CN103817861B - A kind of mould preparing solid-phase extraction muddler and preparation method thereof - Google Patents
A kind of mould preparing solid-phase extraction muddler and preparation method thereof Download PDFInfo
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- CN103817861B CN103817861B CN201410066111.2A CN201410066111A CN103817861B CN 103817861 B CN103817861 B CN 103817861B CN 201410066111 A CN201410066111 A CN 201410066111A CN 103817861 B CN103817861 B CN 103817861B
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- stirring rod
- coating
- mould
- phase extraction
- profiled member
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/26—Moulds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C45/14549—Coating rod-like, wire-like or belt-like articles
Abstract
The invention discloses a kind of mould preparing solid-phase extraction muddler and preparation method thereof, described mould includes coating profiled member and base, described coating profiled member centre is provided with manhole, and centered by described base, position is provided with profiled member detent and the disk of stirring rod detent.Described preparation method comprises the following steps: stirring rod inserted in the stirring rod detent of described mould；Then casting solution is injected in mould, make casting solution in-situ solidifying in a mold be molded by chemical reaction, heating, illumination methods；The extraction coating of stirring rod and outside cladding thereof is spun off together from mould.The method utilizing mould molding mode to prepare solid-phase extraction muddler in the present invention has without main equipment, preparation method simple and fast, extraction coating dimensional controllability is good and extracts coating and stirring rod conjugation high.
Description
Technical field
The invention belongs to Sample Pretreatment Technique field, analytical chemistry field, be specifically related to one and prepare SPE
Mould of stirring rod and preparation method thereof.
Background technology
SPME (Solid Phase Microextraction, SPME) technology is early 1990s
The Sample Pretreatment Technique of development, integrates extraction, is enriched with and desorbs function, with traditional liquid-liquid extraction
Sample-pretreating method is compared, and has that device is simple, easily realizes automating online operation, easy and simple to handle, time-consuming
The features such as less, extracting and enriching efficiency is high, green is solvent-free.Research and application SPME technology find,
Although the concentration of substance to be measured is sufficiently high in sample, but the absolute recovery measured is the lowest, direct shadow
Ringing the sensitivity measured, therefore its application is restricted.1999, Belgium Sandra etc. developed solid
Extraction stirring rod technology (Stir bar sorptive extraction, SBSE) mutually, and by the commercialization of Gerstel company.
The core of extraction stirring rod is one and has magnetic cylinder, and its outer surface is sealed by inert glassy layer
?.Extraction stirring rod self Stirring sample during SBSE extraction, it is to avoid stir in Fiber-SPME
The sub-surface competitive Adsorption to sample.The SBSE product key dimension of commercialization has two kinds, i.e. length is respectively
The stirring rod of 10mm and 20mm, is respectively coated with 24 μ L and the PDMS extraction phase of 126 μ L, and SPME
It is 0.5 μ L that technology PDMS fixes the maximum volume of phase.Therefore, the enrichment times of SBSE technology improves accordingly,
High absolute recovery can be obtained and measure sensitivity, being suitable for the extraction of trace components in sample.But SBSE
Technology requiring, volume and the thickness of extraction phase are relatively large, and the requirement to intensity and heat resistance be higher,
Heatproof must be more than 250 DEG C, and therefore the preparation of the coating in stirring rod has higher difficulty.
At present, the extraction coating of commercialization SBSE technology only has dimethyl silicone polymer (PDMS) a kind of,
Prepared by employing tiretube process, i.e. use high polymer material extruder to be prepared as in specific standard by PDMS raw material
Hollow fiber pipe, on intercepting certain length PDMS pipe box to the glass bar of interior envelope magnetic core, obtains SPE and stirs
Mix rod.There are two problems in the method: (1) PDMS pipe have to use extrusion equipment to be processed shaping,
Therefore complex manufacturing process；(2) the PDMS pipe as extraction coating is the outside being inserted in stirring rod, therefore
Extraction coating is undesirable with the degree of being firmly combined with of stirring rod, and in use coating may mobile even come off.
Owing to commercialization solid-phase extraction muddler only has PDMS mono-kind to extract coating, therefore researcher is to extraction
Coating material and preparation method thereof is studied.At present, the solid-phase extraction muddler preparation method of document report
For using sol-gel technique to prepare PDMS or crown ether extraction coating, coating production is cladding process, i.e.
