Butanol-acetone-water mixture

To obtain anthocyanins closer to their natural state, a number of researchers have performed the initial extraction using neutral solvents such as 60% methanol, n-butanol, cold acetone, acetone/methanol/water mixtures, or simply water (Jackman et al., 1987). Others have isolated anthocyanin pigments with mix-... 

In many cases, minced tissue is extracted with a buffer solution and then centrifuged. In some cases, membrane enzymes that are more firmly bovmd to the structural framework of mitochondria require special methods these include drying with acetone, treatment with butanol-water mixtures, extraction of dried mitochondria with various organic solvents, extraction using aqueous solutions of detergents, treatment with chaotropic ions, or exposure to the action of hydrolytic enzymes. 

This Crude product (15.8 g) In water (360 ml) was added to a prehydrogenated suspension of 10% palladium on charcoal (4 g) in water (400 ml), and hydrogenation was continued for 30 minutes. The catalyst was removed and the filtrate was adjusted to pH 7.5 with sodium bicarbonate, then evaporated at low temperature and pressure. The residue was purified by chromatography on a column of cellulose powder, eluting first with butanol/ ethanol/water mixture and then with acetone/isopropanol/water. The main fraction was evaporated at low temperature and pressure to give a 32% yield of the sodium salt of a-carboxybenzylpenicillin as a white powder. The product was estimated by manometric assay with penicillinase to be 58% pure. 

Many papers concerning salt effect on vapor-liquid equilibrium have been published. The systems formed by alcohol-water mixtures saturated with various salts have been the most widely studied, with those based on the ethyl alcohol-water binary being of special interest (1-6,8,10,11). However, other alcohol mixtures have also been studied methanol (10,16,17,20,21,22), 1-propanol (10,12,23,24), 2-propanol (12,23,25,26), butanol (27), phenol (28), and ethylene glycol (29,30). Other binary solvents studied have included acetic acid-water (22), propionic acid-water (31), nitric acid-water (32), acetone-methanol (33), ethanol-benzene (27), pyridine-water (25), and dioxane-water (26). 

A mixture of potassium permanganate and sodium periodate has also been used to cleave double bonds. This procedure, usually referred to as the Lemieux-von Rudloff reaction, can be carried out in several mixed solvent systems such as butanol and water, dioxane and water " or acetone and water. " It has also been claimed that the addition of phase transfer agents improves yields. 

The 2-D TLC was successfully applied to the separation of amino acids as early as the beginning of thin-layer chromatography. Separation efficiency is, by far, best with chloroform-methanol-17% ammonium hydroxide (40 40 20, v/v), n-butanol-glacial acetic acid-water (80 20 20, v/v) in combination with phenol-water (75 25, g/g). A novel 2-D TLC method has been elaborated and found suitable for the chromatographic identification of 52 amino acids. This method is based on three 2-D TLC developments on cellulose (CMN 300 50 p) using the same solvent system 1 for the first dimension and three different systems (11-IV) of suitable properties for the second dimension. System 1 n-butanol-acetone -diethylamine-water (10 10 2 5, v/v) system 11 2-propanol-formic acid-water (40 2 10, v/v) system 111 iec-butanol-methyl ethyl ketone-dicyclohexylamine-water (10 10 2 5, v/v) and system IV phenol-water (75 25, g/g) (h- 7.5 mg Na-cyanide) with 3% ammonia. With this technique, all amino acids can be differentiated and characterized by their fixed positions and also by some color reactions. Moreover, the relative merits of cellulose and silica gel are discussed in relation to separation efficiency, reproducibility, and detection sensitivity. Two-dimensional TLC separation of a performic acid oxidized mixture of 20 protein amino acids plus p-alanine and y-amino-n-butyric acid was performed in the first direction with chloroform-methanol-ammonia (17%) (40 40 20, v/v) and in the second direction with phenol-water (75 25, g/g). Detection was performed via ninhydrin reagent spray. 

Silica in 80-95% dioxane in the presence of HCI, KOH, and different 1 1 salts was studied in [314]. Silica in nonaqueous solvents containing 1 mass% of water in the presence of CsCl was studied in [3155]. Silica in methanol in the presence of KCl was studied in [282]. Quartz in DMSO in the presence of various 1-1 electrolytes was studied in [3156]. Quartz in ethanol in the presence of various 1-1 electrolytes was studied in [3157,3158]. Quartz in DMSO, acetone, and 1-butanol in the presence of NaBr or LiBr was studied in [3151]. Silica in methanol, acetonitrile, and methanol-water mixtures, with or without NaCl was studied in [1853]. Silica in 99.7% acetone in the presence of Nal and BU4NI was studied in [1908]. Titania in different 99% organic-1% water mixtures in the presence of CsCl and other 1-1 salts was studied in [3160]. Anatase in different organic solvents in the presence of CsOH and HCIO4 was studied in [3161].Titania in -alcohols in the presence of different salts was studied in [2037]. LIF, Cal 2, and MgF, in methanol, acetone, and nitroethane in the presence of NaF were studied in [3162]. Agl in ethanol at concentrations of LiNQ, up to 0.01 M was studied in [3163]. ("aSiO, in DMSO at different concentrations of NaBr and CaBr2 was studied in [3144]. Diamond in 96% ethanol in the presence of various 1-1 salts was studied in [3164]. 

