical field.It is using ito glass as cathode, platinum electrode is as anode, 0.05~0.20M calcium nitrate, 0.015~0.60M diammonium hydrogen phosphate, 0.015~0.60M phosphoric acid mixed solution as electrolyte, the calcium-phosphorus ratio of electrolyte solution is 5:3, the hydroxyapatite films electrode of micro/nano-scale belt structure is obtained by electro-deposition hydroxyapatite, film thickness is 5~35 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, and sedimentation potential is 1.5~2.5V, and sedimentation time is 30~180min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 40~80 DEG C.Hydroxyapatite films electrode prepared by the present invention can be used as heavy metal ion sensor and be applied in heavy metal analysis, and heavy metal ion is lead, copper or the mercury of divalent, and concentration is 0.1~10.0 μM.

Description

It is a kind of for the hydroxyapatite films electrode of detection of heavy metal ion, preparation method And its application
Technical field
The invention belongs to thin-film material technical fields, and in particular to a kind of hydroxyapatite for detection of heavy metal ion Membrane electrode, preparation method and applications.
Background technique
Because heavy metal has high toxicity to human health and the ecosystem, the pollution of heavy metal causes people's Pay much attention to.In each heavy metal species, three kinds of stronger divalent heavy metal ions of toxicity are lead, copper and mercury.It is reported that divalent The accumulation of lead ion can cause various illeffects in human body, such as injury of kidney, anaemia, the loss of memory or even cancer.In addition, Although bivalent cupric ion be to human body it is essential, excess will lead to health problem, such as lung cancer and hepar damnification.It is low dense The dimercurion of degree can also damage central nervous system, brain, kidney and lung.
Currently, the detection of heavy metal ion be usually atomic absorption spectrography (AAS), atomic fluorescence spectrometry, inductive coupling etc. from Daughter mass spectrography etc. is some to be needed expensive instrument, takes considerable time, is inconvenient to the method disposed.Since electrochemical techniques have There are at low cost, high sensitivity, good portability, it is considered to be a kind of effective detection method.
Recently, the electrode of a variety of materials modification is widely used in detection of heavy metal ion.The hydroxyl phosphorus of electrodeposition process preparation The electrode of lime stone modification can provide uniform surface topography, big area and volume ratio and high conductivity, for improving a huge sum of money The detection performance for belonging to ion is extremely important.
Summary of the invention
The present invention be directed to problems of the existing technology, provide a kind of with good stability, highly sensitive and low Cost for the hydroxyapatite films electrode of detection of heavy metal ion, preparation method and applications.With the electrode to difference Divalent heavy metal ions lead, copper and the mercury of concentration are detected, and can monitor each huge sum of money by the variation of response current intensity Belong to the variation of ion concentration.
To achieve the goals above, a kind of hydroxyapatite films electricity for detection of heavy metal ion of the present invention The preparation method of pole, it is characterised in that: in sedimentation basin, using ito glass as cathode, platinum electrode is anode, calcium nitrate, phosphoric acid hydrogen Diammonium, phosphoric acid mixed aqueous solution be electrolyte, obtain hydroxyapatite films electricity by being electrodeposited on ITO cathode deposition Pole；The calcium-phosphorus ratio of electrolyte solution be 5:3, gained hydroxyapatite films electrode with a thickness of 5~35 μm；The current potential of electro-deposition It is to be regulated and controled by D.C. regulated power supply, sedimentation basin, which is placed in water-bath, when deposition heats.
In the above method, nitric acid calcium concentration is 0.05M~0.2M.
In the above method, diammonium hydrogen phosphate concentration is 0.015M~0.06M.
In the above method, phosphoric acid concentration is 0.015M~0.06M.
In the above method, hydroxyapatite films are micro/nano-scale belt structure, and bandwidth is 0.85~3 μm, with a length of 1 ~30 μm, band thickness is 50~200nm.
In the above method, electro-deposition current potential is 1.5~2.5V.
In the above method, electrodeposition time is 30~180min.
In the above method, bath temperature is 40~80 DEG C.
Hydroxyapatite films electrode prepared by the present invention can be used as heavy metal ion sensor and obtain in heavy metal analysis To application.
The application is using hydroxyapatite films electrode as working electrode, and platinum electrode is used as to electrode, saturation Calomel electrode is as reference electrode, and for Applied Electrochemistry work station under differential pulse voltammetry test method, monitoring current response is strong Degree changes with concentration of heavy metal ion, to realize the detection to concentration of heavy metal ion.
Above-mentioned application, the current potential of differential pulse volt are -0.80~0.50V.
Above-mentioned application, heavy metal ion are lead, copper or the mercury of divalent.
Above-mentioned application, the concentration of heavy metal ion are 0.1~10.0 μM.
Hydroxyapatite films electrode prepared by the present invention is as heavy metal ion sensor to responding heavy metal ion Principle: the ion with negative electrical charge of electrode surface first by it is heavy metal ion adsorbed arrive electrode surface, then make current potential from negative sense just Scanning dissolves out its self-electrode, and records electric current-potential curve of process in leaching.Under certain condition its peak height and metal from Sub- concentration is in a linear relationship, and different ions have different spike potentials in certain electrolyte.
The beneficial effects of the present invention are: the present invention is based on the hydroxyapatite films electrodes of electrodeposition process preparation to provide Uniform surface topography, big area and volume ratio and high conductivity, with good stability, highly sensitive and low cost. Preparation method simple process, easily operated, preparation cost is low, easy to spread.
Detailed description of the invention
In order to illustrate more clearly of the technical solution in the present invention and its performance of material is prepared, implementation is given below The relevant indicators of example 1.
Fig. 1 is the X-ray electronic diffraction map of hydroxyapatite films electrode
Fig. 2 is the scanning electron microscope diagram spectrum of hydroxyapatite films electrode.
