Abstract Cement and clinker are complex samples and constitute a challenge for elemental analysis. Manganese, usually present in these matrices, can accumulate in bones, liver, the pancreas, kidneys, and brain and its monitoring is very important. This work presents an alternative method of sample treatment based on ultrasonic-assisted extraction for the determination of trace amounts of manganese in cement and clinker samples by square wave cathodic stripping voltammetry (SWCSV) on a gold working electrodes. The proposed extraction procedure occurs at room temperature inside closed vessels and uses 3.0 mol L−1 HCl solution, a less corrosive extractant compared to concentrated acids. Ultrasonic extraction was compared with conventional extraction by heating on hot plate and no significant differences between the two extraction methods were observed at the 95% confidence level. The possible use of H2O2 in the extraction process was evaluated but not used due to its interferences in the electrochemical determination of manganese. The SWCSV results obtained employing 0.20 mol L−1 H3BO3/0.10 mol L−1 KCl electrolyte at pH 6.5 produced two distinct linear regions of concentration for the analytical curve from 1.1 to 2.0 × 10−7 mol L−1 and from 2.0 to 3.2 × 10−7 mol L−1. The limits of detection and quantification were 3.1 × 10−8 mol L−1 and 9.8 × 10−8 mol L−1, respectively, and suitable for the proposed application. The results obtained by SWCSV were consistent with those obtained by flame atomic absorption spectrometry (FAAS) at the 95% confidence level.

中文翻译：

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用于通过方波阴极溶出伏安法测定锰的水泥和熟料样品的超声波辅助消解

摘要 水泥和熟料是复杂的样品，对元素分析构成挑战。锰通常存在于这些基质中，可在骨骼、肝脏、胰腺、肾脏和大脑中积聚，因此对其进行监测非常重要。这项工作提出了一种基于超声波辅助萃取的样品处理替代方法，用于在金工作电极上通过方波阴极溶出伏安法 (SWCSV) 测定水泥和熟料样品中的痕量锰。建议的萃取程序在室温下在密闭容器内进行，并使用 3.0 mol L-1 HCl 溶液，与浓酸相比，这是一种腐蚀性较小的萃取剂。将超声波提取与通过在热板上加热的常规提取进行了比较，在 95% 的置信水平下没有观察到两种提取方法之间的显着差异。评估了 H2O2 在萃取过程中的可能用途，但由于其对锰电化学测定的干扰而未使用。使用 0.20 mol L-1 H3BO3/0.10 mol L-1 KCl 电解质在 pH 6.5 下获得的 SWCSV 结果为分析曲线产生了两个不同的线性浓度区域，从 1.1 到 2.0 × 10-7 mol L-1 和从 2.0 到 3.2 × 10−7 mol L−1。检测限和定量限分别为 3.1 × 10-8 mol L-1 和 9.8 × 10-8 mol L-1，适用于拟议的应用。