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Sample preparation strategies in ICP-AES and MS
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The most important stage in multielement analysis using ICP-AES and MS is sample preparation. Sample solution integrity and reliability of
preparation protocols dictate whether results are valid. Errors in sample preparation are the main source of uncertainty in the entire analytical
process. This short course will address the status, requirements, and challenges of sample preparation for a wide range of analytical tasks and
materials 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 materials
such 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 and
nonspectroscopic interference effects.

The following issues will be covered

µ Decomposition strategies
µ Advantages of solution techniques, instrumental considerations for calibration and validation
µ Acid decomposition, fusions, sinters, open dish, pressurized containers, microwave dissolution, and digestion
µ Partial decomposition and extraction for determining mode of occurrence of elements and species for their bioavailability
µ Disadvantages - problems of refractory samples, loss of volatiles, poor recovery, reagent cost, and contamination
µ Applications
µ Preparation of geological, environmental, biological, and energy-based samples such as fly ash, crude oil, and multiphase bituminous
sludge.
µ Open dish and closed containers, microwave dissolution and fusion procedures for selected materials
µ The routines will be evaluated using conventional figures of merit such as limits of detection, recovery, sample throughput, and
contamination
µ Sample preparation for analysis of water, wastewater, and solid waste (EPA 200.7, 200.8, SW-846) will be highlighted
µ Partial extractions using species selective reagents
µ Deleterious 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 cones
µ Compensation 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 considerations
µ Discussion and problem solving in sample preparation
µ Alternatives to sample preparation such as direct solids analysis using laser and spark ablation and slurry nebulization

Who should attend

Laboratory 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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