Microwave-induced combustion for further determination of potentially toxic elements in honey by ICP-MS.

Microwave-induced combustion (MIC) was proposed in this study for honey decomposition aiming for As, Cd, Hg, and Pb determination by inductively coupled plasma mass spectrometry (ICP-MS). Sample mass (up to 1.0 g), absorbing solution (0.5 to 14.4 mol L-1 HNO3, and H2O), heating program, and combustion aids were evaluated. The Eurachem guidelines were used for method validation. The proposed method enabled combustion of a high sample mass (0.8 g of honey, with 0.4 g of microcrystalline cellulose and 100 µL of 6 mol L-1 NH4NO3) using 6 mL of an absorbing solution consisting of 1 mol L-1 HNO3, which resulted in low residual carbon in solution (< 25 mg L-1). Honey samples from different geographical origins were analyzed. Results showed no significant difference in comparison to other two microwave decomposition methods, based on microwave-assisted wet digestion with single reaction chamber (MAWD-SRC) and microwave-assisted wet digestion (MAWD). Standard addition experiments resulted in recoveries higher than 98%. The limits of detection ranged from 1.10 (As) to 4.60 ng g-1 (Pb). In addition to using only diluted reagents and resulting in digests virtually free of interferences, the proposed method was faster (< 30 min) than most of those presented in the literature.

Development of an eco-friendly sample preparation protocol for metal determination in food samples: an oxygen pressurized single reaction chamber using diluted nitric acid.

Many efforts have been recently made to improve the digestion efficiency by using powerful equipment or by using an auxiliary reagent. In this work, an alternative method is reported, which explores a digestion system based on a single reaction chamber (SRC) technology pressurized with O2 for reducing the amount of acid, without impairing the digestion efficiency. Before digestion, the system was pressurized with compressed air (20 bar, 20% O2) while the temperature was evaluated from 180 up to 270 °C. The procedure was also carried out under O2 pressure (20 bar). For each temperature several acid concentrations were evaluated (0.1 to 3 mol L-1 HNO3), being possible to correlate the effectiveness of each acid concentration with temperature. The proposed method was applied to the simultaneous digestion of several organic matrices with variable content of fat, protein, and carbohydrate (whole milk powder, bovine liver, parsley, and linseed). The residual carbon content was lower than 4% (C lower than 200 mg L-1 in digests), showing the high digestion efficiency of the proposed approach. Up to 250 mg of all food matrices were digested using a sub-stoichiometric amount of HNO3 (1 mol L-1 solution), which was only achieved due to the use of O2 as an auxiliary reagent. Barium, Ca, Cu, Fe, K, Mg, Mn, Na, Sr, and Zn were determined by ICP-OES, and the accuracy was better than 95% for standard reference materials of corn bran, whole milk powder, and bovine liver. It is an important feature, being in agreement with green chemistry recommendations because very low amounts of reagents are required for sample digestion, as well as low amounts of residues are generated.

Environmental and human health risks associated with exposure to hazardous elements present in urban dust from Barranquilla, Colombian Caribbean.

Urban dust is a mixture of deposited particles from different sources usually linked to potentially toxic elements (PTEs). Despite the industrialization of many South American countries, little is known about the impact of particulate matter in large cities; these data are necessary to promote environmental policies aiming to protect human health. The main objective of this work was to evaluate the particle size distribution, composition, and environmental and human health risks of settled dust particles from Barranquilla, a Colombian Caribbean industrialized area. Trace elements were analyzed by inductively coupled plasma-mass spectrometry from 35 different sites, covering all city areas. Dust was mostly composed of 10-to-70-µm particles. The average concentrations of V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Mo, Ag, Cd, Sn, Sb, Pb, and Bi were above background. High spatial heterogeneity was observed for Cu, Zn, As, Se, Mo, Ag, Sn, Sb, and Bi. Concentration factors suggest that urban dusts are extremely contaminated by Zn and Cu. The ecological risk associated with specific elements decreased in the order Cd > Cu > As > Hg > Pb > Ni > Co ≈ Zn ≈ Cr, and the contamination load index showed that 91% of the samples are polluted by PTEs. Although the carcinogenic risks of Cr, Ni, As, Co, and Cd were low, chronic exposure to several PTEs may affect quality of life. Educational programs, as well as monitoring and greater control on traffic, industry, and construction activities are needed to protect environmental and human health.

Determination of Cl, Br and I in granola: Development of an accurate analytical method using ICP-MS.

