CN113252744B - Photoelectrochemistry-based detector for trace ions/molecules in solution - Google Patents
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention discloses a photoelectrochemistry-based detector for trace ions/molecules in a solution, which comprises a human-computer interaction module, a photoelectric mode recognition module and a control module, wherein the human-computer interaction module is used for manually selecting a trace ion/molecule concentration model according to a detection object and configuring the trace ion/molecule concentration model to the photoelectric mode recognition module; the photoelectric data acquisition module is used for acquiring photoelectric induction current analog signals generated in the solution to be detected; the signal preprocessing module is used for preprocessing the photoelectric induced current analog signal to obtain a photoelectric induced current digital signal; and the photocurrent mode identification module is used for inputting the photoelectric induced current digital signal into the selected trace ion/molecule concentration model and calculating to obtain a corresponding ion/molecule concentration value. The detector has the advantages of environmental friendliness, simplicity in preparation, good portability, low cost, high detection speed, high sensitivity, strong selectivity and wide detection range, different trace ion/molecule concentration models can be selectively introduced to detect the concentrations of different ion/molecule types, and the application is wide.
Description
Technical Field
The invention relates to the field of photoelectrochemistry analysis and detection, in particular to a detector for trace ions/molecules in a solution based on photoelectrochemistry.
Background
With the progress of scientific research and the attention of people to the environment, the quantitative analysis of ion/molecule concentration plays an important role in the fields of clinical medicine, biochemistry, environmental science and the like.
Currently, the ion/molecule detection is mainly performed by an ex-situ detection method, for example, chloride ion/molecule, and commonly used methods are a titration method, a spectrophotometry method, an ion/molecule chromatography method, an atomic absorption method, and the like. The ion/molecule chromatography and the atomic absorption method are not beneficial to popularization and utilization due to the fact that instruments and equipment are complex and expensive; the titration method is greatly influenced by artificial subjectivity, and the reproducibility and the reliability of the titration method need to be improved; the spectrophotometry is relatively suitable for measuring the content of chloride ions/molecules in tap water due to lower cost, higher sensitivity and better reproducibility. However, most of the solutions of the existing spectrophotometry adopt silver nitrate, silver chromate or mercury thiocyanate, and the solutions are strong in toxicity and have serious pollution to the environment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a detector for detecting trace ions/molecules in a solution based on photoelectrochemistry, which has the advantages of environmental friendliness, low cost and high sensitivity.
A photoelectrochemistry-based detector for trace ions/molecules in a solution comprises a photoelectric data acquisition module, a signal preprocessing module, a photocurrent mode identification module, a human-computer interaction module and a result processing module;
the man-machine interaction module is used for manually selecting a trace ion/molecule concentration model according to a detection object and configuring the trace ion/molecule concentration model to the photocurrent mode identification module;
the photoelectric data acquisition module is used for acquiring photoelectric induction current analog signals generated in a solution to be detected;
the signal preprocessing module is used for preprocessing the photoelectric induced current analog signal to obtain a photoelectric induced current digital signal;
the photocurrent mode identification module is used for inputting photoelectric induction current digital signals into the selected trace ion/molecule concentration model and calculating to obtain corresponding ion/molecule concentration values;
and the result processing module is used for outputting and displaying the obtained corresponding ion/molecule concentration value.
Further, the trace ion/molecule concentration model is obtained by the following method:
selecting solutions with different standard concentrations corresponding to ions/molecules, and measuring the corresponding photoelectric induction current value under each standard concentration;
and drawing a standard function model relation based on different standard concentrations and corresponding photoelectric induced current values to obtain a trace ion/molecule concentration model corresponding to the ions/molecules.
Further, the human-computer interaction module is also used for outputting an online modeling instruction to the photocurrent pattern recognition module;
the photocurrent mode identification module is further used for acquiring the concentration of a preset number of standard solutions and corresponding photoelectric induction current digital signals, and constructing a trace ion/molecule concentration model based on the acquired data.
Furthermore, the photoelectric data acquisition module is a three-electrode system and comprises a working electrode, an auxiliary electrode and a reference electrode; wherein the working electrode is a photoelectric sensing electrode.
