The assessment of chlorine, fluorine, and sulfur concentrations in depth profile of drill cuttings was performed using ion chromatography after sample preparation by pyrohydrolysis. The parameters for pyrohydrolysis were optimized using a Box-Behnken design, and the established conditions were 300 mg of sample, 300 mg of V2O5, temperature of 1000 °C, reaction time of 25 min, and absorbing solution of 50 mmol L-1 NH3 + 150 mmol L-1 H2O2. The accuracy was evaluated by the analysis of certified reference materials and recovery tests, and the results showed a good agreement between determined and certified values and recoveries (89-108%). The precision (relative standard deviation (RSD) < 10%), and the limits of detection (0.5-2.5 mg kg 1) were suitable for drill cuttings analysis. The concentration of chlorine, fluorine, and sulfur in drill cuttings at different depths was at mg g-1 range, and its variation is related to the mineral composition of the samples.

This study aims to assess a new approach for concomitant valorization of two industrial wastes - raw glycerin and spent brewer’s yeast - for the bioproduction of valuable carotenoids. Microbial pigments have numerous applications in the food and cosmetic industries. First, four cultures of yeasts were screened using pure glycerol and either (NH4)2SO4 or urea as carbon and nitrogen sources, respectively. The ability of the best performing culture to accumulate carotenoids was investigated in a medium in which only wastes were supplemented as carbon and nitrogen sources. All the fermentations were carried out in 500 mL-Erlenmeyer flasks containing 150 mL of the medium. Microbial culture was incubated at 30 °C and 150 rpm for 120 h. Particularly, R. marina was the strain with the biggest potential to produce total carotenoids (up to 420 μg g-1). The four major carotenoid pigments identified by LCAPCI-MS were β-carotene, γ-carotene, torulene, and torularhodin. All fermentation assays and all the determinations were performed in triplicate. Results show that the bioprocess proposed in this work is technically and environmentally feasible, and sustainable. The simultaneous use of raw glycerin and spent brewer’s yeast for the production of carotenoids by R. marina is reported for the first time.

A fast, simple and reliable method for Hg determination in green coke and oily sludge samples by atomic fluorescence spectrometry is described. Microwave digestion and extraction procedures were evaluated for highly complex samples of coke and oily sludge. The concentrations of SnCl2 and HCl to promote Hg vapor, were optimized, as well as the concentration of KMnO4, to stabilize the Hg2+ before the atomic vapor formation. Accuracy of the method was evaluated through certified reference material, for green coke, and comparison with cold vapor atomic absorption spectrometry (CV AAS), for oily sludge. Recovery tests were also performed. Limits of detection and quantification were 0.8 and 2.6 µg kg−1, respectively. Ten green coke and nine sludge samples were analysed and Hg concentrations in coke are very low, between 0.005 and 0.065 mg kg−1, but oily sludge samples have high concentrations, ranging from 42.5 to 376.6 mg kg−1, requiring careful management.

A determinação de elementos terras raras (REE) em catalisadores gastos provenientes da indústria de petróleo é proposta. Foram testados três procedimentos de tratamento de amostra, um sem adição de HF e outros dois usando diferentes quantidades de HF e ácido bórico, além de uma etapa de evaporação assistida por radiação micro-ondas para dissolução dos fluoretos de REE. O meio contendo 1,0 mL de HF e 8,0 mL de ácido bórico foi eficiente para promover a completa digestão da amostra. Estudos foram realizados usando uma célula de reação para redução de interferências por íons poliatômicos para quatro elementos por espectrometria de massas com plasma acoplado indutivamente (ICP-MS). Material de referência certificado, TDB-1, foi utilizado para avaliar a exatidão do método aplicado a dez amostras de catalisadores. O procedimento proposto é rápido, eficiente e apresentou exatidão e precisão adequadas para 14 dos 16 analitos determinados. Testes de adição e recuperação apresentaram valores entre 87% e 101%.

The determination of rare earth elements (REE) in spent catalyst samples from oil refinery is proposed. Three sample treatment procedures were tested, one without HF and two using different amounts of HF and boric acid. A microwave evaporation step to promote the dissolution of the REE fluorides was carried out. The medium containing 1.0 mL of HF and 8.0 mL of boric acid promoted the complete digestion. Studies were carried out using a reaction cell to overcome polyatomic interferences on four elements by inductively coupled plasma mass spectrometry (ICP-MS). Certified reference material, TDB-1, was used to evaluate the method accuracy applied to ten spent catalysts. The sample treatment is fast and promotes the complete digestion of the samples and the developed procedure led to proper accuracy for 14 of the 16 determined analytes. Recovery tests presented values between 87% and 101%.

Alternatives for the removal of high-molecular weight polycyclic aromatic hydrocarbons (HWM-PAH) from soil were tested by adding fertilizer or glycerol, as well as the combination of both. Experiments were carried out for 60 days in reactors containing a HWM-PAH-contaminated soil (8030 μg kg-1), accompanied by pH monitoring, humidity control and quantification of total heterotrophic bacteria and total fungus. Fertilizer addition removed 41.6% of HWM-PAH. Fertilizer and glycerol in combination removed 46.2%. When glycerol was added individually, degradation reached 50.4%. Glycerol also promoted the increase of degradation rate during the first 30 days suggesting the HMW-PAH removal occurred through cometabolic pathways.