Centro de Ciências e Humanidades Universidade Presbiteriana Mackenzie, São Paulo, Brazil.
Talanta. 2010 Jul 15;82(2):790-5. doi: 10.1016/j.talanta.2010.05.055. Epub 2010 Jun 1.
A sensitive and robust analytical method for spectrophotometric determination of ethyl xanthate, CH(3)CH(2)OCS(2)(-) at trace concentrations in pulp solutions from froth flotation process is proposed. The analytical method is based on the decomposition of ethyl xanthate, EtX(-), with 2.0 mol L(-1) HCl generating ethanol and carbon disulfide, CS(2). A gas diffusion cell assures that only the volatile compounds diffuse through a PTFE membrane towards an acceptor stream of deionized water, thus avoiding the interferences of non-volatile compounds and suspended particles. The CS(2) is selectively detected by UV absorbance at 206 nm (epsilon=65,000 L mol(-1) cm(-1)). The measured absorbance is directly proportional to EtX(-) concentration present in the sample solutions. The Beer's law is obeyed in a 1x10(-6) to 2x10(-4) mol L(-1) concentration range of ethyl xanthate in the pulp with an excellent correlation coefficient (r=0.999) and a detection limit of 3.1x10(-7) mol L(-1), corresponding to 38 microg L(-1). At flow rates of 200 microL min(-1) of the donor stream and 100 microL min(-1) of the acceptor channel a sampling rate of 15 injections per hour could be achieved with RSD<2.3% (n=10, 300 microL injections of 1x10(-5) mol L(-1) EtX(-)). Two practical applications demonstrate the versatility of the FIA method: (i) evaluation the free EtX(-) concentration during a laboratory study of the EtX(-) adsorption capacity on pulverized sulfide ore (pyrite) and (ii) monitoring of EtX(-) at different stages (from starting load to washing effluents) of a flotation pilot plant processing a Cu-Zn sulfide ore.
提出了一种灵敏、稳健的分光光度法,用于测定浮选过程中纸浆溶液中痕量浓度的乙基黄原酸盐 CH(3)CH(2)OCS(2)(-)。该分析方法基于乙基黄原酸盐 EtX(-)与 2.0 mol L(-1) HCl 的分解,生成乙醇和二硫化碳 CS(2)。气体扩散池确保只有挥发性化合物通过 PTFE 膜扩散到去离子水的接受流中,从而避免了非挥发性化合物和悬浮颗粒的干扰。CS(2)通过在 206nm 处的紫外吸光度(ε=65,000 L mol(-1) cm(-1))被选择性地检测到。测量的吸光度与样品溶液中存在的 EtX(-)浓度成正比。在纸浆中乙基黄原酸盐的 1x10(-6) 至 2x10(-4) mol L(-1)浓度范围内,比尔定律得到遵守,相关系数(r=0.999)极好,检测限为 3.1x10(-7) mol L(-1),对应于 38μg L(-1)。在 200μL min(-1)的供体流和 100μL min(-1)的接受通道的流速下,以 15 次/小时的速度可以实现 15 次/小时的采样率,RSD<2.3%(n=10,1x10(-5) mol L(-1) EtX(-)的 300μL 注射)。两个实际应用证明了 FIA 方法的多功能性:(i)评估实验室研究中乙基黄原酸盐在粉碎硫化矿(黄铁矿)上的吸附能力时的游离 EtX(-)浓度,以及(ii)监测浮选中试工厂处理铜-锌硫化矿的不同阶段(从起始负荷到洗涤流出物)的 EtX(-)。