Stirring rod is put in sol solutions, after coating one layer of sol solutions, stirring rod is taken out, sol solutions generation colloidal sol-
Curing molding after gel reaction, outside in stirring rod forms extraction coating.The method there is the problem that painting
Layer thickness controllability is the highest and extraction coating is relatively thin, in order to increase extraction efficiency and the capacity of stirring rod, generally needs
Repeatedly to coat so as to increase extraction coating thickness, thus result in manufacturing process loaded down with trivial details and make repeatability pay no attention to
Think.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of solid-phase extraction muddler prepared
Mould and preparation method thereof, described mould structure is simple, and described preparation method is easy to operate, can be in stirring rod
The upper coating quickly forming uniform thickness, and the controllability extracting coating size is fine.
For achieving the above object, the present invention uses following technical proposals to be achieved:
A kind of mould preparing solid-phase extraction muddler, it includes coating profiled member and base, described painting formable layer
Part centre is provided with manhole, and centered by described base, position is provided with profiled member detent and stirring rod is fixed
The disk of position groove, described stirring rod detent is located at the central part of profiled member detent.
Further improvement to technique scheme: a diameter of 1-10mm of described manhole, height is
5-100mm。
Further improvement to technique scheme: the degree of depth of described stirring rod detent is 1-3mm.
Further improvement to technique scheme: described mold material be stainless steel, iron, copper, aluminium, poly-four
PVF or polymethyl methacrylate.
Present invention also offers the method utilizing described device to prepare solid-phase extraction muddler, it is characterised in that its bag
Include following steps:
(1) stirring rod is inserted through manhole in the stirring rod detent of described mould；
(2) then casting solution is injected in the described manhole of coating profiled member, make the liquid level of casting solution with
Die tip flushes, and makes casting solution in-situ solidifying in a mold be molded by chemical reaction, heating, illumination methods；
(3) the extraction coating of stirring rod and outside cladding thereof is spun off together from mould, the painting of shaping
Layer is coated on the outside of stirring rod as the extraction coating of solid-phase extraction muddler.
Further improvement to technique scheme: the heating-up temperature in described step (2) is 40-150 DEG C.
Further improvement to technique scheme: the solid-phase extraction muddler prepared is placed in methyl alcohol or ethanol is organic
Solvent soaks and goes the removal of impurity, or be placed under nitrogen protection heat ageing at aging heating-up temperature 200-300 DEG C
Go the removal of impurity.
Further improvement to technique scheme: described casting solution is high polymer monomer or performed polymer, or monomer
With the mixed solution of initiator, or the mixed solution of performed polymer and initiator.
Further improvement to technique scheme: described high polymer monomer or performed polymer be acrylate monomer or
Acrylate prepolymer body, described performed polymer is dimethyl silicone polymer and initiator with the mixed solution of initiator
Mixed liquor, described monomer and the mixed liquor that mixed solution is trimethoxy silane monomer and initiator of initiator.
Further improvement to technique scheme: described stirring rod is a length of 0.5-5cm magnetic core or iron core,
Or inorganic material rod or the macromolecular material of envelope magnetic core or iron core are excellent in 0.5-5cm.
Compared with prior art, advantages of the present invention and have the technical effect that preparation method of the present invention and biography
System cladding process is compared, and the in-situ solidifying shaping in mould of extraction coating, dimensional controllability is good, it is not necessary in order to control
System extracts coating layer thickness and repeatedly coats；Compared with tiretube process, it is not necessary to special main equipment is by high score
Sub-materials processing becomes the tubing of specific dimensions, and glass bar is directly immersed in Polymer Solution situ and is solidified into
Type, the conjugation between extraction coating and glass bar is higher.Therefore, if utilize preparation method of the present invention according to
Demand forming mold, extraction coating can be molded at the outside in-situ solidifying of stirring rod, can prepare
The solid-phase extraction muddler that size is controlled and degree of being firmly combined with is high.
The method utilizing mould molding mode to prepare solid-phase extraction muddler in the present invention has and sets without large-scale
Standby, preparation method simple and fast, extraction coating dimensional controllability be good and extraction coating and stirring rod conjugation height
Etc. feature.
Accompanying drawing explanation
Fig. 1 is the structural representation of solid-phase extraction muddler mould of the present invention, wherein, and the one-tenth after 1-assembling
Mould；101-coating profiled member；102-manhole；103-base；104-profiled member detent；105-
Stirring rod detent.
