Rosângela Assis Jacques

Extraction of Grape Seed Oil Using Compressed Carbon Dioxide and Propane: Extraction Yields and Characterization of Free Glycerol Compounds

The main objective of this work was to compare the extraction of grape seed oil with compressed carbon dioxide and propane on the extraction yields and chemical characteristics of free glycerol compounds. The experiments were performed in a laboratory scale unit in the temperature range of 30 to 60 degrees C and pressures from 60 to 254 bar. The results showed that propane is a more suitable solvent for grape seed oil extraction than carbon dioxide, as higher extractions yields and a very fast kinetic of extraction were achieved with this solvent. In relation to compressed carbon dioxide extractions, both temperature and density presented a very pronounced and positive effect on the extraction yield. The oils extracted were analyzed qualitatively and quantitatively with regard to the free glycerol compounds, mainly fatty acids, ethyl, and methyl esters. The results showed that these compounds are present in low concentration in vegetable oil (<3%) and that, in general, samples extracted with propane present a smaller amount of peaks of free glycerol compounds in the oil than samples extracted with carbon dioxide.

Removal of Cu(II), Fe(III), and Cr(III) from Aqueous Solution by Aniline Grafted Silica Gel

Abstract The aniline moiety was covalently grafted onto silica gel surface. The modified silica gel with aniline groups (SiAn) was used for removal of Cu(II), Fe(III), and Cr(III) ions from aqueous solution and industrial effluents using a batch adsorption procedure. The maximum adsorption of the transition metal ions took place at pH 4.5. The adsorption kinetics for all the adsorbates fitted better the pseudo second‐order kinetic model, obtaining the following adsorption rate constants (k2): 1.233 · 10−2, 1.902 · 10−2, and 8.320 · 10−3 g · mg−1 min−1 for Cr(III), Cu(II), and Fe(III), respectively. The adsorption of these transition metal ions were fitted to Langmuir, Freundlich, Sips, and Redlich‐Peterson isotherm models; however, the best isotherm model fitting which presented a lower difference of the q (amount adsorbed per gram of adsorbent) calculated by the model from the experimentally measured, was achieved by using the Sips model for all adsorbates chosen. The SiAn adsorbent was also employed for the removal of the transition metal ions Cr(III) (95%), Cu(II) (95%), and Fe(III) (94%) from industrial effluents, using the batch adsorption procedure.

Pressurized liquid extraction of vitamin E from Brazilian grape seed oil

The goal of this paper is to optimize the pressurized liquid extraction (PLE) of vitamin E from grape seed oil from residues of the wine industry. For this purpose an experimental planning to optimize the extraction of Brazilian grape seed oil by means of PLE with hexane as solvent was applied and the results are compared with conventional methods (Soxhlet and mechanical press extraction). Vitamin E was separated and analyzed using HPLC with UV detection. This study demonstrates the ability of the PLE in extracting grape seed oil rich in vitamin E.

Pressurized liquid extraction of mate tea leaves

The objective of this work is to investigate the influence of process parameters on the pressurized liquid extraction (PLE) of Ilex paraguariensis leaves. A factorial 2(6-2) experimental design was employed using responses as the extraction yield and the chromatographic profile of the extracts. The extraction time, polarity of solvent, amount of sample, numbers of PLE cycles, flushing volume and extraction temperature were selected as independent variables (factors). Results obtained indicated that the solvent polarity was the most significant variable in the study, while the amount of sample and extraction temperature also showed significant effect. The other variables did not present significant influence in the yield of extraction. GC/MS analysis of the extract enabled the identification of saturated hydrocarbons, fatty acids, fatty acid methyl esters, phytosterols and theobromine in the extracts. Quantitative analysis of four compounds presented in the extracts (caffeine, phytol, vitamin E and squalene) was performed by the GC/MS in the SIM mode.

Characterization of naphthenic acids using mass spectroscopy and chromatographic techniques: study of technical mixtures

By the classical definition naphthenic acids (NAs) are a complex mixture of monocarboxylic acids containing one or more alkyl-substituted alicyclic rings or only aliphatic carbon chains. Based on the great interest of the oil industry in the elucidation and characterization of naphthenic acids in petrochemical samples, and the lack of efficient methodologies for the total characterization of these compounds, the goal of this study is to compare three techniques (GC/qMS, ESI-MS/MS and GC × GC/TOF-MS) for the analysis of two technical mixtures of NAs. The results presented here demonstrate the applicability of these techniques and the main advantages of each one. GC/qMS is widely used in the naphthenic acid analysis and still presents a good performance; however the ESI-MS-MS allowed a very quick analysis that provided a general profile of each sample, very useful in preliminary classification of petrochemical mixtures, while GC × GC/TOF-MS delivered a thorough evaluation of the different components of each sample. Technical mixtures analyzed showed different profiles confirmed through the three techniques applied. The mixture SA (Sigma Aldrich) presented a predominance of aliphatic acids (Z = 0) while the mixture MN (Miracema-Nuodex) was composed mainly of naphthenic monocyclic acids.

