将氨浸渣试样用硝酸-硫酸-磷酸混合酸溶解-氢氧化钠分离,2 mol/L的硫酸介质中,在Cu~(2+)催化下,以硫脲将Mo(Ⅵ)还原为Mo(Ⅴ),与硫氰酸盐生成琥珀色配合物,借此进行光度法直接测定.重点研究样品的分解方法、共存元素的干扰以及干扰消除方法等.并采用重量法、全差式光度法和硫氰酸盐直接光度法(本法)3种分析方法,对同一试样分别独立地进行8次测定,将测定结果进行比较.结果表明:本法操作简便,分析结果有较高的精密度、准确度,对氨浸渣中钼的测定达到满意的效果,优于钼酸铅重量法.
The ammonia leaching residue sample was dissolved by HNO_3-H_2SO_4-H_3PO_4 mixed acid and separated by NaOH. With Cu~(2+) and 2 mol/L H_2SO_4, Mo(VI) was reduced to Mo(V) by thiourea, then reacted with thiocyanate to form amber complexes which was used for the determination of Mo by spectrophotometric method. The sample digestion method, co-existence elements interference and their elimination were studied. The 8-time experimental results of the same samples by the proposed method were compared with that of gravimetric method and full-differential spectrophotometric method. The results indicate that the proposed method is simple, accurate and high-precision, and fit to the determination of Mo in ammonia leaching residue with satisfactory effects, prior to gravimetric method.
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