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Accuracy evaluation of ultrasound probe sonication and microwave-assisted extraction systems for rapid single extraction of metals in soils

机译:超声探针超声和微波辅助提取系统快速评估土壤中金属的准确性

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Ultrasonic probe sonication (UPS) and microwave-assisted extraction (MAE) have been evaluated as alternatives to the conventional Standards, Measurements and Testing program (SM&T) procedures for single extraction of metals in soils, in order to reduce the extraction time and the consumption of samples and extracting agents. Optimization studies were carried out on the certified reference materials (CRMs) BCR 483 (sewage sludge amended soil) and BCR 700 (organic rich soil) for accuracy evaluation of the proposed methods. Extractable concentrations of Cd, Cr, Cu, Ni, Pb and Zn using 0.01 mol La?’1 calcium chloride (CaCl2) (in BCR 483), 0.43 mol La?’1 acetic acid (CH3COOH) and 0.05 mol La?’1 ethylenediaminetetraacetic acid (EDTA) at pH 7.0 (in both CRMs) were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The extraction time for the CaCl2 extraction method was reduced from 3 h (conventional procedure) to 2 min by UPS or 5 min at 50 ?°C by MAE. Similarly, the time required for acetic acid extraction was also reduced from 16 h to 15 min by UPS or 15 min at 120 ?°C by MAE. Finally, the extraction time with EDTA was reduced from 1 h (conventional procedure) to 2 min by UPS or 5 min at 50 ?°C by MAE. For these extraction conditions proposed, quantitative extraction recoveries were obtained for most elements studied. In addition, the amount of sample and extractants was drastically reduced, maintaining the sample weight/extractant volume ratio.
机译:超声探头超声(UPS)和微波辅助提取(MAE)已被评估为对土壤中金属的单次提取的常规标准,测量和测试程序(SM&T)程序的替代品,以减少提取时间和消耗样品和萃取剂。对经过认证的参考材料(CRM)BCR 483(污水污泥改良土壤)和BCR 700(富含有机土壤)进行了优化研究,以评估所提出方法的准确性。使用0.01摩尔La?'1氯化钙(CaCl2)(在BCR 483中),0.43摩尔La?'1乙酸(CH3COOH)和0.05摩尔La?'1提取的Cd,Cr,Cu,Ni,Pb和Zn浓度通过电感耦合等离子体原子发射光谱法(ICP-AES)测定pH值为7.0的乙二胺四乙酸(EDTA)。 CaCl2萃取方法的萃取时间由UPS的3 h(常规程序)减少到2分钟,或由MAE在50°C的条件下减少5分钟。同样,通过UPS提取乙酸所需的时间也从16小时减少到15分钟,而通过MAE在120°C下也减少了15分钟。最终,用UPS将EDTA的萃取时间从1小时(常规程序)减少到2分钟,而在50°C的条件下通过MAE将萃取时间减少到5分钟。对于提出的这些提取条件,大多数研究元素均获得了定量提取回收率。另外,大大减少了样品和萃取剂的量,从而保持了样品重量/萃取剂体积比。

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