CN100488592C - Solid-phase extracting disk of single-wall carbon nano-tube substrate - Google Patents
Solid-phase extracting disk of single-wall carbon nano-tube substrate Download PDFInfo
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- CN100488592C CN100488592C CNB2006100896556A CN200610089655A CN100488592C CN 100488592 C CN100488592 C CN 100488592C CN B2006100896556 A CNB2006100896556 A CN B2006100896556A CN 200610089655 A CN200610089655 A CN 200610089655A CN 100488592 C CN100488592 C CN 100488592C
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- 239000007790 solid phase Substances 0.000 title claims description 19
- 239000002109 single walled nanotube Substances 0.000 title abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 19
- 239000000758 substrate Substances 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000007613 environmental effect Effects 0.000 claims abstract description 5
- 239000013076 target substance Substances 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 13
- 238000002414 normal-phase solid-phase extraction Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000003463 adsorbent Substances 0.000 abstract description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 abstract description 3
- -1 bisphenol A Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 230000037303 wrinkles Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000945 filler Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 229940106691 bisphenol a Drugs 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明属于化学分析测试仪器设备领域，涉及一种单壁碳纳米管(SWCNT)为基质的固相萃取圆盘，它将作为新型的样品前处理材料，来富集大体积水样中目标物质。与传统的固相萃取盘相比，该萃取盘制备简单，可以减少污染，萃取盘不易起皱。相对于相同规格的C18固相萃取盘，所需SWCNT吸附剂的量是C18的1/16，进而可以降低萃取盘的成本。而SWCNT吸附剂由于对极性化合物也有很好的分离富集能力，因此该萃取盘比传统的萃取盘可适用的范围更广泛。以双酚A、辛基酚和壬基酚等化合物为对象，对新萃取盘各项性能指标进行了反复测试，具有很好的稳定性。水样通过萃取盘的速度快，最高可达100ml/min，可快速分析环境样品。
The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a single-walled carbon nanotube (SWCNT)-based solid-phase extraction disk, which will be used as a new type of sample pretreatment material to enrich target substances in large-volume water samples . Compared with the traditional solid phase extraction disk, the preparation of the extraction disk is simple, the pollution can be reduced, and the extraction disk is not easy to wrinkle. Compared with the C 18 solid phase extraction disk of the same specification, the amount of SWCNT adsorbent required is 1/16 of that of C 18 , which in turn can reduce the cost of the extraction disk. The SWCNT adsorbent also has a good separation and enrichment ability for polar compounds, so the extraction disc is applicable to a wider range than traditional extraction discs. Taking compounds such as bisphenol A, octylphenol and nonylphenol as objects, the performance indicators of the new extraction disk were repeatedly tested, and it has good stability. The speed of water samples passing through the extraction disk is fast, up to 100ml/min, which can quickly analyze environmental samples.
Description
One, technical field
The invention belongs to chemical analysis test instrument and equipment field, relate to a kind of SWCN (SWCNT) and be the SPE disk of matrix, it will come target substance in the enrichment large volume water sample as novel sample pre-treatments material.
