CN101992072A - Aluminum oxide coating stirring extraction rod of metal carrier - Google Patents
Aluminum oxide coating stirring extraction rod of metal carrier Download PDFInfo
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- CN101992072A CN101992072A CN201010270812XA CN201010270812A CN101992072A CN 101992072 A CN101992072 A CN 101992072A CN 201010270812X A CN201010270812X A CN 201010270812XA CN 201010270812 A CN201010270812 A CN 201010270812A CN 101992072 A CN101992072 A CN 101992072A
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- extraction bar
- adsorbent
- epoxy resin
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Abstract
The invention relates to an aluminum oxide coating stirring extraction rod of a metal carrier. The carrier of the extraction rod is metal, and the coating of the extraction rod contains an adsorbent. When the extraction rod is used in a stirring mode, the metal is iron or nickel or cobalt or stainless steel or alloy; when the extraction rod is used in a headspace or ultrasonic mode, the metal is the stainless steel or copper or aluminum or the alloy. The adsorbent is a metal oxide adsorbent. The extraction rod has higher mechanical strength and is sturdy and durable by replacing the traditional glass rod with a metal rod; and a mode that the adsorbent is combined to the stirring rod is more beneficial to the treatment and the static headspace trapping of liquid samples by the adsorbent.
Description
Technical field
The invention belongs to organic trace analysis field in food, environment, the biological sample, particularly relate to a kind of metallic carrier r-Al
2O
3Coating stirs extraction bar, and that this extraction bar is applicable to is nitrogenous, the enrichment of the heterocycle of phosphorus, sulfenyl, aromatic hydrocarbon, organic amine.
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, is enclosed within on the glass tube that seals magnetic core in to make.But 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 extraction bar, the carrier of this extraction bar is a metal, includes adsorbent in the coating of extraction bar.
Wherein, when extraction bar used with alr mode, metal was iron, nickel, cobalt, stainless steel or alloy, and when extraction bar used with head space or ultrasonic power, metal was stainless steel, copper, aluminium or alloy.
Wherein adsorbent is a metal oxide sorbents, and the preferable alloy oxide adsorbent is selected from one or more in aluminium oxide, titanium oxide, zirconia, the magnesium silicate etc.
Wherein aluminium oxide is r-Al
2O
3, titanium oxide is titanium dioxide.
Wherein, also include high-temperature-resistant epoxy resin or organic siliconresin in the coating.
The present invention also provides the extraction bar of preparation by the following method, and this method comprises the steps:
(1) choosing and preliminary treatment of barred body:
To grow and be that 10-40mm, diameter are that the metal bar of 0.5-5mm carries out preliminary treatment with dichloromethane solvent to its surface;
(2) 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, prepare 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;
(3) 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 (2) pick one deck adsorbent at skin more earlier;
(4) 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;
(5) 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.
In the said method, can pass through repeating step (2) to adjust coating layer thickness.
In the said method, when extraction bar used with alr mode, metal was iron, nickel, cobalt, stainless steel or alloy, and when extraction bar used with head space or ultrasonic power, metal was stainless steel, copper, aluminium or alloy.
In the said method, solvent is selected from dimethylbenzene, toluene, benzene and the acetone and other organic solvent one or more;
Curing agent is selected anhydride type curing agents such as pyromellitic dianhydride for use;
Auxiliary agent is a tertiary amine;
Filler is selected from one or more in flake asbestos, aluminium powder and the titanium dioxide;
Adsorbent is preferably metal oxide sorbents, metal oxide sorbents be selected from aluminium oxide, titanium oxide, zirconia, magnesium silicate etc. one or more.
Wherein aluminium oxide is r-Al
2O
3, titanium oxide is a titanium dioxide.
Extraction bar of the present invention is a carrier with the metal bar, utilizes synthesizing high temperature epoxy resin or organic siliconresin that adsorbent is fixed on the metal bar surface, forms the coating material of Heat stability is good, anti-solvent washing, thereby realizes the 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.If select r-Al
2O
3As adsorbent, the adsorptivity that it has the strong utmost point is specially adapted to the enrichment to nitrogenous, phosphorus, sulfenyl heterocyclic, aromatic hydrocarbon, organic amine.
