CN111638286A - 一种嗅味水样预处理的装置及其运行工艺 - Google Patents
一种嗅味水样预处理的装置及其运行工艺 Download PDFInfo
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Abstract
本发明公开了一种嗅味水样预处理的装置及其运行工艺,该装置包括通过管道依次相连的高纯氮气瓶、水样罐、一级吸收罐和二级吸收罐,其中,所述水样罐、一级吸收罐和二级吸收罐的底部均设有微孔曝气装置,所述一级吸收罐和二级吸收罐内装有吸收试剂。本发明的装置可以实现对嗅味水样中致嗅化合物的有效萃取和收集,有效解决了异味物质气相色谱‑质谱分析时背景物质干扰大的难题。该装置操作简单,成本较低,效率较高,普遍适用于异味水环境中相关化合物的预处理分析。
Description
技术领域
本发明属于环保技术领域,具体涉及一种嗅味水样预处理的装置及其运行工艺。
背景技术
饮用水中产生嗅味的的嗅味物质的嗅阈值较低,往往低于相关的仪器检出限,但是人体气味感觉器官十分灵敏,会感知到水体嗅味。因此选择合适的前处理浓缩方法对于水体中嗅味物质的识别、分析测定非常重要。目前饮用水中常用的前处理浓缩方法主要包括固相萃取法、固相微萃取法、搅拌棒吸附萃取、同时蒸馏萃取法以及液液萃取法等。
1、固相微萃取:固相微萃取技术是20世纪90年代兴起的一项样品前处理与富集技术,其装置类似于气相色谱的微量进样针,萃取头是在一根石英纤维上涂上相应的涂层,外套细不锈钢管以保护石英纤维不被折断,纤维头可在钢管内伸缩,使用时将纤维涂层直接浸入水中或顶空萃取水样中的有机物,平衡后将针头取出,打入GC进样口使纤维涂层迅速高温解析吸附的嗅味物质。但是由于其所用水样较少、并且不浓缩等特点,需要根据待测物的极性不同选择不同极性的纤维涂层,即极性涂层萃取极性化合物、非极性涂层萃取非极性化合物,间接导致其纤维吸附容量有限,进行全物质分析时需要更换萃取纤维,费时费力等缺点。
2、搅拌棒吸附萃取:搅拌棒吸附萃取的原理与固相微萃取基本一致,主要的部件是一个玻璃包裹的磁力搅拌子,玻璃表面涂有约0.5mm厚的聚二甲基硅氧烷层,分析时将搅拌子置于样品中搅拌一定时间,让涂层吸附有机成分,然后将搅拌子放置于热解析装置,解析后用气相色谱-质谱分析检测。然而目前应用的搅拌棒吸附萃取涂层只有非极性的PDMS材质,只适用于半挥发有机物,并且吸附容量有限。
3、蒸馏萃取:同时蒸馏萃取是蒸馏和液液萃取的一个结合体,它把水样和萃取溶剂分别装在不同的烧瓶中进行加热,用溶剂蒸汽来萃取水样中的有机物。通常的操作是将3L水样用50mL二氯甲烷蒸馏萃取2h后,用K-D浓缩器浓缩至数百微升进样分析。然而其萃取容量有限,检测限较高,并且高温蒸馏过程中会导致嗅味化合物发生转化,导致目标嗅味化合物缺失。
4、液液萃取:液液萃取(LLE)是一种采用有机溶剂萃取水样中有机物的方法,此方法采用多次萃取,萃取剂根据目标物的不同来选择,常用的萃取剂是正己烷和二氯甲烷,将含有目标有机物的萃取液采用旋转蒸发和氮吹的方式进行浓缩。液液萃取可以同时萃取水样中的大部分有机物,包括挥发性、半挥发性和难挥发性有机物,进行气相色谱-质谱分析时可以检出大量的化合物,往往需要在上千种上万种色谱峰中找出几种针对性的挥发性嗅味物质,对目标嗅味化合物的筛查、识别、和检测分析带来了很大的困难。
水环境中的嗅味物质一般为挥发性小分子有机物,其嗅阈值浓度较低,水体中嗅味化合物浓度在ng/L~μg/L水平,便会引起显著的嗅味。为了有效识别、分析和检测水中的嗅味化合物,必须在仪器分析之前对嗅味水样进行浓缩预处理。嗅味水样在预处理浓缩过程中,在萃取痕量嗅味物质的同时还提取了大量无异味的其他背景物质,并且某些预处理浓缩技术的加热环节会导致嗅味化合物的变性转化,给嗅味水样中致嗅物质的识别、分析和检测带来了很大困难,并且上述预处理技术回收率较低,费时费力。
发明内容
针对之前嗅味水样预处理技术存在的背景物质干扰大、回收率低、费时费力等问题,本发明提供了一种嗅味水样预处理的装置及其运行工艺,该装置可以实现对嗅味水样中致嗅化合物的有效萃取和收集。
