Packed-column supercritical fluid chromatography with splitless flame ionization detection

2004 ◽  
Vol 82 (3) ◽  
pp. 479-482 ◽  
Author(s):  
Kevin B Thurbide ◽  
Shawn Gilbert
Keyword(s):  
Supercritical Fluid ◽  
Supercritical Fluid Chromatography ◽  
Packed Column ◽  
Flame Ionization Detector ◽  
Gas Flows ◽  
Ionization Detector ◽  
Flow Rates ◽  
Flame Ionization ◽  
Stable Flame

The design and characterization of a flame ionization detector (FID) that is compatible with the high flow rates of packed-column supercritical fluid chromatography (pSFC) is presented. The modified FID uses a large quartz burner (4.0 mm i.d.) in place of the conventional burner (0.4 mm i.d.) and operates a stable flame in the presence of gas flows tested up to nearly 3000 mL/min. This modification allows the full flow of effluent from a pSFC column (i.e., splitless mode) to be directed into the FID. Results demonstrate that the modified FID yields response that is within a factor of 3 to that of a commercial FID. The attributes of the modified detector indicate that this approach could be a reliable and relatively simple means of achieving a splitless pSFC-FID system.Key words: supercritical fluid chromatography, packed column, splitless, flame ionization detector.

Supercritical argon as a mobile phase for the flame photometric detection of sulfur

2003 ◽  
Vol 81 (10) ◽  
pp. 1051-1056 ◽  
Author(s):  
Kevin B Thurbide ◽  
Brad W Cooke
Keyword(s):  
Carbon Dioxide ◽  
Supercritical Carbon Dioxide ◽  
Supercritical Fluid ◽  
Supercritical Fluid Chromatography ◽  
Mobile Phase ◽  
Packed Column ◽  
Flow Rates ◽  
Photometric Detection ◽  
Flame Photometric Detection ◽  
Background Emission

The background emission properties of supercritical argon and supercritical carbon dioxide mobile phases in packed column supercritical fluid chromatography (pSFC) with flame photometric detection (FPD) were compared. As column flow rates were increased toward common values used in pSFC, the carbon dioxide background emission grew enormously. The resulting emission spectrum displayed dominant features at wavelengths between 325 and 525 nm, consisting of a complex series of overlapping molecular emission band systems partly attributed to CO* and CH*. By comparison, when using the same flow rates with a supercritical argon mobile phase, the background emission was identical to that of the FPD flame without column effluent. In terms of intensity, when using a column flow rate of 2 mL/min, supercritical carbon dioxide contributes a background emission in the FPD that is about 3 × 105 times larger than that produced by supercritical argon. This difference leads to an improvement of two orders of magnitude in the pSFC-FPD signal-to-noise ratio for sulfur when a supercritical argon mobile phase is used. Results indicate that supercritical argon could also be advantageous for the pSFC-FPD analysis of other elements.Key words: supercritical fluid chromatography, packed column, flame photometric detection, supercritical argon.

Application of the ionization detector and the alkali flame ionization detector in capillary liquid chromatography

1983 ◽  
Vol 48 (8) ◽  
pp. 2343-2351 ◽  
Author(s):  
Miloš Krejčí ◽  
Miroslav Rusek ◽  
Jana Houdková
Keyword(s):  
Liquid Chromatography ◽  
Capillary Column ◽  
Capillary Liquid Chromatography ◽  
Flame Ionization Detector ◽  
Detection Time ◽  
Ionization Detector ◽  
Flow Rates ◽  
Flame Ionization ◽  
Mass Flow Rates ◽  
Capillary Liquid

A possibility is demonstrated of the use of the flame ionization detector (FID) and the alkali metal flame ionization detector (AFID) in capillary liquid chromatography. The minimum detectable mass flow rates for the FID and the AFID were ≈10-12 and ≈10-13 g s-1, respectively. The detection time constant is about 1 s allows for operation with columns of inner diameters of 10-60 μm and lengths above 1 m. The suggested design of the detector is described. The burner allows the total effluent from the column to enter the detector. The temperature of the end of the capillary column in the burner is controllable.

scholarly journals Gas chromatographic-mass spectrometric (GC-MS) identification of compounds in concentrates of Puerto Rican rum.

1969 ◽  
Vol 77 (1-2) ◽  
pp. 69-93
Author(s):  
Heriberto Batiz ◽  
Carmen L. Cacho
Keyword(s):  
High Performance ◽  
Capillary Column ◽  
Packed Column ◽  
Fold Increase ◽  
Polar Compounds ◽  
Flame Ionization Detector ◽  
Alternative Methods ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Highly Polar Compounds

A procedure is described for the improved identification of compounds in rums. It includes the preparation of rum concentrates using a Kuderna concentrator (KC), and the profiles of the resultant products using a gas chromatographic (GC) system, where the separation with a packed column is compared with that of a capillary column. The packed column was connected in the chromatograph to the flame ionization detector (FID) whereas the capillary column was interfaced, in the same chromatograph, with the mass spectrometry (MS) probe. These techniques assessed simultaneously, provided alternative methods for compound profiles, one using the capillary column only for identification purpose with the GC-MS, and the other with a high performance gas chromatograpy-flame ionization detector (HPGC-FID) with a column. The HPGC-FID offered the best combination for the direct quantitative identification of compounds in rum concentrates. As expected, the number of compounds separated by the two procedures was the same, although some signals in the chromatogram of the packed column were too broad and unresolved. This is the case when highly polar compounds are separated in a packed column with an unmodified liquid phase such as Carbowax 20M. Twenty-two compounds were identified in one rum concentrate, 16 with a probability of 70% or higher of being correctly identified. The present procedure resulted in about a 250 to 500- fold increase in the concentration of compounds, as compared with the concentration of compounds in the original rum sample. The vast majority of these compounds were found at a concentration of 20 ppb or less.

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