The method of separating the gold from the silver in gold-silver alloys by boiling with nitric acid does not act equally well in all cases. An alloy half silver half gold, rolled to thin sheet and boiled for half an hour with nitric acid, may still retain more than two-thirds of its silver. An alloy of 1 part gold and 1.7 parts of silver gives up practically the whole of its silver under similar treatment. The gold is left in a coherent, though easily broken, sheet retaining the shape of the original alloy. The gold thus left is quite spongy and porous, so that the acid can penetrate into its innermost portions. But if the silver is in large excess in the alloy, the removal of the silver is less complete, and the residual gold, instead of holding together in a form easy to manipulate, falls to a powder which requires care and time in its treatment. The older assayers, therefore, added silver to their gold in such proportion that the alloy for parting should be one quarter gold to three quarters silver. This operation they called inquartation.
The modern practice is to aim at getting an alloy with 2½ parts of silver and 1 part of gold. In gold bullion assays this proportion should be obtained with fair exactness. And in the parting of such gold buttons as are obtained in assaying ores it is well to aim at this proportion, though absolute precision is not a matter of importance.
If the button left on cupelling the lead from an assay of an ore appears white, it is best to assume that it already contains at least a sufficiency of silver, in the absence of any knowledge to the contrary. This will be true in almost all cases. But if, on parting, it does not lose at least two-thirds of its weight, this indicates that the assumption was not justified; and also what quantity of silver must be added to the button before again attempting to part. Generally the fault will be in the other direction; the silver will be in excess and the gold will break up and demand very careful treatment.
If, however, such a button is yellow, then, from its weight and depth of colour, a rough estimate can be made of how much gold is contained in it. Silver must be added to make the total weight 3½ times as much as that of the gold supposed to be present. Thus, if the button weighs 10 milligrams and is supposed to contain 8 milligrams of gold, then 8 multiplied by 3½ is 28 ; the button must, in such case, be made up to 28 milligrams by adding 18 milligrams of silver. In judging of the quality of the gold button, no ordinary error will very seriously affect the result. If, in the example just given, the quantity of gold present was really 7 or even 9 milligrams of gold, the resulting alloy would still have been suitable for such partings. In fact, in routine assays, where the quantity as well as the quality of the gold is known within fair limits, it is often the custom to add the silver for inquartation to the lead during the first cupellation.
But in the assay of rich gold alloys such approximate work will not do. If the composition is not already known with a fair degree of accuracy preliminary assays must be made. Weigh up two lots of 100 milligrams of the alloy and wrap each in 3 grams of lead. To one add 300 milligrams of silver. Cupel both. The button containing the added silver must be flattened and boiled with 15 c.c. of nitric acid; and the resulting gold must be washed, dried, ignited and weighed. This, in milligrams, gives directly the percentage of gold. The weight of the other button gives the percentage of gold and silver; the difference between the two gives, the percentage of silver. The rest will, perhaps, be copper.
The composition of the alloy being known, or having been determined as just described, the calculation of how much silver must be added is fairly simple. The following is an example. Suppose the bullion contains 92 per cent, of gold, 1 per cent, of silver and 7 per cent, of copper, and that .5 gram of it is to be taken for an assay. The .5 gram, then, will contain
But the total silver required is .46 gram x 2.5. This equals 1.15. Allowing for the .005 gram of silver already present, 1.145 gram of silver must be added.
The silver is incorporated with the gold, and at the same time the copper is eliminated, by cupelling with sheet lead. How much sheet lead must be used will depend partly on how much bullion is taken, partly on how much copper it contains. Four grams of lead will do for a .5 gram charge; and for a .3 gram charge, 3 grams may be used. But with 20 per cent, of copper these amounts should be doubled; with 40 per cent, of copper they should be trebled ; and with over 60 per cent, of copper four times as much lead should be used. For small buttons of gold as little lead as may be relied on to start cupelling may be taken; the lead may conveniently be in the form of little cups made by folding lead foil on a piece of glass rod. With a large number of bullion assays systematically worked and checked a simple plan would be to always use the quantity of lead required by the alloy containing most copper which turns up for assay. This weight, cut out of lead foil, would be kept in stock folded into little bags ready to receive the bullion and silver.
The silver used for inquartation must, of course, be free from gold and is best prepared by the assayer who is to use it (see p. 66). It should not be in long strips or angular pieces likely to perforate the lead in which it is folded. When wrapped in the lead it should be in the middle and should make as compact a parcel as possible.
Each little parcel, as completed, should be placed on a tray in its properly numbered compartment. Its position here should correspond to that it will occupy in the muffle and eventually in the cupel tray. The cupellation must be made with all the requisite precautions. A good smooth malleable button is needed for the next operation, which is known as flatting.