The Determination of Species in Slags and other Materials

"The determination of the oxidation state(s) of an element present in a solid sample may be required for a number of reasons, including the assessment of the degree of reduction which has taken place during a multi-step production of a metal. In addition, possible flaws in a metal may result from small amounts of oxides included in the solid. The analyte of interest may be present as a major component of a sample of interest, or as a minor impurity - beneficial or requiring removal - in another matrix.Numerous methods have been established for the analysis of species in solution samples - for example, Fe2+ and Fe3+ by titration, Cr6+ by colourimetric means, etc. With appropriate knowledge of the solution being analysed, many of these methods are fairly straightforward, extremely reproducible and accurate. In those instances where the analyte in a solution is known to be in only one form, the analysis is even more straightforward, since it can be achieved instrumentally (by AAS, rCP-OES or rCP-MS, for example).However, the situation with respect to the analysis of solids is not as simple. Various techniques - such as X-ray diffraction - are routinely used by our mineralogists to obtain information about the various minerals present in solid samples, and thus about the oxidation states of the analyte elements present. However, these techniques usually give results that are qualitative, or semi-quantitative at best. They are also usually time-consuming and expensive. One of our colleagues at Mintek, Deshenthree Chetty, has done extensive work in developing a method for the quantification of manganese species in solids using mineralogical methods, and this is no small achievement."