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In this work, a method for total sulphur determination in automotive gasoline using dried matrix spot sampling is proposed. The method is based on the deposition of the sample on a cellulose-based filter paper and subsequent sulphur quantification via CS diatomic molecule using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The sample deposition was carried out, along with the chemical modifier, on a 20-mm filter paper disc previously adapted into a polytetrafluoroethylene (PTFE) mould. The liquid phase was removed by heating the PTFE mould, and then the gasoline sample-embedded filter paper was punched in smaller discs (procedure A) or pulverised (procedure B) before the analyses. The mixture of Pd and Mg was used as chemical modifier to stabilise the sulphur compounds on the filter paper and on the graphite furnace. All the calibration curves constructed using seven different sulphur-containing compounds had a coefficient of determination higher than 0.995 and a linear range from 2 to 150 mg kg-1 S. By using the optimised conditions, the best characteristic mass, limits of detection and quantitation were 6 ng, 0.6 and 1.8 mg kg-1, respectively. The two sampling procedures (A and B) were evaluated for real samples, and procedure B was chosen since it markedly improved the precision. Using this procedure, satisfactory recovery values from 95 to 106% were obtained in the spike-recovery tests. In addition, the S concentrations for the certified reference materials were not statistically different from the certified values at 95% confidence level. Sulphur concentrations from 20 to 46 mg kg-1 were found in the six analysed gasoline samples, and these values were statistically assessed using a reference method (ASTM 5453). Spectral interference caused by MgF and MgCl diatomic molecules was observed and investigated.

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In this work a simple and practical method for the determination of Pb and Ni in automotive gasoline by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry was investigated. In the proposed method, disks of filter paper were used to pre-concentrate and store Pb, Ni and other trace elements from automotive gasoline samples. For this, a volume of sample was deposited and dried out on a filter paper disk previously adapted into a polytetrafluoroethylene mold, and then the gasoline-embedded filter paper was either cut into small pieces or pulverised and introduced directly into the graphite furnace for trace element determination. Temperature program, use of chemical modifier, chromatographic effect and volume of sample were investigated. Calibration curves using organic and inorganic standards of the analytes as well as external and internal calibration methods were evaluated. Using optimised conditions, characteristic masses and limits of detection of 6 and 11 pg, and 0.5 and 2.1 µg L-1 were found for Pb and Ni, respectively. The accuracy of the method was evaluated with spike-recovery tests and a certified reference material of wear lubricant oil. The spike-recovery tests were accomplished for 9 samples and the best results were obtained with the pulverised filter paper. A second method that employs a transversely heated filter atomiser was applied as a comparative one. The filter paper was shown to be a simple and inexpensive tool for storage and transportation of gasoline samples, and it allowed the pre-concentration of the analytes, since a larger volume of sample can be dried out on it.

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BACKGROUND: Microalgae have been used as food supplements owing to their high protein, polyunsaturated fatty acid and carotenoid contents. As different carotenoids have distinct properties and the carotenoid composition of microalgae has been poorly explored in the literature, this study determined the complete carotenoid composition of two microalgae species, Heterochlorella luteoviridis and Dunaliella tertiolecta, using high-performance liquid chromatography coupled with diode array detection and tandem mass spectrometry (HPLC-DAD/MS2 ). Additionally, the proximate composition and major minerals were evaluated. RESULTS: The carotenoid composition of the two microalgae was similar, with 13 carotenoids being found in H. luteoviridis and 12 in D. tertiolecta. The major carotenoids were all-trans-lutein (1.18 mg g-1 in H. luteoviridis and 1.59 mg g-1 in D. tertiolecta), all-trans-violaxanthin (0.52 mg g-1 in H. luteoviridis and 0.45 mg g-1 in D. tertiolecta) and all-trans-ß-carotene (0.50 mg g-1 in H. luteoviridis and 0.62 mg g-1 in D. tertiolecta). All-trans-lutein was the predominant carotenoid in both microalgae, representing around 40% (mass fraction) of the total carotenoids. The lutein content found in these microalgae was significantly higher (2-40 times) than that in other important food sources of lutein (e.g. parsley, carrot, red pepper and broccoli). CONCLUSION: The microalgae H. luteoviridis and D. tertiolecta are excellent sources of lutein that could be commercially exploited by the food and pharmaceutical industries. Moreover, it was confirmed that both microalgae are good sources of protein, lipids and calcium. © 2016 Society of Chemical Industry.

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Organotin compounds are highly versatile group of organometallic chemicals used in industrial and agricultural applications. Their endocrine-disrupting effects are well known and their extensive uses as biocide materials, e.g., in antifouling paints, for many years have led to serious environmental problems. So far, attention has mainly been given to tributyltin pollution in water, sediments, and marine organisms because of its highly toxic effects and high accumulation levels at very low concentrations. In this study, we will focus on the conversion of tributyltin after it is absorbed by zebrafish eleutheroembryos, presented here as an alternative model to adult fish for describing bioconcentration. A simplified analytical extraction procedure based on the use of an assisted ultrasonic probe and derivatization by ethylation, followed by gas chromatography with a flame photometric detector (GC-FPD) is proposed. This classical methodology for organotin determination has been validated by inductively coupled plasma mass spectrometry (ICP-MS) and Zeeman graphite furnace atomic absorption spectrometry (ZGF-AAS) in terms of total tin content. The speciation analysis results show that zebrafish eleutheroembryos absorb high amounts of tributyltin and convert it into monobutyltin and likely in inorganic tin.

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In this work a simple method was described for selective extraction of benzoic acid from landfill leachate samples. The samples were submitted to solid-phase extraction (SPE) with XAD-4 resin as the stationary phase and ion-exchange chromatography (IEC) using the ion-exchange resin Amberlyst A-27. The instrumental analysis was performed by gas chromatography with mass spectrometric detection (GC-MSD). Benzoic acid was isolated, identified and quantified. The extraction process is rapid, simple and of low cost. It was also environmental friendly, that is, it was used a minimum amounts of hazardous organic solvents and produced also minimum quantities of residues.

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In this work, preparative liquid chromatography was used for the separation of the nitrogen compounds in a sample of heavy gas oil from a Brazilian petroleum. Initially it took place a pre-fractionation by neutral aluminium oxide and the compounds were separated in different classes such as: hydrocarbons, resins (compounds of low molecular mass and intermediate polarity) and asphalthenes (polar compounds with high molecular mass). A comparison of the fraction of resins was performed by re-fractionating with modified silica (with potassium hydroxide and hydrochloric acid), or with ion exchange resins (Amberlyst A-27 and A-15), being isolated the basic and neutral compounds, that were analyzed by GC-MS in the scan and selected ion monitoring modes. Quinolines, benzoquinolines, tetrahydroquinolines were found in the basic fraction and carbazoles derivatives were found in the neutral fraction.

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