CN103599764A - Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent - Google Patents
Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent Download PDFInfo
- Publication number
- CN103599764A CN103599764A CN201310601422.XA CN201310601422A CN103599764A CN 103599764 A CN103599764 A CN 103599764A CN 201310601422 A CN201310601422 A CN 201310601422A CN 103599764 A CN103599764 A CN 103599764A
- Authority
- CN
- China
- Prior art keywords
- zif
- adsorbent
- bag
- spe
- woven fabric
- 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
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a non-woven fabric micro solid phase extraction (SPE) bag based on a ZIF-8 adsorbent. In particular, a ZIF-8 porous adsorbing material is prepared by a hydrothermal method and is packaged in a non-woven fabric bag by adopting a heat bonding method after being fully washed, purified and activated to prepare a novel micro SPE device. The method is simple in process and easy to operate. Adsorption experiments show that the ZIF-8 porous adsorbent prepared by the method has a regular structure and high pore capacity, and the micro SPE bag has good adsorption performance. According to the method, the non-woven fabric materials for preparing the extraction bag are unlimited and can adopt non-woven fabrics modified by any group according to the research needs and practical application.
Description
Technical field
The present invention relates to a kind of preparation of micro-SPE bag, this device is the perforated nonwoven fabrics bag for extracting that is packaged with novel absorption material ZIF-8, this bag for extracting adopts the mode of heat bonding 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-SPE bag.
Nonwoven, refers to non-weaving cloth, or is adhesive-bonded fabric.Be a kind of fabric that does not need to spin cotton and weave cloth and form, this fabric just carries out orientation or random support row by textile staple or long filament, forms fibre net structure, then adopts the method reinforcing such as mechanical, hot sticky or chemical to form.Non-weaving cloth has been broken through traditional weaving principle, have that technological process is short, speed of production is fast, the features such as output is high, cost is low, purposes is wide, raw material sources are many, therefore, in recent years, nonwoven textile industry has obtained great development, ends 1998, and global nonwoven consumption figure has reached 2,400,000 tons.
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 heat bonding, be packaged in nonwoven bag for extracting, 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 perforated nonwoven fabrics bag for extracting: perforated nonwoven fabrics is converted into suitable size, cuts redundance, adopt electric sealing machine by the opening heat-sealing of perforated nonwoven fabrics, only surplus next opening, for loading ZIF-8 porous adsorbent.
The preparation of the nonwoven bag for extracting based on ZIF-8 sorbing material: take appropriate metallic organic framework sorbing material, and loaded in perforated nonwoven fabrics bag for extracting, after filling finishes, adopt electric sealing machine by the openend heat bonding of perforated nonwoven fabrics bag for extracting.
The using method of ZIF-8 nonwoven bag for extracting: in advance above-mentioned bag for extracting 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 bag for extracting is directly soaked in sample solution to be detected, sample solution is carried out to mechanical agitation simultaneously, the metallic organic framework adsorbent in bag for extracting can be contacted fully with sample solution, realize the absorption to target components to be measured.After adsorption process finishes, bag for extracting is taken out with tweezers, with filter paper, surperficial liquid is blotted, be then soaked in the solvent of some milliliters (as methyl alcohol, water, n-hexane etc.), object is 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, nonwoven cloth material for the preparation of bag for extracting is without any restrictions, therefore, can adopt the nonwoven through any base group modification or modification according to research needs and practical application, and by similar method, can prepare micro-SPE bag that other non-woven bags cover ZIF-8 adsorbent.
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 for employing heat bonding, is packaged in nonwoven bag for extracting, 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.
