Department of Chemistry, University College Cork, Cork, Ireland.
Talanta. 2003 Jul 4;60(4):715-23. doi: 10.1016/S0039-9140(03)00131-0.
A microwave digestion technique was developed to determine the content of nine heavy metals in sediments and soils. The digests were subsequently analysed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The metals determined were Ca, Mg, Fe, Mn, Zn, Cr, Cd, Cu, Pb and V. The digestion was achieved by using an acid mixture of HNO(3), HF and distilled H(2)O. The experimental study was conducted using four standard reference materials (SRMs): sewage sludge (LGC6136), marine sediment (PACS-1), urban particulate matter (NIST 1648) and coal carbonisation site soil (LGC6138). Two different programs were examined to determine which was optimal for the digestion of real environmental samples. The accuracy and precision of the two digestion programs for the analysis of the SRMs were compared. From the results obtained, the microwave program providing a maximum of power of 650 W and a cycle time of 51 min resulted in the best analytical performance. The experimental results obtained were in good agreement with the certified values and demonstrated that the proposed method is precise and accurate.
建立了一种微波消解技术,用于测定沉积物和土壤中九种重金属的含量。采用电感耦合等离子体原子发射光谱法(ICP-AES)对消解液进行分析。测定的金属为 Ca、Mg、Fe、Mn、Zn、Cr、Cd、Cu、Pb 和 V。消解采用 HNO(3)、HF 和去离子 H(2)O 的酸混合物。实验研究使用了四种标准参考物质(SRM):污水污泥(LGC6136)、海洋沉积物(PACS-1)、城市颗粒物(NIST 1648)和煤焦化场地土壤(LGC6138)。检查了两种不同的方案,以确定哪种方案最适合实际环境样品的消解。比较了两种消解方案分析 SRM 的准确性和精密度。从获得的结果来看,最大功率为 650 W、循环时间为 51 分钟的微波方案可获得最佳分析性能。所得实验结果与认证值吻合良好,表明该方法精确、准确。