CN111579335A - 一种新型循环吹扫吸收蒸馏测定仪 - Google Patents
一种新型循环吹扫吸收蒸馏测定仪 Download PDFInfo
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Abstract
本发明公开了一种新型循环吹扫吸收蒸馏测定仪，适用于食品、药品、环境等领域中易挥发、半挥发或可衍生成挥发性组分的分离、富集及测定。仪器包括释放剂(1)、释放剂泵(2)、释放剂阀(3)、样品瓶(4)、样品温浴槽(5)、冷凝器(6)、吸收瓶(7)、循环气泵(8)、保护气(9)、保护气阀(10)和尾气管(11)。整体采用化学惰性材料，必要时使用惰性气体保护、加热、冷凝等，加快吸收传质，提高分离富集效率，减少分析用时。整体密封设计，易于操作，提高分析的准确度和精密度。
Description
技术领域
本发明适用于分析检测领域的前处理，将挥发性或能转化为挥发性的组分分离、富集后用于测定。加快蒸发的方法有增大表面积、增大表面气体流动、增高温度。本发明使用气路部分增大了接触的表面积和表面的气体流动，同时使用加热部分控制温度，可以大大加快蒸馏过程。
对于易挥发且稳定的气体组分，可直接使用空气吹扫，如二氧化碳、二氧化硫、硫化氢、氟化氢、氨氮、挥发性盐基氮等。对于易挥发却易被氧化破坏的组分，可以采用惰性气体保护，如磷化氢等。对于半挥发的组分，可以通过加热控温再经冷凝的方式，如挥发酚等。对于不易挥发而却可通过衍生形成易挥发的组分，可通过硼氢化钾、氯化亚锡等衍生，如砷、锑、铋、锡、硒、碲、铅、锗、磷等。
对于酸性组分，可使用碱性吸收液，如二氧化碳、二氧化硫、硫化氢、氟化氢、挥发酚等。对于碱性组分，可使用酸性吸收液，如氨氮、挥发性盐基氮等。对于可形成沉淀的组分，可使用沉淀剂吸收，如二氧化碳、二氧化硫、硫化氢等。对于还原性组分，可使用氧化还原法吸收，如砷、锑、铋、锡、硒、碲、铅、锗、磷等的氢化物。
背景技术
在食品、环境、药品、化工、冶金、能源等行业样品的分析测试中，很多复杂基体的样品前处理需要占用大量的人力、物力、财力，尤其是经典的蒸馏技术。蒸馏按照蒸馏压力可分为常压蒸馏、减压蒸馏和加压蒸馏，按照是否吹扫吸收可以分为吹扫蒸馏吸收和非吹扫蒸馏吸收，按照蒸馏热量来源又可以分为一般蒸馏、水蒸气蒸馏，还有特殊的一些蒸馏技术，如共沸蒸馏、油水分离蒸馏等。
如在《饮料通用分析方法》GB/T 12143-2008“7碳酸饮料中二氧化碳的测定方法(蒸馏滴定法)”和《啤酒分析方法》GB/T 4928-2008“11.1二氧化碳基准法”中，均使用了三个吸收管，真空加酸蒸馏法。
如在《葡萄酒、果酒通用分析方法》GB/T 15038-2006的“4.8二氧化硫”中，使用了真空抽气吹扫蒸馏吸收装置。操作过程中，真空度和抽气速度不易控制，样品重复测定精密度和回收率较难保证。而在《淀粉及其衍生物二氧化硫含量的测定》GB/T 22427.13-2008中，为了保证二氧化硫完全吸收，使用了两个起泡器，装置同样复杂，操作繁琐。
如在《粮食卫生标准的分析方法》GB/T 5009.36-2003的“4.3磷化物”和《粮油检验粮食中磷化物残留量的测定分光光度法》GB/T 25222-2010中，使用了氮气或二氧化碳保护的吹扫蒸馏装置，采用多个洗气瓶，三个吸收管，装置及其复杂，操作繁琐。
如在《食品安全国家标准食品中总砷及无机砷的测定》GB 5009.11-2014的“第三法银盐法”中，使用了碘化钾、氯化亚锡将高价砷还原为三价砷，再使用锌粒与酸产生砷化氢，经硝酸银吸收，比色测定。操作中使用玻璃仪器非常容易出现漏气现象，操作时间长达1小时，效率和准确度难以保证。
这些标准操作无疑给日常的分析工作者带来巨大的操作难度和工作量，急需一种简便、快速、有效的前处理技术处理上述问题。
发明内容
本发明以循环吹扫吸收为原理，提出一种增大蒸发面积、增加蒸发表面气体流动和加热控温的一种新型循环吹扫吸收蒸馏测定仪。本发明最大的优势在于释放剂可自动加入，有惰性的保护气保护易变化的目标化合物，同时由循环气泵在密闭环境内增加了目标化合物的气化速度和吸收速度，大大减少样品处理时间，提高实验效率，同时目标化合物的回收率得到保证。
