CN102062753A - Phosphate ion carbon paste electrode and preparation method thereof - Google Patents
Phosphate ion carbon paste electrode and preparation method thereof Download PDFInfo
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- CN102062753A CN102062753A CN2010105787091A CN201010578709A CN102062753A CN 102062753 A CN102062753 A CN 102062753A CN 2010105787091 A CN2010105787091 A CN 2010105787091A CN 201010578709 A CN201010578709 A CN 201010578709A CN 102062753 A CN102062753 A CN 102062753A
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Abstract
本发明涉及一种磷酸根离子碳糊电极及其制备方法，所述方法包括以下步骤：（1）称取石墨粉、羟基磷灰石和液体石蜡；（2）将研钵和碾锤用去离子水清洗干净，烘干；（3）将石墨粉、羟基磷灰石和液体石蜡在研钵中，用碾锤进行研磨，得到化学修饰碳糊；（4）将化学修饰碳糊填入玻璃管或四氟乙烯管中；（5）将化学修饰碳糊压实；（6）将金属导线从填有化学修饰碳糊的玻璃管或者四氟乙烯管的上端插入；（7）在称量纸上打磨玻璃管或四氟乙烯管下端的化学修饰碳糊的表面；（8）将得到的碳糊电极浸入磷酸二氢钾溶液中活化，即得到磷酸根离子碳糊电极。本发明所述的磷酸根碳糊电极的响应时间短，一般小于60s，体积小，成本低，制作简单。
The invention relates to a phosphate ion carbon paste electrode and a preparation method thereof. The method comprises the following steps: (1) weighing graphite powder, hydroxyapatite and liquid paraffin; Clean with ionic water and dry; (3) Grind graphite powder, hydroxyapatite and liquid paraffin in a mortar with a hammer to obtain a chemically modified carbon paste; (4) Fill the chemically modified carbon paste into the glass (5) compact the chemically modified carbon paste; (6) insert the metal wire from the upper end of the glass tube or tetrafluoroethylene tube filled with chemically modified carbon paste; (7) weigh Grinding the surface of the chemically modified carbon paste at the lower end of the glass tube or tetrafluoroethylene tube on paper; (8) immersing the obtained carbon paste electrode in potassium dihydrogen phosphate solution for activation to obtain a phosphate ion carbon paste electrode. The phosphate carbon paste electrode of the present invention has short response time, generally less than 60s, small volume, low cost and simple manufacture.
Description
Technical field
The present invention relates to a kind of phosphate anion carbon paste electrode, especially a kind of phosphate anion carbon paste electrode and preparation method thereof belongs to chemical analysis and related sensor field.
Background technology
P elements is one of indispensable element of nature biotechnology growth, and it is present in occurring in nature widely with various forms.Yet, in case the total phosphorus content in the ambient water quality exceeds standard, very likely cause the eutrophication of water body, cause water quality deterioration, and then threaten existent environment of people.Therefore, total phosphorus content is detected as for important techniques index in the environmental water quality monitoring.
Ion-selective electrode has that response speed is fast, simple to operation, antijamming capability is strong and advantage such as cost of manufacture is low, is applicable to the continuous monitoring and the on-the site analysis of ambient water quality.So phosphoric acid radical ion-selective electrode becomes research focus in the last few years, and can be with it as one of the testing tool of total phosphorus content in the ambient water quality.
Chemically modified carbon paste electrode is one of way of realization of ion-selective electrode.It is the pastel that utilizes electric conductivity dag, chemical modifier and hydrophobic nature bonding agent to be mixed and made into, and it is coated in electrode bar surface or is packed in the glass tube and a class electrode of making.Its bonding agent is divided into two big classes: first nonconductor bonding agent, another kind are the electrolyte solution bonding agents.Chemically modified carbon paste electrode is made simple, favorable reproducibility, surface advantage such as renewal and enjoy favor easily with it.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of volume little, cost is low, makes simple phosphate anion carbon paste electrode and preparation method thereof.
According to technical scheme provided by the invention, in glass tube or tetrafluoroethene pipe, fill carbon magma, in carbon magma, insert plain conductor; Described plain conductor is drawn by the upper end of glass tube or tetrafluoroethene pipe, and the lower surface of described glass tube or tetrafluoroethene pipe is filled by carbon magma, and it is smooth to polish flat.
The internal diameter of described glass tube or tetrafluoroethene pipe is 2 ~ 5mm.
Described plain conductor is a copper conductor.
