炭质页岩及矿化炭质页岩中锇钌的测定

Determination of osmium and ruthenium in carbonaceousshale and mineralized carbonaceous shale

由于炭质页岩及矿化炭质页岩中有较高的碳、硫及有机物 ,无法直接用过氧化钠熔融 ,因此将样品与NH4 Cl、(NH4 ) 2 CO3按 10∶1∶1混合 ,再覆盖一层氢氧化钠作锇、钌保护剂 ,于 5 0 0℃灼烧 ,加速碳、硫及有机物的分解 ,再用过氧化钠分解样品 ;采用一次蒸馏As(Ⅲ ) -Ce(Ⅳ )体系催化光度法测定锇、钌。该方法回收率大于 95 %。

Due to the higher carbon content in carbonaceous shale and mineralized carbon shale,sulfur and organic materials can not be directly smelted.To determine the osmium and ruthenium in the ore,following indicated method should be used.Firstly,mix the sample with NH 4Cl and (NH 4) 2CO 3 together as per the volume ratio of 10∶1∶1,and cover the mixture with a thin layer of NaOH as osmium and ruthenium protective reagent; secondly fire it at 500℃ to speed up the carbon,sulfur and organic materials decomposition; thirdly decompose the mixed sample with Na 2O 2 and finally to determine the osmium and ruthenium through spectrophotometry of As(Ⅲ)-Ce(Ⅳ) system.The method has osmium and ruthenium recovery more than 95%.