CN109085227B - Hydroxyapatite film electrode for heavy metal ion detection, preparation method and application thereof - Google Patents
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Abstract
A hydroxyapatite membrane electrode for heavy metal ion detection, a preparation method and application thereof belong to the technical field of membrane materials. The method comprises the following steps of taking ITO glass as a cathode, a platinum electrode as an anode, and a mixed solution of 0.05-0.20M of calcium nitrate, 0.015-0.60M of diammonium hydrogen phosphate and 0.015-0.60M of phosphoric acid as an electrolyte, wherein the calcium-phosphorus ratio of the electrolyte solution is 5: and 3, electrodepositing hydroxyapatite to obtain the hydroxyapatite membrane electrode with the micro-nano scale strip-shaped structure, wherein the thickness of the membrane is 5-35 μm. The deposition potential is regulated and controlled by a direct current stabilized voltage power supply, the deposition potential is 1.5-2.5V, the deposition time is 30-180 min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled to be 40-80 ℃. The hydroxyapatite membrane electrode prepared by the invention can be used as a heavy metal ion sensor to be applied to heavy metal detection, wherein the heavy metal ions are bivalent lead, copper or mercury, and the concentration is 0.1-10.0 mu M.
Description
Technical Field
The invention belongs to the technical field of film materials, and particularly relates to a hydroxyapatite film electrode for heavy metal ion detection, a preparation method and application thereof.
Background
Heavy metal pollution has attracted much attention because of its high toxicity to human health and the ecosystem. Among the heavy metals, the three more toxic divalent heavy metal ions are lead, copper and mercury. It has been reported that the accumulation of divalent lead ions can cause various harmful effects in humans, such as kidney damage, anemia, memory loss, and even cancer. In addition, although divalent copper ions are essential for the human body, their excess can lead to health problems, such as lung cancer and liver damage. Low concentrations of divalent mercury ions can also damage the central nervous system, brain, kidney, and lung.
At present, the detection of heavy metal ions is generally a method which requires expensive instruments, consumes a lot of time and is inconvenient to install, such as atomic absorption spectrometry, atomic fluorescence spectrometry, inductively coupled plasma mass spectrometry and the like. The electrochemical technology has the advantages of low cost, high sensitivity, good portability and the like, and is considered to be an effective detection method.
Recently, electrodes modified with various materials have been widely used for heavy metal ion detection. The hydroxyapatite modified electrode prepared by the electrodeposition method can provide uniform surface morphology, large area-to-volume ratio and high conductivity, and is very important for improving the detection performance of heavy metal ions.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a hydroxyapatite membrane electrode for heavy metal ion detection, which has good stability, high sensitivity and low cost, a preparation method and application thereof. The electrode is used for detecting the divalent heavy metal ions of lead, copper and mercury with different concentrations, and the change of the concentration of each heavy metal ion can be monitored by responding to the change of the current intensity.
In order to achieve the above object, the present invention provides a method for preparing a hydroxyapatite membrane electrode for detecting heavy metal ions, which is characterized in that: in a deposition tank, taking ITO glass as a cathode, a platinum electrode as an anode and a mixed aqueous solution of calcium nitrate, diammonium phosphate and phosphoric acid as an electrolyte, and depositing on the ITO cathode through electrodeposition to obtain a hydroxyapatite membrane electrode; the calcium-phosphorus ratio of the electrolyte solution is 5:3, the thickness of the obtained hydroxyapatite membrane electrode is 5-35 mu m; the potential of the electrodeposition is regulated and controlled by a direct current stabilized voltage supply, and the sedimentation tank is placed in a water bath for heating during the sedimentation.
In the above method, the concentration of calcium nitrate is 0.05M to 0.2M.
In the method, the concentration of the diammonium hydrogen phosphate is 0.015-0.06M.
In the method, the concentration of the phosphoric acid is 0.015-0.06M.
In the method, the hydroxyapatite film is of a micro-nano scale strip-shaped structure, the bandwidth is 0.85-3 mu m, the strip length is 1-30 mu m, and the strip thickness is 50-200 nm.
In the method, the electrodeposition potential is 1.5-2.5V.
In the method, the electrodeposition time is 30-180 min.
In the method, the water bath temperature is 40-80 ℃.
The hydroxyapatite membrane electrode prepared by the invention can be used as a heavy metal ion sensor to be applied to heavy metal detection.
The application comprises the steps that a hydroxyapatite film electrode is used as a working electrode, a platinum electrode is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and an electrochemical workstation is applied to monitor the change of current response intensity along with the concentration of heavy metal ions under a differential pulse volt-ampere test method, so that the detection of the concentration of the heavy metal ions is realized.
In the application, the potential of the differential pulse voltage is-0.80-0.50V.
In the application, the heavy metal ions are bivalent lead, copper or mercury.
