CN106669446A - SVOCs solid-phase extraction membrane - Google Patents
SVOCs solid-phase extraction membrane Download PDFInfo
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- CN106669446A CN106669446A CN201710008847.8A CN201710008847A CN106669446A CN 106669446 A CN106669446 A CN 106669446A CN 201710008847 A CN201710008847 A CN 201710008847A CN 106669446 A CN106669446 A CN 106669446A
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- Prior art keywords
- svocs
- solid
- membrane
- phase extraction
- dimethyl silicone
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0415—Solvent extraction of solutions which are liquid in combination with membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/32—By heating or pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/30—Cross-linking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Sampling And Sample Adjustment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
An SVOCs solid-phase extraction membrane comprises an electrospinning membrane and a polydimethyl siloxane composite layer on the surface of the electrospinning membrane. The SVOCs solid-phase extraction membrane can be directly immersed into a sample to extract the SVOCs components in the sample, and the SVOCs solid-phase extraction membrane can be subsequently directly combined with an SVOCS separation and detecting device during use. The SVOCs solid-phase extraction membrane has the advantages that the mechanical strength of the electrospinning membrane is increased, moisture absorption and residues on the surface of the membrane are reduced, and the extraction efficiency of hydrophobic SVOCs components is increased.
Description
Technical field
The present invention relates to a kind of composite electrospun cortina, in particular for the material of semi-volatile organic matter SPE analysis
Material.
Background technology
Semi-volatile organic matter (SVOCS) is a big type organic in water body, air, soil, and its boiling point is general at 200 DEG C
~550 DEG C, and the boiling point of volatile organic matter (VOCs) is general below 200 DEG C.Compare the SVOC of concern at presentSIt is dirty chemical industry
Dye thing, residues of pesticides etc., its content is general in trace 10-6W/w or ultra trace 10-9W/w levels, with a large amount of inorganic matters, organic matter
Coexist, directly determine difficult.Therefore, it is necessary to select the suitable sample-pretreating method to carry out SVOCs before analysis is separated
Extracting and enriching, reduces the interference of coexisting substances.The sample pre-treatments mistakes such as solid phase micro-extraction technique will sample, extraction, enrichment, purification
Journey collection is completed in a step, is especially suitable for the extractive analysis of SVOCs.Wherein, effective mass transfer flux of electrospun membrane extraction is fast, extraction
Amount is big, for quickly analyzing significant.
There is open defect in the Electrospun spe membrane of current SVOCs：(1) mechanical strength of electrostrictive polymer spinning is relatively low, holds
Easily scatter, it has not been convenient to use；(2) hygroscopicity of common electrospun membrane is big, many steam of remaining, disturbs follow-up chromatogram point
From, Mass Spectrometer Method；(3) one class materials be typically only suitable for extract a class SVOCs compounds, such as common polyethersulfone ketone (PPESK),
It is adapted to extraction polarity S VOCs, PDMS, reverse-phase chromatography fixing phase more polyimides and is only suitable for extracting apolar SVOCs.
In consideration of it, urgently developing the new Electrospun spe membrane for SVOCs extractive analysis.
The content of the invention
An object of the present invention is to provide a kind of SVOCs solid-phase extraction membranes, including：Electrospun membrane, and, Electrospun
Dimethyl silicone polymer (PDMS) composite bed on film surface.
Wherein, 0.01~1 micron of described dimethyl silicone polymer composite bed thickness.
In the SVOCs solid-phase extraction membranes of the invention described above, described electrospun membrane is selected from following material：It is polystyrene, poly-
To divinylbenzene, polyimides, protein or polysaccharide polymer.
Another aspect of the present invention provides the preparation method of above-mentioned SVOCs solid-phase extraction membranes, is that electrospun membrane is immersed into poly- two
The unnecessary dimethyl silicone polymer (PDMS) of removal is centrifuged 0.1~30 minute in methylsiloxane (PDMS) solution, after taking-up, places
To dimethyl silicone polymer (PDMS) crosslinking curing.
Wherein, the preparation of described dimethyl silicone polymer (PDMS) solution has used silicon rubber for adhesive, adhesive
More specifically citing is DOW CORNING Sylgard 184.Furthermore, when preparing the solution, the solvent for diluting PDMS can basis
Electrospun membrane material is selected, and may be selected from chloroform, dichloromethane, aromatic hydrocarbons, alkane or tetrahydrofuran.For example, as Electrospun is
Polyimides material, then can select tetrahydrofuran solvent.
