Nívia M.M. Coelho

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 microg L(-1) and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 microg L(-1), with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 microg 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%.

Determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line system coupled to FAAS

In this study a new method for determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line preconcentration system coupled to flame atomic absorption spectrometry (FAAS) was developed. Flow and chemical variables of the proposed system were optimized through multivariate designs. The limit of detection for cadmium was 5.50microg L(-1) and the precision was below 2.3% (35.0microg L(-1), n=9). The analytical curve was linear from 5 to 150microg L(-1), with a correlation coefficient of 0.9993. The developed method was successfully applied to spiked alcohol fuel, and accuracy was assessed through recovery tests, with recovery ranging from 97.50 to 100%.

Characterization and use of Moringa oleifera seeds as biosorbent for removing metal ions from aqueous effluents

Moringa oleifera seeds were investigated as a biosorbent for removing metal ions from aqueous effluents. The morphological characteristics as well as the chemical composition of M. oleifera seeds were evaluated using Fourier Transform Infrared (FT-IR) Spectroscopy, Thermogravimetric Analysis (TGA), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The FT-IR spectra showed the presence of lipids and protein components. Scanning electron micrographs showed that Moringa seeds have an adequate morphological profile for the retention of metal ions. The results suggest that M. oleifera seeds have potential application in Cd(II), Pb(II), Co(II), Cu(II) and Ag(I) decontamination from aqueous effluents.

Determination of arsenic compounds in beverages by high-performance liquid chromatography-inductively coupled plasma mass spectrometry.

Arsenic compounds including arsenous acid (As(III)), arsenic acid (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were separated by high-performance liquid chromatography (HPLC) and detected by inductively coupled plasma mass spectrometry (ICP-MS). A Hamilton PRX-100 anionic-exchange column and a pH 8.5 K(2)HPO(4)/KH(2)PO(4) 5.0x10(-3)molL(-1) mobile phase were used to achieve arsenic speciation. The separation of arsenic species provided peaks of As(III) at 2.75min, DMA at 3.33min, MMA at 5.17min and As(V) at 12.5min. The detection limits, defined as three times the standard deviation of the lowest standard measurements, were found to be 0.2, 0.2, 0.3 and 0.5ngmL(-1) for As(III), DMA, MMA and As(V), respectively. The relative standard deviation values for a solution containing 5.0mugL(-1) of As(III), DMA, MMA and As(V) were 1.2, 2.1, 2.5 and 3.0%, respectively. This analytical procedure was applied to the speciation of arsenic compounds in drinking (soft drink, beer, juice) samples. The validation of the procedure was achieved through the analysis of arsenic compounds in water and sediment certified reference materials.

Moringa oleifera Lam. seeds as a natural solid adsorbent for removal of AgI in aqueous solutions

This work describes the sorption potential of Moringa oleifera seeds for the decontamination of AgI in aqueous solutions. Infrared spectroscopy was used for elucidating possible functional groups responsible for uptaking AgI. Sorption studies using AgI standard solutions were carried out in batch experiments as functions of adsorbent mass, extraction time, particle size and pH. The AgI was quantified before and after the removal experiments using flame atomic absorption spectrometry. Furthermore, based on adsorption studies and adsorption isotherms applied to the Langmuir model, it was possible to verify that M. oleifera seeds present a high adsorption capacity. The optimum conditions were: 2.0 g of adsorbent with particle size of 75-500 µm, 100 mL of 25.0 mg L-1 AgI, extraction time of 20 min and pH at 6.5. The results show that Moringa oleifera seeds can be used for removing AgI in aqueous solutions.

Determination of arsenic species in rice samples using CPE and ETAAS.

A highly sensitive and selective procedure for the determination of arsenate and total arsenic in food by electrothermal atomic absorption spectrometry after cloud point extraction (ETAAS/CPE) was developed. The procedure is based on the formation of a complex of As(V) ions with molybdate in the presence of 50.0 mmol L(-1) sulfuric acid. The complex was extracted into the surfactant-rich phase of 0.06% (w/v) Triton X-114. The variables affecting the complex formation, extraction and phase separation were optimized using factorial designs. Under the optimal conditions, the calibration graph was linear in the range of 0.05-10.0 μg L(-1). The detection and quantification limits were 10 and 33 ng L(-1), respectively and the corresponding value for the relative standard deviation for 10 replicates was below 5%. Recovery values of between 90.8% and 113.1% were obtained for spiked samples. The accuracy of the method was evaluated by comparison with the results obtained for the analysis of a rice flour sample (certified material IRMM-804) and no significant difference at the 95% confidence level was observed. The method was successfully applied to the determination of As(V) and total arsenic in rice samples.

