CN101554539A - Ultrasonic assistant liquid-liquid spray extraction method - Google Patents
Ultrasonic assistant liquid-liquid spray extraction method Download PDFInfo
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- CN101554539A CN101554539A CNA2008100514620A CN200810051462A CN101554539A CN 101554539 A CN101554539 A CN 101554539A CN A2008100514620 A CNA2008100514620 A CN A2008100514620A CN 200810051462 A CN200810051462 A CN 200810051462A CN 101554539 A CN101554539 A CN 101554539A
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Abstract
The invention discloses an ultrasonic assistant liquid-liquid spray extraction method. A liquid sample is pressed into an extraction container containing organic solvent in an atomization mode, meanwhile, the extraction container is soaked into an ultrasonic generator, so that the liquid sample and the organic solvent form turbulent flow, then the liquid sample contacts with the organic solvent in a smaller drop form, and the target compound in the sample is rapidly transferred into an organic phase to achieve fast extraction separation. Micromolecules in the atomized liquid sample are beneficial to improving the contact area with the organic solvent to quickly achieve liquid-liquid partition equilibrium; and the assistance of the ultrasonic generator enables the sample in the smaller drop form to contact with extracting agent, thereby the extraction efficiency is improved. The invention can separate and collect the liquid sample and has the advantages of time and labor saving, small dosage of solvent, easy operation, being applicable to large-capacity sample analysis, easy realization of semi-automation, and the like.
Description
Technical field
The present invention relates to a kind of method that is applied to the separation and the enrichment of object in the fluid sample, be meant especially a kind of be suitable for the quick pretreated ultrasonic wave of big capacity water sample auxiliary-liquid-liquid spray extraction method.
Technical background
Traditional extraction method for fluid sample is liquid-liquid extraction, belongs to solvent extraction.But traditional liquid-liquid extraction exist solvent load big, have secondary pollution, preliminary treatment that limitation, especially liquid-liquid extraction such as waste time and energy are not suitable for big capacity water sample.
Summary of the invention
Purpose of the present invention is in order to overcome liquid-liquid extraction length consuming time in the prior art, consumption of organic solvent is big, be difficult to realize shortcomings such as automation, and provide that a kind of solvent load is few, extraction efficiency is high, realize semi-automation, be particularly suitable for the quick pretreated ultrasonic wave of big capacity water sample auxiliary-liquid-liquid spray extraction method.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of ultrasonic wave is assisted-liquid-liquid spray extraction method, fluid sample is equipped with in the extraction container of organic solvent with the atomised form introducing by pressuring method, simultaneously extraction container is immersed in the supersonic generator, make fluid sample and organic solvent form turbulent flow, make fluid sample contact with the extraction organic solvent, thereby the target compound in the sample is transferred to and is carried out quick separating and extracting in the organic facies very soon with littler drop form.
Extracting process of the present invention is to utilize pump and shower nozzle that fluid sample is introduced in the organic facies with atomizing type, and described pressuring method is taked pump pressurization or gas pressurized.
Described fluid sample selects suitable organic solvent to place extractor, and fluid sample sprays into organic solvent by shower nozzle with atomised form, and unnecessary water can be discharged from water out, and organic solvent extraction liquid can take out from the organic solvent outlet.
Described extraction container and fluid sample import form the loop, triple valve is set on the loop controls, and carry out cycling extraction thus.
The spraying phenomenon is a kind of physical phenomenon that people are familiar with very much, and the most frequently used spray technique is liquid-gas atomization in people's daily life.Based on this spraying physical phenomenon, the inventor has invented the liquid-liquid spray extraction technology.At the shortcoming of existing liquid-liquid extraction technology, invented the liquid-liquid spray extraction technology based on the principle of liquid-liquid extraction.The present invention atomizes fluid sample, makes it become little molecule, improves and the organic solvent contact area, helps reaching fast liquid liquid partition equilibrium, and extraction yield is improved.Present technique is specially adapted to the extraction of large volume fluid sample.Below extractor, be close to a supersonic generator in addition, when sample enters extractor under the effect of supersonic generator, between solvent and sample, produce the sound wave cavitation, increase the contact area between sample and the extractant, make sample contact with extractant with littler drop form, further improved extraction efficiency, hyperacoustic in addition vibration homogenize makes the effect unanimity that each point is subjected in the sample media, and it is more even that whole sample is mixed.Thereby can optimize extraction conditions raising extraction yield by regulating factors such as spray velocity, spray angle, ultrasonic energy, spray extraction system bulk, organic facies, spray extraction cycle-index.It is time saving and energy saving that the present invention has the separation of fluid sample and enrichment, and solvent load is little, and is simple to operate, is applicable to big capacity sample analysis, and advantage such as easily realize semi-automation.
