Determination of Cl and S in crude oil by ICP-OES after sample digestion by microwave-induced combustion in disposable vessels.

A simple, fast and promising sample preparation method based on microwave-induced combustion in disposable vessels (MIC-DV) was developed for Cl and S determination in crude oil by inductively coupled plasma optical emission spectrometry (ICP-OES). The MIC-DV consists of a new approach of conventional microwave-induced combustion (MIC). For the combustion, crude oil was pipetted on a disk of filter paper and placed on a quartz holder, followed by the addition of igniter solution (40 µL of 10 mol L-1 NH4NO3). The quartz holder was inserted into a commercial 50 mL disposable polypropylene vessel containing the absorbing solution, which was then inserted in an aluminium rotor. The combustion occurs under atmospheric pressure in a domestic microwave oven not compromising the operator's safety. The following parameters of combustion were evaluated: type, concentration and volume of absorbing solution, sample mass and the possibility of performing consecutive combustion cycles. Using MIC-DV, up to 10 mg of crude oil were efficiently digested, using 2.5 mL of ultrapure H2O as absorbing solution. Moreover, up to 5 consecutive combustion cycles were possible without analyte losses, reaching a total sample mass of 50 mg. The MIC-DV method was validated according to Eurachem Guide recommendations. Results obtained for Cl and S by MIC-DV were in agreement with those obtained using conventional MIC, as well as those obtained for S in a certified reference material of crude oil (NIST 2721). Analyte spike recovery experiments were performed and recoveries at three concentration levels ranged from 99 to 101% for Cl and from 95 to 97% for S, indicating a good accuracy. The limit of quantification achieved by ICP-OES after MIC-DV were 73 and 50 µg g-1 for Cl and S respectively, applying 5 consecutive combustion cycles.

Determination of trace elements in Sergio mirim: an evaluation of sample preparation methods and detection techniques.

In this work, some trace elements (As, Cd, Cr, Cu, and Pb) were determined for the first time in the crustacean Sergio mirim (Decapoda: Thalassinidea: Callianassidae) from Southern Coast (Rio Grande, RS) of Brazil. The trace element determination was carried out by graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different microwave radiation-based sample digestion methods were evaluated. The analyte concentration ranged from 1.45 to 3.70 µg g-1 for As, 0.615 to 0.942 µg g-1 for Cd, 0.884 to 7.20 µg g-1 for Cr, 122 to 275 µg g-1 for Cu, and 0.390 to 0.916 µg g-1 for Pb. The limits of quantification for As, Cd, Cr, Cu, and Pb were 0.12, 0.01, 0.16, 0.92, and 0.06 µg g-1, respectively. The accuracy was evaluated by results comparison between GF AAS and ICP-MS techniques, as well as by analysis of certified reference materials of fish muscle and oyster tissue, with agreement from 92 to 108%. The feasibility of using Sergio mirim as a promising environmental bioindicator candidate was evaluated, since that it is an abundant organism in the studied area (South cost of Brazil) as well as in other places around the world.

Determination of cadmium and lead at sub-ppt level in soft drinks: An efficient combination between dispersive liquid-liquid microextraction and graphite furnace atomic absorption spectrometry.

A DLLME method for extraction and preconcentration of Cd and Pb from soft drinks and further determination by GF AAS was developed. Important parameters of DLLME such as the type and volume of dispersive and extraction solvents, concentration of DDTC (complexing agent) and pH were evaluated. Better results were obtained using 500µL of acetone for Cd and 700µL of acetonitrile for Pb as dispersive solvents, 60µL of CCl4 as extraction solvent for both analytes and 500µL of 1.5% DDTC solution. Accuracy was evaluated by recovery assays and ranged from 91 to 113% for Cd and from 95 to 108% for Pb, with RSD below 10 and 7%, respectively. The LODs were 0.006 and 0.072ngL-1 for Cd and Pb, respectively. The optimized method was applied for the determination of Cd and Pb in soft drinks with different brands and flavours.

Simple and fast method for iron determination in white and red wines using dispersive liquid-liquid microextraction and ultraviolet-visible spectrophotometry.

This work reports the development of a method for Fe extraction in white and red wines using dispersive liquid-liquid microextraction (DLLME) and determination by ultraviolet-visible spectrophotometry. For optimization of the DLLME method, the following parameters were evaluated: type and volume of dispersive (1300 µL of acetonitrile) and extraction (80 µL of C(2)Cl(4)) solvents, pH (3.0), concentration of ammonium pyrrolidinedithiocarbamate (APDC, 500 µL of 1% m/v APDC solution), NaCl concentration (not added), and extraction time. The calibration curve was performed using the analyte addition method, and the limit of detection and relative standard deviation were 0.2 mg L(-1) and below 7%, respectively. The accuracy was evaluated by comparison of results obtained after Fe determination by graphite furnace atomic absorption spectrometry, with agreement ranging from 94 to 105%. The proposed method was applied for Fe determination in white and red wines with concentrations ranging from 1.3 to 4.7 mg L(-1).