本发明是通过以下技术方案实现的:
一种嗅味水样预处理的装置,包括通过管道依次相连的高纯氮气瓶、水样罐、一级吸收罐和二级吸收罐,其中,所述水样罐、一级吸收罐和二级吸收罐的底部均设有微孔曝气装置,所述一级吸收罐和二级吸收罐内装有吸收试剂。
优选地,所述一级吸收罐和二级吸收罐内的吸收试剂为相同或不同极性的吸收试剂。
优选地,当一级吸收罐和二级吸收罐内的吸收试剂为不同极性的吸收试剂时,一级吸收罐内的吸收试剂为弱极性试剂,二级吸收罐内的吸收试剂为强极性试剂。
优选地,所述管道为聚四氟乙烯输气管。
一种嗅味水样预处理的装置的运行工艺:将嗅味水样放入水样罐内,调节高纯氮气瓶开度至水样罐内液体表面微微抖动为止,裹挟着嗅味物质的高氮气体通过微孔曝气装置依次进入装有吸收试剂的一级吸收罐和二级吸收罐,曝气脱附-吸附致嗅化合物1h,对吸收试剂进行脱水处理,最后将样品转移出装置保存即可。
本发明的有益效果如下:
人体感知到水环境异味的过程一般是水体中的嗅味化合物穿过气液界面到空气中,进而扩散到人的嗅觉器官,从而被感知到各种类型和强度的嗅味。本发明提供了一种可以有效提取嗅味水样中致嗅化合物的预处理装置,该装置直接采用高纯氮气吹脱-有机试剂吸收挥发性嗅味化合物技术,相比于传统液液萃取、共同蒸馏萃取等同时对水样中的所有有机化合物进行萃取,本发明技术方案只对高纯氮气吹脱出来的挥发性(嗅味)化合物进行吸收,减少了传统预处理技术在进行气相色谱-质谱分析时背景基质干扰大、导致嗅味化合物难以识别、分析和检测的难题。本发明的装置设置两级吸收罐结构,可对吹脱出来的挥发性(嗅味)化合物进行有效吸收。在实施例2中,本发明技术方案成功应用于某鱼腥味、土霉味饮用水源的致嗅化合物识别分析,成功检出了芳香味、鱼腥味、黄瓜味、芳香味、土霉味和芳香味共6个嗅味峰,识别确认了6种对应的嗅味物质丁酸丁酯、2-壬烯醛、2,6-壬二烯醛、十一醛、土臭素、紫罗兰酮。相比于传统液液萃取预处理技术,经过本技术方案处理的样品感官气相色谱-质谱分析时多检测出了4种嗅味(化合物),并且色谱图背景基线较低,检出的物质色谱峰与背景基线差异显著,预处理浓缩后的进样基质杂质物质较少。该预处理装置有效解决了异味物质气相色谱-质谱分析时背景物质干扰大的难题。本发明操作简单,成本较低,效率较高,普遍适用于异味水环境中相关化合物的预处理分析。
附图说明
图1为本发明的装置的结构示意图;
图1中:1、高纯氮气瓶;2、管道;3、水样罐;4、一级吸收罐;5、二级吸收罐;6、微孔曝气装置;
图2为经实施例2曝气脱附-吸收预处理浓缩后致嗅物质识别分析结果图;
图3为经对比例1预处理浓缩后致嗅物质识别分析结果图。
具体实施方式
下面结合附图与具体实施例对本发明作进一步详细说明。
实施例1
一种嗅味水样预处理的装置,如图1所示,包括通过管道2依次相连的高纯氮气瓶1、水样罐3、一级吸收罐4和二级吸收罐5,其中,所述水样罐3、一级吸收罐4和二级吸收罐5的底部均设有微孔曝气装置6,所述一级吸收罐4和二级吸收罐5内装有吸收试剂。
所述高纯氮气瓶1提供后续吹脱痕量挥发性嗅味物质的载气。
所述管道2为性质稳定的聚四氟乙烯输气管。
所述微孔曝气装置6可以将高氮载气均匀高效的布入嗅味水样罐3;裹挟着嗅味物质的高氮气体通过微孔曝气装置6依次进入装有吸收试剂的一级吸收罐4和二级吸收罐5。一级吸收罐4和二级吸收罐5内可以设置相同吸收液,或者设置极性不同的吸收液;比如一级吸收罐4内设置弱极性有机试剂,吸收弱极性异味化合物,二级吸收罐5内设置强极性试剂,吸收强极性异味化合物。为保证对嗅味水样中致嗅物质的吸收效率,吸收罐底部均设置微孔曝气装置6,以提高有机试剂对嗅味物质的接触和吸收。
实施例2
本实施例以实施例1所述装置进行操作,对当地某土霉味、鱼腥味饮用水源的致嗅物质进行了吹脱-吸收-浓缩预处理,具体步骤如下:
