Archaeological samples are complex in composition since they generally comprise a mixture of materials submitted to deterioration factors largely dependent on the environmental conditions. Therefore, the integration of analytical tools such as TXRF, FT-IR and GC-MS can maximize the amount of information provided by the sample. Recently, two black rock art samples of camelid figures at Alero Hornillos 2, an archaeological site located near the town of Susques (Jujuy Province, Argentina), were investigated. TXRF, selected for inorganic information, showed the presence of manganese and iron among other elements, consistent with an iron and manganese oxide as the black pigment. Aiming at the detection of any residual organic compounds, the samples were extracted with a chloroform-methanol mixture and the extracts were analyzed by FT-IR, showing the presence of bands attributable to lipids. Analysis by GC-MS of the carboxylic acid methyl esters prepared from the sample extracts, indicated that the main organic constituents were saturated (C(16:0) and C(18:0)) fatty acids in relative abundance characteristic of degraded animal fat. The presence of minor C(15:0) and C(17:0) fatty acids and branched-chain iso-C(16:0) pointed to a ruminant animal source.
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