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本文提出在不分离稀土的条件下用硅钼兰分光光度法测定微量硅。大量稀土离子的存在有降泜消光值的作用。我们拟用两种办法消除它的干扰:1.参比及校正曲线的各点均加入同量的除硅稀土。2.以试样本身为参比,进行差示比色。对稀土金属试样,采用盐酸溶解,用硝酸氧化还原性离子(如Fe~(+2)、Ti~(+3)等)。对稀土氧化物试样,先用盐酸溶解,再加氢氟酸于60℃水浴上分解30分钟,使硅完全转变为可与钼酸离子反应的形态。生成硅钼黄的酸度选用0.12N。镨、钕离子本身的颜色不影响硅的测定,磷、砷的干扰加入草酸消除。其分析方法简述如下:
In this paper, the determination of trace silicon with silicon molybdenum blue spectrophotometry without separation of rare earths is proposed. The presence of a large amount of rare earth ions has the effect of lowering the extinction. We intend to use two ways to eliminate its interference: 1. Reference and calibration curve of each point are added the same amount of rare earth except silicon. 2. To the sample itself as a reference, for differential colorimetric. For rare earth metal samples, hydrochloric acid is used to dissolve and nitric acid is used to oxidize and reduce ions (such as Fe ~ (+2), Ti ~ (+3), etc.). Rare earth oxide samples, first dissolved in hydrochloric acid, and then add hydrofluoric acid in 60 ℃ water bath decomposition for 30 minutes, so that silicon can be completely converted to molybdate ion reaction form. Generation of silicon molybdenum yellow acidity use 0.12N. Praseodymium, neodymium ion itself does not affect the color of the determination of silicon, phosphorus, arsenic interference added oxalic acid elimination. The analysis method is as follows: