Determination of Platinum, Gold, and Silver by the Sulfuric acid parting method.

The crux of this technique is that platinum, in the presence of an excess of silver will not dissolve in parting with sulfuric acid but will be dissolved in parting with nitric. So with multiple cupellations we can accomplish a separation. To assure complete removal of the silver, at least 10 times as much silver as platinum must be present. The sulfuric parting solution should be 100 parts sulfuric acid to 22 parts of distilled water. Parting acid should not boil but be kept below boiling. This process involves multiple cupellations, the first one is just a weighed sample of the alloy, wrapped in lead foil, no silver added. The bead resulting from this first cupellation should be well rounded and free of lead. It is accepted that this weight is the total of Platinum, Silver and Gold together. The difference between the starting weight and the weight of this bead gives the total of base metal present in the original alloy. If the beads obtained in the first cupellation are yellow in color no gold has to be added. If the bead is not yellow, add 3 times the bead weight of gold. Note the weight of gold added as it must be subtracted out later. Also add 12 times the bead weight of silver. The weight here is not important as the silver is serving as an inquart. If the gold bead is yellow to start just add 12 times the weight in silver. Wrap the samples with the added silver and (if necessary) gold in lead and cupel at high heat 1050 degrees C. when the bead is finished move the cupels to the front of the muffle and let them continue at 800 850 degrees C for 10 minutes more. Mix 100 ml of sulfuric acid and 22 ml of distilled water and part the beads in the hot mixture, do not boil it but get it close. This parting method is much slower than Nitric parting, continue parting until the reaction stops and leave it on the plate for another 10 minutes. (It can take an hour or more depending on the starting bead size.) Don’t let it dry out!

If the parting acid develops an orange yellow color it contains palladium. To avoid calculating the palladium as part of the platinum, a second parting using 95% H2SO4 hot for 10 minutes should remove all of the palladium. Rinse the sponge and anneal it. Weigh the sponge as gold and platinum. If you added gold to the sample subtract the totals here. Now add 10 times the weight of gold, platinum mix as silver and wrap in lead and cupel at the same temperatures as the last cupellation. Remove the bead and part in nitric acid as a normal gold assay. Anneal the rinsed residue and if the color is good weigh it as gold. It is not unusual for the platinum (if in high enough concentrations) to require up to 3 inquarting / cupelling operations to remove all of the Platinum. The silver is calculated by difference from the first cupellations and the platinum is calculated by difference from the last cupellations. This method is not for quantitative palladium.

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