CN108982641A - A kind of preparation method of the electrochemical sensing of trace lead ion detection - Google Patents
A kind of preparation method of the electrochemical sensing of trace lead ion detection Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the electrochemical sensing of trace lead ion detection, belong to environment measuring analysis technical field.It include: step 1: by the gelatin-based microcapsules of complex coacervation preparation freeze-dried, by the microscapsule powder ultrasonic disperse after carbonization in chitosan acetic acid solution；Step 2: the carbonization micro-capsule dispersion liquid for taking 5 μ L steps 1 made makees electrode material modification in glassy carbon electrode surface, as working electrode；Step 3: the lead ion electrolyte of various concentration being added to composition 5mL prepare liquid in buffer solution, the electrode system in step 2 is inserted into above-mentioned lead ion electrolyte, constant voltage is enriched with the lead ion in electrolyte；Step 4: using Differential Pulse Anodic Stripping Voltammetry, obtain the standard curve of peak point current and plumbum ion concentration；Step 5: plumbum ion concentration in detection sample to be tested.Working electrode decorative material prepared by the present invention has preparation simple, at low cost, structure-controllable and it is reproducible the advantages that.
Description
Technical field
The present invention relates to environment measuring analysis technical fields, particularly relate to a kind of electrochemical sensing of trace lead ion detection
Preparation method.
Background technique
In recent years, with the fast development of industry, the bio-toxicity of heavy metal is big, to the wound of environment and human physical and mental health
Evil should not be underestimated.Lead ion has micro causing toxicity and bioconcentration, and it is carcinogenic to be attributed to II class by international cancer research institution
Object, the generation of environmentally safe and human health seriously threaten.Therefore, the method for simple and convenient and efficient analysis detection lead ion
It is concerned.
Currently, the analyzing detecting method of lead ion has atomic absorption spectrography (AAS), atomic fluorescence spectrometry, biological stain examination
Paper method and electrochemical analysis method.There is detection interference greatly in preceding 3 kinds of detection methods, detect limit for height, complicated for operation, expensive etc.
It is insufficient.And electrochemical analysis method is because its detection limit is low, it is cheap, it is easy to carry, the on-site test of sample may be implemented and
It is concerned.Publication number CN105092683B discloses a kind of electrochemical sensor for detecting lead and preparation method thereof and answers
With being modified with ordered mesopore carbon in glassy carbon electrode surface first, then deposit nanogold particle on the surface of the material, finally by sulfydryl
The capture probe of modification is adsorbed on nanogold particle, which has fast ring to the detection of Lead in Aqueous Solution
It answers, the advantages such as high sensitivity, pinpoint accuracy.J.T.Zhang etc. is using graphene oxide as shape directed agents, resorcinol and formaldehyde
As carbon matrix precursor, novel graphene modified carbon nano tube piece is prepared for by surface assembling method, can be used as high-efficiency electrochemical biography
Sensor, using the high sensitivity of Square wave anodic stripping voltammetry method test lead to 92.86Amol-1, Monitoring lower-cut 1.12nM
(J.T.Zhang etc., Journal of materials chemistry A, 2013, Vol.1, p13139-13145).It is above this
Cost is relatively low for the preparation method of a little electrochemical analysis detection lead ion materials, and detection limit is low, easy to carry, but these materials have
Unpredictability, the controllability and repeatability of pattern need to be further increased.T.Zhang etc. is using TAPB-DMTP-COF
1, the modified carbon electrode of 3,5- tri- (4- aminobenzene) benzene, 2, four acetaldehyde of 5- dimethoxy and covalent organic framework is prepared a kind of novel
Measurement water in lead electrochemical sensor, detected using Differential Pulse Anodic Stripping Voltammetry, on lead and modified electrode
The amino on the surface TAPB-DMTP-COF is complexed, and due to the unique texture of COF, can improve the adsorption capacity to lead, detection limit is reachable
1.9nmol/L.This working electrode decorative material (micropore covalent organic framework) has high stability and repeatability, but makes
Standby more complex, cost is not low (T.Zhang etc., Talanta, 2018, Vol.188, p578-583).
