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自动静态双接收高精度热电离质谱法测定硼同位素
引用本文:贺茂勇,马云麒,金章东,马海州,张艳灵,罗重光,肖军,肖应凯.自动静态双接收高精度热电离质谱法测定硼同位素[J].质谱学报,2013,34(2):75-81.
作者姓名:贺茂勇  马云麒  金章东  马海州  张艳灵  罗重光  肖军  肖应凯
作者单位:1. 中国科学院地球环境研究所黄土与第四纪国家重点实验室, 陕西 西安710075;2. 中国科学院青海盐湖研究所,中国科学院盐湖资源与化学重点实验室,青海 西宁810008
摘    要:在以Cs2BO2+离子进行硼同位素测定时,由于所测定的两种离子133Cs211B16O2+(m/z 309)和133Cs210B16O2+(m/z 308)具有极小的相对质量差(0.032%),一般的商业同位素热电离质谱计无法实现对这两种离子的同时全接收。为此,一些学者对某些商业仪器进行了改造或采用zoom技术,基本实现了对硼同位素高精度测定。本实验利用特制的Triton热电离质谱仪,以Cs2BO2+离子流的自动静态双接收进行硼同位素组成的测定。研究了不同离子流强度和不同带电流对250 ng标准样品NIST 951 H3BO3测定值及测试精度的影响,结果表明,当带电流在1 150~1 350 mA之间变化或者离子流稳定在0.1~10 V之间时,标准样品的硼同位素比值在4.052 63 ~ 4.053 38区间变化。导致二者一致的实验现象是由带电流强度造成的,当带电流越高时,产生的离子流相应也越高,因此可以采用相同的带电流控制不同样品的测试值和测试精度。在此基础上通过优化测试条件, 摸索出硼同位素自动测试程序,并用该程序对标准样品及实际样品进行测定,无论是测试结果还是测定精度均能达到手动测试效果,节省了人力,提高了工作效率。

关 键 词:高精度  热电离  静态双接收  自动测定  硼同位素  

Automatic and High-Precision Determination of Boron Isotopic Ratios Using Thermal Ionization Mass Spectrometry with Static Multi-Collection
HE Mao-yong,MA Yun-qi,JIN Zhang-dong,MA Hai-zhou,ZHANG Yan-ling,LUO Chong-guang,XIAO Jun,XIAO Ying-kai.Automatic and High-Precision Determination of Boron Isotopic Ratios Using Thermal Ionization Mass Spectrometry with Static Multi-Collection[J].Journal of Chinese Mass Spectrometry Society,2013,34(2):75-81.
Authors:HE Mao-yong  MA Yun-qi  JIN Zhang-dong  MA Hai-zhou  ZHANG Yan-ling  LUO Chong-guang  XIAO Jun  XIAO Ying-kai
Affiliation:1. State Key Laboratory of Loess and Quaternary Geology, Institute of Earth Environment, Chinese Academy of Sciences, Xi’an 710075, China;2. CAS Key Laboratory of Salt Lake Resources and Chemistry, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xi’ning 810008, China
Abstract:Due to the small relative mass difference between m/z 308 and m/z 309, simultaneous data collection was not possible using conventional multi-collection mass spectrometers. To conduct multi-collector measurements of m/z 308 (133Cs210B16O2+) and m/z 309 (133Cs211B16O2+), the Faraday cups were configured to measure m/z 308 and m/z 309 array with zoom optics. We utilize thermal ionization mass spectrometry (Trion) to perform automatic and high-precision determination of boron isotope using static multicollection of Cs2BO2+ ions. The research has been performed to investigate the impact of ion current and filament current on the accuracy and reproducibility of boron isotope measurements for NIST 951 Standard, giving values of 11B/10B were in the range of 4.052 63-4.053 38, when ion current varied 0.1-10 V and filament current varied 1 150-1 350 mA.The phenomenon of this study was filament current. With the higher of filament current, the ion current was corresponding to be higher. Based on this discovery, we have established the conditions for precise boron isotopic measurement using the multicollection technique by automatic mode. The proposed method was used for the determination of NIST 951 H3BO3 and natural samples. The results show that the automatic mode and manual mode has same precision and accuracy. And this technique enables us to do speedy analysis of boron isotopes and greatly improve the efficiency.
Keywords:high-precision  thermal ionization  static multicollection  automatic determination  boron isotope  
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