CN101992069A - Preparation method of metal carrier Tenax coating stirring and extracting rod - Google Patents
Preparation method of metal carrier Tenax coating stirring and extracting rod Download PDFInfo
- Publication number
- CN101992069A CN101992069A CN 201010270649 CN201010270649A CN101992069A CN 101992069 A CN101992069 A CN 101992069A CN 201010270649 CN201010270649 CN 201010270649 CN 201010270649 A CN201010270649 A CN 201010270649A CN 101992069 A CN101992069 A CN 101992069A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- coating
- metal
- extraction
- stirring
- 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.)
- Granted
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a metal carrier Tenax coating stirring and extracting rod, which comprises the following steps of: a, selecting and preprocessing a metal rod; b, synthesizing heat-resistant epoxy resin; c, manufacturing a stirring rod coating; d, curing the coating; and e, removing impurities of the extracting rod body, wherein the extracting rod is used in a stirring manner, and the metal is iron, nickel, cobalt, stainless steel or alloy; and when the extracting rod is used in a headspace or ultrasonic manner, the metal is stainless steel, copper, aluminum or alloy. Tenax is fixed on the surface of the metal rod by using the synthesized heat-resistant epoxy resin or organic silicon resin to form a coating material with heat stability and solvent washing resistance, thus the extracting rod realizes the enrichment of trace organic matters. The invention is especially suitable for processing samples of soil, air, essence and spice, indoor air, alcohol, phenol, amine-aldehyde, ketone, aryl halides and the like.
Description
Technical field
The invention belongs to organic trace analysis field in food, environment, the biological sample, the Tenax coating that particularly relates to a kind of metallic carrier stirs the preparation method of extraction bar, and this extraction bar is applicable to the processing to samples such as soil, atmosphere, essence and flavoring agent, room air, alcohol, phenol, amine aldehyde, ketone, halogenated aryl hydrocarbons.
Background technology
Because the matrix of most of analytic sample and composition are quite complicated, sample pre-treatments becomes important step indispensable in the sample analysis under normal conditions.It plays and concentrates tested trace components, the effect of sensitivity of raising method and cleaning sample.
Traditional sample-pretreating method has liquid. liquid extraction, soxhlet extraction, chromatography, distillation, absorption, centrifugal and filtration etc., but these methods generally have and use a large amount of organic solvents, the processing time is long and operating procedure is many shortcoming.These methods are not only lost sample easily, are produced than mistake, and the use of toxic solvent can influence operator ' s health, contaminated environment.For this reason, the research of solvent-free or few solvent, degree of accuracy height, quick, easy sample-pretreating method has become one of forward position research topic of current analytical chemistry.
Solid phase micro-extraction technique is the sample pre-treatments and the beneficiation technologies of a novelty of the rise nineties in 20th century, it developed research by the Pawliszyn professor's of Canadian Waterloo university research group in 1989 at first first, belonged to non-solvent selective extraction method.It almost can be used for the analysis of all kinds of volatility of sample such as gas, liquid, biology, solid or half volatile material.The maximum characteristics of SPME integrate sampling, extraction, enrichment, sample introduction exactly, thereby it is easy and simple to handle, and do not need solvent, rate of extraction is fast, running cost is low, free from environmental pollution, be convenient to realize automation and be easy to efficiently separate the detection means coupling with chromatogram, electrophoresis etc., therefore, in chemistry, medicine, food, environmental area and Pharmaceutical Analysis, obtained using widely.
Stir Bar Sorptive Extraction (Stirbar sorptive extraction, SBSE) propose in 1999 by people such as Erik Baltussen, be in SPME (Solid Phase Micro Extraction, a kind of novel sample pre-treatments technology that SPME) grows up on the basis.This technology is the same with SPME have simple, efficient, fast, favorable reproducibility, green advantage such as solvent-free, and absorption stirring rod self is finished stirring in extraction process, avoided the competitive Adsorption of stirrer in Fiber SPME, and its extraction fixedly the volume ratio SPME of phase is big more than 50 times, therefore the enrichment multiple obviously improves, and is fit to very much trace analysis.This technology successfully is applied to the analysis of pollutant, drugs, medicine and residues of pesticides in environmental sample, the food, human endocrine interfering material, polycyclic aromatic hydrocarbon, benzene series thing and Polychlorinated biphenyls etc. abroad.