The SVOCs solid-phase extraction membranes of the invention described above are immersed during into the sample containing SVOCs, and SVOCs is migrated to film, inhaled
Attached, SVOCs (such as n-alkane, aromatic hydrocarbons) primary attachment of wherein low pole is retained in PDMS coatings, most polarity compared with
Big SVOCs (such as organic phenol, alcohol, acid, halogenated hydrocarbons, nitro hydrocarbon) can migrate across PDMS coatings, adsorbed by electrospun polymer and protected
Stay.The SVOCs being attracted in PDMS layer can be removed by appropriate method, and then analyzed or quantitative determination.
Based on this, the present invention further provides application of the SVOCs solid-phase extraction membranes in SVOCs detections.Specifically,
The present invention discloses a kind of detection method of semi-volatile organic matter (SVOCs), and the method is the SVOCs for using the invention described above
Solid-phase extraction membrane, including the step of extraction absorption and removing absorption is carried out to the semi-volatile organic matter in sample.As specific
Implementation method, SVOCs solid-phase extraction membranes are directly immersed in sample, and sample is liquid or gas.Sample temperature is in normal temperature~200
℃。
Further, in the detection method of SVOCs of the present invention, remove the step of adsorbing and can alternatively be used solvent
Wash-out or heating De contamination.Wherein, most SVOCs components can select appropriate solvent to elute.For resistant to elevated temperatures electrospinning
Cortina, such as polyimides (PI), poly- to divinylbenzene (PDVB), can also directly heat is desorbed SVOCs, for further analysis
Detection.
Compared with existing Electrospun, the electrospun membrane of PDMS modifications prepared by this method, with following obvious advantage：
1st, electrospun membrane toughness is improved, electrospun membrane structural integrity is kept.The glass transition temperature of most of polymer is all remote
Far above room temperature, such as polyimides, polymethyl methacrylate, makrolon, its electrospun membrane is easy for fracture, powder at room temperature
It is broken, it is impossible to operation application.After coating PDMS, the operability of electrospun membrane can be significantly improved.
2nd, the absorption residual of steam is reduced, is easy to follow-up SVOCs chromatographic isolations to detect.The SVOCs of membrane extraction, many situations
Under, all give gas-chromatography separation detection with thermomechanical desorption.If Residual water is more in electrospun membrane, chromatographic column can be damaged,
Flame ionization ditector baseline fluctuation is caused until flame-out, or even allows the disintegration of filament of mass ion source.
3rd, the extraction efficiency of hydrophobicity SVOCs is improved, increases coverage of the membrane extraction method to SVOCs compounds.Invention
The electrospun membrane of PDMS modifications combine extracting power of the electrostrictive polymer spinning to polar compound, and PDMS is to nonpolar
The absorption reserve capability of compound, can cover most target SVOCs in single extraction, improve analysis efficiency.
Brief description of the drawings
The width of accompanying drawing of the present invention 2
Fig. 1 is the polyimides electrospun membrane axial cross section structural representation of PDMS modifications.
Fig. 2 is the polyimides electrospun membrane radial section structural representation of PDMS modifications.
In figure, 101：Electrospun membrane；102：Dimethyl silicone polymer composite bed (102).
Specific embodiment
Refer specifically to coat dimethyl silicone polymer (PDMS) thin layer on electrospun membrane surface, prepare the electricity of PDMS surface modifications
Spinning composite membrane, and corresponding SVOCs membrane extraction analysis methods.Composite membrane can be directly immersed in sample, and extract sample
SVOCs components, it is follow-up to be directly combined SVOCs separation detecting devices.The advantage of the invention is that：(1) machine of electrospun membrane is improved
Tool intensity, (2) reduce absorption and residual of the moisture content on film surface, and (3) improve the extraction efficiency of hydrophobicity SVOCs components.
Following non-limiting examples should be understood not any to the content of the invention for the invention will be further described,
The limitation of form.
Embodiment 1
Prepare the polyimides electrospun membrane of PDMS modifications
Bibliography (Journal of Chromatography A, 1411 (2015) 1-8) prepares polyimides Electrospun
Film 101 (string diameter~400 nanometer, 1 millimeter of thickness), takes the electrospun membrane of 2cm × 2cm sizes, immerses DOW CORNING 10:1 mixing
The glue of Sylgard 184,25 DEG C of vacuum outgas 10 minutes stand 20 minutes.Taking-up lies in a horizontal plane in the stainless steel cloth of 200 mesh
On, it is put into centrifuge tube, 6000 revs/min are centrifuged 5 minutes, remove the PDMS of Electrospun excess surface.After taking-up, 60 DEG C of heating
Polymethyl siloxane is fully cured within 30 minutes, forms the polyimides electrospun membrane of PDMS modifications.The structure of electrospun membrane is such as
Fig. 1 shows.
Embodiment 2
The polyimides electrospun membrane of PDMS modifications prepared by embodiment 1 is used for the extraction point of semi-volatile organic matter in water
Analysis.
