Residue additives antimony

Liquation. Antimony sulfide is readily but inefficiendy separated from the gangue of comparatively rich sulfide ore by heating the gangue to 550—600°C in perforated pots placed in a brick furnace. The molten sulfide is collected in lower containers. A more efficient method uses a reverberatory furnace and continuous liquation however, a reducing atmosphere must be provided to prevent oxidation and loss by volatilization. The residue, containing 12—30% antimony, is usually treated by the volatilization process to recover additional antimony. The liquated product, called cmde or needle antimony, is sold as such for applications requiring antimony sulfide, or is converted to metallic antimony by iron precipitation or careful roasting to the oxide followed by reduction in a reverberatory furnace. 

Conditions that favor dezincification include stagnant solutions, especially acidic ones, high temperatures, and porous scale formation (2). Additions of small amounts of arsenic, antimony, or phosphoms can increase the resistance to dezincification. These elements are, however, not entirely effective in preventing the dezincification of the two-phase (cc—P) brasses because dezincification of the P-phase is not prevented (31). Another area of corrosion concern involves appHed or residual stresses from fabrication that can lead to EIC of brasses in the form of stress-corrosion cracking. 

Dezincification Dezincification is corrosion of a brass alloy containing zinc in which the principal product of corrosion is metallic copper. This may occur as plugs rilling pits (plug type) or as continuous layers surrounding an unattacked core of brass (general type). The mechanism may involve overall corrosion of the alloy followed by redeposition of the copper from the corrosion products or selective corrosion of zinc or a high-zinc phase to leave copper residue. This form of corrosion is commonly encountered in brasses that contain more than 15 percent zinc and can be either eliminated or reduced by the addition ox small amounts of arsenic, antimony, or ph osphorus to the alloy. 

Another approach used to reduce the harmful effects of heavy metals in petroleum residues is metal passivation. In this process an oil-soluble treating agent containing antimony is used that deposits on the catalyst surface in competition with contaminant metals, thus reducing the catalytic activity of these metals in promoting coke and gas formation. Metal passivation is especially important in fluid catalytic cracking (FCC) processes. Additives that improve FCC processes were found to increase catalyst life and improve the yield and quality of products. ... 

The bomb contents are digested with concentrated hydrochloric acid, and material still undissolved is then digested with potassium hydroxide and hydrogen peroxide. A crude separation is made by a sulfide precipitation from the combined digestion solutions. The sulfides are dissolved in aqua regia, the solution is evaporated, and antimony in the residue is reduced to antimony (III) with hydroxylamine hydrochloride. The sample, in ammonium thiocyanate-hydrochloric acid medium, is loaded onto a Dowex 2 column (SCN" form). Arsenic and other impurities are eluted with aliquots of more dilute ammonium thiocyanate-hydrochloric acid solutions. Antimony is eluated with sulfuric acid and fixed in solution by addition of hydrochloric acid. The activity of the solution caused by the 0.56 MeV y-ray of 2.8-day 122Sb is counted. 

The NAA method for the determination of firearm discharge residue has been generally accepted, but applications have been limited to just a few laboratories. In the process of establishing NAA capability for the State of Illinois crime laboratories we re-examined the standard techniques (10). In the course of our work it became clear that post-irradiation is the cause of several constraints which have discouraged a more widespread use of NAA. The inherent time limitation due to the 87 min. half-life of 139Ba necessitates fast manipulations of radioactive solutions which in turn requires an experienced radiochemist. In addition to an ever present danger of overexposure and contamination, typically only a dozen samples can be irradiated per batch, which makes the method quite expensive. The developed statistical bivariate-normal analysis (11) is convenient for routine applications. With this in mind, a method was developed which a) eliminates post-irradiation radiochemistry and thus maximizes time for analysis b) accommodates over 130 samples per irradiation capsule (rabbit) c) does not require a collection of occupational handblanks and d) utilizes a simplified statistical concept based on natural antimony and barium levels on hands for the interpretation of data. The detailed procedure will be published elsewhere (15). 

A representative sample of the gunshot residue is obtained by swabbing the thumb, web and forefinger with a cotton swab moistened with 1M nitric acid. The barium and antimony is leached from the cotton tip by soaking it in 1 or 2 ml of 5% (v/v) nitric acid. Instrumentation Laboratory [30] recommend the neutralisation of the solution by the addition of 0.2 ml concentrated ammonium hydroxide solution. 

Preparation.—The main source of rubidium compounds is the residual mother-liquor obtained in the extraction of potassium chloride from carnallite. The solution contains rubidium-carnallite, RbCl,MgCI2, a substance transformed by addition of aluminium sulphate into rubidium-alum, RbAl(S04)8,12H20. Separation from the potassium and caesium salts also present is effected by fractional crystallization of the alum,8 of the chloroplatinate 8 Rb2PtCl8, of rubidium-iron-alum,4 and of the double chloride with stannous chloride5 or with antimony trichloride.6... 

Wet Tests.— When hydrogen sulphide is passed through an acidified solution containing molybdenum, the trisulphide is thrown dowm. The precipitate dissolves in ammonium sulphide, and it is therefore in ordinary analysis separated with the Group IIb metals, namely, arsenic, antimony, tin, gold, and platinum. The last four metals may be precipitated by addition of metallic zinc, the arsenic expelled by evaporation, and, after taking to dryness with nitric acid, the molybdenum may be extracted from the residue with ammonia. The trisulphide may be reprecipitated directly by the addition of nitric acid to the solution in ammonium sulphide. A soluble sulphide added to a solution of ammonium molybdate gives a blue colour. 

Uranium minerals may be obtained in solution, in a suitable condition for estimation, by the following process. The ore is dissolved in aqua regia, or, if necessary, fused with alkali bisulphate and extracted mth hot hydrochloric acid. After evaporation to drjmess, the residue is taken up with dilute hydrochloric acid, and the solution saturated with hydrogeir sulphide in order to remove any copper, lead, bismuth, arsenic, antimony, or any other metal yielding an insoluble sulphide. The filtrate is concentrated and treated with ammonium carbonate, which precipitates the carbonates of the alkaline earths, iron, and most of the rare earths. The filtrate is neutralised by hydrochloric acid, evaporated to dryness, and the residue ignited to drive off ammonium salts, and then redissolved in dilute acid. The remaining rare earths, and particularly thorium, are next precipitated by the addition of oxalic acid. The filtrate, which contains the uranium in the uranyl condition, may now be precipitated by any of the methods described above. 

An additional small amount of the product may be obtained by boiling the antimony residues with a solution of triethylamine (20 mL) in 200 mL of 40-60° petroleum ether for about 1 hour. The product is then isolated as described above, giving a total yield of 9.2 g (78%). 

Summary of the Method. The sample is digested with concentrated sulfuric acid until most of the sulfuric acid is removed and a carbonaceous residue remains. The sample is then placed in a muffle furnace to destroy the carbonaceous material. Hydrochloric acid and hydroxyl-amine hydrochloride are added to dissolve the inorganic residue and reduce antimony(V) and antimony(IV) to antimony (III). Tartaric acid is then added to complex antimony (III), and the solution is evaporated to a small volume. The antimony content of this solution is determined by heated vaporization atomic absorption using the method of standard additions. 

Yellow Pigment that can be Vitrified.—This is produced by combining the oxide of lead with that of antimony or with the antimonate of potash, obtained by heating a mixture of 2 parts of metallic antimony and 5 parts of nitre in a crucible to red heat. The residue is washed with cold water. This, with the addition of various proportions of oxides of zinc and iron and sometimes tin, is mixed... 

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