Germany Gerstel GnlbH company selects for use PDMS as the extraction coating, has released commercial stirring rod (Twister Gerstel GnlbH).Twister is the PDMS silicone rubber tube by 0.5mm or 1mm, be enclosed within on the glass tube that seals magnetic core in and make. still, commercial SBSE device has only this a kind of fixedly phase coating of PDMS, and commercialization SBSE device price is higher, and the SBSE The Application of Technology has been subjected to bigger restriction.For this reason, be the work that an extremely has novelty and practical significance to the SBSE Study on Technology.
Existing stirring extraction bar is a carrier with the glass bar all, and material is frangible, and the present invention replaces traditional glass bar to make it have higher mechanical strength, sturdy and durable with metal bar.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of extraction bar, this method comprises following steps:
(a) choosing and preliminary treatment of metal bar:
Choose long 10-40mm, diameter is the metal bar of 0.5-5mm, utilizes carrene that preliminary treatment is carried out on its surface;
(b) synthetic high-temperature-resistant epoxy resin:
Take by weighing an amount of epoxy resin, add stirring solvent to dissolving fully, add curing agent, auxiliary agent, filler more successively, stirring is uniformly dispersed each component, get high-temperature-resistant epoxy resin, place below 5 ℃ to store for future use, wherein the weight ratio of epoxy resin, curing agent, auxiliary agent and filler is 20: 3: 3: 4;
(c) making of stirring rod coating:
The high-temperature-resistant epoxy resin or the organic siliconresin of the surface-coated one deck step of the barred body that will handle (b) preparation earlier pick one deck Tenax adsorbent at skin again, can pass through repeating step (c) and adjust coating layer thickness;
(d) curing of coating is handled:
The barred body that is coated with the stain coating is placed and carries out hot setting in the baking oven;
(e) removal of extraction barred body impurity:
With the extraction bar of making, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove the small molecular weight impurity in adsorbent and the epoxy resin.
Wherein, extraction bar is if use metal chosen from Fe, nickel, cobalt, stainless steel or alloy with alr mode; Extraction bar is if use with head space or ultrasonic power, and metal is selected from stainless steel, copper, aluminium or alloy.
Wherein solvent is selected from dimethylbenzene, toluene, benzene or acetone;
Curing agent is a pyromellitic dianhydride;
Auxiliary agent is a tertiary amine.
Filler is selected from flake asbestos, aluminium powder or titanium dioxide.
The Tenax adsorbent is selected from 2,6-dibenzofuran porous polymeric resins or other base polymer coatings.
It is carrier with the metal bar that the Tenax coating of metallic carrier of the present invention stirs extraction bar, utilize synthesizing high temperature epoxy resin or organic siliconresin that Tenax is fixed on the metal bar surface, form Heat stability is good, thus anti-solvent washing coating material realize enrichment to trace organic substance.Barred body self is finished stirring in extraction process, has avoided the competitive Adsorption of stirrer in Fiber SPME; Replace traditional glass bar to make it have higher mechanical strength, sturdy and durable with metal bar; Adsorbent is attached to form on the stirring rod, more helps adsorbent the processing of fluid sample and static head space are captured.Be specially adapted to processing to samples such as soil, atmosphere, essence and flavoring agent, room air, alcohol, phenol, amine aldehyde, ketone, halogenated aryl hydrocarbons.
Description of drawings
Fig. 1 is not for using the gas-chromatography baseline chart that stirs extraction bar
Fig. 2 is the gas-chromatography baseline chart under the stirring extraction bar desorption temperature that uses embodiment 1
Fig. 3 is the stirring extraction bar extraction n-alkane (C that utilizes embodiment 1
10-C
20) gas chromatogram
The specific embodiment
In order to understand the present invention, further specify the present invention with embodiment below, but do not limit the present invention.
