CN108398473A - Mercury ion for detecting sewage selects the preparation method of electrode - Google Patents
Mercury ion for detecting sewage selects the preparation method of electrode Download PDFInfo
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- CN108398473A CN108398473A CN201810033706.6A CN201810033706A CN108398473A CN 108398473 A CN108398473 A CN 108398473A CN 201810033706 A CN201810033706 A CN 201810033706A CN 108398473 A CN108398473 A CN 108398473A
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Abstract
The present invention relates to burnisher technical fields, specifically, being related to a kind of preparation method of the mercury ion selection electrode for detecting sewage：(1) silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then grind mixture broken, obtain powder；(2) powder in step (1) is added in mold, rectangular shape block is made；(3) block in step (2) is added in container, is full of nitrogen, then heating is annealed, block is ground broken, cylinder is made；Cylinder is heated in nitrogen, is annealed, electrode film is made；(4) electrode film is mounted on connecting tube bottom end, connecting tube bottom end is sealed with dope, potassium nitrate solution is packed into electrode tube after waiting drying；(5) reference electrode is passed through into cap and fastened, cap is then fastened on electrode tube top；(6) conducting wire is connect with reference electrode top.The present invention makes simply, can effectively prepare mercury ion selection electrode.
Description
Technical field
The present invention relates to chemical/biological field of sensing technologies, specifically, being related to a kind of mercury ion for detecting sewage
Select the preparation method of electrode.
Background technology
Pollution is a global problem, and due to its severe toxicity and bioconcentration, it has been received more and more attention.
Dimercurion (Hg2+) it is most stable of inorganic mercury, it is present in natural water body, even Hg2+ micro-concentrations can also generate poison
Property, it can be accumulated in vivo, and into the human body by food chain transport, and the Trace Mercury accumulated in human body can not be by certainly
Body metabolism is drained, and be will result directly in heart, liver, thyroid disease, is caused nerve problems, chronic mercury poisoning, even
Cause the formation of malignant tumour.Secondly, the ecological methylate methyl mercury of the microorganism of mercury ion, and it is a kind of strong
Toxin can be transmitted to by food chain in the tissue of fish and marine mammal, and the organic mercury of severe toxicity is converted into.Therefore,
The heavy metal Hg content in the media such as water body in living environment can be quick and precisely analyzed, for improving the life quality of the mankind, protecting
Shield earth environment has a very important significance.
Currently, the method for detection metal mercury ions has very much, as atomic spectroscopy, inductively coupled plasma atom are sent out
Spectrum (ICP-AES methods), spectrophotometry, high performance liquid chromatography are penetrated, inductively coupled plasma mass spectrometry (ICPMS) is changed
Learn luminescence method and fluorescence analysis etc..However, these methods generally require expensive precision instrument, complicated sample preparation flow
And skilled operator, cannot or it is inconvenient be used for quickly detecting outdoors, greatly limit its application.
Ion selective electrode overcomes the deficiency of the above detection method, and not only detection speed is fast, easy to use, for liquid
Body sample need not be pre-processed, and can be with on-line checking, and the potential detection method of ion selective electrode also has choosing
Selecting property is good, high sensitivity, response time are short, easy miniaturization, advantage easy to operate and at low cost；But current mercury ion selection
Property electrode can be further increased in detection speed, sensitivity, accuracy.
Invention content
In order to overcome certain or certain defects of the prior art, the present invention provides a kind of mercury for detecting sewage
The preparation method of ion-selective electrode.
The mercury ion that the present invention provides a kind of for detecting sewage selects the preparation method of electrode, includes the following steps：
(1), silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then mixture is ground it is broken,
Obtain powder；
(2), the powder in step (1) is added in mold, under 10-13MPa pressure, rectangular shape block is made；
(3), the block in step (2) is added in container, nitrogen is full of into container, be heated to 430-450 DEG C, protected
Hold 2h；Then, it anneals naturally, block is ground broken, cylinder is made；Cylinder is heated into 410- under conditions of drying nitrogen
It 430 DEG C, anneals naturally, electrode film is made；
(4), electrode film is mounted on connecting tube bottom end, connecting tube bottom end is sealed with dope, waited after drying to electrode tube
Interior loading potassium nitrate solution；
(5), reference electrode is passed through into cap and fastened, cap is then fastened on electrode tube top, at this moment, reference
Electrode bottom end is extend into sour potassium solution；
(6), conducting wire is connect with reference electrode top.
