CN103776887A - Preparation method of self-assembled film mercury ion selective electrode - Google Patents
Preparation method of self-assembled film mercury ion selective electrode Download PDFInfo
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- CN103776887A CN103776887A CN201410066379.6A CN201410066379A CN103776887A CN 103776887 A CN103776887 A CN 103776887A CN 201410066379 A CN201410066379 A CN 201410066379A CN 103776887 A CN103776887 A CN 103776887A
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Abstract
The invention discloses a self-assembled film mercury ion selective electrode (1) which comprises a substrate (11) of a working gold film (12) modified by a 11-aminohendecylmercaptan film layer (25), wherein the working gold film (12) covered on the substrate (11) is connected with a pin gold film (13) through a gold film layer; the pin gold film (13) is connected with a metal wire (15) coated with a plastic insulation layer (14) through soldering tin (16); the substrate (11) is prepared by gradually spattering and depositing a silicon dioxide film layer (22), a metallic chromium film layer (23), a copper alloy film layer (24) and the gold film layer on a polished silicon borate base plate (21); moreover, the modified 11-aminohendecylmercaptan film layer (25) is assembled on the surface of the working gold film (12). The selective electrode is simple to manufacture, low in cost and convenient to use, and can be used for quickly detecting trace amounts of mercury ions in the environment; the lower limit of detection is 6.3 nmol/L.
Description
Technical field
The present invention relates to a kind of self-assembled film mercury ion based on the amino undecyl mercaptan of 11-and select electrode, belong to chemical/biological field of sensing technologies, be applicable to Environmental security and detect.
Background technology
Mercury pollution is a global problem, and due to its severe toxicity and bioconcentration, it has received increasing concern.Dimercurion (Hg
2+) be the most stable inorganic mercury, be present in natural water body Hg
2+even micro-concentrations also can produce toxicity, it can be accumulated in vivo, by food chain transport in human body, and the Trace Mercury of accumulation cannot be drained by self metabolism in human body, to directly cause heart, liver, thyroid disease, cause nerve problems, chronic mercury poisoning, even causes the formation of malignant tumour.Secondly, the ecological methylate methyl mercury of the microorganism of mercury ion, is also a kind of strong toxin, can be delivered in the tissue of fish and marine mammal by food chain, is converted into hypertoxic organic mercury.Therefore, can quick and precisely analyze the heavy metal Hg content in the media such as water body in living environment, be of great significance for the life quality, the environment tool of preserving our planet that improve the mankind.
At present, the method that detects metal mercury ions has a lot, as atomic spectroscopy, inductively coupled plasma atomic emission spectrum (ICP-AES method), spectrophotometric method, high performance liquid chromatography, inductively coupled plasma mass spectrometry (ICPMS), chemoluminescence method and fluorometry etc.But these methods often need expensive exact instrument, complicated sample preparation flow process and skilled operating personnel, can not or inconvenience carry out out of doors fast detecting, limited to a great extent its application.The novel electrochemical sensor of a class that the seventies grows up as very portable ion-selective electrode (ISE), compared with classic method, because it has the advantages such as low, the simple to operate and easy miniaturization of cost, be subject to many researchers' favor; And, molecular self-assembling monofilm (Self-assembled Monolayers, SAMs) be emerging in recent years a kind of electrochemical analysis interfacial activity sensitive membrane technology, in structure and performance, there is similar biomembranous characteristic, become gradually the focus in electrochemical sensing technical research field.
Based on current correlative study, realize and mercury ion is carried out to qualitative or quantitative research have not been reported in conjunction with self-assembled film technology and ion-selective electrode method.For this reason, the present invention modifies golden film surface by unimolecule self-assembling method by amino 11-undecyl mercaptan assembling, forms a kind of mercury ion based on the amino undecyl mercaptan of 11-self-assembled film and selects electrode.This selection electrode fabrication is simple, with low cost, easy to use, sensitivity is very high, be better than traditional instrument analytical method, can be used for the fast detecting of Trace Mercury ion in environment, in the fields such as environmental monitoring, agricultural food product and biomedicine, there is very important application prospect.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of simple, with low cost, easy to use, highly sensitive self-assembled film mercury ion selection electrode of making, and can be used for Environmental security and detects.