Fig. 3 is that electric current-current potential of the hydroxyapatite films electrode in 0.1~1.0 μM of concentration range of lead (II) ion is bent The linear relationship map (illustration) of line and concentration and current-responsive.
Fig. 4 is electric current-current potential of the hydroxyapatite films electrode in 3.0~10.0 μM of concentration ranges of lead (II) ion The linear relationship map (illustration) of curve and concentration and current-responsive.
Fig. 5 is that electric current-current potential of the hydroxyapatite films electrode in 0.1~1.0 μM of concentration range of bivalent cupric ion is bent The linear relationship map (illustration) of line and concentration and current-responsive.
Fig. 6 is electric current-current potential of the hydroxyapatite films electrode in 1.0~10.0 μM of concentration ranges of bivalent cupric ion The linear relationship map (illustration) of curve and concentration and current-responsive.
Fig. 7 is that electric current-current potential of the hydroxyapatite films electrode in 0.1~1.0 μM of concentration range of dimercurion is bent The linear relationship map (illustration) of line and concentration and current-responsive.
Fig. 8 is electric current-current potential of the hydroxyapatite films electrode in 1.0~10.0 μM of concentration ranges of dimercurion The linear relationship map (illustration) of curve and concentration and current-responsive.
The diffraction peak of target electrode hydroxyapatite and PDF card it can be seen from the X-ray electronic diffraction map of Fig. 1 The characteristic peak of the standard diagram of 09-0432 is corresponding.
Target electrode is the banded hydroxy-apatite of micro/nano-scale it can be seen from the scanning electron microscope diagram spectrum of Fig. 2 Stone membrane electrode.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 3 and the linear relationship map of current-responsive There are very high sensitivity and response current intensity, and lead (II) ion to lead (II) ion in 0.1~1.0 μM of concentration range Concentration and current-responsive intensity have good linear relationship.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 4 and the linear relationship map of current-responsive Have very high sensitivity and response current intensity to lead (II) ion in 3.0~10.0 μM of concentration ranges, and divalent lead from The concentration and current-responsive intensity of son have good linear relationship.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 5 and the linear relationship map of current-responsive There are very high sensitivity and response current intensity, and bivalent cupric ion to bivalent cupric ion in 0.1~1.0 μM of concentration range Concentration and current-responsive intensity have good linear relationship.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 6 and the linear relationship map of current-responsive Have very high sensitivity and response current intensity to bivalent cupric ion in 1.0~10.0 μM of concentration ranges, and cupric from The concentration and current-responsive intensity of son have good linear relationship.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 7 and the linear relationship map of current-responsive There are very high sensitivity and response current intensity, and dimercurion to dimercurion in 0.1~1.0 μM of concentration range Concentration and current-responsive intensity have good linear relationship.
The target electrode it can be seen from the electric current-potential curve and concentration of Fig. 8 and the linear relationship map of current-responsive Have very high sensitivity and response current intensity to dimercurion in 1.0~10.0 μM of concentration ranges, and bivalent mercury from The concentration and current-responsive intensity of son have good linear relationship.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but the invention is not limited to these embodiments.
Embodiment 1:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 2:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.10M, diammonium hydrogen phosphate 0.030M, phosphoric acid The mixed aqueous solution of 0.030M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 9 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 3:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.15M, diammonium hydrogen phosphate 0.045M, phosphoric acid The mixed aqueous solution of 0.045M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 11 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 4:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.20M, diammonium hydrogen phosphate 0.060M, phosphoric acid The mixed aqueous solution of 0.060M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 13 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 5:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.15V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 6:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.17V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 7:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.19V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 8:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.21V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 9:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.23V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 10:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.25V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 11:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 13 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 60min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 12:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 24 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 120min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 13:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 35 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 180min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 60 DEG C.
Embodiment 14:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 5 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 40 DEG C.
Embodiment 15:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 6 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 50 DEG C.
Embodiment 16:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 70 DEG C.
Embodiment 17:
Using ito glass as cathode, platinum electrode is as anode, calcium nitrate 0.05M, diammonium hydrogen phosphate 0.015M, phosphoric acid The mixed aqueous solution of 0.015M is as electrolyte, and calcium-phosphorus ratio 5:3, electro-deposition obtains hydroxyapatite films on ITO cathode Electrode, gained film thickness are 7 μm.Sedimentation potential is regulated and controled by D.C. regulated power supply, sedimentation potential 0.20V, deposition Time is 30min, and sedimentation basin, which is placed in water-bath, when deposition heats, and temperature is controlled at 80 DEG C.

