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，Alfa有98%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：

1）EtOH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 ：

1）Purification 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)

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: 

1）Purification 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.

 

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