为解决上述蒸馏问题，本发明具有如下部件：释放剂(1)、释放剂泵(2)、释放剂阀(3)、样品瓶(4)、样品温浴槽(5)、冷凝器(6)、吸收瓶(7)、循环气泵(8)、保护气(9)、保护气阀(10)和尾气管(11)，整体采用化学惰性材料设计，整体程序分为：循环吹扫、释放剂加入、循环吸收。
释放剂泵(2)采用蠕动泵，或注射泵，或隔膜泵，或离心泵，流速在1～1000mL/min范围内可调。释放剂阀(3)和保护气阀(10)采用单向球阀，或电磁截止阀，或夹管截止阀，工作压力范围为0～0.5MPa。样品温浴槽(5)采用PID温控模式，使用铝、石墨材质，温度范围为20～200℃内可调。凝器(6)采用PID温控模式，使用聚乙烯(PE)、聚丙烯(PP)、聚四氟乙烯(PTFE)管路、玻璃、石英材质，温度范围为-20～20℃内可调。循环气泵(8)采用隔膜泵，或离心泵，流速在0～20L/min范围内可调。
循环吹扫程序为释放剂泵(2)和释放剂阀(3)关闭，循环气泵(8)和保护气阀(10)打开，保护气(9)将样品瓶(7)和样品瓶(4)系统内的空气替换成为保护气(9)，去除反应活性气体。释放剂加入程序为释放剂泵(2)和释放剂阀(3)打开，循环气泵(8)和保护气阀(10)关闭，加入释放剂(1)，待测物微量释放。循环吸收程序为释放剂泵(2)、释放剂阀(3)和保护气阀(10)关闭，循环气泵(8)打开，待测物从样品瓶(4)被吹扫加速释放，被吸收瓶(7)快速吸收，未被吸收的组分循环重复直至完全吸收。整体程序中样品温浴槽(5)和冷凝器(6)均为打开状态。循环吹扫程序、释放剂加入程序和循环吸收程序运行时间均为1～999秒内可调。
附图说明
图1为本发明的新型循环吹扫吸收蒸馏测定仪的循环吹扫程序工作示意图。
图2为本发明的新型循环吹扫吸收蒸馏测定仪的释放剂加入程序工作示意图。
图3为本发明的新型循环吹扫吸收蒸馏测定仪的循环吸收程序工作示意图。
图1～3中：1、释放剂；2、释放剂泵；3、释放剂阀；4、样品瓶；5、样品温浴槽；6、冷凝器；7、吸收瓶；8、循环气泵；9、保护气；10、保护气阀；11、尾气管。
具体实施方式
1、磷化氢测定模式
称取1g(精确至0.001g)样品于样品瓶(4)内。使用高锰酸钾溶液作为吸收液。启动循环吹扫程序，保护气(9)为氮气，吹扫气压力0.05MPa，循环吹扫1min。启动释放剂加入程序，将0.12mol/L硫酸85mL加入样品瓶(4)内，加液流速为60mL/min，加液时间为85s。继续启动循环吸收程序，循环气流流速为1L/min，循环吸收时间为5min。结束后，使用磷钼酸比色测定测量吸收瓶(7)中磷化氢含量。同时做空白。标准曲线同法处理。
豆类种子中磷化锌质控样品中磷化氢为0.12±0.02(k＝2，p＝95％)mg/kg，实测两次分别为0.109mg/kg、0.112mg/kg，符合要求。
2、总砷和无机砷测定模式
样品经消解处理后，使消解液盐酸浓度为3～5％，吸取一定量的溶液于样品瓶(4)内。使用二乙基二硫代氨基甲酸银-三乙醇胺-三氯甲烷溶液作为吸收液，并使用乙酸铅棉花净化管。启动循环吹扫程序，保护气(9)为氩气，吹扫气压力0.1MPa，循环吹扫1min。启动释放剂加入程序，将20g/L硼氢化钾溶液加入样品瓶(4)内，加液流速为60mL/min，加液时间为30s。继续启动循环吸收程序，循环气流流速为1L/min，循环吸收时间为5min。结束后，于波长520nm处测定吸光度。同时做空白。标准系列溶液同法处理。
质控样品GBW(E)100348中总砷为0.23±0.03(k＝2，p＝95％)mg/kg，实测两次分别为0.239mg/kg、0.242mg/kg，符合要求。
3、二氧化硫测定模式