将1000mL嗅味水样放入水样罐内,调节高纯氮气瓶开度至水样罐内液体表面微微抖动为止,一级吸收罐和二级吸收罐均采用150mL二氯甲烷有机试剂,曝气脱附-吸附致嗅化合物1h,二氯甲烷吸收液中加入过量的无水硫酸钠进行脱水处理,然后转移至平底烧瓶中,在30℃、500mbar负压条件下旋蒸至5mL左右,最后氮吹定容至1mL,总浓缩倍数为1000倍,分析前样品置于-20℃冰箱中保存。
对比例1
采用传统水样预处理方法-液液萃取对当地某土霉味、鱼腥味饮用水源的致嗅物质进行了预处理,具体步骤如下:
水样经过1.2μm的玻璃纤维膜(GF-C)过滤后,取1000mL于液液萃取瓶中,加入200mL二氯甲烷与15g氯化钠,震荡10min,分液;再加入100mL二氯甲烷萃取一次。往萃取液中加入过量的无水硫酸钠进行脱水处理,然后转移至平底烧瓶中,在30℃、500mbar负压条件下旋蒸至5mL左右,最后氮吹定容至1mL,总浓缩倍数为1000倍,分析前样品置于-20℃冰箱中保存。
测试例1
将实施例2和对比例1得到的浓缩后的样品利用感官气相色谱-质谱进行致嗅物质的识别检测分析,最后将经实施例2和对比例1预处理的致嗅物质识别分析结果进行对比分析。具体如下:
1、感官气相色谱-质谱分析
感官气相色谱,即在气相色谱(HP 6980GC)-质谱(HP 5973MS)仪(Agilent,USA)上连接一个嗅味检测器(ODP,Gerstel,Germany),用于样品中关键致嗅物质的筛查。色谱柱为Rxi-5silv毛细管柱,具体参数见表1。进样体积为1μL,不分流模式,进样口温度为250℃。载气为高纯氦气,流速为1.0mL/min。样品气化后经过色谱柱,以1:2的比例进入质谱检测器和嗅味检测器。色谱柱升温程序为:40℃保持0.2min,以4℃/min升温速度升至280℃,最后280℃条件下保持5min。质谱检测器为全扫描模式(m/z 50-500),数据采集速率为100spectra/s。
感官气相色谱分析溶剂延迟时间为4.5min。闻测者对嗅味峰的保留时间、嗅味类型、嗅味强度进行记录。嗅味强度用0-4表示:其中0表示没有异味,1表示弱强度异味,2表示中强度异味,3表示中到重度异味,4表示重度异味。
表1 感官气相色谱柱系统参数
2、质量控制
采用感官气相色谱-质谱中分析系统空白的方法控制和验证色谱柱系统、进样隔垫系统等仪器本身系统产生的异嗅味;采用在感官气相色谱-质谱中分析检测超纯水空白和溶剂空白的方法控制样品预处理操作环境和萃取溶剂产生的异嗅味。
3、结果分析
某土霉味、鱼腥味饮用水源水样经过实施例2预处理浓缩后的感官气相色谱-质谱分析结果如图2所示,从图2中可以看出,色谱图背景基线较低,检出的物质色谱峰与背景基线差异显著,说明预处理浓缩后的进样基质杂质较少、比较干净,通过实施例2预处理后共识别出6个嗅味峰,分别为芳香味、鱼腥味、黄瓜味、芳香味、土霉味和芳香味。经过谱库检索识别确认的对应嗅味物质分别为丁酸丁酯、2-壬烯醛、2,6-壬二烯醛、十一醛、土臭素、紫罗兰酮。
图3为经对比例1预处理浓缩后的感官气相色谱-质谱分析结果,相对图2,该色谱图背景基线较高,并且检出大量的化合物,然而只检出2个鱼腥味和黄瓜味两个嗅味峰,图2检出的其他嗅味(化合物)未能在液液萃取预处理浓缩液中检出,该结果表明液液萃取预处理虽然可以提取水样中的大部分有机化合物,但未能有效萃取未检出的挥发性目标嗅味化合物。
Claims (5)
1.一种嗅味水样预处理的装置,其特征在于,包括通过管道依次相连的高纯氮气瓶、水样罐、一级吸收罐和二级吸收罐,其中,所述水样罐、一级吸收罐和二级吸收罐的底部均设有微孔曝气装置,所述一级吸收罐和二级吸收罐内装有吸收试剂。
2.根据权利要求1所述的一种嗅味水样预处理的装置,其特征在于,所述一级吸收罐和二级吸收罐内的吸收试剂为相同或不同极性的吸收试剂。
3.根据权利要求2所述的一种嗅味水样预处理的装置,其特征在于,当一级吸收罐和二级吸收罐内的吸收试剂为不同极性的吸收试剂时,一级吸收罐内的吸收试剂为弱极性试剂,二级吸收罐内的吸收试剂为强极性试剂。
4.根据权利要求1所述的一种嗅味水样预处理的装置,其特征在于,所述管道为聚四氟乙烯输气管。
