CN101992070B - Preparation method of metal carrier extracting rod - Google Patents
Preparation method of metal carrier extracting rod Download PDFInfo
- Publication number
- CN101992070B CN101992070B CN 201010270665 CN201010270665A CN101992070B CN 101992070 B CN101992070 B CN 101992070B CN 201010270665 CN201010270665 CN 201010270665 CN 201010270665 A CN201010270665 A CN 201010270665A CN 101992070 B CN101992070 B CN 101992070B
- Authority
- CN
- China
- Prior art keywords
- metal
- epoxy resin
- rod
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a metal carrier extracting rod, which comprises the steps of: 1, selecting and preprocessing a metal rod body; 2, synthesizing heat-resistant epoxy resin; 3, manufacturing a stirring rod coating; 4, curing the coating; and 5, removing impurities of the extracting rod body. In the method, when the extracting rod is used in a stirring manner, 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. The metal rod is replaced with the traditional glass rod to ensure that the metal rod has higher mechanical strength and is firm and durable. A manner of binding an absorbing agent on the stirring rod is more beneficial to the treatment of the absorbing agent to a liquid sample and the static headspace collection.
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
3The preparation method of coating stirring extraction bar, that the extraction bar of the method preparation 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 very complex, sample pre-treatments becomes important step indispensable in the sample analysis under normal conditions.It plays concentrated tested trace components, the effect of the 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 easily sample, are produced larger error, and the use of toxic solvent can affect 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 Some Questions To Be Researched of current analytical chemistry.
Solid phase micro-extraction technique is 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 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, be widely used.
Stir Bar Sorptive Extraction (Stirbar sorptive extraction, SBSE) proposed in 1999 by people such as Erik Baltussen, it is a kind of novel Sample Pretreatment Technique that grows up on SPME (Solid Phase Micro Extraction, SPME) basis.This technology is the same with SPME have simple, efficient, fast, favorable reproducibility, the 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 large more than 50 times, therefore enrichment times obviously improves, and is fit to very much trace analysis.This technology successfully is applied to the analysis of environmental sample, pollutants in food, drugs, medicine and residues of pesticides, human endocrine interfering material, polycyclic aromatic hydrocarbon, benzene homologues and Polychlorinated biphenyls etc. abroad.
Germany Gerstel GnlbH company selects 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 of an interior envelope magnetic core to make.But commercial SBSE device only has this a kind of fixedly phase coating of PDMS, and commercialization SBSE device price is higher, and the application of SBSE technology has been subject to larger restriction.For this reason, be the work that novelty and practical significance are extremely arranged to the research of SBSE technology.
Existing stirring extraction bar is all take glass bar as carrier, 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 metal carrier extracting rod, the 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 fully dissolving, add successively again curing agent, auxiliary agent, filler, 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:
High-temperature-resistant epoxy resin or the organic siliconresin of the surface-coated one deck step of the barred body that will process first (2) preparation pick one deck adsorbent at skin again;
(4) curing of coating is processed:
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, when extraction bar used with agitating 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 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.
In the said method, solvent is selected from one or more in dimethylbenzene, toluene, benzene and the acetone and other organic solvent;
Curing agent is the anhydride type curing agents such as pyromellitic dianhydride;
Auxiliary agent is tertiary amine;
Filler is selected from one or more in flake asbestos, aluminium powder and the titanium dioxide;
The extraction bar of method preparation of the present invention utilizes synthesizing high temperature epoxy resin or organic siliconresin that adsorbent is fixed on the metal bar surface take metal as carrier, forms the coating material of Heat stability is good, anti-solvent washing, thereby realizes the enrichment to trace organic substance.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 is conducive to 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, the below further specifies the present invention with embodiment, but does not limit the present invention.
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 fully dissolving, add successively 15g pyromellitic dianhydride, 15g tertiary amine, 20g flake asbestos again, 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 processing, 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 processing, 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.
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 processing, 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 the waste water in pharmaceutical plants 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.
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 the 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 deemed to be included within the scope of the present invention.
Claims (7)
1. the preparation method of a metal carrier extracting rod, the 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 fully dissolving, add successively again curing agent, auxiliary agent, filler, 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:
High-temperature-resistant epoxy resin or the organic siliconresin of the surface-coated one deck step of the barred body that will process first (2) preparation pick the layer of metal oxide adsorbent at skin again;
(4) curing of coating is processed:
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.
