Atomic spectrometry sample preparation

The objective of this symposium and this book is to acquaint the readers with the latest advances in the field of elemental analysis and to focus on what avenues of future research to explore in this area. The subjects included are various elemental analysis techniques such as atomic absorption spectrometry, inductively coupled plasma emission and mass spectrometry, isotope dilution mass spectrometry. X-ray fluorescence, ion chromatography, gas chromatography-atomic emission detection, other hyphenated techniques, hetero-atom microanalysis, sample preparation, reference materials, and other subjects related to matrices such as petroleum products, lubricating oils and additives, crude oils, used oils, catalysts, etc. 

The very low Hg concentration levels in ice core of remote glaciers require an ultra-sensitive analytical technique as well as a contamination-free sample preparation methodology. The potential of two analytical techniques for Hg determination - cold vapour inductively coupled plasma mass spectrometry (CV ICP-SFMS) and atomic fluorescence spectrometry (AFS) with gold amalgamation was studied. 

The complex of the following destmctive and nondestmctive analytical methods was used for studying the composition of sponges inductively coupled plasma mass-spectrometry (ICP-MS), X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and atomic absorption spectrometry (AAS). Techniques of sample preparation were developed for each method and their metrological characteristics were defined. Relative standard deviations for all the elements did not exceed 0.25 within detection limit. The accuracy of techniques elaborated was checked with the method of additions and control methods of analysis. 

ASTM. 1998c. ASTM E 1645. Standard practice for the preparation of dried paint samples for subsequent lead analysis by atomic spectrometry. American Society for Testing and Materials. 

Techniques for analysis of different mercury species in biological samples and abiotic materials include atomic absorption, cold vapor atomic fluorescence spectrometry, gas-liquid chromatography with electron capture detection, and inductively coupled plasma mass spectrometry (Lansens etal. 1991 Schintu etal. 1992 Porcella etal. 1995). Methylmercury concentrations in marine biological tissues are detected at concentrations as low as 10 pg Hg/kg tissue using graphite furnace sample preparation techniques and atomic absorption spectrometry (Schintu et al. 1992). 

Segal, I., Kloner, A., and Brenner, I. B. (1994). Multielement analysis of archaeological bronze objects using inductively coupled plasma-atomic emission spectrometry -aspects of sample preparation and spectral-line selection. Journal of Analytical Atomic Spectrometry 9 737-744. 

Atomic absorption provides very high sensitivity but requires careful subsampling, extensive sample preparation, and detailed sample-matrix corrections. X-ray fluorescence requires little in terms of sample preparation but suffers from low sensitivity and the application of major matrix corrections. Inductively coupled argon plasma spectrometry provides high sensitivity and few matrix corrections but requires a considerable amount of sample preparation, depending on the process stream to be analyzed. 

Fast-atom bombardment mass spectrometry (FAB-MS) has been applied to the identification of diterpenoid compounds and their oxidation products. Similarly, laser-induced desorption mass spectrometric (LDMS) techniques have been applied to the identification of natural and synthetic organic pigments in microscopic paint samples prepared as cross sections [60]. 

Until now, little attention has been given to the analysis of ancient copper alloys with LA-ICP-MS. This type of material is usually analyzed with fast or instrumental neutron activation analysis (FNAA or INAA), particle induced X-ray emission (PIXE), X-ray fluorescence (XRF), inductively coupled plasma-atomic emission spectrometry or inductively coupled plasma-atomic absorption spectrometry (ICP-AES or ICP-AAS). Some of these techniques are destructive and involve extensive sample preparation, some measure only surface compositions, and some require access to a cyclotron or a reactor. LA-ICP-MS is riot affected by any of these inconveniences. We propose here an analytical protocol for copper alloys using LA-ICP-MS and present its application to the study of Matisse bronze sculptures. 

Wet chemical methods involve sophisticated sample preparation and standardization with National Bureau of Standards reference materials but are not difficult for the analytical chemist nor necessarily time consuming (Figure 1). The time from sample preparation to final results for various analytical methods, such as GFAA (graphite furnace atomic absorption), ICP (inductively coupled plasma spectroscopy), ICP-MS (ICP-mass spectrometry), and colorimetry, ranges from 0.5 to 5.0 h, depending on the technique used. Colorimetry is the method of choice because of its extreme accuracy. Typical results of the colorimetric analysis of doped oxides are shown in Tables I and II, which show the accuracy and precision of the measurements. 

Hydride generation inductively coupled plasma atomic emission spectrometry has been used to determine arsenic in soils. This technique was found to greatly reduce sample preparation time [38]. 

This chapter presents a rationale for the use of atomic absorption spectrometry (AAS) for trace element analysis of air samples, and a comparison with other analytical methods currently in use. Sampling techniques, sample preparation and analytical methods, and applications to workplace and ambient atmospheres are also discussed. Step-by-step procedures will be given which can be used to analyze air-filter samples for a broad spectrum of possible analytes. 

TIMS has been used for many years as the benchmark technique especially for uranium isotope analysis. Instrumental improvements have enabled ICP-MS to approach the accuracy and precision obtained by TIMS in measuring data. In addition, due to time consuming sample preparation steps and the need for a large volume of urine, the method has been replaced by the more powerful ICP-MS in many laboratories. An interlaboratory analytical exercise on the determination of natural and depleted uranium in urine was carried out by different ICP-MS instruments, by thermal ionization mass spectrometry (TIMS) and instrumental neutron activation analysis. TIMS has also been employed to determine fg quantities of Pu and °Pu in bioassay samples (such as human urine and artificial urine), ° in an interlaboratory comparison for the analysis of the Pu and Pu/ °Pu atomic ratios in synthetic urine by TIMS and AMS as reported in reference. ... 

Bellido-Milla, D., Moreno-Perez, J.M., Hemandez-Artiga, M.P. Differentiation and classification of beers with flame atomic spectrometry and molecular absorption spectrometry and sample preparation assisted by microwaves. Spectrochim. Acta B 55, 855-864 (2000)... 

Detection techniques of high sensitivity, selectivity, and ease of coupling with sample preparation procedures are of special interest for measuring PGM content in biological and environmental samples. ICP MS, electrothermal atomic absorption spectrometry (ET AAS), adsorptive voltammetry (AV), and neutron activation analysis (NAA) have fotmd the widest applications, both for direct determination of the total metal content in the examined samples and for coupling with instrumental separation techniques. Mass spectrometry coupled with techniques such as electrospray ionization (ESI) and capillary electrophoresis (CE) (e.g., ESI MS", LC ESI MS", LC ICP MS, CE MS", and CE ICP MS) offer powerful potential for speciation analysis of metals. MS is widely used for examination of the distribution of the metals in various materials (elemental analysis) and for elucidation of the... 

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