Solvent extraction procedures

Miscellaneous Pharmaceutical Processes. Solvent extraction is used for the preparation of many products that ate either isolated from naturally occurring materials or purified during synthesis. Among these are sulfa dmgs, methaqualone [72-44-6] phenobarbital [50-06-6] antihistamines, cortisone [53-06-5] estrogens and other hormones (qv), and reserpine [50-55-5] and alkaloids (qv). Common solvents for these appHcations are chloroform, isoamyl alcohol, diethyl ether, and methylene chloride. Distribution coefficient data for dmg species are important for the design of solvent extraction procedures. These can be determined with a laboratory continuous extraction system (AKUEVE) (244). 

Direct attack by hot 70—80 wt % hydrofluoric acid, sometimes with nitric acid (qv), is effective for processiag columbites and tantalo-columbites. Yields are >90 wt%. This method, used in the first commercial separation of tantalum and niobium, is used commercially as a lead-in to solvent extraction procedures. The method is not suited to direct processiag of pyrochlores because of the large alkaU and alkaline-earth oxide content therein, ie, ca 30 wt %, and the corresponding high consumption of acid. 

The batch and fed-batch procedures are used for most commercial antibiotic fermentations. A typical batch fermentor may hold over 150,000 Hters. When a maximum yield of antibiotic is obtained, the fermentation broth is processed by purification procedures tailored for the specific antibiotic being produced. Nonpolar antibiotics are usually purified by solvent extraction procedures water-soluble compounds are commonly purified by ion-exchange methods. Chromatography procedures can readily provide high quaHty material, but for economic reasons chromatography steps are avoided if possible. 

It has been demonstrated that a solvent-extraction procedure with N-methyl pyrrolidone is capable of producing coal-derived extract pitches with low-ash contents. Moreover, the properties of the pitches can be varied by partial hydrogenation of the coal prior to extraction. The yield of the pitches along with the physical and chemical properties of the cokes and graphites vai in an understandable fashion. 

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... 

Extraction of the analyte or of the interfering element(s) is an obvious method of overcoming the effect of interferences . It is frequently sufficient to perform a simple solvent extraction to remove the major portion of an interfering substance so that, at the concentration at which it then exists in the solution, the interference becomes negligible. If necessary, repeated solvent extraction will reduce the effect of the interference even further and, equally, a quantitative solvent extraction procedure may be carried out so as to isolate the substance to be determined from interfering substances. 

In an attempt to verify (or refute) this assumption, we have determined the thermodynamic parameters (AH, AS) for the complexes formed between Pu(III), Pu(IV), and HSOi in 1 M acid media utilizing cation-exchange and solvent extraction procedures. 

Using a simple solvent extraction procedure to minimize matrix effects, a diclofop-methyl immunoassay was developed for milk, a number of edible plant products, and other matrices. Gas chromatography (GC) and liquid scintillation counting (LSC) of a C-labeled analyte were used as reference methods to compare with enzyme immunoassay (EIA) results. The methods were well correlated, with comparison of EIA... 

Brzelinski and Nelson [214] have described a solvent extraction procedure for the spectrophotometric determination of nanomolar concentrations of silicic acid in seawater. 

Moore [355] used the solvent extraction procedure of Danielson et al. [119] to determine iron in frozen seawater. To a 200 ml aliquot of sample was added lml of a solution containing sodium diethyldithiocarbamate (1% w/v) and ammonium pyrrolidine dithiocarbamate (1 % w/v) at pH to 4. The solution was extracted three times with 5 ml volumes of 1,1,2 trichloro-1,2,2 trifluoroethane, and the organic phase evaporated to dryness in a silica vial and treated with 0.1 ml Ultrex hydrogen peroxide (30%) to initiate the decomposition of organic matter present. After an hour or more, 0.5 ml 0.1 M hydrochloric acid was added and the solution irradiated with a 1000 W Hanovia medium pressure mercury vapour discharge tube at a distance of 4 cm for 18 minutes. The iron in the concentrate was then compared with standards in 0.1 M hydrochloric acid using a Perkin-Elmer Model 403 Spectrophotometer fitted with a Perkin-Elmer graphite furnace (HGA 2200). 

Flynn [72] has described a solvent extraction procedure for the determination of 54manganese in seawater in which the sample with bismuth, cerium, and chromium carriers, is extracted with a heptane solution of bis(2-ethylhexyl) phosphate and the manganese back-extracted with 1M hydrochloric acid. After... 

These samples are prepared by either wet or dry ashing. Many of the metals can be determined in aqueous solution, but for the more trace ones, solvent extraction procedures similar to those described above are resorted to. Similar sample preparation procedures apply to plants. The elements... 

Some methods are available for determining -hexane in urine and tissues. A modified dynamic headspace extraction method for urine, mother s milk, and adipose tissue has been reported (Michael et al. 1980). Volatiles swept from the sample are analyzed by capillary GC/FID. Acceptable recovery was reported for model compounds detection limits were not reported (Michael et al. 1980). A solvent extraction procedure utilizing isotope dilution followed by GC/MS analysis has been reported for tissues (White et al. 1979). Recovery was good (104%) and detection limits are approximately 100 ng/mL (White etal. 1979). 

Lipids can be extracted from biological samples using a variety of organic solvents. A chloroform-methanol solvent is suitable for all lipids but it is possible to extract different classes of lipid selectively on the basis of their solubility in different organic solvents. This may be achieved by the addition of a solvent that will effect either the precipitation or the extraction of the lipids of interest. An example of the former is the precipitation of high concentrations of phospholipids with cold, dry acetone, and of the latter, the extraction of fatty acids into ether or heptane at an acid pH. However, like all solvent extraction procedures these are not entirely specific. 

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). 

Although widely used, solvent extraction procedures have been demonstrated as sensitive to such variables as the content of humic matter and moisture within samples. Supercritical fluid extraction appears to be a more robust procedure. Thermal extraction procedures are sensitive to the size of the soil sample in some cases since the technique can result in cracking higher-molecular-weight... 

The use of Zn-Cr(III) alloy plating has almost replaced the use of Cr(VI) in the electroplating industry due to its excellent corrosion resistance and its lower toxicity. Recently, a solvent extraction procedure for separating and selectively recovering the two metals, zinc and chromium, from electroplating wastewaters has been demonstrated [10]. 

Both round 0 data (before affinity selection) and round 3 data (after three rounds of affinity selection) are shown, where round 0 represents a sampling prior to any ultrafiltration. Round 0 and round 3 samples undergo identical denaturation/solvent extraction procedures. Data were generated... 

Their solubilities in organic solvents were measured to determine their suitability in solvent-extraction procedures. ... 

Solvent extraction procedures provide simple methods for separating the analyte from excipients in formulations. The analytical method applied to the isolated analyte can be for example either gravimetric, volumetric, spectrophotometric or chromatographic. In most cases in the pharmaceutical industry chromatographic methods are preferred. The extraction method adopted is governed by the need to remove excipients and by the properties of the analyte. 

These must be glycerol free. A solvent extraction procedure must be used prior to GC-MS [2, 5, 6]. If the sample is prepared with ion-exchange chromatography, the glycerol will remain in the neutral fraction and not be detected by GC-MS [2, 5]. Hydrochloric acid (5 N), pH paper, sodium sulfate (anhydrous), ethyl acetate (free of contaminants), diethyl ether (anhydrous, peroxide-free, and free of contaminants except 2,6-ditertbutylcresol, which is an antioxidant found in all ether), and malonic acid (26.25 mg/50 ml methanol). 

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