Liquid residues

Method 2 (from hydrazobenzene). Prepare a solution of sodium hypobromite by adding 10 g. (3-2 ml.) of bromine dropwise to a cold solution of 6-0 g. of sodium hydroxide in 75 ml. of water immersed in an ice bath. Dissolve 9-5 g. of hydrazobenzene (Section IV,87) in 60 ml. of ether contained in a separatory funnel, and add the cold sodimn hypobromite solution in small portions. Shake for 10 minutes, preferably mechanically. Separate the ether layer, pour it into a 100 ml. distilling flask, and distil off the ether by warming gently on a water bath. Dissolve the warm liquid residue in about 30 ml. of alcohol, transfer to a small beaker, heat to boiling on a water bath, add water dropwise to the hot solution until the azobenzene just commences to separate, render the solution clear again with a few drops of alcohol, and cool in ice water. Filter the orange crystals at the pump, and wash with a little 50 per cent, alcohol. Dry in the air. The yield is 8 g. 

Acidify the aqueous solution (60-76 ml.)= prepared from (a) 6-10 g. of the solid mixture, ( >) from 6-10 g. of the liquid residue (fJ) after distillation from a boiling water bath, or (c) from sufHcient of original aqueous solution to contain 6-10 g. of solute) with 20% E fSOf and distil. 

Distillation may be defined as the separation of the constituents of a liquid mixture by partial vaporization of the mixture, followed by separate recovery of the vapor and liquid residue. Since crude petroleum is the most complex mixture of liquids found in nature, it is not surprising that distillation is one of the most important processes in modem petroleum refining. 

Cokers produce no liquid residue but yield up to 30% coke. Much of the low-sulfur product is used for electrolytic electrodes for smelting of aluminum. Lower-quality coke is burned as fuel im.xcd with coal. 

Aldehyde or Ketone may be separated from the other constituents by shaking the liquid, which should be free from water, with a saturated solution of sodium bisulphite, and decanting or filtering the liquid residue. If the liquid is soluble in water, like ethyl alcohol, it may piecipitate the bisulphite of sodium. This is prevented by adding a little ether befoie introducing the bisulphite into the liquid. 

One gram of 6,7-dihydro-5H-dibenz[c,e] azepine hydrochloride was dissolved in water, made alkaline with concentrated ammonia, and the resultant base extracted twice with benzene. The benzene layers were combined, dried with anhydrous potassium carbonate, and mixed with 0.261 g of allyl bromide at 25°-30°C. The reaction solution became turbid within a few minutes and showed a considerable crystalline deposit after standing 3 A days. The mixture was warmed VA hours on the steam bath in a loosely-stoppered flask, then cooled and filtered. The filtrate was washed twice with water and the benzene layer evaporated at diminished pressure. The liquid residue was dissolved in alcohol, shaken with charcoal and filtered. Addition to the filtrate of 0.3 gram of 85% phosphoric acid in alcohol gave a clear solution which, when seeded and rubbed, yielded 6-allyl-6,7-dihydro-5H-dlbenz[c,e] azepine phosphate, MP about 211°-215°C with decomposition. 

Ethyl-lsonicotinic Nitrile The 11 grams of the amide just obtained are treated with 15 grams of phosphorus anhydride at 160° to 180°C in a vacuum. 6 grams of a liquid residue are obtained. 

The reaction mixture is then warmed on the steam bath for an additional two hours (90°C to 95°C). The excess hydrazine hydrate is removed in vacuo. The residue of viscous 1-hy-drazlno-3-morpholinyl-2-propanol Is not distilled, but is mixed with 10.16 g (0.0B6 mol) diethyl carbonate and a solution of 0.3 g sodium metal in 15 ml methyl alcohol. The mixture is refluxed about 2 hours under a 15 cm Widmer column, the alcohol being removed leaving a thick, green liquid residue, which is cooled and the precipitate which forms is removed by filtration and washed well with ether. Yield B2%, MP114°C to 116°C. Recrystallization from isopropanol gives purified 3-amino-5-(N-morpholinyl)-methyl-2-oxazolidone, MP 120°C as the intermediate. 

