Extraction automated solvent

Automation of solvent extraction. Although automatic methods of analysis do not fall within the scope of the present text, it is appropriate to emphasise here that solvent extraction methods offer considerable scope for automation. A fully automated solvent extraction procedure, using APDC, for the determination of... 

Liquid extraction FOR THE SEPARATION and enrichment of organic compounds in aqueous samples has been used successfully. Automated solvent extraction with flow-injection analysis has been reported (I). 

Automated solvent extraction is very efficient and economical (only a fraction of the organic solvent needed for manual procedures is used by the FI A method), and more environmentally acceptable than manual methods because no solvent vapors can escape into the laboratory atmosphere from a closed FI A system. Since very small volumes of solutions are used—less than 1 mL per determination—the hazards associated with the use of inflammable solvents are reduced. It must be borne in mind, however, that certain solvents might attack pump tubing and Perspex or PVC components of the system, and therefore the compatibility of liquids handled with the manifold materials used should always be checked (see Chapter 5 and Section 6.1). 

Solvent-extraction, liquid-liquid systems 161 automation of, 174 backwashing in, 174 batch, 173... 

In the past decade, new sample extraction techniques have been introduced to meet stricter criteria in the areas of food and agriculture, for example, enviromnentally friendly, non-toxic, fast, automated, robust, and cost-efficient techniques. Accelerated solvent extraction (ASE) and pressurized liquid extraction (PEE) are two methods developed for the extraction of chemicals of interest " and provide high yields and efficiency from a wide range of botanical, - animal, and biological samples. ASE and PLE combine solvents at elevated temperatures (40 to 200°C)... 

Solid phase extraction (SPE) is a very simple, rapid and reproducible cleanup technique that is now widely accepted as an alternative to the time-consuming liquid-liquid extractions. Additionally, SPE uses relatively small volumes of solvents, and is easy to automate. It is available in a number of different formats, including cartridges, disks, loose material, well plates or SPME using film-coated capillaries. SPE can be considered as an extraction technique when used for isolation and concentration or a cleanup technique when used to remove co-extractives from solvent extracts. The use of SPE for cleanup is discussed later. 

The pH-metric technique used to determine partition coefficients was first used in the 1950s in solvent extraction of metal complexes [280-282], but it is in pharmaceutical research that it is most widely used thanks to the recent development of a fully automated and computer-controlled apparatus [125,283]. The potentiometric approach has been validated in various solvent systems [284-287], and it has become a relevant and expanding experimental technique to obtain lipophilicity descriptors [257,287-289]. 

In liquid-solid extraction (LSE) the analyte is extracted from the solid by a liquid, which is separated by filtration. Numerous extraction processes, representing various types and levels of energy, have been described steam distillation, simultaneous steam distillation-solvent extraction (SDE), passive hot solvent extraction, forced-flow leaching, (automated) Soxh-let extraction, shake-flask method, mechanically agitated reflux extraction, ultrasound-assisted extraction, y -ray-assisted extraction, microwave-assisted extraction (MAE), microwave-enhanced extraction (Soxwave ), microwave-assisted process (MAP ), gas-phase MAE, enhanced fluidity extraction, hot (subcritical) water extraction, supercritical fluid extraction (SFE), supercritical assisted liquid extraction, pressurised hot water extraction, enhanced solvent extraction (ESE ), solu-tion/precipitation, etc. The most successful systems are described in Sections 3.3.3-3.4.6. Other, less frequently... 

Advantages Low cost No grinding Broad applicability High b.p. solvent contamination of analyte Low investment Simple equipment Simultaneous extractions in series Low investment Simple equipment Rapid Economic solvent use Good reproducibility Low investment Simple equipment Economical Simple equipment Not traumatic Almost solvent free Concentrated analyte Rapid Low temperatures Rapid Automated Simultaneous extraction Low solvent use Rapid User friendly Automated Sequential extractions Not analyst labour intensive... 

The main drawback of this technique is solvent and time-consuming. In the last decade, there have been efforts to develop extraction techniques that allow efficient extraction and reduced solvent volumes in shorter times, incorporating high levels of automation, such as pressurized liquid extraction (PLE) [commonly known as accelerated solvent extraction (ASE)]. 

Automation CL measurements can be performed very rapidly and with minimal human participation if the flow system is carefully designed. Several reagents can be added to the sample if multiple flow lines are used and at predetermined times to fulfill the best condition for maximum CL sensitivity. Introduction of special devices into the flow line, which allow procedures otherwise time-consuming such as solvent extraction or ion exchange, improve substantially the sensitivity and selectivity of the technique. 

Much of the current interest in using analytical-scale SFE systems comes from the need to replace conventional liquid solvent extraction methods with sample preparation methods that are faster, more efficient, have better potential for automation, and also reduce the need for large volumes of potentially hazardous liquid solvents. The need for alternative extraction methods is emphasized by current efforts to reduce the use of methylene chloride as an extraction fluid for environmental sample preparation [158]. The potential for applying SFE to a wide variety of environmental and biological samples for both qualitative and quantitative analyses is widely described in reviews [159-161] and the references therein. Analytical-scale SFE is most often applied to relatively small samples (e.g., several grams or less). 

