Solvent extraction concentration

A method for tributyltin in sediments consists of extraction with anhydrous acetic acid, hydride generation, cold trapping and end analysis by GC-AAS using a quartz furnace75. Reduction with NaBFLi followed by solvent extraction, concentration and GC-FPD was proposed for simulaneous determination of di- and tributyltin residues in sea water LOD 10 ng/L for 1 L sample, with 87.1-98.4% of Sn recovery76. 

Phospholipid-derived fatty acids are often used to identify bacteria by capillary GC analysis after liquid solvent extraction, concentration steps, and chemical derivatization to their methyl esters. Our initial investigations attempted to extract the intact phospholipids, but no significant recoveries were achieved using pure C02. Even if SFE conditions were developed that could extract intact phospholipids, an additional derivatization step would be required before GC analysis of the fatty acid components. For these reasons, chemical derivatization/SFE was investigated in an effort to eliminate the lengthy conventional liquid solvent extractions as well as to combine (and shorten) the extraction and derivatization steps. The derivatization/SFE procedure was performed on samples of whole bacteria using 0.5 mL of 1.5% TMPA in methanol. The static derivatization step was performed for 10 minutes at 80°C and 400 atm C02, followed by dynamic SFE for 15 minutes at a flow rate of ca. 0.5 mL/min of the pressurized C02. Extracts were collected in ca. 3 mL of methanol and immediately analyzed by capillary GC without any further sample preparation. 

A measured volume of aqueous sample pH adjusted to >11 and then mixed and shaken repeatedly with methylene chloride pyridine being basic partitions into the organic layer while acidic compounds partition into the basic aqueous phase aqueous layer discarded organic solvent extract concentrated and separated on a GC column determined by a mass spectrometer, a NPD or a FID. 

A measured volume of aqueous sample acidified to pH <2 and serially extracted with methylene chloride strychnine being basic partitions into aqueous phase organic layer discarded aqueous phase pH adjusted to >10 and serially extracted with methylene chloride solvent extract concentrated analyzed by GC/MS. 

A measured quantity of solid sample mixed with anhydrous Na2S04 the mixture sonicated or Soxhlett extracted with methylene chloride or chloroform solvent extract concentrated cleanup (if required) by acid-base partitioning analyzed as above by GC/MS using an appropriate column. 

APDC/DDDC into chloroform and back-extraction into 7.5 N HN03). Vertical profiles obtained by both techniques are shown in Figure 4. The profiles for cadmium and zinc show good agreement between the solvent extract and Chelex results, although the Chelex results are somewhat lower than those by solvent extraction concentration. The values for nickel were also lower when the Chelex technique was employed. The mean difference between the two techniques was 65 35 ng l-1. 

In order to achieve the desired sensitivity most environmental analytical techniques employ some form of solvent extract concentration. 

Fig. 4.8, but this is frequently only an approximation. For straight equilibrium and operating lines, equations can be evaluated in a similar manner as for the extraction section, to relate the solvent extract concentration to the solvent concentration at the feed point (or any intermediate point). 

For example If S is the stripping factor ValV,K), a the solvent extract concentration, and n the number of stages. 

Antibiotics. Solvent extraction is an important step in the recovery of many antibiotics (qv) such as penicillin [1406-05-9] streptomycin [57-92-17, novobiocin [303-81-1J, bacitracin [1405-87-4] erythromycin, and the cephalosporins. A good example is in the manufacture of penicillin (242) by a batchwise fermentation. Amyl acetate [628-63-7] or -butyl acetate [123-86-4] is used as the extraction solvent for the filtered fermentation broth. The penicillin is first extracted into the solvent from the broth at pH 2.0 to 2.5 and the extract treated with a buffet solution (pH 6) to obtain a penicillin-rich solution. Then the pH is again lowered and the penicillin is re-extracted into the solvent to yield a pure concentrated solution. Because penicillin degrades rapidly at low pH, it is necessary to perform the initial extraction as rapidly as possible for this reason centrifugal extractors are generally used. 

Spinbath concentration can be adjusted to obtain the desired microstmcture. Low spinbath concentration promotes rapid solvent extraction but this also produces a thick skin on each filament which ultimately reduces the rate of solvent extraction and may lead to the formation of macrovoids. High spinbath concentrations give a denser microstmcture, but solvent extraction is slow and filament fusion can occur. Other spinbath conditions that affect coagulation and microstmcture are dope soHds, spinbath temperature, jet stretch, and immersion time. 

Soybean concentrate production involves the removal of soluble carbohydrates, peptides, phytates, ash, and substances contributing undesirable flavors from defatted flakes after solvent extraction of the oil. Typical concentrate production processes include moist heat treatment to insolubilize proteins, followed by aqueous extraction of soluble constituents aqueous alcohol extraction and dilute aqueous acid extraction at pH 4.5. 

