CN101738389A - 离子液体作为萃取剂测量水体中的低含量挥发酚 - Google Patents
离子液体作为萃取剂测量水体中的低含量挥发酚 Download PDFInfo
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Abstract
按照GB-7490-87的4-氨基安替比林方法测量水体中低含量挥发酚的方法,取待测试样溶液250mL(挥发酚的浓度为0.002-0.50mg/L的苯酚)置于500mL分液漏斗中,向其中分别加入2mL缓冲液,1.5mL 4-氨基安替比林溶液,混匀,加入1.5mL铁氰化钾溶液,再混匀。静置10min显色。向分液漏斗中加入1-丁基-3-甲基咪唑六氟磷酸盐10mL,振荡萃取2min,静置分层,将下层离子液体层直接放入1cm比色皿,在分光光度计上选用的波长是440nm测量。
Description
技术领域
本发明涉及离子液体作为萃取剂测量水体中的低含量挥发酚。具体地说,通过选择合适的离子液体代替氯仿作为萃取剂,可以实现水体中的低含量挥发酚的测量,且离子液体可回收重复利用。
背景技术
酚和它的衍生物对人和水生生物是有毒的,并且被列为最常见和最严重的环境污染物之一。酚在河流和水库中天然地有极低的容许浓度,但人类排入过多会引起酚富集进而严重影响水质并且对公众健康引起潜在的伤害[参见:Rosana M.Alberici,Regina Sparrapan.Environ.Sci.Technol 2001,35,2084-2088]。酚类化合物是芳香族羟基化合物,一般可分为一元酚,二元酚及多元酚。根据酚类能否与水蒸气一起蒸出,分为挥发酚(沸点在230℃以下)与不挥发酚(沸点在230℃以上)[参见:郭伟,林守麟.在线膜过滤流动注射-分光光度法直接测定废水中酚.岩矿测试,2005,24(4),245-248]。一元酚除对硝基酚外,各种甲酚、二甲酚、氯酚及硝基酚等沸点均在230℃以下,多属于挥发性酚。
酚类化合物毒性不大,但多有恶臭,特别是苯酚等,在饮用水加氯消毒时能形成臭味更强的氯酚,引起水质异味。酚类为原生质毒物,属高毒类物质,在人体富集时出现头痛、贫血,水中酚含量达0.1~0.2mg/L时会导致生长的鱼虾有异味,浓度大于5mg/L时,会导致水生物中毒死亡[参见:杨亚玲,胡秋芬,杨光宇.固相萃取光度法测定饮用水中的酚,分析化学,2002,30(2),888.]。酚类污染物主要来自主要来自炼油、煤气洗涤、炼焦、造纸和化工等行业[参见:杨安平,李步海,孙小梅.曲拉通增敏的分光光度法测定水中挥发酚类,化学与生物工程,2006,23(9),57-59.]。天然水中一般不含酚类化合物,但受到某些工业废水污染后可检出。
挥发酚类的测定方法通常有容量法、分光光度法、气相色谱法和流动注射分析法(FIA)等后者主要有FIA-安培法,FIA-气体扩散膜电极法,FIA-分光光度法[参见:吴宏,王镇浦.水中痕量挥发性酚类的流动注射-分光光度测定,南京化工大学学报,1999,21(6),60-62]。以上多种方法中尤以4-氨基安替比林分光光度法[参见:GB/T 7490-87]应用最广,而对高浓度含酚废水则可采用溴化容量法。无论哪种方法,当水样中存在氧化剂、还原剂、油类及某些金属离子时,均应设法消除并进行预蒸馏。
用蒸馏法使挥发性酚化合物蒸馏出,并与干扰物和固定剂分离,由于酚类化合物的分离速度随着蒸馏液的体积变化,因此蒸馏液体积必须与样品体积相等。被蒸馏出来的化合物,在pH=10.0+0.2条件及铁氰化钾溶液存在下,与4-氨基安替比林反应生成橙红色的安替比林染料,再用10mL氯仿将染料从水溶液中萃取出,于460nm波长下测定其吸光度,酚颜色变化与吸光度成正比,这是最常用的分析方法,也是国标方法。但实验中使用的氯仿是一种强挥发性的有毒溶剂。
还没有文献报道使用绿色环保的离子液体作为萃取剂测量水体中的低含量挥发酚。
发明内容
本发明的目的是提供一种离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚。
本发明的技术方案如下:
按照国标GB-7490-874-氨基安替比林比色法,取待测试样溶液250mL(挥发酚的浓度为0.002-0.50mg/L的苯酚)置于500mL分液漏斗中,向其中分别加入2mL缓冲液,1.5mL 4-氨基安替比林溶液,混匀,加入1.5mL铁氰化钾溶液,再混匀。静置10min显色。向分液漏斗中加入1-丁基-3-甲基咪唑六氟磷酸盐,振荡萃取,静置分层,将下层离子液体层直接放入1cm比色皿,在分光光度计上测量。
上述离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚的方法,向分液漏斗中加入1-丁基-3-甲基咪唑六氟磷酸盐是10mL。
上述离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚的方法,振荡萃取的时间为2min。
上述离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚的方法,在分光光度计上测量选用的波长是440nm。
