Extraction methods solution

Method 1. Reflux a mixture of pure nicotinic acid (Section V,22), 84 g. (105 ml.) of absolute ethanol and 90 g. (50 ml.) of concentrated sulphuric acid in a flask for 4 hours on a steam bath. Cool the solution and pour it slowly and with stirring on to 200 g. of crushed ice. Add sufficient ammonia solution to render the resulting solution strongly alkaline generally, some ester separates as an oil but most of it remains dissolved in the alkaline solution. Extract the solution with five 25 ml. portions of ether, dry the combined ethereal extracts with anhydrous magnesium sulphate, remove the ether and distil under reduced pressure. The ethyl nicotinate passes over at 117-118°/ 6 mm. the yield is 34 g. The b.p. under normal pressure is 222-224°. 

METHOD 2 [89]--1M MDA or benzedrine and 1M benzaldehyde is dissolved in 95% ethanol (Everclear), stirred, the solvent removed by distillation then the oil vacuum distilled to give 95% yellow oil which is a Schiff base intermediate. 1M of this intermediate, plus 1M iodomethane, is sealed in a pipe bomb that s dumped in boiling water for 5 hours giving an orangy-red heavy oil. The oil is taken up in methanol, 1/8 its volume of dH20 is added and the solution refluxed for 30 minutes. Next, an equal volume of water is added and the whole solution boiled openly until no more odor of benzaldehyde is detected (smells like almond extract). The solution is acidified with acetic acid, washed with ether (discard ether), the MDMA or meth freebase liberated with NaOH and extracted with ether to afford a yield of 90% for meth and 65% for MDMA. That s not a bad conversion but what s with having to use benzaldehyde (a List chemical) Strike wonders if another aldehyde can substitute. 

Analytical and test methods for the characterization of polyethylene and PP are also used for PB, PMP, and polymers of other higher a-olefins. The C-nmr method as well as k and Raman spectroscopic methods are all used to study the chemical stmcture and stereoregularity of polyolefin resins. In industry, polyolefin stereoregularity is usually estimated by the solvent—extraction method similar to that used for isotactic PP. Intrinsic viscosity measurements of dilute solutions in decahn and tetraHn at elevated temperatures can provide the basis for the molecular weight estimation of PB and PMP with the Mark-Houwiok equation, [rj] = KM. The constants K and d for several polyolefins are given in Table 8. 

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),... 

One patent (64) describes an extraction method to remove both trichloropropane and tetrachloropropyl ether from the dichi orohydrin solution by the use of carbon tetrachloride as a solvent. In this way the by-products are removed from the aqueous phase iato an organic phase from which they can be separated by distillation and disposed of ia a safe and proper manner. 

Another way of applying the selective extraction method directly on the initial solution is to produce a solution of low acidity. This can be achieved by using the hydrofluoride method for fluorination and decomposition of raw material. As was discussed in Paragraph 8.2.2, the raw material is fluorinated by molten ammonium hydrofluoride yielding soluble complex fluorides of ammonium and tantalum or niobium. The cake obtained following fluorination is dissolved in water, leading to a solution of low initial acidity that is related for the most part to the partial hydrolysis of complex fluoride compounds. The acidity of the solution is first adjusted to ensure selective tantalum extraction. In the second step, the acidity of the raffinate is increased to provide the necessary conditions for niobium extraction. 

Separation techniques may have to be applied if the given sample contains substances which act as interferences (Section 21.10), or, as explained above, if the concentration of the element to be determined in the test solution is too low to give satisfactory absorbance readings. As already indicated (Section 21.10), the separation methods most commonly used in conjunction with flame spectrophotometric methods are solvent extraction (see Chapter 6) and ion exchange (Chapter 7). When a solvent extraction method is used, it may happen that the element to be determined is extracted into an organic solvent, and as discussed above it may be possible to use this solution directly for the flame photometric measurement. 

The most common method to extract xylan is the alkaline extraction. Several pretreatment methods can be used in association in order to break the covalent bonds that exist between xylan and other carbohydrates during the extraction (Wang Zhang, 2006). A number of articles studied the use of ultrasound on the xylan extraction. Hromadkova and coworkers reported that 36.1% of xylan was extracted from corn cobs with 5% NaOH solution at 60°C for 10 min of ultrasonication in comparison with 31.5% of xylan in the classical extraction. Both extractive methods yielded xylan with immunogenic properties (Hromadkova et al., 1999). 

