Antimony impurity

The reagents required are 96% acetic acid, 30% HCl, 65% HNO3, 96% H2SO4, KI, NH2OH, NaOH, silicone antifoam emulsion, and Na2EDTA. All chemicals should be checked for antimony impurities before use. Antimony is an element that is only occasionally included in purity specifications, e.g., Sb standard, high-purity water, helium (99.999%). 

Jarnstrom (1982) reported that in the first operating cycles of the VVER plants Loviisa 1 and 2 the radionuclides Sb, Sb and "° "Ag were chiefly responsible for the radiation dose rates at the primary circuit. The most important sources for antimony were identified to be the ammonia solutions added, which contained antimony impurities in the range of 10 to 50pg/kg for silver the main source was KOH used for alkalizing the coolant which contained silver impurities in the range of 5 to lOmg/kg. Both impurity elements, as well as their radioisotopes, were removed with a low efficiency from the primary coolant by the action of the purification system. In the course of plant shutdown, a marked increase in the concentrations of these radionuclides in the primary coolant was observed, which was counteracted by a change in the cooldown procedure the purification system was... 

As appears from the Ge(Li) r-spectrum given in Fig. VII-11, no peaks from radionuclides produced from copper appear in the spectrum of the final leadchlorofluoride precipitate. Besides the annihilation peak, there are only the 559 keV and 657 keV Br peaks and the keV peak. These radionuclides arise from arsenic, selenium and antimony impurities in the copper matrix. Only Sr ( 2 ) contributes to the annihilation... 

Crude lead contains traces of a number of metals. The desilvering of lead is considered later under silver (Chapter 14). Other metallic impurities are removed by remelting under controlled conditions when arsenic and antimony form a scum of lead(II) arsenate and antimonate on the surface while copper forms an infusible alloy which also takes up any sulphur, and also appears on the surface. The removal of bismuth, a valuable by-product, from lead is accomplished by making the crude lead the anode in an electrolytic bath consisting of a solution of lead in fluorosilicic acid. Gelatin is added so that a smooth coherent deposit of lead is obtained on the pure lead cathode when the current is passed. The impurities here (i.e. all other metals) form a sludge in the electrolytic bath and are not deposited on the cathode. 

The lead buUion, ready to be shipped to the refinery, contains in solution impurities such as silver, gold, copper, antimony, arsenic, bismuth, nickel, 2inc, cadmium, tin, tellurium, and platinum metals. 

The pyrometaHurgical processes, ie, furnace-kettle refining, are based on (/) the higher oxidation potentials of the impurities such as antimony, arsenic, and tin, ia comparison to that of lead and (2) the formation of iasoluble iatermetaUic compounds by reaction of metallic reagents such as 2iac with the impurities, gold, silver and copper, and calcium and magnesium with bismuth (Fig. 12). 

Removal by Oxidation. The oxidizing process used to remove antimony, arsenic, and tin has been termed softening because lowering these impurities results in a readily detectable softening of the lead. 

The niter and fresh caustic soda, required to maintain the fluidity of the salt bath in the reactor chamber, are added gradually. When the color of the saturated salts turns from a dark gray to white, the impurity metals are at their highest state of oxidation, and the lead content of the spent salts is very low. In a modification, the arsenic and tin are selectively removed as sodium arsenate and sodium stannate, followed by the removal of antimony as sodium antimonate. 

The standard electrode potential for zinc reduction (—0.763 V) is much more cathodic than the potential for hydrogen evolution, and the two reactions proceed simultaneously, thereby reducing the electrochemical yield of zinc. Current efficiencies slightly above 90% are achieved in modem plants by careful purification of the electrolyte to bring the concentration of the most harmful impurities, eg, germanium, arsenic, and antimony, down to ca 0.01 mg/L. Addition of organic surfactants (qv) like glue, improves the quaUty of the deposit and the current efficiency. 

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. 

Instead of depending on the thermally generated carriers just described (intrinsic conduction), it is also possible to deUberately incorporate various impurity atoms into the sihcon lattice that ionize at relatively low temperatures and provide either free holes or electrons. In particular. Group 13 (IIIA) elements n-type dopants) supply electrons and Group 15 (VA) elements (p-type dopants) supply holes. Over the normal doping range, one impurity atom supphes one hole or one electron. Of these elements, boron (p-type), and phosphoms, arsenic, and antimony (n-type) are most commonly used. When... 

Purification. Tellurium can be purified by distillation at ambient pressure in a hydrogen atmosphere. However, because of its high boiling point, tellurium is also distilled at low pressures. Heavy metal (iron, tin, lead, antimony, and bismuth) impurities remain in the still residue, although selenium is effectively removed if hydrogen distillation is used (21). 

AHoy scrap containing tin is handled by secondary smelters as part of their production of primary metals and alloys lead refineries accept solder, tin drosses, babbitt, and type metal. This type of scrap is remelted, impurities such as iron, copper, antimony, and zinc are removed, and the scrap is returned to the market as binary or ternary alloy. The dross obtained by cleaning up the scrap metal is returned to the primary refining process. 