Therefore, it develops and a kind of prepares simple, cheap, the good and repeated high working electrode decorative material use of stability
In the emphasis that environment measuring analysis field is electrochemical sensor research.
Summary of the invention
To solve deficiency in the prior art, the present invention provides a kind of preparation of the electrochemical sensing of trace lead ion detection
Method, preparation method of the present invention is simple, and obtained electrochemical sensing has many advantages, such as that measuring stability is good, repeatability is high.
In order to solve the above technical problems, present invention offer technical solution is as follows:
The present invention provides a kind of preparation method of the electrochemical sensing of trace lead ion detection, comprising:
Step 1: by the gelatin-based microcapsules of complex coacervation preparation after freeze-dried, being carbonized under nitrogen protection, by carbon
Microscapsule powder ultrasonic disperse after change is in chitosan acetic acid solution；
Step 2: glass-carbon electrode polishing, ultrasonic cleaning is clean, and the carbonization for then taking 5 μ L steps 1 made with liquid-transfering gun is micro-
In glassy carbon electrode surface, drying at room temperature obtains working electrode for capsule dispersant liquid modification, and platinized platinum is used as to electrode, silver/silver chlorate
As reference electrode, three-electrode system is constituted；
Step 3: the lead ion electrolyte of various concentration is added to composition 5mL prepare liquid in buffer solution, it will be in step 2
Three-electrode system be inserted into above-mentioned lead ion electrolyte, constant voltage be enriched with electrolyte in lead ion；
Step 4: using Differential Pulse Anodic Stripping Voltammetry, Current-potential curve stacking chart when record dissolves out obtains
The standard curve of peak point current and plumbum ion concentration；
Step 5: measuring the sample to be tested of unknown plumbum ion concentration with above-mentioned three-electrode system, obtain corresponding peak current
Value, then obtains plumbum ion concentration in sample to be tested according to standard curve.
Further, in the step 1, the mass concentration of chitosan acetic acid solution is 1mg/mL, the quality of acetic acid solution
Score is 0.5~5%, and the mass ratio of microscapsule powder and chitosan acetic acid solution after carbonization is 0.5~5 ︰ 1.
Preferably, in the step 1, the cyst material of gelatin-based microcapsules is gelatin-gum arabic, gelatin-carboxymethyl
Sodium cellulosate-lauryl sodium sulfate, gelatin-sodium carboxymethyl cellulose-bis- (2- second hexyl) sodium sulfosuccinates, gelatin-carboxylic
Sodium carboxymethylcellulose pyce-polysiloxanes carboxylic acid acid sodium or gelatin-sodium alginate.
Preferably, in the step 1, carburizing temperature when gelatin-based microcapsules are carbonized is 600~800 DEG C, carbonization time
It is 5~10 hours.
Preferably, in the step 3, leaded ion electrolyte is Pb (NO3)2、Pb(CH3COO)2Or PbSO4, molar concentration
For 1nmol/L~10 μm ol/L.
Further, in the step 3, buffer solution is NaAc_HAc buffer solution, sodium dihydrogen phosphate-phosphoric acid hydrogen
Disodium or ammonia-sal-ammoniac, pH value are 4~5.
Further, in the step 3, the ratio between amount of substance is 1 ︰ when leaded ion electrolyte is mixed with buffer solution
0.04~400.
Preferably, in the step 3, constant voltage is enriched with the lead ion in prepare liquid, and accumulating potential is -1.0~-0.4V,
Enrichment time is 200~500s.
Preferably, in the step 4, the take-off potential of Differential Pulse Anodic Stripping Voltammetry is -1.4V~-0.9V, eventually
Only current potential is -0.4V~-0.2V.
