本文選題：錸粉 + 錸�。� 參考：《冶金分析》2017年07期

【摘要】：通過(guò)先測(cè)定錸粉產(chǎn)品中雜質(zhì)元素總含量,再用差減法計(jì)算錸含量的方法較為繁瑣。根據(jù)低溫氫還原時(shí),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(huì)被揮發(fā)除去這一基本原理,實(shí)驗(yàn)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(jì)算錸的含量,最終實(shí)現(xiàn)了氫還原重量法測(cè)定錸酸銨制備錸粉中錸的方法。確定的實(shí)驗(yàn)條件如下:樣品量約1.0g;采用分段升溫方式進(jìn)行氫還原,其程序?yàn)橄仁覝厣郎刂?00℃,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(shí)驗(yàn)方法適用于錸粉中不揮發(fā)雜質(zhì)元素總質(zhì)量分?jǐn)?shù)不大于0.010%時(shí)錸的測(cè)定。將實(shí)驗(yàn)方法用于3個(gè)錸粉管理樣品、4個(gè)錸粉實(shí)際樣品中99.824%~99.995%錸的測(cè)定,測(cè)定值與參考值基本一致,相對(duì)標(biāo)準(zhǔn)偏差(n=9~22)為0.001 2%~0.003 3%,加標(biāo)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(hào)：1883223