Other impurities

The reports were that water condensed from the vapor phase into 10-100-/im quartz or pyrex capillaries had physical properties distinctly different from those of bulk liquid water. Confirmations came from a variety of laboratories around the world (see the August 1971 issue of Journal of Colloid Interface Science), and it was proposed that a new phase of water had been found many called this water polywater rather than the original Deijaguin term, anomalous water. There were confirming theoretical calculations (see Refs. 121, 122) Eventually, however, it was determined that the micro-amoimts of water that could be isolated from small capillaries was always contaminated by salts and other impurities leached from the walls. The nonexistence of anomalous or poly water as a new, pure phase of water was acknowledged in 1974 by Deijaguin and co-workers [123]. There is a mass of fascinating anecdotal history omitted here for lack of space but told very well by Frank [124]. 

The precautions stated are to avoid uptake of oxygen, nitrogen and other impurities which render the metal brittle the excess magnesium and magnesium chloride can be removed by volatilisation above 1300 K. 

Ether so obtained is anhydrous, and almost entirely free from other impurities. On standing, however, it undergoes slight atmospheric oxidation, with the formation of traces of diethyl peroxide, (CaH jaOa. The formation of this peroxide can be largely checked, however, by storing the distilled ether over fresh sodium wire, preferably in the dark. 

Nitrobenzene. Nitrobenzene, of analytical reagent quality, is satisfactory for most purposes. The technical product may contain dinitrobenzene and other impurities, whilst the recovered solvent may be contaminated with aniline. Most of the impurities may be removed by steam distillation after the addition of dilute sulphuric acid the nitrobenzene in the distillate is separated, dried with calcium chloride and distilled. The pure substance has b.p. 210°/760 mm. and m.p. 5 -7°. 

Also known as nitrolim and lime nitrogen. The fresh product contains approximately 55 per cent, of calcium cyanamide, 20 p>er cent, of lime, 12 per cent, of graphite and small amounts of other impurities. It should be protected from moisture when stored in order to prevent slow polymerisation to dicyano-diamide. 

The first process utilizes a bed of nickel catalyst which has been regenerated with hydrogen to reduce the nickel content to metallic form. The finely divided metal then reacts with impurities and retains them in the bed, probably as nickel oxide in the case of oxygen or as physisorbed compounds for other impurities. Periodically, the bed is regenerated at elevated temperature using hydrogen to restore the metallic content. The nickel process can be used and regenerated indefinitely. 

Cq ), where is the blended impurity concentration of impurity a Cq, the background impurity level and the multiplication constant. Possible sources of background response include instmment noise, sample system outgassing, or interference from other impurity response signals. Proper setup, purging, and operation of the instmment should reduce background levels weU below ippb. 

Acetic acid containing less than 1% water is called glacial. It is hygroscopic and the freezing point is a convenient way to determine purity (7). Water is nearly always present in far greater quantities than any other impurity. Table 1 shows the freezing points for acetic acid-water mixtures. 

Gas chromatography or Hquid chromatography (23) are commonly used to measure impurities such as acetic, dichloroacetic, and trichloroacetic acids. High purity 99+% chloroacetic acid will contain less than 0.5% of either acetic acid or dichloroacetic acid. Other impurities that may be present in small amounts are water and hydrochloric acid. 

The alcoholysis reaction may be carried out either batchwise or continuously by treating the triglyceride with an excess of methanol for 30—60 min in a well-agitated reactor. The reactants are then allowed to settle and the glycerol [56-81-5] is recovered in methanol solution in the lower layer. The sodium methoxide and excess methanol are removed from the methyl ester, which then maybe fed directiy to the hydrogenolysis process. Alternatively, the ester may be distilled to remove unreacted material and other impurities, or fractionated into different cuts. Practionation of either the methyl ester or of the product following hydrogenolysis provides alcohols that have narrow carbon-chain distributions. 

MetaUic ions are precipitated as their hydroxides from aqueous caustic solutions. The reactions of importance in chlor—alkali operations are removal of magnesium as Mg(OH)2 during primary purification and of other impurities for pollution control. Organic acids react with NaOH to form soluble salts. Saponification of esters to form the organic acid salt and an alcohol and internal coupling reactions involve NaOH, as exemplified by reaction with triglycerides to form soap and glycerol,... 

Normally, a slight excess of sulfuric acid is used to bring the reaction to completion. There are, of course, many side reactions involving siHca and other impurity minerals in the rock. Fluorine—silica reactions are especially important as these affect the nature of the calcium sulfate by-product and of fluorine recovery methods. Thermodynamic and kinetic details of the chemistry have been described (34). 

The products manufactured are predominantiy paraffinic, free from sulfur, nitrogen, and other impurities, and have excellent combustion properties. The very high cetane number and smoke point indicate clean-burning hydrocarbon Hquids having reduced harmful exhaust emissions. SMDS has also been proposed to produce chemical intermediates, paraffinic solvents, and extra high viscosity index (XHVI) lubeoils (see Lubrication and lubricants) (44). 

The brine clean-up consists of skimming and settling steps to free the solution from oil, clays, and other impurities. Sulfuric acid is then added until a pH of <2.5 is reached ensuring iodine Hberation by oxidation, precipitation of the soluble barium contained in the brine, and recovery of the remaining iodine. 