Compared with prior art, the invention has the following advantages:
The present invention makees the decorative material of working electrode using carbonization gelatin-based microcapsules.Gelatin-based microcapsules carbonization front surface
With uniform microcellular structure, be carbonized after-contraction, and aperture becomes smaller, and specific surface area is bigger, is conducive to the absorption to lead ion, through carbon
Making electrode material modified glassy carbon electrode after change is working electrode, three-electrode system is constituted with to electrode and reference electrode, using difference
Pulsed anode stripping voltammetry is divided to detect trace plumbum ion concentration.The preparation of working electrode decorative material is simple in the preparation method,
It is at low cost, structure-controllable and reproducible.Prepared electrochemical sensor is low to lead ion detection sensitivity height and detection limit.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of trace lead ion detection electrochemical sensing of the invention；
Fig. 2 is the SEM shape appearance figure before the gelatin-based microcapsules a) of the embodiment of the present invention 1 is carbonized and after b) being carbonized.
Fig. 3 is the differential pulse Stripping Voltammetry response diagram of carbonization capsule modified electrode detection various concentration lead ion.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
Such as no special explanation, agents useful for same of the present invention, component are commercial product.
Embodiment 1
A kind of preparation method of the electrochemical sensing of trace lead ion detection, detailed process are shown in Fig. 1:
By gelatin-sodium carboxymethyl cellulose-polysiloxanes carboxylic acid acid sodium of complex coacervation preparation (referring in particular to " High
blades spreadability of chlorpyrifos microcapsules prepared with polysiloxane
sodium carboxylate/sodium carboxymethylcellulose/gelatin via complex
Coacervation ") after freeze-dried, pattern is shown in Fig. 2 a), it can be seen that the microcellular structure of uniform microcapsule from Fig. 2 a；
Under nitrogen protection, 650 DEG C are carbonized 8 hours, see Fig. 2 b, find out microcapsules carbonization after-contraction from Fig. 2 b, aperture becomes smaller, specific surface area
It is bigger.Take 2mg be carbonized after microscapsule powder ultrasonic disperse in the chitosan acetic acid solution of 2mL 1mg/mL, acetic acid solution
Mass fraction is 5%；Take 5 μ L carbonization micro-capsule dispersion liquid make electrode material modification polished in surface, be cleaned by ultrasonic it is clean after
Glass-carbon electrode, be working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference electrode, constitutes three-electrode system；It will be different
Pb (the NO of concentration (0.007,0.01,0.05,0.07,0.3,0.7,0.9,3,7,9 μm of ol/L)3)2Electrolyte is added to pH value
5mL prepare liquid is constituted in 4.5 NaAc_HAc buffer solution；Three-electrode system is inserted into prepare liquid, the permanent electricity of -0.8V
Lead ion in pressure enrichment prepare liquid, enrichment time 300s；Using Differential Pulse Anodic Stripping Voltammetry, -0.9V~-
It is detected under the potential window of 0.2V, and Current-potential curve stacking chart when record dissolution (see Fig. 3, curve lead from bottom to up in figure
Ion concentration successively increases), the standard curve of peak point current and plumbum ion concentration is obtained, the range of linearity of lead ion detection is
0.007μmol/L-9μmol/L.Finally, calculating plumbum ion concentration in sample to be tested according to standard curve.
Embodiment 2
By gelatin-sodium carboxymethyl cellulose-lauryl sodium sulfate microcapsules of complex coacervation preparation freeze-dried
Afterwards, under nitrogen protection, 600 DEG C are carbonized 10 hours；Take 2mg be carbonized after microscapsule powder ultrasonic disperse 4mL 1mg/mL shell
In glycan acetic acid solution, the mass fraction of acetic acid solution is 1.0%；5 μ L carbonization micro-capsule dispersion liquid is taken to make electrode material modification
Glass-carbon electrode after being polished, being cleaned by ultrasonic completely in surface is working electrode, and platinized platinum is to electrode, and silver/silver chlorate is reference
Electrode constitutes three-electrode system；By the Pb (CH of various concentration 1nmol/L~8 μm ol/L3COO)2It is 5 that electrolyte, which is added to pH value,
Ammonia-chlorination ammonia buffer in constitute 5mL prepare liquid；Three-electrode system is inserted into prepare liquid, -1.0V constant voltage is rich
Collect the lead ion in prepare liquid, enrichment time 200s；Using Differential Pulse Anodic Stripping Voltammetry, in -1.4V~-0.4V
It is detected under potential window, Current-potential curve stacking chart when record dissolves out obtains the standard of peak point current and plumbum ion concentration
Curve calculates plumbum ion concentration in sample to be tested according to standard curve.
