CN104090009A - Preparation method of electrochemical sensor based on graphene nano sheet modified electrode - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 21
- 239000002135 nanosheet Substances 0.000 title abstract 2
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000009514 concussion Effects 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 10
- 230000035945 sensitivity Effects 0.000 abstract description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000001514 detection method Methods 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- -1 Metal oxide di-iron trioxide Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 208000002330 Congenital Heart Defects Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000143432 Daldinia concentrica Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 208000028831 congenital heart disease Diseases 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 208000005135 methemoglobinemia Diseases 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 201000000498 stomach carcinoma Diseases 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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Abstract
The invention relates to an electrochemical sensor based on a ferric oxide nanoparticle-modified reduced graphene oxide nano sheet (Fe2O3/ rGO), which is used for detecting nitrite. A preparation method of the electrochemical sensor comprises the following steps of firstly, preparing a Fe2O3/ rGO compound by an environment-friendly method, and then modifying a glassy carbon electrode by the Fe2O3/ rGO compound, thus preparing the electrochemical sensor for detecting nitrite. When being used for detecting nitrite, the electrochemical sensor is high in sensitivity, stability, repeatability and selectivity, thus having wide application prospect in the fields such as environment and food.
Description
Technical field
The present invention relates to a kind of preparation method of electrochemical sensor, relate in particular to a kind of preparation method of the electrochemical sensor based on the nano-particle modified redox graphene nanometer sheet of di-iron trioxide modified electrode.
Background technology
The use of formulation fertilizer containing nitrogen and the discharge of industrial waste water have caused the mankind can use the pollution of surface water, its nitrite is all toxic to environment and human health, nitrite contacts with amine and forms nitrosamine, can cause as various diseases such as methemoglobinemia, congenital heart defects and cancer of the stomach.The World Health Organization (WHO) stipulates that the high-load of mankind's drinkable water nitrite is 3mg/L, and therefore, for publilc health, environment and food industry, the high-sensitivity detection of nitrite is very important.
Up to the present the method that detects nitrite mainly contains spectrophotometric spectra method, chemiluminescence, electrocapillary phoresis method and chromatography, and these methods need expensive equipment conventionally, complicated trace routine and normally very consuming time.
With these methods, compare, electrochemical method provides a kind of simple, instant analysis method that relative price is cheap, reliable, sensitive, can realize a kind of nitrite detection method that sample is carried out pre-treatment and not disturbed by other material of fast, not needing.
Carbon nanomaterial (fullerene, carbon nano-tube and Graphene) has been widely used in galvanochemistry, these materials have a lot of significant advantages, as little residual current, wide electromotive force mouth, the easy reproducibility of good chemical stability and surface in different electrolyte.Graphene (a kind of desirable two-dimensional layer material) is because its unique physics and chemistry performance has been widely used for fixing metal oxide nano particle, sensor based on copper ingotism and redox graphene (rGO) has shown electro catalytic activity in the detection of nitrite, and graphene nanometer sheet and Nano carbon balls have also shown the electro catalytic activity to nitrite at electrode surface.
Metal oxide di-iron trioxide (Fe
2o
3) be a kind of narrow important N-shaped metal oxide that can band (Eg=2.2eV), in recent years, caused the very large concern of people because its at a low price, nontoxic, easily preparation and the feature that easily stores, Fe
2o
3in catalysis, food, magnetic material, gas sensor, biology sensor and lithium ion battery field, there are a lot of application.
In sum, metal oxide/graphene film compound is applied to electrochemical method, is for detection of nitrite the most reliable the sensitiveest method in prior art.The preparation method of metal oxide/graphene film compound mainly contains pyrolytic, forged burning, electronation, the synthetic harmony chemical synthesis process of microwave, and these methods generally comprise two steps, and the reduction of the graphene film of toxicity hydrazine induction is burnt and added to forged.These methods clearly energy consumption are conventionally all very high, and need to use complex experiment instrument and technology, and can cause certain pollution to environment.
Summary of the invention
For the shortcoming of prior art, the present invention prepared a kind of simple, for nitrite, detect, based on the nano-particle modified redox graphene nanometer sheet of di-iron trioxide (Fe
2o
3/ rGO) the high sensitivity electrochemical sensor of modified electrode.Fe
2o
3/ rGO compound synthesizes by one step hydro thermal method in ethanol, and electrochemical sensor involved in the present invention has demonstrated good sensitivity, selectivity and repeatability.
Step of the present invention is as follows:
(1) preparation of graphene oxide: powdered graphite joins in the concentrated sulphuric acid under 0 ℃ of condition, under ice-water bath stirring condition, add potassium permanganate composition mixture, the mass ratio of powdered graphite and potassium permanganate is 1:6～1:10, preferred 1:8, mass volume ratio (the w/v of powdered graphite and the concentrated sulphuric acid, g/mL) be 1:40～1:50, preferably 1:45.Said mixture stirs after 2～3h at 60～80 ℃, dilute with water at 50 ℃.Last 30% the hydrogen peroxide of dropwise adding, the hydrochloric acid solution with the above 1:10 of 100mL after being filtered washs, then washes until the pH of solution reaches 6.3 grind into powder after 55～80 ℃ of vacuum drying 12～20h of yellow solid that obtain with water.
