Triple-Quadrupole Inductively Coupled Plasma-Mass Spectrometry with a High-Efficiency Sample Introduction System for Ultratrace Determination of 135Cs and 137Cs in Environmental Samples at Femtogram Levels,Analytical Chemistry

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Triple-Quadrupole Inductively Coupled Plasma-Mass Spectrometry with a High-Efficiency Sample Introduction System for Ultratrace Determination of 135Cs and 137Cs in Environmental Samples at Femtogram Levels
Analytical Chemistry ( IF 6.7 ) Pub Date : 2016-08-19 00:00:00 , DOI: 10.1021/acs.analchem.6b02150
Jian Zheng ₁ , Liguo Cao _{1,

2} , Keiko Tagami ₁ , Shigeo Uchida ₁

Affiliation

High yield fission products, ¹³⁵Cs and ¹³⁷Cs, have entered the environment as a result of anthropogenic nuclear activities. Analytical methods for ultratrace measurement of ¹³⁵Cs and ¹³⁷Cs are required for environmental geochemical and nuclear forensics studies. Here we report a highly sensitive method combining a desolvation sample introduction system (APEX-Q) with triple-quadrupole inductively coupled plasma mass spectrometry (AEPX-ICPMS/MS) for the determination of ¹³⁵Cs and ¹³⁵Cs/¹³⁷Cs isotope ratio at femtogram levels. Using this system, we introduced only selected ions into the collision/reaction cell to react with N₂O, significantly reducing the isobaric interferences (¹³⁵Ba⁺ and ¹³⁷Ba⁺) and polyatomic interferences (^95,97Mo⁴⁰Ar⁺, ¹¹⁹Sn¹⁶O⁺, and ¹²¹Sb¹⁶O⁺). Compared to the instrument setup of ICPMS/MS, the APEX-ICPMS/MS enables a 10-fold sensitivity increase. In addition, an effective chemical separation scheme consisting of ammonium molybdophosphate (AMP) Cs-selective adsorption and two-stage ion-exchange chromatographic separation was developed to remove major matrix and interfering elements from environmental samples (10–40 g). This separation method showed high decontamination factors (10⁴–10⁷) for major matrix elements (Al, Ca, K, Mg, Na, and Si) and interfering elements (Ba, Mo, Sb, and Sn). The high sensitivity of APEX-ICPMS/MS and the effective removal sample matrix allowed reliable analysis of ¹³⁵Cs and ¹³⁷Cs with extremely low detection limits (0.002 pg mL^–1, corresponding to 0.006 Bq mL^–1¹³⁷Cs). The accuracy and applicability of the APEX-ICPMS/MS method was validated by analysis of seven standard reference materials (soils, sediment, and plants). For the first time, ultratrace determination of ¹³⁵Cs and ¹³⁵Cs/¹³⁷Cs isotope ratio at global fallout source environmental samples was achieved with the ICPMS technique.

中文翻译：

高效液相引入系统的三重四极杆电感耦合等离子体质谱法在痕量示踪水平上超痕量测定环境样品中的¹³⁵ Cs和¹³⁷ Cs

由于人为核活动，高产裂变产物¹³⁵ Cs和¹³⁷ Cs进入了环境。环境地球化学和核法证学研究需要用于¹³⁵ Cs和¹³⁷ Cs的超痕量测量的分析方法。在这里，我们报告了结合去溶剂化样品引入系统（APEX-Q）和三重四极杆电感耦合等离子体质谱仪（AEPX-ICPMS / MS）的高灵敏度方法，用于在飞度图上测定¹³⁵ Cs和¹³⁵ Cs / ¹³⁷ Cs同位素比水平。使用该系统，我们仅将选定的离子引入到碰撞/反应池中以与N ₂反应O，可显着降低等压干扰（¹³⁵ Ba ⁺和¹³⁷ Ba ⁺）和多原子干扰（^95,97 Mo ⁴⁰ Ar ⁺，¹¹⁹ Sn ¹⁶ O ⁺和¹²¹ Sb ¹⁶ O ⁺）。与ICPMS / MS的仪器设置相比，APEX-ICPMS / MS可使灵敏度提高10倍。此外，还开发了一种有效的化学分离方案，其中包括钼酸铵（AMP）的Cs选择性吸附和两阶段离子交换色谱分离，以从环境样品（10-40 g）中去除主要基质和干扰元素。这种分离方法对主要基质元素（Al，Ca，K，Mg，Na和Si）和干扰元素（Ba，Mo，Sb和Sn）显示出较高的去污因子（10 ⁴ –10 ⁷）。APEX-ICPMS / MS的高灵敏度和有效的去除样品基质，可对¹³⁵ Cs和¹³⁷ Cs进行可靠的分析，并且检出限极低（0.002 pg mL ^–1，对应于0.006 Bq mL ^–1¹³⁷ Cs）。通过分析七种标准参考物质（土壤，沉积物和植物），验证了APEX-ICPMS / MS方法的准确性和适用性。ICPMS技术首次实现了在全球辐射源环境样品中超痕量测定¹³⁵ Cs和¹³⁵ Cs / ¹³⁷ Cs同位素比的方法。

更新日期：2016-08-19

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