Search

An analytical method for multi-elementary determination in powder refreshment, based on sample digestion using dilute mineral acids and detection by inductively plasma coupled optical emission spectrometry (ICP OES) is proposed. Chemometric tools, such as fractional factorial design and principal component analysis (PCA) and hierarchical cluster analysis (HCA) were applied to optimize the sample preparation conditions in closed block digester, and Doehlert design for spectrometer operation. Addition and recovery tests and analyses of certified reference material were performed to evaluate the precision and accuracy, and the results confirm the reliability of the proposed method. Limits of quantification (LOQ) between 0.02 and 36 μg g−1 were obtained. The analytical method was applied for determination of 24 inorganic constituents in 20 powder refreshment samples. Calcium, K, Mg, Na, P, S and Ti presented the highest concentrations. The analytical method was adequate for the determinations of inorganic constituents in powder refreshment samples by ICP OES.

Eight petroleum samples from Potiguar Basin were submitted for determination of saturated biomarkers by gas chromatography (fingerprint), liquid chromatography (saturates, aromatics, resins and asphaltenes), gas chromatography-mass spectrometry (GC-MS), nickel and vanadium by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The geochemical parameters provided information on type of depositional paleoenvironment in which organic matter that gave rise to each oil sample and level of thermal maturation reached by generating rocks that make up the Potiguar Basin were deposited. The relationships between the stable isotopes of carbon (δ13C) and between Ni and V concentrations of each petroleum sample were also evaluated. The evaluations separated for oil samples into two distinct groups. Group 1 formed by samples P1, P2, P5 and P8, with characteristics of generating rock that was deposited in a marine hypersaline environment. Group 2 composed of samples P3, P4, P6 and P7 with freshwater lacustrine depositional paleoenvironment, which were elucidated through the geochemical parameters studied. The hierarchical cluster analysis was presented as promising chemometric tool for characterization of petroleum samples in the according to their origin of the generating rock by ratio parameters of hopane/sterane , tetracyclic polyiprenoids/diastereomers and diastereos R+S/cholestane R+S.

Submitted by Gisele Mara Hadlich (gisele@ufba.br) on 2018-02-27T13:01:30Z No. of bitstreams: 1 0103-5053-jbchs-26-05-0955.pdf: 397772 bytes, checksum: bdd15a95321b07ab2fdc9aec3dfef1fc (MD5) Made available in DSpace on 2018-02-27T13:01:30Z (GMT). No. of bitstreams: 1 0103-5053-jbchs-26-05-0955.pdf: 397772 bytes, checksum: bdd15a95321b07ab2fdc9aec3dfef1fc (MD5) A cloud-point extraction (CPE) method using the surfactant (30)p-tert-octylphenol polyoxyethylene (OPEO30) was proposed as the preceding step for the determination of polycyclic aromatic hydrocarbons (PAHs) by gas chromatography-mass spectrometry (GC-MS). Given the need for surfactant derivatization before the chromatographic analysis, the reaction conditions of coacervate derivatization were studied. The extraction process was also optimized, where surfactant concentration, temperature and time were analyzed as variables. The limits of detection obtained were between 0.02 and 0.05 µg L-1, and the recoveries of analytes were between 70 and 98%, with coefficient of variation better than 10.3%. The analytical method developed provides an efficient, precise and accurate method for the determination of the 16 priority PAHs, generating results in accordance with the USEPA 3510C method. The method was applied to the analysis of groundwater samples collected from artesian wells located at retail fuel stations. Journal of the Brazilian Chemical Society