第31卷 2011年
第3期 9月
核科学与工程
Chinese Journal of Nuclear Science and Engineering
Vol.31 Sep.
真空蒸馏-电位滴定法测定钠中碳
谢
淳，贯云腾，高耀鹅
（中国原子能科学研究院，北京102413)
ON 2011
摘要：快堆冷却剂钠中碳的含量对结构材料的物理和机械性能有影响，为检测钠中碳含量，建立了真空蒸缩-电位滴定测定钠中碳的方法。在氢气气氛下取1~2g钠于石英内，在400℃及6.7X10-Pa 下真空蒸馏除钠，残渣在1100℃下通净化的氧燃烧40min，生成的二氧化碳通人pH为10的BaClz(10头)和Ba(OH)；(0.01N)的吸收剂中，借助于酸碱电位滴定的方法，由消耗的Ba(()H)；量，间接计算出碳的含量。实验中对燃烧和测量等条件做了大量的研究，该法在含碳量为20～100μg范围内，用石墨和Na;CO,为标物做回收实验，回收率分别为(100.9±13.3)%及（102.7±10.1)%。
因此，本分析方
法满足了中国实验快堆(CEFR)钠中碳分析的技术要求，关键词：钠；真空蒸馏；电位滴定
中图分类号：TL43
文献标志码：A
文章编号：0258-0918(2011)03-0230-08
Thedeterminationofcarboninsodiumbyvacuum
distillationpotentiometry XIE Chun,JIA Yun-teng,GAO Yao-peng(China Institute of Atomic Energy, Beijing 102413, China)
Abstract: The amount of carbon in sodium metal which is used as a coolant of fast reactors has the effect on physical and mechanical properties of construction materiais. A method to determine carbon in the primary sodium has been developed. Under the argon atmosphere, 1 ~2 g sodium samples are put into silica crucibles, then crucibles are placed in a stainless steel distillation pot to remove the sodium at 400 C and 6.7 X 10 3 Pa. The residue is combusted at 1 1oo ℃ with pure oxygen for forty minutes. The carbon dioxide formed is collected in a absorbent solution that pH is 10 and measured by potentiometry. Many experiments such as conditions of combustion and measurement and so on have been studied. Standard addition experiments are carried out with graphite and sodium carbonate standards when the content of carbon is at the range of
Within the above range, the recovery rates are (100. 9 ± 13.3)% and
20~100 μg.
(102. 7 ± 10. 1)% respectively. This method has met the technical needs for carbon 收稿日期；2011-07-22；修回日期：2011-08-20
作者简介：谢 230
淳(1964--)，女，湖南人，研究员，硕士，现从事中国实验快堆钠工艺技术的研究工作