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Crossing the Borders: New Methods and Techniques in the Study of Archaeological Materials from the Caribbean

by Corrine L. Hoffman, et. al.

by Corrine L. Hoffman, et. al.

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36 / Cooper, Mart<strong>in</strong>ón- Torres, <strong>and</strong> Valcárcel Rojas<br />

gence <strong>of</strong> social <strong>in</strong>equality associated with <strong>in</strong>herited power (Valcárcel Rojas <strong>and</strong><br />

Rodríguez Arce 2003, 2005). The catalyst for <strong>the</strong> development or material manifestation<br />

<strong>of</strong> this hierarchy was unclear.<br />

Therefore, a comprehensive microanalysis <strong>of</strong> <strong>the</strong> metal objects <strong>from</strong> <strong>the</strong> cemetery<br />

was conducted to study <strong>the</strong>ir composition, manufacture, <strong>and</strong> orig<strong>in</strong> <strong>in</strong> order to<br />

help <strong>in</strong>terpret <strong>the</strong>ir relative value to <strong>the</strong> <strong>in</strong>digenous community that buried <strong>the</strong>m.<br />

Laboratory <strong>Methods</strong><br />

An <strong>in</strong>itial study <strong>of</strong> a sample <strong>of</strong> <strong>the</strong> metal objects was carried out <strong>in</strong> <strong>the</strong> Centre <strong>of</strong><br />

Nuclear Development <strong>and</strong> Technological Application, part <strong>of</strong> <strong>the</strong> M<strong>in</strong>istry <strong>of</strong> Science,<br />

Technology, <strong>and</strong> Environment <strong>in</strong> Havana, Cuba, by energy- dispersive X- ray<br />

fluorescence ( ED- XRF) surface analyses. The corroded condition <strong>and</strong> small size<br />

<strong>of</strong> <strong>the</strong> metal specimens prevented a full quantitative analysis <strong>of</strong> <strong>the</strong> metal compositions;<br />

however, surface analysis <strong>in</strong>dicated ternary gold/ copper/ silver alloys <strong>and</strong><br />

z<strong>in</strong>c- rich copper alloys (Valcárcel Rojas 2002). Subsequently, a more detailed analytical<br />

study <strong>of</strong> <strong>the</strong> metal assemblage was carried out at <strong>the</strong> Wolfson <strong>Archaeological</strong><br />

Science Laboratories, Institute <strong>of</strong> Archaeology UCL, London. These analyses employed<br />

ED- XRF, optical microscopy, <strong>and</strong> scann<strong>in</strong>g electron microscopy with an attached<br />

energy- dispersive spectrometer ( SEM- EDS).<br />

ED- XRF analyses were performed with a Spectro X- Lab Pro 2000; <strong>the</strong> objects<br />

analyzed were smaller than <strong>the</strong> detector w<strong>in</strong>dow (ø 25 mm), <strong>and</strong> were placed directly<br />

<strong>in</strong> <strong>the</strong> chamber without any preparation. These qualitative analyses <strong>of</strong> surface<br />

compositions allowed comparison with <strong>the</strong> ED- XRF results <strong>from</strong> Cuba, <strong>and</strong><br />

also with <strong>the</strong> bulk compositions <strong>of</strong> mounted cross sections <strong>of</strong> specimens exam<strong>in</strong>ed<br />

with <strong>the</strong> SEM- EDS.<br />

Exam<strong>in</strong>ation by optical microscopy <strong>in</strong>volved <strong>the</strong> use <strong>of</strong> a st<strong>and</strong>ard Wild Heerbrugg<br />

stereoscopic microscope for complete objects, <strong>and</strong> a Leica DM LM for reflected<br />

light microscopy <strong>of</strong> metallographic cross sections. These were mounted <strong>in</strong><br />

epoxy res<strong>in</strong> <strong>and</strong> polished to 1 µm gra<strong>in</strong> size follow<strong>in</strong>g established procedures (Scott<br />

1991).<br />

SEM- EDS was carried out us<strong>in</strong>g a Philips XL30 <strong>in</strong>strument with an INCA Oxford<br />

spectrometer package. Specimens were observed <strong>in</strong> secondary electron (SE)<br />

<strong>and</strong> backscattered electron (BSE) modes, <strong>and</strong> analyzed us<strong>in</strong>g <strong>the</strong> EDS system. Operat<strong>in</strong>g<br />

conditions for data collection were as follows: work<strong>in</strong>g distance <strong>of</strong> 10 mm;<br />

accelerat<strong>in</strong>g voltage <strong>of</strong> 20 kV; spot size <strong>of</strong> 4.7 to 5.3 (INCA conventional units) <strong>and</strong><br />

process time 5, correspond<strong>in</strong>g to a detector dead time <strong>of</strong> 25–40 percent; <strong>and</strong> acquisition<br />

time <strong>of</strong> 75 seconds. Based on previous analyses, <strong>the</strong> lower confidence limits<br />

for this <strong>in</strong>strument may be established at 0.3 wt percent, <strong>and</strong> values below this<br />

limit can be taken as <strong>in</strong>dicative only. Bulk compositions given <strong>in</strong> this paper are averages<br />

<strong>of</strong> five measurements taken <strong>in</strong> areas <strong>of</strong> ~100 µm2, ei<strong>the</strong>r on <strong>the</strong> surface <strong>of</strong><br />

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