Perforated nonwoven fabrics is converted into suitable size, and cuts redundance.Adopt electric sealing machine that the opening of perforated nonwoven fabrics is thermally bonded to only surplus next opening.Take ZIF-8 porous adsorbing material prepared by 0.5mg hydro-thermal method, and loaded in nonwoven " pocket ", and openend is adopted to use the same method and carry out heat bonding, obtained the micro-SPE bag of a kind of novel nonwoven 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 nonwoven cloth material is without any restrictions, can be according to actual needs and application select the nonwoven through any base group modification or modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310601422.XA CN103599764A (en) | 2013-11-20 | 2013-11-20 | Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310601422.XA CN103599764A (en) | 2013-11-20 | 2013-11-20 | Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103599764A true CN103599764A (en) | 2014-02-26 |
Family
ID=50118063
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310601422.XA Pending CN103599764A (en) | 2013-11-20 | 2013-11-20 | Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103599764A (en) |
Cited By (4)
| 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 |
| US9421517B2 (en) | 2015-01-20 | 2016-08-23 | Chung Yuan Christian University | Metal-organic framework polymer for solid-phase microextraction |
| 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 |
-
2013
- 2013-11-20 CN CN201310601422.XA patent/CN103599764A/en active Pending
Cited By (5)
| 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 |
| 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 |
| US9421517B2 (en) | 2015-01-20 | 2016-08-23 | Chung Yuan Christian University | Metal-organic framework polymer for solid-phase microextraction |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103551131A (en) | Preparation method of polypropylene film micro solid-phase extraction packet based on MIL-101 adsorbent | |
| CN103611501A (en) | Preparation method of polypropylene film micro-solid phase extraction bag based on ZIF-8 adsorbent | |
| CN101864021B (en) | Preparation method of nanometer silicon gel surface gastrodin molecular engram polymers | |
| CN1928527B (en) | Functional nano-fiber based method for extracting and enriching pollutants in water | |
| CN103599764A (en) | Preparation method of non-woven fabric micro solid phase extraction (SPE) bag based on ZIF-8 adsorbent | |
| CN101706481B (en) | Novel capillary gas chromatographic column based on MOFs and preparation method thereof | |
| CN105148880A (en) | Preparation method and application method for graphene microsphere solid-phase extractant | |
| CN103611510A (en) | Preparation method of non-woven fabric micro-solid phase extraction bag based on MIL-101 adsorbent | |
| CN102532390A (en) | Triazine weedicide, and metabolite molecular engram polymer microspheres, preparation method and application thereof | |
| CN101149359B (en) | Solid phase micro-extraction probe and its analysis method for polycyclic aromatic hydrocarbon of environmental sample | |
| CN105268414B (en) | A kind of solid-phase micro-extraction fibre and preparation method thereof and purposes | |
| CN105974001A (en) | Method for pretreating soil or sediment sample and method for determining dioxin | |
| CN102735500A (en) | Passive sampling technology aiming at anionic polar organic pollutant in water | |
| CN104083904A (en) | Functionalized porous zinc sulfide nano microsphere solid-phase extraction column and preparation method thereof | |
| CN104725190A (en) | Method for using metal-organic skeleton for adsorption and separating of polyol in aqueous solution | |
| Chu et al. | Adsorption/desorption performance of volatile organic compounds on electrospun nanofibers | |
| CN102617813B (en) | Preparation and application of sephadex surface apigenin molecular engram sorbing material | |
| CN103611502A (en) | Preparation method of non-woven fabric petroleum adsorption bag coated with ZIF-8 adsorbent | |
| CN103599752A (en) | Preparation method of non-woven fabric petroleum adsorption bag coated with MIL-101 adsorbent | |
| CN204017444U (en) | A kind of efficient magnetic control disperses solid-phase extraction device | |
| CN105561958B (en) | A kind of ionic liquid bonded silica for saxitoxin enriching and purifying and preparation method thereof | |
| CN105618015B (en) | A kind of preparation of three-dimensional meso-hole carbon composite and its application as solid phase micro-extraction fabric coating material | |
| CN103091150A (en) | Multifunctional needle type filter | |
| CN104353441B (en) | A kind of ion blotting material for enrichment water body ultra trace methyl mercury | |
| CN108855019A (en) | A kind of preparation method and application of float type dispersive solid-phase extraction adsorbent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140226 |
|
| WD01 | Invention patent application deemed withdrawn after publication |