CN107096516A - 一种水质检测用固相微萃取涂层光纤及其制备方法 - Google Patents

一种水质检测用固相微萃取涂层光纤及其制备方法 Download PDF

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CN107096516A
CN107096516A CN201710351378.XA CN201710351378A CN107096516A CN 107096516 A CN107096516 A CN 107096516A CN 201710351378 A CN201710351378 A CN 201710351378A CN 107096516 A CN107096516 A CN 107096516A
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吕光辉
孙小妹
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Anhui Zhongcheng Environmental Testing Co Ltd
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Abstract

本发明公开了一种水质检测用固相微萃取涂层光纤的制备方法，包括如下步骤：S1、将P123、乙醇溶液混合均匀，加入硅基介孔材料，在50‑60℃下超声溶解得到混合液；S2、将不锈钢丝进行表面处理后，放入含有混合液的离心管中，离心，取出不锈钢丝，在室温下将乙醇完全挥发，然后置于110‑130℃条件下真空干燥得到水质检测用固相微萃取涂层光纤；本发明还公开了一种水质检测用固相微萃取涂层光纤，适用于水中苯系物和重金属检测。本发明以P123作为模板剂，与硅基介孔材料原位复合形成固相微萃取涂层材料，提高了的萃取光纤的选择性，提高了检测灵敏度。

Description

一种水质检测用固相微萃取涂层光纤及其制备方法
技术领域
本发明涉及固相微萃取涂层光纤技术领域，尤其涉及一种水质检测用固相微萃取涂层光纤及其制备方法。
背景技术
固相微萃取(SPME)技术是一种集采样、萃取、浓缩和进样于一体的样品前处理与富集技术，已被广泛应用于环境、食品、生物等领域。SPME具有简单、快速、灵敏度高、选择性好、环境友好且便于直接与检测器联用、可实现在线检测等优点。涂层是SPME技术的核心，涂层材料对SPME的选择性和灵敏度起到决定性的作用。已报道的商品化涂层包括聚二甲基硅氧烷、聚二甲基硅氧烷/二乙烯基苯、聚丙烯酸酯等。但是，商品化涂层由于价格昂贵、选择性差等缺点，使用范围比较有限。因而制备萃取效果优良、使用范围广的SPME涂层材料成为水质检测研究的重点。
发明内容
本发明提出了一种水质检测用固相微萃取涂层光纤及其制备方法，本发明以P123作为模板剂，与硅基介孔材料原位复合形成固相微萃取涂层材料，提高了的萃取光纤的选择性，提高了检测灵敏度。
本发明提出的一种水质检测用固相微萃取涂层光纤的制备方法，包括如下步骤：
S1、将P123、乙醇溶液混合均匀，加入硅基介孔材料，在50-60℃下超声溶解得到混合液；
S2、将不锈钢丝进行表面处理后，放入含有混合液的离心管中，离心，取出不锈钢丝，在室温下将乙醇完全挥发，然后置于110-130℃条件下真空干燥得到水质检测用固相微萃取涂层光纤。
优选地，S1中，P123和硅基介孔材料的重量比为1：2-3。
优选地，S1中，P123和乙醇溶液的重量体积比为20-35：100；优选地，乙醇溶液中乙醇浓度为80-95wt％。
优选地，S1中，硅基介孔材料为MCM-48分子筛。
优选地，S2中，不锈钢丝表面处理的具体操作为：将不锈钢丝的一端在丙酮中浸泽10-15min，用高纯水洗涤，在室温下晾干。
优选地，S2中，离心时间为40-60s。
优选地，S2中，真空干燥时间为10-14h。
本发明提出的一种水质检测用固相微萃取涂层光纤，由水质检测用固相微萃取涂层光纤的制备方法制得。
优选地，所述水质检测用固相微萃取涂层光纤可用于水中重金属检测。
优选地，所述水质检测用固相微萃取涂层光纤可用于水中苯系物检测。
本发明中固相微萃取涂层光纤可结合气相色谱、液相色谱、气相色谱-质谱联用、电感耦合等离子体发射光谱仪检测、电感耦合等离子体质谱仪检测或原子吸收分光光度计检测进行水质检测，固相微萃取涂层光纤解析温度为220-290℃。
本发明以P123作为模板剂，加入硅基介孔材料原位复合形成固相微萃取涂层材料，硅基介孔材料具有良好的选择性，其孔径与Hg、Pb、Cr、Cd重金属离子相适配、能够很好的吸附的此类重金属离子，吸附力强，吸附量大，显著提高了检测的灵敏度，同时硅基介孔材料对苯系物也具有很好的吸附性能，亦可适用于水中苯系物的检测；P123与硅基介孔材料在不锈钢表面发生硅烷化反应，提高了涂层与不锈钢基体的粘合力，延长了涂层光纤的使用时间，节约了资源。
具体实施方式
本发明提出的一种水质检测用固相微萃取涂层光纤的制备方法，包括如下步骤：
S1、将P123、乙醇溶液混合均匀，加入硅基介孔材料，在50-60℃下超声溶解得到混合液；
S2、将不锈钢丝进行表面处理后，放入含有混合液的离心管中，离心，取出不锈钢丝，在室温下将乙醇完全挥发，然后置于110-130℃条件下真空干燥得到水质检测用固相微萃取涂层光纤。
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种水质检测用固相微萃取涂层光纤，由如下步骤制得：
S1、称取25gP123，加入100ml浓度为80wt％的乙醇溶液混合均匀，加入50gMCM-48分子筛，在50℃下超声5min溶解得到混合液；
S2、将不锈钢丝的一端在丙酮中浸泽10min，用高纯水洗涤，在室温下晾干，放入含有混合液的离心管中，调节离心机转速为3000r/min离心60s，取出不锈钢丝，用玻璃板划掉多余的混合液，在室温下将乙醇完全挥发，然后置于130℃条件下真空干燥14h得到水质检测用固相微萃取涂层光纤。
将实施例1中制得的水质检测用固相微萃取涂层光纤结合气相色谱，控制解析温度为250℃，对水样中苯系物含量进行检测，检测结果如下表所示：
从检测结果可以看出，本发明对苯系物的检测具有良好的富集效果，提高了检测灵敏度。
实施例2
一种水质检测用固相微萃取涂层光纤，由如下步骤制得：
S1、称取20gP123，加入100ml浓度为90wt％的乙醇溶液混合均匀，加入60gMCM-48分子筛，在60℃下超声3min溶解得到混合液；
S2、将不锈钢丝的一端在丙酮中浸泽15min，用高纯水洗涤，在室温下晾干，放入含有混合液的离心管中，调节离心机转速为5000r/min离心40s，取出不锈钢丝，用玻璃板划掉多余的混合液，在室温下将乙醇完全挥发，然后置于110℃条件下真空干燥10h得到水质检测用固相微萃取涂层光纤。
将实施例2中制得的水质检测用固相微萃取涂层，控制解析温度为290℃，对水样中重金属含量进行检测，检测结果如下表所示：
检测种类 相关系数 检出限(mg/kg) 重复性(％，10次)
汞 0.9994 5.3 3.6
铅 0.9997 5.6 2.2
镉 0.9996 2.5 3.0
铬 0.9994 3.1 2.1
从测试数据可以看出，本发明对水中汞、铅、镉、铬检测具有很好的灵敏度。
实施例3
一种水质检测用固相微萃取涂层光纤，由如下步骤制得：
S1、称取35gP123，加入100ml浓度为95wt％的乙醇溶液混合均匀，加入90gMCM-48分子筛，在55℃下超声4min溶解得到混合液；
S2、将不锈钢丝的一端在丙酮中浸泽12min，用高纯水洗涤，在室温下晾干，放入含有混合液的离心管中，调节离心机转速为4000r/min离心50s，取出不锈钢丝，用玻璃板划掉多余的混合液，在室温下将乙醇完全挥发，然后置于120℃条件下真空干燥12h得到水质检测用固相微萃取涂层光纤。
实施例4
一种水质检测用固相微萃取涂层光纤，由如下步骤制得：
S1、称取25gP123，加入100ml浓度为95wt％的乙醇溶液混合均匀，加入65gMCM-48分子筛，在55℃下超声4min溶解得到混合液；
S2、将不锈钢丝的一端在丙酮中浸泽12min，用高纯水洗涤，在室温下晾干，放入含有混合液的离心管中，调节离心机转速为4000r/min离心50s，取出不锈钢丝，用玻璃板划掉多余的混合液，在室温下将乙醇完全挥发，然后置于120℃条件下真空干燥12h得到水质检测用固相微萃取涂层光纤。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (10)

