Capillary supercritical fluid chromatography-mass spectrometry using a "high mass" quadrupole and splitless injection

Pinkston, J. David; Owens, Grover D.; Burkes, L. J.; Delaney, Thomas E.; Millington, David S.; Maltby, David

doi:10.1021/ac00161a003

Cited by 41 publications

(7 citation statements)

References 24 publications

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“…A second series of protonated oligomers is also clearly visible. These results are in keeping with the previously reported behavior of polysiloxanes under ammonia Cl conditions (1). The spectrometer was calibrated at high mass by using the calculated masses of the ammonium adducts.…”

supporting

confidence: 87%

“…Whether the pressure is slightly above or slightly below the "critical" pressure at this temperature has little effect on the solvating power of the carrier, on the flow rate of modified C02 through the restrictor, and on the pressure within the ion source region. This is borne out by our observations of the ion source pressure during SFI/MS with our sample cylinder and during normal pressure-programmed SFC/MS (1). Thus we feel justified in our use of this simple method to approximate conditions encountered in SFC/MS and in our use of the term "supercritical" in SFI/MS.…”

mentioning

confidence: 78%

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Supercritical fluid injection of polysiloxane solutions for calibration and tuning in supercritical fluid chromatography/mass spectrometry

Pinkston¹,

Owens²,

Petit³

1989

Anal. Chem.

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confidence: 87%

mentioning

confidence: 78%

Supercritical fluid injection of polysiloxane solutions for calibration and tuning in supercritical fluid chromatography/mass spectrometry

Pinkston¹,

Owens²,

Petit³

1989

Anal. Chem.

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“…The chromatographic resolution of the broad peaks assigned as hexa-, hepta-, and octaesters is poorer than that observed in the SFC-FID chromatogram (Figure 1). This may be at least partially due to the use of direct, on-column injection in the SFC/MS run rather than flow-split injection [16]. In addition, the selectivity of the two columns used for the separations shown in Figures 1 and 2 may have differed.…”

Section: Resultsmentioning

confidence: 99%

Use of SFC/MS for the confirmation of peak identities in the SFC/FID chromatogram of olestra

Pinkston

Bowling

1992

J Microcolumn Separations

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Abstract. Open tubular supercritical fluid chromatography (SFC) with flame ionization detection (FID) has been used for characterizing olestra, a mixture of fatty acid sucrose esters. In this publication, we describe SFC/mass spectrometry (SFC/MS) of olestra using the direct fluid introduction interface. Chemical ionization spectra were used in confirming SFC/FID peak identities. Electron ionization SFC/MS of olestra was also investigated. Both major and minor component peaks in the SFC chromatogram of olestra were characterized. A slight modification of the interface-probe tip was necessary for operation at higher temperature. A procedure was developed for tuning and calibrating the instrument in the 10-4O00-u mass range, chemical ionization mode using Ultramark 3200, a perfluorinated polyether. The use of additional pumping in the form of liquid nitrogen cooled cryopumps was key in providing good signal-to-noise ratios for the latereluting (i. e., eluting at higher mobile phase pressures and flow rates) olestra components.

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“…columns, however, packed column SFC/MS is gaining in popularity. 31 A variety of ionization sources have been used,but chemical ionization is the most common. Progress is rapidly being made with common HPLC/MS interfaces such as thermospray and particle beam for use with packed columns.…”

Section: Stationary Phasesmentioning

confidence: 99%

The Future Impact of Supercritical Fluid Chromatography on Packed Columns, Modified Fluids, and Detectors

Taylor

1997

ACS Symposium Series

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Supercritical fluids possess many of the attributes necessary for high performance chromatography. By changing the density of the mobile phase with a change in temperature and/or pressure, one can significantly change the observed chromatographic characteristics in an SFC separation. Polar compounds are widespread and are often nonvolatile and thermally labile. These properties make analysis by GC impossible without derivatization, and make method development for LC complex. SFC does not require solutes to be volatile, since separations are carried out at low temperatures, and method development is straightforward.The future of SFC will focus more on packed columns, modified CO2, and a host of either universal, element specific, or spectrometric detectors. Consequently, SFC will become more viewed like HPLC and will, in fact, replace HPLC in a number of applications because supercritical fluids have both better mass transport properties than liquids and are less harmful to the environment than liquids. The relatively poor solvating power of CO2 has dictated the use of primary and secondary modifiers in the mobile phase. These additives as well as packed columns which have much higher decompressed flow rates place new demands on the employment of detectors in SFC.A supercritical fluid exhibits physico-chemical properties intermediate between those of liquids and gases. Mass transfer is rapid with supercritical fluids. The diffusion coefficient is (in the vicinity of critical point) more than ten times that of a liquid. Density, viscosity, and diffusivity are dependent on temperature and pressure. The viscosity and diffusivity of the supercritical fluid approach that of a liquid as pressure is increased at fixed temperature. Diffusivity will increase with an increase in temperature at fixed pressure; whereas, viscosity decreases (unlike gases) with a temperature increase. Changes in viscosity and diffusivity are more pronounced in the region of the critical point. Even at high pressures (300-400 atm), diffusivity is 1-2 orders of magnitude greater than liquids.Therefore, the properties 134

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Capillary supercritical fluid chromatography-mass spectrometry using a "high mass" quadrupole and splitless injection

Cited by 41 publications

References 24 publications

Supercritical fluid injection of polysiloxane solutions for calibration and tuning in supercritical fluid chromatography/mass spectrometry

Supercritical fluid injection of polysiloxane solutions for calibration and tuning in supercritical fluid chromatography/mass spectrometry

Use of SFC/MS for the confirmation of peak identities in the SFC/FID chromatogram of olestra

The Future Impact of Supercritical Fluid Chromatography on Packed Columns, Modified Fluids, and Detectors

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