为满足新研发的200kV单极静电加速器质谱仪测量14 C的需要,开展了14^ C样品制备技术研究。在自主设计的14C制样装置上优化了H2-Fe法、Zn-Fe法、Zn-H-Fe法制备石墨样品的实验条件,制备的样品经离子源引出12C-的束流均可达15~40μA,稳定性好于0.2%。在加速器质谱仪的调试中发现压低制备样品12^CH+13^C和12^C的粒子个数比更有利于实现14 ^C-SE-AMS小型化及高灵敏测量。14^C-SE-AMS的测试样品中碳含量小于1mg时,采用Zn-Fe法有利于压低12^CH+13^C和12^C的粒子个数比;样品碳含量为1~5mg时,采用Zn-Fe法和Zn-H-Fe法效果相当。建立的制样方法对含碳量为100μg~5mg的样品,其产率均能达到95%以上,且空白样品测试结果表明此系统能有效避免样品制备中的交叉污染。
In order to satisfy 14^C measurement with the new developed 200 kV stage electrostatic accelerator mass spectrometer, the samp 14C were investigated. The graphitization experimental cond Zn-H-Fe methods w beam current of 12^C ter than 0.2%. Th ere e optimized on self-designed 14^C s r all prepared samples can reach C measurement shows that the e preparation process single es for for H2-Fe, Zn-Fe and ample preparation system. The 15 40μA and its stability is bet- lower particle number ratio of 12^CH+13^C and 12^C benefits the high sensitivity and miniaturization of device. The result also shows that the Zn-Fe method can depress the particle number ratio of 12^CH+13^C and 14^C for the samples with the carbon content less than 1 mg, while, for the carbon content among 1 mg to 5 mg, the Zn-Fe and Zn-H-Fe methods have the equivalent effect. For above preparation methods, the yield of carbon can reach more than 95% for the carbon content of 100μg-5 mg. Moreover, through blank sample measurement it is proved that the cross contamination during the sample preparation can be avoided.