Ironmaking refers to those processes which reduce iron oxides to iron. By the nature of the processes, the iron produced usually contains carbon and/or other impurities which are removed in downstream processing. There are three principal categories of ironmaking processes, in order of commercial importance blast furnace, direct reduction, and direct smelting. 

Pemoval of Other Impurities. After softening, the impurities that may stiU remain in the lead are silver, gold, copper, tellurium, platinum metals, and bismuth. Whereas concentrations may be tolerable for some lead appHcations, the market values encourage separation and recovery. The Parkes process is used for removing noble metals and any residual copper, and the KroU-Betterton process for debismuthizing. 

Metals less noble than copper, such as iron, nickel, and lead, dissolve from the anode. The lead precipitates as lead sulfate in the slimes. Other impurities such as arsenic, antimony, and bismuth remain partiy as insoluble compounds in the slimes and partiy as soluble complexes in the electrolyte. Precious metals, such as gold and silver, remain as metals in the anode slimes. The bulk of the slimes consist of particles of copper falling from the anode, and insoluble sulfides, selenides, or teUurides. These slimes are processed further for the recovery of the various constituents. Metals less noble than copper do not deposit but accumulate in solution. This requires periodic purification of the electrolyte to remove nickel sulfate, arsenic, and other impurities. 

Gas—hquid chromatography is used extensively to determine the naphthalene content of mixtures. Naphthalene can be separated easily from thionaphthene, the methyl- and dimethylnaphthalenes, and other aromatics. Analysis of the various other impurities may require the use of high resolution capillary columns. 

The reaction of chlorine gas with a mixture of ore and carbon at 500—1000°C yields volatile chlorides of niobium and other metals. These can be separated by fractional condensation (21—23). This method, used on columbites, is less suited to the chlorination of pyrochlore because of the formation of nonvolatile alkaU and alkaline-earth chlorides which remain in the reaction 2one as a residue. The chlorination of ferroniobium, however, is used commercially. The product mixture of niobium pentachloride, iron chlorides, and chlorides of other impurities is passed through a heated column of sodium chloride pellets at 400°C to remove iron and aluminum by formation of a low melting eutectic compound which drains from the bottom of the column. The niobium pentachloride passes through the column and is selectively condensed the more volatile chlorides pass through the condenser in the off-gas. The niobium pentachloride then can be processed further. 

The dominant commercial form of elemental phosphoms is the a-white aHotrope. a-White phosphoms is often designated simply as because the soHd consists of tetrahedral P molecules. In its pure form, it is a white soHd that forms a clear Hquid when melted. However, the commercial product is generally somewhat yellow, both as a soHd and as a Hquid, owing to the presence of small amounts of a ted phosphoms aHotrope. Commercial white phosphoms may also be slightly gray in color because of incomplete separation of coke dusts and other impurities generated in the manufacturing process. 

Hydrolysis of Dimethyl Terephthalate. Hoechst Celanese and Eormosa Chemical Eibers Corp. produce a polymer-grade terephthahc acid by hydrolysis of high purity dimethyl terephthalate. Hbls-Troisdorf AG hcenses a process with this step (70). Hydrolysis occurs at 260—280°C and 4500—5500 kPa (45—55 atm) in a hydrolysis reactor without catalysis. The overhead methanol and water vapor is separated and the methanol is returned to the dimethyl terephthalate section for reuse. The reactor hquid is crystallized, cycloned, washed, and further cooled. Einahy, the slurry is centrifuged and dried. The product has less than 25 ppm of 4-formylbenzoic acid and very low levels of other impurities. There may be several hundred parts per million of monomethyl terephthalate, which is incompletely hydrolyzed dimethyl terephthalate. 

Also present are other impurities such as benzoic acid and residual catalyst metals. All isophthahc acid made by this hquid-phase oxidation is now purified in a process similar to that used for terephthahc acid, as shown in Figure 4. Lower temperatures are used owing to the greater solubihty of isophthahc acid vs terephthahc acid. 

Chemical fertiliser is the predominant market for langbeinite. Comparatively small but increasing amounts of langbeinite are used by the animal feed ingredient industry (see Feeds and feed additives). Producers who supply this market must take special precautions to be sure that any langbeinite intended as an animal feed ingredient meets all USDA specifications for toxic heavy metals and other impurities. 

Selenium and precious metals can be removed selectively from the chlorination Hquor by reduction with sulfur dioxide. However, conditions of acidity, temperature, and a rate of reduction must be carefliUy controlled to avoid the formation of selenium monochloride, which reacts with elemental selenium already generated to form a tar-like substance. This tar gradually hardens to form an intractable mass which must be chipped from the reactor. Under proper conditions of precipitation, a selenium/precious metals product substantially free of other impurities can be obtained. Selenium can be recovered in a pure state by vacuum distillation, leaving behind a precious metals residue. 

Tellurium and many other impurities remain undissolved. The solution is filtered and cooled to reverse the reaction and to deposit soHd selenium. Oeselenized liquor is recycled to the dissolution step. 

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