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

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.

[1]  B. W. Wright,et al.  Supercritical fluid extraction and direct fluid injection mass spectrometry for the determination of trichothecene mycotoxins in wheat samples. , 1986, Analytical chemistry.

[2]  B. W. Wright,et al.  Performance of capillary restrictors in supercritical fluid chromatography , 1986 .

[3]  K. Markides,et al.  Capillary Supercritical Fluid Chromatography of Labile Carboxylic Acids , 1986 .

[4]  J. M. Levy,et al.  Investigations of the Uses of Modifiers in Supercritical Fluid Chromatography , 1986 .

[5]  D. R. Kalkwarf,et al.  Characterization of supercritical fluid solvents using solvatochromic shifts , 1986 .

[6]  H. Schwartz,et al.  Integral Pressure Restrictor for Capillary SFC , 1986 .

[7]  B. W. Wright,et al.  Ammonia and methane chemical ionization mass spectra of acid and carbamate pesticides using direct supercritical fluid injection , 1986 .

[8]  B. W. Wright,et al.  Investigation of polar modifiers in carbon dioxide mobile phases for capillary supercritical fluid chromatography , 1986 .

[9]  B. W. Wright,et al.  Pressure programming in supercritical fluid chromatography , 1985 .

[10]  B. W. Wright,et al.  Investigation of retention and selectivity effects using various mobile phases in capillary supercritical fluid chromatography , 1985 .

[11]  J. Henion,et al.  Supercritical fluid chromatography of polar drugs using small-particle packed columns with mass spectrometric detection. , 1985, Analytical chemistry.

[12]  T. L. Chester,et al.  Separation of sucrose polyesters by capillary supercritical-fluid chromatography/flame ionization detection with robot-pulled capillary restrictors , 1985 .

[13]  B. W. Wright,et al.  Rapid and high resolution capillary supercritical fluid chromatography (SFC) and SFC/MS of trichothecene mycotoxins. , 1985, Journal of chromatographic science.

[14]  B. W. Wright,et al.  Rapid capillary supercritical fluid chromatographic analysis of carbamate pesticides , 1985 .

[15]  Richard D. Smith,et al.  Capillary supercritical fluid chromatography/mass spectrometry with electron impact ionization , 1984 .

[16]  B. W. Wright,et al.  Rapid and efficient capillary column supercritical fluid chromatography with mass spectrometric detection , 1984 .

[17]  B. W. Wright,et al.  New methods for characterization of supercritical fluid solutions , 1984 .

[18]  Milton L. Lee,et al.  Effect of column diameter on efficiency in capillary supercritical fluid chromatography , 1984 .

[19]  B. W. Wright,et al.  Supercritical fluid chromatography and supercritical fluid chromatography—mass spectrometry of marine diesel fuel , 1984 .

[20]  T. L. Chester.  Capillary supercritical-fluid chromatography with flame-ionization detection: reduction of detection artifacts and extension of detectable molecular weight range , 1984 .

[21]  G. Guiochon,et al.  Chapter 1 Narrow-Bore and Micro-Bore Columns in Liquid Chromatography , 1984 .

[22]  M. Vestal.  Ionization techniques for nonvolatile molecules , 1983 .

[23]  Richard D. Smith,et al.  Mass spectrometry with direct supercritical fluid injection , 1983 .

[24]  Milton L. Lee,et al.  Capillary supercritical-fluid chromatography with conventional flame detectors , 1983 .

[25]  H. Lauer,et al.  Mobile-phase transport properties of liquefied gases in near critical and supercritical fluid chromatography , 1983 .

[26]  B. W. Wright,et al.  Free radical cross-linking in the preparation of non-extractable stationay phases for capillary gas chromatography , 1982 .

[27]  Richard D. Smith,et al.  Direct fluid injection interface for capillary supercritical fluid chromatography-mass spectrometry , 1982 .

[28]  A. L. Wahrhaftig,et al.  Direct coupling of a dense (supercritical) gas chromatograph to a mass spectrometer using a supersonic molecular beam interface , 1981 .