(2) Fe
2o
3the preparation of/rGO compound: 20～40mg graphene oxide is distributed to the solution of ultrasonic concussion 50～120min formation homogeneous in 80～120mL ethanol, adds FeCl
2with 25% ammoniacal liquor in above-mentioned solution, FeCl
2with 25% ammoniacal liquor be (g/mL/mL): 1:1:1000 with the ratio of above-mentioned solution, the potpourri obtaining in muffle furnace 90～110 ℃ add then cool to room temperature gradually of thermal response 5～8h; After sediment leaches, with deionized water and ethanol, wash 7～10 times, then vacuum drying 7～12h under 50～70 ℃ of conditions.
(3) Fe
2o
3the preparation of/rGO compound modified electrode: the aluminum oxide suspension for surface of glassy carbon electrode (0.6～0.9 μ mol/L) carries out physics polishing, then electrode is successively used to second alcohol and water supersound washing 3～8min, gets 10 μ L Fe
2o
3/ rGO compound, is distributed in water, and concentration is 0.5mg/mL, and the surperficial final vacuum that drips to glassy carbon electrode is dry, can obtain Fe
2o
3/ rGO compound modified electrode.
First the present invention has prepared Fe by eco-friendly method
2o
3/ rGO compound, then uses Fe
2o
3/ rGO compound carries out modification to glassy carbon electrode and has prepared a kind of novel electrochemical sensor detecting for nitrite.Fe
2o
3/ rGO modified electrode can provide high specific surface area, thereby the medium shifting as electronics improves the charge transfer between electrode surface and nitrite.Electrochemical sensor involved in the present invention has presented high sensitivity, stability, repeatability and selectivity to the detection of nitrite, can be widely used in the fields such as environment, food.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with implementing, the invention will be further described.
The preparation method of the high sensitivity electrochemical sensor detecting for nitrite based on the nano-particle modified redox graphene nanometer sheet of di-iron trioxide, its step is as follows:
(1) preparation of graphene oxide: 4g powdered graphite joins in the 180mL concentrated sulphuric acid under 0 ℃ of condition, under ice-water bath stirring condition, add 32g potassium permanganate composition mixture, after stirring 3h at 75 ℃, dilutes with 800mL water at 50 ℃ in potpourri, the last hydrogen peroxide that dropwise adds 50mL30%, hydrochloric acid solution with 100mL1:10 after being filtered washs, wash again until the pH of solution reaches 6.3 grind into powder after the 60 ℃ of vacuum drying 15h of yellow solid that obtain with water.
(2) Fe
2o
3the preparation of/rGO compound: 40mg graphene oxide is distributed to the solution of ultrasonic concussion 50min formation homogeneous in 200mL ethanol, 0.2gFeCl
2join in above-mentioned solution with the ammoniacal liquor of 200 μ L20%, the potpourri obtaining in muffle furnace 90 ℃ add after thermal response 5h, cool to room temperature gradually, after sediment leaches, with deionized water and ethanol washing 7 times, then vacuum drying 8h under 70 ℃ of conditions.
(3) Fe
2o
3the preparation of/rGO compound modified electrode: first physics polishing is carried out with the aluminum oxide suspension of 0.8 μ mol/L in the surface of glassy carbon electrode, then electrode is successively used to second alcohol and water supersound washing 3min; 10 μ LFe
2o
3(be distributed in water, the surperficial final vacuum that 0.5mg/mL) drips to glassy carbon electrode is dry, can obtain Fe for/rGO compound
2o
3/ rGO compound modified electrode.
Claims (6)
1. a preparation method for the electrochemical sensor based on graphene nanometer sheet modified electrode, its step is as follows:
(1) preparation of graphene oxide: powdered graphite joins in the concentrated sulphuric acid under 0 ℃ of condition, under ice-water bath stirring condition, add potassium permanganate to form potpourri, the mass ratio of powdered graphite and potassium permanganate is 1:6～1:10, mass volume ratio (the w/v of powdered graphite and the concentrated sulphuric acid, g/mL) be 1:40～1:50, said mixture stirs then dilute with water at 50 ℃ of 2～3h at 60～80 ℃, dropwise add 30% hydrogen peroxide, hydrochloric acid solution with the above 1:10 of 100mL after being filtered washs, wash with water again until the pH of solution reaches 6.3, grind into powder after 55～80 ℃ of vacuum drying 12～20h of yellow solid that obtain,
(2) Fe
2o
3the preparation of/rGO compound: 20～40mg graphene oxide is distributed to the solution of ultrasonic concussion 50～120min formation stable homogeneous in 80～120mL ethanol, adds FeCl
2with 25% ammoniacal liquor in above-mentioned solution, FeCl
2with 25% ammoniacal liquor be (g/mL/mL): 1:1:1000 with the ratio of above-mentioned solution, the potpourri obtaining in muffle furnace 90～110 ℃ add thermal response 5～8h cool to room temperature gradually, sediment leaches rear deionized water and the ethanol used and washs 7～10 times, then vacuum drying 7～12h under 50～70 ℃ of conditions;
(3) Fe
2o
3the preparation of/rGO compound modified electrode: the aluminum oxide suspension for surface of glassy carbon electrode (0.6～0.9 μ mol/L) carries out physics polishing, then electrode is successively used to second alcohol and water supersound washing 3～8min, gets 10 μ L Fe
2o
3/ rGO compound, is distributed in water, is mixed with the solution that concentration is 0.5mg/mL, and the surperficial final vacuum that drips to glassy carbon electrode is dry, can obtain Fe
2o
3/ rGO compound modified electrode.
