Department of Agricultural Chemistry, University Autónoma of Madrid, Madrid 28049, Spain.
Talanta. 2012 Jan 15;88:375-84. doi: 10.1016/j.talanta.2011.11.003. Epub 2011 Nov 6.
Six digestion procedures were tested to improve extraction methods for determination of trace elements in various organic amendments with high inorganic fractions. These procedures were tested in terms of pH, CaCO(3), organic matter, elemental analysis, BCR sequential extraction and X-ray diffraction analysis. Aqua regia extraction (ISO 11466), total digestion HF-HNO(3)-HClO(4) and four microwave-assisted digestions (i.e., HNO(3), HCl-HNO(3), HNO(3)-HF and HCl-HNO(3)-HF) were used. The effect of acid mixtures on microwave-assisted digestion of mineral fractions was assessed by Si and Al analysis and X-ray diffraction in the solid residues obtained. Microwave HF acid mixtures obtained highest trace element recoveries for all tested metals except Al. CaF(2) and CaAlF(5) precipitates were also detected using X-ray diffraction in the residues after microwave digestions with HF acid mixtures of amendments with high calcium content. A decision flowchart was suggested to determine the best acid mixture according to the amendment and the metals to be analyzed.
六种消化程序被测试以改进提取方法,用于测定高无机部分的各种有机肥料中的痕量元素。这些程序是根据 pH 值、CaCO(3)、有机质、元素分析、BCR 顺序提取和 X 射线衍射分析进行测试的。王水提取(ISO 11466)、总消化 HF-HNO(3)-HClO(4)和四种微波辅助消化(即 HNO(3)、HCl-HNO(3)、HNO(3)-HF 和 HCl-HNO(3)-HF)被使用。通过对获得的固体残渣中的 Si 和 Al 分析和 X 射线衍射评估了酸混合物对矿物分数微波辅助消化的影响。除了 Al 之外,对于所有测试金属,微波 HF 酸混合物都获得了最高的痕量元素回收率。在用 HF 酸混合物进行微波消化后,还通过 X 射线衍射在高钙含量的肥料残渣中检测到了 CaF(2)和 CaAlF(5)沉淀物。根据要分析的肥料和金属,建议了一个决策流程图来确定最佳的酸混合物。