Further, the preprocessing process of the signal preprocessing module comprises: and sequentially carrying out signal noise reduction, signal normalization, signal amplification, I/V conversion and A/D conversion on the photoelectric induced current analog signals to finally obtain the photoelectric induced current digital signals.
Further, the signal noise reduction process includes:
carrying out N-layer wavelet decomposition on the photoelectric induction current analog signal, selecting a threshold value for each layer coefficient obtained by decomposition, carrying out soft threshold value processing on each layer coefficient, and carrying out wavelet reconstruction on each processed layer coefficient to obtain a noise-reduced photoelectric induction current analog signal; the threshold value obtaining method comprises the following steps:
a specified decomposition layer number j is given, and all coefficients of j +1 and higher layers are reserved;
for the ith layer, i is more than or equal to 1 and less than or equal to j, and n with the maximum absolute value is reserved i Coefficient of n i Is determined by the following formula:
n i ＝M(j+2-i) α
in the formula, M and alpha are empirical coefficients.
Further, the photoelectric data acquisition module is used for continuously sampling photoelectric induction current analog signals, when the sampling data reach a preset number, the sampling is judged to be successful, and otherwise, the sampling is carried out again.
The automatic detection device further comprises an initialization module, wherein the initialization module is used for initializing and self-checking the detection device when the human-computer interaction module is selected to start manually.
Furthermore, the human-computer interaction module is also used for manually selecting a result processing request, sending the result processing request to the result processing module and inputting a query instruction to check a historical detection result; and the result processing module is used for storing and/or printing the obtained corresponding ion/molecule concentration value according to the result processing request.
Further, when the photoelectric data acquisition module is used for acquiring photoelectric induction current analog signals, the solution to be detected and the photoelectric data acquisition module are placed in a dark environment, and a unique light source is adopted for irradiation under a preset bias voltage; wherein the preset bias voltage value range is-0.5-0.5V vs. RHE; the light source adopts one of sunlight, xenon lamp, halogen tungsten lamp, metal halogen lamp, incandescent lamp, fluorescent lamp, LED lamp, mercury lamp and laser, and the power is 1mW/cm 2 ～300mW/cm 2 (ii) a The temperature of the solution to be measured is 10-60 ℃, and the pH value is 3-10.
Further, the ion/molecule concentration in the solution to be detected is 0.1 mu mol/L-10 m mol/L; wherein the ions comprise Cu 2+ 、Pb 2+ 、Hg 2+ 、Cr 6+ 、Cd 2+ 、Fe 3+ 、Cl - 、I - 、Br - 、S 2- The molecules include protein molecules, DNA molecules and amino acid molecules.
The detection process by using the detector for detecting the trace ions/molecules in the solution based on photoelectrochemistry is as follows:
(1) Selecting the type of ions/molecules to be detected through a human-computer interaction module, starting the selection, initializing and self-checking the initialization module, and leading a trace ion/molecule concentration model corresponding to the type of the ions/molecules to be detected into a photocurrent mode identification module;
(2) If the step (1) can not be passed, displaying the reasons of abnormity and failure, and restarting the step (1) after the abnormity is processed; if the step (1) is passed, an operator puts the photoelectric data acquisition module into the solution to be detected;
(3) Standing the solution to be detected and a photoelectric data acquisition module for a preset time length to enable the photoelectric data acquisition module to be fully reflected with the solution to be detected to form a photoelectric material, turning on a light source and generating a photoelectric induced current analog signal;
(4) The signal preprocessing module converts the photoelectric induction current analog signal into a photoelectric induction current digital signal;
(5) Transmitting the photoelectric induced current analog signal into a trace ion/molecule concentration model in a photocurrent mode identification module, and calculating to obtain the concentration value of the ions/molecules in the solution to be detected;
(6) The result processing module displays the concentration value of the obtained ions/molecules; and storing and/or printing the concentration value of the ions/molecules according to a result processing request output by the man-machine interaction module.