2. the preparation method of electrochemical sensor according to claim 1, is characterized in that: described in step (1), the mass ratio of powdered graphite and potassium permanganate is 1:8.
3. the preparation method of electrochemical sensor according to claim 1, is characterized in that: described in step (1), the mass volume ratio (w/v, g/mL) of powdered graphite and the concentrated sulphuric acid is 1:45.
4. the preparation method of electrochemical sensor according to claim 1, is characterized in that: grind into powder after 60 ℃ of vacuum drying 15h of yellow solid described in step (1).
5. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the amount of the described graphene oxide of step (2) and ethanol is respectively 40mg and 200mL, and the time of described ultrasonic concussion is 50min.
6. the preparation method of electrochemical sensor according to claim 1, is characterized in that: the concentration of the described aluminum oxide suspension of step (3) is: 0.8 μ mol/L.
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| CN201410368085.9A CN104090009B (en) | 2014-07-29 | 2014-07-29 | The preparation method of a kind of electrochemical sensor based on graphene nanometer sheet modified electrode |
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| CN104090009B CN104090009B (en) | 2016-06-01 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104634848A (en) * | 2015-01-25 | 2015-05-20 | 浙江大学 | Nitrite electrochemical sensor and manufacturing method thereof |
| CN105136886A (en) * | 2015-10-14 | 2015-12-09 | 无锡百灵传感技术有限公司 | Electrode for detecting Sudan red rapidly and quantitatively |
| CN105911120A (en) * | 2016-04-13 | 2016-08-31 | 中国科学院过程工程研究所 | Sulfur-doped graphene oxide modified glassy carbon electrode, preparation method and detection method for heavy metals in water |
| CN106910902A (en) * | 2017-01-22 | 2017-06-30 | 济南大学 | A kind of fuel cell oxygen reduction catalyst and preparation method thereof |
| CN110609069A (en) * | 2019-10-16 | 2019-12-24 | 常州大学 | Preparation of a CuNi/reduced graphene non-enzymatic sulfite electrochemical sensor |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102507693A (en) * | 2011-11-03 | 2012-06-20 | 桂林医学院 | Functional-material-based glucose biosensor and manufacturing method thereof |
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2014
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| CN102507693A (en) * | 2011-11-03 | 2012-06-20 | 桂林医学院 | Functional-material-based glucose biosensor and manufacturing method thereof |
Non-Patent Citations (4)
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| NAGAPPA L.TERADAL等: "Electro-reduced graphene oxide film modified glassy carbon electrode as an electrochemical sensor for sibutramine", 《ANALYTICAL METHODS》 * |
| SONG BAI等: "Nanocomposites of hematite (a-Fe2O3) nanospindles with crumpled reduced graphene oxide nanosheets as high-performance anode material for lithiumion batteries", 《RSC ADV.》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104634848A (en) * | 2015-01-25 | 2015-05-20 | 浙江大学 | Nitrite electrochemical sensor and manufacturing method thereof |
| CN105136886A (en) * | 2015-10-14 | 2015-12-09 | 无锡百灵传感技术有限公司 | Electrode for detecting Sudan red rapidly and quantitatively |
| CN105136886B (en) * | 2015-10-14 | 2018-05-01 | 广州智谱慧科技有限公司 | A kind of electrode of Quantitative detection tonyred |
| CN105911120A (en) * | 2016-04-13 | 2016-08-31 | 中国科学院过程工程研究所 | Sulfur-doped graphene oxide modified glassy carbon electrode, preparation method and detection method for heavy metals in water |
| CN105911120B (en) * | 2016-04-13 | 2018-07-06 | 中国科学院过程工程研究所 | Glass-carbon electrode, preparation method and the method for carrying out heavy metal analysis in water of sulfur doping graphene oxide modification |
| CN106910902A (en) * | 2017-01-22 | 2017-06-30 | 济南大学 | A kind of fuel cell oxygen reduction catalyst and preparation method thereof |
| CN110609069A (en) * | 2019-10-16 | 2019-12-24 | 常州大学 | Preparation of a CuNi/reduced graphene non-enzymatic sulfite electrochemical sensor |
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| CN104090009B (en) | 2016-06-01 |
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