Synthesis and identification of meta-(4-bromobenzyloxy) benzaldehyde thiosemicarbazone (MBBOTSC) as novel ligand for cadmium extraction by ultrasound assisted-dispersive-ionic liquid-liquid micro extraction method

A. Hassanzadeh, B. Amirheidari, Ahmad Salarifar, A. Asadipour, Yaghoub Pourshojaei
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Abstract

In this research, meta-(4-bromobenzyloxy) benzaldehyde thiosemicarbazone (MBBOTSC) as a novel ligand was synthesized from the reaction between meta-(4-bromobenzyloxy) benzaldehyde and thiosemicarbazide under basic condition in water and ethanol as solvents. Ligand has the ability to chelate ions and therefore, it was used to form a complex and extract ions. Then, the cadmium ions in water and wastewater samples were separated based on MBBOTSC by ultrasound assisted-dispersive-ionic liquid-liquid microextraction method (USA-D-ILLME) before determination by AT-F-AAS. The MBBOTSC ligand was added to the mixture of the ionic liquid/acetone (IL/AC, [OMIM][PF6]) and then injected by syringe to 50 mL of water samples at pH 6-7. The sample was put into the ultrasonic accessory for 5 minutes, after complexation (Ligand-Cd; RS…Cd….RS), the water sample was centrifuged for 3 min for phase separation.  Due to complexation and back-extraction of Cd in liquid phase, the amount of Cd ions in the water samples was determined by AT-F-AAS . In optimized conditions, the Linear ranges and LOD for 50 mL of water samples were obtained 1-36 μg L-1 and 0.3 μg L-1, respectively (Mean RSD= 1.26%). The validation results were successfully achieved by spiking real samples and using ET-AAS.
超声辅助-分散-离子液-液微萃取法提取镉的新型配体-(4-溴苄氧基)苯甲醛硫代氨基脲(MBBOTSC)的合成与鉴定
本研究以间(4-溴苄氧基)苯甲醛和硫代氨基脲为原料,在水和乙醇为溶剂的碱性条件下合成了间(4-溴苄氧基)苯甲醛硫代氨基脲(MBBOTSC)作为一种新型配体。配体具有螯合离子的能力,因此,它被用来形成络合物和提取离子。然后,采用超声辅助分散离子液-液微萃取法(USA-D-ILLME)对MBBOTSC水溶液和废水样品中的镉离子进行分离,并用AT-F-AAS法进行测定。将MBBOTSC配体加入到离子液体/丙酮混合物(IL/AC, [OMIM][PF6])中,然后在pH 6-7的条件下,用注射器注射到50 mL的水样中。将样品置于超声附件中5分钟,络合(配体- cd;RS…Cd....RS),水样离心3min进行相分离。由于Cd在液相中的络合作用和反萃取作用,采用AT-F-AAS法测定了水样中Cd离子的含量。优化条件下,50 mL水样的检出限分别为0.3 μg L-1和1 ~ 36 μg L-1(平均RSD= 1.26%)。通过对实际样品进行峰化和ET-AAS验证,验证结果得到了满意的结果。
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