Description of drawings
Fig. 1 is not for using the gas-chromatography baseline chart that stirs extraction bar
Fig. 2 is for using the gas-chromatography baseline chart of stirring extraction bar under desorption temperature of embodiment 1
Fig. 3 is the gas chromatogram that utilizes the stirring extraction bar extraction benzene series material of embodiment 1, and wherein 1 is benzene, and 2 is toluene, and 3 is fluorobenzene.
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, obtains high-temperature-resistant epoxy resin.With the surface-coated one deck high-temperature-resistant epoxy resin of the iron staff of handling, pick one deck r-Al at skin again
2O
3Adsorbent 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.
Wherein epoxy resin is multifunctional glycidol type epoxy resin, and market is bought and obtained.
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 r-Al2O3 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 layer of titanium dioxide 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 4
Utilize the stirring extraction bar of making among the embodiment 1 that aniline category matter in pharmaceutical factory's waste water is detected, take to stir the extraction mode, the desorb of thermal desorption method.
Embodiment 5
Utilize the stirring extraction bar of making among the embodiment 1 that perfume ingredient is fragrant and analyze, take the head space mode to extract, the desorb of thermal desorption method.
Embodiment 6
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.
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. extraction bar, the carrier of this extraction bar is a metal, include adsorbent in the coating of extraction bar, when extraction bar uses with alr mode, metal is iron, nickel, cobalt, stainless steel or alloy, when extraction bar used with head space or ultrasonic power, metal was stainless steel, copper, aluminium or alloy, and adsorbent is a metal oxide sorbents.
2. extraction bar according to claim 1, wherein metal oxide sorbents is selected from one or more in aluminium oxide, titanium oxide, zirconia, the magnesium silicate etc.
3. extraction bar according to claim 2, wherein aluminium oxide is r-Al
2O
3, titanium oxide is titanium dioxide.
4. extraction bar according to claim 1 also includes high-temperature-resistant epoxy resin or organic siliconresin in the coating.
5. extraction bar, this extraction bar is by comprising the method preparation of following steps:
(1) choosing and preliminary treatment of barred body:
To grow and be that 10-40mm, diameter are that the metal bar of 0.5-5mm carries out preliminary treatment with dichloromethane solvent to its surface;
(2) 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, prepare 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;
(3) 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 (2) pick one deck adsorbent at skin more earlier;
(4) 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;
(5) 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 when extraction bar used with alr mode, metal was iron, nickel, cobalt, stainless steel or alloy, and when extraction bar used with head space or ultrasonic power, metal was stainless steel, copper, aluminium or alloy; Solvent is selected from dimethylbenzene, toluene, benzene and the acetone one or more; Curing agent is a pyromellitic dianhydride; Filler is selected from one or more in flake asbestos, aluminium powder and the titanium dioxide; Adsorbent be selected from aluminium oxide, titanium oxide, zirconia, magnesium silicate etc. one or more.
6. extraction bar according to claim 5, wherein aluminium oxide is r-Al
2O
3, titanium oxide is a titanium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010270812XA CN101992072A (en) | 2010-09-02 | 2010-09-02 | Aluminum oxide coating stirring extraction rod of metal carrier |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010270812XA CN101992072A (en) | 2010-09-02 | 2010-09-02 | Aluminum oxide coating stirring extraction rod of metal carrier |
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| CN101992072A true CN101992072A (en) | 2011-03-30 |
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| CN201010270812XA Pending CN101992072A (en) | 2010-09-02 | 2010-09-02 | Aluminum oxide coating stirring extraction rod of metal carrier |
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Cited By (4)
| 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 |
| CN104307498A (en) * | 2014-10-31 | 2015-01-28 | 武汉大学 | Stainless steel extraction stir bar and preparation method 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 |
| CN109289816A (en) * | 2018-10-29 | 2019-02-01 | 湖北文理学院 | A kind of sulfhydryl modified spiral mixing rod and its preparation method and application |
-
2010
- 2010-09-02 CN CN201010270812XA patent/CN101992072A/en active Pending
Cited By (6)
| 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 |
| 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 |
| 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 |
| CN109289816A (en) * | 2018-10-29 | 2019-02-01 | 湖北文理学院 | A kind of sulfhydryl modified spiral mixing rod and its preparation method and application |
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Application publication date: 20110330 |