Wavelength dispersion X-ray fluorescence spectrometry (WDXRF) is a non-destructive technique and therefore attractive for gunshot residues (GSR) analysis. It is well known for determination of inorganic constituents of samples. However, X-ray scattering region spectral data is not commonly used, although it may provide information about organic constituents and their interactions. This work employed X-ray scattering region and inorganic elements spectral data for a better characterization of GSR. Swabs containing residues collected from the hand of people who fired (shooters group) and also from the hands of people which did not fire (control group) with guns were analyzed directly by the WDXRF. Brake pad and people who perform activities that favor the accumulation of characteristic elements of GSR on their hands were chosen to compose the control group. Principal components analysis (PCA) discriminated the GSR according to the firearm/cartridge used. However, similar GSR clustering did not occur without X-ray scatter data, showing the importance of X-ray scattering spectrum for GSR evaluation. The k-nearest neighbors (k-NN) method correctly classified all samples from shooters and control groups, employing from 1 to 5 nearest neighbors. No anomalous behavior was detected by PCA and hierarchical cluster analysis (HCA).

Biodiesel is obtained by the transesterification of vegetable oil (or fat) and alcohol, with methanol being the most used alcohol. Methanol can be replaced by ethanol; however, this alcohol acts as a surfactant in the reaction mixture, promoting a stable dispersion of the glycerol in biodiesel, which hinders the separation of the glycerol-biodiesel phases. In this study, it was found that the addition of 1% v/v water relative to the total volume of the reaction mixture expedites the separation of the phases by interrupting the emulsifying action of ethanol with an immediate separation of glycerol from biodiesel. The characterization of the produced biodiesels was performed using hydrogen nuclear magnetic resonance (1H NMR) and gas chromatography (GC). 1H NMR indicated a 96.9% conversion of triglycerides to biodiesel. The fatty acid compositions of the synthesized ethyl and methyl biodiesels determined using GC are essentially the same.

<p>Two methods for determining the iodine value in vegetable oils are described. One employs mid-infrared (mid-IR) spectroscopy and the other uses hydrogen nuclear magnetic resonance (¹H NMR). The determination of the iodine value is based on either the transmittance intensity of mid-IR signals or on the 1H NMR signal integration and multivariate calibration. Both of the methods showed adequate coefficients of determination (r² = 0.9974 and 0.9978, respectively) when compared to Wijs method, which is recommended by the norm EN 14111. A statistical comparison between the results from the proposed methods and from Wijs method shows that both instrumental methods offer equivalent results and greater precisions compared to Wijs method. The regressions obtained from the constructed models were considered statistically significant and useful for making predictions. The proposed methods present several advantages compared to Wijs method because they significantly reduce analysis time, reagent consumption and waste generation. Furthermore, an analyst can choose between the mid-IR or ¹H NMR to determine the iodine value.</p>

Em análise forense, uma pequena quantidade de um determinado material (cabelo, fibras, solo, vidro, pintura, entre outros) pode ser fundamental para elucidar a sequência de eventos em uma cena de crime ou para estabelecer a relação entre sujeitos e fatos. Existem vários exemplos de cosméticos usados como provas forenses, tais como batons e esmaltes de unhas. A composição desses esmaltes pode variar de acordo com a marca, cor e finalidade do produto. Neste trabalho, a classificação de esmaltes de unha brasileiros de acordo com a marca foi avaliada usando um espectrômetro portátil de fluorescência de raios X por energia dispersiva (EDXRF) e análise de componentes principais (PCA). A classificação não supervisionada das cinco marcas indica que a metodologia proposta pode ser uma alternativa rápida, de baixo custo e compatível com a química verde para discriminar marcas e outras características relacionadas a uma amostra de esmalte de unha, como possível evidência em cenas de crime.

In forensic analysis, a small quantity of a particular material (hairs, fibers, soils, glasses, paints, among others) can be important to elucidate the sequence of events in a crime scene or to establish the relationship among subjects and facts. There are several examples of cosmetics used as forensic evidences, such as lipsticks and nail polishes. The composition of nail polishes varies according to brand, color and purpose of the product. In this work, the separation of Brazilian nail polishes according to their brand was evaluated using a portable energy dispersive X-ray fluorescence spectrometer (EDXRF) and principal component analysis (PCA). The nonsupervised classification of five brands indicates that the proposed methodology may be a quick, low cost and green alternative to discriminate brands and other characteristics related to a nail polish sample, as possible evidence in crime scenes.

Antimony is a common catalyst in the synthesis of polyethylene terephthalate used for food-grade bottles manufacturing. However, antimony residues in final products are transferred to juices, soft drinks or water. The literature reports mentions of toxicity associated to antimony. In this work, a green, fast and direct method to quantify antimony, sulfur, iron and copper, in PET bottles by X-ray fluorescence spectrometry is presented. 2.4 to 11 mg Sb kg-1 were found in 20 samples analyzed. The coupling of the multielemental technique to chemometric treatment provided also the possibility to classify PET samples between bottle-grade PET/recycled PET blends by Fe content.