CN105352782B - 一种沉积物中硫醚类致臭物质的测定前处理方法 - Google Patents
一种沉积物中硫醚类致臭物质的测定前处理方法 Download PDFInfo
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Abstract
本发明公开一种沉积物中硫醚类致臭物质的测定前处理方法,首先对沉积物样品预处理,然后分步提取硫醚类物质。萃取后的上清液在固相萃取柱进行分离纯化并利用乙酸乙酯进行洗脱,最后收集洗脱、并浓缩后上气相色谱测定。目前环境样品中主要针对水样、藻类及鱼类等样品形态中硫醚类物质的提取及测定,而缺少沉积物样品中硫醚类物质的快速、准确提取方法,这已经成为进一步深入研究硫醚类物质在湖泊水生态系统沉积物‑水体系中环境地球化学过程循环的瓶颈。本发明可为及时准确地掌握硫醚类物质在沉积物归趋及沉积物‑水界面的环境地球化学行为提供科技支撑。
Description
技术领域
本发明属于环保技术领域,具体涉及一种沉积物中硫醚类物质的测定前处理方法。
背景技术
目前,针对我国城市河道及湖泊局部地区出现水体黑臭问题,但有关水体硫醚类物质的前处理技术主要关注点在于水体、生物样品如鱼类。专利201120511340.2提到利用微波加热法加速沉积物中二甲基三硫醚的挥发,然后利用吹捕扫集收集挥发出来的嗅味物质气体进行测定的方法。此方法最大缺陷为方法多偏重于定性分析嗅味物质,只是将沉积物中部分弱吸附态的二甲基三硫醚物质解析然后收集测定,仍有大部分残留在沉积物中。另外沉积物作为湖泊生态系统的主要组成部分,其中含硫类化合物在地壳中生物环境地球化学过程循环产生大量的含硫类物质,除了二甲基三硫醚外,甲硫醚、二甲基三硫醚、二甲基二硫醚等,这些物质均为水体重要的嗅味物质,据文献报道2007产生的太湖水危机,主要成因是水体中二甲基三硫醚、二甲基二硫醚含量过高而引发水体发臭。除了一部分是藻类腐烂分解产生外,大部分硫醚类物质来源于沉积物扩散释放到上覆水体中。因此掌握沉积物中硫醚类的环境信息至关重要。
随着研究工作的深入发展,简单的定性或半定量地获取沉积物中硫醚类物质的含量及种类已不能满足需求精确获悉硫醚类物质在沉积物-水界面环境地球化学信息。有关分析化学工作中要求沉积物中硫醚类物质的快速、精确地提取方法已成为目前硫醚类化物研究的制约瓶颈,掌握其快速精确的前处理方法更为深入研究硫醚类化合物在湖泊水体的环境地球化学行为、掌握其在沉积物水界面的扩散机制和科学地指导黑臭水体治理基石,具有着重要的科技支撑意义。
发明内容
本发明旨在提供一种沉积物中硫醚类挥发性化合物的测定前处理方法,所述的硫醚类物质的测定前处理方法应用于湖泊、水库或河道局部厌氧水体及底泥嗅味物质种类及含量的快速检测。
为实现上述目的,本发明采用如下技术方案:
一种沉积物中硫醚类致臭物质的测定前处理方法,所述的方法包括以下步骤:
(1)样品采集和避光密封保存。利用柱状沉积物采泥器从湖泊或河道采集的新鲜沉积物柱状芯样并保留一定长度的水柱,剔除泥样中石块、螺丝、河蚬及植物根系等动植物残体。收集其中若干新鲜泥样迅速装入棕色玻璃瓶中且保留1cm左右水面,然后密封。
(2)样品保鲜及厌氧预处理。在新鲜沉积物表层加入适量的0.1%HgCl2灭菌,同时加入若干剂量干冰,保持样品冷藏同时营造沉积物表层厌氧环境。最后将棕色样品瓶放入液氮罐冷藏保存,并及时运回实验室待测。
(3)硫醚类物质提取。物质提取为两步连续提取法,包含第一步的醇/水交换步骤和第二步混合提取剂超声萃取。
