Modified dry bean pod waste (Phaseolus vulgaris) as a biosorbent for fluorescein removal from aqueous media: Batch and fixed bed studies.

This study presents the use of dry bean pods as a solid phase for fluorescein removal from water. The non-pretreated solid phase did not display any sorption properties for the chosen dye. However, interesting sorption properties were observed following a chemical derivative treatment with nitric acid. The study was carried out using both batch and column approaches. Regarding the batch study, all parameters that influence sorption capacity, such, as pH, adsorbent mass, ionic strength, temperature and contact time, were evaluated. A sorptive capacity of 36.80 mg g-1 was obtained in the optimized condition. In the fixed column bed study, the influence of particle size, flow rate and initial concentration of the dye were evaluated through breakthrough curves and a sorptive capacity of 4.35 mg g-1 was obtained. Thermodynamic studies revealed that the adsorption is exothermic and spontaneous. Four different models, Langmuir, Freundlich, Temkin and Redlich-Patterson, were employed. The Akaike information criterion (AIC) was employed to rank the best equilibrium model, which was determined as the Freundlich isotherm. The method was applied to a real sample and the same removal rate was obtained, thus indicating its suitability to wastewater treatment.

An improved drop casting electrochemical strategy for furosemide quantification in natural waters exploiting chemically reduced graphene oxide on glassy carbon electrodes.

This work exploits the applicability of a chemically reduced graphene oxide (CRGO) modification on the electrochemical response of a glassy carbon electrode (GCE) for the first-time sensitive determination of furosemide in natural waters. The batch injection analysis (BIA) is proposed as an analytical method, where CRGO-GCE is coupled to a BIA cell for amperometric measurements. Acetate buffer (0.1 µmol L-1, pH 5.2) was used as the background electrolyte. The modification provided an increase in sensitivity (0.024 µA/µmol L-1), low limit of detection (0.7 µmol L-1), RSD (< 4%), and broad linear range (1-600 µmol L-1). Recovery tests performed in two different concentration ranges resulted in values between 89 and 99%. Recovery tests were performed and compared with high-performance liquid chromatography (HPLC) with UV-Vis detection using Student's t test at a 95% significance level, and no significant differences were found, confirming the accuracy of the method. The developed method is proven faster (169 h-1) compared with the HPLC analysis (5 h-1), also comparable with other flow procedures hereby described, offering a low-cost strategy suitable to quantify an emerging pharmaceutical pollutant. Graphical abstract.

Determination of heavy metals in activated charcoals and carbon black for Lyocell fiber production using direct solid sampling high-resolution continuum source graphite furnace atomic absorption and inductively coupled plasma optical emission spectrometry.

Reactivity and concentration of additives, especially activated charcoal, employed for the Lyocell process, enhance the complexity of reactions in cellulose/N-methylmorpholine-N-oxide monohydrate solutions. Analytical control of the starting materials is a basic requirement to know the concentration of heavy metals, which are potential initiators of autocatalytic reactions. Seven activated charcoal and two carbon black samples have been analyzed regarding their content of seven elements, Cr, Cu, Fe, Mn, Mo, Ni and V using direct solid sampling high-resolution continuum source graphite furnace AAS (SS-HR-CS GF AAS) and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acidic digestion as a reference method. The limits of detection of the former technique are 1-2 orders of magnitude lower than those of ICP OES and comparable to those of more sophisticated techniques. For iron the working range of HR-CS GF AAS has been expanded by simultaneous measurement at two secondary absorption lines (344,099nm and 344,399nm). Partial least-squares regression between measured and calculated temperatures for beginning exothermicity (T(on)) has been used to investigate the prediction capability of the investigated techniques. Whereas the ICP OES measurements for seven elements resulted in an error of prediction of 3.67%, the results obtained by SS-HR-CS GF AAS exhibited a correlation coefficient of 0.99 and an error of prediction of only 0.68%. Acceptable correlation has been obtained with the latter technique measuring only three to four elements.

Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces--A review.

The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.

Determination of Co, Cu, Fe, Mn, Ni and V in diesel and biodiesel samples by ETV-ICP-MST.

This work presents the determination of Co, Cu, Fe, Mn, Ni and V in diesel and biodiesel samples by ETV-ICP MS using emulsion sample preparation. The emulsion composition was: 1.0 g of the diesel or biodiesel sample, 2.0 mL of a 5% m/v Triton X-100 solution, 0.5 mL of HNO3 and deionized water to a 10 mL final volume. The optimized parameters were mass of carrier/modifier (1.0 microg Pd), RF power (1100 W), carrier gas flow rate (0.95 L min(-1)) and inner ETV gas flow rate (0.15 L min(-1)). The determinations were performed against aqueous solutions using 10 microg L(-1) Rh as internal standard. The accuracy of the method was verified through the analysis of the NIST 1634c reference residual fuel oil, recovery tests and comparison of the results with those obtained by GF AAS. The results were in agreement according to the t-test at a 95% confidence level. The RSD values were lower than 20%, the recoveries were between 80 and 120% and the LOD values were in the order of ng g(-1), showing the good accuracy and sensitivity of the method.

Determination of vanadium in petroleum and petroleum products using atomic spectrometric techniques.

Vanadium is recognized worldwide as the most abundant metallic constituent in petroleum. It is causing undesired side effects in the refining process, and corrosion in oil-fired power plants. Consequently, it is the most widely determined metal in petroleum and its derivatives. This paper offers a critical review of analytical methods based on atomic spectrometric techniques, particularly flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ET AAS), inductively coupled plasma optical emission spectrometry (ICP OES), inductively coupled plasma mass spectrometry (ICP-MS). In addition an overview is provided of the sample pretreatment and preparation procedures for vanadium determination in petroleum and petroleum products. Also included are the most recent studies about speciation and fractionation analysis using atomic spectrometric techniques.