A kind of preparation method of phosphate anion carbon paste electrode may further comprise the steps:
(1) takes by weighing dag, hydroxyapatite and whiteruss by weight 1 ~ 3:1 ~ 3:1 ~ 2;
(2) abradant mortar and stone roller hammer are cleaned up with deionized water, and put into oven for drying;
(3) dag, hydroxyapatite and whiteruss are put into mortar, the medication spoon stirs, and grinds 72 ~ 96 hours with grinding hammer, and dag, hydroxyapatite and whiteruss are fully mixed, and obtains carbon magma;
(4) carbon magma is inserted in glass tube or the tetrafluoroethene pipe, during filling, carbon magma is inserted from the upper end of glass tube or tetrafluoroethene pipe, and the lower end of glass tube or tetrafluoroethene pipe is blocked with a shelter, in order to avoid carbon magma drops in managing;
(5) will insert the interior carbon magma compacting of pipe with a diameter less than the cylindrical metal rod of glass tube or tetrafluoroethene bore, the inner consolidation of the carbon magma in guaranteeing to manage is difficult for coming off in managing;
(6) plain conductor is inserted from the upper end of the glass tube that is filled with carbon magma or tetrafluoroethene pipe, in lead is nuzzled carbon paste, fix plain conductor then, from carbon paste in order to avoid metal skids off;
(7) shelter of glass tube or tetrafluoroethene pipe lower end is removed, smooth on the surface of the carbon magma that is tiled in polish on the pan paper of desktop glass tube or tetrafluoroethene pipe lower end until the smooth surface of carbon magma, promptly obtain carbon paste electrode;
(8) carbon paste electrode that obtains is immersed in the potassium dihydrogen phosphate that concentration is 0.001 ~ 0.1 mol/L activate 12 ~ 20 hours, promptly obtain can be used for testing the phosphate anion carbon paste electrode of phosphate anion.
The response time of phosphate radical carbon paste electrode of the present invention is short, is generally less than 60s, and volume is little, and cost is low, makes simple.
Description of drawings
Fig. 1 is the structural representation of carbon paste electrode of the present invention.
Fig. 2 is the electrode performance canonical plotting of carbon paste electrode of the present invention.
Embodiment
The invention will be further described below in conjunction with concrete drawings and Examples.
As shown in Figure 1: phosphate anion carbon paste electrode of the present invention, in glass tube or tetrafluoroethene pipe 2, fill carbon magma 1, in carbon magma 1, insert plain conductor 3; Described plain conductor 3 is drawn by the upper end of glass tube or tetrafluoroethene pipe 2, and the lower surface of described glass tube or tetrafluoroethene pipe 2 is filled by carbon magma 1, and it is smooth to polish flat.
The dag that dag used in the present invention can adopt the safe lubrication and seal science and technology limited Company of Qingdao China to produce;
The nanometer carboxylic apatite that hydroxyapatite used in the present invention can adopt Nanjing Ai Purui nano material company limited to produce;
The whiteruss that whiteruss used in the present invention can adopt the Henan sharp chemical industry of perseverance company limited to produce.
Embodiment one: a kind of preparation method of phosphate anion carbon paste electrode may further comprise the steps:
(1) takes by weighing the dag of 30mg, the hydroxyapatite of 30mg and the whiteruss of 12mL respectively;
(2), and put into 80 ℃ baking oven and dry with abradant mortar with grind hammer and clean up with deionized water;
(3) dag, hydroxyapatite and whiteruss are put into mortar, the medication spoon stirs, and grinds 72 hours with grinding hammer, and dag, hydroxyapatite and whiteruss are fully mixed, and obtains carbon magma;
(4) carbon magma is inserted in glass tube or the tetrafluoroethene pipe, during filling, carbon magma is inserted from the upper end of glass tube or tetrafluoroethene pipe, and the lower end of glass tube or tetrafluoroethene pipe is blocked with a shelter, in order to avoid carbon magma drops in managing;
(5) will insert the interior carbon magma compacting of pipe with a diameter less than the cylindrical metal rod of glass tube or tetrafluoroethene bore, the inner consolidation of the carbon magma in guaranteeing to manage is difficult for coming off in managing;
(6) plain conductor is inserted from the upper end of the glass tube that is filled with carbon magma or tetrafluoroethene pipe, in lead is nuzzled carbon paste, fix plain conductor then, from carbon paste in order to avoid metal skids off;
(7) shelter of glass tube or tetrafluoroethene pipe lower end is removed, smooth on the surface of the carbon magma that is tiled in polish on the pan paper of desktop glass tube or tetrafluoroethene pipe lower end until the smooth surface of carbon magma, promptly obtain carbon paste electrode;
(8) carbon paste electrode that obtains is immersed in the potassium dihydrogen phosphate that concentration is 0.001mol/L activation 12 hours, promptly obtain can be used for testing the phosphate anion carbon paste electrode of phosphate anion.