Electrospun membrane (2cm × 2cm) prepared by embodiment 1, is directly immersed in 50mL, 1ppb SVOCs simulation aqueous solution,
600 revs/min of stirrings, extract 20 minutes.After 20 minutes, spe membrane is taken out, be put into hot parser, SVOCs heated and is desorbed, entered
Enter gas-chromatography separation detection.
Experiment finds：The pure polyimides electrospun membrane of contrast, in the polyimides electrospun membrane of PDMS modifications, nitro
Benzene, the extraction efficiency of phenol are similar to, but polycyclic aromatic hydrocarbon, n-alkane extraction efficiency improve 3-10 times.
Claims (7)
1. a kind of SVOCs solid-phase extraction membranes, including：
Electrospun membrane (101), and,
The dimethyl silicone polymer composite bed (102) on electrospun membrane (101) surface.
2. SVOCs solid-phase extraction membranes according to claim 1, it is characterised in that described dimethyl silicone polymer composite bed
0.01~1 micron of thickness.
3. SVOCs solid-phase extraction membranes according to claim 1, it is characterised in that described electrospun membrane is selected from following material
Matter：It is polystyrene, poly- to divinylbenzene, polyimides, protein or polysaccharide polymer.
4. the preparation method of the SVOCs solid-phase extraction membranes described in claim 1, is that electrospun membrane is immersed into dimethyl silicone polymer
The unnecessary dimethyl silicone polymer of removal is centrifuged 0.1~30 minute in solution, after taking-up, places solid to dimethyl silicone polymer crosslinking
Change.
5. method according to claim 4, it is characterised in that described dimethyl silicone polymer solution is matched somebody with somebody by silicon rubber
System, solvent is selected from chloroform, dichloromethane, aromatic hydrocarbons, alkane and tetrahydrofuran.
6. the detection method of semi-volatile organic matter, it is characterised in that including the SVOCs SPEs described in usage right requirement 1
Film carries out the step of extraction absorption and removing absorption to the semi-volatile organic matter in sample.
7. detection method according to claim 6, it is characterised in that the step of described removing is adsorbed is washed using solvent
De- or heating De contamination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710008847.8A CN106669446A (en) | 2017-01-06 | 2017-01-06 | SVOCs solid-phase extraction membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710008847.8A CN106669446A (en) | 2017-01-06 | 2017-01-06 | SVOCs solid-phase extraction membrane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126737A (en) * | 2018-06-25 | 2019-01-04 | 宁波大学 | A kind of solid phase extraction material |
Citations (5)
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|---|---|---|---|---|
| CN101497034A (en) * | 2009-01-05 | 2009-08-05 | 东南大学 | Solid phase extraction method based on nylon nano fiber film and extractor |
| CN101900646A (en) * | 2010-07-27 | 2010-12-01 | 北京师范大学 | Rapid sampler of micro polycyclic aromatic hydrocarbon in water based on electrospinning nano-fiber membrane |
| CN102338713A (en) * | 2011-07-13 | 2012-02-01 | 东南大学 | Method for simultaneous extraction of a plurality of target substances with different polarity in sample |
| CN103816695A (en) * | 2014-02-25 | 2014-05-28 | 东南大学 | Solid phase extraction method of phenolic endocrine disrupting chemicals in sample |
| US20160354758A1 (en) * | 2015-06-03 | 2016-12-08 | Tadeusz Gorecki | Thermally Modified Polymeric Organosilicon Material, Method for Preparing Said Material and the Uses Thereof |
-
2017
- 2017-01-06 CN CN201710008847.8A patent/CN106669446A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497034A (en) * | 2009-01-05 | 2009-08-05 | 东南大学 | Solid phase extraction method based on nylon nano fiber film and extractor |
| CN101900646A (en) * | 2010-07-27 | 2010-12-01 | 北京师范大学 | Rapid sampler of micro polycyclic aromatic hydrocarbon in water based on electrospinning nano-fiber membrane |
| CN102338713A (en) * | 2011-07-13 | 2012-02-01 | 东南大学 | Method for simultaneous extraction of a plurality of target substances with different polarity in sample |
| CN103816695A (en) * | 2014-02-25 | 2014-05-28 | 东南大学 | Solid phase extraction method of phenolic endocrine disrupting chemicals in sample |
| US20160354758A1 (en) * | 2015-06-03 | 2016-12-08 | Tadeusz Gorecki | Thermally Modified Polymeric Organosilicon Material, Method for Preparing Said Material and the Uses Thereof |
Non-Patent Citations (3)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126737A (en) * | 2018-06-25 | 2019-01-04 | 宁波大学 | A kind of solid phase extraction material |
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