CN1975398A - Full solid Zn ion selective electrode and producing method thereof - Google Patents
Full solid Zn ion selective electrode and producing method thereof Download PDFInfo
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- CN1975398A CN1975398A CN 200610017275 CN200610017275A CN1975398A CN 1975398 A CN1975398 A CN 1975398A CN 200610017275 CN200610017275 CN 200610017275 CN 200610017275 A CN200610017275 A CN 200610017275A CN 1975398 A CN1975398 A CN 1975398A
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- paxilla
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Abstract
A whole solid Zn2+ selective electrode is made up of the resin tube, the back cover which the column material is sensitive to the Zn2+, the copper lead and the resin cover. The spectrally ZnS, Ag2S, As2S3 and the AgI are mixed according to the mole ratio of 35:15:25:5 to 45:25:35:15 and grinded to press to the small cuboid and put in the quartz bottle, then it is heated to 600DEG C and keep for 3h in the drying N2; next to anneal naturally and grind out the small cuboid to get the small columella with high/wide of 0.25-4, then it is heated to 600DEG C and keep for 3h next to anneal naturally. After polishing it gets the product. The invention is convenience to carry and detects the Zn2+ in water, blood, vegetable and fruit quickly and accurately.
Description
Technical field
The invention belongs to the used a kind of electrode of analysis field, relate in particular to the preparation method of a kind of full solid Zn ion selective electrode and this electrode thereof.
Background technology
As everyone knows, heavy metal ion is (as Zn
2+, Pb
2+, Cd
2+, Cu
2+, Cr
6+, Mn
5+, As
3+, Fe
3+, Hg
2+) can produce harm even fatal influence to human body after exceeding standard, so the detection by quantitative of heavy metal has very important meaning at aspects such as medicine, food, clinical and environmental monitorings.Present detection method mainly contains atomic absorption spectrophotometry and mass spectroscopy etc., but adopt the equipment of these methods huge, and expensive, need complicated pretreatment, measuring period is long and need skilled operating personnel, and this gives in the practical application and brings many inconveniences.This problem has caused the leader of this area and the common concern of vast technology, and becomes the important topic of development and exploitation.
Summary of the invention
The objective of the invention is to solve the problem of above-mentioned existence, provide a kind of volume little, easy to carry, measure accurately, be used to detect the preparation method of full solid Zn ion selective electrode and this electrode thereof of zinc ion.
The objective of the invention is to adopt following technical scheme to realize:
A kind of full solid Zn ion selective electrode is characterized in that: it is by pitch tube, is encapsulated in the Zn ion pillar shape sensitive material in the pitch tube lower nozzle, for the resin capping in back cover, copper conductor and the pitch tube upper orifice of pitch tube is formed; Copper conductor is drawn from the resin capping, and described Zn ion pillar shape sensitive material is to select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, its mol ratio is 35: 15: 25: 5 to 45; 25: 35: 15, process from strand: the preparation method of this selection electrode:
With spectra pure compound ZnS, Ag
2S, As
2S
3And AgI, by above-mentioned molar ratio ingredient, behind abundant mixed grinding, be pressed into little rectangular parallelepiped, be put in the quartzy bottle, under the condition of nitrogen gas of drying, be heated to 600 ℃, kept 3 hours; Naturally annealing then, broken little rectangular parallelepiped grinding again again, making height/wide ratio is 0.25～4 paxilla; This paxilla is placed in the vitreosil bottle, is heated to 600 ℃, kept 3 hours, naturally annealing; Take out paxilla,, make Zn ion pillar shape sensitive material its polishing; With this paxilla and copper conductor upward fixing with the welding of silver slurry and that draw thereof, be encapsulated in pitch tube (1) lower nozzle, its paxilla (2) is a back cover again, and upper orifice is provided with the resin capping, and copper conductor is drawn from the resin capping, makes full solid Zn ion selective electrode.
A kind of preparation method of full solid Zn ion selective electrode is characterized in that it is made up of following two step processes:
1. the preparation of Zn ion-sensitive material and full solid Zn ion pillar shape sensitive material
Select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, by 35: 15: 25: 5 to 45; Mol ratio was prepared burden in 25: 35: 15, behind abundant mixed grinding, under 14Mpa pressure, made little rectangular parallelepiped, was put in the quartzy bottle, under the condition of nitrogen gas of drying, was heated to 600 ℃, kept 3 hours; Naturally annealing then, broken little rectangular parallelepiped grinding again again, making height/wide ratio is 0.25～4 paxilla; Place it in then in the vitreosil bottle, be heated to 600 ℃, kept 3 hours, naturally annealing; Take out paxilla,, make Zn ion pillar shape sensitive material its polishing;
2. the encapsulation of full solid Zn ion selective electrode
After connecing, a face down bonding of above-mentioned paxilla draws a copper conductor with conductive silver paste, the full solid Zn ion pillar shape sensitive material that 1. step is made and on copper conductor be encapsulated in the pitch tube, described paxilla is a back cover, the pitch tube upper orifice is provided with the resin capping, copper conductor is drawn from the resin capping, makes full solid Zn ion selective electrode.