Preferably, the volume of potassium nitrate solution is 2/3rds of electrode tube and connecting tube volume.
Preferably, in step (1) mixture grinding it is broken after, cross 80 mesh sieve；In step (3) block grinding it is broken after,
It sieves with 100 mesh sieve.
Preferably, the weight ratio in step (1) between silver iodide, silver sulfide and mercuric iodixde is 32:17:7.
Preferably, connecting tube is L-shape, connecting tube one end is connected to electrode tube side, and the connecting tube other end extends downwardly.
Connecting tube and electrode tube integral structure, are integrally formed.
The mercury ion that the present invention provides a kind of for detecting sewage selects the preparation method of electrode, electrode film to use iodate
Silver-colored, silver sulfide and mercuric iodixde mixture can be effectively and precisely by the cooperation of electrode film and potassium nitrate solution, reference electrode
Detect metal mercury ions.The setting of the connecting tube of L shapes enables this mercury ion selection electrode to be effectively placed on container, just
It is measured in the sewage in container.Present invention making is simple, of low cost, easy to use, is better than traditional Instrumental Analysis
Method can be used for the quick detection of micro mercury ion in environment, have in the fields such as environmental monitoring, agricultural food product and biomedicine
There is very important application prospect.
Description of the drawings
Fig. 1 is a kind of structural schematic diagram of mercury ion selection electrode for detecting sewage in embodiment 1.
Specific implementation mode
To further appreciate that present disclosure, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.It should be understood that
, embodiment be only to the present invention explain and and it is non-limiting.
Embodiment 1
The present embodiment additionally provides a kind of preparation method of the mercury ion selection electrode for detecting sewage, including following step
Suddenly：
(1), silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then mixture is ground it is broken,
Obtain powder；
(2), the powder in step (1) is added in mold, under 10MPa pressure, rectangular shape block is made；
(3), the block in step (2) is added in container, nitrogen is full of into container, be heated to 430 DEG C, kept
2h；Then, it anneals naturally, block is ground broken, cylinder is made；Cylinder is heated 410 DEG C under conditions of drying nitrogen,
Naturally it anneals, electrode film is made；
(4), electrode film is mounted on 140 bottom end of connecting tube, 140 bottom end of connecting tube is sealed with dope, waited dry backward
Potassium nitrate solution 160 is packed into electrode tube 110；
(5), reference electrode 120 is passed through into cap 111 and fastened, cap 111, which is then fastened on electrode tube 110, pushes up
End, at this moment, 120 bottom end of reference electrode is extend into sour potassium solution 160；
(6), conducting wire 130 is connect with 120 top of reference electrode.
Wherein,
The volume of potassium nitrate solution 160 is 2/3rds of 140 volume of electrode tube 110 and connecting tube.
In step (1) mixture grinding it is broken after, cross 80 mesh sieve；In step (3) block grinding it is broken after, sieve with 100 mesh sieve.
In the present embodiment, the weight ratio in step (1) between silver iodide, silver sulfide and mercuric iodixde is 32:17:7.
In the present embodiment, connecting tube is L-shape, and connecting tube one end is connected to electrode tube side, and the connecting tube other end is to downward
It stretches.