Description of drawings
Fig. 1 is the technology of the present invention route schematic diagram.
The specific embodiment
A kind of ultrasonic wave is assisted-liquid-liquid spray extraction method, utilizing pump and shower nozzle that fluid sample is introduced with atomised form by pressuring method is equipped with in the extraction container of organic solvent, pressuring method is taked pump pressurization or gas pressurized, gas pressurized is by controlling with bomb or pressure regulator in airtight system, select suitable organic solvent to place extractor according to fluid sample, simultaneously extraction container is immersed in the supersonic generator, under action of ultrasonic waves, make fluid sample and organic solvent form turbulent flow, make fluid sample contact with the extraction organic solvent with littler drop form, thereby the target compound in the sample is transferred to very soon and is carried out quick separating and extracting in the organic facies, unnecessary water can be discharged from water out, and organic solvent extraction liquid can take out from the organic solvent outlet.
With reference to figure 1, implement above-mentioned a kind of ultrasonic wave auxiliary-technology path diagrammatic sketch that liquid-liquid spray extraction method is taked, its extracting system is by forming with the lower part: 1-pump, 2-cycling extraction pipeline, the 3-filter, the 4-flowmeter, 5-triple valve, 6-shower nozzle, the 7-flowmeter, the outlet of 8-solvent samples, 9-water sample inlet ducts, the 10-solvent adds the inlet conduit, the 11-flowmeter, the 12-supersonic generator, the 13-control valve, 14-reclaims the extract mouth, the 15-extraction container, the 16-separator, 17-control valve, 18-waste liquid outlet.
Concrete implementation step:, the suitable organic solvent of the certain volume of 1. packing in extractor adds the water sample that will extract in the container that is filled with water; 2. shower nozzle all is immersed in below the organic solvent liquid level, keeps the distance with container bottom, in order to avoid influence spray effect; 3. open the supersonic generator switch; 4. open switch pump; 5. water sample by water sample inlet ducts (making), filter and shower nozzle by polytetrafluoroethylmaterial material with the form of spraying enter organic solvent mutually in, the flow velocity of pressure by pump and flowmeter control spraying; 6. according to requirement, regulate triple valve and sample inlet port control valve, can carry out cycling extraction sample determination; 7. the water sample that was extracted is with automatic mode inflow separation device; 8. organic solvent is separated with water in separator; 9. abolish the water sample of separated mistake, reclaim the organic solvent of separated mistake and be incorporated into the liquid-liquid spray extraction system; 10. after extraction finishes, close switch pump, close the supersonic generator switch, open the solvent outlet valve, collect extract.
The application of the present invention in actual sample also obtains good effect.Simulate experiment with dimethylbenzene, organo-chlorine pesticide (BHC and DDT), polycyclic aromatic hydrocarbon and alkyl phenol as target compound respectively, all obtain extraction yield preferably.Simulated experiment is an extractant with the 200mL carrene, adds the compound standard specimen of dissimilar variable concentrations in 1L distilled water, and the spraying flow velocity is 420mL/min, and the rate of recovery is seen attached list.
