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Use of a PTV injector to achieve inverse‐large volume injection: Injection of volatile analytes in a semi‐volatile solvent
Author(s) -
Combs Michael T.,
Noe Okey
Publication year - 2001
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/1615-9314(20010401)24:4<291::aid-jssc291>3.0.co;2-d
Subject(s) - analyte , solvent , injector , chemistry , volume (thermodynamics) , chromatography , propylene carbonate , analytical chemistry (journal) , organic chemistry , thermodynamics , electrode , physics , electrochemistry
Large volume injection of volatile analytes in a semi‐volatile solvent, termed inverse‐LVI, has been accomplished using a programmable‐temperature vaporizing (PTV) injector. It was found that simple optimization of the time the split valve remained closed allowed complete analyte transfer to the column, while venting most of the solvent. Increasing the PTV temperature ramp from 10 K/s to 15 K/s was found to improve peak shapes, especially of the early eluting peaks, by decreasing the injection bandwidth. In addition, the optimum splitless time was found to be independent of injection volume (up to solvent limits) meaning only a single optimization was necessary for quantitative analyte transfer from each solvent. The ability to quantitatively transfer the analyte to the column was also found to be solvent independent (propylene carbonate, tridecane, and Butyl CARBITOL® Solvent were evaluated). Excellent data were obtained for injection volumes up to 15 μL of propylene carbonate and 36 μL of tridecane using an unpacked fritted PTV liner.