Two, background technology
The background in present technique field and current situation are roughly as follows: since have simple, fast, easily be automated and characteristics such as environmental friendliness, solid phase extraction techniques has replaced traditional liquid-liquid extraction gradually, becomes method for separating and concentrating main in the sample pre-treatments.Solid-phase extraction column is modal a kind of operation format, fill the filler of the 40 μ m of 100～500mg mostly, and be furnished with the metal or the plastics sieve plate of porous at the post two ends, this larger particles filler and specific configuration thereof have caused in the extraction process must having channeling to produce as the liquid circulation is out-of-date, thereby reduction mass-transfer efficiency, application of sample flow velocity when making extraction can not be too big, otherwise can cause the reduction of extraction efficiency, obtains the lower rate of recovery.And solid-phase extracting disk is another operation format.The commodity solid-phase extracting disk at first comes across 1989, and Minnesota Mining and Manufacturing Company has released Empore series SPE disk product.This novel SPE mode of operation provides another kind sample pre-treatments new method more effectively and rapidly for analytical work person.SPE disk and filter membrane are quite similar, and it generally is to add the compacting of small amount of polytetrafluoroethylmay or glass fiber by the bonded silica gel of particle diameter very thin (8～12 μ m) or polymeric adsorbent filler to form the about 0.5～1mm of its thickness.In this extraction disk, polytetrafluoroethylene (PTFE) or glass fibre support substrate account for the 10-40% of gross mass, and filler then accounts for 60～90%.This structure of solid-phase extracting disk has increased area, has reduced thickness, and for the filler of equal quality, the cross-sectional area of SPE disk is about 10 times of solid-phase extraction column.Thereby improved extraction efficiency, increased loading capacity and extracted flow velocity.Solid-phase extracting disk has been applied to Organic Pollutants such as agricultural chemicals, PCBs aspect in the environment water at present.But the kind of solid-phase extracting disk is still fewer now, and preparation is complicated, therefore needs the preparation of development of new simple, to all effective solid-phase extracting disk of various polar organic matters.CNT is a kind of novel nano material, has showed very big potentiality in environment aspect the organic enrichment, and it is prepared into extracting disk should have broad application prospects.The document of relevant this respect can referring to:
[1]Westbon，R.；
L.；Zorita，S.；Mathiasson，L.；
E.J.Chromatogr.A?2004，1033，1-8.
[2]Martínez-Barrachina，S.；Valle，M.D.Microchemical?Journal?2006，83，48-54.
[3]Riley，M.B.；Dumas，J.A.；Gbur，E.E.；Massey，J.H.；Mattice，J.D.；Mersie，W.；Mueller，T.C.；Potter，T.；Senseman，S.A.；Watson，E.J.Agric.Food?Chem.2005，53，5079-5083.
[4]Schwedler，D.A.；Thomas，A.D.；Yeh，L.T.J.Agric.Food?Chem.2000，48，5138-5145.
[5]Ruberu，S.R.；Draper，W.M.；Perera，S.K.J.Agric.Food?Chem.2000，48，4109-4115.
[6]Senaeman，S.A.；Lavy，T.L.；Mattice，J.D.；Gbur，E.E.；Skulman，B.W.Environ.Sci.Technol.1997，31，395-401.
[7]Thurman，E.M.；Snavely，K.Trends?Anal.Chem.2000，19，18-26.
Three, summary of the invention
The invention provides a kind of solid-phase extracting disk that is used for the target substance of enrichment environment sample (as river, sewage), can handle a large amount of environmental samples fast, its stability and repeatability meet the requirement of sampling fully.
The preparation schematic diagram of Fig. 1 SWCNT matrix solid-phase extracting disk.SWCNT is dispersed in the solution of 5% dodecyl sodium sulfate, is supporter with the quantitative filter paper again, filters this solution under the negative pressure, and SWCN is evenly distributed on the filter paper.The extracting disk for preparing is dried, promptly obtain extracting disk shown in Figure 2.
Compare with existing solid-phase extracting disk, this extracting disk mainly contains following advantage:
1. simple only need of preparation filtered the extracting disk that can obtain being evenly distributed with filter paper, and operation is simple, reduces and pollute, and good mechanical strength is arranged, and do not crease easily.
2. widely applicable traditional reversed phase extraction dish is (as C
18) compound of low pole and middle polarity in the only suitable enrichment environment, can not be used to analyze polar compound.And as a kind of anti-phase adsorbent, SWCNT also has very strong adsorption capacity to polar compound.
3. though the price comparison of SWCNT with low cost is expensive, (as standard-sized diameter is the extracting disk of 47mm, and the present invention only needs the SWCNT of 30mg, and traditional C because the amount of preparation this extracting disk needed adsorbent is few
18Adsorbent then needs 500mg), so the solid-phase extraction column of its price and commodity is suitable.Can be for the disposable use in each laboratory.
