Innovative Analytical Methodology Combining Micro-X-Ray Diffraction, Scanning Electron Microscopy-Based Mineral Maps, and Diffuse Reflectance Infrared Fourier Transform Spectroscopy to Characterize Ar

详细信息    查看全文

• 作者：Carolina Cardell ; Isabel Guerra ; Julia Romero-Pastor ; Giuseppe Cultrone ; Alejandro Rodriguez-Navarro
• 刊名：Analytical Chemistry
• 出版年：2009
• 出版时间：January 15, 2009
• 年：2009
• 卷：81
• 期：2
• 页码：604-611
• 全文大小：322K
• 年卷期：v.81,no.2(January 15, 2009)
• ISSN：1520-6882

文摘

Excavations at the 14th century Moorish rampart (Granada, Spain) unearthed a brick oven alongside black ash and bone stratigraphic layers. In situ evidence suggests the oven served to fabricate a wall coating including powdered burnt bones. Original ad hoc analyses improved on conventional methods were used to confirm this hypothesis. These methods enable (i) nondestructive micro-X-ray diffraction (μ-XRD) for fast mineralogical data acquisition (10 s) and moderately high spatial (500 μm) resolution and (ii) identification and imaging of crystalline components in sample cross-sections via mineral maps, yielding outstanding visualization of grain distribution and morphology in composite samples based on scanning electron microscopy-energy dispersion X-ray spectrometry (SEM-EDX) elemental maps. Benefits are shown for applying diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) vs transmittance-FT-IR (T-FT-IR) to analyze organic and inorganic components in single samples. Complementary techniques to fully characterize artifacts were gas chromatography/mass spectroscopy (GC/MS), optical microscopy (OM), conventional powder XRD, and ¹⁴C dating. Bone-hydroxyapatite was detected in the coating. Mineralogical transformations in the bricks indicate oven temperatures well above 1000 °C, supporting the hypothesis.