Claims (8)

1. a kind of preparation method of the hydroxyapatite films electrode for detection of heavy metal ion, it is characterised in that: depositing Chi Zhong, using ito glass as cathode, platinum electrode is anode, calcium nitrate, diammonium hydrogen phosphate, phosphoric acid mixed aqueous solution be electrolyte, Hydroxyapatite films electrode is obtained by being electrodeposited in deposition on ITO cathode；The calcium-phosphorus ratio of electrolyte solution is 5:3, gained Hydroxyapatite films electrode with a thickness of 5~35 μm；The current potential of electro-deposition is regulated and controled by D.C. regulated power supply, when deposition Sedimentation basin is placed in water-bath and heats.
2. a kind of preparation method of the hydroxyapatite films electrode for detection of heavy metal ion as described in claim 1, It is characterized by: nitric acid calcium concentration is 0.05M~0.2M, diammonium hydrogen phosphate concentration is 0.015M~0.06M, and phosphoric acid concentration is 0.015M~0.06M.
3. a kind of preparation method of the hydroxyapatite films electrode for detection of heavy metal ion as described in claim 1, It is characterized by: electro-deposition current potential is 1.5~2.5V, electrodeposition time is 30~180min.
4. a kind of preparation method of the hydroxyapatite films electrode for detection of heavy metal ion as described in claim 1, It is characterized by: bath temperature is 40~80 DEG C.
5. a kind of hydroxyapatite films electrode for detection of heavy metal ion, it is characterised in that: be by Claims 1 to 4 Method described in any one is prepared.
6. a kind of hydroxyapatite films electrode for detection of heavy metal ion described in claim 5 is in heavy metal analysis Application.
7. a kind of hydroxyapatite films electrode for detection of heavy metal ion as claimed in claim 6 is in heavy metal analysis In application, it is characterised in that: heavy metal ion be divalent lead, copper or mercury.
8. a kind of hydroxyapatite films electrode for detection of heavy metal ion as claimed in claim 6 is in heavy metal analysis In application, it is characterised in that: the concentration of heavy metal ion be 0.1~10.0 μM.
CN201810693693.5A 2018-06-29 2018-06-29 Hydroxyapatite film electrode for heavy metal ion detection, preparation method and application thereof Active CN109085227B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111135801A (en) * 2020-01-19 2020-05-12 浙江大学 Preparation method of hydroxyapatite flat plate wire composite material with heavy metal adsorption function

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111135801A (en) * 2020-01-19 2020-05-12 浙江大学 Preparation method of hydroxyapatite flat plate wire composite material with heavy metal adsorption function
CN111135801B (en) * 2020-01-19 2021-06-01 浙江大学 Preparation method of hydroxyapatite flat plate wire composite material with heavy metal adsorption function

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