1.一种水质检测用固相微萃取涂层光纤的制备方法，其特征在于，包括如下步骤：
S1、将P123、乙醇溶液混合均匀，加入硅基介孔材料，在50-60℃下超声溶解得到混合液；
S2、将不锈钢丝进行表面处理后，放入含有混合液的离心管中，离心，取出不锈钢丝，在室温下将乙醇完全挥发，然后置于110-130℃条件下真空干燥得到水质检测用固相微萃取涂层光纤。
2.根据权利要求1所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S1中，P123和硅基介孔材料的重量比为1：2-3。
3.根据权利要求1所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S1中，P123和乙醇溶液的重量体积比为20-35：100；优选地，乙醇溶液中乙醇浓度为80-95wt％。
4.根据权利要求1-3任一项所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S1中，硅基介孔材料为MCM-48分子筛。
5.根据权利要求1-3任一项所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S2中，不锈钢丝表面处理的具体操作为：将不锈钢丝的一端在丙酮中浸泽10-15min，用高纯水洗涤，在室温下晾干。
6.根据权利要求1-3任一项所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S2中，离心时间为40-60s。
7.根据权利要求1-3任一项所述的水质检测用固相微萃取涂层光纤的制备方法，其特征在于，S2中，真空干燥时间为10-14h。
8.一种水质检测用固相微萃取涂层光纤，其特征在于，由权利要求1-7任一项所述的水质检测用固相微萃取涂层光纤的制备方法制得。
9.根据权利要求8所述的水质检测用固相微萃取涂层光纤，其特征在于，所述水质检测用固相微萃取涂层光纤可用于水中重金属检测。
10.根据权利要求8所述的水质检测用固相微萃取涂层光纤，其特征在于，所述水质检测用固相微萃取涂层光纤可用于水中苯系物检测。
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