Inorganic residues

Ash is the inorganic residue that remains after the coal has been burned under specified conditions, and it is composed largely of compounds of sihcon, aluminum, iron, and calcium, and minor amounts of compounds of magnesium, sodium, potassium, phosphorous, sulfur, and titanium. Ash may vaiy considerably from the original mineral matter, which is largely kaolinite, iUite, montmoriUonite, quartz, pyrites, and gypsum. 

Organic polymer materials may be analyzed by ashing at relatively high temperatures. This involves oxidation of the carbon containing matrix, leaving an inorganic residue that is taken up in acid. An alternadve in some cases is to dissolve the polymer in solvent and analyze the nonaqueous solution direcdy. Nonaqueous media will be discussed in a later secdon. 

Ash The nonvolatile inorganic residue left when a fuel is fully combusted. 

Reduction of 6p, 9-Oxidoprogesterone to 9-Hydroxyprogesterone. Zinc powder Note 2) (4. g) is added in small portions to a solution of 2 g of 6)5,19-oxidoprogesterone in 40 ml glacial acetic acid Note i). The mixture is stirred for 40 min, then an additional 4 g zinc is added and stirring is continued for another 40 min at 30°. The cooled solution is filtered, the inorganic residue washed with methanol and the filtrate evaporated under reduced pressure. The resultant crude product is dissolved in 60 ml of chloroform and filtered. Concentrated hydrochloric acid (0.6 ml) is added and the solution stirred for 10 min at 25°. The reaction mixture is diluted with ether, washed successively with water, sodium bicarbonate solution and again with water, dried and evaporated under reduced pressure. The... 

The extensive industrial and commercial utilization of water-soluble polymers (polyelectrolytes) in water treatment has been developed based on the charge along the polymer chains and the resultant water solubility. The use of water-soluble polymers in water treatment has been investigated by several authors [5-26] in the recovery of metals radioactive isotopes, heavy metals, and harmful inorganic residues. This allows recycling water in the industrial processes and so greatly saves... 

Acetyl-5-deoxy-l,2-0-isopropylidene-[3-iJ - threo - pent - 4 - enofura-nose (34). (1) From 3-0-acetyl-5-deoxy-5-iodo-1,2-0-isopropylidene- -d-xylofuranose (31). Anhydrous silver fluoride (7.5 grams) was added to a solution of 7.2 grams 26 in dry pyridine (50 ml.), and the mixture shaken at room temperature for 24 hours. The black reaction mixture was diluted with ether (50 ml.), and the supernatant liquid was decanted from the dark, inorganic residue. The residue was further extracted with ether (3 X 50 ml.) and the pyridine-ether solution partially decolorized... 

Morris [814] separated microgram amounts of vanadium, chromium, manganese, iron, cobalt, nickel, copper, and zinc from 800 ml of seawater by precipitation with ammonium tetramethylenedithiocarbamate, and extraction of the chelates at pH 2.5 with methylisobutyl ketone. Solvent was removed from the extract, the residue was dissolved in 25% nitric acid, and the inorganic residue was dispersed in powdered cellulose. The mixture was pressed into a pellet for X-ray fluorescence measurements. The detection limit was 0.14 pig or better when a 10 min counting period was used. 

Copeland A process for oxidizing organic wastes in a fluidized bed of inert particles. The wastes may be solid, liquid, or gaseous, and the oxidant is air. Inorganic residues are collected as granular solids and the heat generated is normally utilized. Developed and marketed by Copeland Systems, Oak Brook, IL, United States, and used in a wide variety of industries. 

The ash values usually represent the inorganic residue present in official herbal drugs and pharmaceutical substances. These values are categorized into four heads, namely ... 

Inorganic residue is rinsed with diethyl ether. The combined ethereal extracts are added to the filtered solution and the mixture is concentrated to ca. 10 mL by evaporation of the solvent under reduced pressure. The residue is treated with a saturated solution of potassium chloride (KCI) (50 mL), extracted with dichloromethane (3 x 50 mL), and the combined extracts are dried over anhydrous sodium sulfate (Note 21). Removal of volatile material under reduced pressure gives an oil that is flash Chromatographed (silica, diethyl ether - petroleum ether 1 1) to afford 1.77 g (62%) of 2-0-benzyl-3,4-isopropylidene-D-erythrose (Note 22). 

