CN102809554A - Nano-sensitive material for dichlorodiphenyltrichloroethane pesticide - Google Patents
Nano-sensitive material for dichlorodiphenyltrichloroethane pesticide Download PDFInfo
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- CN102809554A CN102809554A CN2011103497370A CN201110349737A CN102809554A CN 102809554 A CN102809554 A CN 102809554A CN 2011103497370 A CN2011103497370 A CN 2011103497370A CN 201110349737 A CN201110349737 A CN 201110349737A CN 102809554 A CN102809554 A CN 102809554A
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Abstract
The invention relates to a nano-sensitive material for monitoring a dichlorodiphenyltrichloroethane pesticide. The nano-sensitive material is characterized by consisting of Pd atom-doped La2O3, Fe2O3 and NiO nano-powder, wherein the Pd atom-doped La2O3, Fe2O3 and NiO nano-powder comprises the following components: 2 to 3 percent of Pd, 29 to 35 percent of La2O3, 38 to 44 percent of Fe2O3 and 18 to 24 percent of NiO; and the particle size range is 15 to 35nm. A dichlorodiphenyltrichloroethane pesticide 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 dichlorodiphenyltrichloroethane pesticide on line, and is not affected by coexisting substances.
Description
Technical field
The present invention relates to a kind of dopen Nano sensitive material that is used to monitor biconjugate chlorphenyl trichloroethanes agricultural chemicals, the La that especially mixes up by the Pd atom
2O
3, Fe
2O
3Sensitive material with the NiO nano-powder is formed belongs to field of sensing technologies.
Background technology
Along with the development of agriculture industrialization, chemical pesticide is being brought into play more and more important effect in the production of agricultural product such as China's grain, vegetables, fruit, tealeaves and medicinal material.But; Because people are to the characteristics of motion of agricultural chemicals in the nature biotechnology body; The acquisition of knowledge such as aspects such as metabolic pathway, degraded mode and residual savings is not enough, when the enjoyment chemical pesticide brings good harvest happy, has usually ignored its residual harm that brings.In the control agricultural product one of key link of persticide residue be exactly to persticide residue in the agricultural product carry out in time, analyzing and testing exactly, with the reasonable use of monitoring agricultural chemicals, prevent that the launch that residues of pesticides exceed standard from selling, guarantee agricultural product quality and safety.
Biconjugate chlorphenyl trichloroethanes (Dichlorodiphenyltrichloroethane) is D.D.T. (dichloro-diphenyl-trichloroethane) (DDT), chemical formula (ClC again
6H
4)
2CH (CCl
3), be white crystal, water insoluble, be dissolved in kerosene, can be made into emulsion, be the effective insecticidal agent.Be that 20 th Century prevent agricultural pest, very big effect has been played in the disease harm that alleviates mosquitos and flies propagation such as malaria typhoid fever.DDT is reined in 1874 first by the diligent moral of Ou Tema to synthesize, and but is nineteen thirty-nine just to be realized out by Miller but this compound has the characteristic of pesticide effect.This product is almost all very effective to all insects.During the World War II, the usable range of DDT has obtained expansion rapidly, and is exhibiting one's skill to the full aspect the treatment of diseases such as malaria, dysentery, has given treatment to a lot of life, but also has brought the raising the output of crops.But find D.D.T. (dichloro-diphenyl-trichloroethane) very difficult degradation in environment in the eighties of last century scientists sixties; And can in animal tallow, accumulate; Even in the blood of antarctic penguin, also detect D.D.T. (dichloro-diphenyl-trichloroethane); The birds body includes D.D.T. (dichloro-diphenyl-trichloroethane) and can cause producing soft-shelled egg and can not hatch, and therefore the bird of prey such as the U.S. national bird white-crowned sea eagle that especially are in the food chain climax almost become extinct.1962, U.S. scientist Lei Qieerkaxun suspected that in its works " silent spring " it is to cause the main cause of the bird of some food meat and ichthyophagy near extinction that DDT gets into food chain.Therefore D.D.T. (dichloro-diphenyl-trichloroethane) is prohibited by countries in the world gradually and is produced and use after the seventies.DDT can be in the medium-term and long-term accumulation of body fat; Be proved and can have upset biological hormone secretion; " epidemiology " magazine of calendar year 2001 is mentioned, and scientist has confirmed first that through 24 16 to 28 years old Mexico man's of selective examination blood sample the rising of DDT level can cause sperm number to reduce in the human body.In addition, the increase of neonatal premature labor and nascent body weight also has certain contact with DDT, and existing medical research has shown that also it is influential to the mankind's liver function and form, and tangible carcinogenic performance is arranged.