5.权利要求1所述的一种嗅味水样预处理的装置的运行工艺,其特征在于,将嗅味水样放入水样罐内,调节高纯氮气瓶开度至水样罐内液体表面微微抖动为止,裹挟着嗅味物质的高氮气体通过微孔曝气装置依次进入装有吸收试剂的一级吸收罐和二级吸收罐,曝气脱附-吸附致嗅化合物1h,对吸收试剂进行脱水处理,最后将样品转移出装置保存即可。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112285312A (zh) * | 2020-10-30 | 2021-01-29 | 浙江大学 | 一种基于电子鼻检测饮用水异嗅等级的方法 |
CN112730650A (zh) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | 大体积水质中超痕量有机物富集方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62166878A (ja) * | 1986-01-17 | 1987-07-23 | Takashi Toda | 発酵槽の給排気装置 |
RU30742U1 (ru) * | 2003-04-04 | 2003-07-10 | Непаридзе Рауль Шалвович | Установка для обработки сточных вод |
CN103820645A (zh) * | 2014-03-21 | 2014-05-28 | 山东腾跃化学危险废物研究处理有限公司 | 一种五氯化锑废液处置系统 |
CN105233629A (zh) * | 2015-09-29 | 2016-01-13 | 厦门钨业股份有限公司 | 一种气体吸收装置及工艺 |
CN108201871A (zh) * | 2018-01-10 | 2018-06-26 | 南通大学 | 铝灰渣水解除氮装置 |
-
2020
- 2020-06-11 CN CN202010528495.0A patent/CN111638286A/zh active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS62166878A (ja) * | 1986-01-17 | 1987-07-23 | Takashi Toda | 発酵槽の給排気装置 |
RU30742U1 (ru) * | 2003-04-04 | 2003-07-10 | Непаридзе Рауль Шалвович | Установка для обработки сточных вод |
CN103820645A (zh) * | 2014-03-21 | 2014-05-28 | 山东腾跃化学危险废物研究处理有限公司 | 一种五氯化锑废液处置系统 |
CN105233629A (zh) * | 2015-09-29 | 2016-01-13 | 厦门钨业股份有限公司 | 一种气体吸收装置及工艺 |
CN108201871A (zh) * | 2018-01-10 | 2018-06-26 | 南通大学 | 铝灰渣水解除氮装置 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112285312A (zh) * | 2020-10-30 | 2021-01-29 | 浙江大学 | 一种基于电子鼻检测饮用水异嗅等级的方法 |
CN112730650A (zh) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | 大体积水质中超痕量有机物富集方法 |
CN112730650B (zh) * | 2020-12-15 | 2022-08-09 | 湖北微谱技术有限公司 | 大体积水质中超痕量有机物富集方法 |
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