Advantageous effects
The invention provides a detector for detecting trace ions/molecules in a solution based on photoelectrochemistry, which is used for detecting liquid ions/molecules based on the comprehensive use of a photoelectrochemical material and an intelligent detection technology, and the combination of the two methods has the advantages of environment friendliness, simple preparation, low cost, high sensitivity, strong selectivity and wide detection range when the photoelectrochemical material is detected, and also has the advantages of high detection speed, high sensitivity, good portability and easy operation of the intelligent detection. Meanwhile, different trace ion/molecule concentration models can be selectively introduced to detect the concentrations of different ion/molecule types, the application is wide, and the method can be widely applied to the detection of the ion/molecule concentrations in aqueous solutions, human blood and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a block diagram of a trace ion/molecule detector according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a trace ion/molecule detection process provided by an embodiment of the present invention;
fig. 3 is a schematic diagram of a data acquisition process of the trace ion/molecule detector according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
As shown in FIG. 1, the embodiment provides a detector for detecting trace ions/molecules in a solution based on photoelectrochemistry, which can be used to detect a solution to be detected with a trace ion/molecule concentration of 0.1 μmol/L to 10m mol/L; wherein the ion includes but is not limited to Cu 2+ 、Pb 2+ 、Hg 2+ 、Cr 6+ 、Cd 2+ 、Fe 3+ 、Cl - 、I - 、Br - 、S 2- Molecules include, but are not limited to, protein molecules, DNA molecules, amino acid molecules.
Specifically, the detector comprises a photoelectric data acquisition module 2, a signal preprocessing module 3, a photocurrent mode identification module 4, a human-computer interaction module 5, a result processing module 7 and an initialization module 6;
the human-computer interaction module 5 is used for manually selecting a trace ion/molecule concentration model according to a detection object and configuring the trace ion/molecule concentration model to the photocurrent mode identification module 4; the system is also used for manually selecting a result processing request and sending the result processing request to the result processing module 7, and for inputting a query instruction to view historical detection results;
the initialization module 6 is used for initializing and self-checking the detector when the human-computer interaction module 5 is manually selected to start;
the photoelectric data acquisition module 2 is used for acquiring photoelectric induction current analog signals generated in a solution to be detected;
the signal preprocessing module 3 is used for preprocessing the photoelectric induced current analog signal to obtain a photoelectric induced current digital signal;
the photocurrent mode identification module 4 is used for inputting photoelectric induced current digital signals into the selected trace ion/molecule concentration model and calculating to obtain corresponding ion/molecule concentration values;
the result processing module 7 is used for outputting and displaying the obtained corresponding ion/molecule concentration value; and the ion/molecule concentration value processing module is also used for storing and/or printing the obtained corresponding ion/molecule concentration value according to the result processing request.
Before the detector is used, a trace ion/molecule concentration model corresponding to each ion/molecule needs to be obtained in advance and stored in a storage module of the detector, and the trace ion/molecule concentration model is obtained through the following processes:
respectively selecting different standard concentration solutions corresponding to each ion/molecule, and measuring the corresponding photoelectric induction current value under each standard concentration;
and drawing a standard function model relation (namely a linear relation between the concentration value of the ions/molecules and the photoelectric induction current value) based on different standard concentrations and corresponding photoelectric induction current values to obtain a trace ion/molecule concentration model corresponding to the ions/molecules.
The detector also has an online modeling function, and the specific process is as follows: outputting an online modeling instruction to the photocurrent mode identification module 4 by a human-computer interaction module 5; then, acquiring photoelectric induction current digital signals corresponding to a preset number of standard solutions with different concentrations by using the detector, and inputting the concentration of each standard solution through a human-computer interaction module 5; the photocurrent mode identification module 5 acquires the concentration of a preset number of standard solutions and corresponding photoelectric induction current digital signals, and constructs a trace ion/molecule concentration model based on the acquired data.
