CN103611501A - Preparation method of polypropylene film micro-solid phase extraction bag based on ZIF-8 adsorbent - Google Patents
Preparation method of polypropylene film micro-solid phase extraction bag based on ZIF-8 adsorbent Download PDFInfo
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Abstract
The invention relates to a preparation method of a polypropylene film micro-solid phase extraction bag based on a ZIF-8 adsorbent. The preparation method comprises the specific steps of preparing a ZIF-8 porous adsorption material by a hydrothermal method, fully washing, purifying and activating, and packaging in a polypropylene fiber film by a hot pressing and sealing method to manufacture a novel micro-solid phase extraction device. The preparation method has the advantages of simple process and easiness in operation. Adsorption experiments prove that the ZIF-8 porous adsorbent prepared by the preparation method provided by the invention has the advantages of regular structure and large pore volume, and the micro-solid phase extraction bag has good adsorption performance. In the method, a film material for preparing the extraction bag has no limitation, and any organic film material can be adopted according to research needs and actual applications.
Description
Technical field
The present invention relates to a kind of preparation of micro-solid-phase extraction device, this device is the porous polypropylene membrane extraction bag that is packaged with novel absorption material ZIF-8, this extraction bag adopts thermosealed mode to encapsulate, and develops a kind of novel fast simple micro-SPE method with this.
Background technology
ZIF-8 is the rigid backbone porous adsorbing material with special cage structure that a class is formed by self assembly effect by metal ion and organic ligand.The well-regulated pore passage structure of ZIF-8 tool, (BET specific area is up to 2000m for the specific area of super large
2/ g), the remarkable advantages such as good heat endurance and solvent stability, therefore, have been widely used in sample adsorbing domain.The present invention adopts this novel porous adsorbing material of ZIF-8 as adsorbent, prepares micro-solid-phase extraction device.
Micro-solid phase extraction techniques is a kind of Sample Pretreatment Technique Used, and this method has that to consume solvent few, highly sensitive, the advantage such as easily is automated.Traditional SPE method mainly contains following three kinds of extraction patterns, the first is to adopt the autonomous solid-phase extraction column of loading of commercialization or laboratory to extract, the second is to adopt commercial solid-phase micro-extraction fibre to extract, and the third is Dispersive solid phase extraction.
Adopt solid-phase extraction column to carry out sample extraction, sorbing material need to be loaded in plastics or glass column, the filler of conventional solid-phase extraction column mainly comprises silica type filler, alundum (Al2O3) filler, Fo Luoli tripoli-magnesium silicate filler etc.When determining adsorption, sample solution need to be poured in solid-phase extraction column and adsorb, after sample solution drains off completely, then adopt the component that a large amount of organic solvents adsorbs adsorbent to carry out wash-out.Therefore, this SPE method not only use amount of adsorbent is large, and in extraction process, needs to consume a large amount of organic solvents, is not a kind of green, the analytical method of environmental protection.Meanwhile, because the liquid rate of outflow is slower, the method is also more consuming time.
Existing commercialization solid-phase micro-extracting device mainly scribbles the fixedly vitreous silica fibre abstraction head of phase by handle and surface and forms, and vitreous silica fiber is hidden in syringe needle conventionally, can promote injector push rod quartz fibre is stretched out in syringe needle while needing.This extracting head is all that fixing phase coating is coated with and is steeped on quartz fibre as extracting fiber, these fixedly phase coating mainly comprise dimethyl silicone polymer, polyacrylate, carbon molecular sieve/vinyl benzene or carbon molecular sieve/molecular template resin, polyethylene glycol/dimethyl silicone polymer.But this type coating is all, by photocuring or heating means, high polymer is fixed on to quartz fibre surface, so mechanical strength and heat endurance are all poor.Vitreous silica fibre abstraction head stretches out and retracts in the syringe needle of being everlasting, and coating easy fracture is peeled off, and quartz fibre frangibility, and this has greatly limited the scope of application and the life-span of extracting head.In addition, commercial solid-phase micro-extraction fibre is more expensive, the price of a fiber conventionally hundreds of to several thousand yuan not etc., use cost is higher.
Dispersive solid phase extraction is directly adsorbent to be immersed in sample solution to be determined, extracts enrichment component to be detected by adsorbent.After adsorption process finishes, adopt centrifugal mode that solid absorbent is separated with sample solution, adopt again subsequently the component that the solvent of particular polarity adsorbs adsorbent to carry out wash-out, and measure.The method does not need preparation or builds any extraction equipment, but in once complete extraction process, need to be through repeatedly centrifugal, and need by mode ultrasonic or concussion, solid absorbent to be disperseed again after each centrifugal, therefore in actual mechanical process, extremely waste time and energy.