In order to achieve the above object, the technical solution used in the present invention is: a kind of self-assembled film mercury ion is selected electrode, it is characterized in that this selection electrode comprises the substrate of the work gold film of the amino undecyl mercaptan of 11-rete modification, the work gold film covering on this substrate is connected by golden membranous layer with pin gold film, pin gold film is connected by scolding tin with the tinsel wire that is surrounded by plastic insulating layer outward, the material of tinsel wire is copper wire, aluminium wire or filamentary silver, junction epoxide-resin glue environmental sealing, to guarantee good conduction, conduction, and guarantee the usable floor area of work gold film and the uniqueness of work conduction, interference-free impact.Configuration design that it should be noted that described substrate is shown an interesting new approach, as follows: the work that covers on substrate gold film be shaped as square, the length of side is 2 ~ 12mm; Pin gold film be shaped as small rectangle, length is 1 ~ 6mm, wide is 1 ~ 4mm; Whole substrate be shaped as rectangle, length is 3 ~ 18mm, wide is 2 ~ 12mm, its edge is all with epoxide-resin glue sealing, to guarantee good electrical insulating property.The configuration design of whole substrate can fully guarantee the consistance of the effective usable floor area of square of all selection electrode work gold films, can guarantee to select again the long-time stability of electrode life.
Aspect the Design & preparation of selection electrode, selecting the different preparation that also has described substrate of electrode method from conventional ion is to deposit to form fine and close senser element structure by vacuum coating, select the controlled preparation of electrode and select the long-term stability using of electrode effectively guaranteeing, its preparation process is as follows: adopt magnetron sputtering embrane method, by controlling plated film vacuum tightness≤2.0 × 10
-3pa, coating speed≤2.0/s, progressively sputtering sedimentation silica coating, crome metal rete, aldary rete on the borosilicate substrate surface of polishing; Aldary rete, after polishing, then adopts mask plate method sputtering sedimentation work in its surface gold film and pin gold film; The golden film of working is assembled in its surface again and is modified the amino undecyl mercaptan of 11-rete after chemical cleaning is processed.Wherein, on the borosilicate substrate surface of polishing, progressively the thickness of the silica coating of sputtering sedimentation is 60 ~ 400nm, and the thickness of crome metal rete is 20 ~ 120nm, and the thickness of aldary rete is 60 ~ 400nm; Aldary rete after polishing, in its surface the thickness of deposition work gold film and pin gold film be 20 ~ 420nm.And, the quality percentage composition of tin-copper alloy film WU layer material each component is respectively: Cu 45 ~ 60%, Mn 20 ~ 28%, Ni 12 ~ 24%, Fe 4 ~ 9%, Ti 0.1 ~ 0.4%, Nb 0.01 ~ 0.05%, wherein, the use of niobium makes the crystal grain of aldary more careful evenly, the use of titanium makes aldary flexible more, and improves acid and alkali-resistance and anti-corrosion capability.
Aspect the modification of selection electrode film, the present invention proposes the assembling method of modifying of the amino undecyl mercaptan of a kind of simple 11-rete, first the high-purity pure water in work gold film surface of selecting electrode base sheet is cleaned, successively at high-purity pure water, each 0.1 ~ 20 minute of ultrasonic cleaning in absolute ethyl alcohol, then take out in the amino undecyl mercaptan/ethanol solution of 11-that immerses 0.1 ~ 200mmol/L, self assembly 1 ~ 72 hour in 4 ℃ of refrigerators, take out dry, obtain the selection electrode that the amino undecyl mercaptan of 11-rete is modified, the used time is not placed in deionized water in 4 ° of C refrigerator sealing preservations.Wherein, described high-purity pure water is the high purity water that resistivity is greater than 18M Ω cm, the anhydrous ethanol solvent that absolute ethyl alcohol is re-distillation.