2. method according to claim 1, wherein when extraction bar used with agitating mode, metal was iron, nickel, cobalt or alloy, when extraction bar used with head space or ultrasonic power, metal was copper, aluminium or alloy.
3. method according to claim 1, wherein metal oxide sorbents is selected from one or more in aluminium oxide, titanium oxide, the zirconia.
4. method according to claim 3, wherein aluminium oxide is r-Al
2O
3, titanium oxide is titanium dioxide.
5. each described method according to claim 1-4, wherein solvent is selected from one or more in dimethylbenzene, toluene, benzene and the acetone.
6. each described method according to claim 1-4, wherein curing agent is pyromellitic dianhydride.
7. each described method according to claim 1-4, wherein filler is selected from one or more in flake asbestos, aluminium powder and the titanium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010270665 CN101992070B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier extracting rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010270665 CN101992070B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier extracting rod |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101992070A CN101992070A (en) | 2011-03-30 |
| CN101992070B true CN101992070B (en) | 2013-02-20 |
Family
ID=43783114
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010270665 Expired - Fee Related CN101992070B (en) | 2010-09-02 | 2010-09-02 | Preparation method of metal carrier extracting rod |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101992070B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102846221A (en) * | 2012-09-11 | 2013-01-02 | 吴江市聚力机械有限公司 | Food stirring rod |
Citations (1)
| 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 |
-
2010
- 2010-09-02 CN CN 201010270665 patent/CN101992070B/en not_active Expired - Fee Related
Patent Citations (1)
| 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 |
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. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101992070A (en) | 2011-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101992069B (en) | Preparation method of metal carrier stirring and extracting rod | |
| Bigham et al. | Sol− gel capillary microextraction | |
| Weggler et al. | Inlets and sampling | |
| Paiva et al. | Fundamentals of and recent advances in sorbent-based headspace extractions | |
| Li et al. | Preparation of C18 composite solid-phase microextraction fiber and its application to the determination of organochlorine pesticides in water samples | |
| CN101992072A (en) | Aluminum oxide coating stirring extraction rod of metal carrier | |
| Wen | Recent advances in solid-phase extraction techniques with nanomaterials | |
| CN101992070B (en) | Preparation method of metal carrier extracting rod | |
| CN102366721A (en) | Stirring and extracting bar for polydimethylsiloxane compounded carbon molecular sieve coating | |
| CN102068966A (en) | Metal carrier stirring and extracting rod | |
| CN101942762B (en) | Preparation method of metal carrier solid phase micro-extraction fiber | |
| CN101992062B (en) | Method for preparing metal carrier stirring extraction rod | |
| CN102008944A (en) | Stirring and extracting bar for beta-cyclodextrin matrix | |
| CN102049244A (en) | Method for preparing Beta-cyclodextrin matrix stir extraction bar | |
| CN101972635B (en) | Preparation method of stir and extraction bar for polymer coating | |
| CN102068963B (en) | Stainless steel solid phase micro extraction fiber | |
| CN102114417A (en) | Preparation method of stainless steel solid-phase microextraction fiber | |
| CN101992073A (en) | Metal carrier Tenax coating solid-phase microextraction fiber | |
| CN102366718A (en) | Stir extraction bar with carbon nanofiber coating and preparation method thereof | |
| CN101934224A (en) | Method for preparing polymer coating stir extraction bar | |
| CN101992071A (en) | Metal carrier stirring extraction rod | |
| CN102068962B (en) | Preparation method of metal carrier solid-phase micro-extraction fiber | |
| CN101961637A (en) | Method for preparing metal carrier solid-phase micro-extraction fiber | |
| CN101992074B (en) | Metal carrier solid phase microextraction fiber | |
| CN101947437B (en) | Solid-phase micro-extraction fiber with polymer 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: TIANJIN CHUNFA FOOD INGREDIENTS CO., LTD. TO: TIANJIN CHUNFA BIO-TECHNOLOGY GROUP 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: 20130220 Termination date: 20150902 |
|
| EXPY | Termination of patent right or utility model |