CN100422728C - Metal antimony oxide electrode and method for tracking and detecting medium pH change - Google Patents
Metal antimony oxide electrode and method for tracking and detecting medium pH change Download PDFInfo
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- CN100422728C CN100422728C CNB2006100500440A CN200610050044A CN100422728C CN 100422728 C CN100422728 C CN 100422728C CN B2006100500440 A CNB2006100500440 A CN B2006100500440A CN 200610050044 A CN200610050044 A CN 200610050044A CN 100422728 C CN100422728 C CN 100422728C
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Abstract
The present invention relates to a method for tracing and measuring the pH of a culture medium by using an electrode of metal oxide. The working electrode of metallic antimony oxide has the preparation steps: 1, a metallic antimony filament is put in a container, and the surface of the metallic filament is washed so as to remove oxides and impurities on the surface of the metallic antimony filament; 2, the washed metallic antimony filament is dried, and solid potassium nitrate is added until the whole metallic filament is covered with the solid potassium nitrate; 3, the metallic antimony filament is heated to a temperature of 500 DEG C ((+/-)20 DEG C) for 3 hours ((+/-) 1 hour), and the surface of the metallic antimony filament is covered with a dense oxidizing layer; 4, one exposed end of the metallic filament is connected with a conducting wire; and the working electrode of metallic antimony oxide is obtained. The method for tracing and measuring the variation of the pH value of the solid culture medium comprises the following steps: 5, the drawing of a working curve: the working electrode of metallic antimony oxides and a reference electrode capable of being sterilized at a high temperature are respectively soaked in a buffer solution of which the pH value is known, and the electric potential difference between solutions of which the pH values are different is measured so as to draw a working curve of electrical potential and the pH values; 6, the working electrode of metallic antimony oxides and the reference electrode are respectively arranged in an airtight container for high-temperature sterilization; 7, on an ultraclean working table, the working electrode of metallic antimony oxide and the reference electrode are respectively inserted into the culture medium after inoculation; 8, and according to the working curve, the electric potential difference between the two electrodes are measured so as to trace and detect the variation of the pH value of the.
Description
Technical field
The present invention relates to a kind of method of using the electrode tracking and detecting medium pH of burning antimony.
Technical background
Biosome is very responsive to pH.For some was biological, the pH value of its system changed slightly, will cause the death of biosome.Therefore, in the process that biological tissue cultivates, the variation of tracking and detecting medium pH value is very important.
General biology laboratory is all selected the pH test paper for use.But its shortcoming is that error is big, and introduces easily in the measuring process and pollute.If tracking measurement, workload are also very big.
Commercially available glass electrode is a pH measuring method commonly used at present.Yet owing to glass electrode needs to be immersed in the electrode protection liquid at ordinary times, otherwise can influence the life-span, therefore not be suitable for following the tracks of and detect.In addition, because glass electrode can not high-temperature sterilization, and can't use in the agar system, therefore need a kind of new electrode to satisfy the demand.
Metal oxide is done electrode very long history.Yet the problem that exists has stability not enough; Entry material comes off easily and remains in the tested systems; Potential drifting takes place easily; Costing an arm and a leg or the like of some metal.
Summary of the invention
One of the object of the invention provides a kind of metal oxide working electrode that the tracking and detecting medium pH value changes that is suitable for, and two of purpose provides the method that the electrode tracking and detecting medium pH changes.