Aspect the electro-chemical test of selection electrode, proving installation is simple, easy to operate, it is as follows that this self-assembled film mercury ion is selected the electrochemical testing device of electrode: select electrode as working electrode take this self-assembled film mercury ion, saturated calomel electrode is contrast electrode, and two electrodes are connected with pot by wire; When test, self-assembled film mercury ion selects electrode and saturated calomel electrode to insert in the beaker that stirring magneton is housed, and beaker is placed on magnetic stirring apparatus, and the pH buffer solution of mercurous ion is housed in beaker; By testing the potential value of mercury ion standard solution of a series of concentration known, with potential value to the concentration value curve of working, then test the potential value of unknown concentration mercury ion sample solution, obtain concentration value or the content of mercury ion in sample solution by working curve.Wherein, the Tris-HCl solution that described pH buffer solution is pH4.0 ~ 10.0, its compound method is that the HCl solution of the Tris solution of 0.1mol/L and 0.1mol/L is mixed by proper proportion, regulates its pH value with the NaOH solution of 0.1mol/L or the HCl solution of 0.1mol/L.Find by test experiments, the potential response value of this selection electrode and the concentration of mercury ion are 1.0 × 10
-8~ 1.0 × 10
-4linear within the scope of mol/L, the detection lower limit of mercury ion is reached to 6.3 × 10
-9mol/L, i.e. 6.3nmol/L.
The invention has the beneficial effects as follows, this selection electrode fabrication is simple, with low cost, easy to use, and golden film flatness is high, easily carry out finishing, sensitivity is very high, be better than traditional instrument analytical method, can be used for the fast detecting of Trace Mercury ion in environment, in the fields such as environmental monitoring, agricultural food product and biomedicine, there is very important application prospect.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described.
Accompanying drawing 1 is the electrochemical testing device schematic diagram that self-assembled film mercury ion is selected electrode.
Accompanying drawing 2 is planar structure schematic diagram that self-assembled film mercury ion is selected electrode.
Accompanying drawing 3 is cross-sectional view that self-assembled film mercury ion is selected electrode base sheet.
In accompanying drawing 1,1. self-assembled film mercury ion is selected electrode, 2. saturated calomel electrode, and 3. pot, 4. stirs magneton, 5. beaker, 6. magnetic stirring apparatus.
In accompanying drawing 2 and accompanying drawing 3,11. substrates, the golden film of 12. work, 13. pin gold films, 14. plastic insulating layers, 15. tinsel wires, 16. scolding tin, 17. epoxide-resin glues, 21. borosilicate substrates, 22. silica coatings, 23. crome metal retes, 24. aldary retes, the amino undecyl mercaptan of 25. 11-rete, the amino undecyl thiol molecule of 26. 11-.
Embodiment
embodiment 1
Select the assembling preparation of electrode:
A kind of planar structure schematic diagram of self-assembled film mercury ion selection electrode as shown in Figure 2, this selection electrode comprises the substrate 11 of the work gold film 12 that the amino undecyl mercaptan of 11-rete 25 modifies, the work gold film 12 covering on this substrate 11 is connected by golden membranous layer with pin gold film 13, pin gold film 13 is connected by scolding tin 16 with the tinsel wire 15 that is surrounded by plastic insulating layer 14 outward, the material of tinsel wire 15 is copper wire, epoxide-resin glue 17 environmental sealings for junction, to guarantee good conduction, conduction.