A convenient method is the spectrometric determination of Li in aqueous solution by atomic absorption spectrometry (AAS), using an acetylene flame—the most common technique for this analyte. The instrument has an emission lamp containing Li, and one of the spectral lines of the emission spectrum is chosen, according to the concentration of the sample, as shown in Table 2. The solution is fed by a nebuhzer into the flame and the absorption caused by the Li atoms in the sample is recorded and converted to a concentration aided by a calibration standard. Possible interference can be expected from alkali metal atoms, for example, airborne trace impurities, that ionize in the flame. These effects are canceled by adding 2000 mg of K per hter of sample matrix. The method covers a wide range of concentrations, from trace analysis at about 20 xg L to brines at about 32 g L as summarized in Table 2. Organic samples have to be mineralized and the inorganic residue dissolved in water. The AAS method for determination of Li in biomedical applications has been reviewed . 

Inorganic residues present in water can be simply classified in terms of the anions such as phosphates, sulfates, nitrates, chlorides, etc. and cations such as transition metals and alkaline and alkaline earths. As the methodology for removal of these species tends to be somewhat specific and reported studies tend to tackle these on an individual basis, the following sections look at these on a species by species basis. However, it is clear that remediation technologies must involve integration of the different approaches used to treat the individual contaminants. 

The excess thionyl chloride is removed by distillation under reduced pressure (15-20 mm.) with the bath temperature below 50°, and the last traces are eliminated by one or two evaporations under reduced pressure after the addition of 50-ml. portions of anhydrous ether (Note 4). The residue consists of a viscous yellow oil containing a suspension of white granular inorganic solid. The crude sulfinyl chloride is readily dissolved by three successive treatments with portions of anhydrous ether (50, 30, and 30 ml., respectively) which are decanted without difficulty from most of the inorganic residue (Note 5). Removal of the solvent by distillation at reduced pressure leaves the sulfinyl chloride as a clear, pale, straw-yellow oil. The yield is 30-32 g. (86-92%) (Note 6). Distillation at reduced pressure (Note 5) yields -toluenesulfinyl chloride as a deep yellow mobile oil, b.p. 113—115°/3.5 mm. or 99-102°/0.5 mm, (Note 7). The yield of redistilled material is 23-26 g. (66-74%). A small quantity (2-3 g.) of a dark tarry residue remains in the distilling flask. 

A solution of sucrose (34.2 g, 0.1 mol) in dry DMF (400 mL) containing molecular sieve pellets (Vis in., type 3 A) was stirred with 2-methoxypropene (12.1 mL, 0.13 mol) in the presence of dry p-toluenesulfonic add (25 mg) for 40 min at 70°C, cooled to room temperature, and made neutral with anhydrous sodium carbonate. The inorganic residue wss filtered off and the filtrate evaporated to a syrup. Elution of the syrup from a column of silica gel with 1 1 ethyl acetate/acetone afforded the diacetal 2, l- 4,6-di-0-isopropylidene-sncn>8e 35 as a syrup 3 g (7%) [a]D +25.5° (c 1, methanol). Further elution gave the major product 4,6-O-isopropylidene-sucrose 34 yield 23 g (60%) white powder [a]D +45.4° (c 1.0, methanol).. 

To dried resins 19 and 21 (0.1 g resin, approximately 0.04 mmol with respect to the loading of the phenol) are added Pd(OAc)2 (8.0 mg), 1,3-bis (diphenyl-phosphino)propane (dppp, 17.0 mg), DMF (1.4 ml), and a mixture of HC02H (0.2 ml) and TEA (0.8 ml). The mixture is shaken at 85° for 2 h, and then the resin is filtered and washed several times with diethyl ether. The combined organic phase is washed with aqueous sodium carbonate solution then water and evaporated to dryness. The residue obtained is dissolved in diethyl ether and eluted through a short column of alumina to remove any remaining inorganic residues. The crude products are purified by preparative TLC (or other suitable methods) to give the desired products 20 and 22 in >95% purity. 

The entire inventory of munitions at the PCD contains mustard agent. Most projectiles contain agent HD, which is distilled P,P -dichloroethyl sulfide. Some contain HT, a 60 40 eutectic mixture of HD and bis[2-(2-chloroethylthio)-ethyl] ether. All munitions may contain manufacturing byproducts or impurities, degradation products, and inorganic residues. 

Detectable quantities of organic and inorganic residues were recovered from the laboratory coats. The amounts of NG, DPA, and EC detected were well above the detection limits of the systems. A smaller number of inorganic FDR particles were recovered from the laboratory coats compared to the garments doped with six shots. 

The ester decomposes via dehydration resulting in the formation of a carbon-inorganic residue. 

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