In this embodiment, the photoelectric data acquisition module 2 is a three-electrode system, and includes a working electrode, an auxiliary electrode, and a reference electrode; the working electrode is a photoelectric sensing electrode, and photoelectric sensing electrodes made of different materials can be replaced according to different detection objects. When data acquisition is carried out, firstly, a solution to be detected is placed in a detection pool 1 in a full-dark environment, and a unique light source is also configured in the detection pool 1; then, the three-electrode system is put into the solution to be measured, and is kept stand for a preset time (for example twenty minutes) to ensure that the photoelectric sensing electrode and the solution to be measured are filledRespectively reflecting to form a photoelectric material; then the light source is turned on to generate a photoelectric induction current analog signal. And is also provided with a preset bias voltage when the light source irradiates. In specific implementation, the bias voltage value range is preset to be-0.5-0.5Vvs.RHE; the light source adopts one of sunlight, xenon lamp, halogen tungsten lamp, metal halogen lamp, incandescent lamp, fluorescent lamp, LED lamp, mercury lamp and laser, and the power is 1mW/cm 2 ～300mW/cm 2 (ii) a The temperature of the solution to be measured is 10-60 ℃, and the pH value is 3-10.
The photoelectric data acquisition module 2 transmits the acquired photoelectric induced current analog signals to the signal preprocessing module 3, and the signal preprocessing module 3 sequentially carries out signal noise reduction, signal normalization, signal amplification, I/V conversion and A/D conversion on the photoelectric induced current analog signals to finally obtain photoelectric induced current digital signals. Wherein the signal denoising process comprises:
carrying out N-layer wavelet decomposition on the photoelectric induction current analog signal, selecting a threshold value for each layer coefficient obtained by decomposition, carrying out soft threshold value processing on each layer coefficient, and carrying out wavelet reconstruction on each processed layer coefficient to obtain a noise-reduced photoelectric induction current analog signal; the threshold value obtaining method comprises the following steps:
a specified decomposition layer number j is given, and all coefficients of j +1 and higher layers are reserved;
for the ith layer, i is more than or equal to 1 and less than or equal to j, and n with the maximum absolute value is reserved i Coefficient of n i Is determined by the following formula:
n i ＝M(j+2-i) α
in the formula, M and alpha are empirical coefficients.
During implementation, the photoelectric data acquisition module 2 is used for continuously sampling photoelectric induction current analog signals, when the sampling data reach a preset number, the sampling is judged to be successful, and otherwise, the sampling is carried out again. As shown in fig. 3, the data acquisition process is a schematic diagram, the initialization module 5 performs initialization and self-inspection on the detector after the start of the data acquisition is confirmed by the human-computer interaction module 5, and after a sampling command output by the human-computer interaction module 5 is received, a sampling program is started to perform sampling, and whether the number of sampling points reaches a preset number or not is judged, if so, the sampling is completed, and if not, the sampling is unsuccessful and the sampling is performed again.
In implementation, the result processing module 7 outputs the obtained corresponding ion/molecule concentration value to a display for displaying, stores the result in the storage module 8 when storing the obtained corresponding ion/molecule concentration value according to the result processing request, and prints the obtained corresponding ion/molecule concentration value through the printer 9 connected thereto when printing the obtained corresponding ion/molecule concentration value according to the result processing request. The display can be a single display, or can be realized by sharing a touch display screen with the human-computer interaction module 5.
As shown in fig. 2, in specific implementation, the photocurrent pattern recognition module 4 and the result processing module 7 are configured in a single chip, the single chip is used for calculating the concentration and outputting the result, the human-computer interaction module 5 is a touch display screen, and the single chip is in communication connection with the touch display screen, the storage module 8 and the printer 9 to realize data transmission. The photoelectric data acquisition module 2 acquires photoelectric induction current analog signals, and the photoelectric induction current analog signals are processed by the signal preprocessing module 3 and then output to the photocurrent mode identification module 4 in the single chip microcomputer. Optionally, the only light source in the detection pool 1 can be controlled by a single chip microcomputer, and a light source on-off instruction is input by the human-computer interaction module 5; and the power management module supplies power to other modules of the detector.
In order to further understand the technical scheme of the invention, the effect of the detector is illustrated by taking chloride ion detection as an example and two sets of experiments.