Even complex procedures can be automated, such as dialysis to clean up dirty samplers, solvent extraction, automatic distillation and on-hne UV digestion. Unhke the earlier AutoAnalyzer systems which use a purely step-wise autosampler, the TRAACS is fitted with a random-access sampler as standard. 

Solvent extraction can be automated in continuous-flow analysis. For both conventional AutoAnalyzer and flow-injection techniques, analytical methods have been devised incorporating a solvent extraction step. In these methods, a peristaltic pump dehvers the hquid streams, and these are mixed in a mixing coil, often filled with glass ballotini the phases are subsequently separated in a simple separator which allows the aqueous and organic phases to stratify. One or both of these phases can then be resampled into the analyser manifold for further reaction and/or measurement. The sample-to-extractant ratio can be varied within the limits normally applying to such operations, but the maximum concentration factor consistent with good operation is normally about 3 1. 

Table 1.2 gives some of the reasons for the LGC setting up its automation team. The primary motivation was economic. LGC was often subject to constraints on staffing in parallel with large increases in analytical commitments. The introduction of cost-effective analyses, using mechanical or automatic instruments, reduces staff involvement and allows well qualified people to be released for the development of new analytical requirements. The analysis of beer samples by multi-channel continuous flow analyser [S, 6, 7] and the introduction of a mechanical solvent extraction and identification system to analyse and measure levels of quinizarin in gas oil, both for duty purposes, were prime examples [8], Both systems involved commercially available components and/or instruments integrated with modules designed and built in-house. 

Speed and improved quahty are also important. In the analysis of quinizarin in gas oil, transfer to the automatic regime immediately improved performance. Manual solvent extraction is a very boring task. An analyst, in an attempt to relieve the monotony, will set up a series of extractions in parallel. However, the sodium salt of the quinizarin is an unstable complex. Inevitably, variable times are taken for the solvent extraction, which leads to variable product development and imprecise results. Automation accurately sets the time for the extraction, removes this area of variability and provides consistent and rehable results. 

Chemical separation techniques can be used to reduce spectral interferences and concentrate the analyte. These techniques include solvent extraction(39) and hydride generation(39, 46, 47). At Imperial College, the hydride generation technique is being used on a daily basis(46) for the analysis of soils, sediments, waters, herbage, and animal tissue. The solvent extraction technique is ideally suited for automated systems where the increased manipulation is carried out automatically, and a labor intensive step and sources of contamination are avoided. 

Some of the newer procedures use the same basic principles as the older extraction methods but provide fast and easy-to-use options and generally consume less organic solvent. For the most part, they have higher initial purchase price than the traditional methods. Examples include supercritical fluid extraction, accelerated solvent extraction, and automated solid-phase extraction and microextraction. Modular systems are now readily available that automate these proce-... 

By analogy to solvent extraction, the column containing the solid adsorbent corresponds to the separatory funnel containing the immiscible organic solvent. The transfer of the solute to the solid adsorbent occurs in an unattended operation requiring no manual effort or additional equipment such as the shakers used in solvent extraction or the distillation apparatus used in some of the automatic extraction devices. This simplicity allows for facile automation either off-line or on-line with the separation and detection procedure (495, 512, 536). 

Extraction of fat by supercritical carbon dioxide was investigated as an important option for minimizing the expanded use of frequently flammable and carcinogenic solvents in food analysis. Unfortunately, the presence of moisture in foods has an adverse effect on the quantitative extraction of fat by supercritical fluid extraction (SEE). Hence, samples have to be lyophilized first. The total fat content of freeze-dried meat and oilseed samples was found to be comparable to values derived from Soxhlet-extracted samples (26). Besides, only small amounts of residual lipids could be recovered by an additional extraction of the SFE-extracted matrix by the Bligh and Dyer solvent extraction procedure. As far as the minor constituents are concerned, it was found that the extraction recovery ranged from 99% for PC to 88% for PA. Hence, Snyder et al. concluded that SFE can be used as a rapid, automated method to obtain total fat, including total phospholipids, from foods (26). 

ASE—also referred to as pressurized fluid extraction (PFE)—offers an order of magnitude of additional reductions in solvent use with faster sample processing time, and with the potential of automated, unattended extraction of multiple samples. Briefly, with ASE a solid sample is enclosed in a cell containing an extraction solvent after the cell has been sealed, the sample is permeated by... 

This chapter covers techniques for the extraction of semivolatile organics from solid matrices. The focus is on commonly used and commercially available techniques, which include Soxhlet extraction, automated Soxhlet extraction, ultrasonic extraction, supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), and microwave-assisted extraction (MAE). The underlying principles, instrumentation, operational procedures, and selected applications of these techniques are described. In a given application, probably all the methods mentioned above will work, so it often boils down to identifying the most suitable one. Consequently, an effort is made to compare these methodologies. 

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