CN102302928A - New resin surface modified material and solid-phase extraction column thereof - Google Patents
New resin surface modified material and solid-phase extraction column thereof Download PDFInfo
- Publication number
- CN102302928A CN102302928A CN201110147850A CN201110147850A CN102302928A CN 102302928 A CN102302928 A CN 102302928A CN 201110147850 A CN201110147850 A CN 201110147850A CN 201110147850 A CN201110147850 A CN 201110147850A CN 102302928 A CN102302928 A CN 102302928A
- Authority
- CN
- China
- Prior art keywords
- solid
- resin
- phase extraction
- new
- column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention provides a new resin surface modified material and a solid-phase extraction column thereof, and belongs to the technical field of chemistry. In the new solid-phase extracted resin surface modified material, the average grain diameter difference is within +/-20 percent, and the specific weight difference is within +/-20 percent. In a solid-phase column prepared by solid-phase extraction mixed packing, mixed packing is filled in a column tube, sieve plates are arranged outside two ends of the packing to prevent the mixed packing from leaking, a sample is fed from one end of the column tube and flows out from the other end of the column tube, and eluent enters the solid-phase extraction column from a feed port. The new material and the solid-phase extraction column thereof are applied to selective extraction of polar and non-polar compounds in solution in an aqueous environment.
Description
Technical field
The present invention relates to technical field of analytical chemistry, particularly a kind of surface modification of resin new material and solid-phase extraction column thereof.
Background technology
New material is a kind of widely used sample pre-treatments technology filler; The sample pre-treatments technology for the SPE basic principle be in the sample with fixing have mutually pretend component firmly and on solid-phase extraction column, keep; And flow out solid-phase extraction column very soon, thereby reach the separation purpose with the more weak component of fixing active force mutually.
Use more SPE material to mainly contain bonded silica gel SPE material, inorganic matrix SPE material, organic polymer SPE material and mixed type SPE material 4 big classes at present.
Wherein using maximum is carbon 18 bonded silica gel solid-phase extraction columns; Generally regarded universal adsorbent; Can be from the aqueous solution adsorb organic compound; Especially be suitable for organic desalination, its major defect be selectivity low, to strong polarity and water-soluble sample keep weak, volume containing the sample is low, dust removal rate is low etc.
The inorganic matrix solid material mainly is inorganic oxide and graphitized carbon class inorganic matter, and the common feature of these inorganic material is that the surface has activity hydroxy, is mainly used in the positive extraction.
Organic polymer SPE material is that matrix is carried out modification with polystyrene divinylbenzene resin (PS); In recent years; Constantly there is new high-crosslinking-degree polymer resin SPE material to put on market, as contains methylol, benzoyl and adjacent carboxylbenzoyl, sulfonic group, trimethylamine etc.These modified resin have good hydrophily, when extraction water Semi-polarity compound, can obtain the higher rate of recovery.
Mixed type SPE material mainly is that solid-phase extraction column is inserted in sorbing material layering more than 2 kinds or 2 kinds; Reach under the prerequisite of not losing target compound; Utilize the characteristic of mixed type solid-phase extraction column different functional groups, remove the purpose of sample substrate intermediate ion type and nonpolar chaff interference through the pH value in the adjusting extraction process respectively.
But above material all has its defective, and silica gel material exists the silica gel dissolving dangerous for the analysis of high pH value; The characteristics that the resin material pore-size distribution is too wide and mechanical strength is bad; The inorganic material range of application is narrower; We take the resin-coated silica filler, and itself will have the two-fold advantage of resin and silica gel.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of resin surface modification new material is provided.
The technical scheme that the present invention adopts is following:
Resin is bonded to the silica matrix surface through chemical method, two kinds of materials of resin and silica gel are organically combined, thereby bring into play the purpose of two kinds of material advantages.
1, a kind of surface modification of resin new material; It is characterized in that: the surperficial key and a kind of Bian chloro-methyl group that are included in the SDVB polymerization; As; Through step chemical bonding mode; Control different functional groups ratio is 100: 1-1: 100; Average grain diameter differ+/-20% in, proportion differ+/-20% in;
2, surface modification of resin new material according to claim 1; It is characterized in that: with the 1 said resin-based ball that contains the Bian chloro-methyl group; In the system of disperseing and existing is arranged, carry out affine substitution reaction with the a-pyrrolidones, obtain containing the modified new-material of pyrrolidone group.
