Study on the Determination of Trace Lead by Spectrophotometry after Flotation Separation with Ternary Association Complex System

Wen Xinrong, Tu Changqing
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Abstract

The paper presents a novel method for the flotation separation of Pb2+ with ternary association complex system prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of KI and hexa decyl trim ethyl ammonium bromide (CTMAB), various salts and acidity etc. on the flotation yield of Pb 2+ have been investigated to select the experimental conditions. The possible flotation mechanism of Pb2+ was discussed. The results showed that by controlling pH1.0, in the presence of 1.0g NaNO3, when the dosage of 0.1 mol¡¤L-1 KI solution was 1.00 mL and 0.01 mol¡¤L-1CTMAB solution was 0.50 mL respectively, the water-insoluble ternary association complex of (CTMAB)2(PbI4) which produced by Pb2+ and I-, CTMAB cation (CTMAB+) floated above water phase and liquid-solid phases were formed with clear interface, while Fe2+, Co2+, Ni2+, Zn2+, Mn2+ and Al3+ could not be floated, so Pb2+ was floated quantitatively at pH1.0. Thereby, the quantitative separation of Pb2+ from the above metal ions could be achieved. A new method of determination of trace lead by flotation separation was established. The proposed method has been successfully applied to the determination of Pb2+ in the sample of synthetic water and the flotation yield was96.3%~106.6%.
三元缔合络合物浮选分离后分光光度法测定痕量铅的研究
提出了在分光光度法测定前用三元缔合络合物浮选分离Pb2+的新方法。考察了KI和六癸基甲基溴化铵(CTMAB)用量、不同盐类和酸度等参数对pb2 +浮选产率的影响,选择了实验条件。探讨了Pb2+的可能浮选机理。结果表明:通过控制pH1.0,在1.0g NaNO3存在下,当0.1 mol·L-1 KI溶液用量为1.00 mL和0.01 mol·L-1CTMAB溶液用量为0.50 mL时,Pb2+和I-生成的(CTMAB)2(PbI4)水不溶性三元缔合物,CTMAB阳离子(CTMAB+)浮于水相和液固相之上,形成界面清晰,而Fe2+、Co2+、Ni2+、Zn2+、Mn2+和Al3+不能浮于水相和液固相之上;因此,Pb2+在pH1.0下定量漂浮。从而实现了Pb2+与上述金属离子的定量分离。建立了浮选分离法测定痕量铅的新方法。该方法已成功应用于合成水中Pb2+的测定,浮选率为96.3%~106.6%。
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