Detection method: the three-electrode system that adopts electrochemical workstation, with silver chloride electrode as contrast electrode, platinum electrode is to electrode, the resulting chemically modified carbon paste electrode of the present invention is a working electrode, test solution is the potassium dihydrogen phosphate of a series of concentration, can obtain corresponding response voltage value after the test, and with concentration-log has tangible linear relationship, slope is stable simultaneously, is approximately 19mV/decade.
Calibration curve method is adopted in the test of described phosphate anion carbon paste electrode, with analyzing the test solution that pure level potassium dihydrogen phosphate is configured to a series of variable concentrations respectively.Test macro uses the three-electrode system of electrochemical workstation, and wherein contrast electrode is a silver chloride electrode, is platinum electrode to electrode, and working electrode is the electrode that foregoing invention is made.The current potential of difference test electrode in the potassium dihydrogen phosphate of a series of variable concentrations is in order to estimate the performance of this novel phosphoric acid radical ion-selective electrode.As shown in Figure 2, the linear response concentration range of this electrode is 10
-1~ 10
-4Mol/L, promptly this electrode can measure 10
-1~ 10
-4The ion concentration value of phosphate radical in the mol/L concentration range, and magnitude of voltage and solution concentration value-log is linear, and its slope is 19 mV/decade, and phosphate anion detects down and is limited to 10
-4Mol/L.
Embodiment two: a kind of preparation method of phosphate anion carbon paste electrode may further comprise the steps:
(1) takes by weighing the dag of 10mg, the hydroxyapatite of 10mg and the whiteruss of 22mL respectively;
(2) abradant mortar and stone roller hammer are cleaned up with deionized water, and put into oven for drying;
(3) dag, hydroxyapatite and whiteruss are put into mortar, the medication spoon stirs, and grinds 96 hours with grinding hammer, and dag, hydroxyapatite and whiteruss are fully mixed, and obtains carbon magma;
(4) carbon magma is inserted in glass tube or the tetrafluoroethene pipe, during filling, carbon magma is inserted from the upper end of glass tube or tetrafluoroethene pipe, and the lower end of glass tube or tetrafluoroethene pipe is blocked with a shelter, in order to avoid carbon magma drops in managing;
(5) will insert the interior carbon magma compacting of pipe with a diameter less than the cylindrical metal rod of glass tube or tetrafluoroethene bore, the inner consolidation of the carbon magma in guaranteeing to manage is difficult for coming off in managing;
(6) plain conductor is inserted from the upper end of the glass tube that is filled with carbon magma or tetrafluoroethene pipe, in lead is nuzzled carbon paste, fix plain conductor then, from carbon paste in order to avoid metal skids off;
(7) shelter of glass tube or tetrafluoroethene pipe lower end is removed, smooth on the surface of the carbon magma that is tiled in polish on the pan paper of desktop glass tube or tetrafluoroethene pipe lower end until the smooth surface of carbon magma, promptly obtain carbon paste electrode;
(8) carbon paste electrode that obtains is immersed in the potassium dihydrogen phosphate that concentration is 0.1 mol/L activation 20 hours, promptly obtain can be used for testing the phosphate anion carbon paste electrode of phosphate anion.
Embodiment three: a kind of preparation method of phosphate anion carbon paste electrode may further comprise the steps:
(1) takes by weighing the dag of 15mg, the hydroxyapatite of 15mg and the whiteruss of 17mL respectively;
(2) abradant mortar and stone roller hammer are cleaned up with deionized water, and put into oven for drying;
(3) dag, hydroxyapatite and whiteruss are put into mortar, the medication spoon stirs, and grinds 80 hours with grinding hammer, and dag, hydroxyapatite and whiteruss are fully mixed, and obtains carbon magma;
(4) carbon magma is inserted in glass tube or the tetrafluoroethene pipe, during filling, carbon magma is inserted from the upper end of glass tube or tetrafluoroethene pipe, and the lower end of glass tube or tetrafluoroethene pipe is blocked with a shelter, in order to avoid carbon magma drops in managing;
(5) will insert the interior carbon magma compacting of pipe with a diameter less than the cylindrical metal rod of glass tube or tetrafluoroethene bore, the inner consolidation of the carbon magma in guaranteeing to manage is difficult for coming off in managing;
(6) plain conductor is inserted from the upper end of the glass tube that is filled with carbon magma or tetrafluoroethene pipe, in lead is nuzzled carbon paste, fix plain conductor then, from carbon paste in order to avoid metal skids off;
(7) shelter of glass tube or tetrafluoroethene pipe lower end is removed, smooth on the surface of the carbon magma that is tiled in polish on the pan paper of desktop glass tube or tetrafluoroethene pipe lower end until the smooth surface of carbon magma, promptly obtain carbon paste electrode;
(8) carbon paste electrode that obtains is immersed in the potassium dihydrogen phosphate that concentration is 0.005mol/L activation 16 hours, promptly obtain can be used for testing the phosphate anion carbon paste electrode of phosphate anion.