Bioremediation of Waters Contaminated with Heavy Metals Using Moringa oleifera Seeds as Biosorbent

Water is not only a resource, it is a life source. It is well established that water is important for life. Water is useful for several purposes including agricultural, industrial, household, recreational and environmental activities. Despite its extensive use, in most parts of the world water is a scarce resource. Ninety percent of the water on earth is seawater in the oceans, only three percent is fresh water and just over two thirds of this is frozen in glaciers and polar ice caps. The remaining unfrozen freshwater is found mainly as groundwater, with only a small fraction present above ground or in the air. Thus, almost all of the fresh water that is available for human use is either contained in soils and rocks below the surface, called groundwater, or in rivers and lakes.

Removal of BTEX from aqueous solution using Moringa oleifera seed cake

In this study, the removal of BTEX (benzene, toluene, ethylbenzene, p-xylene and o-xylene) from aqueous solution using Moringa oleifera seed cake (MOSC) was investigated. The effect of parameters such as contact time, pH and initial BTEX concentration were studied to optimize the conditions for maximum removal. Maximum removal values of 75±1%, 85±2%, 86±2%, 88±2% and 87±1% were obtained for benzene, toluene, ethylbenzene, p-xylene and o-xylene, respectively, at pH 7.0, with a 20 min contact time for an adsorbent dose of 10 g L−1 of 1 mg L−1 BTEX concentration. The adsorption data fitted the Langmuir and Freundlich adsorption isotherms. The capacity of MOSC to adsorb BTEX was compared with that for a commercial activated carbon. The results from the two methods were not significantly different (judged by t-test at 95% confident interval). A low cost, easy purchase and the satisfactory experimental results indicated that MOSC is a promising natural material for the removal of BTEX from aqueous solution.

Removal of Ni(II) from aqueous solution using Moringa oleifera seeds as a bioadsorbent.

Metal contaminants are generally removed from effluents by chemical and physical processes which are often associated with disadvantages such as the use of toxic reagents, generation of toxic waste and high costs. Hence, new techniques have been developed, among them the study of natural adsorbents, for instance, the use of Moringa oleifera seeds. The potential of M. oleifera seeds for nickel removal in aqueous systems was investigated. The seeds utilized were obtained from plants grown in Uberlândia/Brazil. After being dried and pulverized, the seeds were treated with 0.1 mol/L NaOH. Fourier transform infrared spectroscopy, scanning electron microscopy and thermogravimetric analyses were used for the characterization of the material. Using the optimized methodology (50 mL of 4.0 mg/L Ni(II), pH range of 4.0-6.0, agitation time of 5 min and adsorption mass of 2.0 g) more than 90% of Ni(II) could be removed from water samples. The sorption data were fitted satisfactorily by the Langmuir adsorption model. Evaluation applying the Langmuir equation gave the monolayer sorption capacity as 29.6 mg/g. The results indicate that this material could be employed in the extraction of nickel, considering its ease of use, low cost and environmental viability, which make it highly attractive for application in developing countries.

Evaluation of vermicompost as a raw natural adsorbent for adsorption of pesticide methylparathion

The assessment of vermicompost (VC) as a low-cost and alternative adsorbent for the removal of the pesticide methylparathion (MP) from an aqueous medium has been investigated by batch and column experiments. Parameters related to MP adsorption, i.e. equilibrium time (61.5 min) and adsorption pH (6.8) were optimized by using Doehlert design. The initial and final MP concentrations after adsorption assays were determined by square-wave adsorptive cathodic stripping voltammetry using an electrode composed of a multiwalled carbon nanotube dispersed in mineral oil. Batch adsorption experimental data were fitted to the Langmuir and Freundlich isotherm adsorptions, and a very good fit to the Langmuir linear model, giving a maximum adsorption capacity (MAC) of 0.17 mg g−1. This result was very similar to that obtained with the column experiments. In order to evaluate the MP desorption from column packed VC, 100.0 ml of nitric acid solution (pH 3.0) has been percolated through material. No leaching of MP was observed, thus confirming the strong interaction between MP and VC. The satisfactory MAC obtained and low cost makes the VC a reliable natural material for the removal of MP from aqueous effluents.