Abstract: A method of microwave assisted chemical reaction includes providing a microwavable reaction vessel which contains at least one material in a sample. The sample is heated by microwave energy to elevate the temperature of the reagent and at least partially volatilize the sample to establish a gas phase within the vessel followed by positive cooling of the gas phase to reduce the temperature and responsively reduce the pressure of the gas phase without effecting substantial cooling of the liquid phase. The method may involve employing cooling exteriorly of and adjacent to the gas phase containing portion of the vessel or cooling by means of a coolant flowing within coils disposed in the interior of the vessel or both. The process is preferably a continuous process. The apparatus may be a vessel transparent to microwave energy for receiving the sample. The vessel has space overlying the liquid phase containing portion for a gas phase.

Abstract: A method of microwave assisted chemical reaction includes providing a microwavable reaction vessel which contains at least one material in a sample. The sample is heated by microwave energy to elevate the temperature of the reagent and at least partially volatilize the sample to establish a gas phase within the vessel followed by positive cooling of the gas phase to reduce the temperature and responsively reduce the pressure of the gas phase without effecting substantial cooling of the liquid phase. The method may involve employing cooling exteriorly of and adjacent to the gas phase containing portion of the vessel or cooling by means of a coolant flowing within coils disposed in the interior of the vessel or both. The process is preferably a continuous process. The apparatus may be a vessel transparent to microwave energy for receiving the sample. The vessel has space overlying the liquid phase containing portion for a gas phase.

Abstract: The method of determining the concentration of a specie in a sample includes providing at least one predetermined, enriched isotope in the same speciated form as the species to be measured, spiking the sample containing the species to be measured, equilibrating the spiked species with the species to be measured, separating the species from the sample and subsequently determining the concentration of the species to be measured by employing isotopic element specie ratios. In one embodiment, a single speciated isotope spike is employed and, in others, two or more such spikes may be employed. In a preferred embodiment, time resolution chromatography is used to effect separation of these species from the sample and mass spectrometer is employed in determining isotopic elemental ratios. It is also preferred that a method be employed to determine if there has been conversion from one species to another.

Abstract: A system is provided for the detection of transition elements and/or rare earth elements in an aqueous sample which also contains high concentrations of alkali and alkaline earth metals. The system is effective for determination of transition elements and/or rare earth elements in sea water, industrial waste streams, biological fluids and biological issue samples.

Abstract: A method for the detection of trace transition elements and rare earth elements in a sample also containing alkali metals or alkaline earth elements. The sample is flowed through a chelator column which retains the transition elements and rare earth elements. Then a first eluent (e.g. ammonium acetate) is passed through the column to strip the alkali and alkaline earth metals retained on the column. Then a second eluent (e.g. a strong acid) is passed through the chelator column to remove the transition elements in a chelator effluent which flows through an ion exchange resin concentrator to retain only the transition elements and rare earth elements. Then, a chelator complexing agent (e.g. pyridine-2,6 dicarboxylic acid or an oxalate) flows through the concentrator column to remove the transition elements and rare earth elements.