Monitoring Sb in lead refining using advanced techniques in Industry 4.0

An increase of 22 per cent in lead usage is expected in the European Union by 2050. During lead refining, the Harris process is a critical step in which a salt melt is used to remove arsenic, tin and antimony. During this process, the caustic salt melt absorbs these impurities, requiring regular evacuation before saturation. Current metallurgical practices for: 1) determining the end point of the lead alloy involve time-consuming sampling and offline analysis, and 2) determining the end point of the caustic salt melt are based on subjective visual observations by the operator. In the context of Industry 4.0 concept, automating these processes becomes desirable, as smart sensors systematically collect real-time data in an unbiased manner. This research focuses on monitoring the Harris refining process using objective methodologies. Two different methodologies are investigated. The first methodology focuses on electrical conductivity changes of the caustic salt melt as function of Sb content. For this study, synthetic and industrial samples are used. A lab-scale electrical conductivity set-up was built to accommodate the aggressiveness of the salt melt. Initial findings suggest a promising relationship between electrical conductivity and Sb content in the caustic salt melt. Although the results are preliminary, the study provides valuable insights by enabling real-time measurements. The second methodology focuses on measuring the electromotive force (EMF) in lead doped with Sb at pilot-scale. Multiple probes are reevaluated for their effectiveness in Sb measurement. Ultimately, a partially stabilised MgO probe with Ni as a reference, without cardboard and copper protection caps, yields promising results. A correlation between EMF and Sb content is observed. However, repeatability issues arise due to possible wire interference at low temperatures. The results underscore the potential of advanced measurement techniques in optimising lead alloy production within the context of Industry 4.0.