Distillation-extraction techniques

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),... 

Solid-phase microextraction is an adsorption/desorption technique used to analyze the volatile and non-volatile compounds in both liquid and gaseous samples used as an alternative to the headspace, purge-and-trap, solid-phase extraction, or simultaneous distillation/extraction techniques. Analytes are thermally desorbed and directly introduced into any gas chromatograph or GC/mass spectrometry (MS) system. When coupled to HPLC with the proper interface, the analytes are washed out of the fiber by the mobile phase. 

Initial Extraction Technique Continuous extraction apparatus was employed, including an extractor designed to contain the starting plant materials, a distillation flask to hold the solvent mixture, the flask being equipped with a reflux condenser, a drip device to facilitate the removal of the volatilized mixture from the condenser and to percolate it through the continuous extractor, and a Soxhiet type return. Means for heating the continuous extraction system were provided. 

Distillation, extractive distillation, liquid-liquid extraction and absorption are all techniques used to separate binary and multicomponent mixtures of liquids and vapors. Reference 121 examines approaches to determine optimum process sequences for separating components from a mixture, primarily by distillation. 

The caprolactam obtained must meet die specifications of permanganate number, volatile bases, hazen color, UV transmittance, solidification point, and turbidity in order to be used for repolymerization alone or in combination witii virgin CL.5 Reported CL purification methods include recrystallization, solvent extraction, and fractional distillation. One solvent extraction technique involves membrane solvent extraction. Ion exchange resins have been shown to be effective in the purification of aqueous caprolactam solutions. In one such process,... 

Shen, S. et al.. Comparison of solid-phase microextraction, supercritical fluid extraction, steam distillation, and solvent extraction techniques for analysis of volatile consituents in Fructus amomi, J. AOAC Int., 88, 418, 2005. 

Separations for removing undesirable by-products and impurities, and making suprapure fine chemicals constitute a major fraction of the production costs. There is an enormous variety of methods for product separation and purification and many books on the subject have been published. Here, we deal with the problem in a very general way and we refer the reader to advanced books for details. Conventional techniques for product isolation and purification, such as fractional distillation, extraction, and crystallization, still predominate. Some guidelines for scale-up of these techniques and producing experimental data for scale-up are given in Chapter 5. More information on specific separation and purification techniques applied to particular problems of fine chemicals manufacture the reader can find in Chapter 6. 

The most frequently used methods of analyte isolation and concentration for organic compounds involve distillation, extraction auid adsorption techniques. Some typical applications of these techniques and their attendant -advantages and disadvantages for the analysis of trace organic solutes in water are summarized in Table 8.1 [4,26]. These methods will be elaborated on below and in subsequent sections of this chapter. 

Bierl [28] has described a procedure based on the micro-steam distillation and extraction technique for recovery and determination of low and medium-boiling chlorinated organic compounds. Recoveries of around 90%... 

As documented in Chapter 5, zeolites are very powerful adsorbents used to separate many products from industrial process steams. In many cases, adsorption is the only separation tool when other conventional separation techniques such as distillation, extraction, membranes, crystallization and absorption are not applicable. For example, adsorption is the only process that can separate a mixture of C10-C14 olefins from a mixture of C10-C14 hydrocarbons. It has also been found that in certain processes, adsorption has many technological and economical advantages over conventional processes. This was seen, for example, when the separation of m-xylene from other Cg-aromatics by the HF-BF3 extraction process was replaced by adsorption using the UOP MX Sorbex process. Although zeolite separations have many advantages, there are some disadvantages such as complexity in the separation chemistry and the need to recover and recycle desorbents. 

The aerial parts were leached by soaking 100 g of fresh plants in 100 mL of distilled water. Soil extracts were prepared in a 2 1 proportion. The organic extracts of leaves were obtained with the following solvents hexane, ethyl acetate, chloroform, benzene, acetone, and methanol. The essential oils were obtained by steam distillation and the pure substances with several extraction techniques (11, 12, 13, 14). 

Besides classical headspace analysis, simultaneous distillation-extraction and solvent extraction, new sampling and enrichment developments include solvent-assisted flavour evaporation (SAFE) [3] and sorptive techniques like SPME solid-phase microextraction (SPME) [4,5] and stir-bar sorptive extraction (SBSE) [6], which are treated in a dedicated chapter in this book. This contribution will deal with advanced developments of GC techniques for improvement of separation and identification (classical multidimensional GC, or... 

It is very common to combine methods in obtaining aroma isolates. The simultaneous distillation/extraction method previously described is an example. Another popular combination method initially involves the solvent extraction of volatiles from a food and then high-vacuum distillation of the solvent/aroma extract to provide a fat-free aroma isolate. This technique is broadly used today to provide high-quality aroma extracts for numerous purposes. The apparatus used in solvent removal has been improved upon to reduce analysis time and efficiency the modified method is termed solvent-assisted flavour extraction (SAFE) [16]. 

Aroma compounds are present in minute levels in foods, often at the ppb level ( ig/liter). In order to analyze compounds at these levels, isolation and concentration techniques are needed. However, isolation of aroma compounds from a food matrix, which contains proteins, fats, and carbohydrates, is not always simple. For foods without fat, solvent extraction (unit gu) can be used. In foods containing fat, simultaneous distillation extraction (SDE see Basic Protocol 1) provides an excellent option. Concentration of headspace gases onto volatile traps allows sampling of the headspace in order to obtain sufficient material for identification of more volatile compounds. A separate protocol (see Basic Protocol 2) shows how volatile traps can be used and then desorbed thermally directly onto a GC column. For both protocols, the subsequent separation by GC and identification by appropriate detectors is described in unitgu. 

Of the two techniques described here, simultaneous distillation extraction (SDE) is a more complete volatile extraction procedure that serves to obtain quantitative information on the compounds contained in a food. Volatile trapping is a partial extraction procedure that samples the vol a-tiles present in the headspace above a food, which are those with higher volatili ty. Extended trapping also induces additional volatilization of compounds initially contained in the food. 

Hubert et al. [101] state that accelerated solvent extraction compared to alternatives such as Soxhlet extraction, steam distillation, microwave extraction, ultrasonic extraction and, in some cases, supercritical fluid extraction is an exceptionally effective extraction technique. Hubert et al. [ 101 ] studied the effect of operating variables such as choice of solvent and temperature on the solvent extraction of a range of accelerated persistent organic pollutants in soil, including chlorobenzenes, HCH isomers, DDX, polychlorobiphenyl cogeners and polycyclic aromatic hydrocarbons. Temperatures ofbetween 20 and 180 °C were studied. The optimum extraction conditions use two extraction steps at 80 and 140 °C with static cycles (extraction time 35 minutes) using toluene as a solvent and at a pressure of 15 MPa. 

Heymann, et al (24) have used solid phase extraction techniques for the isolation of pyrazines from wines. In this analysis, it was necessary to first distill the pyrazines from the wine and then pass the distillate through a Sep-Pak C-18 cartridge (Waters Assoc.). To speed the analysis, the distillate was forced through the cartridge at a rate of 30 ml/min. 

Upon employing the more rigorous simultaneous distillation-extraction (SDE) technique (100°C pH 3.7) to isolate the quince fruit volatiles, the resulting aroma composition distinctly differed from that obtained by HVD/SE. After SDE the hydrocarbon 5, the bicyclic alcohol 6 and 3,4-didehydro-(B-ionol (7) were identified as... 

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