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首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection
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Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

机译:基质辅助光化学蒸气发生原子荧光光谱法直接测定白醋中的汞

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This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg~0, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL~(-1) for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).
机译:本文提出了使用乙酸产生光化学蒸气作为样品引入方法,通过原子荧光光谱法直接测定白醋中超痕量汞的方法。在紫外线照射下,样品基质(乙酸)可以将汞离子还原为原子汞Hg〜0,然后将其通过氩气吹扫到原子荧光光谱仪中进行后续分析测量。讨论并优化了乙酸浓度,辐照时间,载气流速和基质效应等因素的影响,对汞的检测限为0.08 ng mL〜(-1)。使用优化过程中建立的实验条件(3%v / v乙酸,30 s辐照时间和20 W水银灯),以相对标准偏差表示的精度水平为4.6%(一天)和7.8%(内部天)中的汞含量(n = 9)。用于评估准确性的附加/回收测试范围为汞的92-98%。该方法还通过对醋样品进行分析而得到验证,该醋样品中没有掺入水含量标准参考物质(GBW(E)080392和GBW(E)080393)的可检测量的汞。还将结果与通过酸消解程序和ICP-MS测定汞得到的结果进行比较。两种方法基于t检验的结果(在95%置信水平下)之间没有显着差异。

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