Embodiment 3
Bis- (2- second hexyl) the sodium sulfosuccinate microcapsules of gelatin-sodium carboxymethyl cellulose-prepared by complex coacervation are existed
After freeze-dried, under nitrogen protection, 800 DEG C are carbonized 5 hours；Microscapsule powder ultrasonic disperse after taking 5mg to be carbonized is in 1mL
In the chitosan acetic acid solution of 1mg/mL, the mass fraction of acetic acid solution is 0.5%；5 μ L carbonization micro-capsule dispersion liquid is taken to make electricity
Pole material modifies the glass-carbon electrode after being polished, being cleaned by ultrasonic completely in surface, is working electrode, and platinized platinum is to electrode, silver/chlorine
Changing silver is reference electrode；By the Pb (NO of various concentration 1nmol/L~5 μm ol/L3)2Electrolyte is added to the di(2-ethylhexyl)phosphate that pH value is 4
In hydrogen sodium-disodium hydrogen phosphate buffer solution, -0.4V constant voltage is enriched with the lead ion in prepare liquid, enrichment time 500s；Using
Differential Pulse Anodic Stripping Voltammetry detects under -1.0V~-0.3V potential window, and current-potential when record dissolves out is bent
Line stacking chart obtains the standard curve of peak point current and plumbum ion concentration, calculates lead ion in sample to be tested according to standard curve
Concentration.
Embodiment 4
By the gelatin-gum arabic microcapsules of complex coacervation preparation after freeze-dried, under nitrogen protection, 700 DEG C of carbon
Change 6 hours；For microscapsule powder ultrasonic disperse after taking 4mg to be carbonized in the chitosan acetic acid solution of 2mL 1mg/mL, acetic acid is molten
The mass fraction of liquid is 2.0%；It takes 5 μ L carbonization micro-capsule dispersion liquid to make electrode material modification polished, be cleaned by ultrasonic in surface
Glass-carbon electrode after clean is working electrode, and platinized platinum is to electrode, and silver/silver chlorate is reference electrode；By various concentration 1nmol/
The PbSO of L~8 μm ol/L4Electrolyte is added in the NaAc_HAc buffer solution that pH value is 4.5, the enrichment of -0.6V constant voltage
Lead ion in prepare liquid, enrichment time 400s；Using Differential Pulse Anodic Stripping Voltammetry, in -1.2V~-0.4V electricity
It is detected under the window of position, Current-potential curve stacking chart when record dissolves out, the standard for obtaining peak point current and plumbum ion concentration is bent
Line calculates plumbum ion concentration in sample to be tested according to standard curve.
Embodiment 5
By gelatin-sodium alginate micro gel capsule of complex coacervation preparation after freeze-dried, under nitrogen protection, 650 DEG C of carbon
Change 9 hours；Microscapsule powder ultrasonic disperse after taking 3mg to be carbonized is in the chitosan acetic acid solution of 1.5mL 1mg/mL, acetic acid
The mass fraction of solution is 0.5%；5 μ L carbonization micro-capsule dispersion liquid is taken to make electrode material modification clear through polishing, ultrasound in surface
Glass-carbon electrode after wash clean is working electrode, and platinized platinum is to electrode, and silver/silver chlorate is reference electrode；By various concentration
Pb (the CH of 2nmol/L~10 μm ol/L3COO)2It is molten that electrolyte is added to sodium dihydrogen phosphate-disodium hydrogen phosphate buffering that pH value is 4
In liquid, -0.8V constant voltage is enriched with the lead ion in prepare liquid, enrichment time 400s；Using differential pulse anodic stripping voltammetry
Method detects under -1.4V~-0.4V potential window, and Current-potential curve stacking chart when record dissolves out obtains peak current
The standard curve of value and plumbum ion concentration calculates plumbum ion concentration in sample to be tested according to standard curve.
