CN1736581A - Carbon-ceramic utilized absorption material - Google Patents

Carbon-ceramic utilized absorption material Download PDF

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Publication number
CN1736581A
CN1736581A CN 200510017012 CN200510017012A CN1736581A CN 1736581 A CN1736581 A CN 1736581A CN 200510017012 CN200510017012 CN 200510017012 CN 200510017012 A CN200510017012 A CN 200510017012A CN 1736581 A CN1736581 A CN 1736581A
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carbon
spe
ceramic
ceramics
extraction
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CN 200510017012
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CN100341618C (en
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徐国宝
史立红
刘晓庆
李海娟
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Changchun Institute of Applied Chemistry of CAS
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The present invention relates to carbon-ceramic utilized absorption material, belong to the sorbing material field.Carbon ceramics can be made the packing material of SPE sorbing material, SPME sorbing material or the chromatographic column of required form as required.If carbon ceramics is to conduct electricity, just carbon ceramics can be made the electrode of required size and shape, use this electrode pair sample to carry out SPE or SPME after, just can be used for material outside the electrochemical gaging ferronickel with electro-chemical activity.By selecting different material with carbon elements, ceramic material and corresponding dressing agent, can obtain the different carbon ceramic material of character, satisfy needs to various inorganic matters and organic matter extraction.Carbon ceramics as the SPE material have the preparation condition gentleness, applied widely, rate of extraction is fast, extraction efficiency is high, extraction process is followed the tracks of easily and be easy to advantage such as batch process.

Description

Carbon-ceramic utilized absorption material
Technical field
The present invention relates to carbon-ceramic utilized absorption material, belong to the sorbing material field.
Background technology
Sorbing material is widely used in SPE, SPME, chromatographic isolation and electrochemical analysis.SPE is extraction and a kind of technology of separate analytes from solution or gas.Because that it has is simple to operate, use flexibly, the rate of recovery is high, consume solvent few, be easy to advantage such as automation, adopted by many laboratories and analytical work person.But this method complex operation, blank value height, easily stop up adsorption column and cause reappearance not ideal enough.SPME is similar to the SPE principle, but operates diverse a kind of sample preparation and pretreatment technology.This technology proposed (R.G.Belardi, J.Pawliszyn, Water Pollution Research J.Canada.1989,24,179) first by Pawliszyn seminar of Canadian Waterloo university at Canadian water Pollution Study magazine in 1989.SPME has kept most of advantage of SPE, some shortcomings of SPE have been overcome again, it is combined as a whole sampling, extraction, concentration and separation and sample introduction, is easy to and multiple separate analytical technique couplings such as gas-chromatography, high performance liquid chromatography, Capillary Electrophoresis, mass spectrum and uv-spectrophotometric.Extracting head is the core of whole solid-phase micro-extracting device.Commercialization extracting head coating kind is less at present, mainly by development of Supelco company and production, comprises the homogeneous polymer coating, as dimethyl silicone polymer (PDMS) and polyacrylate (PA); The multiphase polymer coating is as dimethyl silicone polymer/divinylbenzene (PDMS/DVB), polyethylene glycol/template resin (CW/TPR) and carbon molecular sieve/divinylbenzene (Carboxen/DVB).The preparation of these coatings all is that high polymer is fixed on diameter hundreds of micron vitreous silica fiber surface by the method that photocuring or high temperature heat, its selectivity is relatively poor, serviceability temperature is on the low side (200-280 ℃), service life short (being generally 40-100 time), cost an arm and a leg, its application is restricted.In order to address these problems, multiple noncommodity coating material appears recently, and its technology of preparing has physics to be coated with stain, colloidal sol-gel, electrochemical polymerization, molecular imprinting technique etc.There are problems such as the slow or extraction quantity of rate of extraction is few in these materials, and development high selectivity, high stability and extracting head coating material and relevant technology of preparing thereof are efficiently widened the sample scope, are the keys of solid phase micro-extraction technique development.1994, the Lev of Hebrew Univ Jerusalem Israel etc. reported the making (M.Tsionsky, G.Guan, V.Glezer, O.Lev, Anal.Chem., 1994,66,1747 ~ 1753) that colloidal sol-gel technique is used for carbon ceramic composite materials first on U.S.'s analytical chemistry.But, carbon ceramics mainly is used as electrode material so far and is used for electrochemical research, only Wang seminar and Guadalupe seminar have successively reported that in Electroanalytical Chemistry carbon ceramics that usefulness is added with complexing agent is used for the extraction electrochemical gaging (J.Wang of nickel and iron as electrode in 1997 and 1999, P.V.A.Pamidi, V.B.Nascimento, L.Angnes, Electroanalysis, 1997,9,689; Z.Q.Ji, A.R.Guadalupe, Electroanalysis, 1999,11,167).Because carbon ceramics has porous, the adsorptivity of heterogeneity and carbon dust, much inorganic, organic compound rapid diffusion and a large amount of absorption therein that carbon ceramics allows can be used as the adsorbent of SPE and micro-extraction and as the packing material of chromatographic column.When employed carbon ceramic material has electric conductivity, can be used as sorbing material double as electrode and be used for other material outside the electrochemical gaging ferronickel.
Summary of the invention
The objective of the invention is carbon ceramic material as a kind of novel sorbing material.Owing to be easy to prepare different shape and component, carbon ceramic material can be widely used in SPE sorbing material, SPME sorbing material and as the packing material of various chromatographic columns.Because the carbon ceramic material that has has good electrical conductivity, on the one hand, can use carbon ceramic material that sample is carried out SPE simultaneously, directly carry out the material outside the Electrochemical Detection ferronickel then with electro-chemical activity; On the other hand, can regulate and control the SPE process, as just quickening to extract or quicken extract desorption from the adsorbent of SPE by applying certain current potential by electrochemical method.
For achieving the above object, the technical solution adopted in the present invention is: colloidal sol and carbon dust are mixed in the proper ratio, then mixture is made particle, coating or the electrode of different shape, promptly be can be used for SPE sorbing material, SPME sorbing material after the curing and as the packing material of various chromatographic columns.Wherein preparing the employed carbon dust of carbon ceramics is graphite powder, amorphous carbon powder, glass carbon dust, carbon fiber powder, CNT, carbon nano powder, bortz powder, carbon aerogels, lonsdaleite powder, carbon nanometer foam or fullerene.Select to have in the said mixture electric conductivity material, just said mixture can be made electrode, use this electrode pair sample to carry out SPE after, just can carry out the material outside the electrochemical measurement ferronickel with electro-chemical activity.
Carbon ceramic material with the preparation of so-gel method among the present invention has the tridimensional network that is cross-linked with each other, it is a kind of porous material, effective area is big, and nature difference is bigger between carbon and the ceramic material, cause material to have mass transfer rate faster, thereby can realize rapidly and efficiently extracting at carbon ceramic material.Less with the carbon ceramic material stress of colloidal sol-gel method preparation simultaneously, therefore can be used to prepare SPE material with big thickness or large-size.And, can obtain the different carbon ceramic material of character by selecting different material with carbon elements, ceramic material and corresponding dressing agent, satisfy needs to various inorganic matters and organic matter extraction.
Material of the present invention have the preparation condition gentleness, applied widely, rate of extraction is fast, extraction efficiency is high, extraction process is followed the tracks of easily and be easy to advantages such as batch process.
The specific embodiment
Embodiment 1: get colloidal sol, 1 milligram of laurate and 25 milligrams of carbon dusts that 100 microlitres are made by 5 to 80 microlitre trimethoxymethylsila,e and mix, then mixture is applied to the quartz fibre surface, after the curing, promptly can be used for the SPME sorbing material.
Embodiment 2: get colloidal sol and 25 milligrams of carbon dusts that 100 microlitres are made by 5 to 80 microlitre trimethoxy-benzene base silanes and mix, to make particle then, and after the curing, promptly can be used for SPE mixture is applied to the quartz fibre surface, after the curing, promptly can be used for SPME.
Embodiment 3: colloidal sol and carbon dust are mixed in the proper ratio, make particle, the content that makes the carbon dust in the dry carbon ceramics is 10%, and prepared carbon ceramics promptly can be used as the packing material of chromatographic column.
Embodiment 4: colloidal sol and carbon dust are mixed in the proper ratio, make particle, the content that makes the carbon dust in the dry carbon ceramics is 50%, and prepared carbon ceramics promptly can be used as the packing material of chromatographic column.
Embodiment 5: colloidal sol and carbon dust are mixed in the proper ratio, make particle, the content that makes the carbon dust in the dry carbon ceramics is 90%, and prepared carbon ceramics promptly can be used as the packing material of chromatographic column.
Embodiment 6: get the colloidal sol that 100 microlitres are made by 5 to 25 microlitre trimethoxymethylsila,e and the carbon dust of 25 milligrams of conductions and mix, then mixture is made electrode.To in the electrode immersion sample of polishing after the extraction, take out, carry out electrochemical measurement then with the flushing of secondary water.

