Chemical process to separate iron oxides particles in pottery sample for EPR dating

Ancient potteries usually are made of the local clay material, which contains relatively high concentration of iron. The powdered samples are usually quite black, due to magnetite, and, although they can be used for thermoluminescene (TL) dating, it is easiest to obtain better TL reading when clearest natural or pre-treated sample is used. For electron paramagnetic resonance (EPR) measurements, the huge signal due to iron spin-spin interaction, promotes an intense interference overlapping any other signal in this range. Sample dating is obtained by dividing the radiation dose, determined by the concentration of paramagnetic species generated by irradiation, by the natural dose so as a consequence, EPR dating cannot be used, since iron signal do not depend on radiation dose. In some cases, the density separation method using hydrated solution of sodium polytungstate [Na(G)(H(2)W(12)O(40))center dot H(2)O] becomes useful. However, the sodium polytungstate is very expensive in Brazil: hence an alternative method for eliminating this interference is proposed. A chemical process to eliminate about 90% of magnetite was developed. A sample of powdered ancient pottery was treated in a mixture (3:1:1) of HCI, HNO(3) and H(2)O(2) for 4 h. After that, it was washed several times in distilled water to remove all acid matrixes. The original black sample becomes somewhat clearer. The resulting material was analyzed by plasma mass spectrometry (ICP-MS), with the result that the iron content is reduced by a factor of about 9. In EPR measurements a non-treated natural ceramic sample shows a broad spin-spin interaction signal, the chemically treated sample presents a narrow signal in g= 2.00 region, possibly due to a radical of (SiO(3))(3-), mixed with signal of remaining iron [M. lkeya, New Applications of Electron Spin Resonance, World Scientific, Singapore, 1993, p. 285]. This signal increases in intensity under -gamma-irradiation. However, still due to iron influence, the additive method yielded too old age-value. Since annealing at 300 degrees C, Toyoda and Ikeya IS. Toyoda, M. Ikeya, Geochem. J. 25 (1991) 427-445] states that E `(1)-signal with maximum intensity is obtained, while annealing at 400 degrees C E`(1)-signal is completely eliminated, the subtraction of the second one from 300 degrees C heat-treated sample isolate E`(1)-like signal. Since this is radiation dose-dependent, we show that now EPR dating becomes possible. (C) 2008 Elsevier B.V. All rights reserved.

SEM, EPR and ToF-SIMS analyses applied to unravel the technology employed for pottery-making by pre-colonial Indian tribes from Pantanal, Brazil

The present work aims at elucidating the technology applied in the fabrication of ceramic objects by the ancient ceramists that inhabited the western border of Pantanal, Mato-Grosso do Sul, with the help of a multidisciplinary approach making use of chemical and physical methods of analysis. The potshards under study show the presence of different types of additives, as determined by scanning electron microscopy (SEM) and time of flight secondary ion mass spectrometry (ToF-SIMS). The dispersion of the additives within the ceramic matrix was also addressed by SEM, which shed light on the mounting technique used by the potters to assemble the ceramic vessels. Moreover, the tensile strength conferred to the pottery by the use of a specific type of additive was evaluated by applying a mechanical test. These results were correlated with the firing temperature of the potshards, determined by means of electron paramagnetic resonance (EPR). (C) 2010 Elsevier Ltd. All rights reserved.

Dating archeological ceramics from the Valley of Vitor, Arequipa by the TL method

The age of some ancient pottery from the Valley of Vitor in the region of Arequipa, Peru, is determined by the thermoluminescence (TL) method. For dating, a 325 degrees C TL peak was used and irradiation with -dose from 5 to 50Gy was carried out for the additive method, and from 0.4 to 5Gy for the regeneration method. For these dose values, the TL intensity is observed to grow linearly, obtaining an accumulated dose of 1.62 +/- 0.09Gy and 1.36 +/- 0.03Gy for the additive and regeneration methods, respectively. The age (A) of the sample was calculated by the two methods, being A=867 +/- 195 years after Christ (AC) for the additive method and A=1050 +/- 157 years AC for the regeneration method. Both results are within 800-1200 years AC, which is the period of the Wari culture.

Correlations between chemical composition and provenance of Justino site ceramics by INAA

Instrumental neutron activation analysis (INAA), have been used for the definition of compositional groups of potteries from Justino site, Brazil, according to the chemical similarities of ceramic paste. The outliers were identified by means of robust Mahalanobis distance. The temper effect in the ceramic paste was studied by means of modified Mahalanobis filter. The results were interpreted by means of cluster, principal components, and discriminant analyses. This work provides contributions for the reconstruction of the prehistory of baixo Sao Francisco region, and for the reconstitution of the Brazilian Northeast ceramist population of general frame.