Headspace analysis solvent trapping

Separation of carbon tetrachloride from biological samples may achieved by headspace analysis, purge-and-trap collection from aqueous solution or slurry samples, solvent extraction, or direct collection on resins. Headspace analysis offers speed, simplicity, and good reproducibility, but partitioning of the analyte between the headspace and the sample matrix is dependent upon the nature of the matrix and must be determined separately for each different kind of matrix (Walters 1986). 

The headspace is the air above or around a fragrant substance that contains the volatile compounds. This can be collected for analysis when extraction of the volatiles from the material is not viable. This technique has been extensively developed for the collection and analysis of flower volatiles since many flowers do not yield an extract that reflects the odour of the fresh flower, while others are simply too rare to be available in sufficient quantity for extraction. Many different techniques have been applied to the collection of volatiles from the air above flowers including the use of cold traps, solvent traps, adsorbent materials... 

When analytes are under the limit of detection (LOD) of the technique is necessary to use enrichment techniques. In headspace analysis, for this purpose the target analytes must be separated from the headspace gas either by absorption into a liquid or by adsorption onto a solid adsorbent and also by condensation in a cold trap. (Kolb, 1999). Solvent free techniques are particularly desirable in case of trace analysis to avoid problems with solvent impurities. Consequently, cryogenic trapping is the preferred choice to improved detection limits in static headspace analysis... 

Distillation. Essential Oils. Extraction Solvent Extraction Principles Solid-Phase Extraction Solid-Phase Microextraction. Gas Chromatography Detectors Mass Spectrometry Chiral Separations. Headspace Analysis Static Purge and Trap. Mass Spectrometry Principles Selected Ion Monitoring. Quality Assurance Quality Control. Sensors Overview. 

The discussion of headspace methods for blood alcohol and solid-phase micro extraction (SPME) in Section 4.2 introduced the concept of creating an enriched head-space above a sample. Headspace methods may be passive or active and may involve heating the sample. Dynamic headspace (DHS) methods, used in arson analyses, exploit the equilibrium at the liquid-sample interface by sweeping tire headspace with a constant stream of gas, usually helium. DHS is also referred to as purge-and-trap (FT), allhough the latter can also mean a specific t) of sample preconcentrator used in environmental analysis. The trap material can be thermally desorbed or desorbed wifii a solvent. The thermal method is preferred, but is not always possible. The choice of trapping or sorbent materials depends on fire application arson typically requires charcoal or charcoal combinations. 

Heat extraction techniques for solid sample preparation in GC are static and dynamic headspace analysis (SHS, DHS, HS-SPME and HSSE), thermal desorption (TD-GC, TD-GC-MS), pyrolysis and thermochromatography. Nomenclature is not unambiguous as to DHS, TD and PT. The terminology purge-and-trap is usually preferred for the simplest dynamic technique in which it is not necessary to subject the sample to either solvents or elevated temperatures. Scheme 2.7 shows the family of headspace sampling techniques. Headspace sorptive extraction (HSSE) and HS-SPME represent high capacity static headspace. 

A comprehensive overview of the techniques most commonly used for instrumental analysis of flavor compounds in food has been recently reported [3]. Several methods used for sample treatment are described, as well as the following techniques for extraction prior to GC analysis solvent extraction and distillation techniques, headspace methods, and solid-phase microextraction. The use of GC-olfactometry and of ion-trap MS in food aroma analysis is also described. 

Fig. 3. Combined headspace sampiing, themnai desorption and purge and trap injection system with exampie headspace chromatogram, (a) injection system (b) Headspace chromatogram. Detection of solvents In blood sample by headspace analysis as part of an Industrial hygiene study. Sample held at 60°C. Column UCON LB 550, 25 m, at 40°C. Produced tom D.W. Grant, Capillary Gas Chromatography, 1996. John Wiiey Sons Ltd. Reproduced with permission.

Hcxanc can be determined in biological fluids and tissues and breath using a variety of analytical methods. Representative methods are summarized in Table 6-1. Most methods utilize gas chromatographic (GC) techniques for determination of -hexane. The three methods used for preparation of biological fluids and tissues for analysis are solvent extraction, direct aqueous injection, and headspace extraction. Breath samples are usually collected on adsorbent traps or in sampling bags or canisters prior to analysis by GC. 

The analysis involves gas chromatographic methods such as purge and trap, vacuum distillation, and headspace (Askari et al., 1996). On the other hand, samples for the determination of semi- and nonvolatile hydrocarbons need not be collected in such a rigorous manner. On arrival at the laboratory, they require extraction by techniques such as solvent or supercritical fiuid. Some cleanup of... 

For a compound to contribute to the aroma of a food, the compound must have odor activity and volatilize from the food into the head-space at a concentration above its detection threshold. Since aroma compounds are usually present in a headspace at levels too low to be detected by GC, headspace extraction also requires concentration. SPME headspace extraction lends itself to aroma analysis, since it selectively extracts and concentrates compounds in the headspace. Some other methods used for sample preparation for aroma analysis include purge-and-trap or porous polymer extraction, static headspace extraction, and solvent extraction. A comparison of these methods is summarized in Table Gl.6.2. 

There are many techniques available for the preparation of volatile analytes prior to instrumental analysis. In this chapter the major techniques, leading primarily to gas chromatographic analysis, have been explored. It is seen that the classical techniques purge and trap, static headspace extraction, and liquid-liquid extraction still have important roles in chemical analysis of all sample types. New techniques, such as SPME and membrane extraction, offer promise as the needs for automation, field sampling, and solvent reduction increase. For whatever problems may confront the analyst, there is an appropriate technique available the main analytical difficulty may lie in choosing the most appropriate one. 

Determination of volatiles at the trace level is also possible by pre-concentrating the headspace volatiles on a suitable adsorbent. The trapped compounds are subsequently recovered by thermal desorption in front of a cooled trap connected to the capillary column or by solvent elution followed by splitless or on-column injection. These methods, called dynamic headspace enrichment or purge-and-trap , have been applied to trace level analysis of volatiles, using conventional electrically heated systems [ 31, 32 ], a Curie-point Pyrolyser... 

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