ORGANIC SALTS, LIQUID AT ROOM-TEMPERATURE, AS MOBILE PHASES IN LIQUID-CHROMATOGRAPHY
ORGANIC SALTS, LIQUID AT ROOM-TEMPERATURE, AS MOBILE PHASES IN LIQUID-CHROMATOGRAPHY
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DOI：
10.1016/s0021-9673(01)83397-5
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发表时间：
1986-02-21
期刊：
影响因子：
--
通讯作者：
FURTON, KG
中科院分区：
文献类型：
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作者：
POOLE, CF;KERSTEN, BR;FURTON, KG
描述了通式为Rn-aNH+aX-的六种烷基铵盐的合成，其中R =乙基、丙基、丁基或仲丁基，X-=硝酸盐或硫氰酸盐，n< 4且a = 0、1、2或3。其中四种盐在室温下是液体，以前是未知的。通过NMR（1H，13 C，15 N），IR和快原子轰击质谱进行结构表征。上述硝酸盐和硫氰酸盐以及三种其它已知的液体盐，三乙基己基氯化铵，通过标准物理测量技术表征，以确定它们作为色谱溶剂的适用性。测定了它们的熔点、折光率、紫外光谱、与常用有机溶剂的相容性、水溶液的pH值、密度和粘度等物理性质，得出结论：硝酸烷基铵和硫氰酸盐可作为液相色谱中的移动的相，当它们与低粘度的第二溶剂混合时，可作为液相色谱中的流动相。给出了合适的方程来预测烷基硝酸铵和硫氰酸盐与水、甲醇、乙腈、四氢呋喃和二氯甲烷的所有体积比的混合物的粘度。液体有机盐与非极性有机溶剂形成不混溶的溶剂对，并且还应当适用于液-液色谱法和液-液萃取。
The synthesis of six alkylammonium salts of the general formula Rn—aNH+aX−, where R = ethyl, propyl, butyl or sec.−butyl, X−= nitrate or thiocyanate,n< 4 and a = 0, 1,2 or 3 is described. Four of these salts, which are liquid at room temperature, were previously unknown. Structural characterization was performed by NMR (1H,13C,15N), IR and fast-atom bombardment mass spectrometry. The above nitrate and thiocyanate salts and three other known liquid salts, triethylhexylammonium chloride, were characterized by standard physical measurement techniques to determine their suitability as chromatographic solvents. The physical properties measured include melting point, refractive index, UV spectra, miscibility with common organic solvents, aqueous solution pH, density and viscosity.It was concluded that the alkylammonium nitrate the thiocyanate salts could be used as mobile phases in liquid chromatography when mixed with a second solvent of low viscosity. Suitable equations are given to predict the viscosity of mixtures of alkylammonium nitrate and thiocyanate salts in all volume proportions with water, methanol, acetonitrile, tetrahydrofuran and dichloromethane. The liquid organic salts form immiscible solvent pairs with non-polar organic solvents and should also be suitable for use in liquid—liquid chromatography and liquid—liquid extraction.