本发明使用的离子液体1-丁基-3-甲基咪唑六氟磷酸盐([BMIM]PF6),极低挥发性,无毒,不污染环境,萃取效率高,且易回收。
附图说明
图1为本发明中测量离子液体中挥发酚显色物质的测定波长选择图。
具体实施方式
实施例1.利用这种萃取方法,配制标准的苯酚溶液作为测定对象,测量其含量。
按照国标GB-7490-874-氨基安替比林比色法,取标准配制的浓度为0.10mg/L的苯酚溶液250mL置于500mL分液漏斗中,向其中分别加入2mL缓冲液,1.5mL 4-氨基安替比林溶液,混匀,加入1.5mL铁氰化钾溶液,再混匀。静置10min显色。
向分液漏斗中加入10mL1-丁基-3-甲基咪唑六氟磷酸盐,振荡2min萃取,静置分层,将下层离子液体层直接放入1cm比色皿,在波长440nm处测量。
以标准曲线法测量,溶液中含酚量0.095mg/L。
实施例2.
取实际水样,含酚约0.05mg/L,其它都同实施例1,实际检测结果为0.052mg/L。
实施例3.
取实际水样,含酚约0.45mg/L,其它都同实施例1,实际检测结果为0.043mg/L。
Claims (4)
1.离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚,其特征是:在测量水体中的低浓度挥发酚时,以1-丁基-3-甲基咪唑六氟磷酸盐([BMIM]PF6)作为萃取剂,萃取后用分光光度计检测离子液体中有色物质的吸光度,根据吸光度的大小计算水体中挥发酚的含量。
2.根据权利要求1所述的离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚,其特征是:用与溶液比为1∶25的体积比的离子液体,以250mL的溶液测量,则应用10mL1-丁基-3-甲基咪唑六氟磷酸盐([BMIM]PF6)。
3.根据权利要求1所述的离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚,其特征是:萃取时间为2min。
4.根据权利要求1所述的离子液体替代氯仿作为萃取剂测量水体中的低含量挥发酚,其特征是:在波长为440nm下测量。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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RU2549452C1 (ru) * | 2013-12-23 | 2015-04-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Экстракционно-флуориметрический способ определения фенолов в водных растворах |
CN105372358A (zh) * | 2015-12-08 | 2016-03-02 | 重庆市中药研究院 | 一种基于离子液体-超声辅助-hplc的昆明山海棠活性成分检测方法 |
CN113354174A (zh) * | 2021-06-21 | 2021-09-07 | 华电水务工程有限公司 | 一种含酚废水萃取脱酚方法 |
CN113567365A (zh) * | 2021-07-05 | 2021-10-29 | 云南省生态环境厅驻昆明市生态环境监测站 | 液液微萃取结合纳米酶检测水中挥发酚的方法 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2549452C1 (ru) * | 2013-12-23 | 2015-04-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государственный университет" | Экстракционно-флуориметрический способ определения фенолов в водных растворах |
CN105372358A (zh) * | 2015-12-08 | 2016-03-02 | 重庆市中药研究院 | 一种基于离子液体-超声辅助-hplc的昆明山海棠活性成分检测方法 |
CN113354174A (zh) * | 2021-06-21 | 2021-09-07 | 华电水务工程有限公司 | 一种含酚废水萃取脱酚方法 |
CN113567365A (zh) * | 2021-07-05 | 2021-10-29 | 云南省生态环境厅驻昆明市生态环境监测站 | 液液微萃取结合纳米酶检测水中挥发酚的方法 |
CN113567365B (zh) * | 2021-07-05 | 2023-09-29 | 云南省生态环境厅驻昆明市生态环境监测站 | 液液微萃取结合纳米酶检测水中挥发酚的方法 |
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