Embodiment 2
The present embodiment additionally provides a kind of preparation method of the mercury ion selection electrode for detecting sewage, including following step
Suddenly：
(1), silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then mixture is ground it is broken,
Obtain powder；
(2), the powder in step (1) is added in mold, under 12MPa pressure, rectangular shape block is made；
(3), the block in step (2) is added in container, nitrogen is full of into container, be heated to 440 DEG C, kept
2h；Then, it anneals naturally, block is ground broken, cylinder is made；Cylinder is heated 420 DEG C under conditions of drying nitrogen,
Naturally it anneals, electrode film is made；
(4), electrode film is mounted on 140 bottom end of connecting tube, 140 bottom end of connecting tube is sealed with dope, waited dry backward
Potassium nitrate solution 160 is packed into electrode tube 110；
(5), reference electrode 120 is passed through into cap 111 and fastened, cap 111, which is then fastened on electrode tube 110, pushes up
End, at this moment, 120 bottom end of reference electrode is extend into sour potassium solution 160；
(6), conducting wire 130 is connect with 120 top of reference electrode.
Wherein,
The volume of potassium nitrate solution 160 is 2/3rds of 140 volume of electrode tube 110 and connecting tube.
In step (1) mixture grinding it is broken after, cross 80 mesh sieve；In step (3) block grinding it is broken after, sieve with 100 mesh sieve.
In the present embodiment, the weight ratio in step (1) between silver iodide, silver sulfide and mercuric iodixde is 32:17:7.
In the present embodiment, connecting tube is L-shape, and connecting tube one end is connected to electrode tube side, and the connecting tube other end is to downward
It stretches.
Embodiment 3
The present embodiment additionally provides a kind of preparation method of the mercury ion selection electrode for detecting sewage, including following step
Suddenly：
(1), silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then mixture is ground it is broken,
Obtain powder；
(2), the powder in step (1) is added in mold, under 13MPa pressure, rectangular shape block is made；
(3), the block in step (2) is added in container, nitrogen is full of into container, be heated to 450 DEG C, kept
2h；Then, it anneals naturally, block is ground broken, cylinder is made；Cylinder is heated 430 DEG C under conditions of drying nitrogen,
Naturally it anneals, electrode film is made；
(4), electrode film is mounted on 140 bottom end of connecting tube, 140 bottom end of connecting tube is sealed with dope, waited dry backward
Potassium nitrate solution 160 is packed into electrode tube 110；
(5), reference electrode 120 is passed through into cap 111 and fastened, cap 111, which is then fastened on electrode tube 110, pushes up
End, at this moment, 120 bottom end of reference electrode is extend into sour potassium solution 160；
(6), conducting wire 130 is connect with 120 top of reference electrode.
Wherein,
The volume of potassium nitrate solution 160 is 2/3rds of 140 volume of electrode tube 110 and connecting tube.
In step (1) mixture grinding it is broken after, cross 80 mesh sieve；In step (3) block grinding it is broken after, sieve with 100 mesh sieve.
In the present embodiment, the weight ratio in step (1) between silver iodide, silver sulfide and mercuric iodixde is 32:17:7.
In the present embodiment, connecting tube is L-shape, and connecting tube one end is connected to electrode tube side, and the connecting tube other end is to downward
It stretches.
In embodiment 1-3, the conducting wire 130 in electrode is selected to be connect with computer mercury ion obtained, by computer
The potential value that display and statistics measure, first measures a series of potential value of the mercury ion standard solution of known concentrations, with potential value
It works curve to concentration value, then tests the potential value of unknown concentration mercury ion sample solution, sample is found out by working curve
The concentration value or content of mercury ion in product solution.It is found by test experiments, the selection electrode reaches the Monitoring lower-cut of mercury ion
To 7.5 × 10-9mol/L。
The measurement of precision
Take a mercury ion content be 0.05mg/L ground water sample, in embodiment 1-3 mercury ion selection electrode and
Spectrophotometry continuously measures 10 times, and experimental result is as follows：
From the above it can be seen that the mercury ion selection electrode in embodiment 1-3 has preferably stability and accuracy.
Schematically the present invention and embodiments thereof are described above, description is not limiting, institute in attached drawing
What is shown is also one of embodiments of the present invention, and actual structure is not limited to this.So if the common skill of this field
Art personnel are enlightened by it, without departing from the spirit of the invention, are not inventively designed and the technical solution
Similar frame mode and embodiment, are within the scope of protection of the invention.
