CN104667574A - Rotational detachable film solid phase micro extraction device - Google Patents
Rotational detachable film solid phase micro extraction device Download PDFInfo
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- CN104667574A CN104667574A CN201510119661.0A CN201510119661A CN104667574A CN 104667574 A CN104667574 A CN 104667574A CN 201510119661 A CN201510119661 A CN 201510119661A CN 104667574 A CN104667574 A CN 104667574A
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- molecular sieve
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- phase micro
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Abstract
The invention discloses a rotational detachable film solid phase micro extraction device which comprises a ceramic column substrate and a polydimethylsiloxane composite film, wherein the polydimethylsiloxane composite film is arranged on the surface of the ceramic column substrate and is internally embedded with a carbon molecular sieve; a rotating shaft rod is fixedly arranged on the ceramic column substrate; a motor is arranged on the rotating shaft rod. Compared with the prior art, the rotational detachable film solid phase micro extraction device effectively overcomes the defect that a small-volume solution is hard to stir with a magnetic force, and meanwhile the defect that a solid micro extraction stirring rod has high probability of abrasion is reduced, so that the service life of the rotational detachable film solid phase micro extraction device can be prolonged; as a Caboxen-PDMS composite film is used as an adsorption material, the extraction amount and the detection sensitivity can be improved; the method is simple and convenient, easy to operate and high in flexibility.
Description
Technical field
The present invention relates to a kind of rotary detachable film solid-phase micro-extracting device.
Background technology
Chinese patent 201110176522.3 relates to a kind of dimethyl silicone polymer complex carbon molecules sieve coating stirring extraction bar, this stirring extraction bar application dimethyl silicone polymer complex carbon molecules sieve is as the coating material stirring extraction bar coating, application barred body is as the matrix stirring the coating of extraction bar coating, and described barred body is encapsulated in glass tube by the iron core shorter than glass tube to make.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of rotary detachable film solid-phase micro-extracting device, overcome the shortcoming being difficult to use magnetic agitation in reduced volume of solution, decrease the shortcoming that stir bar sorptive extraction is easy to wear and tear simultaneously, thus can increase the service life.
The present invention is achieved through the following technical solutions:
A kind of rotary detachable film solid-phase micro-extracting device, comprises ceramic cylinder substrate, is arranged on the dimethyl silicone polymer laminated film of the embedded carbon molecular sieve of ceramic cylinder substrate surface.
Further, described ceramic cylinder substrate is fixedly installed rotating shaft bar, described rotating shaft bar is provided with motor.
Further, the dimethyl silicone polymer laminated film thickness of described embedded carbon molecular sieve is 100 ~ 200 μm, and embedded carbon molecular sieve is of a size of 50 ~ 75 μm.
Further, the preparation method of the dimethyl silicone polymer laminated film of described embedded carbon molecular sieve is: carbon molecular sieve particles added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10:1 ~ 10.5:1, again stir 10 ~ 15min, after mixing by mixture as molding on spin coating instrument, then at the temperature of 80 ~ 90 DEG C, 1 ~ 1.5h is cured, after solidification, again the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is heated to 120 ~ 130 DEG C, keeps 2 ~ 3h.
Further, carbon molecular sieve particles is added inside polydimethylsiloxane prepolymer thing and stir, then add curing agent according to the ratio of 10: 1 ~ 10.5:1, and utilize the mode vacuumized make the bubble floating in mixed liquor to surface and break, after waiting for that bubble removes completely, by mixture molding.
Further, described motor is adjustable rotating speed motor.
A kind of using method of rotary detachable film solid-phase micro-extracting device, the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is placed in sample, starting motor makes it rotate, concentration per sample or viscosity, adjustable rotating speed is 0 ~ 500rpm, may ultimately reach the effect of the target analytes in Rapid Extraction sample, after having sampled, the dimethyl silicone polymer laminated film of embedded carbon molecular sieve can be disassembled from ceramic cylinder substrate, seal up for safekeeping after curling, then analyzed by gas chromatography series connection system.
