CN103551131A - Preparation method of polypropylene film micro solid-phase extraction packet based on MIL-101 adsorbent - Google Patents
Preparation method of polypropylene film micro solid-phase extraction packet based on MIL-101 adsorbent Download PDFInfo
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Abstract
The invention relates to a preparation method of a polypropylene film micro solid-phase extraction packet based on an MIL-101 adsorbent. The method specifically comprises the following steps: preparing an MIL-101 porous adsorbing material by using a hydrothermal method, sufficiently washing, purifying and activating, packaging in a polypropylene fiber film through a hot-pressing mode to manufacture a novel micro solid-phase extraction device. The method is simple in process and easy to operate. The adsorption test shows that the MIL-101 porous adsorbing material prepared by the method is regular in structure and large in pore capacity, and the micro solid-phase extraction packet has good adsorptive property. According to the method, the film materials for preparing the extraction packet are not restricted, and any organic film material can be adopted according to research needs and actual application.
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 MIL-101, this extraction bag adopts thermosealed mode to encapsulate, and develops a kind of novel fast simple micro-SPE method with this.
Background technology
MIL-101 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 MIL-101 tool, (BET specific area is up to 4500m 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 MIL-101 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 MIL-101 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 MIL-101 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 MIL-101 is: by 0.325 gram of chromic nitrate, 0.410 gram of terephthalic acid (TPA) is dissolved in 20 milliliters of high purity waters, add 1 milliliter of hydrofluoric acid solution, after within ultrasonic 10 minutes, making it dissolve, mixed solution is placed in to 35 milliliters of polytetrafluoroethylene (PTFE) reactors, and 220 ℃ are reacted 8 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 MIL-101 porous adsorbent.
The preparation of the polypropylene screen extraction bag based on MIL-101 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 MIL-101 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.
In the present invention, without any restrictions for the preparation of the membrane material of extraction bag, therefore, according to actual needs and application select any organic film material, by similar method, can prepare micro-SPE bag of the coated MIL-101 adsorbent of other membrane materials.
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 MIL-101 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 MIL-101 is: by 0.325 gram of chromic nitrate, 0.410 gram of terephthalic acid (TPA) is dissolved in 20 milliliters of high purity waters, add 1 milliliter of hydrofluoric acid solution, after within ultrasonic 10 minutes, making it dissolve, mixed solution is placed in to 35 milliliters of polytetrafluoroethylene (PTFE) reactors, and 220 ℃ are reacted 8 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 MIL-101 porous adsorbing material prepared by 0.5mg hydro-thermal method, and loaded and polypropylene screen " pocket " in, 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 MIL-101 adsorbent.
Claims (4)
1. a MIL-101 adsorbent, it is characterized in that: it is the green 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 terephthalic acid (TPA).
2. a MIL-101 adsorbent for high-specific surface area, good adsorption characteristic, is characterized in that: MIL-101 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 MIL-101 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 MIL-101 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 (8)
| 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 |
| CN104043397A (en) * | 2014-03-31 | 2014-09-17 | 中国石油大学(华东) | MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof |
| CN104324696A (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 mesoporous composite material |
| CN104475028A (en) * | 2014-11-11 | 2015-04-01 | 天津工业大学 | Novel preparation and application methods of water treatment film doped with one-dimensional-pore-passage-structured composite material |
| CN104475026A (en) * | 2014-11-12 | 2015-04-01 | 天津工业大学 | Novel preparation and application methods of water treatment film doped with MTN-zeolite-configuration composite material |
| CN112083101A (en) * | 2020-09-14 | 2020-12-15 | 江南大学 | Needle type filter solid phase extraction device for metal organic framework filler |
| CN112354520A (en) * | 2020-11-05 | 2021-02-12 | 南宁兴科净医疗科技有限公司 | Preparation method and application of solid-phase microextraction coating |
| CN115508475A (en) * | 2022-11-01 | 2022-12-23 | 未名环境分子诊断(广东)有限公司 | Method for detecting content of diphenoxylate in sewage |
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2013
- 2013-11-20 CN CN201310601164.5A patent/CN103551131A/en active Pending
Cited By (9)
| 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 |
| CN104043397A (en) * | 2014-03-31 | 2014-09-17 | 中国石油大学(华东) | MIL-53 needle tube-type solid phase microextraction probe and preparation method thereof |
| 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 |
| CN104324696A (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 mesoporous composite material |
| CN104475028A (en) * | 2014-11-11 | 2015-04-01 | 天津工业大学 | Novel preparation and application methods of water treatment film doped with one-dimensional-pore-passage-structured composite material |
| CN104475026A (en) * | 2014-11-12 | 2015-04-01 | 天津工业大学 | Novel preparation and application methods of water treatment film doped with MTN-zeolite-configuration composite material |
| CN112083101A (en) * | 2020-09-14 | 2020-12-15 | 江南大学 | Needle type filter solid phase extraction device for metal organic framework filler |
| CN112354520A (en) * | 2020-11-05 | 2021-02-12 | 南宁兴科净医疗科技有限公司 | Preparation method and application of solid-phase microextraction coating |
| CN115508475A (en) * | 2022-11-01 | 2022-12-23 | 未名环境分子诊断(广东)有限公司 | Method for detecting content of diphenoxylate in sewage |
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Application publication date: 20140205 |