Headspace sampling techniques static

Prom the experimental point of view the static headspace sampling technique is very simple. The sample, either solid or liquid, is placed in a glass vial of appropriate size and closed with a Teflon-lined silicone septum. The 1 is carefully... 

A substantial amount of information on volatiles can be obtained with less than 30 g of each of these samples in a direct DHS/GC/MS analysis. DHS operation sweeps volatile flavors from the surface of food samples in a similar way as we sniff for the volatile flavors of a food. DHS does not require high sampling temperature or solvent for extraction and may be considered as a lcw-artifact arcma sampling technique. The concentrating effect of DHS provides better sensitivity than static headspace sampling. Techniques such as GC-coupled aroma perception and GC/MS identification can be used to complement other approaches in improvement of flavor quality of a variety of products. 

Before analysis, the bacterial cultures should be transferred into standard 20 ml headspace vials and sealed with PTFE-lined Teflon caps to equilibrate the headspace. Sample handling is a critical step affecting the analysis by E-nose. The quality of the analysis can be improved by adopting an appropriate sampling technique. To introduce the volatile compounds present in the headspace (HS) of the sample into the E-nose s detection system, several headspace sampling techniques have been used in E-nose. Typically, the methods of headspace sampling (Ayoko, 2004) include static headspace (SHS) technique, purge and trap (P T) technique, stir bar sorptive extraction (SBSE) technique, inside-needle dynamic... 

The different headspace sampling techniques can be classified into one-step procedures, such as static headspace, where an aliquot of the vapor phase is transferred in a closed container directly to the gas chromatograph, and two-step procedures, where the volatile analytes are transferred from the matrix of the headspace to a "trap" where they are released... 

The coupling of a pervaporator to a gas chromatograph is one of the most promising uses of pervaporation and is worth a more detailed discussion, because of the advantages that pervaporation presents as compared with both static and dynamic headspace sampling techniques. In the static approach, the sample is placed in a closed chamber and heated until the volatile compoimds in the headspace reach the equilibrium with the sample. Then, part of... 

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. 

Despite the utility of these techniques, a distinct disadvantage is that very low concentration components may be masked by higher concentration interferants in such cases, devices based on thermal desorption (absorbent packing, static headspace sampling, cryogenic trapping) may prove useful. 

Headspace sampling is usually employed to identify the volatile constituents of a complex matrix without actually taking a sample of the material itself. There are three variations of the technique (a) static head-space sampling, (b) dynamic headspace sampling, and (c) purge and trapping. 

A sampling technique known as headspace , of which there are two modes, static and dynamic, is very widespread in GC for the qualitative and even quantitative analyses of volatile constituents present in some samples (cf. Chapter 21). 

An essential oil (EO) is internationally defined as the product obtained by hydro-, steam-, or dry-distillation of a plant or of some of its parts, or by a suitable mechanical process without heating, as in the case of Citrus fruits (AFNOR, 1998 Council of Europe, 2010). Vacuum distUladon solvent extraction combined offline with distillation simultaneous distillation extraction supercritical fluid extraction microwave-assisted extraction and hydro-distiUation and static, dynamic, and high concentration capacity headspace sampling are other techniques used for extracting the volatile fraction from aromatic plants, although the products of these processes cannot be termed EOs (Faleiro and Miguel, 2013). 

Liquid-liquid extraction has a counterpart for the determination of VOCs in the technique known as static or equilibrium headspace sampling. The technique is most often combined with the determinative step and is often referred to as static headspace gas chromatography, abbreviated HS-GC. The principles that underlie this technique will be outlined in this section. The decision to measure VOCs in the environment by either HS or purge and trap (P T or dynamic headspace) represents one of the ongoing controversies in the field of TEQA. This author has worked in two different environmental laboratories in which one used P T as the predominant technique to determine VOCs in the environment and the other used HS-GC. 

Yes there is and it is Method 5021 from the recently updated SW-846 series of methods published by the Office of Solid Waste at EPA. The method uses the static HS technique to determine VOCs from soil or other solid matrix. This section will focus on some of the details of this method because it includes many of the quality control (QC) features that were absent in the method just discussed. This method also introduces some experimental considerations with respect to trace VOC analyses of soil samples (34). The method is applicable to a wide range of organic compounds that have sufficiently high volatility to be effectively removed from soil samples using static HS techniques. The method is used in combination with a determinative technique that is described in the 8000 series. The method cautions the user to the fact that solid samples whose organic matter content exceeds 1% or for compounds with high octanol/water partition coefficients may yield a lower result for the determination of VOCs by static HS in comparison to dynamic headspace (P T). It is... 

Method 5021 describes the automated static-HS technique. Static HS has been introduced in this book from a theoretical viewpoint. A soil sample is placed in a tared septum-sealed vial at the time of sampling. A matrix modifier containing internal and/or surrogate standards is added. The sample vial is placed into an automated equilibrium headspace sampler. The vial s temperature is elevated to a fixed value that does not change over time and the contents of the vial is mixed by mechanical agitation. A measured volume of headspace is automatically introduced into a GC or a GC-MS. The method is automated and downtime is minimal. However, the cost of the automated system is appreciable. Contamination of the instru-... 

Trace environmental quantitative analysis (TEQA) utilizes various determinative teehniques (Chapter 4) in combination with various sample prep techniques (Chapter 3). In this appendix, one specific trace analysis using static headspace sampling automatically coupled to capillary gas chromatography with element specific detection is described. LSQUARES is a computer program developed by the author in BASIC and is used in the quantitative analysis discussed below. The actual program written in GWBASIC is also listed after illustrating its use in TEQA. 

Automated headspace systems have been offered by several manufacturers for many years, including Thermo Electron Corporation (San Jose, California, U.S.A.), PerkinElmer (Wellesley, Massachusetts, U.S.A.), Tekmar (Mason, Ohio, U.S.A.), and Agilent Technologies (Palo Alto, California, U.S.A.). There are essentially three injection techniques for static headspace sampling gas-tight syringe, balanced-pressure, and pressure-loop injection (Eig. 2). All these techniques are used on commercial headspace systems and are described. 

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