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Instument Methods
Chapter22: Gas and Liquid Chromatography12014 - 2015
22.4 Simple Preparation Sample preparation is the process of transforming a sample into a form that is suitable for analysis. Solid-phase microextraction is a method to extract compounds from liquids, air, or even sludge without using any solvent. 2
Syringe barrel
Septum piercing needle Fiber attachment tubingFused silica fiber with stationary liquid-phase coating Figure 24-24 Syringe for solid-phase microextraction. The fused silica fiber is withdrawn inside the steel needle after sample collection and when the syringe is used to pierce a septum.3
Retract fiber and withdraw needle
Figure 24-25 Sampling by solid-phase microextraction and desorption of analyte from the coated fiber into a gas chromatograph. [Adapted from Supelco Chromatography Products catalog, Bellefonte, PA.]
Expose hot fiber tocarrier gas for fixed time(column is cold) Piercechromatographyseptum withmetal needleRetract fiberand withdrawneedleExpose fiberto solution orheadspace forfixed time withstirringPierce sampleseptum withmetal needle
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Purge and trap is a method for removing volatile analytes from liquids or solids (such as groundwater or soil), concentrating the analytes, and introducing them into a gas chromatograph.5Sample Cleanup Refers to the removal of undesirable components of an unknow that interfere with measurement of analyte.
Injection portOvenSample vialPurge gasAdsorption tubeSilanized glass woolStrongestadsorbentStrongeradsorbentModerateadsorbent Figure 24-27 Purge and trap apparatus for extracting volatile substances from a liquid or solid by flowing gas.AB6
Chapter26: Chromatographic Methods and Capillary Electrophoresis7
26-1. Ion-Exchange Chromatography In ion-exchange chromatography, retention is based on the attraction between solute ions and charged sites bound to the stationary phase. In anion exchangers, positively charged groups on the stationary phase attract solute anions. Cation exchangers contain covalently bound, negatively charged sites that attract solute cations.8
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