3, resin surface modification of resin new material according to claim 2 is characterized in that: described resin-coated type silica gel new material, and particle diameter is 30-60 μ m, average pore size is 5-10nm.
4, surface modification of resin new material according to claim 1 is characterized in that: described alkene is CH
3OCH
2Cl, CH
2ClOCl
5, be the a-pyrrolidones according to the said described modified feedstock of claim 2.
6, the solid-phase extraction column processed of the described resin-coated silica gel of claim 2 new packing; It is characterized in that: column jecket inside is carried and is filled new type resin coating silica filler; The filler two ends are sealed by sieve plate; Prevent that mixed fillers from leaking outside; Column jecket one end is sample or solvent inlet; One end is sample or solvent streams outlet, and sample or solvent inject from pillar one end.
7, solid-phase extraction column according to claim 6 is characterized in that: column jecket is a polypropylene plastics, and its volume is the 0.1-100 milliliter.
8, solid-phase extraction column post according to claim 6 is characterized in that: contain 0-100% water in the described flowing phase, when moisture, other composition should can dissolve each other with water; Can contain 0-10mol/L acid, alkali or other buffer salt in the flowing phase; PH is 1-14, and temperature is 5-50 ℃.
The beneficial effect that the present invention had:
1, the present invention all has the good adsorption effect to polarity and non-polar compound, can use eluting solvent widely, has wider range of application;
2, selectivity of the present invention is good, highly versatile, and volume containing the sample is high, the pH value scope of application of broad;
3, filler synthesis step of the present invention is simple, operation easily, good reproducibility.
Description of drawings
Fig. 1 is the solid-phase extraction column sketch map;
Among the figure, 1-1 is medical type PA tube, and 1-2 is sieve plate (the porous polypropylene materials of 20 μ m), and 1-3 is that filler, 1-4 are general-purpose interface.
Fig. 2 is a solid-phase extraction column separation method sketch map;
Among the figure, 2-1 is the post preliminary treatment, and 2-2 is that sample adds, and 2-3 is the post washing, and 2-4 is the analyte wash-out, and 2-5 is an object, and 2-6 is a chaff interference.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1:
The preparation of SDVB polymer
Add running water 450ml in the 1000ml four-hole boiling flask, 10%PVA22.5ml, 40 ℃ are stirred 1h down, are warming up to 60 ℃ again, and it is subsequent use that other joins oil phase.60 ℃ are dropped into down oil phase, leave standstill 10 minutes after, open and stir, the adjustment rotating speed, the diameter (38-75 μ m) of oil droplet is fit to after, be warming up to 80 ℃ with the speed of 1 ℃～2 ℃/min, 80 ± 1 ℃ of insulations 2 hours; Continuation heats up 85 ℃ again, and 85 ± 1 ℃ of insulations continue to heat up 95 ℃ after 4 hours again, and 95 ± 1 ℃ are incubated 4 hours, discharging.
Hot water wash to water is clear, drains, and ethanol extracts three times, screening, and benzinum dress post is carried pore-foaming agent to there not being wax.
Embodiment 2:
The preparation of the SDVB polymer of chloromethylation
Method one:
With the material of preparation in the instance 1 in the 1000ml there-necked flask in carrene swelling 2 hours; Under nitrogen protection, add 14g chloracetyl chloride, 10g AlCl
3, add above-mentioned substance in 40 ℃ of reactions 4 hours, discharging.
Method two:
With the material of preparation in the instance 1 in the 1000ml there-necked flask in N, swelling is 2 hours in the dinethylformamide (DMF); Filtering material, and 500ml chloromethyl ether, 50g zinc (Zn) grain, and reflux 4 hours, discharging.
Embodiment 3:
The preparation of a-pyrrolidones modified phenylethylene divinyl benzene polymers
Material in the instance 2 is swollen in mixed solvent (methyl alcohol: water=5: 5) 2 hours in the 500ml there-necked flask; Add NaOH 1.11g, potash 3.83g, a-pyrrolidones 25.1g then; Stir and begin heating after 10 minutes, and reaction 48 hours under the solvent refluxing condition, be cooled to room temperature, discharging, sand core funnel filters mother liquor, and deionization washing ball is to neutral, and methyl alcohol is given a baby a bath on the third day after its birth time.
