The morbidity and mortality, especially regarding elders and children, caused by the atmospheric particulate matter (PM) have increased over the last decades the number of studies concerned on the identification of PM sources. Source apportionment models are widely used for the air quality management, modeling source contributions based on the physical and/or chemical composition of PM at the receptor. Among the most diverse analytical techniques that can be used for PM characterization, energy dispersive X-ray fluorescence (EDXRF) and resonant synchrotron X-ray diffraction (RSr-XRD) appear to be useful techniques for the elucidation of complex environmental problems. In this work, PM samples from the outer area of an industrial site were collected from 2016 to 2017 and analyzed by EDXRF and RSr-XRD for elemental and crystallographic characterization. The results showed that only the elemental analysis used as receptor models input data do not provide satisfactory results due to the similarity between the chemical source profiles, which minimize the sensibility of the receptor model (PMF). RSr-XRD results showed to be good complementation, helping to identify the contributions of specific sources in a region with great complexity. The RSr-XRD analysis determined some crystalline phases such as α-Fe 2 O 3 , FeS 2 , and BaTiO 3 showing to be associated with specific sources, acting as specific source markers. RESUMOA morbidade e mortalidade, principalmente em idosos e crianças, causada pelo material particulado atmosférico (MP), aumentou nas últimas décadas o número de estudos preocupados com a identificação de fontes de MP. Os modelos de contribuição de fonte são amplamente utilizados para o gerenciamento da qualidade do ar, modelando contribuições de fontes baseadas na composição física e/ou química de PM no receptor. Entre as mais diversas técnicas analíticas que podem ser usadas para caracterização de PM, as técnicas de fluorescência de raios-X por energia dispersiva (EDXRF) e difração ressonante de raios-X por luz sincrotron (RSr-XRD) parecem ser úteis para a elucidação de problemas ambientais complexos. Neste trabalho, amostras de MP da área externa de um sítio industrial foram coletadas de 2016 a 2017, e analisadas por EDXRF e RSr-XRD para caracterização elementar e cristalográfica. Os resultados mostraram que apenas a análise elementar utilizada como modelo de entrada de dados dos receptores, não fornece resultados satisfatórios devido à semelhança entre os perfis das fontes químicas, o que minimiza a sensibilidade do modelo de receptor (PMF). Os resultados do RSr-XRD mostraram-se uma boa complementação, ajudando a identificar as contribuições de fontes específicas em uma região com grande complexidade. A análise por RSr-XRD determinou algumas fases cristalinas, como α-Fe2O3, FeS2 e BaTiO3, mostrando-se associadas a fontes específicas, podendo atuar como marcadores de fontes específicos.

X-ray fluorescence (XRF) has been widely used in the analysis of the inorganic/metallic composition of samples in the most diverse areas of science. Among some aspects of the XRF principle, X-ray Fluorescence by Dispersive Energy (EDXRF) stands out, due to its low analytical cost, analytical simplicity and the almost non-existent need of preparation and manipulation of the samples previous the analysis. Several variables are related to the fundamental parameters, the method used to quantify the elemental composition of samples analyzed by XRF, as a way of correcting matrix effects that occur inside the samples. Since studied the variables influencing the matrix effect, an adequate form of quantification of the samples can be performed by means of the construction of calibration curves. In the present study, calibration curves were made for the quantification of samples analyzed by EDXRF, using calibration standards with elements deposited in Mylar® films, for 32 elements varying from Na (Z = 11) to Nd (Z = 60). All analyses were performed on a Shimadzu spectrophotometer, model EDX-720/800HS. The results show the quality of the curves obtained for elements separated by groups of atomic number, in which the curves presented coefficients R equal or superior to 0.89. RESUMOA fluorescência de raios X (XRF) tem sido amplamente utilizada em análises da composição