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Dry or Fire Assaying

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DRY OR FIRE ASSAYING Gold and Silver Ores.—Gold and silver are bought by the ounce (Troy), and, for convenience in the evaluation of ores, the contents of precious metals are not reported in percentages, but in oz., or decimals of an oz. (Troy), per ton of ore. The ton (Avoirdupois) contains 32,666.6 oz. (Troy), and, to save calculation, the weight of ore taken for assay is 32.67 grammes, or some multiple of this. This weight is known as the Long Assay Ton (A.T.), and has the advantage that every o.00i gramme of metal found represents i oz. (Troy) per ton of ore. In some countries it is more usual to employ the Short Ton of 2,000 lb., and the Short Assay Ton of 29.17 grammes is used in assaying. In many of the Latin countries the Metric Ton of i,000 kilos is the standard, and the values are reported in grammes per ton, no Assay Ton being required. Sometimes the gold or silver present is reported in its money value (e.g., $42.50 per ton). The assay consists of three operations: (i) fusion, (2) cupel lation, and (3) parting.

(I) Fusion.--This may be carried out by two methods.

(a) In the "Pot Fusion" method, one A.T. or more of the crushed ore is mixed and fused in a clay crucible, or pot, with lead oxide (about 3o grammes), a reducing agent such as char coal, argol, or flour (up to about 5 grammes), and a suitable quantity of reagents called "fluxes" which combine with the "gangue," or waste matter in the ore, forming a "flowing," or fusible slag. The fluxes used depend upon the nature of the ore. If the gangue contains silica, tin 'r zinc, soda is required; for iron, lime, or other basic materials, borax, crushed quartz, or similar fluxes are introduced. The quantity of these fluxes is varied to suit the requirements of the ore under examination, and will be nearly twice the weight of the ore. The crucible is placed in a coke, oil, or gas furnace at a fairly low temperature, and kept at a dull-red heat for about ten minutes, to allow the chemical reactions to be completed. By the action of the reduc ing agent, metallic lead is formed, which sinks through the charge to the bottom of the pot, alloying with, and so collecting the gold and silver. The temperature is then raised until the whole charge is molten and thoroughly fluid, and the contents of the pot are poured into a dry, iron mould. When cold, the brittle slag is broken away with a hammer, leaving a "button" of lead which contains the precious metals.

Certain types of ore require special treatment. Sulphide ores may be given a preliminary roasting at a red heat to burn off the sulphur, or the ore is desulphurised during fusion by adding suitable reagents to the charge. Cupriferous ores are treated with acid before fusion, to dissolve away the copper. Arsenical ores are roasted before fusion, and antimonial ores are oxidised by adding nitre to the charge.

(b) In the "Scorification" method, about io grammes or A.T. of ore is mixed with 30-35 grammes of granulated lead in a "Scorifier," which is a shallow fireclay dish. Another 30-40 grammes of granulated lead are placed on top of the charge, and about i gramme of borax is added as a thin cover. The scorifier is placed in a muffle furnace at a very high temperature, when simultaneous oxidation of the lead and of the ore takes place. Some impurities volatilise, and the remainder combines with the oxidised lead and the borax, forming a slag. A ring of this slag soon forms round the surface of the molten lead, and, as oxidation proceeds, the ring extends towards the centre and finally covers the whole surface. At this point the oxidation ceases, and the charge is poured as before. The quantities of granulated lead and borax required will depend upon the nature of the ore, and are variable. It will be seen that, as a smaller quantity of ore is used, the method is only suitable for rich ma terials, and hence is practically confined to the assay of rich silver ores, very high grade gold ores being rarely found.

(2) Cupellation.--By this process the gold and silver are isolated from the lead obtained in the first operation. A cupel is a shallow cup made of bone-ash or some other absorbent matter, which, when hot, is capable of absorbing any molten material which wets its surface. The lead button is fused upon a red-hot cupel in a muffle furnace. The lead melts and oxidises, forming molten litharge, which is absorbed, together with any oxidised impurities, into the cupel. The gold and silver do not oxidise, but remain on the cupel, forming a small bead of "Bullion," which is weighed.

(3) Parting.—The bullion bead is attacked with nitric acid which dissolves, or "parts," the silver from the gold. Before commencing this operation, it is necessary to ensure that the alloy is of such a composition that the whole of the silver will be dissolved away from the gold. The proportion, by weight, of silver to gold should be at least 4:1 if the gold present exceeds 0.01 gramme, and this ratio is increased for smaller amounts of gold. If there is insufficient silver present, more must be added by the process of "Inquartation." This consists of adding a sufficient weight of silver to the bead, either by melting the metals together with a blow-pipe flame, or by recupelling them in a small piece of pure lead. The name "Inquartation" was introduced in early times, when it was believed that the proportion of silver to gold should always be 3:1. The inquarted alloy is flattened under a hammer and dropped into boiling nitric acid. The silver dissolves, leaving a brown residue of gold. This is washed with distilled water, dried, and annealed by heating it to redness, when it takes on the familiar yellow colour of pure gold. The weight of this residue gives, by calculation, the gold content of the ore, and the silver is determined by difference from the weight of the bullion.

Gold Bullion.

This is assayed by cupellation. A representa tive sample of o.5 gramme of the alloy is wrapped in 2-6 grammes of pure, silver-free lead foil, the exact weight of the lead depend ing on the purity of the alloy. The lead packet is cupelled in the usual manner, and the resulting bead of gold and silver is weighed. The bead is again wrapped in lead foil, together with sufficient silver to form a parting alloy, the proportion of silver to gold in this case being 2 : i. The bead obtained after cupella tion, is cleaned and rolled into a thin strip, or "fillet," which is curled into a small "cornet" or coil. The cornet is treated twice with boiling nitric acid, and is then washed, dried, annealed, and weighed. Errors introduced during cupellation and parting are corrected by carrying out simultaneous "check" assays on test pieces made up to the same composition as the alloy. The gold present is reported as so many parts of gold in i,000 parts of alloy. This is called "Fineness," and British gold coinage is said to be "916.6 Fine." Lead Ores.—The assay consists of fusion with suitable fluxes and a reducing agent, in a clay or iron crucible. The charge is varied to suit the ore. A typical example being about one part of ore, 21 parts of soda, one half part of borax and one half part of argol. When a clay crucible is used, a piece of hoop iron, in length about twice the height of the crucible, is pushed down into the mixture to act as a desulphurising agent. When an iron crucible is used, the pot itself acts in this way. The crucible is heated in a wind furnace, and it is important to work the charge at the lowest temperature which will give a fluid slag, in order to prevent undue loss of lead, and to minimise the amount of metallic impurities which will pass into the button. On com pletion of the fusion, the charge is poured into a mould, and the lead button is separated from the slag and weighed.

Tin Ores.

The smelting assay is unsuitable for crude tin ores, but satisfactory results may be obtained with high-grade concentrates, provided the charge is run at a low temperature and is not left in the fire longer than necessary. The sample of ore is mixed with four times its weight of crude potassium cyanide, and is placed in a clay crucible. The pot is put in a furnace, and the temperature is raised to dull redness, and kept there until the charge is thoroughly fused. The temperature is further raised for a few minutes to render the slag quite fluid, and the charge is poured as usual. Many metallic impurities in the ore are reduced and pass into the tin button ; consequently the method is unreliable except for fairly clean concentrates.

gold, lead, ore, silver and charge