The advantage that the present invention has is: can detect the Zn ion, the electrode corrosion resistance is strong, and the life-span can reach more than 1 year, and required sample is few, measures fast, and is easy to use, measures accurately, and interfering ion is few.This all solid-state electrode can carry out qualitative and detection by quantitative to the Zn ion in fields such as rivers,lakes and seas, biomedical sector such as blood, body fluid etc., industrial waste water, Chinese medicine, vegetables, fruit, tealeaves.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the structural drawing of full solid Zn ion selective electrode of the present invention;
Fig. 2 is the typical curve of full solid Zn ion selective electrode; Wherein
1-pitch tube 2-Zn ion pillar shape sensitive material 3-copper conductor
Embodiment
Now the present invention is further described as follows with embodiment in conjunction with the accompanying drawings:
Embodiment 1:
As shown in Figure 1, full solid Zn ion selective electrode is to be back cover by epoxy (or tygon) pitch tube 1, full solid Zn ion pillar shape sensitive material 2, draws copper conductor 3 and epoxy (or tygon) resin capping composition with conductive silver paste after a face down bonding of above-mentioned paxilla connects.Described Zn ion pillar shape sensitive material 2 is by spectra pure compound ZnS, Ag
2S, As
2S
3And AgI, be 40: 20: 30 in molar ratio: 10 are processed into.
The preparation of full solid Zn ion selective electrode;
1. the preparation of Zn ion pillar shape sensitive material
Select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, mol ratio 40: 20: 30: 10, fully behind the mixed grinding, under 14Mpa pressure, make little rectangular parallelepiped, be put in the quartzy bottle, under the condition of nitrogen gas of drying, be heated to 600 ℃, kept 3 hours; Naturally annealing then, broken little rectangular parallelepiped grinding again again, making diameter is 1cm, thickness is the paxilla (cylinder or square column type) of 1cm; Be placed in the vitreosil bottle, be heated to 600 ℃, kept 3 hours; Naturally small cylinder is taken out in annealing, with its polishing, promptly makes Zn ion pillar shape sensitive material 2;
2. the encapsulation of full solid Zn ion selective electrode
Adopt conductive silver paste to weld and draw a copper conductor 3 at the upper surface of small cylinder, and with copper conductor 3 and full solid Zn ion pillar shape sensitive material 2, be encapsulated in an epoxy (tygon) pitch tube 1 lower nozzle, pillar shape sensitive material is the back cover of pitch tube, copper conductor 3 is drawn from the resin capping of the upper orifice of pitch tube, promptly makes full solid Zn ion selective electrode.
1. the spectra pure compound ZnS, the Ag that select for use of example 1～3
2S, As
2S
3, AgI consumption and pillar height/wide
| The embodiment sequence number | Spectra pure compound of selecting for use and consumption | Paxilla height and width cm | |||
| ZnS(mol) | Ag 2S(mol) | As 2S 3(mol) | AgI(mol) | ||
| 1 | 40 | 20 | 30 | 10 | 1 |
| 2 | 45 | 25 | 35 | 15 | 4 |
| 3 | 35 | 15 | 25 | 5 | 0.5 |
The selectivity principle of full solid Zn ion selective electrode electrode:
Zn ion in the full solid Zn ion selective electrode in the Zn ion pillar shape sensitive body material and the Zn ion in the measured solution produce ion-exchange reactions.
The characteristic of full solid Zn ion selective electrode:
Full solid Zn ion selective electrode to the typical curve of Zn ion selectivity as shown in Figure 2.Detect lower limit and be respectively 3 * 10
-7Mol/L.The response time of electrode omits hurry up when concentration is high relatively less than 3min.And after measuring high concentration Zn solion, when measuring low concentration again, do not find significant concentration hesitation phenomenon.
The application of full solid Zn ion selective electrode of the present invention:
With full solid Zn ion selective electrode of the present invention, the saturated KCl mercurous chloride electrode of purchasing from the market, be connected with universal meter with lead respectively, place desire to detect the sample solution of its Zn ion concentration at above-mentioned two electrodes, after the energized, current potential E (mV) value that shows on the universal meter, in above-mentioned full solid Zn ion selective electrode shown in Figure 2, to determining this current potential E (mV) value on the canonical plotting ordinate of Zn ion selectivity, the 1g[Zn of its abscissa correspondence] value, be exactly the logarithm value that desire is surveyed the Zn ion concentration that is contained in the solution, can find Zn ion concentration value the actual detected solution from table of logarithm.From above-mentioned we be not difficult to find out: full solid Zn ion selective electrode of the present invention has easy to carry, and Zn ion concentration in the sample that desire is detected can be rapidly, quantitatively measure accurately, and is easy to use, provides reliable data foundation for science decision person fast.
