摘要
本工作选择m/z88(23 Na210BO2+)和m/z89(23 Na211BO2+)的Na2BO2+作为检测离子,研究了同位素干扰、涂样技术、ZrB2样品处理等对硼同位素测定的影响,建立了快速准确测定ZrB2中硼同位素丰度的正热电离质谱法。实验复现了硼同位素标准物质的标准值,对酸溶法分解试样后涂样和直接熔融法涂样测量结果的精密度进行了比较。结果表明,采用直接熔融法涂样可以快速准确地测定ZrB2中硼同位素丰度,δ10B同位素丰度测定结果精密度优于0.020%。
Positive thermal ionization mass spectrometry(PTIMS)method was used to determine boron isotope in ZrB2 for Na2BO2+with m/z 88(23 Na210 BO2+)and m/z 89(23 Na211BO2+)as analytical ion.Imported high purity tantalum belt was used as sample filament.The isotope interference,coating technology,pretreatment of the ZrB2 sample were researched.There is no interference of strontium and yttrium in the background by mass peak scanning and analysis,while the effect of oxygen isotope was deducted by formula.The graphite was attached to the sample filament with diluent graphite slurry instead of graphite turbid liquid as emission reagent.The method of which used Cs2BO2+as analytical ion was reproduced by samples coating with graphite slurry,and using diluent graphite slurry instead of graphite turbid liquid.Enhanced effect of graphite on Na2BO2+emission was proved by comparison with the direct coating method.Although the effect was inapparent about the enhanced effect of graphite on Cs2BO2+emission,the reduction of ion beam was inhibited effectively in analysis after addinggraphite.The phenomenon shows that graphite coating method is propitious to gain stabler ion beam and improve the precision of analytical results.The value of boron isotope standard substance was reproduced,and the analytical value was consistent with the standard value.When sample quantity was 8.0μg,acid dissolution sample application and direct fusion sample application were compared.The results show that the direct fusion sample application is not easy to introduce interference ions,and the precision is less than 0.020%.This method can shorten the time of sample pretreatment and improve the detection efficiency.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2015年第6期565-570,共6页
Journal of Chinese Mass Spectrometry Society