The metal oxide working electrode that tracking and detecting medium pH value of the present invention changes adopts the preparation of metallic antimony and oxide thereof, and step is as follows:
1. metal antimony wire is placed in the container, uses watery hydrochloric acid respectively, isopropyl alcohol, the oxide and the impurity on metal antimony wire surface are removed in the surface of deionized water clean metal silk under the environment of ultrasonic concussion;
2. the metal antimony wire that will clean is dried at 120 ℃ (± 20 ℃), drying time 24 hours;
3. with treated metal antimony wire, be placed in the crucible, add solid nitric acid potassium, until with the whole covering of tinsel;
4. crucible is put into muffle furnace, be heated to 500 ℃ (± 20 ℃), continue 3 hours (± 1 hour);
5. after the cooling, clean the potassium nitrate solid of removing the metal antimony wire surface;
6. the tinsel that will handle spends the night about 10 hours (± 2 hours) in 120 ℃ (± 20 ℃) oven dry; This moment metal antimony wire surface coverage one deck compact oxide;
7. the end with the metal antimony wire of capping oxidation layer cleans with chloroazotic acid, removes oxide layer, and the tinsel that exposes is linked to each other with lead, and the junction is silica gel protected with what insulate, obtains burning antimony working electrode of the present invention.
The method that the pH value of tracking measurement solid medium changes, step is as follows:
1) drawing curve: respectively burning antimony working electrode and the contrast electrode that can stand high-temperature sterilization are immersed in the buffer solution of known pH value, record the electric potential difference in the solution of different pH values, be depicted as the working curve of electromotive force and pH value;
2) respectively burning antimony working electrode and contrast electrode are contained in the airtight container, and high-temperature sterilization (according to laboratory sterilization standard commonly used, the wet method sterilization, sterilization is 20 minutes under 121 ℃ of temperature);
3) on superclean bench, after the inoculation, burning antimony working electrode and contrast electrode are inserted respectively in the nutrient culture media, working electrode can not contact with contrast electrode, seals mouth, and the joint of two electrodes is drawn with lead;
4) by measuring the electric potential difference of two electrodes, according to working curve, the variation of tracking and detecting medium pH value at any time.
Institute of the present invention responds all indoor, carries out under the atmospheric pressure.
When the present invention cleans, at first use the hydrochloric acid of 1M, use pure isopropyl alcohol then, use deionized water at last.All carry out under the environment of ultrasonic concussion, liquid-immersed tinsel gets final product, and every kind of cleaning fluid cleaned 5-10 minute.
The amount of adding solid nitric acid potassium of the present invention is that the liquid-immersed metal antimony wire of potassium nitrate of fusion gets final product.
The potassium nitrate solid on metal antimony wire surface is removed in cleaning of the present invention, uses washed with de-ionized water, or carries out in the ultrasonic oscillation system with hot water.
Working curve of the present invention is a straight line, R
2Be 0.98.Accurate for what measure, damping fluid is selected nutrient culture media to be measured for use.
Contrast electrode of the present invention can stand high-temperature sterilization, adopts silver/silver chloride electrode.
Metal antimony oxide electrode of the present invention adopts high-temperature sterilization, can use in the agar system, burning antimony price is cheaper, the surface oxide layer densification of metal antimony wire, stability is high, it is simple to have method, easily goes low cost, pollution-free, advantages such as accurate are measured in noresidue, the common laboratory enforcement of all having ready conditions.
Description of drawings
Accompanying drawing 1 Escherichia coli are at the working curve diagram of LB fluid nutrient medium buffer solution electromotive force and pH value
Accompanying drawing 2 tracking and detecting medium pH variation diagrams
Concrete embodiment
Embodiment 1:
● when metal antimony wire cleans, at first use the hydrochloric acid of 1M, use pure isopropyl alcohol then, use deionized water at last.All carry out under the environment of ultrasonic concussion, liquid-immersed tinsel gets final product, and every kind of cleaning fluid cleaned 8 minutes.
● the metal antimony wire that will clean was handled 24 hours 120 ℃ of oven dry;
● with treated metal antimony wire, be placed in the crucible, add solid nitric acid potassium, tinsel is covered fully;
● crucible is put into muffle furnace, be heated to 500 ℃, continue 3 hours;
● after the cooling, clean the potassium nitrate solid of removing the metal antimony wire surface;
● with 120 ℃ of oven dry of tinsel 12 hours, surface coverage one deck compact oxide of metal antimony wire;
● an end of the metal antimony wire of capping oxidation layer is cleaned with chloroazotic acid, remove oxide layer, the tinsel that exposes is linked to each other with lead, the junction is silica gel protected with what insulate, obtains burning antimony working electrode of the present invention.
