CN107175090B - 一种多孔碳固相微萃取涂层及其制备方法和应用 - Google Patents
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Abstract
一种多孔碳固相微萃取涂层及其制备方法和应用。该多孔碳涂层材料以柠檬酸钾作为碳前驱体,氮气保护下高温碳化,自身活化并产生模板,经盐酸和超纯水清洗产生发达的孔隙结构。无需使用模板剂和活化剂,绿色、简单、便捷、廉价。该材料具有发达的孔隙,巨大的比表面积和高电负性,对含苯环有机物具有强力的吸附作用。多孔碳固相微萃取涂层萃取效率高,重现性好。因此,可用于监测环境中痕量的挥发性有机污染物。
Description
技术领域
本发明涉及分析化学和环境监测领域,特别是涉及一种多孔碳固相微萃取涂层及其制备方法和应用。
背景技术
固相微萃取集采样、富集、纯化和进样于一体,无需使用有机试剂,是一种绿色的分析检测技术。因此,近些年来迅速发展,尤其是在挥发性和半挥发性有机污染物的监测和检测领域。固相微萃取技术的原理是基于扩散和吸附理论,所以涂层是该技术的核心部件,直接决定测定方法的灵敏度和准确度。目前,商品化的涂层种类有限,且存在易损坏、价格昂贵和热稳定性差的缺点。所以,发明简单的、新型的、廉价的、稳定性好的和萃取性能强的涂层是十分必要和迫切的。
近些年,碳材料因具有优良的热稳定性和巨大的比表面积,迅速发展,特别是在电能储备材料领域。但是,该材料在固相微萃取领域研究较少,且制造过程较为复杂。目前,多孔碳的制备方法有限,共有两大类:1,使用氢氧化钾、氯化锌和磷酸等物质进行活化。2,使用氧化锰、二氧化硅和氧化锌等作为模板成孔。这两类制备方法不仅生产成本高昂、过程复杂,且使用腐蚀性物质,对环境造成一定的污染。鉴于此,一种绿色的可持续生产方法是十分必要的。此外,生产出的碳材料是否适用于固相微萃取有待探究。
挥发性有机污染物是一类沸点较低、迁移性强、易对人体健康造成一定危害的物质。在当今中国,污染严重、治理难度大,一直是环境领域的热点和重点。为了保障居民的身体健康,对人们的生活环境进行痕量监测是十分必要的。但是,针对于挥发性有机污染物的监测手段仍不成熟,且难以监测痕量水平的挥发性有机物。
发明内容
解决的技术问题:针对上述技术缺陷,本发明提供了一种新型的、简单的、廉价的、性能好的多孔碳固相微萃取涂层及其制备方法和应用,用于测定水体中痕量水平的挥发性有机污染物。
技术方案:一种多孔碳固相微萃取涂层的制备方法,加热烘干的柠檬酸钾,以3℃/min升温至850℃,保持1h,全过程通氮气保护,最后自然降温完成碳化过程,材料降至室温后,使用盐酸进行清洗、抽滤,去除杂物,然后使用过量的去离子水清洗,最后用0.45μm滤膜收集固体残余物,烘干后研磨粉碎得到碳材料粉末,最后将碳材料粉末粘附于硅酮密封胶表面得多孔碳固相微萃取涂层。
碳材料粉末制备涂层的具体方法为:涂层制备工艺具体为,0.5g硅酮密封胶置于1mL环己烷中,25℃超声30min促进溶解、稀释备用;取不锈钢丝,于丙酮、乙醇内分别25℃超声清洗10min,置于烘箱中110℃烘干;待冷却,插入稀释的硅酮密封胶溶液中,旋转1圈,立即拔出,擦掉多余的胶水,在碳材料粉末上反复转动,置于烘箱中90℃老化10min,反复三次,得到涂层。
优选的,涂层厚度为40μm。
优选的,盐酸的体积浓度为10%(V/V)。
上述方法制得的多孔碳固相微萃取涂层。
上述多孔碳固相微萃取涂层在测定水体中挥发性有机污染物中的应用。
监测水体中挥发性有机污染物:取一定体积水样,置于棕色玻璃瓶中,加入聚四氟乙烯包裹的转子,含垫片中空盖盖紧。固相微萃取装置穿刺垫片,将自制涂层暴露于样品正上方,加热,一段时间后取出,在气相进样口进行热解吸进样。
有益效果:相对于前人的涂层材料制备过程,本发明的涂层材料生产过程简单,且无需使用模板和活化试剂,绿色、环保和廉价。相对于商业涂层和前人研究的涂层,本发明的涂层具有优良的热稳定性,巨大的比表面积和高电负性,对含苯环的挥发性有机污染物具有强大的萃取性能。
附图说明
图1为本发明制备的多孔碳涂层的扫描电镜图;
图中a:放大200倍,b:放大1000倍,c:放大5000倍,d:放大10000倍。从a和b中可以看出,制备的多孔碳涂层被均匀的涂布在不锈钢丝上,厚度约为40μm。将比例进一步放大,从c和d中可以看出制备的碳材料是一种尺寸约为1μm的片状物。
图2为本发明制备的多孔碳材料的X衍射图谱;
从衍射峰中可以看出,共有两个特征峰,较大的002峰表征本材料为无定形材料,较小的100峰表征此材料具有一定的石墨化。