称取5g(精确至0.001g)样品于样品瓶(4)内。样品温浴槽(5)为150℃，冷凝器(6)为5℃。使用乙酸铅溶液作为吸收液。启动循环吹扫程序，保护气(9)为氮气，吹扫气压力0.05MPa，循环吹扫1min。启动释放剂加入程序，将1+1盐酸10mL加入样品瓶(4)内，加液流速为60mL/min，加液时间为10s。继续启动循环吸收程序，循环气流流速为1L/min，循环吸收时间为5min。结束后，使用碘量法测量吸收瓶(7)中二氧化硫含量。同时做空白。
红酒质控样品中总二氧化硫含量为0.13±0.05(k＝2，p＝95％)g/kg，实测两次分别为0.129mg/kg、0.135mg/kg，符合要求。
Claims (13)
1.一种新型循环吹扫吸收蒸馏测定仪，其特征在于，包括释放剂(1)、释放剂泵(2)、释放剂阀(3)、样品瓶(4)、样品温浴槽(5)、冷凝器(6)、吸收瓶(7)、循环气泵(8)、保护气(9)、保护气阀(10)和尾气管(11)部分。
2.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，整体采用化学惰性材料设计。
3.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，样品处理可分为3个操作程序，分别为循环吹扫、释放剂加入、循环吸收。
4.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，释放剂泵(2)采用蠕动泵，或注射泵，或隔膜泵，或离心泵，流速在1～1000mL/min范围内可调。
5.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，释放剂阀(3)和保护气阀(10)采用单向球阀，或电磁截止阀，或夹管截止阀，工作压力范围为0～0.5MPa。
6.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，样品温浴槽(5)采用PID温控模式，使用铝、石墨材质，温度范围为20～200℃内可调。
7.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，冷凝器(6)采用PID温控模式，使用聚乙烯(PE)、聚丙烯(PP)、聚四氟乙烯(PTFE)管路、玻璃、石英材质，温度范围为-20～20℃内可调。
8.根据权利要求1所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，循环气泵(8)采用隔膜泵，或离心泵，流速在0～20L/min范围内可调。
9.根据权利要求3所述的新型循环吹扫吸收蒸馏测定仪，其特征在于循环吹扫中保护气(9)通过保护气阀(10)通入样品溶液和蒸馏的管路系统中，最终从尾气管(11)排出，其操作程序为释放剂泵(2)和释放剂阀(3)关闭，循环气泵(8)和保护气阀(10)打开，保护气(9)将样品瓶(7)和样品瓶(4)系统内的空气替换成为保护气(9)，去除反应活性气体。
10.根据权利要求3所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，释放剂加入程序为释放剂泵(2)和释放剂阀(3)打开，循环气泵(8)和保护气阀(10)关闭，加入释放剂(1)，待测物微量释放。
11.根据权利要求3所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，循环吸收程序为释放剂泵(2)、释放剂阀(3)和保护气阀(10)关闭，循环气泵(8)打开，待测物从样品瓶(4)被吹扫加速释放，被吸收瓶(7)快速吸收，未被吸收的组分循环重复直至完全吸收。
12.根据权利要求3所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，整体程序中样品温浴槽(5)和冷凝器(6)均为打开状态。
13.根据权利要求3所述的新型循环吹扫吸收蒸馏测定仪，其特征在于，循环吹扫程序、释放剂加入程序和循环吸收程序运行时间均为1～999秒内可调。
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