靛酚法测定快堆冷却剂钠中微量氮  

Spectrophotometric determination of nitrogen in sodium as indophenol

作　　者：谢淳[1] 李煦[1] 徐迟[1] 贾云腾[1] 俞晓琛[1] 

机构地区：[1]中国原子能科学研究院,北京102413

出　　处：《核科学与工程》2011年第4期310-316,共7页Nuclear Science and Engineering

摘　　要：研究和建立了快中子反应堆冷却剂钠中微量氮的分析方法。该法在氩气保护、液氮冷却下,钠样品溶于去离子水中,加去离子水稀释,蒸馏,以氨的形式释放出的氮用0.1mol/L盐酸吸收后,加入次氯酸钠、苯酚进行显色,用分光光度计进行比色测定。工作中选择了756MC型分光光度计的最佳工作条件,比色条件和溶样装置,采用标准加入法进行了回收实验,方法的回收率为88.0%～102.0%,相对标准偏差为±4.8%,用建立的分析方法测定了内蒙古和洛阳工业钠以及中国实验快堆核级钠中的杂质氮,取得了满意的结果。因此,用此方法来分析各种纯度级钠中微量氮是可行的。An analytical method has been developed to determinate trace levels of nitrogen in sodium coolant fast reactor.The sodium is dissolved in deionized water with argon covering and liquid nitrogen cooling.The solution is diluted with deionized water and distilled,and the nitrogen is released out in the form of ammonia.The ammonia is absorbed in a dilute hydrochloric acid solution（0.1 mol/L） and converted to indophenol by the reaction with sodium hypochlorite and phenol.The blue color solution developed is measured photometrically.The work conditions of 756MC spectrometer,colorimetric conditions and the devices for dissolving sodium sample have been studied.Standard addition experiments are carried out with ammonium chloride.The recovery percentage is 88.0%~102.0% and relative standard deviation is ±4.8%.Satisfying results have been acquired when nitrogen in the industrial sodium produced by Iner-Mongolia and Luoyang and nuclear grade sodium of China Experimental Fast Reactor are analyzed by the method.Therefore,the analytical method can be used to determinate the impurity of nitrogen in sodium of various purity grade.

关 键 词：金属钠 次氯酸钠 苯酚 分光光度法 

分 类 号：TL43[核科学技术—核技术及应用]