Claims (2)
1, a kind of full solid Zn ion selective electrode is characterized in that: it is made up of for back cover, copper conductor (3) and the capping of pitch tube (1) upper orifice resin pitch tube (1), the Zn ion pillar shape sensitive material (2) that is encapsulated in pitch tube (1) lower nozzle; Copper conductor (3) is drawn from the resin capping; Described Zn ion-sensitive material is to select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, with 35: 15: 25: 5 to 45: 25: 35: 15 molar ratio ingredients are processed into; Its preparation method:
Select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, behind abundant mixed grinding, be pressed into little rectangular parallelepiped by above-mentioned molar ratio ingredient, be put in the quartzy bottle, under the drying nitrogen condition, be heated to 600 ℃, kept 3 hours; Naturally annealing is then ground little rectangular parallelepiped brokenly more again, makes height/wide ratio and be 0.25～4 cylinder or square column type paxilla, places it in the vitreosil bottle, is heated to 600 ℃, keeps 3 hours, anneals naturally; Take out paxilla,, make Zn ion pillar shape sensitive material (2) its polishing; Again with this paxilla (2) and copper conductor (3) upward fixing and that draw thereof with the welding of silver slurry, be encapsulated in cylindrical or square column type pitch tube (1) lower nozzle in, its paxilla (2) is a back cover, upper orifice is provided with the resin capping, copper conductor 3 is drawn from the resin capping, makes full solid Zn ion selective electrode.
2, the preparation method of a kind of full solid Zn ion selective electrode as claimed in claim 1 is characterized in that it is made up of following two step processes:
1. the preparation of Zn ion-sensitive material and Zn ion pillar shape sensitive material thereof
Select spectra pure compound ZnS, Ag for use
2S, As
2S
3And AgI, its mol ratio is 35: 15: 25: 5 to 45: 25: 35: 15, behind abundant mixed grinding, under 14Mpa pressure, make little rectangular parallelepiped, and be put in the quartzy bottle, under the condition of nitrogen gas of drying, be heated to 600 ℃, kept 3 hours; Naturally annealing is then ground little rectangular parallelepiped brokenly more again, makes height/wide ratio and be 0.25～4 cylindrical or square column type paxilla; Place it in then in the vitreosil bottle, be heated to 600 ℃, kept 3 hours; Naturally paxilla is taken out in annealing, with its polishing, makes Zn ion pillar shape and selects sensitive material (2);
2. the encapsulation of full solid Zn ion selective electrode
Weld and draw a copper conductor (3) with conductive silver paste at above-mentioned paxilla upper surface, the full solid Zn ion pillar shape sensitive material (2) that 1. step is made and on copper conductor be encapsulated in a pitch tube (1) lower nozzle, described paxilla is a back cover, the pitch tube upper orifice is provided with the resin capping, copper conductor is drawn from the resin capping, makes full solid Zn ion selective electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100172751A CN100434908C (en) | 2006-10-24 | 2006-10-24 | Full solid Zn ion selective electrode and producing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100172751A CN100434908C (en) | 2006-10-24 | 2006-10-24 | Full solid Zn ion selective electrode and producing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1975398A true CN1975398A (en) | 2007-06-06 |
| CN100434908C CN100434908C (en) | 2008-11-19 |
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ID=38125620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100172751A Expired - Fee Related CN100434908C (en) | 2006-10-24 | 2006-10-24 | Full solid Zn ion selective electrode and producing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915798A (en) * | 2010-08-04 | 2010-12-15 | 三峡大学 | Ion selective electrode |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4224114A (en) * | 1979-05-24 | 1980-09-23 | Fiedler Linnersund Ulla M | Method and apparatus for detecting zinc ion activity |
| JPH02304346A (en) * | 1989-05-19 | 1990-12-18 | Nippon Parkerizing Co Ltd | Zinc ion selective electrode |
| JP3306506B2 (en) * | 1999-08-23 | 2002-07-24 | 独立行政法人産業技術総合研究所 | Ion sensor using acyclic peptide |
| NO316341B1 (en) * | 2000-04-14 | 2004-01-12 | Iyvind Mikkelsen | Electrode for voltammetric analysis |
| CN2702309Y (en) * | 2004-06-18 | 2005-05-25 | 刘文涛 | Polarographic apparatus |
-
2006
- 2006-10-24 CN CNB2006100172751A patent/CN100434908C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915798A (en) * | 2010-08-04 | 2010-12-15 | 三峡大学 | Ion selective electrode |
| CN101915798B (en) * | 2010-08-04 | 2014-04-09 | 三峡大学 | Ion selective electrode |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100434908C (en) | 2008-11-19 |
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Granted publication date: 20081119 Termination date: 20111024 |