Extraction purge and trap

Amaral OC, Olivella L, Grimalt JO. 1994. Combined solvent extraction-purge and trap method for the determination of volatile organic compounds in sediments. J Chromatogr A 675(1) 177-187. 

In dynamic headspace extraction (purge and trap extraction mode), the constant passage of carrier gas through a warmed sample (purge), followed by trapping of the purged volatiles on a sorbent (trap) and desorption into a gas chromatograph take place. 

No information on analysis of tetrachloroethylene in soil or sediment was located. Several procedures for determination of the chemical in plants and food were located. GC/ECD and GC/HSD are most commonly used to analyze solid samples for tetrachloroethylene contamination. Extraction, purge-and-trap, and headspace analysis have all been used to prepare samples. Analysis of headspace gases by GC coupled with ECD, MS, or HSD has proven relatively sensitive (low- to sub-ppb range) and reproducible for a variety of foods (Boekhold et al. 1989 Entz and Hollifield 1982 EPA 1982c Pocklington 1992 ... 

SPME has become a valuable alternative to solvent extraction, purge-and-trap (dynamic), and static headspace methods (1 ). This is true for the analysis of flavors, fragrances, food aromas, and biological systems as is evidenced by... 

Adjusting the Analyte s Concentration Analytes present at concentrations too small to give an adequate signal need to be concentrated before analyzing. A side benefit of many of the extraction methods outlined earlier is that they often concentrate the analytes. Volatile organic materials isolated from aqueous samples by a purge and trap, for example, can be concentrated by as much as 1000-fold. 

To satisfy the Resource Conservation and Recovery Act (1977) and its amendment for hazardous and solid waste (1984), the 80(K) Series Methods have been designed to analyze solid waste, soUs, and groundwater. In particular, methods 8240/8260 require the use of a purge-and-trap device in conjunction with packed or capillary GC/MS, respectively, for the analysis of purgeable organic compounds. Methods 8250/8270 concern analyses for the less-volatile bases, neutrals, and acids by GC/MS after extraction from the matrix by an organic solvent. 

Target compounds are specified for each Series Method. Volatile compounds that need to be analyzed can be extracted from the matrix by a purge-and-trap device. 

Figure 15-12 is a schematic illustration of a technique known as acid volatile sulfides/ simultaneously extracted metals analysis (AVS/SEM). Briefly, a strong acid is added to a sediment sample to release the sediment-associated sulfides, acid volatile sulfides, which are analyzed by a cold-acid purge-and-trap technique (e.g., Allen et ai, 1993). The assumption shown in Fig. 15-12 is that the sulfides are present in the sediments in the form of either FeS or MeS (a metal sulfide). In a parallel analysis, metals simultaneously released with the sulfides (the simultaneously extracted metals) are also quantified, for example, by graphite furnace atomic absorption spectrometry. Metals released during the acid attack are considered to be associated with the phases operationally defined as "exchangeable," "carbonate," "Fe and Mn oxides," "FeS," and "MeS."... 

Analysis of soils and sediments is typically performed with aqueous extraction followed by headspace analysis or the purge-and-trap methods described above. Comparison of these two methods has found them equally suited for on-site analysis of soils (Hewitt et al. 1992). The major limitation of headspace analysis has been incomplete desorption of trichloroethylene from the soil matrix, although this was shown to be alleviated by methanol extraction (Pavlostathis and Mathavan 1992). 

Solid-phase microextraction eliminates many of the drawbacks of other sample preparation techniques, such as headspace, purge and trap, LLE, SPE, or simultaneous distillation/extraction techniques, including excessive preparation time or extravagant use of high-purity organic solvents. SPME ranks amongst other solvent-free sample preparation methods, notably SBSE (Section 3.5.3) and PT (Section 4.2.2) which essentially operate at room temperature, and DHS (Section 4.2.2),... 

