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络合滴定法测定高合金材料中的铜一般均需要分离.作者研究了硫氰酸亚铜均相沉淀分离的条件,发现1mg以上的铜在高氯酸介质中,加3g柠檬酸、0.5g硫氰酸钠和适当的抗坏血酸,铜以硫氰酸亚铜能定量沉淀.大量钾、钠、钙、镁,高至1g的铁,0.5g钴、铝,0.4g镍、铬、钨,0.2g锰、锌、锡、钒0.1g铅、硅、钼、铌、锆、钛,0.05g稀土和大量氟离子、酒石酸、草酸均不干扰.在酸性溶液中沉淀,EDTA也不干扰.沉淀溶解氧化后,于pH5用EDTA法测定.
Complexometric titration of copper in high alloyed materials generally needs to be separated. The authors studied the conditions for the homogeneous precipitation of cuprous thiocyanate and found that 1mg of copper in perchloric acid medium, add 3g of citric acid, 0.5g Sodium thiocyanate and appropriate ascorbic acid, copper is quantitatively precipitated with cuprous thiocyanate Large amounts of potassium, sodium, calcium, magnesium, up to 1 g of iron, 0.5 g of cobalt, aluminum, 0.4 g of nickel, chromium, tungsten, 0.2 g manganese, zinc, tin, vanadium 0.1g lead, silicon, molybdenum, niobium, zirconium, titanium, 0.05g rare earth and a large amount of fluoride ions, tartaric acid, oxalic acid are not disturbed precipitation in an acidic solution, EDTA does not interfere precipitation dissolved After oxidation, the pH was determined by EDTA method.