CN116099512A - 一种用于测定水中全氟化合物的管状被动采样器吸附相 - Google Patents
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Abstract
本发明涉及环境监测技术领域，且公开了一种用于测定水中全氟化合物的管状被动采样器吸附相，包括以下制备步骤：S1、使用甲醇净化、活化WAX吸附剂，将WAX吸附剂上的吸附结合位点上的杂质溶解在甲醇中，后用超纯水淋洗；S2、将淋洗后的WAX吸附剂和10mL胶联剂‑聚丙烯酰胺溶胶按质量比2∶5的比例混合均匀，后依次加入160μL 10％过硫酸铵溶液和30μL催化剂N,N,N’N’四甲基乙二胺溶液，继续混匀；S3、将适当上述溶液注入PE管中，两头封上后置于滚动混匀器中，以70rpm转速滚动10min，形成凝胶后将PE管划开，将胶棒完整取出。本发明公开的一种用于测定PFAS的CFT吸附相在制备过程中无需加热，耗时短、耗能小，具有制备工艺简单、规范性高、成胶强壮等优点。
Description
技术领域
本发明涉及环境监测技术领域，具体为一种用于测定水中全氟化合物的陶瓷管被动采样器(Ceramic filter tube,CFT)的吸附相。
背景技术
全氟烷基化合物(Perfluoroalkyl substances，PFAS)是自20世纪40年代末以来生产的一类人工合成化学品，并广泛应用于许多工业和商业领域。PFAS排放到环境中有直接和间接两种来源。直接来源为PFAS的工业生产和使用过程；而间接来源是PFAS以化学反应杂质的形式或物质可能降解形成PFAS。由于PFAS的化学性质非常稳定，释放到自然环境中不容易被物理、化学和生物机制分解，在全球范围内的各种环境介质(水体、土壤、大气等)中均有检出。有研究表明，PFAS具有生物积累性，可以通过食物链传递，并且有致癌性、免疫毒性和发育毒性等多种毒性。目前，PFAS污染已引起世界范围内的广泛关注，国际上许多组织以都对PFAS的生产和使用进行了规范。其中，PFOA和PFOS及相关化合物已被列入《关于持久性有机污染物的斯德哥尔摩公约》。因此，对水环境中PFAS污染水平的监测对PFAS生态风险评估和完善环境立法具有重要意义。
水环境中PFAS的检测多采用现场采样后带回实验室富集分析的方式。这种方式在样品运输过程中，污染物成分可能会发生改变，且前处理过程繁琐，需要花费大量时间、人力和资源。被动采样技术作为一种新兴的采样技术，可以集采集和富集于一体，省时省力并能提供样品在采样过程的时间加权平均浓度。陶瓷管被动采样技术是一种新兴的被动采样技术，它具有动力学采样、操作简单、不需要野外校正等特点。其核心部分为固定目标物的吸附相。目前用于管状被动采样技术的吸附相主要有吸附树脂颗粒，如Amberlite IRA、Dowex Optipore L-493、HLB等和吸附剂凝胶，如TiO2琼脂凝胶。但这些吸附相均不能有效吸附PFAS,且不可重复利用。
发明内容
(一)解决的技术问题
针对现有技术的不足，本发明提供了一种用于测定水中全氟化合物的管状被动采样器吸附相，解决了上述背景技术中所存在的问题。
(二)技术方案
为实现上述目的，本发明提供如下技术方案：一种用于测定水中全氟化合物的管状被动采样器吸附相及再生方法，包括以下制备步骤：
S1、使用甲醇净化、活化WAX吸附剂，将WAX吸附剂上的吸附结合位点上的杂质溶解在甲醇中，后用超纯水淋洗；
S2、将淋洗后的WAX吸附剂和10mL胶联剂-聚丙烯酰胺溶胶按质量比2∶5的比例混合均匀，后依次加入160μL 10％过硫酸铵溶液和30μL催化剂N,N,N’N’四甲基乙二胺溶液，继续混匀；
S3、将适当上述溶液注入PE管中，两头封上后置于滚动混匀器中，以70rpm转速滚动10min，形成凝胶后将PE管划开，将胶棒完整取出；
S4、将凝胶置于超纯水中浸泡24h，使其充分膨胀，并多次换水直至水溶液PH为7；
S5、充分膨胀后胶棒呈均匀乳白色，将凝胶切割成直径为4.5cm的胶棒，即得所需CFT吸附相。
优选的，所述胶棒的尺寸可根据陶瓷管尺寸制备，直径≥7mm，长度≥4.5cm。
优选的，所述步骤S1中活化、淋洗依次采用甲醇和超纯水进行，所用的WAX材料、甲醇和超纯水的体积比约为1∶10∶10。
优选的，所述步骤S2中的WAX吸附剂和丙烯酰胺溶胶的质量比为2∶5。
(三)有益效果
本发明提供了一种用于测定水中全氟化合物的管状被动采样器吸附相，具备以下有益效果：
(1)、本发明公开的一种用于测定PFAS的CFT吸附相可用于CFT中测定溶液中PFAS的浓度。
(2)、本发明公开的一种用于测定PFAS的CFT吸附相在制备过程中无需加热，耗时短、耗能小，具有制备工艺简单、规范性高、成胶强壮、可重复利用等优点。
