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Mass spectrometer interface for microbore and high flow rate capillary supercritical fluid chromatography with splitless injection

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00128a005· OSTI ID:7006351

Improved methods for interfacing microbore and capillary supercritical fluid chromatography (SFC) with mass spectrometry, using a high flow rate interface with splitless injection, are described. The new interface incorporated a mechanically pumped expansion region behind the chemical ionization repeller electrode, allowing higher gas flow rates (100-200 mg of CO/sub 2//min) than previous interfaces and providing an improvement over direct pumping of the ion source in terms of background contributions, ionization efficiency, and sensitivity. The effects of sample flow rate, restrictor geometry, and effluent heating were studied relevant to the transfer and detection of nonvolatile analytes. Separations are compared both microbore and capillary columns for a polarity test mixture, pesticides, and the nonionic surfactant Triton X-100 polymer using supercritical carbon dioxide and carbon dioxide modified with methanol. Microbore columns were shown to have greater limitations for pressure programming, and superior results were obtained with capillary columns.

Research Organization:
Pacific Northwest Lab., Richland, WA
DOE Contract Number:
AC06-76RL01830
OSTI ID:
7006351
Journal Information:
Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 59:1; ISSN ANCHA
Country of Publication:
United States
Language:
English