本文選題：錸粉 + 錸��； 參考：《冶金分析》2017年07期

【摘要】：通過先測定錸粉產(chǎn)品中雜質(zhì)元素總含量,再用差減法計算錸含量的方法較為繁瑣。根據(jù)低溫氫還原時,除了錸氧化物Re_2O_7、ReO_2,共存金屬雜質(zhì)元素和他們的氧化物均被還原為金屬單質(zhì)而不揮發(fā)外,其余非金屬元素和他們的氧化物,以及水分、銨鹽均會被揮發(fā)除去這一基本原理,實驗提出了采用低溫氫還原樣品,以氫還原前后樣品質(zhì)量之比計算錸的含量,最終實現(xiàn)了氫還原重量法測定錸酸銨制備錸粉中錸的方法。確定的實驗條件如下:樣品量約1.0g;采用分段升溫方式進行氫還原,其程序為先室溫升溫至200℃,恒溫30min后升溫至400℃,接著恒溫30min后升溫至600℃,最后再恒溫30min;將盛有氫還原后錸粉的石英舟置于干燥器中冷卻30min,恒重1次。實驗方法適用于錸粉中不揮發(fā)雜質(zhì)元素總質(zhì)量分數(shù)不大于0.010%時錸的測定。將實驗方法用于3個錸粉管理樣品、4個錸粉實際樣品中99.824%~99.995%錸的測定,測定值與參考值基本一致,相對標準偏差(n=9~22)為0.001 2%~0.003 3%,加標回收率99.99%~100.01%。
[Abstract]:The method of determining the total content of impurity elements in rhenium powder and then calculating the content of rhenium by subtraction method is more complicated. According to the low temperature hydrogen reduction, in addition to the rhenium oxide Re2O7 / ReO _ 2, the metal impurity elements and their oxides are reduced to metallic elements without volatilization, the rest of the non-metallic elements and their oxides, as well as water, Based on the principle that ammonium salts can be removed by volatilization, a new method for the determination of rhenium in rhenium powder by hydrogen reduction gravimetric method is proposed, in which the samples are reduced by hydrogen at low temperature and the mass ratio of samples before and after hydrogen reduction is used to calculate the content of rhenium. The experimental conditions are as follows: sample quantity is about 1.0 g, hydrogen reduction is carried out by means of stepwise heating, which is programmed to increase temperature to 200 鈩，

本文編號：1883223