The ether filtrate and washings were evaporated at room temperature under reduced pressure to give a clear liquid residue (801 grams). This residue was distilled under high vacuum to give trichloroethyl phosphorodichloridate (556 grams, 62.4% of theory), boiling point 75°C/0.8 mm. 

Next the xylene was distilled away, the liquid residue dissolved in about 80 ml carbon tetrachloride and the hydrochloride precipitated through introduction of hydrochloric acid gas. The hydrochloride was dissolved in about 100 ml acetone and the solvent subsequently distilled away, whereby excess hydrochloric acid passed over with it. This operation was repeated until no excess acid was present. 

It must be noted that impurities in the ionic liquids can have a profound impact on the potential limits and the corresponding electrochemical window. During the synthesis of many of the non-haloaluminate ionic liquids, residual halide and water may remain in the final product [13]. Halide ions (Cl , Br , I ) are more easily oxidized than the fluorine-containing anions used in most non-haloaluminate ionic liquids. Consequently, the observed anodic potential limit can be appreciably reduced if significant concentrations of halide ions are present. Contamination of an ionic liquid with significant amounts of water can affect both the anodic and the cathodic potential limits, as water can be both reduced and oxidized in the potential limits of many ionic liquids. Recent work by Schroder et al. demonstrated considerable reduction in both the anodic and cathodic limits of several ionic liquids upon the addition of 3 % water (by weight) [14]. For example, the electrochemical window of dry [BMIM][BF4] was found to be 4.10 V, while that for the ionic liquid with 3 % water by weight was reduced to 1.95 V. In addition to its electrochemistry, water can react with the ionic liquid components (especially anions) to produce products... 

After 8 h of reaction, the reactor was allowed to cool. A two-layer liquid formed. The top layer was found to contain mostly polypropylene ether triols with about 20% by weight diethylene glycol and 5% by weight toluene diamines. The top layer was purified by vacuum distillation at 2 mm Hg and 200° C to produce 320 g of a light brown liquid residue. This residue (polyols) was used as a replacement for 5% by weight of the Pluracol 535 polyol in the formulation of a flexible polyurethane foam. A flexible foam which had good resiliency and a density of 2.2 Ib/ft3 was obtained. At higher replacement levels, lesser quality foams were obtained. 

ASTM E 1385-90, Standard Practice for Separation and Concentration of Flammable or Combustible Liquid Residues from Fire Debris Samples by Steam Distillation, American Society for Testing and Materials, Philadelphia, PA (1991). 

Table VII shows that the SCT-SRC plus upgrading yields significantly less gas and more liquid (residual material included) than the other processes. The hydrogen consumption in the two-step SCT process is higher than for the SRC-I process however, it is still lower than for the SRC-II process and significantly lower than for the H-Coal Syncrude operation.

POLYURETHANE FOAM SHEETS OR BLOCKS. These are required to resist ignition source 5 (17 gram wood crib) of BS5852 Part 2 except that the flames may penetrate the full depth of the specimen and that the mass loss (due to burning and liquid residues falling from the test rig) shall not exceed 60 grams. 

The carbon disulfide is decanted, and 200-300 ml. of water is added to the contents of the flask. Initially the mixture reacts slowly, but after some time the reaction becomes so vigorous that it is necessary to pour off the water (Notes 1 and 2). The addition of water, followed by its removal when the reaction becomes very vigorous, is repeated until decomposition is complete. The combined aqueous solutions are extracted several times with chloroform, and the combined extracts are dried over anhydrous sodium sulfate. Distillation of the solvent gives a dark brown liquid residue which is distilled under reduced pressure to give 310.3 g. (89%) of the thioamide as a yellow liquid, b.p. 133-135° (12 mm.) (Note 3). 

