CN101337178A - Development of New Adsorbents in Adsorption Thermal Desorption Tubes - Google Patents
Development of New Adsorbents in Adsorption Thermal Desorption Tubes Download PDFInfo
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- CN101337178A CN101337178A CN 200810060708 CN200810060708A CN101337178A CN 101337178 A CN101337178 A CN 101337178A CN 200810060708 CN200810060708 CN 200810060708 CN 200810060708 A CN200810060708 A CN 200810060708A CN 101337178 A CN101337178 A CN 101337178A
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- thermal desorption
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- desorption tube
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- 238000003795 desorption Methods 0.000 title claims abstract description 21
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 12
- 239000003463 adsorbent Substances 0.000 title claims abstract description 11
- 239000002608 ionic liquid Substances 0.000 claims abstract description 16
- 239000003365 glass fiber Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000000605 extraction Methods 0.000 claims abstract description 5
- 238000004817 gas chromatography Methods 0.000 claims abstract description 5
- 150000001450 anions Chemical class 0.000 claims abstract description 4
- 150000001768 cations Chemical class 0.000 claims abstract description 4
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 4
- 231100000719 pollutant Toxicity 0.000 claims abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims description 2
- 239000012491 analyte Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 3
- 230000018109 developmental process Effects 0.000 abstract description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N alpha-methyl toluene Natural products CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 150000001555 benzenes Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CNDHHGUSRIZDSL-UHFFFAOYSA-N 1-chlorooctane Chemical compound CCCCCCCCCl CNDHHGUSRIZDSL-UHFFFAOYSA-N 0.000 description 1
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 1
- KTUWFYALZIAAGE-UHFFFAOYSA-N 1-methyl-3-octyl-2h-imidazole Chemical class CCCCCCCCN1CN(C)C=C1 KTUWFYALZIAAGE-UHFFFAOYSA-N 0.000 description 1
- -1 1-octyl-3-methylimidazolium hexafluorophosphate Chemical compound 0.000 description 1
- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229940078552 o-xylene Drugs 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012428 routine sampling Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
Abstract
吸附热脱附管中新型吸附剂的研制，本发明提供了一种新型、高效吸附－热解吸管吸附剂的研制，它是采用惰性的玻璃纤维材料涂覆已制备好的离子液体，经过一定温度的老化再充填到常规的吸附热脱附管中，从而制成一种新型的吸附－热脱附管。通过选择合适的阴阳离子组合成的离子液体有较强萃取富集效率，通过联用气相色谱或气相色谱－质谱可测定大气中痕量的污染物。The development of a new type of adsorbent in the adsorption thermal desorption tube, the present invention provides a new type of high-efficiency adsorption-thermal desorption tube adsorbent development, which is to use inert glass fiber material to coat the prepared ionic liquid, after a certain The temperature aging is then filled into the conventional adsorption thermal desorption tube, thus making a new type of adsorption-thermal desorption tube. The ionic liquid formed by selecting suitable anions and cations has a strong extraction and enrichment efficiency, and the trace pollutants in the atmosphere can be determined by using gas chromatography or gas chromatography-mass spectrometry.
Description
技术领域 technical field
本发明涉及一种新型、高效吸附-热解吸管吸附剂的研制，该吸附剂可使用在常规的热脱附仪或热脱附联用气相色谱分析空气痕量的有机污物，测定时先选择合适的阴、阳离子合成离子液体，然后涂覆在惰性的玻璃纤维材料，经过一定温度的老化再充填到常规的热脱附吸附管中，从而制成一种新型的吸附-热解吸管。由于离子液体有较强萃取富集效率，可萃取富集大气中痕量的污染物。The present invention relates to the development of a new type of high-efficiency adsorption-thermal desorption tube adsorbent, which can be used in conventional thermal desorption instrument or thermal desorption gas chromatography to analyze trace organic pollutants in the air. A new type of adsorption-thermal desorption tube is made by selecting suitable anions and cations to synthesize ionic liquids, and then coating them on inert glass fiber materials, aging at a certain temperature, and then filling them into conventional thermal desorption adsorption tubes. Due to the strong extraction and enrichment efficiency of ionic liquids, trace pollutants in the atmosphere can be extracted and enriched.
