Chromium determination by supercritical fluid chromatography with inductively coupled plasma mass spectrometric and flame ionization detection.
Supercritical fluid chromatography (SFC) has been investigated for the separation of a pair of beta-ketonate chromium compounds and a thermally labile organochromium dimer. A limited comparison between flame ionization detection (FID) and inductively coupled plasma mass spectrometric (ICP-MS) detection of these compounds is presented. The beta-ketonate complexes were observed with both detectors, while the thermally labile dimer was not observed with ICP-MS detection. Detection limits for these compounds with ICP-MS were in the range of 0.9 to 3 pg with FID giving values between 10 and 250 pg. Reproducibility of the method is between 1 and 4% relative standard deviation (R.S.D.). The technique provided a linear response over approximately three orders of magnitude. The effect of two mobile phases (nitrous oxide and carbon dioxide) on the detection by each of the detectors are presented in a qualitative manner. Finally, the SFC-ICP interface heating method and the manner in which the restrictor is heated in the FID system are compared and there effect on the chromatography discussed.
Carey
J M
JM
University of Cincinnati, Department of Chemistry, OH 45221-0172.
Vela
N P
NP
Caruso
J A
JA
D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002853:Chromatography, Liquid; D002857:Chromium / Q000032:analysis*; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D013056:Spectrophotometry, Ultraviolet; D013696:Temperature
D007202:Indicators and Reagents; D002857:Chromium