Embodiment 1
Choose long 25mm, diameter is the iron staff of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.Take by weighing 100g epoxy resin, add dimethylbenzene and be stirred to dissolving fully, add 15g pyromellitic dianhydride, 15g tertiary amine, 20g flake asbestos more successively, stirring is uniformly dispersed each component.With the surface-coated one deck high-temperature-resistant epoxy resin of the barred body of handling, pick one deck Tenax adsorbent at skin again, barred body is placed in the baking oven in 180 ℃ of hot setting 60min.With the extraction bar of making, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Epoxy resin is multifunctional glycidol type epoxy resin, and market is bought and obtained.The Tenax adsorbent is Tenax TA.
Embodiment 2
Choose long 25mm, diameter is the nickel rod of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.With the surface-coated one deck organic siliconresin of the barred body of handling, pick one deck Tenax adsorbent at skin again, barred body is placed in the baking oven in 180 ℃ of hot setting 60min.With the extraction bar of making, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Embodiment 3
Choose long 25mm, diameter is the stainless steel bar of 2mm, utilizes carrene that preliminary treatment is carried out on its surface.With the surface-coated one deck organic siliconresin of the barred body of handling, pick one deck 2 at skin again, 6-dibenzofuran porous polymeric resins places in the baking oven barred body in 180 ℃ of hot setting 60min.With the extraction bar of making, place in the middle of the cable type extractor according, utilize carrene in 60 ℃ of backflow 40min.
Embodiment 4
Utilize the stirring extraction bar of making among the embodiment 1 that multiring aromatic hydrocarbon substance in the water is analyzed, take to stir the extraction mode, the solvent method desorb.
Embodiment 5
Utilize the stirring extraction bar of making among the embodiment 1 to analyze, take the head space mode to extract, the desorb of thermal desorption method perfume ingredient being fragrant.
Product of the present invention is described by specific embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose, its relevant change does not all break away from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all be regarded as comprising within the scope of the present invention.
Claims (6)
1. the preparation method of an extraction bar, this method comprises following steps:
(a) choosing and preliminary treatment of metal bar:
Choose long 10-40mm, diameter is the metal bar of 0.5-5mm, utilizes carrene that preliminary treatment is carried out on its surface;
(b) synthetic high-temperature-resistant epoxy resin:
Take by weighing an amount of epoxy resin, add stirring solvent to dissolving fully, add curing agent, auxiliary agent, filler more successively, stirring is uniformly dispersed each component, get high-temperature-resistant epoxy resin, place below 5 ℃ to store for future use, wherein the weight ratio of epoxy resin, curing agent, auxiliary agent and filler is 20: 3: 3: 4;
(c) making of stirring rod coating:
The high-temperature-resistant epoxy resin or the organic siliconresin of the surface-coated one deck step of the barred body that will handle (b) preparation earlier pick one deck Tenax adsorbent at skin again, can pass through repeating step (c) and adjust coating layer thickness;
(d) curing of coating is handled:
The barred body that is coated with the stain coating is placed and carries out hot setting in the baking oven;
(e) removal of extraction barred body impurity:
With the extraction bar of making, place in the middle of the cable type extractor according, utilize carrene in 40-80 ℃ of backflow 20-120min, to remove the small molecular weight impurity in adsorbent and the epoxy resin.
2. method according to claim 1, wherein extraction bar is if use metal chosen from Fe, nickel, cobalt, stainless steel or alloy with alr mode; Extraction bar is if use with head space or ultrasonic power, and metal is selected from stainless steel, copper, aluminium or alloy.
3. method according to claim 1, wherein solvent is selected from dimethylbenzene, toluene, benzene or acetone;
4. method according to claim 1, wherein curing agent is a pyromellitic dianhydride;
5. method according to claim 1, wherein filler is selected from flake asbestos, aluminium powder or titanium dioxide.