Embodiment 6
By gelatin-sodium carboxymethyl cellulose-lauryl sodium sulfate microcapsules of complex coacervation preparation freeze-dried
Afterwards, under nitrogen protection, 800 DEG C are carbonized 5 hours；Take 1mg be carbonized after microscapsule powder ultrasonic disperse 2mL 1mg/mL shell
In glycan acetic acid solution, the mass fraction of acetic acid solution is 5%；Take 5 μ L carbonization micro-capsule dispersion liquid make electrode material modification in
Surface polished, be cleaned by ultrasonic it is clean after glass-carbon electrode, be working electrode, platinized platinum is to electrode, and silver/silver chlorate is reference electricity
Pole；By the Pb (NO of various concentration 1nmol/L~5 μm ol/L3)2Electrolyte is added to ammonia-sal-ammoniac buffering that pH value is 4.8
In solution, -1.0V constant voltage is enriched with the lead ion in prepare liquid, enrichment time 200s；It is lied prostrate using differential pulse Anodic Stripping
An Fa is detected under -1.0V~-0.3V potential window, Current-potential curve stacking chart when record dissolves out, and obtains peak electricity
The standard curve of flow valuve and plumbum ion concentration calculates plumbum ion concentration in sample to be tested according to standard curve.
The Monitoring lower-cut of carbonization microcapsules electrode in above-described embodiment 1-6 is 2nmol/L (S/N=3), and detection limit is low.
Carbonization microcapsules electrode stability in above-described embodiment 1-6 is assessed, carbonization microcapsules electrode is had studied
To the stability of lead ion detection.Continuous 10 detections are carried out to 0.5 μM of lead ion.The result shows that the peak current of lead ion is several
Be it is constant, the relative standard deviation (RSD) of acquired peak current is only 4.3%, this show be carbonized microcapsules electrode have
Good stability.
The performance of carbonization microcapsules electrode detection lead ion in above-described embodiment 1-6 is measured, investigate interference from
The variation of the dissolution peak current of son addition front and back lead ion (0.5 μM), as a result, it has been found that, 100 times of Na is added respectively+、Ca2+、Mg2 +、K+、Al3+、Zn2+、Li+、Cd2+、Cu2+、Cr3+、Mn2+、Ni2+And various anion such as Br-、Cl-、NO3 -、H2PO4 -、SO4 2-
Afterwards, the dissolution peak current of lead ion does not have significant change (± 5.0% error range), thus exclude some common yin-yang from
The interference of son.It can be seen that modified electrode of the invention has the selectivity of height to lead ion.
The detection and analysis of plumbum ion concentration in tap water: apparent signal is not had to go out when directly being detected to actual water sample
It is existing, therefore, tap water and buffer are mixed with the ratio of 1 ︰ 9, tap water is not further processed.Due in tap water
Plumbum ion concentration is especially low, is detected using standard addition method to it.By 0.010 μM, 0.070 μM, 0.10 μM of lead ion
Solution is added in mixed liquor, is tested and analyzed using carbonization microcapsules electrode to it, the results showed that 0.0098 μM, 0.0717
μM and 0.099 μM of lead ion be present in detection solution, the rate of recovery shows the modification between 98.0% to 102.5%
Detection and analysis of the electrode for lead ion actual sample are feasible.