Subordinate list:
| Sequence number | Title | Mark-on concentration (ng/L) | Rate of recovery % (n 〉=6) | Sequence number | Title | Mark-on concentration (ng/L) | Rate of recovery % (n 〉=6) |
| 1 | α-HCH | 50 | 90 | 13 | Luxuriant and rich with fragrance | 200 | 103 |
| 2 | β-HCH | 50 | 87 | 14 | Pyrene | 200 | 89 |
| 3 | δ-HCH | 50 | 88 | 15 | Anthracene | 200 | 87 |
| 4 | γ-HCH | 50 | 90 | 16 | Benzo a anthracene | 200 | 92 |
| 5 | p，p’-DDT | 50 | 89 | 17 | Benzo a pyrene | 200 | 91 |
| 6 | o，p’-DDT | 50 | 85 | 18 | Butylphenol | 200 | 90 |
| 7 | p，p’-DDE | 50 | 91 | 19 | 2.4-two chlorophenols | 200 | 89 |
| 8 | p，p’-DDD | 50 | 83 | 20 | Amyl phenol | 200 | 91 |
| 9 | Naphthalene | 200 | 99 | 21 | Nonyl phenol | 200 | 92 |
| 10 | Acenaphthene | 200 | 89 | 22 | Octyl phenol | 200 | 90 |
| 11 | Acenaphthene is rare | 200 | 93 | 23 | Pentachlorophenol | 200 | 89 |
| 12 | Fluorenes | 200 | 95 | 24 | Dimethylbenzene | 86000 | 95 |
The invention discloses a kind of new extraction and separation technology to fluid sample, this technology has broad application prospects in environmental analysis. Easy to operate, easy realization semi-automation that the present invention has, saving time, save the labour, effective to the separating and extracting of hydrophobic organic compound, can be used for the advantage such as large capacity fluid separation applications.
Claims (5)
1, a kind of ultrasonic wave is assisted-liquid-liquid spray extraction method, it is characterized in that fluid sample is equipped with in the extraction container of organic solvent with the atomised form introducing by pressuring method, simultaneously extraction container is immersed in the supersonic generator, make fluid sample and organic solvent form turbulent flow, make fluid sample contact with the extraction organic solvent, thereby the target compound in the sample is transferred to and is carried out quick separating and extracting in the organic facies very soon with littler drop form.
2, a kind of ultrasonic wave according to claim 1 is assisted-liquid-liquid spray extraction method, it is characterized in that utilizing pump and shower nozzle that fluid sample is introduced in the organic facies with atomizing type, and described pressuring method is taked pump pressurization or gas pressurized.
3, a kind of ultrasonic wave according to claim 1 is assisted-liquid-liquid spray extraction method, it is characterized in that selecting suitable organic solvent to place extractor according to fluid sample, fluid sample sprays into organic solvent by shower nozzle with atomised form, unnecessary water can be discharged from water out, and organic solvent extraction liquid can take out from the organic solvent outlet.
4, a kind of ultrasonic wave according to claim 1 is assisted-liquid-liquid spray extraction method, it is characterized in that described extraction container and fluid sample import form the loop, triple valve is set on the loop controls, and carries out cycling extraction thus.
5, a kind of ultrasonic wave according to claim 1 auxiliary-liquid-liquid spray extraction method, it is characterized in that described supersonic generator is close to the bottom of extractor.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100514620A CN101554539A (en) | 2008-11-21 | 2008-11-21 | Ultrasonic assistant liquid-liquid spray extraction method |
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| CNA2008100514620A CN101554539A (en) | 2008-11-21 | 2008-11-21 | Ultrasonic assistant liquid-liquid spray extraction method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102313665A (en) * | 2010-06-30 | 2012-01-11 | 浙江工商大学 | Liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid |
| CN102690193A (en) * | 2012-03-28 | 2012-09-26 | 西安鸿生生物技术有限公司 | Preparation technology of tanshinol using spray counterflow extraction method |