DDT has advantages of higher stability and persistence, in the farmland of medication after 6 months, still can detect the evaporation of DDT.DDT pollutes various places all over the world, from drift about 1000 kilometers with dust far away with still can detect the snow-broth that dissolves from the South Pole trace DDT.Generally speaking, the concentration range of the non-agricultural airborne DDT in district is 1~2.36 * 10
-6Ng/m
3, its concentration range of agriculture residential block is 1~22 * 10
-6Ng/m
3, the concentration of DDT more can be up to 8.5 * 10 in the resident who carries out the kill mosquito spraying
-3Mg/m
3
The assay method of biconjugate chlorphenyl trichloroethanes agricultural chemicals mainly contains vapor-phase chromatography, liquid phase chromatography, mass spectroscopy, liquid-matter coupling method, electrochemical process and AAS etc.;, these methods measure the therefore difficult popularization of length consuming time because needing preconcentration and suitable processing could pass through the large-sized analytic instrument completion more.
Summary of the invention
The purpose of this invention is to provide dopen Nano sensitive material of a kind of easy monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals and preparation method thereof.The sensor of the monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals made from this sensitive material can fast, accurately be measured micro-biconjugate chlorphenyl trichloroethanes agricultural chemicals at the scene and not receive the interference of other concurrent.
Dopen Nano sensitive material of the present invention is the La that is mixed up by the Pd atom
2O
3, Fe
2O
3Form with the NiO nano-powder, its preparation method is:
(1) lanthanum salt, molysite and nickel salt are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, use ammoniacal liquor to regulate the pH value and be 2.6-3.8; Continue to stir 5-8 hour, still aging, solution is obtained gel at 70-85 ℃ of rotary evaporation; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 550-600 ℃ with per minute; Keep this temperature 2-3 hour, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Wherein, The lanthanum salt that uses in the step (1) is meant one or more potpourri of anhydride or the hydrate of lanthanum nitrate, lanthanum chloride and lanthanum acetate; Molysite is that molysite is one or more a potpourri of anhydride or the hydrate of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate, and nickel salt is one or more a potpourri of anhydride or the hydrate of nickel chloride, nickelous bromide, nickelous sulfate and nickel nitrate.
When the particle diameter of nanometer powder scope that makes is 15~35nm, and each component satisfies Pd (2-3%), La
2O
3(29-35%), Fe
2O
3(38-44%) and during NiO (18-24%), be used for having very high sensitivity and selectivity as the sensitive material of monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals.
Embodiment
Embodiment 1
(1) lanthanum nitrate, iron sulfate and nickel chloride are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, using ammoniacal liquor to regulate the pH value is 2.8; Continue to stir 6 hours, still aging, solution is obtained gel at 75 ℃ of rotary evaporations; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 560 ℃ with per minute; Keep this temperature 2 hours, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 19~33nm; It is carried out constituent analysis, record and consist of 2.1%Pd, 34.1%La
2O
3, 40.7%Fe
2O
3And 23.1%NiO.
Use: with the catalytic luminescence sensitive material of this powder as mensuration biconjugate chlorphenyl trichloroethanes, the range of linearity 1.5~70mg/m
3, detection limit can reach 0.50mg/m
3, common agricultural chemicals concurrent does not disturb.
Embodiment 2
(1) lanthanum acetate, iron chloride, ferric perchlorate and nickel nitrate are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, using ammoniacal liquor to regulate the pH value is 3.0; Continue to stir 7 hours, still aging, solution is obtained gel at 71 ℃ of rotary evaporations; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 590 ℃ with per minute; Keep this temperature 2 hours, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 16~33nm; It is carried out constituent analysis, record and consist of 2.9%Pd, 32.5%La
2O
3, 43.8%Fe
2O
3And 20.8%NiO.
Use: with the catalytic luminescence sensitive material of this powder as mensuration biconjugate chlorphenyl trichloroethanes, the range of linearity 1.4~60mg/m
3, detection limit can reach 0.50mg/m
3, common agricultural chemicals concurrent does not disturb.
Embodiment 3
(1) lanthanum nitrate, lanthanum chloride, iron chloride, nickel chloride and nickel nitrate are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, using ammoniacal liquor to regulate the pH value is 3.7; Continue to stir 6 hours, still aging, solution is obtained gel at 84 ℃ of rotary evaporations; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 580 ℃ with per minute; Keep this temperature 3 hours, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 15~30nm; It is carried out constituent analysis, record and consist of 2.5%Pd, 32.3%La
2O
3, 41.5%Fe
2O
3And 23.7%NiO.
Use: with the catalytic luminescence sensitive material of this powder as mensuration biconjugate chlorphenyl trichloroethanes, the range of linearity 1.5~70mg/m
3, detection limit can reach 0.60mg/m
3, common agricultural chemicals concurrent does not disturb.
