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首页> 外文OA文献 >Determination of cadmium at ultratrace levels in environmental water samples by means of total reflection X-ray spectrometry after dispersive liquid-liquid microextraction
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Determination of cadmium at ultratrace levels in environmental water samples by means of total reflection X-ray spectrometry after dispersive liquid-liquid microextraction

机译：分散液-液微萃取-全反射X射线光谱法测定环境水样中痕量镉

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Until now, the determination of Cd at trace levels in aqueous samples by TXRF has been restricted. When Mo-target X-ray tubes are used, low sensitivity and interferences with Cd L-lines used for quantification prevent trace analysis. Alternatively, when W-target X-ray tubes are used Cd excitation is limited. For this reason, a sample pretreatment is usually necessary to extract, isolate and concentrate Cd prior to TXRF analysis. In the present contribution, the feasibility of a dispersive liquid-liquid microextraction approach (DLLME) combined with TXRF for ultratrace Cd determination in different types of environmental waters is shown. Parameters affecting the extraction procedure and TXRF measurement conditions have been carefully evaluated to ensure the highest sensitivity for Cd determination. Using the best analytical conditions, it was found that the minimum cadmium content that could be detected in an aqueous solution was 0.04 μg L-1. This value is more than two orders of magnitude lower compared with the direct TXRF analysis of Cd in aqueous samples. The precision of the methodology was evaluated in terms of relative standard deviation (RSD) of six replicate analyses of a standard solution containing 3 μg L-1. The precision of the method was determined to be approximately 5% RSD. In order to test the suitability of the method when dealing with complex matrices as well as the influence of interfering ions, the determination of Cd in spiked water samples (sea water, estuarine water and river water) at the levels of 1 μg L-1 and 5 μg L-1 was undertaken and Cd added to the samples was quantitatively determined. Our results give insight into the possibilities of the combination of DLLME and TXRF for ultratrace Cd determination in different types of environmental waters. © 2013 The Royal Society of Chemistry.
机译：迄今为止，通过TXRF测定水样中痕量水平的Cd一直受到限制。使用Mo靶X射线管时，低灵敏度和对定量使用的Cd L线的干扰会阻止痕量分析。可替代地，当使用W目标X射线管时，Cd激发受到限制。因此，在TXRF分析之前，通常需要样品预处理以提取，分离和浓缩Cd。在本论文中，显示了将分散液-液微萃取方法（DLLME）与TXRF结合用于不同类型环境水中超痕量Cd测定的可行性。已经仔细评估了影响萃取程序和TXRF测量条件的参数，以确保对Cd测定具有最高的灵敏度。使用最佳分析条件，发现可以在水溶液中检测到的最小镉含量为0.04μgL-1。与水性样品中镉的直接TXRF分析相比，该值低两个数量级以上。该方法的准确性是通过对含有3μgL-1的标准溶液进行六次重复分析的相对标准偏差（RSD）进行评估的。该方法的精度确定为约5％RSD。为了测试该方法在处理复杂基质时的适用性以及干扰离子的影响，在加标水样品（海水，河口水和河水）中以1μgL-1的水平测定Cd取5μgL-1进行定量测定。我们的研究结果揭示了将DLLME和TXRF结合用于不同类型环境水中超痕量Cd测定的可能性。 ©2013皇家化学学会。

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