激光共振电离质谱法测量锡的同位素比

采用实验室研制的激光共振电离质谱仪,建立了锡(Sn)同位素的激光共振电离质谱分析方法。测量了锡原子的自电离态光谱,确认了锡的一条三色三光子共振电离路径,其各步激发/电离的激光波长分别为λ1=286.4 nm、λ2=811.6 nm、λ3=823.7 nm;通过将样品与氧化石墨烯溶液混合制样,有效提高了锡样品的电热原子化效率,1μg锡的总探测效率达到3×10^-5以上,是直接滴样方式的4.5倍左右。采用本方法对锡、锑、碲(1∶1∶1,m/m)混合模拟样品进行测试,实现了锡的选择性电离,有效避免了测量过程中锑、碲对锡的同量异位素干扰,样品中主要同位素比^116Sn/^120Sn,^117Sn/^1...

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Published in分析化学 Vol. 45; no. 3; pp. 342 - 347
Main Author 沈小攀 李志明 王文亮 翟利华 邓虎 徐江 韦冠一 汪伟
Format Journal Article
LanguageChinese
Published 西北核技术研究所,西安,710024 2017
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ISSN0253-3820
DOI10.11895/j.issn.0253-3820.160840

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Summary:采用实验室研制的激光共振电离质谱仪,建立了锡(Sn)同位素的激光共振电离质谱分析方法。测量了锡原子的自电离态光谱,确认了锡的一条三色三光子共振电离路径,其各步激发/电离的激光波长分别为λ1=286.4 nm、λ2=811.6 nm、λ3=823.7 nm;通过将样品与氧化石墨烯溶液混合制样,有效提高了锡样品的电热原子化效率,1μg锡的总探测效率达到3×10^-5以上,是直接滴样方式的4.5倍左右。采用本方法对锡、锑、碲(1∶1∶1,m/m)混合模拟样品进行测试,实现了锡的选择性电离,有效避免了测量过程中锑、碲对锡的同量异位素干扰,样品中主要同位素比^116Sn/^120Sn,^117Sn/^120Sn,^118Sn/^120Sn和^119Sn/^120Sn测量的相对标准偏差均〈1%。结果表明,本方法能够有效解决TIMS、ICP-MS等商业质谱仪在锡同位素质谱分析过程中的同量异位素干扰难题,有望应用于反应堆乏燃料中裂变产物^121mSn、^126Sn的测量。
Bibliography:Laser resonance ionization mass spectrometry; Tin; Isobaric interference ; Isotope ratio; Element selectivity
22-1125/O6
A preliminary method based on the laser resonance ionization mass spectrometer (LRIMS) developed in the laboratory was established to determine tin isotope ratios. By measuring the auto-ionization spectrum of tin atoms, a three-color-three-photon resonance ionization scheme was confirmed, and the laser wavelengths of each excitation/ionization step were A1 =286.4 nm, A2 =811.6 nm and A3 =823.7 nm. More effective electrothermal atomization of tin was implemented by mixing the samples and grapheme oxide solution, and the total detection efficiency of 1 μg of tin sample was above 3×10-5, which was about 4.5 times as high as the method of directly dropping samples. A tin-antimony-tellurium mixture at a ratio of 1 : 1 : 1 (m/m) was prepared as a simulant sample, and the major tin isotope ratios in the sample were determined. Results showed that the isobaric interference from antimony and tellurium
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.160840