Claims (4)
1. a phosphate anion carbon paste electrode is characterized in that, fills carbon magma (1) in glass tube or tetrafluoroethene pipe (2), inserts plain conductor (3) in carbon magma (1); Described plain conductor (3) is drawn by the upper end of glass tube or tetrafluoroethene pipe (2), and the lower surface of described glass tube or tetrafluoroethene pipe (2) is filled by carbon magma (1), and it is smooth to polish flat.
2. phosphate anion carbon paste electrode as claimed in claim 1 is characterized in that, the internal diameter of described glass tube or tetrafluoroethene pipe is 2 ~ 5mm.
3. phosphate anion carbon paste electrode as claimed in claim 1 is characterized in that, described plain conductor is a copper conductor.
4. the preparation method of a phosphate anion carbon paste electrode as claimed in claim 1 is characterized in that, comprises following processing step:
(1) takes by weighing dag, hydroxyapatite and whiteruss by weight 1 ~ 3:1 ~ 3:1 ~ 2;
(2) abradant mortar and stone roller hammer are cleaned up with deionized water, and put into oven for drying;
(3) dag, hydroxyapatite and whiteruss are put into mortar, the medication spoon stirs, and grinds 72 ~ 96 hours with grinding hammer, and dag, hydroxyapatite and whiteruss are fully mixed, and obtains carbon magma;
(4) carbon magma is inserted in glass tube or the tetrafluoroethene pipe, during filling, carbon magma is inserted from the upper end of glass tube or tetrafluoroethene pipe, and the lower end of glass tube or tetrafluoroethene pipe is blocked with a shelter, in order to avoid carbon magma drops in managing;
(5) will insert the interior carbon magma compacting of pipe with a diameter less than the cylindrical metal rod of glass tube or tetrafluoroethene bore, the inner consolidation of the carbon magma in guaranteeing to manage is difficult for coming off in managing;
(6) plain conductor is inserted from the upper end of the glass tube that is filled with carbon magma or tetrafluoroethene pipe, in lead is nuzzled carbon paste, fix plain conductor then, from carbon paste in order to avoid metal skids off;
(7) shelter of glass tube or tetrafluoroethene pipe lower end is removed, smooth on the surface of the carbon magma that is tiled in polish on the pan paper of desktop glass tube or tetrafluoroethene pipe lower end until the smooth surface of carbon magma, promptly obtain carbon paste electrode;
(8) carbon paste electrode that obtains is immersed in the potassium dihydrogen phosphate that concentration is 0.001 ~ 0.1mol/L activate 12 ~ 20 hours, promptly obtain can be used for testing the phosphate anion carbon paste electrode of phosphate anion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253095A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院长春应用化学研究所 | Carbon paste electrode and preparation method thereof |
| CN106483177A (en) * | 2016-11-08 | 2017-03-08 | 哈尔滨师范大学 | A kind of preparation method of graphene oxide/EDTA decorating carbon paste electrode |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060160100A1 (en) * | 2005-01-19 | 2006-07-20 | Agency For Science, Technology And Research | Enzymatic electrochemical detection assay using protective monolayer and device therefor |
| CN101074941A (en) * | 2007-06-21 | 2007-11-21 | 中国科学院长春应用化学研究所 | Method for producing carbon magma bismuth membrane electrode |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060160100A1 (en) * | 2005-01-19 | 2006-07-20 | Agency For Science, Technology And Research | Enzymatic electrochemical detection assay using protective monolayer and device therefor |
| CN101074941A (en) * | 2007-06-21 | 2007-11-21 | 中国科学院长春应用化学研究所 | Method for producing carbon magma bismuth membrane electrode |
Non-Patent Citations (2)
| Title |
|---|
| GIOVANNI C. PETRUCELLI等: "Hydroxyapatite-based Electrode: A New Sensor for Phosphate", 《ANALYTICAL COMMUNICATIONS》, vol. 33, 31 July 1996 (1996-07-31), pages 227 - 229 * |
| 蔡晓华: "分析化学中的化学修饰碳糊电极", 《海南大学学报自然科学版》, vol. 11, no. 4, 31 December 1993 (1993-12-31), pages 63 - 69 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253095A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院长春应用化学研究所 | Carbon paste electrode and preparation method thereof |
| CN106483177A (en) * | 2016-11-08 | 2017-03-08 | 哈尔滨师范大学 | A kind of preparation method of graphene oxide/EDTA decorating carbon paste electrode |
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