电感耦合等离子体质谱法测定氮化铝纳米粉中单质铝  

Determination of Elemental Aluminum in Aluminum Nitride Nanometer Powder by Inductively Coupled Plasma Mass Spectrometry

作　　者：杨永明[1,2] 葛宁 YANG Yong-ming;GE Ning(China North Nuclear Fuel Co.,Ltd,Baotou 014035,China;China National Nuclear Corporation Key Laboratory on New Materials Research and Application Development,Baotou 014035,China)

机构地区：[1]中核北方核燃料元件有限公司,内蒙古包头014035 [2]中核反应堆辐照特种元件制备工艺重点实验室,内蒙古包头014035

出　　处：《核化学与放射化学》2024年第5期468-472,I0002,共6页Journal of Nuclear and Radiochemistry

摘　　要：放射性核素^(14)C应用十分广泛,国内逐步实现^(14)C的自主化生产。氮化铝粉末是制备^(14)C的主要原料。氮化铝中单质铝会直接影响^(14)C靶件在核反应堆内运行安全和质量。根据氮化铝不溶于酸的特点,采用硝酸、盐酸、硫酸分别考察了氮化铝纳米粉中单质铝的溶解效果。发现上述酸能够溶解少量的氮化铝粉末,而且还有少量粉末颗粒能够在溶液中悬浮,对单质铝的检测产生严重干扰。采用置换法对单质铝进行选择性溶解,并用滤膜器分离悬浮的氮化铝粉末,解决了少量氮化铝溶于酸溶液和氮化铝纳米粉颗粒悬浮对单质铝检测的干扰。采用电感耦合等离子体质谱仪(ICP-MS)建立了氮化铝纳米粉中单质铝的检测方法,线性范围在10~100μg/g,相对标准偏差为3.8%(n=6)。使用高纯氧化铝粉末验证建立的检测方法,置换效率能达到96%~98%。^(14)C,a radionuclide,which is widely used in all works of life,such as medical research and determination of PM2.5,has been realized autonomous production in China.It relied on imports,which was expensive and unstable supply in the past time.At present,Qinshan Nuclear Power has started ^(14)C production to completely solve the problem of the serious shortage of ^(14)C independent supply in China.Aluminum nitride powder is the main raw material for the preparation of ^(14)C,whose elemental aluminum directly affects the safety and quality of ^(14)C isotopic targets in nuclear reactors.Aluminum nitride is very stable in an inert high temperature environment.But a lot of elemental aluminum will react with water producing hydrogen in a high temperature environment which can result in the expansion of component rods or it will react with cladding tubes producing hydrogen embrittling effect,and these can affect the quality of ^(14)C isotopic target.According to the characteristic of aluminum nitride insoluble in acid,this study researched different dissolution effect of elemental aluminum in aluminum nitride nano-powder by nitric acid,hydrochloric acid and sulfuric acid.It was found that the above mentioned acid can only dissolve a small amount of aluminum nitride powder,and there was a small amount of aluminum nitride powder suspending in solution,which would seriously interfere the determination of elemental aluminum.At present,microwave digestion,laser ablation,X-ray fluorescence and other methods are used to dissolve or determinate aluminum nitride,but they are not suitable for the determination of elemental aluminum.The determination of elemental aluminum is generally used in pharmaceutical,soil,tea and other samples,but most of the aluminum in the above samples exists as an impurity element,or aluminum is combined with organic matter,which is easy to separate from elemental aluminum.However,it is difficult to achieve complete separation of elemental aluminum(unbound elemental aluminum)and the aluminum nitride mat

关 键 词：^(14)C靶件 氮化铝 ICP-MS 单质铝 

分 类 号：O657.63[理学—分析化学]