Characterization of the yerba mate (Ilex paraguariensis) volatile fraction using solid-phase microextraction-comprehensive 2-D GC-MS

The present research is focused on the use of a solid-phase microextraction-comprehensive 2-D GC methodology, in the analysis of the volatile fraction of yerba mate. Yerba mate is used for the generation of a tea-like beverage, widely consumed in South America. A rapid-scanning quadrupole mass spectrometer (qMS), employed as a detection system and operated at a 25 Hz scanning frequency, supplied high-quality mass spectra. The effectiveness of the 3-D comprehensive 2-D GC-qMS experiment was compared to that of GC-qMS analysis on the same sample. Peak identification, in both applications, was achieved through MS library matching, with the support of linear retention index data. Apart from a great increase in the number of analytes separated (approx. by a factor of 5) and identified (approx. by a factor of 3.5), the comprehensive 2-D GC-qMS approach enabled the determination of a high number of hazardous contaminants (aliphatic hydrocarbons, polycyclic aromatic hydrocarbons, and plasticizers), barely visible in the GC-qMS analysis.

Comprehensive two dimensional gas chromatography with fast-quadrupole mass spectrometry detector analysis of polar compounds extracted from the bio-oil from the pyrolysis of sawdust

In this paper it is studied the most polar fractions of bio-oil produced by fast pyrolysis of Lignocel BK40-90 (sawdust from forest timber). The biomass was submitted to the pyrolysis in an existing FCC pilot plant that was adapted for this procedure. The equipment consists of a fluidized bed reactor with nitrogen injection. The unit operates with continuous biomass feeding and continuous solids circulation. The produced bio-oil was submitted to an aqueous alkaline extraction, isolating the acidic compounds that were analyzed by one-dimensional gas chromatography and comprehensive two-dimensional gas chromatography with quadrupole mass spectrometry detection (qMS). One hundred and thirty compounds (mainly phenols and ketones) were tentatively identified in the extract, some of them by the use of retention indexes. The main differences between chromatographic techniques were the substantial increasing in the peak capacity of GC×GC and the resolution of some co-elutions that occurred in GC/qMS. It is also possible to conclude that this extract is rich in important raw materials for the chemical industry and can be used for this end.

Pré-tratamentos de melaço de cana-de-açúcar e água de maceração de milho para a bioprodução de carotenóides

This work studied the pretreatment of sugarcane molasses (CM) and corn steep liquor (CS) for the production of carotenoids by Sporidiobolus salmonicolor (CBS 2636). The acid pretreatment removed less micronutrients than that with activated carbon and led to high removals of Cu and Mn. Reduction in optical density of the prepared medium and removal of glucose from it were 22% and 7% for CM and 95% and 38% for CS, respectively. Total carotenoids obtained with substrates pretreated with acids (541 mg/L) were higher than the results obtained when the medium was treated with activated carbon (208 mg/L).

Ácidos naftênicos no petróleo

Brazilian petroleum is known by its high acidity due to the presence of acidic constituents, especially naphthenic acids (NA). The total characterization of the NA in petrochemical samples has been receiving special attention in research and comprises an analytical challenge, mainly due to the complexity of their mixtures. Gas chromatography with mass detector (GC/MS) is the technique of analysis more used, but recently comprehensive two-dimensional gas chromatography (GC × GC) has been used, due to its high resolution, peak capacity and sensitivity. The goal of this article is to discuss the techniques for sample preparation and analysis of NA in petroleum.

Extração de Al(III), Cr(III) e Fe(III) de meio etanólico usando o xerogel anilinapropilsílica

In this study, the preparation of the xerogel anilinepropylsilica is reported. The ability of the xerogel for extracting Al(III), Cr(III) and Fe(III) from ethanol was investigated at 25 oC. The xerogel adsorption capacities were obtained from the adsorption isotherms by using the batch method. Flame atomic absorption spectrometry (FAAS) was used to estimate the concentration of metal ions in solution. The adsorption affinity follows the series Cr(III) > Fe(III) > Al(III) and the maximum adsorption capacities of the metal ions were 0.61, 0.52 and 0.43 mmol g-1, respectively.