Claims (7)

1. carbon ceramics is characterized in that it is used as sorbing material.
2. carbon-ceramic utilized absorption material as claimed in claim 1 is characterized in that it can be used as the sorbing material of SPE.
3. carbon-ceramic utilized absorption material as claimed in claim 1 is characterized in that it can be used as the sorbing material of SPME.
4. as the described carbon-ceramic utilized absorption material of any one claim of 1-3, it is characterized in that selecting the carbon ceramics of electric conductivity to can be used as SPE sorbing material double as electrode.
5. as the described carbon-ceramic utilized absorption material of any one claim of 1-3, it is characterized in that selecting the carbon ceramics of electric conductivity can be used as, the little collection sorbing material of solid phase double as electrode.
6 carbon-ceramic utilized absorption materials as claimed in claim 1 is characterized in that it can be used as the packing material of various chromatographic columns.
7. as the described carbon-ceramic utilized absorption material of 1,2,3 or 6 any one claim, it is characterized in that employed carbon dust is graphite powder, amorphous carbon powder, glass carbon dust, carbon fiber powder, CNT, carbon nano powder, bortz powder, carbon aerogels, lonsdaleite powder, carbon nanometer foam or fullerene.
CNB2005100170126A 2005-07-29 2005-07-29 Carbon-ceramic utilized absorption material Expired - Fee Related CN100341618C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101992074A (en) * 2010-09-02 2011-03-30 天津春发食品配料有限公司 Metal carrier solid phase microextraction fiber
CN107607611A (en) * 2017-09-06 2018-01-19 大连工业大学 A kind of high resolution mass spec analysis method using SPE direct injected

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1022478C (en) * 1991-03-21 1993-10-20 清华大学 Reinforcing of carbon-ceramics composite material with flexibilizer for coystal whiskers
DE19625813A1 (en) * 1996-06-28 1998-01-02 Ecm Ingenieur Unternehmen Fuer Device for removing fluid media
JPH10211428A (en) * 1997-01-29 1998-08-11 Aramitsuku:Kk Adsorptive ceramic

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101992074A (en) * 2010-09-02 2011-03-30 天津春发食品配料有限公司 Metal carrier solid phase microextraction fiber
CN101992074B (en) * 2010-09-02 2012-09-26 天津春发生物科技集团有限公司 Metal carrier solid phase microextraction fiber
CN107607611A (en) * 2017-09-06 2018-01-19 大连工业大学 A kind of high resolution mass spec analysis method using SPE direct injected

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