The object of the invention is to overcome above shortcomings in existing method and technology, a kind of novel micro-solid-phase extraction device is provided, and the preparation method of this micro-solid-phase extraction device is provided.Therefore,, by invention and the use of this device, both can effectively simplify the preparation process of extraction equipment, in extraction process, effectively reduce the use amount of organic solvent, reduce and pollute, can reach time saving and energy saving, realize the object that the rapid analysis of sample is measured simultaneously.
Summary of the invention
For realizing technical scheme provided by the present invention, be:
With hydro-thermal method, prepare ZIF-8 porous adsorbing material, through washing fully, purify, after activation, adopt the method for hot pressing envelope, be packaged in polypropylene fibre film, be made into novel micro-solid-phase extraction device.
Through adsorption experiment, show, this method is prepared ZIF-8 porous adsorbent tactical rule, and pore capacities is large, and micro-SPE bag absorption property is good.
Wherein, the hydrothermal synthesis method of porous adsorbing material ZIF-8 is: by 0.210 gram of zinc nitrate, 0.060 gram of glyoxal ethyline is dissolved in 18 milliliters of N, in dinethylformamide, after within ultrasonic 10 minutes, making it dissolve, mixed solution is placed in to 20 milliliters of polytetrafluoroethylene (PTFE) reactors, and 140 ℃ are reacted 24 hours.Question response still is cooling, adopts water/ethanolic solution to wash resulting metallic organic framework sorbing material, 200 ℃ of dry for standby.
The preparation method of porous polypropylene membrane extraction bag: porous polypropylene film is converted into suitable size, cuts redundance, adopt electric sealing machine by the opening heat-sealing of porous polypropylene film, only surplus next opening, for loading ZIF-8 porous adsorbent.
The preparation of the polypropylene screen extraction bag based on ZIF-8 sorbing material: take appropriate metallic organic framework sorbing material, and loaded in porous polypropylene extraction bag, after filling finishes, adopt electric sealing machine by the openend heat seal of porous polypropylene extraction bag.
The using method of ZIF-8 polypropylene screen extraction bag: in advance above-mentioned extraction bag is cleaned with the solvent (as methyl alcohol, water, n-hexane etc.) of particular polarity before use, and dried.When carrying out micro-SPE experiment, this extraction bag is directly soaked in sample solution to be detected, sample solution is carried out to mechanical agitation simultaneously, the metallic organic framework adsorbent in extraction bag can be contacted fully with sample solution, realize the absorption to target components to be measured.After adsorption process finishes, will extract tweezers for bag and take out, with filter paper, surperficial liquid be blotted, be then soaked in the solvent of some milliliters (as methyl alcohol, water, n-hexane etc.), object will be carried out to wash-out.Eluent can directly be measured (gas chromatography, liquid chromatography, spectra methods etc.), determines the content of target components.
Not only manufacturing process is simple to adopt the prepared SPME bag of method of the present invention, making and use cost are minimized, and in the process of using, also need not centrifuge, the expensive experiment equipment such as vortex mixed instrument, oscillator, the quantity of solvent that sorption and desorption process consumes is less, therefore, both can save certain equipment cost, time cost and human cost, also can reduce the pollution of experimental waste liquid to environment simultaneously.
The specific embodiment
For better understanding the present invention, below in conjunction with embodiment, the present invention is done further and described in detail, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment:
The ZIF-8 porous adsorbing material of preparing with hydro-thermal method, the method that adopts hot pressing to seal, is packaged in polypropylene fibre film, is made into novel micro-solid-phase extraction device:
The hydrothermal synthesis method of porous adsorbing material ZIF-8 is: by 0.210 gram of zinc nitrate, 0.060 gram of glyoxal ethyline is dissolved in 18 milliliters of DMFs, after within ultrasonic 10 minutes, making it dissolve, mixed solution is placed in to 20 milliliters of polytetrafluoroethylene (PTFE) reactors, and 140 ℃ are reacted 24 hours.Question response still is cooling, adopts water/ethanolic solution to wash resulting metallic organic framework sorbing material, 200 ℃ of dry for standby.
Porous polypropylene film is converted into suitable size, and cuts redundance.Adopt electric sealing machine that the opening of porous polypropylene film is heat-sealing to only surplus next opening.Take ZIF-8 porous adsorbing material prepared by 0.5mg hydro-thermal method, and loaded in polypropylene screen " pocket ", and openend is adopted to use the same method and carry out heat seal, obtained the micro-SPE bag of a kind of novel polypropylene screen based on ZIF-8 adsorbent.