As shown in Figure 2, as follows to the configuration design of described substrate 11: the work gold film 12 covering on substrate 11 be shaped as square, the length of side is 6mm; Pin gold film 13 be shaped as small rectangle, long is 3mm, wide is 1mm; Whole substrate 11 be shaped as rectangle, long is 9mm, wide is 6mm, its edge all seals with epoxide-resin glue.
As shown in Figure 3, the preparation process of described substrate 11 is as follows: adopt magnetron sputtering embrane method, controlling plated film vacuum tightness is 1.2 × 10
-3pa, coating speed is 1.0/s, progressively sputtering sedimentation silica coating 22, crome metal rete 23, aldary rete 24 on borosilicate substrate 21 surfaces of polishing; Aldary rete 24, after polishing, then adopts mask plate method sputtering sedimentation work in its surface gold film 12 and pin gold film 13; The golden film 12 of working is assembled in its surface again and is modified the amino undecyl mercaptan of 11-rete 25 after chemical cleaning is processed.Wherein, on borosilicate substrate 21 surfaces of polishing, progressively the thickness of the silica coating 22 of sputtering sedimentation is 280nm, and the thickness of crome metal rete 23 is 40nm, and the thickness of aldary rete 24 is 220nm; Aldary rete 24 after polishing, in its surface the thickness of deposition work gold film 12 and pin gold film 13 be 150nm; The quality percentage composition of aldary rete 24 material each components is controlled respectively and is: Cu 54.8%, Mn 23.7%, Ni 14.9%, Fe 6.36%, Ti 0.21%, Nb 0.03%.
It should be noted that the assembling method of modifying of the amino undecyl mercaptan of 11-rete 16, first the high-purity pure water in work gold film 12 surfaces of selecting electrode base sheet 11 is cleaned, each 1 minute of ultrasonic cleaning in high-purity pure water, absolute ethyl alcohol successively, then take out in the amino undecyl mercaptan/ethanol solution of 11-that immerses 10mmol/L, self assembly 12 hours in 4 ℃ of refrigerators, take out dry, obtain the selection electrode that the amino undecyl mercaptan of 11-rete 25 is modified, the used time is not placed in deionized water in 4 ° of C refrigerators sealing preservations.Wherein, high-purity pure water is the high purity water that resistivity equals 18.3M Ω cm, the anhydrous ethanol solvent that absolute ethyl alcohol is re-distillation.
embodiment 2
The detection of mercury ion:
The mercury ion that the amino undecyl mercaptan of the 11-rete 25 that said method assembling is modified is modified selects electrode 1 for working electrode, and saturated calomel electrode 2 is as contrast electrode, and two electrodes are connected with pot 3 by wire, carry out electrochemical potential test; When test, self-assembled film mercury ion selects electrode 1 and saturated calomel electrode 2 to insert in the beaker 5 that stirring magneton 4 is housed, and beaker 5 is placed on magnetic stirring apparatus 6, and the pH buffer solution of mercurous ion is housed in beaker 5; By testing the potential value of mercury ion standard solution of a series of concentration known, with potential value to the concentration value curve of working, then test the potential value of unknown concentration mercury ion sample solution, obtain concentration value or the content of mercury ion in sample solution by working curve.Find by test experiments, the potential response value of this selection electrode and the concentration of mercury ion are 1.0 × 10
-8~ 1.0 × 10
-4linear within the scope of mol/L, the detection lower limit of mercury ion is reached to 6.3 × 10
-9mol/L, i.e. 6.3nmol/L.
embodiment 3
Select the reappearance of electrode:
The mercury ion that the amino undecyl mercaptan of 10 11-rete 25 of assembling as stated above modification is modified selects electrode 1 for working electrode, and saturated calomel electrode 2 is as contrast electrode, respectively to 1.0 × 10
-6mol/L and 1.0 × 10
-7the mercury ion solution example of mol/L carries out electrochemical potential test, can find out, is carrying out continuously after 10 mensuration, and relative standard deviation is respectively 0.55% and 0.52%, shows the favorable reproducibility of this selection electrode detection method.
