CN102809628B - Nano-sensitive material for trimethylamine - Google Patents
Nano-sensitive material for trimethylamine Download PDFInfo
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- CN102809628B CN102809628B CN201210170269.5A CN201210170269A CN102809628B CN 102809628 B CN102809628 B CN 102809628B CN 201210170269 A CN201210170269 A CN 201210170269A CN 102809628 B CN102809628 B CN 102809628B
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- nano
- powder
- sensitive material
- trimethylamine
- chromic
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Abstract
The invention relates to a doped nano-sensitive material for monitoring trimethylamine. The nano-sensitive material is characterized by consisting of Ag atom-doped Fe2O3 and Cr2O3 nano-powder, wherein the Ag atom-doped Fe2O3 and Cr2O3 nano-powder comprises the following components: 12 to 18 percent of Ag, 45 to 55 percent of Fe2O3 and 33 to 45 percent of Cr2O3; and the particle size is less than 30nm. A trimethylamine sensor which is prepared from the sensitive material has a relatively wide linear range, is high in selectivity and relatively high in sensitivity, can monitor a trace amount of trimethylamine in the air on line, and is not affected by coexisting substances.
Description
Technical field
The present invention relates to a kind of for monitoring the dopen Nano sensitive material of trimethylamine, the Fe especially being mixed up by Ag atom
2o
3and Cr
2o
3the sensitive material that nano-powder forms, belongs to field of sensing technologies.
Background technology
Trimethylamine belongs to vaporous pollutant, under normal temperature, be the colourless gas (fishy smell of fish products mainly comes from trimethylamine) that has fish oil stink, inflammable and explosive, and eye, nose, throat and respiratory tract to people have stronger spread effect, Long Term Contact harm is larger, the existence of trimethylamine and concentration thereof are the major criterions of assessment meat and fish food quality, it is the odor identification that characterizes some metabolic deficiency disease, being the main object of environment odor pollution control, is the key parameter of some industrial and agricultural production quality control.Therefore, the Accurate Determining of trimethylamine concentration is significant.The detection method of trimethylamine has a variety of, and better simply have acid base titration, the kjeldahl determination way of distillation, but these two kinds of methods analyst resultant errors are large, are only used as Preliminary Determination; Spectrophotometric method, the chromatography of ions, high performance liquid chromatography, headspace gas chromatography, column front derivation vapor-phase chromatography, direct injected vapor-phase chromatography, the precision such as vapor-phase chromatography are high, detection is accurate, but shortcoming is analytical procedure complexity, length consuming time and equipment that need to be expensive.
Summary of the invention
The object of the invention is to overcome the deficiency of conventional art, dopen Nano sensitive material of a kind of trimethylamine and preparation method thereof is provided.The sensor of the monitoring trimethylamine of making of this sensitive material, can be at the scene fast, the airborne micro-trimethylamine of Accurate Determining and be not subject to the interference of other concurrent.
Dopen Nano sensitive material of the present invention is the Fe being mixed up by Ag atom
2o
3and Cr
2o
3nano-powder forms, and its preparation method is:
(1) molysite and chromic salts are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.1-5.8, continue to stir 5-10 hour, still aging, solution is obtained to gel at 75-85 ℃ of rotary evaporation, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 610-650 ℃, keep this temperature 2-3 hour, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 160～200 ℃, heat reduction is 5～10 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Wherein, the molysite using in step (1) is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate, and chromic salts is one or more potpourri of the anhydride of chromium chloride, chloric acid chromium, chromic acetate, chromic nitrate and chromium sulfate or hydrate.In step (2), heat reduction temperature is controlled to 160～200 ℃, can guarantees that silver ion can be by glucose fast restore when this temperature and not oxidized.
When the particle diameter of nanometer powder making is no more than 30nm, and each component meets Ag (12-18%), Fe
2o
3(45-55%) and Cr
2o
3(33-45%), time, for the sensitive material as monitoring trimethylamine, there is very high sensitivity and selectivity.