The method that the pH value of tracking measurement nutrient culture media changes, step is as follows:
● drawing curve: be that contrast electrode is immersed in the Escherichia coli of known pH value in LB fluid nutrient medium buffer solution with burning antimony working electrode and silver/silver chloride electrode respectively, record the electric potential difference in the solution of different pH values, be depicted as the working curve of electromotive force and pH value, referring to accompanying drawing 1 Escherichia coli at LB fluid nutrient medium buffer solution working curve;
● respectively burning antimony working electrode and silver/silver chloride electrode contrast electrode are contained in the airtight container high-temperature sterilization;
● on superclean bench, after the inoculation, burning antimony working electrode and contrast electrode are inserted Escherichia coli respectively in LB fluid nutrient medium nutrient culture media, working electrode can not contact with contrast electrode, seals mouth, and the joint of two electrodes is drawn with lead;
● by measuring the electric potential difference of two electrodes,, measured the pH situation of change of the growth courses of Escherichia coli in the LB fluid nutrient medium according to working curve.The gained result is than the measurement result unanimity of commercially available glass electrode.
Before and after measuring,, find that quality does not change with the weight of rigorous analysis balance weighing working electrode.Illustrate that the material on the electrode does not remain in the system to be measured.
Repeatedly duplicate measurements in 3 months, gained is there was no significant difference as a result.
Embodiment 2:
The preparation of electrode is identical with embodiment 1 with sterilization, and just nutrient culture media is the solid medium that has added 1% agar herein,
On superclean bench, after the inoculation, burning antimony working electrode and contrast electrode are inserted respectively in the MS solid medium nutrient culture media of dendrobium candidum, working electrode can not contact with contrast electrode, seal mouth, the joint of two electrodes is drawn with lead, and the gained result measures consistent with the result of bibliographical information than pH test paper.
Before and after measuring,, find that quality does not change with the weight of rigorous analysis balance weighing working electrode.Even if illustrate that the material on the electrode does not remain in the system to be measured yet in agar solid medium the inside.
, in MS solid medium buffer solution growth course, record the medium pH value with burning antimony working electrode and contrast electrode and change referring to accompanying drawing 2 dendrobium candidums, repeatedly duplicate measurements in 3 months, gained is there was no significant difference as a result.
Claims (7)
1. the burning antimony working electrode preparation method that changes of a tracking and detecting medium pH value, preparation process is as follows:
(1) metal antimony wire is placed in the container, uses watery hydrochloric acid respectively, isopropyl alcohol, the oxide and the impurity on metal antimony wire surface are removed in the surface of deionized water clean metal silk under the environment of ultrasonic concussion;
(2) metal antimony wire that will clean is at 120 ℃ ± 20 ℃ oven dry, drying time 24 hours;
(3) with treated metal antimony wire, be placed in the crucible, add solid nitric acid potassium, until with the whole covering of tinsel
(4) crucible is put into muffle furnace, be heated to 500 ℃ ± 20 ℃, continue 3 hours ± 1 hour;
(5) after the cooling, clean the potassium nitrate solid of removing the metal antimony wire surface;
(6) with 120 ℃ ± 20 ℃ oven dry of tinsel oven dry, drying time 10 hours ± 2 hours, surface coverage one deck compact oxide of metal antimony wire;
(7) end with the metal antimony wire of capping oxidation layer cleans with chloroazotic acid, removes oxide layer, and the tinsel that exposes is linked to each other with lead, and the junction is silica gel protected with what insulate, obtains burning antimony working electrode of the present invention.
2. burning antimony working electrode preparation method according to claim 1 is characterized in that cleaning, and at first uses the hydrochloric acid of 1M, use pure isopropyl alcohol then, use deionized water at last, all under the environment of ultrasonic concussion, carry out, liquid-immersed tinsel gets final product, and every kind of cleaning fluid cleaned 5-10 minute.