embodiment 4
Select the selectivity of electrode:
The mercury ion that the amino undecyl mercaptan of 10 11-rete 25 of assembling as stated above modification is modified selects electrode 1 for working electrode, and saturated calomel electrode 2, as contrast electrode, has been investigated respectively the impact that Common Cations is measured mercury ion, finds K
+, Ca
2+, Na
+, Mg
2+, Ba
2+, Cu
2+, Fe
2+, Ag
+, Zn
2+, Bi
3+, Co
2+, Sr
2+, Mn
2+, NH
4 +interference Deng 16 metal ion species is not obvious, shows that the selectivity of this selection electrode detection method is good.
embodiment 5
The mensuration of mercury ion in environmental wastewater sample:
The mercury ion that the amino undecyl mercaptan of 10 11-rete 25 of assembling as stated above modification is modified selects electrode 1 for working electrode, saturated calomel electrode 2 is as contrast electrode, the mark-on of having investigated respectively mercury ion in 8 water samples detects, the recovery, between 93.7 ~ 105.8%, illustrates that the method recovery is good; And contrast with standard dithizone spectrophotometry, the measurement result of sample is more consistent, meets the requirement of quantitative test, illustrates that this selection electrode can be applicable to the detection of mercury ion in real wastewater samples.
Claims (11)
1. a self-assembled film mercury ion is selected electrode (1), it is characterized in that this selection electrode comprises the substrate (11) of the work gold film (12) of the amino undecyl mercaptan rete of a 11-(25) modification, the upper work gold film (12) covering of this substrate (11) is connected by golden membranous layer with pin gold film (13), pin gold film (13) is connected by scolding tin (16) with the tinsel wire (15) that is surrounded by plastic insulating layer (14) outward, epoxide-resin glue for junction (17) environmental sealing.
2. selection electrode according to claim 1, is characterized in that the configuration design of described substrate (11) is as follows: the upper work gold film (12) covering of substrate (11) be shaped as square, the length of side is 2 ~ 12mm; Pin gold film (13) be shaped as small rectangle, length is 1 ~ 6mm, wide is 1 ~ 4mm; Whole substrate (11) be shaped as rectangle, length is 3 ~ 18mm, wide is 2 ~ 12mm, its edge all seals with epoxide-resin glue.
3. selection electrode according to claim 1, the material that it is characterized in that described tinsel wire (15) is copper wire, aluminium wire or filamentary silver.
4. selection electrode according to claim 1, is characterized in that the preparation process of described substrate (11) is as follows: adopt magnetron sputtering embrane method, by controlling plated film vacuum tightness≤2.0 × 10
-3pa, coating speed≤2.0/s, progressively sputtering sedimentation silica coating (22), crome metal rete (23), aldary rete (24) on borosilicate substrate (21) surface of polishing; Aldary rete (24), after polishing, then adopts mask plate method sputtering sedimentation work in its surface gold film (12) and the golden film of pin (13); The golden film (12) of working is assembled in its surface and is modified the amino undecyl mercaptan rete of 11-(25) again after chemical cleaning is processed.
5. selection electrode according to claim 4, it is characterized in that: on borosilicate substrate (21) surface of polishing, progressively the thickness of the silica coating of sputtering sedimentation (22) is 60 ~ 400nm, the thickness of crome metal rete (23) is 20 ~ 120nm, and the thickness of aldary rete (24) is 60 ~ 400nm; Aldary rete (24) after polishing, in its surface the thickness of deposition work gold film (12) and the golden film of pin (13) be 20 ~ 420nm.
6. selection electrode according to claim 4, is characterized in that the quality percentage composition of aldary rete (24) material each component is respectively: Cu 45 ~ 60%, Mn 20 ~ 28%, Ni 12 ~ 24%, Fe 4 ~ 9%, Ti 0.1 ~ 0.4%, Nb 0.01 ~ 0.05%.