After above-mentioned steps finishes, will react the back material and place the 500ml there-necked flask, and in above-mentioned reaction bulb, add 200ml methyl alcohol, then methyl alcohol boiling temperature backflow 6-8 hour, discharging detects, and is for use.
Embodiment 4:
Resin surface modification new material is taken by weighing 500mg, pack band into down in the 6ml column jecket of sieve plate, insert behind the upper sieve plate evenly, use the presser-into-rod compacting with the concussion of vibrations bed.
Embodiment 5:
Pillar is 3 earlier in the instance 4, and respectively with 5ml methyl alcohol, 0.5mol/L H is used in the activation of 5ml water
2SO
4Regulate pH to 1.5～2 of 300mL water sample, flow through pillar, 5mL water wash pillar with the flow velocity of 4～5mL/min; Blow pillar 20min with nitrogen, then with the residual moisture in the 0.9mL methyl alcohol displacement pillar, then with 5mL oxolane wash-out; Nitrogen is concentrated into 1mL, analyzes with HPLC.
Embodiment 6:
Pillar is 3 earlier in the instance 4, and respectively with 5ml methyl alcohol, isopropyl alcohol concentration to 10% is added in the activation of 5ml water in the 300mL water sample, flows through pillar with the flow velocity of 4～5mL/min.Owing to polycyclic aromatic hydrocarbon can be lost by the absorption of container and pipeline,, go up then kind to post so deposit the container bottle and the transfer pipeline of water sample with 50% the isopropanol water solution rinse of 10mL.5mL water wash pillar.Blow pillar 20min with nitrogen, with the residual moisture in the 0.9mL methyl alcohol displacement pillar, then use 5mL methyl alcohol: carrene (3: 7) mixed liquor wash-out then; Nitrogen is concentrated into 1mL, analyzes with HPLC.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (8)
1. surface modification of resin new material; It is characterized in that: the surperficial key and a kind of Bian chloro-methyl group that are included in the SDVB polymerization; As; Through step chemical bonding mode; Control different functional groups ratio is 100: 1-1: 100; Average grain diameter differ+/-20% in, proportion differ+/-20% in;
2. surface modification of resin new material according to claim 1; It is characterized in that: with the 1 said resin-based ball that contains the Bian chloro-methyl group; In the system of disperseing and existing is arranged, carry out affine substitution reaction with the a-pyrrolidones, obtain containing the modified new-material of pyrrolidone group.
3. resin surface modification of resin new material according to claim 2 is characterized in that: described resin-coated type silica gel new material, and particle diameter is 30-60 μ m, average pore size is 5-10nm.
4. surface modification of resin new material according to claim 1 is characterized in that: described alkene is CH
3OCH
2Cl, CH
2ClOCl
5. be the a-pyrrolidones according to the said described modified feedstock of claim 2.
6. the solid-phase extraction column processed of the described resin-coated silica gel of claim 2 new packing; It is characterized in that: column jecket inside is carried and is filled new type resin coating silica filler; The filler two ends are sealed by sieve plate; Prevent that mixed fillers from leaking outside; Column jecket one end is sample or solvent inlet; One end is sample or solvent streams outlet, and sample or solvent inject from pillar one end.
7. solid-phase extraction column according to claim 6 is characterized in that: column jecket is a polypropylene plastics, and its volume is the 0.1-100 milliliter.