Embodiment
Embodiment 1
(1) appropriate iron chloride and chromium chloride are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.2, continue to stir 5.5 hours, still aging, solution is obtained to gel at 76 ℃ of rotary evaporations, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 612 ℃, keep this temperature 2.5 hours, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 162 ℃, heat reduction is 6 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 25nm, and mean grain size is about 15nm; It is carried out to constituent analysis, record and consist of 12.5%Ag, 45.7%Fe
2o
3and 41.8%Al
2o
3.
Application: usining this powder body material measures airborne trimethylamine as sensitive material, the range of linearity 1～150mg/m
3, detection limit can reach 0.3mg/m
3, concurrent does not disturb.
Embodiment 2
(1) appropriate ferric nitrate and chloric acid chromium are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.3, continue to stir 9.5 hours, still aging, solution is obtained to gel at 84 ℃ of rotary evaporations, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 648 ℃, keep this temperature 2 hours, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 198 ℃, heat reduction is 7 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 28nm, and mean grain size is about 18nm; It is carried out to constituent analysis, record and consist of 15.1%Ag, 49.2%Fe
2o
3and 35.7%Al
2o
3.
Application: usining this powder body material measures airborne trimethylamine as sensitive material, the range of linearity 0.7～120mg/m
3, detection limit can reach 0.1mg/m
3, concurrent does not disturb.
Embodiment 3
(1) appropriate iron sulfate and chromic acetate are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.7, continue to stir 7 hours, still aging, solution is obtained to gel at 79 ℃ of rotary evaporations, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 625 ℃, keep this temperature 3 hours, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 178 ℃, heat reduction is 8 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 30nm, and mean grain size is about 20nm; It is carried out to constituent analysis, record and consist of 17.8%Ag, 47.1%Fe
2o
3and 35.1%Al
2o
3.
Application: usining this powder body material measures airborne trimethylamine as sensitive material, the range of linearity 0.9～113mg/m
3, detection limit can reach 0.5mg/m
3, concurrent does not disturb.
Embodiment 4
(1) appropriate ferric perchlorate and chromium sulfate are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.5, continue to stir 8 hours, still aging, solution is obtained to gel at 82 ℃ of rotary evaporations, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 640 ℃, keep this temperature 2.5 hours, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 185 ℃, heat reduction is 7 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 29nm, and mean grain size is about 20nm; It is carried out to constituent analysis, record and consist of 13.1%Ag, 52.5%Fe
2o
3and 34.4%Al
2o
3.
Application: usining this powder body material measures airborne trimethylamine as sensitive material, the range of linearity 1～140mg/m
3, detection limit can reach 0.5mg/m
3, concurrent does not disturb.
Embodiment 5
(1) appropriate iron chloride and chromic nitrate are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.8, continue to stir 5 hours, still aging, solution is obtained to gel at 77 ℃ of rotary evaporations, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 610 ℃, keep this temperature 3 hours, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 165 ℃, heat reduction is 9 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 26nm, and mean grain size is about 15nm; It is carried out to constituent analysis, record and consist of 12.9%Ag, 51.7%Fe
2o
3and 35.4%Al
2o
3.
Application: usining this powder body material measures airborne trimethylamine as sensitive material, the range of linearity 0.8～98mg/m
3, detection limit can reach 0.2mg/m
3, concurrent does not disturb.
Claims (2)
1. a nano sensitive material for trimethylamine, is characterized in that the Fe being mixed up by Ag atom
2o
3and Cr
2o
3nano-powder forms, and wherein each component concentration scope is 12-18%Ag, 45-55%Fe
2o
3and 33-45%Cr
2o
3, the particle diameter of sensitive material is less than 30nm, and its preparation method is:
(1) molysite and chromic salts are dissolved in aqueous hydrochloric acid solution altogether, under high-speed stirred state, with ammoniacal liquor, regulating pH value is 5.1-5.8, continue to stir 5-10 hour, still aging, solution is obtained to gel at 75-85 ℃ of rotary evaporation, by gel infra-red drying 2 hours, after fully grinding, in high temperature box type resistance furnace, with per minute, be no more than the speed of 5 ℃ and be warming up to 610-650 ℃, keep this temperature 2-3 hour, obtain Fe
2o
3and Cr
2o
3nano-powder;
(2) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to be uniformly mixed, directly be placed in drying box and dry, at 160～200 ℃, heat reduction is 5～10 minutes, obtains the Fe that Ag atom mixes up
2o
3and Cr
2o
3nano-powder.