6. method according to claim 1, wherein the Tenax adsorbent is 2,6-dibenzofuran porous polymeric resins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010270649 CN101992069B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier stirring and extracting rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010270649 CN101992069B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier stirring and extracting rod |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101992069A true CN101992069A (en) | 2011-03-30 |
| CN101992069B CN101992069B (en) | 2012-09-05 |
Family
ID=43783113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010270649 Expired - Fee Related CN101992069B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier stirring and extracting rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101992069B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028381A (en) * | 2013-01-09 | 2013-04-10 | 福州大学 | Solid phase microextraction coating and preparation method thereof |
| CN103949229A (en) * | 2014-02-28 | 2014-07-30 | 武汉大学 | Stainless steel extraction stirring rod and preparation method thereof |
| CN104307498A (en) * | 2014-10-31 | 2015-01-28 | 武汉大学 | Stainless steel extraction stir bar and preparation method thereof |
| CN104475053A (en) * | 2014-11-19 | 2015-04-01 | 武汉大学 | Graphene oxide/polyethylene glycol coating stirring rod, and preparation method and application thereof |
| CN106544613A (en) * | 2016-11-30 | 2017-03-29 | 佛山市高明区诚睿基科技有限公司 | A kind of preparation method of use for laboratory rustless steel stirring rod |
| CN110161150A (en) * | 2019-06-26 | 2019-08-23 | 山东省城市供排水水质监测中心 | GC-MS method based on boiling characteristics organic matter in multi-functional online sample introduction measurement water |
| JP2022028061A (en) * | 2016-02-03 | 2022-02-14 | ゲステル株式会社 | Organic component extraction method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1268667A (en) * | 1999-03-26 | 2000-10-04 | 格斯特尔系统技术两合公司 | Solid state micro-extraction and analysis method, and collecting means therefor |
| CN102068966A (en) * | 2010-09-02 | 2011-05-25 | 天津春发食品配料有限公司 | Metal carrier stirring and extracting rod |
-
2010
- 2010-09-02 CN CN 201010270649 patent/CN101992069B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1268667A (en) * | 1999-03-26 | 2000-10-04 | 格斯特尔系统技术两合公司 | Solid state micro-extraction and analysis method, and collecting means therefor |
| CN102068966A (en) * | 2010-09-02 | 2011-05-25 | 天津春发食品配料有限公司 | Metal carrier stirring and extracting rod |
Non-Patent Citations (2)
| Title |
|---|
| 《ANALYTICAL CHEMISTRY》 20010501 Xia XR,et al. Preparation and characterization of porous silica coated multifibers for solid-phase microextraction 第2042页 1-6 第73卷, 第9期 * |
| 《JOURNAL OF MICROCOLUMN SEPARATIONS》 19991231 Baltussen E,et al. Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: Theory and principles 第740页 1-6 第11卷, 第10期 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028381A (en) * | 2013-01-09 | 2013-04-10 | 福州大学 | Solid phase microextraction coating and preparation method thereof |
| CN103949229A (en) * | 2014-02-28 | 2014-07-30 | 武汉大学 | Stainless steel extraction stirring rod and preparation method thereof |
| CN104307498A (en) * | 2014-10-31 | 2015-01-28 | 武汉大学 | Stainless steel extraction stir bar and preparation method thereof |
| CN104307498B (en) * | 2014-10-31 | 2016-05-11 | 武汉大学 | A kind of stainless steel extraction stirring rod and preparation method thereof |
| CN104475053A (en) * | 2014-11-19 | 2015-04-01 | 武汉大学 | Graphene oxide/polyethylene glycol coating stirring rod, and preparation method and application thereof |
| CN104475053B (en) * | 2014-11-19 | 2016-09-14 | 武汉大学 | Graphene oxide/Polyethylene Glycol coating stirring rod and preparation method and application |
| JP2022028061A (en) * | 2016-02-03 | 2022-02-14 | ゲステル株式会社 | Organic component extraction method |
