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Purification of supporting electrolyte Tetra-n-butylammonium

已有 4373 次阅读 2012-2-16 21:57 |个人分类:化学|系统分类:科研笔记| 电化学, 电解质, tbapf6

Purification of supporting electrolyte Tetra-n-butylammonium hexafluorophosphate (TBAPF6)
English

A17196 Tetra-n-butylammonium hexafluorophosphate (TBAPF6), 98%, CAS    3109-63-5, is common supporting electrolyte in electrochemistry test. Alfa corp sell it of 98% purity. According our lab’s experience, there was impurity in the raw commercial material, which meet rough electrochemistry rather than explicit test, e.g. OSWV of open-hole fullerene. We’d better to purify it by recrystalization. Two method:

1) recrystallization by ethanol and water.

2) recrystallization by absolute ethanol three times, however, recrystallization once is enough to common test. The recrystallization condition is : 25 g TBAPF6 was dissolved heatedly in 100mL EtOH, cooled down naturally , then cooled in fridg at -16 degree, filtered, dried in vacuo for 24~48h. Yield, 97%.

References: 

1Purification of Laboratory Chemicals (4th Edition)

2)Robert L. Bedard, Lawrence F. Dahl, "Electrochemical analysis of biocapped triangular cobalt cyclopentadienyl clusters, [Co3(.eta.5-C5H5-xMex)3(.mu.3-X)(.mu.3-Y)]n (x = 0, 1, 5), containing mixed .pi.-acceptor X and .pi.-donor Y capping ligands [X = CO, NO; Y = NSiMe3, NC(O)NH2, NH]: pronounced variations in redox behavior as a function of coordinating ligands", Journal of the American Chemical Society, 1986, 108, 5933.

中文:

A17196 Tetra-n-butylammonium hexafluorophosphate, 98%  

CAS 3109-63-5, 

四正丁基六氟磷酸铵, TBAPF6是常用的支持电解质,Alfa98%的物质销售,25g 400元。据本实验室经验,Alfa所售是有杂质的,对于高精度的电化学测量,比如说开孔富勒烯的OSWV测量是有影响的,这时需要对其进行纯化。

有两种纯化方法:

1EtOH和水重结晶。

2)无水EtOH乙醇重结晶三次,不过在我们实验室中发现重结晶一次足以应对我们的电化学实验室,条件为25g TBAPF6>100mL 乙醇(EtOH),热溶,几乎全溶,自然冷却后冰箱冷冻-16度进一步析出,抽滤,真空干燥24~72h,收率97%

参选文献 

1Purification of Laboratory Chemicals (4th Edition)

2)Robert L. Bedard, Lawrence F. Dahl, "Electrochemical analysis of biocapped triangular cobalt cyclopentadienyl clusters, [Co3(.eta.5-C5H5-xMex)3(.mu.3-X)(.mu.3-Y)]n (x = 0, 1, 5), containing mixed .pi.-acceptor X and .pi.-donor Y capping ligands [X = CO, NO; Y = NSiMe3, NC(O)NH2, NH]: pronounced variations in redox behavior as a function of coordinating ligands", Journal of the American Chemical Society, 1986, 108, 5933.

 

Purification of supporting electrolyte Tetra-n-butylammonium hexafluorophosphate (TBAPF6)



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