Few well characterized, validated methods are available for the determination of w-hexane in blood. A purge-and-trap method for volatiles has been developed and validated by researchers at the Centers for Disease Control and Prevention (CDC) (Ashley et al. 1992, 1994). Extension of the method to include /7-hexane should be possible. Current analytical methods utilize capillary GC columns and MS detection to provide the sensitivity and selectivity required for the analysis. Detection limits are in the low ppb range (Brugnone et al. 1991 Schuberth 1994). Headspace extraction followed by GC analysis has also been utilized for the determination of /7-hexanc in blood (Brugnone et al. 1991 Michael et al. 1980 Schuberth 1994) however, very little performance data are available. 

Dynamic headspace-extraction stripping and purge-and-trap methodology are used most often for determination of M-hcxanc in water and hazardous wastes. Dynamic headspace extraction techniques have been applied to water samples (Roberts and Burton 1994) and sediment (Bianchi et al. 1991). Detection limits of 0.5 g/L were reported for lake water (Roberts and Burton 1994) and 20 ng/kg (ppt) for sediment (Bianchi et al. 1991). Supercritical fluid extraction (SFE) is a relatively new technique that has been applied to -hcxane in soil (Yang et al. 1995). Membrane extraction of M-hexane from water samples has been developed to provide online, continuous monitoring (Wong et al. 1995 Xu and Mitra... 

Kester [5] has discussed the application of the purge and trap gas chromatographic method to the determination of aliphatic chloro-compounds in soil. Following methanol extraction of the soil the extract is gas purged and the purge gases trapped on a Tenax silica gel/ charcoal trap followed by thermal desorption from the trap and examination by gas chromatography and mass spectrometry. Compounds that have been determined by this method are listed in Table 5.1. 

Askari et al. [15] have compared purge and trap, methanol immersion and hot solvent extraction methods for the determination of volatile organic compound in aged soil. These workers found that hot solvent extraction is much more effective than the US Environmental Protection Agency approved purge and trap technique [7, 8]. 

Solvent extraction procedures involve collection of sample by an appropriate device and subsequent immediate placement into a borosilicate glass vessel, which contains a known quantity of ultrapure methanol. The bottle is then transported to the laboratory at 4°C, and the methanol fraction analyzed by purge-and-trap gas chromatography (or a similar procedure). 

In general, zero-headspace procedures are employed when the concentrations of volatiles in the soil are relatively low, and solvent extraction methods are used for more polluted soils. Irrespective of which procedure is used, quantitation of volatiles in soil is subject to serious errors if sufficient care is not taken with the sampling operation. Although direct purge-and-trap methods are frequently advocated for the determination of volatiles in samples collected by zero-headspace procedures, there are certain problems associated with this technique. Caution is advised since the procedure really collects only that fraction of the volatile that exists in a free form within the soil pore spaces or is at least in a facile equilibrium with this fraction. 

Soxhlet, sonication, supercritical fluid, subcritical or accelerated solvent, and purge-and-trap extraction have been introduced into a variety of methods for the extraction of contaminated soil. Headspace is recommended as a screening method. Shaking/vortexing is adequate for the extraction of petroleum hydrocarbons in most environmental samples. For these extraction methods, the ability to extract petroleum hydrocarbons from soil and water samples depends on the solvent and the sample matrix. Surrogates (compounds of known identity and quantity) are frequently added to monitor extraction efficiency. Environmental laboratories also generally perform matrix spikes (addition of target analytes) to determine if the soil or water matrix retains analytes. 

Purge and trap Separatory funnel extraction Headspace Continuous liquid-liquid extraction Solid-phase extraction... 

For example, if gasoline is suspected to be the sole contaminant, the method will use purge-and-trap sample introduction. If higher-boiling petroleum fractions (diesel, middle distillates, motor oil) are the contaminants, the analysis will use direct injection and hotter oven temperatures. Mixtures or unknown contamination may require both volatile range and extractable range analyses. Alternatively, a single injection can be used to analyze the entire sample, but the extraction method must not use a solvent evaporation step. 

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... 

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