第一步醇/水交换:首先称取若干沉积物样品于离心管中,按照一定的固液比加入无水甲醇和NaCl,充分震荡,然后离心、静置后收集上清液,重复进行三次,最后合并上述三次提取的上清液备用。
第二步混合提取剂超声萃取:在第一步提取后的残渣泥样中按照一定固液比加入甲醇/环己烷混合提取溶液,在一定温度下的超声细胞破碎仪器中进行超声萃取。连续重复三次,最后合并三次的提取超声萃取液备用。
(4)沉积物提取液的纯化。收集第一步及第二步的提取液合并,然后在固相萃取柱以一定流速进行对提取液中的杂质进行分离纯化。最后利用乙酸乙酯溶液进行洗脱,收集洗脱并在旋转蒸发仪上浓缩后待测。
(5)样品测定。将浓缩后的待测液上色谱仪器测定,具体仪器检测参数设定及样品进样要求参照水体中硫醚类物质样品测定。
上述步骤(1)中一定长度的水柱:具体为尽量保障表层沉积物厌氧环境不受影响,水柱长度一般为10~50cm,以保障底层水体氧动态短时间内不受表层水体影响。优选20~25cm长的水柱。
上述步骤(2)中0.1%HgCl2的用量一般为5~15ml HgCl2/kg土,干冰用量占瓶泥样上方剩余体积的3/4以上。
上述步骤(3)和(4),为保证沉积物中硫醚类不被空气氧化变质,其以下样品的提取工作均在厌氧环境中进行,优选的装置为大型室内厌氧操作箱。
上述步骤(3)中第一步醇/水交换中固液混合物震荡及离心的温度应保持一致,优选温度为10~15℃。固液比的数值优选为1:2~1:5;上述提取剂甲醇不仅限于此一种,可用乙醇代替。NaCl的添加浓度为10~20%(W/V,氯化钠/甲醇)。
上述步骤(3)第二步混合提取剂超声萃取,针对不同性质沉积物样品上述提取剂的甲醇/环己烷配比为1:0.5~1:3,优选为1:0.5~1:1;提取的固液比为1:2~1:3,超声萃取温度应与第一步提取温度一致。超声萃取时间优选为10~30min。超声萃取仪器装置应选择仪器功率大于800w,频率20KHz。优选功率为900~1200w。上述提取剂甲醇也不仅限于此一种,亦可用乙醇代替。
上述步骤(4)上述固相萃取柱填料为Florisil(弗罗里硅土),XAD-16。优选的弗罗里硅土做为固相萃取填料,杂质分离的较为彻底,硫醚类物质在气相色谱谱图干扰物少。固相萃取柱最下端放入2cm长的脱脂棉,然后在填料上下两端各装填2cm长的无水亚硫酸钠,进一步脱水。洗脱液优选为乙酸乙酯,脱液流速控制在5~15ml/min进行硫醚类物质解析。优选洗脱液流速为7ml/min。将洗脱液在旋转蒸发以上进一步浓缩至1~2ml,然后上气相色谱仪器或气质联用色谱仪器进行检测。
上述步骤(4)中固相萃取填料Florisil(弗罗里硅土)、XAD-16以及无水硫酸钠及脱脂棉在装填层析柱前进行预处理,具体方法为:
弗罗里硅土预处理:称取粒径为100目弗罗里硅土,首先在680℃灼烧8h,放入干燥器中保存。在每次填柱之前首先在140℃下烘6h,冷却至室温后,加入5%的重蒸馏水脱活,混合摇匀1h后,置密封容器中。
XAD-16预处理:用95%的乙醇浸泡24h,然后用去离子水淋洗至洗脱液与水混合不呈白色浑浊为止,再用蒸馏水洗至无醇味为止。加入4%盐酸溶液浸泡树脂5h,然后用去离子水洗至中性;再用5%的NaOH溶液浸泡树脂5h,用去离子水洗至中性。在真空泵下进行抽滤,至不滴水为止,备用。
无水硫酸钠预处理:在500℃高温炉中烘制4h,冷至室温后,收集于广口玻璃瓶中密封贮存备用。
脱脂棉预处理:用环己烷蒸汽回流16h,取出晾干后备用。