In the application, the concentration of the heavy metal ions is 0.1-10.0 mu M.
The principle that the hydroxyapatite membrane electrode prepared by the invention is used as a heavy metal ion sensor to respond to heavy metal ions is as follows: the ions with negative charges on the surface of the electrode firstly adsorb heavy metal ions on the surface of the electrode, then the potential is scanned from negative direction to positive direction, so that the heavy metal ions are dissolved out from the electrode, and a current-potential curve in the dissolving-out process is recorded. Under certain conditions, the peak height and the metal ion concentration are in a linear relationship, and different ions have different peak potentials in certain electrolyte.
The invention has the beneficial effects that: the hydroxyapatite thin film electrode prepared based on the electrodeposition method can provide uniform surface morphology, large area-volume ratio and high conductivity, and has good stability, high sensitivity and low cost. The preparation method has the advantages of simple process, easy operation, low preparation cost and easy popularization.
Drawings
In order to more clearly illustrate the technical solution of the present invention and the properties of the material prepared by the same, a diagram related to example 1 is given below.
FIG. 1 is an X-ray electron diffraction pattern of a hydroxyapatite membrane electrode
FIG. 2 is a scanning electron microscope atlas of hydroxyapatite membrane electrode.
FIG. 3 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 0.1-1.0 μ M of divalent lead ions.
FIG. 4 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 3.0-10.0 μ M of divalent lead ions.
FIG. 5 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 0.1-1.0 μ M of divalent copper ions.
FIG. 6 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 1.0-10.0 μ M of divalent copper ions.
FIG. 7 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 0.1-1.0 μ M of divalent mercury ions.
FIG. 8 is a graph (inset) showing the current-potential curve and the linear relationship between the concentration and the current response of the hydroxyapatite membrane electrode in the concentration range of 1.0-10.0 μ M of divalent mercury ions.
As can be seen from the X-ray electron diffraction pattern of FIG. 1, the diffraction peak position of the hydroxyapatite of the target electrode corresponds to the characteristic peak of the standard pattern of PDF card 09-0432.
As can be seen from the scanning electron microscope atlas of fig. 2, the target electrode is a hydroxyapatite membrane electrode with a micro-nano scale strip shape.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the range of 0.1-1.0 mu M, the target electrode has high sensitivity and response current intensity to the divalent lead ions, and the concentration of the divalent lead ions has good linear relation with the current response intensity.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the range of 3.0-10.0 mu M, the target electrode has high sensitivity and response current intensity to the divalent lead ions, and the concentration of the divalent lead ions has good linear relation with the current response intensity.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the range of 0.1-1.0 mu M, the target electrode has high sensitivity and response current intensity to the bivalent copper ions, and the concentration of the bivalent copper ions has a good linear relation with the current response intensity.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the range of 1.0-10.0 mu M, the target electrode has high sensitivity and response current intensity to the bivalent copper ions, and the concentration of the bivalent copper ions has a good linear relation with the current response intensity.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the figure 7, the target electrode has high sensitivity and response current intensity to the divalent mercury ions within the concentration range of 0.1-1.0 mu M, and the concentration of the divalent mercury ions has good linear relation with the current response intensity.
As can be seen from the current-potential curve and the linear relation graph of the concentration and the current response of the target electrode in the range of 1.0-10.0 mu M, the target electrode has high sensitivity and response current intensity to the divalent mercury ions, and the concentration of the divalent mercury ions has a good linear relation with the current response intensity.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
Example 1:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 2:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.10M of calcium nitrate, 0.030M of diammonium phosphate and 0.030M of phosphoric acid as an electrolyte, and carrying out electrodeposition on the ITO cathode to obtain a hydroxyapatite membrane electrode, wherein the thickness of the obtained hydroxyapatite membrane is 9 microns, and the calcium-phosphorus ratio is 5: 3. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 3:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.15M of calcium nitrate, 0.045M of diammonium phosphate and 0.045M of phosphoric acid is used as an electrolyte, the calcium-phosphorus ratio is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 11 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 4:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.20M of calcium nitrate, 0.060M of diammonium phosphate and 0.060M of phosphoric acid as an electrolyte, wherein the ratio of calcium to phosphorus is 5:3, and electrodepositing on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 13 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 5:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.15V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 6:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.17V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 7:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.19V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 8:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.21V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 9:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.23V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 10:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.25V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 11:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid as an electrolyte, and carrying out electrodeposition on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 13 microns, and the calcium-phosphorus ratio is 5: 3. The deposition potential is regulated and controlled by a direct current stabilized voltage power supply, the deposition potential is 0.20V, the deposition time is 60min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 12:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid as an electrolyte, wherein the calcium-phosphorus ratio is 5:3, and electrodepositing on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 24 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 120min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 13:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid as an electrolyte, wherein the calcium-phosphorus ratio is 5:3, and electrodepositing on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 35 mu M. The deposition potential is regulated and controlled by a direct current stabilized voltage power supply, the deposition potential is 0.20V, the deposition time is 180min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 60 ℃.