附图说明
图1为组装有本发明制备的吸附相的CFT装置示意图；
图2为本发明制备的用于测定PFAS的CFT吸附相对水体中5种PFAS的吸附效果对比结果图；
图3为组装有本发明制备的用于测定PFAS的CFT吸附相采集PFAS后重复利用性图；
图4为组装有本发明制备的用于测定PFAS的CFT吸附相的CFT装置(CFT-WAX)与传统主动采样-固相萃取法(Grab-SPE)测定污水中PFAS的浓度的对比图。
图中：1、陶瓷管；2、WAX吸附胶棒；3、橡胶堵头。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
将本发明所制备的WAX吸附相，置于10mL含有浓度为50μg/L 5种PFAS水溶液(PFBA、PFBS、PFHxA、PFOA和PFOS)中，于摇床震荡吸附，在吸附0min、4h、18h、24h后分别取0.1mL样品，使用超高效液相色谱质谱联用仪测定吸附前后溶液中抗生素的浓度，以计算WAX吸附胶对PFAS的吸附效率。由图2可以看出，本发明所制备的WAX吸附胶对目标PFAS的吸附在前4个小时达到了50％以上，并且在18h后都将实验水溶液中的目标PFAS完全吸附。表明本发明制备的WAX吸附胶对目标PFAS具有较高的吸附效率。
实施例2
将本发明所制备的WAX结合相，加入到10mL含有50μg/L的目标PFAS水溶液中，吸附24h后将WAX胶取出，并置于5mL 0.5％氨水甲醇和5mL乙腈中超声清洗1h。将洗脱溶液倒出后，将WAX吸附胶泡在超纯水中至复原形态。随后，在下一个吸附循环中重复使用，通过对含有目标PFAS水溶液中的吸附率判定重复使用效果。由图3中可以看出，WAX吸附胶第5次对目标PFAS的平均吸附率均>82％。表现出了良好的重复使用的可能性。
实施例3
将含有本发明所制备WAX结合相的CFT装置(CFT-WAX)如图1所示，应用于污水处理厂进水中PFAS的测定。将CFT装置置于污水处理厂进水水面30cm以下，放置2、3、5、7天,放置CFT和取出CFT的同时取水样1L进行常规固相萃取方法(Grab-SPE)测定。取回的CFT将WAX吸附胶取出，使用5mL0.5％氨水甲醇/乙腈(V:V＝1:1)，超声30min，重复两次，合并两次洗脱液。将洗脱液氮吹至近干，以0.5mL甲醇和0.5mL水复溶并涡旋混匀。所有样品利用超高效液相色谱质谱联用仪测定PFAS含量。目标PFAS在CFT-WAX上积累量随着时间的增加而增加，说明在7天的采样时间内，WAX吸附胶没有达到饱和，CFT-WAX在污水处理厂进水口的放置采样的持续时间可大于7天。而传统的抓取式采样和CFT-WAX采样方法均能检测到五种目标PFAS化合物(图4)，CFT-WAX测量结果略高于抓取式采样的方法测定结果，由于传统抓取式采样只能反映取样时目标物的瞬时浓度，污水处理厂进水中PFAS的浓度会随时间变化有波动，所以传统抓取式采样的方法测定结果偏低，符合预期。结果表明CFT-WAX可以用于在短时间内测定水环境中PFAS的时间加权平均浓度。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (4)
1.一种用于测定水中全氟化合物的管状被动采样器吸附相，其特征在于，包括以下制备步骤：
S1、使用甲醇净化、活化WAX吸附剂，将WAX吸附剂上的吸附结合位点上的杂质溶解在甲醇中，后用超纯水淋洗；
S2、将淋洗后的WAX吸附剂和10mL胶联剂-聚丙烯酰胺溶胶按质量比2∶5的比例混合均匀，后依次加入160μL 10％过硫酸铵溶液和30μL催化剂N,N,N’N’四甲基乙二胺溶液，继续混匀；
S3、将适当上述溶液注入PE管中，两头封上后置于滚动混匀器中，以70rpm转速滚动10min，形成凝胶后将PE管划开，将胶棒完整取出；
S4、将凝胶置于超纯水中浸泡24h，使其充分膨胀，并多次换水直至水溶液PH为7；
S5、充分膨胀后胶棒呈乳白色，吸附剂均匀分布，将凝胶切割成直径为4.5cm的胶棒，即得所需CFT吸附相。
2.根据权利要求1所述的一种用于测定水中全氟化合物的管状被动采样器吸附相，其特征在于：所述胶棒的尺寸可根据陶瓷管尺寸制备，直径≥7mm，长度≥4.5cm。
3.根据权利要求1所述的一种用于测定水中全氟化合物的管状被动采样器吸附相，其特征在于：所述步骤S1中活化、淋洗依次采用甲醇和超纯水进行，所用的WAX材料、甲醇和超纯水的体积比约为1∶10∶10。
4.根据权利要求1所述的一种用于测定水中全氟化合物的管状被动采样器吸附相，其特征在于：所述步骤S2中的WAX吸附剂和丙烯酰胺溶胶的质量比为2∶5。
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