背景技术 Background technique
气相色谱是目前色谱领域使用最广泛、也是目前气体及挥发性物质最有效的分析手段。但大气中一些痕量的有机污染物由于含量较低，不能进行常规进样检测，热脱附就是在此基础上发展起来。目前用于捕集空气中的各种挥发性有机污染物主要是一些固体吸附材料(而作为吸附剂是填充在热脱附管中专门富集待测的物质)：它们主要有活性碳、碳分子筛、各种多孔高分子聚合物及多孔硅球等，它们的吸附特性主要取决于吸附剂的比表面积、孔径分布、极性、颗粒度及相对密度等。这些吸附剂具有自身的优点，但价格较高，使用户无法接受。Gas chromatography is currently the most widely used in the field of chromatography, and it is also the most effective analysis method for gases and volatile substances. However, due to the low content of some trace organic pollutants in the atmosphere, routine sampling detection cannot be performed. Thermal desorption is developed on this basis. Currently used to capture various volatile organic pollutants in the air are mainly some solid adsorption materials (and as adsorbents are filled in thermal desorption tubes to specifically enrich the substances to be measured): they mainly include activated carbon, carbon Molecular sieves, various porous polymers and porous silicon balls, etc., their adsorption characteristics mainly depend on the specific surface area, pore size distribution, polarity, particle size and relative density of the adsorbent. These adsorbents have their own advantages, but the high price makes them unacceptable to users.
直至目前尝无报道，采用离子液体涂覆制成吸附材料充填进吸附管联用色谱仪器进行环境中痕量挥发性有机污染物的测定。So far, there has been no report on the use of ionic liquids to coat and make adsorption materials and fill them into adsorption tubes coupled with chromatographic instruments for the determination of trace volatile organic pollutants in the environment.
发明内容 Contents of the invention
本发明的目的是提供一种新的热吸附脱附管新型材料的研究，该方法是选择合适的阴、阳离子进行离子液体的合成，然后涂覆在惰性的玻璃纤维上，在一定的温度下老化再充填在热吸附脱附管中联用气相色谱或气相色谱质谱分析大气中痕量的有机化合物。由于离子液体有较强的富集萃取效率，所以测定时可大大提高灵敏度，可广泛应用于环境监测、车间空气、卫生防疫等各类化合物。The purpose of this invention is to provide a new thermal adsorption desorption tube new material research, the method is to select the appropriate anion and cation to carry out the synthesis of ionic liquid, and then coated on the inert glass fiber, at a certain temperature Aging and refilling in thermal adsorption desorption tubes coupled with gas chromatography or gas chromatography mass spectrometry to analyze trace organic compounds in the atmosphere. Due to the strong enrichment and extraction efficiency of ionic liquids, the sensitivity can be greatly improved during determination, and can be widely used in various compounds such as environmental monitoring, workshop air, sanitation and epidemic prevention.
国内外尚无同类功能装置。There is no similar functional device at home and abroad.
具体实施方式 Detailed ways
实施实例Implementation example
吸附热脱附联用气相色谱质谱测定大气中苯系物Determination of Benzene Series in Atmosphere by Adsorption Thermal Desorption with Gas Chromatography-Mass Spectrometry
具体步骤如下：Specific steps are as follows:
1、离子液体1-辛基-3-甲基咪唑六氟磷酸盐([[C8mim][PF6])的合成：原料1-甲基咪唑和1-氯正辛烷按1∶1.2(物质的量)的比例混合，然后在80℃下回流24h。反应完毕后趁热用分液漏斗分出下层的离子液体；用少量的乙酸乙酯洗涤离子液体3～5次，而后在75℃真空干燥12h，冷却至室温后取出，得到产物氯化1-辛基-3-甲基咪唑([C8mim]Cl)。1. Synthesis of ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate ([[C 8 mim][PF 6 ]): raw materials 1-methylimidazole and 1-chloro-n-octane at 1:1.2 (amount of substance) was mixed and then refluxed at 80° C. for 24 h. After the reaction is complete, use a separatory funnel to separate the ionic liquid in the lower layer; wash the ionic liquid with a small amount of ethyl acetate for 3 to 5 times, then dry it in vacuum at 75°C for 12 hours, take it out after cooling to room temperature, and obtain the product chlorinated 1- Octyl-3-methylimidazole ([C 8 mim]Cl).
将[C8mim]Cl溶于少量水中，加入六氟磷酸钾固体，在常温下搅拌12h，分层后分出下层离子液体，用少量水洗涤，在洗过离子液体的水中滴加1mol/L的AgNO3水溶液数滴后无白色沉淀产生，表明其中的Cl-已被除净。产物在70℃真空干燥12h，得到最终产物[C8mim][PF6]。Dissolve [C 8 mim]Cl in a small amount of water, add potassium hexafluorophosphate solid, stir at room temperature for 12 hours, separate the lower layer ionic liquid after layering, wash with a small amount of water, add 1mol/ There was no white precipitate after a few drops of AgNO 3 aqueous solution in L, indicating that the Cl - in it had been removed. The product was vacuum-dried at 70°C for 12 hours to obtain the final product [C 8 mim][PF 6 ].