本发明的有益效果:(1)发明中涉及样品的采集、保存可最大限度地保障底泥中硫醚类物质在离开水生态系统后的赋存形态、数值及种类为原始状态。(2)本发明两步连续提取法可同步提取且有效纯化及沉积物中多种硫醚类物质,而在气象色谱检测时样品测定谱图不受杂质峰掩盖或重叠干扰。(3)发明涉及泥样中硫醚类物质在提取及纯化过程提取温度、时间、仪器超声功率的选择、固相萃取柱的选择、洗脱液及流速等诸多参数进行优化,最大限度保障较高的样品加标回收率,在萃取过程中总的加标回收率为85~115%,完全满足样品测定需求。
本发明的技术进步性:本发明的涉及沉积物中二甲基二硫醚等物质的提取方法,可快速且精确地提取沉积物中大部分组分,提取加标回收率为85~114%,满足样品测定需求。采用高效率的超声提取沉积物中硫醚类物质的方法,不仅提出了针对不同性质的沉积物的提取及纯化过程中关键步骤和提取参数完整解决方案,而且针对过程中可能出现硫化物损失的系统误差进行严格控制,包括提取时间在保障提取率稳定的前提下尽可能缩短提取时间,提取温度控制在10~15℃,基本不产生硫醚类物质的挥发。相比传统的索氏提取需要提取近48h,提取过程明显过长,且增大了挥发性硫醚类物质的损失风险,样品的加标回收率会进一步下降,影响测定的准确性。本发明的方法耗时短,提取时间缩短为15min、且在低温下超声萃取大大降低提取过程中待测物质的挥发损失的可能性。
附图说明
图1是太湖梅梁蓝藻区沉积物硫醚类物质种类含量的气相色谱图,其中a为硫化氢,b为甲硫醇,c为二甲基一硫醚,d为二甲基二硫醚,e为二甲基二硫醚。
图2是太湖梅梁湾芦苇湿地沉积物硫醚类物质种类含量的气相色谱图,其中a为硫化氢,b为甲硫醇,c为二甲基一硫醚,d为二甲基二硫醚,e为二甲基二硫醚。
图3是常州武南河河道沉积物硫醚类物质种类含量的气相色谱图谱,其中a为硫化氢,b为甲硫醇,c为二甲基一硫醚,d为二甲基二硫醚,e为二甲基二硫醚。
具体实施方式
下面结合具体实施例和附图说明对本发明的技术方案进行详细描述。本发明的保护范围并不以具体实施方式为限,而是由权利要求加以限定。
实施例1
根据本发明,采集的太湖梅梁湾蓝藻区沉积物样品中硫醚类物质的提取的方法如下:
(1)样品采集和避光密封保存。利用柱状沉积物采泥器从湖泊或河道采集的新鲜沉积物柱状芯样并保留20cm长水柱,剔除泥样中石块、螺丝、河蚬及植物根系等动植物残体。收集表层0~10cm的新鲜泥样,充分混合后取其中30g迅速装入50ml棕色玻璃瓶中且保留1cm左右水面,然后密封。
(2)样品保鲜及厌氧预处理。在新鲜沉积物表层加入5ml的0.1%HgCl2灭菌,同时加入15g干冰,最后将棕色样品瓶放入液氮罐冷藏保存,并及时运回实验室待测。
(3)硫醚类物质提取。
第一步粗提,首先称取5g左右沉积物样品于50ml离心管中,按照1:3固液比加入无水甲醇和10%NaCl溶液,在15℃下充分震荡,然后在15℃下离心机上5000rpm离心10min、静置后收集上清液,重复进行3次,最后合并上述三次提取的上清液备用。
第二步混合提取剂超声萃取。在第一步提取后的残渣泥样中按照1:2固液比加入配比为1:0.5的甲醇/环己烷混合提取溶液,在超声细胞破碎仪器(仪器超声强度的功率900w)中15℃温度下的进行超声萃取15min。然后在15℃下离心机上5000rpm离心10min、静置后收集上清液,连续重复3次,最后合并3次的提取超声萃取液备用。
(4)提取液的纯化。收集第一步及第二步的提取液并合并,用承接有无水亚硫酸钠的脱脂棉进一步脱水,然后在Florisil(弗罗里硅土)固相萃取柱进行纯化,Florisil(弗罗里硅土)长度为25cm长,以5ml/min流速进行对提取液中的杂质进行分离纯化。最后利用50ml乙酸乙酯溶液进行洗脱,重复3次。收集洗脱并在旋转蒸发上浓缩至1ml备用,然后待测。