| JP7253212B2 (en) | 2016-02-03 | 2023-04-06 | ゲステル株式会社 | Organic component extraction method |
| CN106544613A (en) * | 2016-11-30 | 2017-03-29 | 佛山市高明区诚睿基科技有限公司 | A kind of preparation method of use for laboratory rustless steel stirring rod |
| CN106544613B (en) * | 2016-11-30 | 2019-01-22 | 佛山市高明区诚睿基科技有限公司 | A kind of preparation method of use for laboratory stainless steel stirring rod |
| CN110161150A (en) * | 2019-06-26 | 2019-08-23 | 山东省城市供排水水质监测中心 | GC-MS method based on boiling characteristics organic matter in multi-functional online sample introduction measurement water |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101992069B (en) | 2012-09-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101992069B (en) | Preparation method of metal carrier stirring and extracting rod | |
| Paiva et al. | Fundamentals of and recent advances in sorbent-based headspace extractions | |
| Dietz et al. | Recent developments in solid-phase microextraction coatings and related techniques | |
| Chong et al. | Sol− gel coating technology for the preparation of solid-phase microextraction fibers of enhanced thermal stability | |
| Bigham et al. | Sol− gel capillary microextraction | |
| Liu et al. | Solid-phase microextraction of PAHs from aqueous samples using fibers coated with HPLC chemically bonded silica stationary phases | |
| Costa | Newly introduced sample preparation techniques: towards miniaturization | |
| Li et al. | Preparation of C18 composite solid-phase microextraction fiber and its application to the determination of organochlorine pesticides in water samples | |
| Yun | High extraction efficiency solid-phase microextraction fibers coated with open crown ether stationary phase using sol–gel technique | |
| CN101992072A (en) | Aluminum oxide coating stirring extraction rod of metal carrier | |
| Abboud et al. | Calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction combined with gas chromatography-flame ionization detection for the determination of polycyclic aromatic hydrocarbons in water samples | |
| Nolvachai et al. | Miniaturized molecularly imprinted polymer extraction method for the gas chromatographic analysis of flavonoids | |
| CN102068966A (en) | Metal carrier stirring and extracting rod | |
| CN102366721A (en) | Stirring and extracting bar for polydimethylsiloxane compounded carbon molecular sieve coating | |
| CN101992070B (en) | Preparation method of metal carrier extracting rod | |
| CN102008944A (en) | Stirring and extracting bar for beta-cyclodextrin matrix | |
| CN101992073A (en) | Metal carrier Tenax coating solid-phase microextraction fiber | |
| CN101992062B (en) | Method for preparing metal carrier stirring extraction rod | |
| CN102068963B (en) | Stainless steel solid phase micro extraction fiber | |
| CN102049244A (en) | Method for preparing Beta-cyclodextrin matrix stir extraction bar | |
| CN101972635B (en) | Preparation method of stir and extraction bar for polymer coating | |
| CN101942762A (en) | Metal carrier solid phase micro-extraction fiber | |
| CN102114417A (en) | Preparation method of stainless steel solid-phase microextraction fiber | |
| CN101992075B (en) | Preparation method of solid phase micro extraction fiber of metal carrier Tenax coating | |
| CN102366718A (en) | Stir extraction bar with carbon nanofiber coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 300300 Dongli Dongli Economic Development Zone, North Road, No. 11, North Road, No. Applicant after: Tianjin Chunfa Biotechnology Group Co., Ltd. Address before: 300300 Dongli Dongli Economic Development Zone, North Road, No. 11, North Road, No. Applicant before: Tianjin Chunfa Food Ingredients Co., Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: CHUNFA FOOD MATERIAL CO., LTD., TIANJIN TO: TIANJIN CHUNFA BIO-TECHNOLOGYGROUP CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120905 Termination date: 20150902 |
|
| EXPY | Termination of patent right or utility model |