Extraction of hemiceUulose is a complex process that alters or degrades hemiceUulose in some manner (11,138). Alkaline reagents that break hydrogen bonds are the most effective solvents but they de-estetify and initiate -elimination reactions. Polar solvents such as DMSO and dimethylformamide are more specific and are used to extract partiaUy acetylated polymers from milled wood or holoceUulose (11,139). Solvent mixtures of increasing solvent power are employed in a sequential manner (138) and advantage is taken of the different behavior of various alkaUes and alkaline complexes under different experimental conditions of extraction, concentration, and temperature (4,140). Some sequences for these elaborate extraction schemes have been summarized (138,139) and an experimenter should optimize them for the material involved and the desired end product (102). 

Preparation of soil—sediment of water samples for herbicide analysis generally has consisted of solvent extraction of the sample, followed by cleanup of the extract through Uquid—Uquid or column chromatography, and finally, concentration through evaporation (285). This complex but necessary series of procedures is time-consuming and is responsible for the high cost of herbicide analyses. The advent of soUd-phase extraction techniques in which the sample is simultaneously cleaned up and concentrated has condensed these steps and thus gready simplified sample preparation (286). 

The solution leaving the flotation cell, containing about 0.4 g/L iodine, is sent to a kerosene solvent extraction process to recover the dissolved product. After neutralization with soda ash to the initial incoming alkalinity, the solution is returned to the nitrate lixiviation process. The iodine-chaiged kerosene is contacted with an acidic concentrated iodide solution containing SO2, which reduces the iodine to iodide. 

Another characteristic of the solvent extraction system is the high solute concentration in both aqueous and organic phases, which influences greatly the size of the required installation. Concentrations of rare-earth oxides (REO) higher than 100 g/L are often reached in both phases. The process therefore requires only relatively small equipment. 

U02(C02) 3. The pregnant solution is concentrated and purified by ion exchange or solvent extraction, yielding a stripping solution of ca 50 kg/m U Og. Uranium is then precipitated chemically. Pure U Og is obtained by calcination (see Uraniumand URANIUM COMPOUNDS). 

The chain-growth catalyst is prepared by dissolving two moles of nickel chloride per mole of bidentate ligand (BDL) (diphenylphosphinobenzoic acid in 1,4-butanediol). The mixture is pressurized with ethylene to 8.8 MPa (87 atm) at 40°C. Boron hydride, probably in the form of sodium borohydride, is added at a molar ratio of two borohydrides per one atom of nickel. The nickel concentration is 0.001—0.005%. The 1,4-butanediol is used to solvent-extract the nickel catalyst after the reaction. 

Solvent extraction—purification of wet-process phosphoric acid is based on preferential extraction of H PO by an organic solvent vs the cationic impurities present in the acid. Because selectivity of acid over anionic impurities is usually not sufficient, precipitation or evaporation steps are included in the purification process for removal. Cmde wet-process acid is typically concentrated and clarified prior to extraction to remove post-precipitated sludge and improve partition of the acid into the solvent. Concentration also partially eliminates fluoride by evaporation of HF and/or SiF. Chemical precipitation of sulfate (as Ba or Ca salts), fluorosiUcates (as Na salt), and arsenic (as sulfides) may also be used as a prepurification step preceding solvent extraction. 

The purified acid is recovered from the loaded organic stream by contacting with water in another countercurrent extraction step. In place of water, an aqueous alkafl can be used to recover a purified phosphate salt solution. A small portion of the purified acid is typically used in a backwashing operation to contact the loaded organic phase and to improve the purity of the extract phase prior to recovery of the purified acid. Depending on the miscibility of the solvent with the acid, the purified acid and the raffinate may be stripped of residual solvent which is recycled to the extraction loop. The purified acid can be treated for removal of residual organic impurities, stripped of fluoride to low (10 ppm) levels, and concentrated to the desired P2 s Many variations of this basic scheme have been developed to improve the extraction of phosphate and rejection of impurities to the raffinate stream, and numerous patents have been granted on solvent extraction processes. 

The PGM concentrate is attacked with aqua regia to dissolve gold, platinum, and palladium. The more insoluble metals, iridium, rhodium, mthenium, and osmium remain as a residue. Gold is recovered from the aqua regia solution either by reduction to the metallic form with ferrous salts or by solvent-extraction methods. The solution is then treated with ammonium chloride to produce a precipitate of ammonium hexachloroplatinate(IV),... 

Nuclear Waste. NRC defines high level radioactive waste to include (/) irradiated (spent) reactor fuel (2) Hquid waste resulting from the operation of the first cycle solvent extraction system, and the concentrated wastes from subsequent extraction cycles, in a faciHty for reprocessing irradiated reactor fuel and (3) soHds into which such Hquid wastes have been converted. Approximately 23,000 metric tons of spent nuclear fuel has been stored at commercial nuclear reactors as of 1991. This amount is expected to double by the year 2001. 

---