目的 探究电感耦合等离子体质谱(ICP-MS)法测定汞元素时加金与不加金对记忆效应和稳定性的影响,以及考察加金量。方法 采用ICP-MS测定溶液中汞元素的量。射频功率为1 550 W,载气(高纯氩气)流速为1.05 L·min-1,等离子气体流速为15.0 L·min-1,蠕动泵转速0.2 r·s-1,采样深度8 mm,积分时间为0.1 s。结果 汞溶液质量浓度在0.4 ng·mL-1时开始形成较明显的记忆效应;汞溶液在不加任何稳定剂的情况下常温放置超过2 h后逐渐不稳定,相对标准偏差(RSD)逐渐变大,而加入金元素后在48 h内较为稳定,RSD在5%以内;金汞比为2∶1时就能够降低记忆效应,同时很好的保证其稳定性;汞元素标准溶液单独制备与其他元素混合制备并无区别。结论 本实验对汞元素检测分析具有参考作用,为相关检测标准方法的修订和提高提供了技术支持。
Abstract
OBJECTIVE To investigate the effect of adding gold when determing the memory effect and stability of mercury by ICP-MS, and determine the appropriate amount of gold. METHODS ICP-MS method was used to determine the amount of mercury in the solution. The RF power was 1 550 W, flow rate of carrier gas was 1.05 L·min-1, plasma gas flow rate was 15.0 L·min-1, peristaltic pump speed was 0.2 r·s-1, and sampling depth was 8 mm. The integration time was 0.1 s. RESULTS Mercury solution began to demonstrate obvious memory effect at the concentration of 0.4 ng·mL-1. It gradually became unstable and the coefficient of variation gradually increased after being placed at room temperature for more than 2 h in the absence of stabilizer. After adding gold, the mercury soulution was stable within 48 h, and the coefficient of variation was within 5%. When the ratio of gold to mercury was 2∶1, the memory effect of mercury was decreaed, and its stability was well guaranteed. There was no difference when the mercury standard solution was prepared with or without other elements. CONCLUSION This study plays a reference role in the detection and analysis of mercury and provides technical support for the revision and improvement of relevant detection methods.
关键词
汞 /
稳定性 /
金 /
记忆效应 /
电感耦合等离子体质谱
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Key words
mercury /
stability /
gold /
memory effect /
ICP-MS
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中图分类号：
R917
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脚注
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基金
国家十二五“重大新药创制”课题“中药质量安全检测和风险控制技术平台”资助(2014ZX09304307-002)
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