In summary, the preparation method of the electrochemical sensing of trace lead ion detection of the invention, the modification of working electrode
Material preparation is simple, at low cost, structure-controllable and reproducible.Prepared electrochemical sensor is to detecting and selecting property of lead ion
High and detection limit is low, reproducible.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the electrochemical sensing of trace lead ion detection characterized by comprising
Step 1: by the gelatin-based microcapsules of complex coacervation preparation after freeze-dried, being carbonized under nitrogen protection, after carbonization
Microscapsule powder ultrasonic disperse in chitosan acetic acid solution；
Step 2: glass-carbon electrode polishing, ultrasonic cleaning is clean, the carbonization microcapsules for then taking 5 μ L steps 1 made with liquid-transfering gun
In glassy carbon electrode surface, drying at room temperature obtains working electrode for dispersion liquid modification, and platinized platinum is used as to electrode, silver/silver chlorate conduct
Reference electrode constitutes three-electrode system；
Step 3: the lead ion electrolyte of various concentration being added to composition 5mL prepare liquid in buffer solution, by three in step 2
Electrode system is inserted into above-mentioned lead ion electrolyte, and constant voltage is enriched with the lead ion in electrolyte；
Step 4: using Differential Pulse Anodic Stripping Voltammetry, Current-potential curve stacking chart when record dissolves out obtains peak electricity
The standard curve of flow valuve and plumbum ion concentration；
Step 5: the sample to be tested of unknown plumbum ion concentration is measured with above-mentioned three-electrode system, obtains corresponding peak point current,
Then plumbum ion concentration in sample to be tested is obtained according to standard curve.
2. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 1, the mass concentration of chitosan acetic acid solution is 1mg/mL, and the mass fraction of acetic acid solution is 0.5~5%, after carbonization
The mass ratio of microscapsule powder and chitosan acetic acid solution is 0.5~5 ︰ 1.
3. the preparation method of trace lead ion detection electrochemical sensing according to claim 2, which is characterized in that the step
In rapid 1, the cyst material of gelatin-based microcapsules is gelatin-gum arabic, gelatin-sodium carboxymethyl cellulose-dodecyl sulphate
Sodium, gelatin-sodium carboxymethyl cellulose-bis- (2- second hexyl) sodium sulfosuccinates, gelatin-sodium carboxymethyl cellulose-polysiloxanes
Carboxylic acid acid sodium or gelatin-sodium alginate.
4. the preparation method of trace lead ion detection electrochemical sensing according to claim 3, which is characterized in that the step
In rapid 1, carburizing temperature when gelatin-based microcapsules are carbonized is 600~800 DEG C, and carbonization time is 5~10 hours.
5. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 3, leaded ion electrolyte is Pb (NO3)2、Pb(CH3COO)2Or PbSO4, molar concentration is 1nmol/L~10 μm ol/L.
6. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 3, buffer solution is that NaAc_HAc buffer solution, sodium dihydrogen phosphate-disodium hydrogen phosphate or ammonia-sal-ammoniac, pH value are
4~5.
7. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 3, the ratio between amount of substance is 1 ︰ 0.04~400 when leaded ion electrolyte is mixed with buffer solution.
8. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 3, constant voltage is enriched with the lead ion in prepare liquid, and accumulating potential is -1.0~-0.4V, and enrichment time is 200~500s.
9. the preparation method of trace lead ion detection electrochemical sensing according to claim 1, which is characterized in that the step
In rapid 4, the take-off potential of Differential Pulse Anodic Stripping Voltammetry is -1.4V~-0.9V, and termination current potential is -0.4V~-0.2V.
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| CN109884147A (en) * | 2019-03-22 | 2019-06-14 | 石河子大学 | A kind of electrochemical method of walnut shell base Carbon Materials modified glassy carbon electrode detection trace heavy metal |
| CN115753933A (en) * | 2022-12-22 | 2023-03-07 | 中国热带农业科学院南亚热带作物研究所 | Preparation method and application of carboxymethyl chitosan-based hydrogel modified electrode |
| CN115753933B (en) * | 2022-12-22 | 2023-08-11 | 中国热带农业科学院南亚热带作物研究所 | Preparation method and application of carboxymethyl chitosan-based hydrogel modified electrode |
| CN117191898A (en) * | 2023-09-13 | 2023-12-08 | 北京工商大学 | Electrode material, preparation method and manganese ion sensor |
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