In the experiment, the photoelectric sensing electrode is prepared, and a standard curve model is drawn, so that a trace ion/molecule concentration model (hereinafter referred to as a chloride ion standard current-concentration curve model) is obtained. The ion chromatograph is one of the fastest developed analysis methods in the field of analytical chemistry in recent years, and as a common ion detection method in a laboratory, the ion chromatograph has the recognized advantages of high detection speed, high sensitivity and good selectivity, but has the defects of being not portable and expensive. In the experiment, the detection result of the ion chromatograph is compared with the detection result of the detector of the invention.
Experiment one
50ml of solution to be detected is taken, and the prepared photoelectric sensing electrode is placed in the solution to be detected and soaked for 20min at the temperature of 30 ℃. The pretreated photoelectric sensing electrode is used as a working electrode, the graphite electrode is used as an auxiliary electrode, and the saturated calomel electrode is used as a reference electrode to form a three-electrode system. The light response current of the photoelectric sensing electrode is collected under the environment that the light source is a xenon lamp and the bias voltage is 0.5V vs. And the photoresponse current passes through the signal preprocessing module, the photoelectric induction current analog signal is converted into a current digital signal, the current digital signal is transmitted into the pattern recognition module, and the current digital signal is substituted and calculated with the existing chloride ion standard current-concentration curve model to obtain the concentration of the chloride ions in the solution to be detected.
The average value of the concentration of the chloride ions in the solution to be measured, which is obtained after the system of experiment one of the invention is used for measuring three times, is 4.65 mu mol, and is basically consistent with the average value of the concentration of the chloride ions, which is obtained after the system of experiment one is used for measuring three times, is 4.58 mu mol/L. The relative error of this method was calculated to be δ =1.53%.
Experiment two
50ml of solution to be detected is taken, and the prepared photoelectric sensing electrode is placed in the solution to be detected and soaked for 30s at the temperature of 60 ℃. And constructing a three-electrode system in a phosphate buffer solution by taking the pretreated photoelectric sensing electrode as a working electrode, a platinum electrode as an auxiliary electrode and a silver chloride electrode as a reference electrode. Under the irradiation of a daylight lamp light source (the luminous power is 20 mW/cm) 2 ) And collecting the photoresponse current of the photoelectric sensing electrode under the bias voltage of-0.2V vs. And the photoresponse current passes through the signal preprocessing module, the photoelectric induction current analog signal is converted into a current digital signal, the current digital signal is transmitted into the pattern recognition module, and the current digital signal is substituted and calculated with the existing chloride ion standard current-concentration curve model to obtain the concentration of the chloride ions in the solution to be detected.
The average value of the concentration of the chloride ions in the solution to be measured, which is obtained after the system of experiment two is adopted for three times of measurement, is 0.823 mu mol/L, and is basically consistent with the average value of the concentration of the chloride ions, which is obtained after the system of experiment two is adopted for three times of measurement, of 0.830 mu mol/L. Calculated, the relative error of this method δ =0.84%.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. A photoelectrochemistry-based detector for trace ions/molecules in a solution is characterized by comprising a photoelectric data acquisition module, a signal preprocessing module, a photocurrent mode identification module, a human-computer interaction module and a result processing module;
the man-machine interaction module is used for manually selecting a trace ion/molecule concentration model according to a detection object and configuring the trace ion/molecule concentration model to the photocurrent mode identification module;
the photoelectric data acquisition module is used for acquiring photoelectric induction current analog signals generated in a solution to be detected;
the signal preprocessing module is used for preprocessing the photoelectric induced current analog signal to obtain a photoelectric induced current digital signal;
the photocurrent mode identification module is used for inputting photoelectric induction current digital signals into the selected trace ion/molecule concentration model and calculating to obtain corresponding ion/molecule concentration values;
the result processing module is used for outputting and displaying the obtained corresponding ion/molecule concentration value;
the preprocessing process of the signal preprocessing module comprises signal noise reduction, and the signal noise reduction process comprises the following steps:
carrying out N-layer wavelet decomposition on the photoelectric induction current analog signal, selecting a threshold value for each layer coefficient obtained by decomposition, carrying out soft threshold value processing on each layer coefficient, and carrying out wavelet reconstruction on each processed layer coefficient to obtain a noise-reduced photoelectric induction current analog signal; the threshold value obtaining method comprises the following steps:
a specified decomposition layer number j is given, and all coefficients of j +1 and higher layers are reserved;
for the ith layer, i is more than or equal to 1 and less than or equal to j, and n with the maximum absolute value is reserved i Coefficient of n i Is determined by the following formula:
n i ＝M(j+2-i) α
in the formula, M and alpha are empirical coefficients.