固相萃取填料Florisil(弗罗里硅土)以及无水硫酸钠及脱脂棉在装填层析柱前进行预处理,具体方法为:
弗罗里硅土预处理:称取粒径为100目弗罗里硅土,首先在680℃温度下灼烧8h,放入干燥器中保存。在每次填柱之前首先在140℃下烘6h,冷却至室温后,加入5%的重蒸馏水脱活,混合摇匀1h后,置密封容器中。
无水硫酸钠预处理:在500℃高温炉中烘制4h,冷至室温后,收集于广口玻璃瓶中密封贮存备用。
脱脂棉预处理:用环己烷蒸汽回流16h,取出晾干后备用。
(5)样品测定。将浓缩后的待测液上安捷伦气相色谱仪器测定,具体Agilent7890A GC-FPD测定条件:载气为高纯He,流量为3mL/min;氢气流量:50mL/min;空气流量:65.0mL/min;尾吹流量(He):30.0mL/min;进样口温度:250℃,无分流进样;检测器温度:250℃;柱初始温度为50℃,保持5min,以20℃/min升温至250℃,保持7min。
经测定,图1为太湖梅梁湾沉积物中硫醚类物质在蓝藻区沉积物的分布信息,为科学评估硫醚类物质在沉积物-水界面扩散通量提供强有力的技术支撑。
实施例2
根据本发明,采集的太湖梅梁湾芦苇湿地沉积物样品中硫醚类物质的提取的方法如下:
(1)样品采集和避光密封保存。利用柱状沉积物采泥器从湖泊或河道采集的新鲜沉积物柱状芯样并保留22cm长水柱,剔除泥样中石块、螺丝、河蚬及植物根系等动植物残体。收集表层0~10cm的新鲜泥样,充分混合后取其中30g迅速装入50ml棕色玻璃瓶中且保留1cm左右水面,然后密封。
(2)样品保鲜及厌氧预处理。在新鲜沉积物表层加入10ml的0.1%HgCl2灭菌,同时加入15g干冰,最后将棕色样品瓶放入液氮罐冷藏保存,并及时运回实验室待测。
(3)硫醚类物质提取。
第一步粗提,首先称取5g左右沉积物样品于50ml离心管中,按照1:2固液比加入无水乙醇和20%NaCl溶液,在10℃下充分震荡,然后在10℃下离心机上5000rpm离心10min、静置后收集上清液,重复进行3次,最后合并上述三次提取的上清液备用。
第二步混合提取剂超声萃取。在第一步提取后的残渣泥样中按照1:3固液比加入配比为1:1的乙醇/环己烷混合提取溶液,在超声细胞破碎仪器(仪器超声强度的功率1200w)中10℃温度水浴下的进行超声萃取10min。然后在10℃下离心机上5000rpm离心10min、静置后收集上清液,连续重复3次,最后合并3次的提取超声萃取液备用。
(4)提取液的纯化。收集第一步及第二步的提取液并合并,用承接有无水亚硫酸钠的脱脂棉进一步脱水,然后在XAD-16树脂填料的固相萃取柱进行纯化,XAD-16树脂填充长度为25cm长,以7ml/min流速进行对提取液中的杂质进行分离纯化。最后利用50ml乙酸乙酯溶液进行洗脱,重复3次。收集洗脱并在旋转蒸发上浓缩至1ml备用,然后待测。
固相萃取填料XAD-16,以及无水硫酸钠及脱脂棉在装填层析柱前进行预处理,XAD-16预处理方法如下:
用95%的乙醇浸泡24h,然后用去离子水淋洗至洗脱液与水混合不呈白色浑浊为止,再用蒸馏水洗至无醇味为止。加入4%盐酸溶液浸泡树脂5h,然后用去离子水洗至中性;再用5%的NaOH溶液浸泡树脂5h,用去离子水洗至中性。在真空泵下进行抽滤,至不滴水为止,备用。
无水硫酸钠及脱脂棉预处理方法同实施例1。
