Comparison of extraction and derivatization methods for fatty acid analysis in solid environmental matrixes

This study involved comparison of different extraction and derivatization methods for determining FAs in soil and in four highly organic matrixes (cattle manure, pig slurry, compost, and vermicompost), by application of a multifactor categorical design. Although some studies have been carried out regarding the application of FA analysis to highly organic matrixes, comparison and verification are still required to test which methods of extraction and derivatization of FAs function best for these matrixes. We compared three extraction methods (one in which the same extraction mixture as used in the Folch method was employed, a modification of the Bligh and Dyer method, and a microwave-assisted extraction) and two derivatization procedures (alkaline methanolysis and derivatization with trimethylsulfonium hydroxide (TMSH)). The highest yields of FAs belonging to different structural classes, and of individual FAs used as microbial biomarkers were obtained by application of the same extraction mixture as in the Folch method and use of TMSH as derivatization agent. These methods also involved a significant reduction in the complexity and time involved in sample preparation.     

Evaluation of vermicompost as bioadsorbent substrate of Pb,Ni, V and Cr for waste waters remediation using Total Reflection X-ray Fluorescence

The use of vermicompost as adsorbent substrate for removing Pb, Ni, V and Cr from waste waters is proposed. In this work, after a preliminary physical and chemical characterization of the vermicompost, the optimal parameters for the heavy metal adsorption were obtained. A synthetic multielemental solution of Pb, Cr and Ni and a solution of NH₄VO₃ for vanadium were evaluated. The optimized parameters were pH, vermicompost mass to volume ratio, agitation time and particle size of the adsorbent. A batch system was employed for the assays. The elements were determined in the supernatant solution after filtration of the substrate. An optimal pH of 4.5 was found for ion removal. The agitation time slightly influences the adsorption of Pb and Cr, but it has a high influence on the Ni and V adsorption. The highest adsorption and removal of the metals was observed for a vermicompost mass of 2 g per 500 mL using a particle size between 75 to 841 µm for Pb, Cr and Ni, and 841 till 1192 µm for V. The mean removal percentage for each element is around 95% for Pb. Ni and Cr in the multielemental synthetic sample, demonstrating a high removal capacity of the substrate. For V it was found a removal efficiency of 50%.     

Preconcentration of Cd(II) and Pb(II) Using Humic Substances and Flow Systems Coupled to Flame Atomic Absorption Spectrometry

This paper demonstrates the potential of two natural adsorbents, vermicompost and humic acid, for preconcentration of cadmium(II) and lead(II) using flow systems coupled to flame atomic absorption spectrometry (FAAS). The procedure involves the adsorption of Cd(II) or Pb(II) on these materials (using columns containing 25mg) and subsequent elution for determination by FAAS. Cadmium(II) was preconcentrated for 4min (flow rate of 4.0mLmin^–1) and eluted with 220µL of 3.0molL^–1 HNO₃. Under these conditions, preconcentration factors of 46 and 27 were obtained for vermicompost and humic acid, respectively. Except when using 1.0molL^–1 nitric acid (for humic acid), all conditions for lead(II) preconcentration were identical to those for cadmium(II), and preconcentration factors of 62 and 83 were obtained when vermicompost and humic acid, respectively, were used. The systems were stable with only slight variations in the slopes of the analytical curves (ca. 5% after 8h working period). The long-term stability shows that a minimum of 120 and 100 cycles, respectively, can be run using the same masses of vermicompost or humic acid. The detection limits for Cd(II) were 0.4 and 0.8µgL^–1 for vermicompost and humic acid respectively, while the detection limits for Pb(II) were 8.8 and 12.1µgL^–1, also for vermicompost and humic acid. The accuracy of the methods was checked by using spiked and real (certified and reference) samples. Due to the concomitant sorption of other metals leading to variable slopes for lead and cadmium determination, it was necessary to adopt the standard addition method for calibration purposes.     

Development of a flow system for the determination of cadmium in fuel alcohol using vermicompost as biosorbent and flame atomic absorption spectrometry

In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L⁻¹, a sample flow rate of 4.5 mL min⁻¹ and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 μg L⁻¹ and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 μg L⁻¹, with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 μg L⁻¹, n = 7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%.