RESUMO
Soils have distinctive chemical, physical, mineralogical and biological properties, which make it possible to differentiate them in different environments and also to test for an association of a particular questioned item with a crime scene. Mineral compositions and structures in the soil clay fraction can reflect a distinct characteristic when analyzed by powerful techniques. In this way, the aim of this study was to compare the discriminative power of Fe-oxides concentrated clay samples from the same soil class with and without differences in parent material when analyzed using the Rietveld method and two sources of X-ray diffraction: conventional and high-resolution synchrotron radiations. Clay samples were Fe concentrated (kaolinite and gibbsite removal) to clarify mineralogical composition of 12 samples from three simulated crime scenes, developed under claystone and granite. By Rietveld refinement, detailed crystallographic data were obtained to discriminate samples according their provenance. By synchrotron radiation, mineral data demonstrated the power of quantitative (crystallite size and minerals contents) and qualitative (identification of majoritarian and accessory minerals) analysis by Rietveld refinement, which provides well-resolved data able to discriminate samples from different and same geology. The techniques can be applied in other criminal investigations given their potential of discrimination.
Assuntos
Óxidos , Síncrotrons , Argila , Análise dos Mínimos Quadrados , Minerais/análise , Óxidos/análise , Solo/química , Difração de Raios XRESUMO
Abstract The purpose of this research was to discriminate soil fractions using mineralogical and elemental analyses and to show those fractions that present greater contribution to the soil mass attenuation coefficient (μ) as well as their partial cross-sections for photoelectric absorption (PA), coherent scattering (CS) and incoherent scattering (IS). Soil samples from different places of Brazil classified as Yellow Argisol, Yellow Latosol and Gray Argisol were submitted to elemental and mineralogical analyses through energy dispersive X-ray fluorescence (EDXRF) and Rietveld Method with X-ray diffraction data (RM-XRD). The mixture rule was utilized to calculate μ of each soil. The EDXRF analysis showed as predominant elements Si, Al, Fe and Ti oxides. The highest contents were Si (914.3 to 981.3 g kg-1) in the sand fractions, Al (507.9 to 543.7 g kg-1) and Fe (32.5 to 76.7 g kg-1) in the clay fractions, and Ti (18.0 to 59.0 g kg-1) in the silt fractions. The RM-XRD allowed identifying that the sand fractions are predominantly made of quartz (913.3 to 995.0 g kg-1), while the clay greatest portion is made of kaolinite (465.0 to 660.6 g kg-1) and halloysite (169.0 to 385.0 g kg-1). The main effect responsible for μ was IS (50 to 61.4%) followed by PA (28 to 40.1%) and CS (9.9 to 10.6%). By using the principal component analysis (PC-1: 57.5% and PC-2: 20.9%), the samples were differentiated through the discrimination between physical, chemical and mineralogical properties. The results obtained suggest that general information about the radiation interaction in soils can be obtained through the elemental and mineralogical analyses of their fractions.