Electrothermal atomization ceramics analysis

Thirty-two sherds representing five different examples of Kayenta Anasazi Pueblo II pottery (Tusayan Corrugated [TC], Medicine Black-on-Red [MB], Tusayan Black-on-Red [TB], Dogoszhi Black-on-White [DB], and Sosi Black-on-White [SB]) have been analyzed for the elements As, Ba, Co, Cr, Cm, Fe, Mn, Ni, Pb, Se, V, and Zn by using the techniques of flame atomic absorption spectroscopy (.FAA) and electrothermal atomic absorption spectroscopy (ETAA). Analytical procedures for the chemical analysis of ceramics afford accuracy and sensitivity and require only a modest capital investment for instrumentation. The sherd samples were collected at two sites, one in southern Utah (Navajo Mountain [NM]) and the second in northern Arizona (Klethla Valley [KV]). These sites are approximately 60 km apart. Statistical treatment of the data shows that only three clay types were used in the 32 sherds analyzed, and that only three elements (Fe, Pb, and Ni) are necessary to account for 100% of the dispersion observed within this sample set. 

Traditional flame atomization methods have been preferred for atomic absorption analysis of ceramics. Very little mention has been made of electrothermal atomization (ETAA) in the literature. Although ETAA offers increased sensitivity with lower detection limits and smaller sample sizes, the problems of matrix interference (22-25) have resulted in the development of sample-specific methods for ETAA. 

Atomic absorption spectrometry (AAS) was established as the most popular gas chromatography (GC) detection technique for lead speciation analysis in the first years of speciation studies. The increase of the residence time of the species in the flame using a ceramic tube inside the flame and, later, the use of electrically heated tubes, made out of graphite or quartz where electrothermal atomization was achieved, provided lower detection limits but still not sufficiently low. Later, the boom of plasma detectors, mainly microwave induced plasma atomic emission (MIP-AES) and, above all, inductively coupled plasma atomic emission and mass spectrometry (ICP-AES and ICP-MS, respectively) allowed the sensitivity requirements for reliable organolead speciation analysis in environmental and biological samples (typically subfemtogram levels) to be achieved. These sensitivity requirements makes speciation analysis of organolead compounds by molecular detection techniques such as electrospray mass spectrometry (ES-MS) a very difficult task and, therefore, the number of applications in the literature is very limited. 

Lucic M. and Krivan V. (1999) Analysis of aluminium-based ceramic powders by electrothermal vaporization inductively coupled plasma atomic emission spectrometry using a tungsten coil and slurry sampling, Fresenius J Anal Chem 363 64-72. 

CONTENTS 1. Basic Principles (J. W. Robinson). 2. Instrumental Requirements and Optimisation (J. E. Cantle). 3. Practical Techniques (J. E. Cantle). 4a. Water and Effluents (B. J. Farey and L A. Nelson). 4b. Marine Analysis by AAS (H. Haraguchi and K. Fuwa). 4c. Analysis of Airborne Particles in the Workplace and Ambient Atmospheres (T.J. Kneip and M. T. Kleinman). 4d. Application of AAS to the Analysis of Foodstuffs (M. Ihnat). 4e. Applications of AAS in Ferrous Metallurgy (K. Ohis and D. Sommer). 4f. The Analysis of Non-ferrous Metals by AAS (F.J. Bano). 4g. Atomic Absorption Methods in Applied Geochemistry (M. Thompson and S. J. Wood). 4h. Applications of AAS in the Petroleum Industry W. C. Campbell). 4i. Methods forthe Analysis of Glasses and Ceramics by Atomic Spectroscopy (W. M. Wise et al.). 4j. Clinical Applications of Flame Techniques (B.E. Walker). 4k. Elemental Analysis of Body Fluids and Tissues by Electrothermal Atomisation and AAS (H. T. Delves). 4I. Forensic Science (U. Dale). 4m. Fine, Industrial and Other Chemicals. Subject Index. (All chapters begin with an Introduction and end with References.)... 

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