Väisänen Ari, Suontamo Reijo, Silvonen Janne, Rintala Jukka
University of Jyväskylä, Department of Chemistry, P.O. Box 35, 40351, Jyväskylä, Finland.
Anal Bioanal Chem. 2002 May;373(1-2):93-7. doi: 10.1007/s00216-002-1290-2. Epub 2002 Apr 11.
An extraction method was developed for the determination of toxic elements in contaminated soil samples by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination of arsenic, cadmium, lead, and silver in ultrasound-assisted extracts of SRM 2710 and SRM 2711 by ICP-AES was carried out with high accuracy and precision (RSD<3.7%). The certified concentrations of the SRMs were obtained for arsenic, cadmium, lead, and silver by using an ultrasound-assisted extraction method with a digestion solution of (1+1)-diluted aqua regia. The determination of copper in SRMs by the ultrasound-assisted extraction method and analysis by ICP-AES failed to obtain the certified concentrations at the 95% level of confidence using (+/-2 s) as confidence limits of the mean. However, the same results were observed with the use of the microwave digestion method and reflux, which is the ISO 11466 standard method. The analysis of the SRMs showed that the ultrasound-assisted extraction method is highly comparable with the other methods used for such purposes. The major advantages of the ultrasound-assisted extraction method compared to the microwave and reflux methods are the high treatment rate (50 samples simultaneously in nine minutes) and low reagent usage, the main benefit of which are the low chloride and nitrate concentrations in the extracts.
开发了一种电感耦合等离子体原子发射光谱法（ICP-AES）测定污染土壤样品中有毒元素的萃取方法。采用ICP-AES对标准参考物质（SRM）2710和SRM 2711的超声辅助提取物中的砷、镉、铅和银进行测定，结果具有很高的准确度和精密度（相对标准偏差<3.7%）。通过使用（1+1）稀释王水的消解溶液的超声辅助萃取方法，获得了SRM中砷、镉、铅和银的认证浓度。采用超声辅助萃取方法并通过ICP-AES分析SRM中的铜，以（±2s）作为平均值的置信限，在95%的置信水平下未能获得认证浓度。然而，使用微波消解方法和回流法（即ISO 11466标准方法）时也观察到了相同的结果。对SRM的分析表明，超声辅助萃取方法与用于此类目的的其他方法具有高度可比性。与微波和回流方法相比，超声辅助萃取方法的主要优点是处理速度快（9分钟内可同时处理50个样品）且试剂用量少，其主要好处是提取物中的氯化物和硝酸盐浓度低。