2. the nano sensitive material of a kind of trimethylamine according to claim 1, it is characterized in that described molysite is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate or hydrate, chromic salts is one or more potpourri of the anhydride of chromium chloride, chloric acid chromium, chromic acetate, chromic nitrate and chromium sulfate or hydrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210170269.5A CN102809628B (en) | 2012-05-29 | 2012-05-29 | Nano-sensitive material for trimethylamine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210170269.5A CN102809628B (en) | 2012-05-29 | 2012-05-29 | Nano-sensitive material for trimethylamine |
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| Publication Number | Publication Date |
|---|---|
| CN102809628A CN102809628A (en) | 2012-12-05 |
| CN102809628B true CN102809628B (en) | 2014-10-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107976434B (en) * | 2017-11-01 | 2019-10-08 | 北京联合大学 | The sensitive material of formaldehyde in air, benzene and trimethylamine is measured simultaneously |
| CN108190831B (en) * | 2017-11-28 | 2019-06-28 | 郑州大学 | A method of doping regulation hot melt Ag nanoparticle micro-nano interconnection line performance |
Citations (4)
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| CN1804609A (en) * | 2006-01-17 | 2006-07-19 | 山东师范大学 | Formaldehyde gas sensitive device with laminated sensitive layer and preparation method thereof |
| CN101706485A (en) * | 2009-11-23 | 2010-05-12 | 北京联合大学生物化学工程学院 | Doped nano sensitive material for monitoring benzene |
| CN101887057A (en) * | 2010-06-30 | 2010-11-17 | 北京联合大学生物化学工程学院 | Nano sensitive material of carbamic acid ester pesticides |
| CN102175815A (en) * | 2010-12-07 | 2011-09-07 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring sulfur dioxide |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1234167A4 (en) * | 1999-11-18 | 2005-06-29 | Mst Technology Gmbh | Optical hydrogen detector |
| US20080077037A1 (en) * | 2003-04-21 | 2008-03-27 | Pelagia-Irene Gouma | Selective point of care nanoprobe breath analyzer |
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2012
- 2012-05-29 CN CN201210170269.5A patent/CN102809628B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1804609A (en) * | 2006-01-17 | 2006-07-19 | 山东师范大学 | Formaldehyde gas sensitive device with laminated sensitive layer and preparation method thereof |
| CN101706485A (en) * | 2009-11-23 | 2010-05-12 | 北京联合大学生物化学工程学院 | Doped nano sensitive material for monitoring benzene |
| CN101887057A (en) * | 2010-06-30 | 2010-11-17 | 北京联合大学生物化学工程学院 | Nano sensitive material of carbamic acid ester pesticides |
| CN102175815A (en) * | 2010-12-07 | 2011-09-07 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring sulfur dioxide |
Non-Patent Citations (4)
| Title |
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| 刘湘军 等.金属氧化物气敏传感器.《广州大学学报》.2007,第16卷(第5期),第42-46页. |
| 半导体氧化物气体传感器测试新原理与方法;张正勇 等;《传感技术学报》;20000630(第2期);第106-110页 * |
| 张正勇 等.半导体氧化物气体传感器测试新原理与方法.《传感技术学报》.2000,(第2期),第106-110页. |
| 金属氧化物气敏传感器;刘湘军 等;《广州大学学报》;20071030;第16卷(第5期);第42-46页 * |
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| CN102809628A (en) | 2012-12-05 |
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Granted publication date: 20141022 Termination date: 20160529 |