2、吸附热脱附管的制备：称取一定量的干洁的玻璃纤维，涂覆上述已制备好的离子液体，放在一定温度下烘干，取出备用。2. Preparation of adsorption thermal desorption tube: Weigh a certain amount of dry glass fiber, coat the above prepared ionic liquid, dry it at a certain temperature, and take it out for later use.
3、各种参数的选择：试验了大气采样器、热脱附等各种参数，最后能成功地分离并萃取大气中痕量的污染物。3. Selection of various parameters: Various parameters such as atmospheric sampler and thermal desorption were tested, and finally the trace pollutants in the atmosphere were successfully separated and extracted.
附图说明 Description of drawings
图1为充填新型吸附剂吸附热脱附-色谱质谱联用测定大气中苯系物的总离子流图Figure 1 is the total ion chromatogram for the determination of benzene series in the atmosphere by filling the new adsorbent with adsorption thermal desorption-chromatographic mass spectrometry
图1中标记为：Marked in Figure 1 as:
1-苯；2-甲苯；3-乙苯；4-对二甲苯；5-邻二甲苯。1-benzene; 2-toluene; 3-ethylbenzene; 4-p-xylene; 5-o-xylene.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103197023A (en) * | 2013-04-20 | 2013-07-10 | 北京工业大学 | Thermal desorption-gas phase-mass spectra combining method for collecting air contaminants based on ionic liquid |
| CN103923015A (en) * | 2013-01-14 | 2014-07-16 | 北京工业大学 | Two selective ionic liquids and synthesis method thereof |
| CN105115785A (en) * | 2015-08-26 | 2015-12-02 | 杭州普洛赛斯检测科技有限公司 | Preparation method of sampling tube of dimethylamine and trimethylamine in air and waste gas |
| CN105784887A (en) * | 2016-03-09 | 2016-07-20 | 上海烟草集团有限责任公司 | Ageing device for thermal desorption pipes and ageing method thereof |
| CN109632402A (en) * | 2019-01-23 | 2019-04-16 | 大连理工大学 | A kind of novel thermal desorption adsorption tube |
| CN112169764A (en) * | 2019-07-01 | 2021-01-05 | 江汉大学 | Glass fiber cotton containing fluorine tail and preparation method and application thereof |
| CN112169765A (en) * | 2019-07-01 | 2021-01-05 | 江汉大学 | Fluoro-aryl glass fiber cotton and preparation method and application thereof |
-
2008
- 2008-04-25 CN CN 200810060708 patent/CN101337178A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923015A (en) * | 2013-01-14 | 2014-07-16 | 北京工业大学 | Two selective ionic liquids and synthesis method thereof |
| CN103197023A (en) * | 2013-04-20 | 2013-07-10 | 北京工业大学 | Thermal desorption-gas phase-mass spectra combining method for collecting air contaminants based on ionic liquid |
| CN105115785A (en) * | 2015-08-26 | 2015-12-02 | 杭州普洛赛斯检测科技有限公司 | Preparation method of sampling tube of dimethylamine and trimethylamine in air and waste gas |
| CN105115785B (en) * | 2015-08-26 | 2017-10-10 | 杭州普洛赛斯检测科技有限公司 | The preparation method of dimethylamine and trimethylamine sampling pipe in a kind of air and waste gas |
| CN105784887A (en) * | 2016-03-09 | 2016-07-20 | 上海烟草集团有限责任公司 | Ageing device for thermal desorption pipes and ageing method thereof |
| CN105784887B (en) * | 2016-03-09 | 2018-09-25 | 上海烟草集团有限责任公司 | The aging equipment and its aging method of thermal desorption pipe |
| CN109632402A (en) * | 2019-01-23 | 2019-04-16 | 大连理工大学 | A kind of novel thermal desorption adsorption tube |
| CN112169764A (en) * | 2019-07-01 | 2021-01-05 | 江汉大学 | Glass fiber cotton containing fluorine tail and preparation method and application thereof |
| CN112169765A (en) * | 2019-07-01 | 2021-01-05 | 江汉大学 | Fluoro-aryl glass fiber cotton and preparation method and application thereof |
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Open date: 20090107 |