We examine separation of the mixtures, concentration space of which contains region of existence of two hquid phases and points of heteroazeotropes. It is considerably easier to separate such mixtures into pure components because one can use for separation the combination of distillation columns and decanters (i.e., heteroazeotropic and heteroextractive complexes). Such complexes are widely used now for separation of binary azeotropic mixtures (e.g., of ethanol and water) and of mixtures that form a tangential azeotrope (e.g., acetic acid and water), adding an entrainer that forms two liquid phases with one or both components of the separated azeotropic mixture. In a number of cases, the initial mixture itself contains a component that forms two liquid phases with one or several components of this mixture. Such a component is an autoentrainer, and it is the easiest to separate the mixture under consideration with the help of heteroazeotropic or heteroextractive complex. The example can be the mixture of acetone, butanol, and water, where butanol is autoentrainer. First, heteroazeotropic distillation of the mixture of ethanol and water with the help of benzene as an entrainer was offered in the work (Young, 1902) in the form of a periodical process and then in the form of a continuous process in the work (Kubierschky, 1915). 

Figure 6.16. Trajectories of heteroazeotropic distiUation (a) distillate from azeocolumn to decanter for separation toluene(l)-ethanol(2)-water(3) mixture (b) distillate from azeocolumn to decanter and a recycle stream of the entrainer from decanter to azeocolumn for separation benzene(l)-isopropanol(2)-water(3) mixture (c) distillate from azeostripping to decanter and a recycle stream of the entrainer from decanter to azeostripping for separation benzene(l)-isopropanol(2)-water(3) mixture (d) distillate from azeocolumn to decanter and a recycle stream of the entrainer from decanter to azeocolumn for separation acetic add(l)-n-butyl acetate (2)-water(3) mixture (e) bottom from azeocolumn to decanter for separation butanol(l)-acetone(2)-water(3) mixture and (f) side product from azeocolumn to decanter for separation butanol(l)-acetone(2)-water(3) mixture. Regions of two liquid phases Regi,i 1,2 are shaded.

Figure 6.16e shows separate usage of a distillation column and a decanter at the bottom product when binary heteroazeotrope is saddle. The example can be separation of the mixture butanol(l)-acetone(2)-water(3) (Pucci, Mihitenho, Asselineau, 1986). Sections trajectories do not differ from trajectories at separation of homogeneous mixture of the same type. Figure 6.16f shows joint usage of the distillation column and decanter for the same mixture. The decanter is installed at the side product. Water is withdrawn from the decanter, and the organic phase is returned into the column. The bottom product of the column is butanol. 

On the base of various heterogeneous azeotropic mixtures, as acetone/toluene/water or 1-propanol/l-butanol/water, the distillation behaviour and its modelling in a packed column is discussed. A detailed description of the experimental equipment and the results is presented in (Repke and Wozny, 2002) and in (Repke, 2002), but a brief overview is listed in (Table 1). 

Polymeric films based on maleic copolymers are used for enteric, ocular, and trans-dermal drug delivery (Table 10.5) because they were proved to be bioadhesive and mucoadhesive [151-153], Loaded films can be prepared by dissolving the drug and the copolymer in anhydride form in organic solvents (acetone-water mixture, isopropanol, 2-butanol) and casting [139,154-159]. Water can also be a solvent for the formation of the films/hydrogels, but in this case the hydrolysis of the maleic copolymer takes place before the contact with the body [151-153,160-162]. 

Standard-grade silica gel is recommended since the trace metals present aid the separation of peonidin and malvidin from cyanidin and delphinidin (Harbome, 1998). Preparative TLC of anthocyanins using 20 X 20 cm chromatoplates with 1-mm layers of a mixture of 2/3 silica gel (adsorbosil-2) and 1 /3 cellulose powder (MN-300, gypsum free) was described by Asen (1965). He employed the following solvent systems to purify milligram quantities of anthocyanins from plant tissues w-butanol/water (1 1), water/HCl/formic acid (8 4 1), 1 % HCl, and acetone/0.5 N HCl (1 3). Table 5.2 lists Rf values of some common anthocyanidins on microcrystalline cellulose (Strack and Wray, 1989). The simultaneous analysis of anthocyanidins and anthocyanins on cellulose layers using a solvent system of concentrated HCl/formic acid/water (24.9 23.7 51.4) has been demonstrated by Andersen and Francis (1985). 

H. is produced by - alkoxylation of alkali-cellulose suspended in solvents, such as acetone, isopropanol or tcrt.butanol 0.8-1.5 moles of alkali per AGU are necessary. To decrease viscosity, the alkali-cellulose is degraded by aging (- cellulose) before reaction or by adding hydrogen peroxide to the alkaline reaction mixture. For better efficiency, the addition of ethylene oxide is carried out in two stages. After the first reaction step, only catalytic amounts of alkali are necessary. Reaction takes place in 1-4 h at 30-80 °C and is stopped by neutralization with hydrochloric or acetic acid. Salts are removed by washing with alcohol/water mixtures. If retarded dissolution in water is desired, the wet product is treated with glyoxal. 

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