Compared with prior art, the present invention effectively overcomes the shortcoming being difficult to use magnetic agitation in reduced volume of solution, decrease the shortcoming that stir bar sorptive extraction is easy to wear and tear simultaneously, thus can increase the service life, with Caboxen-PDMS laminated film for sorbing material, improve extraction quantity and detection sensitivity; Method is easy, easily operates, and flexibility is high.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is total ion figure that the embodiment of the present invention 4 obtains.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
As shown in Figure 1, a kind of rotary detachable film solid-phase micro-extracting device, comprise ceramic cylinder substrate 3, be arranged on the dimethyl silicone polymer laminated film of the embedded carbon molecular sieve on ceramic cylinder substrate 3 surface, described ceramic cylinder substrate 3 is fixedly installed rotating shaft bar 2, described rotating shaft bar 2 is provided with motor 1.
Embodiment 1
Carbon molecular sieve particles is added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10:1, again stir 10min, after mixing by mixture as molding on spin coating instrument, then at the temperature of 80 DEG C, 1h is cured, after solidification, then the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is heated to 120 DEG C, keeps 2h.
Embodiment 2
Carbon molecular sieve particles is added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10.5:1, again stir 15min, after mixing by mixture as molding on spin coating instrument, then at the temperature of 90 DEG C, 1.5h is cured, after solidification, then the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is heated to 130 DEG C, keeps 3h.
Embodiment 3
Carbon molecular sieve particles is added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10:1 ~ 10.5:1, again stir 10 ~ 15min, after mixing by mixture as molding on spin coating instrument, then at the temperature of 80 ~ 90 DEG C, 1 ~ 1.5h is cured, after solidification, then the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is heated to 120 ~ 130 DEG C, keeps 2 ~ 3h.
Embodiment 4
By 50mL, (1000ppm mixes buying tender in Sigma-Aldrich to the semi-volatile organic matter standard liquid of 25ppm, 25ppm is diluted to pure water) be placed in wide-mouth bottle, ceramic cylinder and Caboxen-PDMS laminated film are placed in standard liquid, starting motor makes it rotate, adjusting rotary speed is 200rpm, after 10min extraction, Caboxen-PDMS laminated film is disassembled, the curling rear vaporizer directly putting into GC-MS QP2010Plus (Japanese Shimadzu Corporation) carries out resolving and analyzing, and obtains total ion figure as shown in Figure 2.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. a rotary detachable film solid-phase micro-extracting device, is characterized in that, comprises ceramic cylinder substrate, is arranged on the dimethyl silicone polymer laminated film of the embedded carbon molecular sieve of ceramic cylinder substrate surface.
2. a kind of rotary detachable film solid-phase micro-extracting device according to claim 1, is characterized in that, described ceramic cylinder substrate is fixedly installed rotating shaft bar, described rotating shaft bar is provided with motor.
3. a kind of rotary detachable film solid-phase micro-extracting device according to claim 1 and 2, is characterized in that, the dimethyl silicone polymer laminated film thickness of described embedded carbon molecular sieve is 100 ~ 200 μm, and embedded carbon molecular sieve is of a size of 50 ~ 75 μm.
4. a kind of rotary detachable film solid-phase micro-extracting device according to claim 3, it is characterized in that, the preparation method of the dimethyl silicone polymer laminated film of described embedded carbon molecular sieve is: carbon molecular sieve particles added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10:1 ~ 10.5:1, again stir 10 ~ 15min, after mixing by mixture as molding on spin coating instrument, then at the temperature of 80 ~ 90 DEG C, 1 ~ 1.5h is cured, after solidification, again the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is heated to 120 ~ 130 DEG C, keep 2 ~ 3h.
5. a kind of rotary detachable film solid-phase micro-extracting device according to claim 4, it is characterized in that, carbon molecular sieve particles is added inside polydimethylsiloxane prepolymer thing and stir, then curing agent is added according to the ratio of 10:1 ~ 10.5:1, and utilize the mode vacuumized make the bubble floating in mixed liquor to surface and break, after waiting for that bubble removes completely, by mixture molding.