Fig. 2 is the structural representation of the split parts of solid-phase extraction muddler mould of the present invention.
Fig. 3 is that the present invention utilizes mould molding to prepare the preparation process schematic diagram of solid-phase extraction muddler, wherein
The glass stirring rod of envelope magnetic core in 2-；3-macromolecule extraction coating；4-solid-phase extraction muddler.
Detailed description of the invention
With detailed description of the invention, technical scheme is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
One, processing mold
See Fig. 1 and Fig. 2, the described device i.e. solid-phase extraction muddler shaping mould preparing solid-phase extraction muddler
Tool is made up of coating profiled member 101 and base 103 two parts: coating profiled member 101 centre is provided with circle
Through hole 102, through-hole diameter is 1-10mm, and height is 5-100mm, and the size of through hole determines SPE
The external diameter of stirring rod extraction coating and length；Base 103 is for including that there is profiled member detent 104 at center and stirs
Mixing the disk of rod detent 105, profiled member detent 104 is tight with described coating profiled member external dimensions
Coordinating, the diameter of stirring rod detent 105 closely cooperates with the external diameter of stirring rod, and the degree of depth is 1-3mm.
Coating profiled member 101 is put on base 103, is combined into mould.Mold material can be stainless steel, iron,
The metal material such as copper, aluminium, it is also possible to for the macromolecular material such as polytetrafluoroethylene (PTFE) or polymethyl methacrylate.
Two, prepared by stirring rod
Seeing Fig. 3, the preparation method of described solid-phase extraction muddler comprises the following steps:
1, stirring rod chloroform, methyl alcohol and pure water are respectively washed totally, and stirring rod is put into the centre bit of mould
Putting, stirring rod bottom is inserted in described stirring rod detent 105；Stirring rod can be a length of 0.5-5cm
Magnetic core or iron core, it is also possible to for seal in a length of 0.5-5cm magnetic core or iron core inorganic material rod (such as glass and
Quartz) or macromolecular material rod (such as polytetrafluoroethylene (PTFE)).
2, casting solution is injected the manhole 102 in described mould, make stirring rod be immersed in casting solution, make
The liquid level of casting solution flushes with die tip, then makes casting solution by modes such as chemical reaction, heating, illumination
Curing molding, forms extraction coating on stirring rod surface.
Described casting solution can be high polymer monomer or performed polymer, it is also possible to molten with the mixing of initiator for monomer
Liquid, or the mixed solution of performed polymer and initiator.Described high polymer monomer or performed polymer be acrylate monomer or
Acrylate prepolymer body, described performed polymer is that dimethyl silicone polymer mixes with initiator with the mixed solution of initiator
Closing liquid, described monomer is trimethoxy silane and initiator mixed liquor with the mixed solution of initiator.
3, after casting solution curing molding, coating profiled member 101 and base 103 two parts are separated, then will
The extraction coating of stirring rod and outside cladding thereof spins off together from coating profiled member, obtains SPE and stirs
Mix rod.
4, soak during solid-phase extraction muddler can be placed in the organic solvent such as methyl alcohol or ethanol and go the removal of impurity, it is possible to
Go the removal of impurity, aging heating-up temperature 200-300 DEG C being placed in the nitrogen lower heat ageing of protection.
Embodiment 2
One, processing mold
Mould structure as described in Example 1, prepares described mould, wherein manhole with stainless steel for material
102 a diameter of 8 μm, height is 50mm；Groove 105 degree of depth is 2mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Polydimethylsiloxane prepolymer body and the mixed liquor (2:1, v:v) of initiator benzoyl peroxide, stirring rod is interior
The glass bar of envelope magnetic core.Then make casting solution curing molding, heating-up temperature 80 DEG C by mode of heating, become
Extraction coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.
4, solid-phase extraction muddler can be placed in methanol solvate immersion and go the removal of impurity.
Embodiment 3
The present embodiment illustrates by arranging three comparative examples.
