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测定岩石、矿石中的铅一般采用直接极谱法,为更准确地分析微量铅,需分离伴生元素。共沉淀法分离铅早有应用,本实验用预先煮沸的碳酸钠溶液将锶铅的硫酸共沉淀物进行快速热转化,沉淀易“形成块状”的问题得到解决,提高了铅的转化回收率,并以吸滤法代替两次漏斗过滤,使本法操作快速简易、结果准确稳定。本法空白恒定、检测下限低(0.05微克·毫升~(-1)),适于分析组分较复杂的样品。仪器与试剂 JP-1A型示波极谱仪及MK-Ⅲ型方波极谱仪;滴汞电极,银片或铂丝螺旋对极。氨性碳酸钠溶液:10%,100克结晶碳酸钠(三级)、0.5克明矾和20毫升浓氨水(二级),制成1升溶液,澄清后使用。
Determination of rock, ore lead generally adopt direct polarography, in order to more accurately analyze trace lead, the need to separate associated elements. The coprecipitation method for the separation of lead has been used for a long time. In this experiment, the pre-boiled sodium carbonate solution was used to rapidly convert the strontium-lead sulfuric acid coprecipitate to precipitate, and the problem of “forming lumps” was solved and the conversion of lead was improved Recovery rate, and filtration instead of two funnel filtration filtration method to make this method quick and easy operation, the result is accurate and stable. This method has a constant blank and low detection limit (0.05 μg · mL -1), which is suitable for the analysis of more complex samples. Instruments and reagents JP-1A oscillopolarography and MK-Ⅲ square wave polarography; drop mercury electrode, silver or platinum wire spiral pole. Ammonia sodium carbonate solution: 10%, 100 g of crystalline sodium carbonate (third grade), 0.5 g of alum and 20 ml of concentrated ammonia (second grade), made of 1 liter of solution, used after clarification.