B. a-Ketoglutaric acid. A mixture of 225 g. (0.82 mole) of triethyl oxalylsuccinate, 330 ml. of 12N hydrochloric acid, and 660 ml. of water is heated under reflux for 4 hours, and the mixture is distilled to dryness under reduced pressure at a bath temperature of 60-70° (Note 4). The liquid residue, which solidifies readily on standing, is warmed with 200 ml. of nitroethane on a steam bath until it is in solution. The warm solution is filtered, the funnel is washed with 40 ml. of nitroethane, and the filtrate is stirred at 0-10° for 5 hours. a-Ketoglutaric acid is separated by filtration and dried at 90° under reduced pressure for 4 hours. It is obtained as a tan solid weight 88-99 g. (73-83%) m.p. 103-110° (Note 5). 

Standard Practice for Separation and Concentration of Ignitable Liquid Residues in Extracts from Samples of Fire Debris by Gas Chromatography, ASTM E138701, ASTM, West Conshohocken, PA, 2001. 

Each of the above liquid residues was tritrated against standard sodium hydroxide, using phenolphthalein as indicator. Identical titer values were obtained the same titer value was also given by the original solid residue of unreacted TBTA (0-1). Such an observation of identical titer Values should be expected if the conversion of TBTA, by reaction with sodium chloride, is solj.ly to TBTCl. However, any side reaction leading to TBT hydroxide or TBTO will result in lower titer values since these tin compounds, unlike TBTA or TBTCl cannot be titrated like weak acids. Clearly, the side reactions are not noticeable in these experiments. Hydrolysis is not competitive under the conditions of this study, probably because chloride concentration never drops below 10-1 whereas hydroxide concentration is always below 10 s. (It was noticed that the pH of the aqueous layer in each case had risen from 6.5 to 9.0.)... 

Phenylazide and 3-methyl-1-butene were dissolved in n-hexane and stirred for 20 days in the dark. Then, unreacted phenylazide and 3-methyl-1-butene were removed by distillation. A liquid residue with a higher boiling point was obtained. The electronic spectrum of the residue differs from both components. It gives absorption peaks at 287nm and 303nm as is shown in Figure 1. 

Characteristics of solid and liquid residuals in relation to land disposal restrictions requirements using the toxic constituent leaching procedure and analysis of the underlying hazardous constituents such that implementation of proper disposal options can be ensured. 

B. A -Butenolide. In a 500-ml. three-necked flask fitted with a mechanical stirrer, a reflux condenser, and a 250-ml. dropping funnel containing a solution of 61 g. (84.5 ml., 0.6 mole) of triethylamine in 70 ml. of dry diethyl ether, a solution of 83 g. (0.5 mole) of a-bromo-Y-butyrolactone and 200 ml. of dry diethyl ether is heated to reflux, with stirring. The amine solution is added, slowly, during 5 hours and the stirring under reflux continued for an additional 24 hours. The brown precipitate (40 g.) is removed by filtration. Most of the solvent is removed from the filtrate by evaporation, and the additional precipitate (8 g.) is removed. This precipitate is predominantly triethylamine hydrobromide. The liquid residue is distilled under reduced pressure and the -butenolide is collected at 107-109° (24 mm.) ... 

The suitability of ionic liquids (e.g., [EMIM]BF4, [BMIMjPFg, or [OMIM]Tf2N) for free-radical polymerization was explored 249). The homopolymerization of 1-vinyl-2-pyrrolidinone in [BMIMJPFg or that of 4-vinylpyridine in [OMIM]Tf2N resulted in polymers with Mw of 162 500 and 71 500 g/mol, respectively. However, detectable ionic liquid residues were retained in the isolated polymers, even after repeated precipitations from methanol, which is known to dissolve the ionic liquid. The residue may limit the usefulness of ionic liquids as the media for free-radical polymerizations. 

Benzene was discovered in 1825 by Michael Faraday who identified it from a liquid residue of heated whale oil. Faraday called the compound bicarburet of hydrogen and its name was later changed to benzin by Eilhardt Mitscherlich (1794—1863) who isolated the compound from benzoin. Benzene s formula indicates it is highly unsaturated. This would suggest benzene... 

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