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Water as an in situ NMR indicator for impurity acids in ionic liquids. | LitMetric

Water as an in situ NMR indicator for impurity acids in ionic liquids.

Anal Chem

Institute for Chemical Research, Kyoto University, Kyoto 611-0011, Japan.

Published: January 2009

AI Article Synopsis

  • A new NMR spectroscopic method was developed to detect acid contamination in ionic liquids (ILs) using the chemical shift and spectral width of added water as indicators.
  • The detection limit of this method is very low, below 10(-3) mol kg(-1), making it highly effective for various imidazolium- and ammonium-based ILs, unless they contain acidic components.
  • The method was shown to successfully monitor the purification of 1-butyl-3-methylimidazolium methanesulfonate from acetone, revealing that impurity acids can be nearly completely eliminated through single or double recrystallization.

Article Abstract

A sensitive in situ NMR spectroscopic method for detecting acids contaminating ionic liquids (ILs) has been developed. The chemical shift and the spectral width of water added to ILs were used as indicators to measure the impurity acid level. Owing to the high resolution power of NMR, the detection limit is below the level of 10(-3) mol kg(-1). A new method is applicable to a number of commonly used ILs such as the imidazolium- and ammonium-based ILs except for those composed of acidic cations or anions. The method was utilized to monitor the purification efficiency in the recrystallization of a typical hydrophilic IL, 1-butyl-3-methylimidazolium methanesulfonate from acetone. It was demonstrated that impurity acids can be almost perfectly removed by single or double recrystallization.

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Source
http://dx.doi.org/10.1021/ac801767uDOI Listing

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