CN101992069B - Preparation method of metal carrier stirring and extracting rod - Google Patents
Preparation method of metal carrier stirring and extracting rod Download PDFInfo
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- CN101992069B CN101992069B CN 201010270649 CN201010270649A CN101992069B CN 101992069 B CN101992069 B CN 101992069B CN 201010270649 CN201010270649 CN 201010270649 CN 201010270649 A CN201010270649 A CN 201010270649A CN 101992069 B CN101992069 B CN 101992069B
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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 is quite complicated with composition, 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 the sample-pretreating method that solvent-free or few solvent, the degree of accuracy are high, quick, easy 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 and high efficiency separation detection means couplings such as chromatogram, electrophoresis, 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 accomplished 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, so the enrichment multiple obviously improves very suitable trace analysis.Abroad should technology successfully be 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.
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 process. 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 received 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 the conventional glass rod 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, gets 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 earlier (b) preparation pick one deck Tenax adsorbent at skin again, can pass through repeating step (c) adjustment coating layer thickness;
(d) cured of coating:
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 xylenes, 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 white powder.
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 accomplished and is stirred in extraction process, has avoided the competitive Adsorption of stirrer in Fiber SPME; Replace the conventional glass rod to make it have higher mechanical strength, sturdy and durable with metal bar; Adsorbent is attached to the 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 xylenes 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 through concrete 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 all to be regarded as and are included within the scope of the present invention.
Claims (7)
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, gets 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 earlier (b) preparation pick one deck Tenax adsorbent at skin again, can pass through repeating step (c) adjustment coating layer thickness;
(d) cured of coating:
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 or alloy with alr mode; Extraction bar is if use with head space or ultrasonic power, and metal is selected from copper, aluminium or alloy.
3. method according to claim 1, wherein extraction bar is if use metal chosen from Fe, nickel, cobalt or stainless steel with alr mode; Extraction bar is if use with head space or ultrasonic power, and metal is selected from stainless steel, copper or aluminium.
4. method according to claim 1, wherein solvent is selected from xylenes, toluene, benzene or acetone.
5. method according to claim 1, wherein curing agent is a pyromellitic dianhydride.
6. method according to claim 1, wherein filler is selected from flake asbestos, aluminium powder or titanium white powder.
7. method according to claim 1, wherein the Tenax adsorbent is 2,6-dibenzofuran porous polymeric resins.
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| CN 201010270649 CN101992069B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier stirring and extracting rod |
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| CN 201010270649 CN101992069B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier stirring and extracting rod |
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| CN101992069A CN101992069A (en) | 2011-03-30 |
| CN101992069B true CN101992069B (en) | 2012-09-05 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028381B (en) * | 2013-01-09 | 2014-06-25 | 福州大学 | Solid phase microextraction coating and preparation method thereof |
| CN103949229B (en) * | 2014-02-28 | 2016-05-11 | 武汉大学 | A kind of stainless steel extraction stirring rod 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 |
| CN104475053B (en) * | 2014-11-19 | 2016-09-14 | 武汉大学 | Graphene oxide/Polyethylene Glycol coating stirring rod and preparation method and application |
| US20190009248A1 (en) * | 2016-02-03 | 2019-01-10 | Gerstel K.K. | Element for extracting organic components |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE19933017A1 (en) * | 1999-03-26 | 2001-01-18 | Gerstel Systemtechnik Gmbh | Solid phase micro-extrusion and analysis procedures |
| 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 |
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Non-Patent Citations (3)
| Title |
|---|
| Baltussen E,et al..Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: Theory and principles.《JOURNAL OF MICROCOLUMN SEPARATIONS》.1999,第11卷(第10期),第740页. * |
| BaltussenE et al..Stir bar sorptive extraction (SBSE) |
| Xia XR,et al..Preparation and characterization of porous silica coated multifibers for solid-phase microextraction.《ANALYTICAL CHEMISTRY》.2001,第73卷(第9期),第2042页. * |
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