The most important stage in multielement analysis using ICP-AES and MS is sample preparation. Sample solution integrity and reliability ofpreparation protocols dictate whether results are valid. Errors in sample preparation are the main source of uncertainty in the entire analyticalprocess. This short course will address the status, requirements, and challenges of sample preparation for a wide range of analytical tasks andmaterials using ICP-AES and MS. Advantages and disadvantages of various procedures will be critically evaluated.Several selected applications for analysis of environmental, geological, biological, metallurgical, petrochemical and energy-based materialssuch as fly ash and coal, crude oils and multiphase bituminous sludges will be described. Aspects of laboratory accreditation will be highlighted.This course will provide an insight to practical sample preparation strategies and their interaction with sample introduction, spectroscopic andnonspectroscopic interference effects.

The following issues will be coveredDecomposition strategiesAdvantages of solution techniques, instrumental considerations for calibration and validationAcid decomposition, fusions, sinters, open dish, pressurized containers, microwave dissolution, and digestionPartial decomposition and extraction for determining mode of occurrence of elements and species for their bioavailabilityDisadvantages - problems of refractory samples, loss of volatiles, poor recovery, reagent cost, and contaminationApplicationsPreparation of geological, environmental, biological, and energy-based samples such as fly ash, crude oil, and multiphase bituminoussludge.Open dish and closed containers, microwave dissolution and fusion procedures for selected materialsThe routines will be evaluated using conventional figures of merit such as limits of detection, recovery, sample throughput, andcontaminationSample preparation for analysis of water, wastewater, and solid waste (EPA 200.7, 200.8, SW-846) will be highlightedPartial extractions using species selective reagentsDeleterious effects on plasma and sample introduction systems. Salt and acid interferences, memory effects. Easily ionized element effects,salt clogging in torch injectors and in ICP-MS conesCompensation of interference effects. Review of approaches to overcoming sample-preparation related interference effects. Flow injection,internal standards, and collision cells, robust interfaces axial vs. radial ICP-AES considerationsDiscussion and problem solving in sample preparationAlternatives to sample preparation such as direct solids analysis using laser and spark ablation and slurry nebulization

Who should attendLaboratory managers, quality control and assurance specialists, research scientists, environmental chemists, geochemists, biologists, metallurgists,toxicologists, new and experienced users of atomic absorption and plasma spectrometries, and technical personnel at all levels

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