Factors affecting high-pressure solvent extraction (accelerated solvent extraction) of additives from polymers.

Irganox 1010 (pentaerythritol tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)] propionate) is successfully extracted from polypropylene using solvents at high temperatures and pressures in a homemade accelerated solvent extraction system. For example, using freeze-ground polymer, 90% extraction is possible within 5 min with 2-propanol at 150 °C. Extraction curves for 2-propanol and acetone fit well to the "hot ball" model, previously developed for supercritical fluid extraction. Diffusion coefficients are determined for extractions with 2-propanol, acetone, and cyclohexane over a range of temperatures, and the activation energies for the diffusion are 134, 107, and 61 kJ mol(-)(1), respectively. The lower figure for acetone and cyclohexane indicates that these solvents swell the polymer more than does 2-propanol. The polymer dissolves in the solvent at too high a temperature, which causes blockage of the transfer lines. For maximum extraction rates, the highest temperature for each solvent that avoids dissolution of the polymer should be used. The use of mixed solvents is investigated and shows advantages in some cases, with the aim of producing a solvent that will swell the polymer but not dissolve it.

Solubility of chelating agents and metal-containing compounds in supercritical fluid carbon dioxide.

The solubility of 49 metal-containing compounds and 15 "free" ligands in supercritical fluid carbon dioxide is reviewed. Solubilities were found to range over eight orders of magnitude, with the highest value of solubility being 56 g l(-1). Metals complexed with fluorine substituted ligands were found to be the most soluble, and metals complexed with phenyl-substituted ligands the least soluble. A general trend for increasing solubility with increasing oxidation state is observed and this is correlated with the increased number of coordinating ligands protecting the metal center from interaction with the supercritical fluid and also due to the increased number of solvation interactions with the increased number of ligand groups.

Supercritical fluid extraction of sulphamethazine and its metabolites from meat tissues.

An investigation is reported of factors affecting the supercritical fluid extraction of sulphamethazine and five of its metabolites from spiked meat (swine liver and kidney). The addition of the polar modifier methanol to the carbon dioxide extracting fluid was found to generally enhance recoveries under subcritical and supercritical conditions. Recoveries of the ionic metabolites were increased by up to 72% when employing tetramethylammonium hydroxide for ion pairing in situ with the supercritical fluid extraction. Extraction efficiency is demonstrated to be dependent on the matrix. Extractions of the less polar compounds from the kidney are more successful than from the liver, which corresponds to their partitioning into the supercritical fluid and/or the greater fraction of highly extractable fatty materials. The kidney was more retentive than liver for the relatively more polar compounds, which suggests that the liver offers a less polar environment under the same extraction conditions.

Rapid analysis of polyolefin antioxidants and light stabilisers by supercritical fluid chromatography.

Nineteen commercial antioxidants and light stabilisers, with a wide range of relative molecular masses and boiling-points, present in polyolefins were analysed by packed column supercritical fluid chromatography on four different phases with CO2 or 10% MeOH-CO2 as the mobile phase and with UV detection. The technique is shown to yield short analysis times and sufficient resolution for a number of additives present in a given polyolefin.