Quantitative Gas Chromatography University of 定量气相色谱大学.pptVIP

* Quantitative Gas Chromatography Chem 2223 Lab Prep * Goals and Objectives Goals To become familiar with basic methods of quantitative analysis by gas chromatography Specific Objectives Use the standard additions technique to determine the identities and concentrations of the components in a mixture of volatile organic compounds * Agilent 6850 Gas Chromatograph Top view showing injection port * Setup * The Chromatogram tR * A Capillary Column for GLC Fused silica tubing dc ? 0.3 mm df ? 1 ?m L = 15 - 60 m Polydimethylsiloxane (silicone) Good for retaining and separating nonpolar solutes by boiling point A thin layer of nonvolatile stationary phase is coating on the inner wall of the tubing (WCOT) * GC Analysis Conditions Inlet Split mode, 250 ?C. Split ratio: 5:1 Sample injection volume 0.5 ?L Carrier gas Helium Column ZB-5. Poly(dimethylsiloxane) with 5% phenyl substitution. 15 m long x 0.32 mm i.d., 1.0 ?m film thickness. Oven Temperatures (?C) and times Initial: 40.0 (4.50 min) Ramp: 45.0/min Final: 120.0 (1.00 min) Detector Thermal conductivity, 300 ?C Signal Date rate: 20 Hz * Sample Injection Rubber septum * Compound Structure or Formula Boiling Point, oC Relative Polarity Methanol (solvent) CH3OH 64.6 Polar Toluene 110.6 Nonpolar Ethylbenzene 135.2 Nonpolar p-Xylene 138.4 Nonpolar Bromobenzene (internal standard) 156.0 Polar Solutes and Internal Standard * Sample Chromatogram and Integration Report * Internal Standard Method Description In this approach, an internal standard is added to the sample, and the response from the analyte peak is compared to the internal standard. This approach corrects for minor variations in the injection volume. Response Factor (RF) The response factor accounts for differences in the detector response between the analyte and standard. * Internal Standard Method Description In this approach, an internal standard is added to the sample, and the response from the analyte peak is compared to the internal standard. Th