Embodiment 4
(1) lanthanum chloride, lanthanum acetate, ferric nitrate and nickelous sulfate are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, using ammoniacal liquor to regulate the pH value is 3.5; Continue to stir 7 hours, still aging, solution is obtained gel at 78 ℃ of rotary evaporations; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 599 ℃ with per minute; Keep this temperature 2 hours, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 21~34nm; It is carried out constituent analysis, record and consist of 2.7%Pd, 31.1%La
2O
3, 42.7%Fe
2O
3And 23.5%NiO.
Use: with the catalytic luminescence sensitive material of this powder as mensuration biconjugate chlorphenyl trichloroethanes, the range of linearity 1.2~63mg/m
3, detection limit can reach 0.40mg/m
3, common agricultural chemicals concurrent does not disturb.
Embodiment 5
(1) lanthanum chloride, ferric perchlorate, nickelous sulfate and nickel nitrate are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, using ammoniacal liquor to regulate the pH value is 2.6; Continue to stir 6 hours, still aging, solution is obtained gel at 72 ℃ of rotary evaporations; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 551 ℃ with per minute; Keep this temperature 3 hours, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
Analyze: with this powder body material of transmissioning electric mirror test, its particle size range is 17~33nm; It is carried out constituent analysis, record and consist of 2.6%Pd, 30.8%La
2O
3, 43.6%Fe
2O
3And 23.0%NiO.
Use: with the catalytic luminescence sensitive material of this powder as mensuration biconjugate chlorphenyl trichloroethanes, the range of linearity 1.0~58mg/m
3, detection limit can reach 0.40mg/m
3, common agricultural chemicals concurrent does not disturb.
Claims (3)
1. a nano sensitive material of monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals is characterized in that the La that is mixed up by the Pd atom
2O
3, Fe
2O
3Form with the NiO nano-powder, wherein each component concentration is Pd (2-3%), La
2O
3(29-35%), Fe
2O
3(38-44%) and NiO (18-24%), its preparation method is:
(1) lanthanum salt, molysite and nickel salt are dissolved in the WS of watery hydrochloric acid altogether, under the high-speed stirred state, add an amount of citric acid and make solution keep clear state, use ammoniacal liquor to regulate the pH value and be 2.6-3.8; Continue to stir 5-8 hour, still aging, solution is obtained gel at 70-85 ℃ of rotary evaporation; With gel infra-red drying 1 hour, after fully grinding, in high temperature box type resistance furnace, be no more than 5 ℃ speed and be warming up to 550-600 ℃ with per minute; Keep this temperature 2-3 hour, and obtained La
2O
3, Fe
2O
3With the NiO nano-powder;
(2) palladium bichloride being dissolved in massfraction is in 8% the aqueous hydrochloric acid solution; Under constantly stirring; The above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, and continuation stirring and dropping massfraction are 35% hydrazine hydrate aqueous solution, mix; Directly place drying box to dry, promptly get the La that the Pd atom mixes up
2O
3, Fe
2O
3With the NiO nano-powder.
2. a kind of nano sensitive material of monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals according to claim 1; It is characterized in that described lanthanum salt is meant one or more potpourri of anhydride or the hydrate of lanthanum nitrate, lanthanum chloride and lanthanum acetate; Molysite is that molysite is one or more a potpourri of anhydride or the hydrate of iron chloride, ferric perchlorate, iron sulfate and ferric nitrate, and nickel salt is one or more a potpourri of anhydride or the hydrate of nickel chloride, nickelous bromide, nickelous sulfate and nickel nitrate.
3. a kind of nano sensitive material of monitoring biconjugate chlorphenyl trichloroethanes agricultural chemicals according to claim 1, the particle diameter particle size range that it is characterized in that described nano sensitive material is 15~35nm.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109187512A (en) * | 2018-09-17 | 2019-01-11 | 四川大学 | A kind of catalytic luminescence analysis method based on nickel oxide detection hydrogen sulfide |
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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 |
-
2011
- 2011-11-08 CN CN201110349737.0A patent/CN102809554B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US5981424A (en) * | 1997-07-31 | 1999-11-09 | Sunoco, Inc. (R&M) | Catalysts for hydroxylation and ammination of aromatics using molecular oxygen as the terminal oxidant without coreductant |
CN100580455C (en) * | 2007-12-28 | 2010-01-13 | 北京联合大学生物化学工程学院 | Ammoniacal nanometer composite oxides sensitive material |
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 |
Non-Patent Citations (1)
Title |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109187512A (en) * | 2018-09-17 | 2019-01-11 | 四川大学 | A kind of catalytic luminescence analysis method based on nickel oxide detection hydrogen sulfide |
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