3. burning antimony working electrode preparation method according to claim 1, the amount that it is characterized in that solid nitric acid potassium are that the liquid-immersed metal antimony wire of potassium nitrate of fusion gets final product.
4. burning antimony working electrode preparation method according to claim 1 is characterized in that cleaning the potassium nitrate solid of removing the metal antimony wire surface, uses washed with de-ionized water, or carries out in the ultrasonic oscillation system with hot water.
5. the method that changes of the described burning antimony of claim 1 working electrode tracking and detecting medium pH value, step is as follows:
1) drawing curve: be that contrast electrode is immersed in the buffer solution of known pH value with burning antimony working electrode with the silver/silver chloride electrode that can stand high-temperature sterilization respectively, record the electric potential difference in the solution of different pH values, be depicted as the working curve of electromotive force and pH value;
2) respectively burning antimony working electrode and contrast electrode are contained in high-temperature sterilization in the airtight container;
3) on superclean bench, after the inoculation, burning antimony working electrode and contrast electrode are inserted respectively in the nutrient culture media, working electrode can not contact with contrast electrode, seals mouth, and the joint of two electrodes is drawn with lead;
4) by measuring the electric potential difference of two electrodes, according to working curve, the variation of tracking and detecting medium pH value at any time.
6. the method that burning antimony working electrode tracking and detecting medium pH value according to claim 5 changes is characterized in that buffer solution selects nutrient culture media to be measured for use.
7. the method that burning antimony working electrode tracking and detecting medium pH value according to claim 5 changes is characterized in that high-temperature sterilization in the airtight container, adopts the wet method sterilization, and sterilization is 20 minutes under 121 ℃ of temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100500440A CN100422728C (en) | 2006-03-28 | 2006-03-28 | Metal antimony oxide electrode and method for tracking and detecting medium pH change |
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| CNB2006100500440A CN100422728C (en) | 2006-03-28 | 2006-03-28 | Metal antimony oxide electrode and method for tracking and detecting medium pH change |
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| CN1821770A CN1821770A (en) | 2006-08-23 |
| CN100422728C true CN100422728C (en) | 2008-10-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102565164B (en) * | 2012-02-01 | 2014-03-12 | 江苏大学 | Method for producing antimony pH electrode modified by two layers of films |
| CN109030587B (en) * | 2015-05-29 | 2021-04-20 | 天津大学 | Application of antimony-lead anodic oxidation composite reference electrode in high-concentration sulfuric acid system |
| CN107202823B (en) * | 2017-06-20 | 2019-10-29 | 龚雨 | A kind of ink jet printing prepares the method and its application of microelectrode array sensor |
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| US4561963A (en) * | 1984-07-30 | 1985-12-31 | Zinetics Medical Technology Corporation | Antimony and graphite hydrogen ion electrode and method of making such electrode |
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2006
- 2006-03-28 CN CNB2006100500440A patent/CN100422728C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4561963A (en) * | 1984-07-30 | 1985-12-31 | Zinetics Medical Technology Corporation | Antimony and graphite hydrogen ion electrode and method of making such electrode |
| EP0471330A1 (en) * | 1990-08-15 | 1992-02-19 | Degussa Ag | PH-measuring device |
| CN2100627U (en) * | 1991-02-22 | 1992-04-01 | 邢志东 | Palladium ph electrode |
| CN2143332Y (en) * | 1991-09-10 | 1993-10-06 | 钦州市技术监督局 | Non-scale stibium electrode |
| CN1064175A (en) * | 1992-01-08 | 1992-09-02 | 南开大学 | Magnesium-base hydrogenous alloy electrode |
| CN1098503A (en) * | 1993-07-31 | 1995-02-08 | 福建星光造纸集团公司 | A kind of application of modified acidometer |
| CN1595133A (en) * | 2004-06-29 | 2005-03-16 | 西安理工大学 | Process for making puncture composite sensor for measuring pH and sensor therefor |
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| 超细氧化锑阻燃剂的研究进展. 李宾杰，吴志申，周静芳.塑料工业，第31卷第9期. 2003 * |
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