Analysis of coal fly ash and environmental materials by inductively coupled plasma atomic emission spectrometry: comparison of different decomposition procedures

Bettinelli, M.; Baroni, U.; Pastorelli, N.

doi:10.1039/ja9870200485

“…The dry methods (ashing), even at low temperatures, are not feasible for an element of such high volatility as mercury. Wet methods (Pollock, 1975) need to be performed inside a closed vessel at high or low pressures, in order to avoid any loss of mercury (Bettinelli et al, 1987;Park et al, 2006;Wu et al, 1996).…”

Section: Solid and Liquid Samplesmentioning

confidence: 99%

Analytical methods for mercury analysis in coal and coal combustion by-products

López-Antón

¹

,

Dı́az-Somoano

²

,

Ochoa-González

³

et al. 2012

International Journal of Coal Geology

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This review deals with the analysis of mercury present in different types of solid, liquid and gaseous samples involved in the coal combustion process, focusing on the specific characteristics of each type of sample and the problems typically associated with these products. The main aim of the paper is to describe the methods that, at the current stage of development, are preferable in each case (i.e. the most frequently used in most laboratories and the standard methods). The advantages and disadvantages of each method are discussed with reference to the quality of the results and the uncertainties involved in the evaluation of mercury behaviour during coal combustion processes.

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“…Fusion with lithium metaborate is feasible for geological samples provided the melt is subsequently dissolved in acid in the course of a pressure-or microwave-assisted ashing process [90].…”

Section: Comparative Merits Of the Various Sample-preparation Techniquesmentioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow

¹

,

Dunemann

²

2006

Ullmann's Encyclopedia of Industrial Chemistry

2

0

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The article contains sections titled: 1. Introduction 1.1. A Strategy Appropriate to Trace Analysis 1.2. Avoidance of Systematic Errors 1.2.1. Trace Losses and Contamination 1.2.2. Uncertainty 2. Sample Preparation and Digestion in Inorganic Analysis 2.1. Sample Treatment after the Sampling Process 2.1.1. Stabilization, Drying, and Storage 2.1.2. Homogenization and Aliquoting 2.1.3. Requirements with Respect to Materials and Chemicals 2.2. Sample‐Preparation Techniques; General Considerations 2.2.1. Special Factors Associated with Microwave‐Assisted Digestion 2.2.2. Safety Considerations 2.3. Wet Digestion Techniques 2.3.1. Wet Digestion at Atmospheric Pressure 2.3.2. Pressure Digestion 2.3.2.1. Thermally Convective Pressure Digestion 2.3.2.2. Microwave‐Assisted Pressure Digestion 2.4. “Dry” Digestion Techniques 2.4.1. Combustion in Air 2.4.2. Combustion in Oxygen 2.4.3. Cold‐Plasma Ashing 2.4.4. Fusion 2.5. Illustrative Examples 2.5.1. Sample Preparation as a Function of Analytical Method 2.5.2. Combined Use of Multiple Decomposition Techniques 2.5.3. Comparative Merits of the Various Sample‐Preparation Techniques 2.5.4. Decomposition Procedures for Determining Nonmetals 2.6. Evaluation Criteria 2.6.1. Completeness 2.6.2. Uncertainty 2.6.3. Time Factors 2.6.4. The Final Result 2.7. Concentration and Separation of Inorganic Trace Materials 2.8. Automation and Direct Analysis 2.8.1. Automation 2.8.2. Direct Analysis 2.9. Analysis of Element Species 3. Sample Preparation in Organic Analysis 3.1. Sample Treatment after the Sampling Process 3.1.1. Stabilization, Drying, and Storage 3.1.2. Homogenization and Aliquoting 3.1.3. Requirements with Respect to Materials and Chemicals 3.2. Separation of the Analyte 3.2.1. Hydrolysis 3.2.2. Liquid ‐ Liquid Extraction 3.2.3. Soxhlet Extraction 3.2.4. Microwave‐Assisted Solvent Extraction 3.2.5. Supercritical Fluid Extraction (SFE) 3.2.6. Solid‐Phase Extraction (SPE) 3.2.7. Solid‐Phase Microextraction (SPME) 3.2.8. Stir‐Bar Adsorptive Extraction (SBSE) 3.2.9. Miscellaneous Techniques 3.3. Headspace Techniques 3.3.1. Static Headspace Technique 3.3.2. Dynamic Headspace Technique (Purge and Trap) 3.4. Determination of Trace Organic Materials in Air Samples 3.5. Analyte Concentration 3.6. Derivatization 3.7. Coupled Techniques Trace analysis is a very relevant and applications‐oriented branch of analytical chemistry. The sample preparation for trace analysis must be custom‐tailored to the problem at hand. Systematic errors can arise by contact with vessel materials, reagents, or the ambient atmosphere, as well as any change in chemical or physical state. In inorganic analysis, sample preparation has to meet the requirements for a substantially trouble‐free determination of the analyte. Digestion of the matrix (microwave digestion, wet digestion, dry digestion techniques) and subsequent careful comparison of several decomposition techniques is therefore an essentially important step. Some separation and concentration techniques of the analytes are liquid –liquid extraction, solid‐phase extraction, special precipitation reactions, and electrolytic deposition. The introduction of laboratory robots should make it possible to incorporate a significant degree of automation into the time‐consuming, labor‐intensive area of sample preparation as well, leading to more efficient, reliable, and reproducible sample work‐up. The goal of sample preparation in organic trace analysis is to isolate the analyte from the sample matrix (e.g., liquid‐liquid extraction, Soxhlet extraction, microwave‐assisted solvent extraction, steam distillation) and then concentrate it and convert it into a form suitable for analysis by the selected method. Separation and concentration of an analyte must often be followed by some type of derivatization. Various coupled sample preparation and determination processes are increasingly utilized in trace organic analysis.

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“…Fusion with lithium metaborate is feasible for geological samples provided the melt is subsequently dissolved in acid in the course of a pressure-or microwave-assisted ashing process [85].…”

Section: Comparative Merits Of the Various Sample-preparation Techniquesmentioning

confidence: 99%