Pure and Applied Chemistry

Gas adsorption is an important tool for the characterisation of porous solids and fine powders. Major advances in recent years have made it necessary to update the 1985 IUPAC manual on Reporting Physisorption Data for Gas/Solid Systems. The aims of the present document are to clarify and standardise the presentation, nomenclature and methodology associated with the application of physisorption for surface area assessment and pore size analysis and to draw attention to remaining problems in the interpretation of physisorption data.

We report here the first systematic study of the effect of impurities and additives (e.g., water, chloride, and cosolvents) on the physical properties of room-temperature ionic liquids. Remarkably, it was discovered that the viscosity of mixtures was dependent mainly on the mole fraction of added molecular solvents and only to a lesser extent upon their identity, allowing viscosity changes during the course of a reaction to be entirely predictable. While the addition of such molecular solvents decreases the viscosity and density, chloride impurities, arising from the preparation of the ionic liquids, increase viscosity dramatically. The commonly used methods of preparation were validated with respect to chloride impurity.

Method validation is one of the measures universally recognized as a necessary part of a comprehensive system of quality assurance in analytical chemistry. In the past, ISO, IUPAC, and AOAC International have cooperated to produce agreed protocols or guidelines on the "Design, conduct and interpretation of method performance studies" [1], on the "Proficiency testing of (chemical) analytical laboratories" [2], on "Internal quality control in analytical chemistry laboratories" [3], and on "The use of recovery information in analytical measurement" [4]. The Working Group that produced these protocols/guidelines has now been mandated by IUPAC to prepare guidelines on the single-laboratory validation of methods of analysis. These guidelines provide minimum recommendations on procedures that should be employed to ensure adequate validation of analytical methods.

A draft of the guidelines has been discussed at an International Symposium on the Harmonization of Quality Assurance Systems in Chemical Laboratory, the proceedings from which have been published by the UK Royal Society of Chemistry.

The use of standards for the measurement of photoluminescence quantum yields (QYs) in dilute solutions is reviewed. Only three standards can be considered well established. Another group of six standards has been investigated by several independent researchers. A large group of standards is frequently used in recent literature, but the validity of these is less certain. The needs for future development comprise: (i) confirmation of the validity of the QY values of many commonly used standard materials, preferably in the form of SI traceable standards; (ii) extension of the set of standard materials to the UV and near-IR spectral ranges; and (iii) good standards or robust protocols for the measurements of low QYs.