| CN102788855A (en) * | 2012-07-27 | 2012-11-21 | 中国科学院合肥物质科学研究院 | On-line detection device and detection method for atomizing extraction for volatile organic matters in water |
| CN102847339A (en) * | 2012-09-07 | 2013-01-02 | 福州大学 | Gas phase extraction and enrichment method for liquid phase volatile material, and system thereof |
| CN103278595A (en) * | 2013-05-07 | 2013-09-04 | 大连依利特分析仪器有限公司 | Special automatic detection equipment for benzopyrene |
| CN105126386A (en) * | 2015-08-03 | 2015-12-09 | 清华大学 | Enriching device and method based on liquid-liquid extraction |
| CN105536290A (en) * | 2015-12-19 | 2016-05-04 | 西安鸿生生物技术有限公司 | Dynamic and continuous atomizing extraction method |
| CN106994263A (en) * | 2016-01-25 | 2017-08-01 | 北京华阳利民仪器有限公司 | A kind of ultrasonic atomizatio liquid liquid extraction plant |
| CN107126725A (en) * | 2017-05-19 | 2017-09-05 | 江苏宏博机械制造有限公司 | A kind of continuous flow upstream supercritical extraction unit |
| CN110333312A (en) * | 2019-08-13 | 2019-10-15 | 暨南大学 | The device and method of organotin in a kind of extraction plastics |
| CN114797169A (en) * | 2022-04-11 | 2022-07-29 | 辽宁大学 | Hydrodynamic cavitation assisted liquid-liquid extraction device and extraction method |
| CN114849274A (en) * | 2022-05-13 | 2022-08-05 | 西安交通大学 | Hydrogen protection extraction method and device for plants rich in easily-oxidized active ingredients |
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2008
- 2008-11-21 CN CNA2008100514620A patent/CN101554539A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102313665A (en) * | 2010-06-30 | 2012-01-11 | 浙江工商大学 | Liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid |
| CN102690193A (en) * | 2012-03-28 | 2012-09-26 | 西安鸿生生物技术有限公司 | Preparation technology of tanshinol using spray counterflow extraction method |
| CN102788855A (en) * | 2012-07-27 | 2012-11-21 | 中国科学院合肥物质科学研究院 | On-line detection device and detection method for atomizing extraction for volatile organic matters in water |
| CN102788855B (en) * | 2012-07-27 | 2014-08-06 | 中国科学院合肥物质科学研究院 | On-line detection device and detection method for atomizing extraction for volatile organic matters in water |
| CN102847339A (en) * | 2012-09-07 | 2013-01-02 | 福州大学 | Gas phase extraction and enrichment method for liquid phase volatile material, and system thereof |
| CN102847339B (en) * | 2012-09-07 | 2014-11-05 | 福州大学 | Gas phase extraction and enrichment method for liquid phase volatile material, and system thereof |
| CN103278595A (en) * | 2013-05-07 | 2013-09-04 | 大连依利特分析仪器有限公司 | Special automatic detection equipment for benzopyrene |
| CN105126386B (en) * | 2015-08-03 | 2017-02-01 | 清华大学 | Enriching device and method based on liquid-liquid extraction |
| CN105126386A (en) * | 2015-08-03 | 2015-12-09 | 清华大学 | Enriching device and method based on liquid-liquid extraction |
| CN105536290A (en) * | 2015-12-19 | 2016-05-04 | 西安鸿生生物技术有限公司 | Dynamic and continuous atomizing extraction method |
| CN106994263A (en) * | 2016-01-25 | 2017-08-01 | 北京华阳利民仪器有限公司 | A kind of ultrasonic atomizatio liquid liquid extraction plant |
| CN106994263B (en) * | 2016-01-25 | 2020-08-11 | 北京华阳利民仪器有限公司 | Method for extracting urine by ultrasonic atomization liquid-liquid extraction device |
| CN107126725A (en) * | 2017-05-19 | 2017-09-05 | 江苏宏博机械制造有限公司 | A kind of continuous flow upstream supercritical extraction unit |
| CN110333312A (en) * | 2019-08-13 | 2019-10-15 | 暨南大学 | The device and method of organotin in a kind of extraction plastics |
| CN114797169A (en) * | 2022-04-11 | 2022-07-29 | 辽宁大学 | Hydrodynamic cavitation assisted liquid-liquid extraction device and extraction method |
| CN114797169B (en) * | 2022-04-11 | 2023-11-10 | 辽宁大学 | Hydrodynamic cavitation-assisted liquid-liquid extraction device and extraction method |
| CN114849274A (en) * | 2022-05-13 | 2022-08-05 | 西安交通大学 | Hydrogen protection extraction method and device for plants rich in easily-oxidized active ingredients |
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