8. solid-phase extraction column according to claim 6 is characterized in that: contain 0-100% water in the described flowing phase, when moisture, other composition should can dissolve each other with water; Can contain 0-10mol/L acid, alkali or other buffer salt in the flowing phase; PH is 1-14, and temperature is 5-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110147850A CN102302928A (en) | 2011-06-03 | 2011-06-03 | New resin surface modified material and solid-phase extraction column thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110147850A CN102302928A (en) | 2011-06-03 | 2011-06-03 | New resin surface modified material and solid-phase extraction column thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102302928A true CN102302928A (en) | 2012-01-04 |
Family
ID=45376897
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110147850A Pending CN102302928A (en) | 2011-06-03 | 2011-06-03 | New resin surface modified material and solid-phase extraction column thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102302928A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437438A (en) * | 2014-12-18 | 2015-03-25 | 天津博纳艾杰尔科技有限公司 | Resin surface modified chromatographic packing, preparation method thereof and solid-phase extraction column |
| CN104475049A (en) * | 2014-11-07 | 2015-04-01 | 安徽瑞研新材料技术研究院有限公司 | Alkene-silica gel bonded new material and processing method thereof |
| CN105268406A (en) * | 2015-09-09 | 2016-01-27 | 上海出入境检验检疫局工业品与原材料检测技术中心 | Isocyanate solid phase extraction column and preparation method and application thereof |
| CN105547523A (en) * | 2014-10-29 | 2016-05-04 | 上海辰竹仪表有限公司 | Functional safety type HART measuring system |
-
2011
- 2011-06-03 CN CN201110147850A patent/CN102302928A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105547523A (en) * | 2014-10-29 | 2016-05-04 | 上海辰竹仪表有限公司 | Functional safety type HART measuring system |
| CN104475049A (en) * | 2014-11-07 | 2015-04-01 | 安徽瑞研新材料技术研究院有限公司 | Alkene-silica gel bonded new material and processing method thereof |
| CN104437438A (en) * | 2014-12-18 | 2015-03-25 | 天津博纳艾杰尔科技有限公司 | Resin surface modified chromatographic packing, preparation method thereof and solid-phase extraction column |
| CN105268406A (en) * | 2015-09-09 | 2016-01-27 | 上海出入境检验检疫局工业品与原材料检测技术中心 | Isocyanate solid phase extraction column and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104231166B (en) | A kind of preparation method of bionical artemisinin molecularly imprinted composite membrane | |
| CN102350327A (en) | Novel hydrophilic C18 filling material and its solid phase extraction column | |
| Wei et al. | Poly (styrenesulfonic acid)-impregnated alginate capsule for the selective sorption of Pd (II) from a Pt (IV)-Pd (II) binary solution | |
| Maya et al. | Emerging materials for sample preparation | |
| CN102974324A (en) | Strong-polarity macroporous adsorption resin | |
| CN105611996A (en) | Sorbens for binding metals and production thereof | |
| CN103048400A (en) | Solid-phase extraction column and preparation method thereof | |
| JP2004325425A (en) | Method of manufacturing standard powder sample of in-water fulvic acid | |
| CN104558409A (en) | Surface molecular imprinting polymer made from nanoflower material, and preparation and application of surface molecular imprinting polymer | |
| CN105675759A (en) | Separation and detection method of BPA (bisphenol A) | |
| CN102302928A (en) | New resin surface modified material and solid-phase extraction column thereof | |
| CN102085490A (en) | Solid-phase extraction mixed filler and solid-phase extraction column | |
| CN102516679A (en) | Magnetic microsphere resin with high specific surface area and preparation method and application thereof | |
| CN108970589B (en) | Hydrotalcite-based composite gel ball and preparation method and application thereof | |
| Wang et al. | Continuous fixed bed adsorption of Cu (II) by halloysite nanotube–alginate hybrid beads: an experimental and modelling study | |
| Chai et al. | In-suit ion-imprinted bio-sorbent with superior adsorption performance for gallium (III) capture | |
| CN101880355A (en) | Preparation and application of Sudan red I molecular imprinted polymeric adsorbent | |
| CN107652377A (en) | The preparation method of the chelating resin of polyfunctional group modification | |
| Coşkun | Removal of cationic dye from aqueous solution by adsorption onto crosslinked poly (4-vinylpyridine/crotonic acid) and its N-oxide derivative | |
| CN112705179A (en) | Hierarchical different-pore covalent organic framework material and preparation method and application thereof | |
| CN101898937B (en) | Method for adsorbing and recycling phenol in wastewater by polyamine macroporous resin | |
| Sun et al. | Adsorption behavior of benzenesulfonic acid by novel weakly basic anion exchange resins | |
| CN104437438B (en) | Surface modification of resin chromatograph packing material and preparation method thereof and solid-phase extraction column | |
| CN102172516B (en) | Novel resin-coated silica-gel adsorption material | |
| Ma et al. | Functionally modified cross-linked molecularly imprinted resins: separation and purification of camptothecin and its theoretical study |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120104 |