(5)样品测定。将浓缩后的待测液上安捷伦气相色谱仪器测定,具体Agilent7890A GC-FPD测定条件:载气为高纯He,流量为3mL/min;氢气流量:50mL/min;空气流量:65.0mL/min;尾吹流量(He):30.0mL/min;进样口温度:250℃,无分流进样;检测器温度:250℃;柱初始温度为50℃,保持5min,以20℃/min升温至250℃,保持7min。
经测定,图2为太湖梅梁湾沉积物中硫醚类物质在芦苇湿地沉积物的分布信息,为科学评估硫醚类物质在沉积物-水界面扩散通量提供强有力的技术支撑。
实施例3
1、利用本发明的技术方案,采集的河道沉积物进行提取硫醚类的前处理:
(1)样品采集和避光密封保存。利用柱状沉积物采泥器从湖泊或河道采集的新鲜沉积物柱状芯样并保留25cm长水柱,剔除泥样中石块、螺丝、河蚬及植物根系等动植物残体。收集表层0~10cm的新鲜泥样,充分混合后取其中25g迅速装入50ml棕色玻璃瓶中且保留1cm左右水面,然后密封。
(2)样品保鲜及厌氧预处理。在新鲜沉积物表层加入15ml的0.1%HgCl2灭菌,同时15g干冰,最后将棕色样品瓶放入液氮罐冷藏保存,并及时运回实验室待测。
(3)硫醚类物质提取。
第一步粗提,首先称取5g左右沉积物样品于50ml离心管中,按照1:5固液比加入无水甲醇和15%NaCl溶液,在12℃下充分震荡,然后在12℃下离心机上5000rpm离心10min、静置后收集上清液,重复进行3次,最后合并上述三次提取的上清液备用。
第二步混合提取剂超声萃取。在第一步提取后的残渣泥样中按照1:2.5固液比加入配比为1:3的甲醇/环己烷混合提取溶液,在超声细胞破碎仪器(仪器超声强度的功率1000w)中12℃温度下的进行超声萃取30min。然后在12℃下离心机上5000rpm离心10min、静置后收集上清液,连续重复3次,最后合并3次的提取超声萃取液备用。
(4)提取液的纯化。收集第一步及第二步的提取液并合并,用承接有无水亚硫酸钠的脱脂棉进一步脱水,然后在XAD-16固相萃取柱进行纯化,XAD-16树脂填料的填充长度为25cm长,以15ml/min流速进行对提取液中的杂质进行分离纯化。最后利用50ml乙酸乙酯溶液进行洗脱,重复3次。收集洗脱并在旋转蒸发上浓缩至1ml备用,然后待测。
固相萃取填料XAD-16,以及无水硫酸钠及脱脂棉在装填层析柱前进行预处理,预处理方法同实施例2。
(5)样品测定。将浓缩后的待测液上安捷伦气相色谱仪器测定,具体Agilent7890A GC-FPD测定条件:载气为高纯He,流量为3mL/min;氢气流量:50mL/min;空气流量:65.0mL/min;尾吹流量(He):30.0mL/min;进样口温度:250℃,无分流进样;检测器温度:250℃;柱初始温度为50℃,保持5min,以20℃/min升温至250℃,保持7min。
经测定,图3为常州武南河河道沉积物中硫醚类物质在芦苇湿地沉积物的分布信息,为科学评估硫醚类物质在沉积物-水界面扩散通量提供强有力的技术支撑。通过河道沉积物中硫醚类物质的测定,可及时准确掌握硫醚类物质在沉积物的垂向及水平空间分布信息,为进一步实施生态工程消除河道黑臭提供技术支撑。
Claims (9)
1.一种沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述方法包括以下步骤:
(1)样品采集和避光密封保存:利用柱状沉积物采泥器从湖泊或河道采集的新鲜沉积物柱状芯样并保留20~25cm长的水柱,剔除泥样中石块、和动植物残体;收集其中若干新鲜泥样迅速装入棕色玻璃瓶中且保留1cm左右水面,然后密封;
(2)样品保鲜及厌氧预处理:在新鲜沉积物表层加入0.1%HgCl2灭菌,同时加入干冰,保持样品冷藏同时营造沉积物表层厌氧环境,最后将棕色样品瓶放入液氮罐冷藏保存;