Claims (5)
1. the preparation method of the mercury ion selection electrode for detecting sewage, it is characterised in that：Include the following steps：
(1), silver iodide, silver sulfide and mercuric iodixde are added in blender and are sufficiently mixed, then grind mixture broken, obtained
Powder；
(2), the powder in step (1) is added in mold, under 10-13MPa pressure, rectangular shape block is made；
(3), the block in step (2) is added in container, nitrogen is full of into container, be heated to 430-450 DEG C, kept
2h；Then, it anneals naturally, block is ground broken, cylinder is made；Cylinder is heated into 410- under conditions of drying nitrogen
It 430 DEG C, anneals naturally, electrode film (150) is made；
(4), electrode film (150) is mounted on connecting tube (140) bottom end, seals connecting tube (140) bottom end with dope, waits dryings
It is packed into potassium nitrate solution (160) in backward electrode tube (110)；
(5), reference electrode (120) is passed through into cap (111) and fastened, cap (111) is then fastened on electrode tube
(110) top, at this moment, reference electrode (120) bottom end are extend into sour potassium solution (160)；
(6), conducting wire (130) is connect with reference electrode (120) top.
2. the preparation method of the mercury ion selection electrode according to claim 1 for detecting sewage, it is characterised in that：Nitre
The volume of sour potassium solution (160) is 2/3rds of electrode tube (110) and connecting tube (140) volume.
3. the preparation method of the mercury ion selection electrode according to claim 2 for detecting sewage, it is characterised in that：Step
Suddenly in (1) mixture grinding it is broken after, cross 80 mesh sieve；In step (3) block grinding it is broken after, sieve with 100 mesh sieve.
4. the preparation method of the mercury ion selection electrode according to claim 3 for detecting sewage, it is characterised in that：Step
Suddenly the weight ratio in (1) between silver iodide, silver sulfide and mercuric iodixde is 32:17:7.
5. the preparation method of the mercury ion selection electrode according to claim 4 for detecting sewage, it is characterised in that：Even
Take over that (140) are L-shape, and connecting tube (140) one end is connected to electrode tube (110) side, connecting tube (140) other end is to downward
It stretches.
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| CN201810033706.6A CN108398473B (en) | 2018-01-15 | 2018-01-15 | Preparation method of mercury ion selective electrode for detecting sewage |
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| CN201810033706.6A CN108398473B (en) | 2018-01-15 | 2018-01-15 | Preparation method of mercury ion selective electrode for detecting sewage |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2045940A (en) * | 1979-04-06 | 1980-11-05 | Searle & Co | Device for measuring ionic concentration |
| JPH09229896A (en) * | 1996-02-27 | 1997-09-05 | Yokogawa Electric Corp | Ion concentration measuring device |
| CN1547004A (en) * | 2003-12-14 | 2004-11-17 | 浙江大学 | Film optical addressing electric potential sensor used for detecting Hg2+ and preparation method thereof |
| CN106908503A (en) * | 2017-03-08 | 2017-06-30 | 东北大学 | A kind of PVC film Ce（Ⅳ）ISE and its preparation method and application |
-
2018
- 2018-01-15 CN CN201810033706.6A patent/CN108398473B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2045940A (en) * | 1979-04-06 | 1980-11-05 | Searle & Co | Device for measuring ionic concentration |
| JPH09229896A (en) * | 1996-02-27 | 1997-09-05 | Yokogawa Electric Corp | Ion concentration measuring device |
| CN1547004A (en) * | 2003-12-14 | 2004-11-17 | 浙江大学 | Film optical addressing electric potential sensor used for detecting Hg2+ and preparation method thereof |
| CN106908503A (en) * | 2017-03-08 | 2017-06-30 | 东北大学 | A kind of PVC film Ce（Ⅳ）ISE and its preparation method and application |
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Application publication date: 20180814 Assignee: Zhejiang Andu E-commerce Co.,Ltd. Assignor: NINGBO College OF HEALTH SCIENCES Contract record no.: X2022980025842 Denomination of invention: Preparation method of mercury ion selective electrode for sewage detection Granted publication date: 20200612 License type: Common License Record date: 20221209 |