2. The photoelectrochemical-based detector for trace ions/molecules in solution according to claim 1, wherein the trace ion/molecule concentration model is obtained by:
selecting solutions with different standard concentrations corresponding to ions/molecules, and measuring the corresponding photoelectric induction current value under each standard concentration;
and drawing a standard function model relation based on different standard concentrations and corresponding photoelectric induced current values to obtain a trace ion/molecule concentration model corresponding to the ions/molecules.
3. The photoelectrochemistry-based detector for ions/molecules in solution as recited in claim 1 or 2, wherein the human-computer interaction module is further configured to output an online modeling instruction to the photocurrent pattern recognition module;
the photocurrent mode identification module is further used for acquiring the concentration of a preset number of standard solutions and corresponding photoelectric induction current digital signals, and constructing a trace ion/molecule concentration model based on the acquired data.
4. The photoelectrochemical-based detector for trace ions/molecules in solution according to claim 1 or 2, wherein the signal preprocessing module comprises: and sequentially carrying out signal noise reduction, signal normalization, signal amplification, I/V conversion and A/D conversion on the photoelectric induced current analog signals to finally obtain the photoelectric induced current digital signals.
5. The photoelectrochemistry-based detector for ions/molecules in solution according to claim 1 or 2, wherein the photoelectric data acquisition module is configured to continuously sample the photoelectric sensing current analog signal, and when the number of the sampled data reaches a preset number, it is determined that the sampling is successful, and otherwise, the sampling is performed again.
6. The photoelectrochemical-based detector for ions/molecules in solution according to claim 1 or 2, further comprising an initialization module for initializing and self-testing the detector when a manual selection is started in the human-computer interaction module.
7. The photoelectrochemistry-based detector for ions/molecules in solution according to claim 1 or 2, wherein the human-computer interaction module is further configured to manually select a result processing request and send the result processing request to the result processing module, and to input a query instruction to view historical detection results; and the result processing module is used for storing and/or printing the obtained corresponding ion/molecule concentration value according to the result processing request.
8. The photoelectrochemistry-based detector for ions/molecules in solution in trace amounts according to claim 1 or 2, wherein when the photoelectric data acquisition module is used for acquiring photoelectric induced current analog signals, the solution to be detected and the photoelectric data acquisition module are placed in a dark environment and irradiated by a unique light source under a preset bias voltage; wherein the preset bias voltage value range is-0.5-0.5Vvs.RHE; the light source adopts one of sunlight, xenon lamp, halogen tungsten lamp, metal halogen lamp, incandescent lamp, fluorescent lamp, LED lamp, mercury lamp and laser, and the power is 1mW/cm 2 ～300mW/cm 2 (ii) a The temperature of the solution to be measured is 10-60 ℃, and the pH value is 3-10.
9. The apparatus for detecting trace ions/molecules in a solution based on photoelectrochemistry according to claim 1 or 2, wherein the concentration of ions/molecules in the solution to be detected is 0.1 μmol/L to 10m mol/L; wherein the ions comprise Cu 2+ 、Pb 2+ 、Hg 2+ 、Cr 6+ 、Cd 2+ 、Fe 3+ 、Cl - 、I - 、Br - 、S 2- The molecules include protein molecules, DNA molecules and amino acid molecules.
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| CN109655502A (en) * | 2017-10-11 | 2019-04-19 | 中山大学 | A kind of portable multi-channel electrochemical detection system |
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