(3)硫醚类物质提取:物质提取为两步连续提取法,包含第一步的醇/水交换步骤和第二步混合提取剂超声萃取:
第一步醇/水交换:首先称取若干沉积物样品于离心管中,按照1:2~1:5的固液比加入无水甲醇和NaCl或无水乙醇和NaCl,充分震荡,然后离心、静置后收集上清液,重复进行三次,最后合并上述三次提取的上清液备用;
第二步混合提取剂超声萃取:在第一步提取后的残渣泥样中按照1:2~1:3的固液比加入配比为1:0.5~1:3的甲醇/环己烷或乙醇/环己烷混合提取溶液,后在超声细胞破碎仪器中进行超声萃取,连续重复三次,最后合并三次的提取超声萃取液备用;
(4)沉积物提取液的纯化:收集合并步骤(3)中两步提取的提取液,用承接有无水亚硫酸钠的脱脂棉进一步脱水,然后在固相萃取柱以5~15ml/min流速进行对提取液中的杂质进行分离纯化;最后利用乙酸乙酯溶液进行洗脱,收集洗脱并在旋转蒸发仪上浓缩后待测。
2.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(2)中0.1%HgCl2的用量为5~15ml HgCl2/kg土。
3.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(3)的提取操作在室内厌氧箱中进行。
4.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(3)硫醚类物质提取温度为10~15℃,提取时间为10~30min。
5.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(3)醇水交换过程中NaCl的添加浓度为10~20%W/V。
6.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(3)混合提取剂超声萃取过程混合提取液中甲醇或乙醇和环己烷的配比为1:0.5~1:1。
7.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(3)中超声萃取仪器装置仪器功率为900W~1200W。
8.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(4)中固相萃取柱填料为Florisil(弗罗里硅土),XAD-16。
9.根据权利要求1所述沉积物中硫醚类致臭物质的测定前处理的方法,其特征在于,所述步骤(4)中的固相萃取填料Florisil(弗罗里硅土)、XAD-16,以及无水硫酸钠及脱脂棉在装填层析柱前进行预处理,具体方法为:
弗罗里硅土预处理:称取粒径为100目弗罗里硅土,首先在680℃温度下灼烧8h,放入干燥器中保存;在每次填柱之前首先在140℃下烘6h,冷却至室温后,加入5%的重蒸馏水脱活,混合摇匀1h后,置密封容器中;
XAD-16预处理:用95%的乙醇浸泡24h,然后用去离子水淋洗至洗脱液与水混合不呈白色浑浊为止,再用蒸馏水洗至无醇味为止;加入4%盐酸溶液浸泡树脂5h,然后用去离子水洗至中性;再用5%的NaOH溶液浸泡树脂5h,用去离子水洗至中性;在真空泵下进行抽滤,至不滴水为止,备用;
无水硫酸钠预处理:在500℃高温炉中烘制4h,冷至室温后,收集于广口玻璃瓶中密封贮存备用;
脱脂棉预处理:用环己烷蒸汽回流16h,取出晾干后备用。
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