Developments in Ceramic Materials Research
Developments in Ceramic Materials Research
Developments in Ceramic Materials Research
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Postclassic Maya <strong>Ceramic</strong> Advances 11<br />
then fired to 700ºC <strong>in</strong> an electric kiln. After the clays cooled, they are processed <strong>in</strong> the same<br />
manner as ceramic samples.<br />
Portions of approximately 150 mg of powder were weighed <strong>in</strong>to clean high-density<br />
polyethylene vials used for short irradiations at MURR. At the same time, 200 mg of each<br />
sample were weighed <strong>in</strong>to clean high-purity quartz vials used for long irradiations. Along<br />
with the unknown samples, standards made from National Institute of Standards and<br />
Technology (NIST) certified standard reference materials of SRM-1633a (coal fly ash) and<br />
SRM-688 (basalt rock) were similarly prepared, as were quality control samples (e.g.,<br />
standards treated as unknowns) of SRM-278 (obsidian rock) and Ohio Red Clay (a standard<br />
developed for <strong>in</strong>-house applications).<br />
Neutron activation analysis of ceramics at MURR, which consists of two irradiations and<br />
a total of three gamma counts, constitutes a superset of the procedures used at most other<br />
NAA laboratories (Glascock 1992; Neff 1992, 2000). The 720-second count yields gamma<br />
spectra conta<strong>in</strong><strong>in</strong>g peaks for n<strong>in</strong>e short-lived elements alum<strong>in</strong>um (Al), barium (Ba), calcium<br />
(Ca), dysprosium (Dy), potassium (K), manganese (Mn), sodium (Na), titanium (Ti), and<br />
vanadium (V). The long irradiation is analogous to the s<strong>in</strong>gle irradiation utilized at most other<br />
laboratories. After the long irradiation, samples decay for seven days, and then are counted<br />
for 1,800 seconds (the "middle count") on a high-resolution germanium detector coupled to<br />
an automatic sample changer. The middle count yields determ<strong>in</strong>ations of seven medium halflife<br />
elements, namely arsenic (As), lanthanum (La), lutetium (Lu), neodymium (Nd),<br />
samarium (Sm), uranium (U), and ytterbium (Yb). After an additional three- or four-week<br />
decay, a f<strong>in</strong>al count of 8,500 seconds is carried out on each sample. The latter measurement<br />
yields the follow<strong>in</strong>g 17 long half-life elements: cerium (Ce), cobalt (Co), chromium (Cr),<br />
cesium (Cs), europium (Eu), iron (Fe), hafnium (Hf), nickel (Ni), rubidium (Rb), antimony<br />
(Sb), scandium (Sc), strontium (Sr), tantalum (Ta), terbium (Tb), thorium (Th), z<strong>in</strong>c (Zn), and<br />
zirconium (Zr) (Glascock 1992).<br />
Laser Ablation Inductively Coupled Mass Spectroscopy (LA-ICP-MS)<br />
Of the 210 sherds submitted for INAA, 100 1 exterior slips recovered from excavations at<br />
Ch’ich’, Ixlú, Zacpetén, and Tipuj were analyzed by LA-ICP-MS at California State<br />
University-Long Beach (Cecil and Neff 2006). In addition to analyz<strong>in</strong>g exterior slips, black<br />
(n=17) and red (n=17) pa<strong>in</strong>ted decorations were also tested on those sherds with decoration.<br />
LA-ICP-MS was chosen because of its success with analyz<strong>in</strong>g slips and pa<strong>in</strong>ts (Neff 2002;<br />
Speakman 2005; Vaughn et al. 2005; among others). In addition to previous success with the<br />
technique, it is very difficult to extricate the Postclassic slip and pa<strong>in</strong>t pigments from the<br />
sherd paste without also <strong>in</strong>clud<strong>in</strong>g part of the sherd paste <strong>in</strong> the analysis. Therefore, analyz<strong>in</strong>g<br />
slips and pa<strong>in</strong>ts <strong>in</strong> situ is ideal. Because the laser ablates only the first five microns (Neff<br />
2002), it is unlikely to penetrate beyond the level of the slip and/or pa<strong>in</strong>ted decoration to<br />
<strong>in</strong>clude chemical analysis of the underly<strong>in</strong>g pottery sherd paste composition.<br />
The laboratory at California State University-Long Beach operates a Perk<strong>in</strong>-Elmer ELAN<br />
6100 DRC quadrupole ICP-MS and a New Wave UP-213 laser ablation system. The laser<br />
was run with a raster spac<strong>in</strong>g of 150 microns, a spot size of 100 microns, and a laser scan<br />
speed of 70 microns/second. Laser power was set at 60% and the repetition rate was 20Hz.<br />
1 Exterior slips on three samples were too th<strong>in</strong> (paste was also ablated) and not <strong>in</strong>cluded <strong>in</strong> the study. As a result,<br />
only 97 exterior slip samples are <strong>in</strong>cluded <strong>in</strong> this study.