In finishing process of the present invention, we are object with pollutants such as bisphenol-A, octyl phenol and nonyl phenols, and the every performance indications of new extracting disk have been carried out test repeatedly, have good stability (experimental provision is seen Fig. 3).During with single extracting disk enrichment, each analyte result's reappearance RSD≤10%; Reappearance between three extracting disk except that the RSD=15% of bisphenol-A, the RSD of other two kinds of analytes＜10%.For improving the enrichment capacity, several extracting disk series connection can be used.Water sample is fast by the speed of extracting disk, can reach 30-50ml/min, but the rapid analysis environmental sample.
Four, description of drawings
Fig. 1 SWCNT matrix solid-phase extracting disk prepares schematic diagram.Among the figure, 1 is filtering container, 2 pump interfaces, and 3 is the filtrate receiving flask.
The outward appearance of Fig. 2 SWCNT matrix solid-phase extracting disk and SEM figure.The device schematic diagram of Fig. 3 SWCNT solid-phase extracting disk enriched sample.Among the figure, 1 is reservoir, 2 geometrical clamps, 3 filter paper, 4 extracting disk, 1,5 extracting disk, 2,6 dish supporters, 7 pump interfaces, 8 filtrate receiving flasks, 9 eluent receiving flasks.
Five, the specific embodiment
Below in conjunction with accompanying drawing 1, the preparation method of the solid-phase extracting disk of single-wall carbon nano-tube substrate is described in detail as follows: get the quantitative filter paper of a slice certain diameter, earlier with methyl alcohol and water washing.Take by weighing the 30mg SWCN, join 50ml and contain in 5% the sodium dodecyl sulfate solution ultrasonic 30min.Under negative pressure, filter this solution then, SWCN is evenly distributed on the filter paper with washed filter paper.After solution has filtered,, remove residual dodecyl sodium sulfate, promptly make extracting disk after drying with a large amount of methyl alcohol and water washing.Extracting disk can be reused, and when handling water sample, can activate.
Claims (1)
1. solid-phase extracting disk, it is characterized in that: this solid-phase extracting disk is a matrix with the SWCN, is supporter with the quantitative filter paper; SWCN is dispersed in the solution that contains 5% dodecyl sodium sulfate, filters this solution under the negative pressure, SWCN is evenly distributed on the quantitative filter paper, forms solid-phase extracting disk; The diameter of this solid-phase extracting disk is 47mm, has excellent mechanical intensity, and the opposed polarity organic matter is had strong adsorption capacity, can fast enriching large volume environmental water sample in target substance.
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| CNB2006100896556A CN100488592C (en) | 2006-07-10 | 2006-07-10 | Solid-phase extracting disk of single-wall carbon nano-tube substrate |
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| CN101028570A CN101028570A (en) | 2007-09-05 |
| CN100488592C true CN100488592C (en) | 2009-05-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105251238A (en) * | 2015-11-13 | 2016-01-20 | 黑龙江省科学院科技孵化中心 | Solid phase extraction column capable of achieving negative pressure suction and using method |
| CN108956258A (en) * | 2017-05-22 | 2018-12-07 | 上海安谱实验科技股份有限公司 | Solid-phase extracting disk and its processing method for bulk sample |
| CN118758708A (en) * | 2024-09-09 | 2024-10-11 | 国科大杭州高等研究院 | On-site enrichment instrument for new pollutants in water |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003247154A (en) * | 2002-02-19 | 2003-09-05 | Denso Corp | Method for producing formed article comprising carbon nanofiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003247154A (en) * | 2002-02-19 | 2003-09-05 | Denso Corp | Method for producing formed article comprising carbon nanofiber |
Non-Patent Citations (2)
| Title |
|---|
| 固相萃取技术及其演化发展. 孙天华，刘晓茹.首都师范大学学报（自然科学版），第25卷第s1期. 2004 * |
| 碳纳米管作为吸附剂在环境分析中的应用. 李权龙，袁东星.第二届全国环境化学学术报告会论文集. 2004 * |
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Granted publication date: 20090520 Termination date: 20110710 |