Microwave-induced combustion (MIC) system for further Cl, Br, and I determination in granola by inductively coupled plasma mass spectrometry (ICP-MS) was proposed. A high sample mass of granola was pressed as pellets and inserted into the proposed MIC system. Water and NH4OH were evaluated as absorbing solutions. The accuracy was estimated by the analysis of two certified reference materials and also by spike recoveries. Using the optimized conditions (zirconium ball milling, 1 g of granola and 6 mL of 50 mmol L-1NH4OH), the agreement with the certified values ranged from 94 to 98% and recoveries higher than 95% were obtained. Low carbon concentration in digests (<25 mg L-1) was achieved, minimizing interferences by ICP-MS. Blanks were negligible and only diluted solutions were required. The concentration in samples ranged from 322 to 896, 0.618 to 0.980 and < 0.002 to 0.181 µg g-1 for Cl, Br and I, respectively.

Determination of halogens and sulfur in honey: a green analytical method using a single analysis.

The halogen determination is important in view of their biological and environmental roles, but their determination has still been considered a challenge, especially at low concentrations. Therefore, a method for honey decomposition using microwave-induced combustion (MIC) combined with ion chromatography and conductimetric detection (for Cl, F, and S determination) or mass detection (for Br and I determination) (IC-CD-MS) is proposed. Trueness was evaluated by adding reference materials (RMs) or a standard solution in the sample. By using 50 mmol L-1 NH4OH as the absorbing solution, recoveries for all analytes were between 94 and 103%, in both tests. Moreover, no statistical difference (t test, confidence level of 95%) was observed for the results obtained by IC in comparison with those obtained by inductively coupled plasma optical emission spectroscopy (Cl and S) and by inductively coupled plasma mass spectrometry (Br and I). Finally, the proposed method was applied to 19 honey samples from different origins. The concentrations ranged from < 0.45 to 2.39 mg kg-1 (Br), 21.8 to 671 mg kg-1 (Cl), and 11 to 154 mg kg-1 (S), while the F and I concentrations were below that their quantification limits (LOQs) in all analyzed samples. The LOQs for Br, Cl, F, I, and S were 0.45, 21, 3.7, 0.077, and 8.7 mg kg-1, respectively. The MIC method provided a compatible solution to IC for the halogen and S determination in honey by a single analysis. Graphical abstract.

New possibilities for pharmaceutical excipients analysis: Combustion combined with pyrohydrolysis system for further total chlorine determination by ICP-OES.

An alternative method for the determination of total chlorine content in hydroxypropyl cellulose (HPC) was applied, combining a recently developed system based on a combustion step followed by pyrohydrolysis reaction. Using this approach it the determination of total chlorine by inductively coupled plasma optical emission spectrometry (ICP-OES) without interferences was feasible. It overcame the limitations of European Pharmacopoeia (EP) method for HPC analysis regarding to the inability to determine total chlorine in HPC, once some chlorine compounds (e.g., chloroform) that can not be identified by the official method (EP). The following parameters of combustion and pyrohydrolysis were evaluated: absorbing solution, sample mass, the use of powdered silica as retardant of combustion, oxygen flow rate and reaction time. Reference values for total chlorine were obtained after digestion using microwave-induced combustion and determination by ion chromatography (IC). Microwave-assisted extraction (MAE) was also investigated for Cl extraction. The accuracy of the proposed method was also evaluated by analyte recovery tests (agreement of 95-103%), as well as by the analysis of certified reference materials (CRMs). The agreement with the certified values was higher than 95% and the limit of quantification (LOQ) was 50 µg g-1. Up to 500 mg of sample were efficiently digested by the proposed method in 5 min (dissolved carbon in digests was below 50 mg L-1). Total chlorine content in samples of modified cellulose ranged from 284 to 576 µg g-1. Despite the relatively high chlorine content in all samples, the concentration was lower than the maximum limit allowed by the EP for HPC (0.5%).

Continuous flow electrocoagulation in the treatment of wastewater from dairy industries.

Dairy industry wastewater contains high levels of organic matter, consisting mainly of fat, protein and products of their partial microbial decomposition. In the present study, the use of continuous electrocoagulation is proposed for the primary treatment of dairy wastewater. The electrochemical treatment was carried out in a continuous flow cell with aluminum electrodes. The influence of the voltage, the distance between the electrodes and the hydraulic residence time (HRT) on the process performance was assessed, by measuring the removal of color, turbidity, total organic carbon (TOC) and chemical oxygen demand (COD). The optimum voltage, distance between the electrodes and HRT were 10 V, 1 cm and 90 min, respectively, yielding a current density of 13.3 A.m(-2). Under these conditions, removal of color, turbidity, TOC and COD were 94%, 93%, 65% and 69%, respectively, after a steady state was reached in the continuous flow reactor.