Claims (4)
1. a ZIF-8 adsorbent, it is characterized in that: it is the white solid particle that adopts hydro-thermal method to prepare, and this solid particle needs first with distilled water, repeatedly clean, to remove unreacted slaine, with ethanol, repeatedly clean again, remove unreacted glyoxal ethyline.
2. a ZIF-8 adsorbent for high-specific surface area, good adsorption characteristic, is characterized in that: ZIF-8 adsorbent claimed in claim 1 is impregnated in hot ethanol solution, and stirred for several hour, ultrasonic a few hours, centrifugal afterwards, 200 ℃ of high-temperature roasting a few hours.
3. the purification method of the ZIF-8 adsorbent of high-specific surface area according to claim 2, good adsorption characteristic, is characterized in that: described ultrasonic step is that low energy is ultrasonic.
4. the SPE bag of ZIF-8 absorbent preparation according to claim 2, is characterized in that: described membrane material is without any restrictions, can be according to actual needs and application select any organic film material.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877942A (en) * | 2014-03-31 | 2014-06-25 | 中国石油大学(华东) | Micro solid phase extraction probe made by MIL-101 type metal organic framework (MOF) material and preparation method of probe |
| CN104324694A (en) * | 2014-11-11 | 2015-02-04 | 天津工业大学 | Novel preparation and application method of water treatment thin film doped with SOD zeolite configuration composite material |
| CN105363413A (en) * | 2014-08-22 | 2016-03-02 | 中国科学院生态环境研究中心 | Multidimensional mesoporous metal organic frameworks adsorbent and application thereof |
| CN108241027A (en) * | 2016-12-26 | 2018-07-03 | 昆明学院 | The assay method of chlorobenzene compound in environmental water sample |
| CN108311125A (en) * | 2018-01-26 | 2018-07-24 | 南京理工大学 | Solid-phase micro-extraction coating and preparation method thereof based on hollow carbon nanomaterial |
| CN110813265A (en) * | 2019-10-21 | 2020-02-21 | 宁夏大学 | Preparation method and application of β -CD/ZIF-8/PMMA composite cationic dye solid-phase extraction adsorbent |
| CN111841074A (en) * | 2020-07-29 | 2020-10-30 | 杭州职业技术学院 | Porous membrane protection nano material solid phase micro-extraction device and application thereof |
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2013
- 2013-12-06 CN CN201310673612.2A patent/CN103611501A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877942A (en) * | 2014-03-31 | 2014-06-25 | 中国石油大学(华东) | Micro solid phase extraction probe made by MIL-101 type metal organic framework (MOF) material and preparation method of probe |
| CN103877942B (en) * | 2014-03-31 | 2016-06-01 | 中国石油大学(华东) | The micro-Solid-Phase Extraction probe of MIL-101 type MOF material and preparation method |
| CN105363413A (en) * | 2014-08-22 | 2016-03-02 | 中国科学院生态环境研究中心 | Multidimensional mesoporous metal organic frameworks adsorbent and application thereof |
| CN105363413B (en) * | 2014-08-22 | 2018-12-04 | 中国科学院生态环境研究中心 | A kind of multidimensional mesoporous metal organic framework sorbent and its application |
| CN104324694A (en) * | 2014-11-11 | 2015-02-04 | 天津工业大学 | Novel preparation and application method of water treatment thin film doped with SOD zeolite configuration composite material |
| CN108241027A (en) * | 2016-12-26 | 2018-07-03 | 昆明学院 | The assay method of chlorobenzene compound in environmental water sample |
| CN108311125A (en) * | 2018-01-26 | 2018-07-24 | 南京理工大学 | Solid-phase micro-extraction coating and preparation method thereof based on hollow carbon nanomaterial |
| CN108311125B (en) * | 2018-01-26 | 2020-09-18 | 南京理工大学 | Solid phase micro-extraction coating based on hollow carbon nano material and preparation method thereof |
| CN110813265A (en) * | 2019-10-21 | 2020-02-21 | 宁夏大学 | Preparation method and application of β -CD/ZIF-8/PMMA composite cationic dye solid-phase extraction adsorbent |
| CN110813265B (en) * | 2019-10-21 | 2022-05-31 | 宁夏大学 | Preparation method and application of beta-CD/ZIF-8/PMMA composite cationic dye solid-phase extraction adsorbent |
| CN111841074A (en) * | 2020-07-29 | 2020-10-30 | 杭州职业技术学院 | Porous membrane protection nano material solid phase micro-extraction device and application thereof |
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Application publication date: 20140305 |