小型化电晕放电-原子发射光谱仪检测痕量汞
采用电晕放电激发源和手持式电荷耦合检测器组装了小型化原子发射光谱仪,将其用于检测痕量汞。以光化学蒸气发生技术作为进样手段,在甲酸辅助下用紫外光照射样品溶液产生汞蒸气,并由氩气带入电晕放电光源中,激发后产生汞原子发射光谱信号,用电荷耦合检测器在253.7 nm处检测。经优化得到的最佳实验条件为甲酸浓度4%,电晕放电电压90 V,载气流速200 m L/min;检测信号稳定,相对标准偏差为2.5%;标准曲线线性范围为0.5~1000μg/L,线性相关系数大于0.99,汞的检出限可以低至0.03μg/L。同时,对两种含汞的标准样品进行了分析,t检验表明,检测结果与样品标准值在95%的置信水平上无显著...
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Published in | 分析化学 Vol. 43; no. 9; pp. 1291 - 1295 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
Published |
四川师范大学化学与材料科学学院,成都610068%四川大学分析测试中心,成都,610064
2015
四川大学建筑与环境学院,成都610065 |
Subjects | |
Online Access | Get full text |
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Summary: | 采用电晕放电激发源和手持式电荷耦合检测器组装了小型化原子发射光谱仪,将其用于检测痕量汞。以光化学蒸气发生技术作为进样手段,在甲酸辅助下用紫外光照射样品溶液产生汞蒸气,并由氩气带入电晕放电光源中,激发后产生汞原子发射光谱信号,用电荷耦合检测器在253.7 nm处检测。经优化得到的最佳实验条件为甲酸浓度4%,电晕放电电压90 V,载气流速200 m L/min;检测信号稳定,相对标准偏差为2.5%;标准曲线线性范围为0.5~1000μg/L,线性相关系数大于0.99,汞的检出限可以低至0.03μg/L。同时,对两种含汞的标准样品进行了分析,t检验表明,检测结果与样品标准值在95%的置信水平上无显著性差异;另外,对成都市府南河水和四川大学校园荷花池水的汞含量进行了测定,加标回收率在93.8%~103%范围之内。该小型化原子发射光谱测汞仪具有组装简单、低能耗、高灵敏度、便携式适用于现场分析等优点。 |
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Bibliography: | LUO Hong , HOU Xian-Deng, LONG Zhou 1( College of Architecture and Environment, Sichuan University, Chengdu 610065, China) 2( College of Chemistry and Material Science, Sichuan Normal University, Chengdu 610068, China) 3(Analytical & Testing Center, Sichuan University, Chengdu 610064, China) 22-1125/O6 Corona discharge; Mercury; Photochemical vapor generation; Atomic emission spectrometry A miniaturized atomic emission spectrometer composed of a corona discharge source and ahandheld charge-coupled device photochemical vapor generation detector was constructed for the sensitive determination of trace for sample introduction. By using formic acid, mercury vapor mercury, with was generated under the irradiation of UV light, and then the vapor was introduced into the corona discharge area with the cartier gas flow of argon. The optical signals were captured and analyzed by the charge-coupled device detectorat 253.7 nm. Under the optimized conditions including 4% formic acid, discharge voltage of 90 V, and carrier ga |
ISSN: | 0253-3820 |
DOI: | 10.11895/j.issn.0253-3820.141027 |