Comparative example 1
One, processing mold
With stainless steel for material preparation such as Fig. 1 processing mold, wherein a diameter of 8 μm of manhole 102, highly
For 50mm；Groove 105 degree of depth is 2mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Polydimethylsiloxane prepolymer body and the mixed liquor (2:1, v:v) of initiator benzoyl peroxide, stirring rod is interior
The glass bar of envelope magnetic core.Then make casting solution curing molding, heating-up temperature 200 DEG C by mode of heating, become
Extraction coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.Now stirring rod surface folding, sends out
Raw orange peel phenomenon.
The heating-up temperature that test result indicate that in step 2 of comparative example 1 is too high, and stirring rod surface can be caused to occur
Orange peel phenomenon, thus affect the performance of stirring rod.
Comparative example 2
One, processing mold
With stainless steel for material preparation such as Fig. 1 processing mold, wherein a diameter of 8 μm of manhole 102, highly
For 50mm；Groove 105 degree of depth is 2mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Polydimethylsiloxane prepolymer body and the mixed liquor (2:1, v:v) of initiator benzoyl peroxide, stirring rod is interior
The glass bar of envelope magnetic core.Then make casting solution curing molding, heating-up temperature 80 DEG C by mode of heating, become
Extraction coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.
4, solid-phase extraction muddler can be placed in the lower heat ageing of nitrogen protection and go the removal of impurity, aging heating-up temperature
350 DEG C, now stirring rod generation surface oxidation, color blackening.
Comparative example 2 test result indicate that then stirring rod surface can aoxidize if aging heating-up temperature is too high
The absorption property causing stirring rod is affected.
Comparative example 3
One, processing mold
With stainless steel for material preparation such as Fig. 1 processing mold, wherein a diameter of 8 μm of manhole 102, highly
For 50mm；Groove 105 degree of depth is 2mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Polydimethylsiloxane prepolymer body and the mixed liquor (2:1, v:v) of initiator benzoyl peroxide, stirring rod is interior
The glass bar of envelope magnetic core.Then make casting solution curing molding, heating-up temperature 80 DEG C by mode of heating, become
Extraction coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.
4, solid-phase extraction muddler can be placed in the lower heat ageing of nitrogen protection and go the removal of impurity, aging heating-up temperature
150 DEG C, now stirring rod adsorption effect is the best, more impurity peaks occurs.
Comparative example 3 test result indicate that if aging heating-up temperature is too low, then can affect stirring largely
The absorption property of rod.
The present embodiment proves the heating temperature in solid-phase extraction muddler preparation process of the present invention by three comparative examples
Degree and aging heating-up temperature all can produce extreme influence to the performance of stirring rod, therefore choose suitable heating-up temperature
Significant for preparing of stirring rod with aging heating-up temperature.
Embodiment 4
One, processing mold
Mould structure as described in Example 1, prepares described processing mold with stainless steel for material, wherein circular logical
A diameter of 8 μm in hole 102, height is 50mm；Groove 105 degree of depth is 2mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Trimethoxy silane and the mixed liquor (1.5:1, v:v) of initiator trifluoroacetic acid (water containing 5%), stirring rod
Glass bar for interior envelope magnetic core.Then make casting solution curing molding by sol-gel chemistry reaction, become extraction
Take coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.
4, solid-phase extraction muddler can be placed in the lower heat ageing of nitrogen protection and go the removal of impurity, heating-up temperature
300℃。
Embodiment 5
One, processing mold
Mould structure as described in Example 1, prepares described processing mold with polymethyl methacrylate for material,
Mould has light transmission, wherein a diameter of 10 μm of manhole 102, and height is 30mm；Groove 105
The degree of depth is 3mm.
Two, prepared by stirring rod
1, stirring rod is inserted perpendicularly in mould in stirring rod detent 105；
2, injecting in mould by casting solution, make the liquid level of casting solution flush with die tip, casting solution consists of
Acrylate or its performed polymer, stirring rod is the glass bar of interior envelope magnetic core.Then made by ultraviolet light initiation method
Casting solution curing molding, becomes extraction coating；
3, coating profiled member 101 and base 103 two parts are separated, then by stirring rod together with extraction coating
Spin off from coating profiled member together, obtain solid-phase extraction muddler.
4, solid-phase extraction muddler can be placed in the lower heat ageing of nitrogen protection and go the removal of impurity, heating-up temperature
260℃。
Above example is only in order to illustrate technical scheme, rather than is limited；Although with reference to front
State embodiment the present invention has been described in detail, for the person of ordinary skill of the art, still may be used
So that the technical scheme described in previous embodiment is modified, or wherein portion of techniques feature is equal to
Replace；And these amendments or replacement, do not make the essence of appropriate technical solution depart from the present invention required for protection
The spirit and scope of technical scheme.