7. selection electrode according to claim 4, it is characterized in that the assembling method of modifying of the amino undecyl mercaptan rete of 11-(25), first will select the high-purity pure water in work gold film (12) surface of electrode base sheet (11) to clean, successively at high-purity pure water, each 0.1 ~ 20 minute of ultrasonic cleaning in absolute ethyl alcohol, then take out in the amino undecyl mercaptan/ethanol solution of 11-that immerses 0.1 ~ 200mmol/L, self assembly 1 ~ 72 hour in 4 ℃ of refrigerators, take out dry, obtain the selection electrode that the amino undecyl mercaptan rete of 11-(25) is modified, the used time is not placed in deionized water in 4 ° of C refrigerator sealing preservations.
8. selection electrode according to claim 7, is characterized in that described high-purity pure water is the high purity water that resistivity is greater than 18M Ω cm, the anhydrous ethanol solvent that absolute ethyl alcohol is re-distillation.
9. selection electrode according to claim 1, the electrochemical testing device that it is characterized in that this self-assembled film mercury ion selection electrode (1) is as follows: select electrode (1) as working electrode take this self-assembled film mercury ion, saturated calomel electrode (2) is contrast electrode, and two electrodes are connected with pot (3) by wire; When test, self-assembled film mercury ion selects electrode (1) and saturated calomel electrode (2) to insert in the beaker (5) that stirring magneton (4) is housed, and it is upper that beaker (5) is placed on magnetic stirring apparatus (6), and the pH buffer solution of mercurous ion is housed in beaker (5); By testing the potential value of mercury ion standard solution of a series of concentration known, with potential value to the concentration value curve of working, then test the potential value of unknown concentration mercury ion sample solution, obtain concentration value or the content of mercury ion in sample solution by working curve.
10. selection electrode according to claim 9, it is characterized in that the Tris-HCl solution that described pH buffer solution is pH4.0 ~ 10.0, its compound method is that the HCl solution of the Tris solution of 0.1mol/L and 0.1mol/L is mixed by proper proportion, regulates its pH value with the NaOH solution of 0.1mol/L or the HCl solution of 0.1mol/L.
11. selection electrodes according to claim 9, is characterized in that the potential response value of this selection electrode and the concentration of mercury ion are 1.0 × 10
-8~ 1.0 × 10
-4linear within the scope of mol/L, the detection lower limit of mercury ion is reached to 6.3 × 10
-9mol/L, i.e. 6.3nmol/L.
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| CN102778492A (en) * | 2012-07-13 | 2012-11-14 | 首都师范大学 | Electrochemical transducer for mercury ion detection and manufacturing method and detection method thereof |
| CN103105424A (en) * | 2013-01-30 | 2013-05-15 | 首都师范大学 | Electrochemical sensor for mercury ion detection, and manufacturing method and detection method thereof |
| CN103344683A (en) * | 2013-07-15 | 2013-10-09 | 长沙理工大学 | Sensing chip method for detecting mercury ions |
| CN203337596U (en) * | 2013-07-15 | 2013-12-11 | 长沙理工大学 | Sensing chip for detecting mercury ions |
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2014
- 2014-02-26 CN CN201410066379.6A patent/CN103776887B/en active Active
Patent Citations (6)
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|---|---|---|---|---|
| US20090260984A1 (en) * | 2008-04-22 | 2009-10-22 | Indian Institute Of Technology | Ultra-Sensitive Simultaneous Electrochemical Determination of Arsenic, Mercury and Copper |
| CN102706940A (en) * | 2012-06-15 | 2012-10-03 | 湖南大学 | Electrochemical sensor capable of detecting trace mercury in water body, and preparation method and application thereof |
| CN102778492A (en) * | 2012-07-13 | 2012-11-14 | 首都师范大学 | Electrochemical transducer for mercury ion detection and manufacturing method and detection method thereof |
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