图3为本发明制备的多孔碳材料的热重图;
从热重图中可以看出,400℃之前,此材料是很稳定的一种碳材料,耐高温,解决了在固相微萃取在仪器上热解吸的需求。
图4为本发明制备的多孔碳材料的氮气吸附-脱附曲线图;
本发明使用氮气吸附解吸实验,测定了BET比表面积为1236.04m2·g-1,孔体积为:0.82cm3·g-1。表明是一种孔隙发达的碳材料,为固相微萃取提供了充足的吸附位点和较强的表面吸附能。
图5为本发明制备的多孔碳涂层与商业化聚二甲基硅氧烷涂层萃取六种氯苯的性能比较;图中每组数据柱的左侧为聚二甲基硅氧烷,右侧为多孔碳涂层。
具体实施方式
实施例1
本例通过选取六种氯苯化合物作为挥发性有机污染物的代表物质,对新型多孔碳固相微萃取涂层测定水体中挥发性有机污染物的方法进行说明,制备涂层的分析结果参见附图1~5。
制备多孔碳材料:将柠檬酸钾置于烘箱中120℃过夜烘干,用高精度天平称取5.0000g柠檬酸钾,置于船型坩埚中,然后放置于TL1200管式炉中,3℃/min升温至850℃,保持1h,全过程通氮气(50mL/min)保护,最后自然降温完成碳化过程。材料降至室温后,使用大量10%(V/V)盐酸进行清洗、抽滤,去除杂物,然后使用过量的去离子水清洗,最后用0.45μm滤膜收集固体残余物,并置于烘箱中120℃烘干过夜。用玛瑙研钵粉碎得到碳材料粉末备用。
制备多孔碳材料涂层:0.5g西卡硅酮密封胶置于1mL环己烷中,25℃超声30min促进溶解、稀释备用。取3cm左右的不锈钢丝,用丙酮、乙醇分别25℃超声清洗10min,置于烘箱中110℃烘干。待冷却,插入已经稀释的西卡硅酮密封胶溶液中,旋转1圈,立即拔出,用称量纸擦掉多余的胶水,在碳材料粉末上反复转动,置于烘箱中90℃老化10min,反复三次,得到约40μm厚度的涂层。装入商用空管中,于气相进样口氮气保护,250℃老化1h备用。
监测水体中六种氯苯:取10mL江苏省玄武湖水置于棕色玻璃瓶中,加入聚四氟乙烯包裹的转子,含垫片中空盖盖紧。固相微萃取装置穿刺垫片,将自制涂层暴露于样品正上方,80℃加热,萃取10min,迅速取出,在气相进样口进行310℃热解吸5min进样。同时,添加一定浓度氯苯,测定加标回收率。结果见表1。回收率在82.28-102.44%之间,满足分析需求。
表1
实施例2
本例通过对比商业化涂层聚二甲基硅氧烷对六种氯苯化合物的萃取量,对新型多孔碳固相微萃取涂层的萃取性能进行说明。制备多孔碳材料、多孔碳材料涂层和萃取操作过程同实例1一致。先用聚二甲基硅氧烷萃取六种氯苯,然后再用多孔碳涂层萃取相同浓度的六种氯苯,各重复三次,进行分析,结果见图5。对于六种氯苯化合物,多孔碳涂层的萃取量均高于商业化聚二甲基硅氧烷涂层,且萃取量是聚二甲基硅氧烷的2.14-42.37倍。说明本发明的多孔碳涂层可高效、精准测定水体环境中痕量的挥发性有机污染物,尤其是氯苯化合物。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何不经过创造性劳动想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书所限定的保护范围为准。
Claims (3)
1.一种多孔碳固相微萃取涂层的制备方法,其特征在于制备多孔碳材料:将柠檬酸钾置于烘箱中120℃过夜烘干,用高精度天平称取5.0000 g柠檬酸钾,置于船型坩埚中,然后放置于TL1200 管式炉中,3℃/min升温至850℃,保持1 h,全过程通氮气50mL/min保护,最后自然降温完成碳化过程;材料降至室温后,使用体积比10 %盐酸进行清洗、抽滤,去除杂物,然后使用过量的去离子水清洗,最后用0.45μm滤膜收集固体残余物,并置于烘箱中120℃烘干过夜;用玛瑙研钵粉碎得到碳材料粉末备用;制备多孔碳材料涂层:0.5 g 西卡硅酮密封胶置于1mL 环己烷中,25℃超声30 min促进溶解、稀释备用;取不锈钢丝,用丙酮、乙醇分别25℃超声清洗10 min,置于烘箱中110℃烘干;待冷却,插入已经稀释的西卡硅酮密封胶溶液中,旋转1圈,立即拔出,用称量纸擦掉多余的胶水,在碳材料粉末上反复转动,置于烘箱中90℃老化10 min,反复三次,得到40μm厚度的涂层;装入商用空管中,于气相进样口氮气保护,250℃老化1h备用。
2.权利要求1所述方法制得的多孔碳固相微萃取涂层。
3.权利要求2所述多孔碳固相微萃取涂层在测定水体中挥发性有机污染物中的应用。
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