The concentrations of nitrosamines were reduced to undetectable levels by ultraviolet treatment of the amine solutions and were not increased by addition of 2 ppm NaN02> indicating that the nitrosamines were present originally in the amines and were not formed in the GC injection port. Similar concentrations were found when the amine samples were analyzed using the column extraction method. Direct injection is appropriate for analysis of relatively simple mixtures, if adequate precautions are taken ( ), but can result in significant artifact formation in more complex systems (42). 

Production of the color involves centrifugal separation of the biomass, cell breakage, and extraction. Use of a salt solution rather than water as an extraction medium increases stability of the color during extraction. Methods for partial exclusion of the polysaccharide from the color extract in order to enhance resolubilization of the dried color were developed. These processes include either microfiltration or co-precipitation of the polysaccharide with an added positively charged polysaccha-... 

Sample preparation techniques vary depending on the analyte and the matrix. An advantage of immunoassays is that less sample preparation is often needed prior to analysis. Because the ELISA is conducted in an aqueous system, aqueous samples such as groundwater may be analyzed directly in the immunoassay or following dilution in a buffer solution. For soil, plant material or complex water samples (e.g., sewage effluent), the analyte must be extracted from the matrix. The extraction method must meet performance criteria such as recovery, reproducibility and ruggedness, and ultimately the analyte must be in a solution that is aqueous or in a water-miscible solvent. For chemical analytes such as pesticides, a simple extraction with methanol may be suitable. At the other extreme, multiple extractions, column cleanup and finally solvent exchange may be necessary to extract the analyte into a solution that is free of matrix interference. 

Extraction of lyophilized protein powder by w/o-ME solution (solid-phase extraction method, SPE). 

The most common method of isolation and sample cleanup involves contacting a filtered aqueous solution with an appropriate immiscible organic solvent in a. aboratory separatory funnel of appropriate size. Some specific examples are discussed later. With multicomponent samples a single solvent or solvent mixture is unlikely to extract all components equally causing discrimination. Ihis discrimination may be useful if the solvent discriminates against the extraction of solutes that are not of interest in the analysis. 

Applications The in-vial LSE of additives is used in several laboratories (e.g. GE, DSM Plant Laboratories) but other extraction methods are more popular. Use may be envisaged in particular for specific routine applications in plant services at low cost. Desrosiers [23] has reported that up to 3 g of either ground or thin disk strips may be put completely into solution at 140 °C and an extraction period of 15min. Ashton [111] used... 

One of the attractive features of SFE with CO2 as the extracting fluid is the ability to directly couple the extraction method with subsequent analytical methods (both chromatographic and spectroscopic). Various modes of on-line analyses have been reported, and include continuous monitoring of the total SFE effluent by MS [6,7], SFE-GC [8-11], SFE-HPLC [12,13], SFE-SFC [14,15] and SFE-TLC [16]. However, interfacing of SFE with other techniques is not without problems. The required purity of the CO2 for extraction depends entirely on the analytical technique used. In the off-line mode SFE takes place as a separate and isolated process to chromatography extracted solutes are trapped or collected, often in a suitable solvent for later injection on to chromatographic instrumentation. Off-line SFE is inherently simpler to perform, since only the extraction parameters need to be understood, and several analyses can be performed on a single extract. Off-line SFE still dominates over on-line determinations of additives-an... 

Sze, Y. K. P. Lam, J. K. S. A study of a solvent extraction method for the treatment of spent electrolyte solutions generated in nickel-cadmium (Ni-Cd) battery manufacturing. Environ. Technol. 1999, 20, 943-951. 

M. L. Aleksandrov, L. N. Gall, V. N. Krasnov, V. I. Nikolaev, V. A. Pavlenko and V. A. Shkurov, Ion extraction from solutions at atmospheric pressure a method for mass spectrometric analysis of bioorganic substances, DoklAkadNaukSSSR, 277, 379 383 (1984) (in Russian). 

The potentially tautomeric side-chain thiol systems exist mainly in the thiol form in liquid solution and in the gas phase, as found by IR and NMR spectroscopy and by a study of ionization potentials.126 Upon alkylation using the ion-pair extraction method, only the S-alkylated compounds were obtained. The synthesis, reactions, and properties of some selenides of thiophene, furan, and selenophene have been reviewed.127... 

Cereal proteins when classified by the Osborne sequential extraction method yield four different classes albumins, which are water soluble, globulins, which are soluble in salt solutions, prolamins, which are soluble in alcohol-water mixtures, and glutelins, which are soluble in dilute acid or alkali. Chen and Bushuk added a fifth fraction by dividing the glutelin into two fractions, one soluble in dilute (0.05 m) acetic acid and the other insoluble in this reagent.5... 

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