Example 14:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid as an electrolyte, wherein the calcium-phosphorus ratio is 5:3, and electrodepositing on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 5 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 40 ℃.
Example 15:
taking ITO glass as a cathode, a platinum electrode as an anode, taking a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid as an electrolyte, wherein the calcium-phosphorus ratio is 5:3, and electrodepositing on the ITO cathode to obtain a hydroxyapatite film electrode, wherein the thickness of the obtained film is 6 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 50 ℃.
Example 16:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 70 ℃.
Example 17:
ITO glass is used as a cathode, a platinum electrode is used as an anode, a mixed aqueous solution of 0.05M of calcium nitrate, 0.015M of diammonium phosphate and 0.015M of phosphoric acid is used as an electrolyte, the ratio of calcium to phosphorus is 5:3, a hydroxyapatite film electrode is obtained by electrodeposition on the ITO cathode, and the thickness of the obtained hydroxyapatite film electrode is 7 microns. The deposition potential is regulated by a DC regulated power supply, the deposition potential is 0.20V, the deposition time is 30min, the deposition pool is placed in a water bath for heating during deposition, and the temperature is controlled at 80 ℃.
Claims (4)
1. A preparation method of a hydroxyapatite membrane electrode for heavy metal ion detection is characterized by comprising the following steps: in a deposition tank, taking ITO glass as a cathode, a platinum electrode as an anode and a mixed aqueous solution of calcium nitrate, diammonium phosphate and phosphoric acid as an electrolyte, and depositing on the ITO cathode through electrodeposition to obtain a hydroxyapatite membrane electrode; the calcium-phosphorus ratio of the electrolyte solution is 5:3, the thickness of the obtained hydroxyapatite membrane electrode is 5-35 mu m; the potential of the electrodeposition is regulated and controlled by a direct current stabilized voltage supply, and a sedimentation tank is placed in a water bath for heating during the sedimentation; the concentration of calcium nitrate is 0.05-0.2M, the concentration of diammonium hydrogen phosphate is 0.015-0.06M, and the concentration of phosphoric acid is 0.015-0.06M; the electro-deposition potential is 1.5-2.5V, and the electro-deposition time is 30-180 min; the temperature of the water bath is 40-80 ℃.
2. A hydroxyapatite membrane electrode for heavy metal ion detection is characterized in that: is prepared by the method of claim 1.
3. The application of the hydroxyapatite membrane electrode for heavy metal ion detection in the heavy metal detection according to claim 2, is characterized in that: the heavy metal ions are divalent lead, copper or mercury.
4. The application of the hydroxyapatite membrane electrode for heavy metal ion detection in heavy metal detection according to claim 3, wherein: the concentration of the heavy metal ions is 0.1-10.0 mu M.
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Non-Patent Citations (7)
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| Evaluation of a platinum electrode modified with hydroxyapatite in the lead(II) determination in a square wave voltammetric procedure;El Mhammedi, Achak et al.;《Arabian Journal of Chemistry》;20101016;第6卷(第3期);全文 * |
| Fabrication of nano-porous hydroxyapatite modified electrode and its application for determination of p-chlorophenol;Chu, Zhang;《Journal of nanoscience and nanotechnology》;20120101;第12卷(第1期);第300-306页 * |
| Flower-like hydroxyapatite modified carbon paste electrodes applicable for highly sensitive detection of heavy metal ions;Ying Zhang et al.;《Journal of Materials Chemistry》;20110419(第21期);全文 * |
| Rod-like hydroxyapatite and Nafion nanocomposite as an electrochemical matrix for simultaneous and sensitive detection of Hg2+, Cu2+, Pb2+ and Cd2+;Feng Gao et al.;《Journal of Electroanalytical Chemistry》;20160525;第775卷;全文 * |
| Sea cucumber-like hydroxyapatite: cation exchange membrane-assisted synthesis and its application in ultra-sensitive heavy metal detection;Ying Zhang et al.;《Chemical Communications》;20110307;第47卷(第14期);全文 * |
| Simultaneous determination of ultra-trace lead and cadmium at a hydroxyapatite-modified carbon ionic liquid electrode by square-wave stripping voltammetry;Li, Liu et al.;《Sensors and Actuators B: Chemical》;20090331;第139卷(第2期);全文 * |
| Square wave voltammetry for analytical determination of cadmium in natural water using Ca10(PO4)6(OH)2-modified platinum electrode;El Mhammedi et al.;《American Journal of Analytical Chemistry》;20111110;第1卷(第3期);第150-167页 * |
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