6. a kind of rotary detachable film solid-phase micro-extracting device according to claim 2, is characterized in that, described motor is adjustable rotating speed motor.
7. the using method of a rotary detachable film solid-phase micro-extracting device, it is characterized in that, the dimethyl silicone polymer laminated film of embedded carbon molecular sieve is placed in sample, starting motor makes it rotate, concentration per sample or viscosity, adjustable rotating speed is 0 ~ 500rpm, may ultimately reach the effect of the target analytes in Rapid Extraction sample, after having sampled, the dimethyl silicone polymer laminated film of embedded carbon molecular sieve can be disassembled from ceramic cylinder substrate, seal up for safekeeping after curling, then analyzed by gas chromatography series connection system.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510119661.0A CN104667574A (en) | 2015-03-18 | 2015-03-18 | Rotational detachable film solid phase micro extraction device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510119661.0A CN104667574A (en) | 2015-03-18 | 2015-03-18 | Rotational detachable film solid phase micro extraction device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105403646A (en) * | 2015-11-02 | 2016-03-16 | 刘泰峰 | Embedded type chromatographic column capable of randomly cutting color tape |
| CN106731887A (en) * | 2017-01-06 | 2017-05-31 | 宁波大学 | A kind of VOCs extracts perforated membrane |
| CN107008032A (en) * | 2017-05-18 | 2017-08-04 | 大连民族大学 | A kind of Echinoid type fibrous nodules solid-phase micro-extracting device |
| CN112588265A (en) * | 2020-11-06 | 2021-04-02 | 中山大学 | Solid-phase microextraction film for enriching hydroxyl polycyclic aromatic hydrocarbon and preparation and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201555732U (en) * | 2009-10-19 | 2010-08-18 | 中国水产科学研究院东海水产研究所 | Solid phase microextraction sampling rod |
| CN102294131A (en) * | 2011-06-20 | 2011-12-28 | 大连理工大学 | Electricity enhanced molecular imprinting solid phase micro-extraction method |
| CN102366721A (en) * | 2011-06-28 | 2012-03-07 | 天津春发食品配料有限公司 | Stirring and extracting bar for polydimethylsiloxane compounded carbon molecular sieve coating |
-
2015
- 2015-03-18 CN CN201510119661.0A patent/CN104667574A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201555732U (en) * | 2009-10-19 | 2010-08-18 | 中国水产科学研究院东海水产研究所 | Solid phase microextraction sampling rod |
| CN102294131A (en) * | 2011-06-20 | 2011-12-28 | 大连理工大学 | Electricity enhanced molecular imprinting solid phase micro-extraction method |
| CN102366721A (en) * | 2011-06-28 | 2012-03-07 | 天津春发食品配料有限公司 | Stirring and extracting bar for polydimethylsiloxane compounded carbon molecular sieve coating |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105403646A (en) * | 2015-11-02 | 2016-03-16 | 刘泰峰 | Embedded type chromatographic column capable of randomly cutting color tape |
| CN106731887A (en) * | 2017-01-06 | 2017-05-31 | 宁波大学 | A kind of VOCs extracts perforated membrane |
| CN107008032A (en) * | 2017-05-18 | 2017-08-04 | 大连民族大学 | A kind of Echinoid type fibrous nodules solid-phase micro-extracting device |
| CN112588265A (en) * | 2020-11-06 | 2021-04-02 | 中山大学 | Solid-phase microextraction film for enriching hydroxyl polycyclic aromatic hydrocarbon and preparation and application thereof |
| CN112588265B (en) * | 2020-11-06 | 2022-03-22 | 中山大学 | Solid-phase microextraction film for enriching hydroxyl polycyclic aromatic hydrocarbon and preparation and application thereof |
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Application publication date: 20150603 |