所有的酸洗过程都是在1000级净化室和净化室内100级层流超净工作台进行的.超纯水是由Millipore RO和Milli—Q Element超纯水系统制备.3种纯度的硝酸选用Merck公司试剂纯硝酸、Fisher公司“TraeeMetal”级和“Optima”级超纯硝酸.各种与样品直接接触的容器及相关工具、耗材主要选用Nalgene低密度聚乙烯和特氟隆材料制成的产品.酸洗程序是在四周时间内把样品瓶等依次浸泡在四遍不同浓度和纯度逐渐增加的硝酸溶液里进行清洗.除了第一遍酸洗是在室温下进行的以外,后三遍酸洗都是用加热板加热使硝酸溶液表面温度保持在45℃左有.用Finnigan MAT Element电感耦合等离子体质谱仪(ICP-MS)对该方法酸洗的样品瓶进行了空白检验,结果表明:所有测量的重金属元素的浓度都低于检测限.该方法对促进我国极地雪冰重金属研究具有重要意义,也可应用到其它环境介质中超痕量重金属分析.
All acid cleaning was performed inside a class 1000 clean room and class 100 laminar flow clean benches. The ultrapure water was produced by Millipore RO (Reverse Osmosis) water purification system and Milli-Q water purification system. The three purity grades of the nitric acid are the Merck reagent grade HNOa, the Fisher "TraceMetal" grade HNO3 and the purest Fisher "Optima" grade HNO3. The various bottles, containers and other labwares mainly ordered from Nalgene, Nalge Company, which are in contact with the samples, are made of low density polyethylene and FEP or PFA Teflon material. The acidcleaning procedure of all the bottles and containers mainly followed a successive four times cleaning through immersion in increasing purity at different concentration nitric acid bathes during four weeks.Except the first time acid-cleaning was performed at room temperature, the last three acid-cleanings were heated on hotplates with a temperature of 45℃ of acid solutions. In order to verify the validity of acid-cleaning method, the cleaned sample bottles were performed blank determination using Finnigan MAT Element double focusing inductively coupled plasma spectrometry (ICP-MS). The results show that all measured heavy metals were below the limits of detection (LOD). Although the acidcleaning method is developed mainly for the relia ble measurement of the ultra low concentration heavy meals in Antarctic and Arctic snow and ice samples, it also can be used for ultra low concen-tration heavy metals in other environmental samples.