Analysis of ZrO2 powders by microwave assisted digestion at high pressure and ICP atomic spectrometry

Merten, D.; Broekaert, J. A. C.; Brandt, Rolf; Jakubowski, Norbert

doi:10.1039/a900676a

Cited by 22 publications

(15 citation statements)

References 17 publications

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“…4) is that almost complete dissolution can be accomplished with a single-stage process, even in the case of complex matrices. Examples found in the recent literature consist of new successful developments in the technique and apparatus [52] and applications to biological tissues [53] or technical products [54].…”

Section: Microwave-assisted Pressure Digestionmentioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow

Dunemann

2006

Ullmann's Encyclopedia of Industrial Chemistry

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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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Section: Microwave-assisted Pressure Digestionmentioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow

Dunemann

2006

Ullmann's Encyclopedia of Industrial Chemistry

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show abstract

“…4) is that almost complete dissolution can be accomplished with a single-stage process, even in the case of complex matrices. Examples found in the recent literature consist of new successful developments in the technique and apparatus [49] and applications to biological tissues [50] or technical products [51]. Examples of almost completely mineralizable matrices include resistant inorganic and high-fat organic samples.…”

Section: High-pressurementioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow¹,

Dunemann²

2001

Ullmann's Encyclopedia of Industrial Chemistry

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“…Pyrochlore Nd 2 Zr 2 O 7 is a Zr contained compound and is a derivative of the fluorite structure. Efforts have been made on digestion of ZrO 2 , a compound which also has a fluorite type structure; it was found that dissolution of ZrO 2 typically requires using hydrofluoric acid (HF) or concentrated sulfuric acid (H 2 SO 4 ) at high temperature or high pressure conditions [30,31]. Microwave digestion has also been studied but corrosive etchant such as HF or concentrated H 2 SO 4 is still required [32,33].…”

Section: Introductionmentioning

confidence: 99%