Recycling of antimony provides a large proportion of the domestic supply of antimony. Secondary antimony is obtained from the treatment of antimony-hearing lead and tin scrap such as battery plates, type metal, beating metal, antimonial lead, etc. The scrap are charged iato blast furnaces, reverberatory furnaces, or rotary furnaces, and an impure lead bulHon or lead alloy is produced. Pure lead or antimony is then added to meet the specifications of the desired lead—antimony alloy. 

Antimony is also used as a dopant in n-ty e semiconductors. It is a common additive in dopants for siHcon crystals with impurities, to alter the electrical conductivity. Interesting semiconductor properties have been reported for cadmium antimonide [12050-27-0] CdSb, and zinc antimonide [12039-35-9] ZnSb. The latter has good thermoelectric properties. Antimony with a purity as low as 99.9+% is an important alloying ingredient in the bismuth teUuride [1304-82-17, Bi Te, class of alloys which are used for thermoelectric cooling. 

High purity stibiae is used as an -type, gas-phase dopant for Si in semiconductors (14). Low temperature distillation of stibiae at <53.3 kPa (400 torr) yields a product that on decomposition gives metallic antimony having less than 8 x lO " % impurity (18). A method for determining quantities of stibiae in the neighborhood of 0.1 mg/m in air has been reported (19). 

Betts Electrolytic Process. The Betts process starts with lead bullion, which may carry tin, silver, gold, bismuth, copper, antimony, arsenic, selenium, teUurium, and other impurities, but should contain at least 90% lead (6,7). If more than 0.01% tin is present, it is usually removed from the bullion first by means of a tin-drossing operation (see Tin AND TIN ALLOYS, detinning). The lead bullion is cast as plates or anodes, and numerous anodes are set in parallel in each electrolytic ceU. Between the anodes, thin sheets of pure lead are hung from conductor bars to form the cathodes. Several ceUs are connected in series. 

The washed slime is dried and melted to produce slag and metal. The slag is usually purified by selective reduction and smelted to produce antimonial lead. The metal is treated ia the molten state by selective oxidation for the removal of arsenic, antimony, and some of the lead. It is then transferred to a cupel furnace, where the oxidation is continued until only the silver—gold alloy (dorn) remains. The bismuth-rich cupel slags are cmshed, mixed with a small amount of sulfur, and reduced with carbon to a copper matte and impure bismuth metal the latter is transferred to the bismuth refining plant. 

Hydrochloric acid digestion takes place at elevated temperatures and produces a solution of the mixed chlorides of cesium, aluminum, and other alkah metals separated from the sUiceous residue by filtration. The impure cesium chloride can be purified as cesium chloride double salts such as cesium antimony chloride [14590-08-0] 4CsCl SbCl, cesium iodine chloride [15605 2-2], CS2CI2I, or cesium hexachlorocerate [19153 4-7] Cs2[CeClg] (26). Such salts are recrystaUized and the purified double salts decomposed to cesium chloride by hydrolysis, or precipitated with hydrogen sulfide. Alternatively, solvent extraction of cesium chloride direct from the hydrochloric acid leach Hquor can be used. 

Impurities ate elirninated in fire refining in the foUowing sequence slag, that is, oxides of iron, magnesium, aluminum, and sihcon fluxing, that is, arsenic and antimony and vapors, that is, sulfur (as SO2), cadmium, and zinc. 

The precipitated copper from this reaction is an important constituent of the slime that collects at the bottom of the electrolytic cells. The accumulation of copper as well as of impurities such as nickel, arsenic, antimony, and bismuth is controlled by periodic bleed-off and treatment in the electrolyte purification section. 

Although some changes occur in the melting furnace, cathode impurities are usually reflected directly in the final quaUty of electrorefined copper. It is commonly accepted that armealabiUty of copper is unfavorably affected by teUurium, selenium, bismuth, antimony, and arsenic, in decreasing order of adverse effect. Silver in cathodes represents a nonrecoverable loss of silver to the refiner. If the copper content of electrolyte is maintained at the normal level of 40—50 g/L, and the appropriate ratio of arsenic to antimony and bismuth (29) is present, these elements do not codeposit on the cathode. 

Lead The production of lead from lead sulphide minerals, principally galena, PbS, is considerably more complicated than the production of zinc because tire roasting of the sulphide to prepare the oxide for reduction produces PbO which is a relatively volatile oxide, and therefore the temperature of roasting is limited. The products of roasting also contain unoxidized galena as well as die oxide, some lead basic sulphate, and impurities such as zinc, iron, arsenic and antimony. 

The principal constituents of the paniculate matter are lead/zinc and iron oxides, but oxides of metals such as arsenic, antimony, cadmium, copper, and mercury are also present, along with metallic sulfates. Dust from raw materials handling contains metals, mainly in sulfidic form, although chlorides, fluorides, and metals in other chemical forms may be present. Off-gases contain fine dust panicles and volatile impurities such as arsenic, fluorine, and mercury. 

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