Claims (3)
1. utilize the method that solid-phase extraction muddler prepared by mould, described mould includes coating profiled member and base, described coating profiled member centre is provided with manhole, centered by described base, position is provided with profiled member detent and the disk of stirring rod detent, and described stirring rod detent is located at the central part of profiled member detent；The a diameter of 1-10mm of described manhole, height is 5-100mm；It is characterized in that: said method comprising the steps of:
(1) stirring rod is inserted through manhole in the stirring rod detent of described mould；
(2) then casting solution is injected in the described manhole of coating profiled member, make the liquid level of casting solution flush with die tip, make casting solution in-situ solidifying in a mold be molded by chemical reaction, heating, illumination methods；Heating-up temperature is 40-150 DEG C；Described casting solution is high polymer monomer or performed polymer, or the mixed solution of monomer and initiator, or the mixed solution of performed polymer and initiator；
(3) the extraction coating of stirring rod and outside cladding thereof being spun off from mould together, the coating of shaping is coated on the outside of stirring rod as the extraction coating of solid-phase extraction muddler.
The method preparing solid-phase extraction muddler the most according to claim 1; it is characterized in that: the solid-phase extraction muddler prepared is placed in methyl alcohol or ethanol organic solvent immersion and goes the removal of impurity, or be placed under nitrogen protection heat ageing at aging heating-up temperature 200-300 DEG C and go the removal of impurity.
The method preparing solid-phase extraction muddler the most according to claim 1, it is characterized in that: described high polymer monomer or performed polymer are acrylate monomer or acrylate prepolymer body, described performed polymer is dimethyl silicone polymer and the mixed liquor that mixed solution is trimethoxy silane monomer and initiator of the mixed liquor of initiator, described monomer and initiator with the mixed solution of initiator.
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| CN201410066111.2A CN103817861B (en) | 2014-02-26 | 2014-02-26 | A kind of mould preparing solid-phase extraction muddler and preparation method thereof |
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| CN106902772B (en) * | 2017-03-29 | 2019-10-18 | 青岛贞正分析仪器有限公司 | Chelating resin solid-phase extraction muddler and preparation method thereof |
| CN107091767B (en) * | 2017-04-19 | 2020-08-04 | 苏州贞成分析仪器有限公司 | Solid-phase microextraction sampling-thermal desorption method and device for water pollutants |
Citations (3)
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|---|---|---|---|---|
| CN102099171A (en) * | 2008-05-07 | 2011-06-15 | 克劳斯玛菲科技有限公司 | Method and device for producing a coated component |
| CN102869488A (en) * | 2010-02-19 | 2013-01-09 | 赢创罗姆有限公司 | Method for producing coated molded bodies |
| CN103395162A (en) * | 2013-08-05 | 2013-11-20 | 太仓顺达磁力泵科技有限公司 | Manufacture method for full-coating corrosion-resisting magnetic drive pump shaft and pump shaft thereby |
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| DE102004062511A1 (en) * | 2004-12-24 | 2006-07-13 | Bayer Materialscience Ag | Formation and coating of substrate in a form tool, comprises forming the substrate in a cavity of the form tool, introducing the substrate into a another cavity of the form tool and coating the substrate with a lacquer in the cavity |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102099171A (en) * | 2008-05-07 | 2011-06-15 | 克劳斯玛菲科技有限公司 | Method and device for producing a coated component |
| CN102869488A (en) * | 2010-02-19 | 2013-01-09 | 赢创罗姆有限公司 | Method for producing coated molded bodies |
| CN103395162A (en) * | 2013-08-05 | 2013-11-20 | 太仓顺达磁力泵科技有限公司 | Manufacture method for full-coating corrosion-resisting magnetic drive pump shaft and pump shaft thereby |
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Effective date of registration: 20170918 Address after: 266199 No. four, No. 33 North Stream Road, Licang District, Shandong, Qingdao Patentee after: Qingdao's Secret Scientific Instrument Co. Address before: 266199 No. 805 Jinshui Road, Licang District, Shandong, Qingdao Patentee before: The loyal positive analysis Instrument Ltd. in Qingdao |
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