“…Thus, in all the remaining experiments, a 0.10 mol/L hydrochloric acid was used as extracting solution. The fixed volume adopted (20 mL) has been chosen due to prior literature results which achieved easily homogeneized liquid phase of the solution and lead to higher analyte extraction in acidic medium when ultrasonic probes were used [ 23 – 26 ].…”
A sample preparation method based on ultrasound assisted-extraction (UAE) of Ca, Mg and P from swine feed has been described. The experiment was performed to cover the variables influencing the sonication process and, the method validation using standard reference material. Final solutions obtained upon sonication were analyzed by flame atomic absorption spectrometry (for Ca and Mg) and by UV–vis spectrophotometry (for P). The best conditions for metal extraction were as follows: sample mass: 100 mg in 20 mL 0.10 mol/L HCl, a particle size: <60 μm, sonication time: 5 cycles of 10 s and ultrasound power: 102 W. The UAE method was applied in digestibility assays in different piglet feeds and their results showed that it is highly comparable (P > 0.05) to the other methods used for such purposes, as block digestion, and offered a Ca, Mg and P method of quantification limit of 10.6, 12.4 and 14 mg/kg, respectively. The major advantages of the UAE method compared to other methods are the high treatment rate, low reagent usage in the extracts and, it does not generate toxic residues that might negatively affect human health and the environment, accompanied by good precision and accuracy.
“…Thus, in all the remaining experiments, a 0.10 mol/L hydrochloric acid was used as extracting solution. The fixed volume adopted (20 mL) has been chosen due to prior literature results which achieved easily homogeneized liquid phase of the solution and lead to higher analyte extraction in acidic medium when ultrasonic probes were used [ 23 – 26 ].…”
A sample preparation method based on ultrasound assisted-extraction (UAE) of Ca, Mg and P from swine feed has been described. The experiment was performed to cover the variables influencing the sonication process and, the method validation using standard reference material. Final solutions obtained upon sonication were analyzed by flame atomic absorption spectrometry (for Ca and Mg) and by UV–vis spectrophotometry (for P). The best conditions for metal extraction were as follows: sample mass: 100 mg in 20 mL 0.10 mol/L HCl, a particle size: <60 μm, sonication time: 5 cycles of 10 s and ultrasound power: 102 W. The UAE method was applied in digestibility assays in different piglet feeds and their results showed that it is highly comparable (P > 0.05) to the other methods used for such purposes, as block digestion, and offered a Ca, Mg and P method of quantification limit of 10.6, 12.4 and 14 mg/kg, respectively. The major advantages of the UAE method compared to other methods are the high treatment rate, low reagent usage in the extracts and, it does not generate toxic residues that might negatively affect human health and the environment, accompanied by good precision and accuracy.
“…Hairs were dried at 808C to constant weight (6 hours) and fixed between 2 pieces of plastic tape (Scotch MagicTape 810, USA) to make a bsandwich.Q Rectangular segments 3 mm wide and weighing 0.5 to 1.0 mg were cut along the hair sandwich starting from the proximal toward the distal end, and the Cr content was determined by solid sampling electrothermal atomic absorption spectrometry. A detailed description of the instrument and the experimental parameters are given elsewhere [59,62,63]. The accuracy of the results was checked by the hair reference sample (Chinese reference hair GBW09191), which was measured with each set of samples.…”
“…A comprehensive description of the instrument has been given elsewhere [12]. A graphite cup of type A without the inner cup was used for chromium measurements, whereas for lead and cadmium determination a cup of type B with an inner cup acting as a platform was found to be optimum.…”
Section: Apparatus and Instrumental Conditionsmentioning
The so called "tape sandwich", a novel sample-introduction technique developed for SS-ETAAS, has been employed in a study of the microheterogeneity of some biological CRM. Pb, Cd, and Cr were measured by use of a laboratory-assembled instrument with graphite-cup atomizer. Aqueous standards were found satisfactory for calibration. The average mass of sub-samples atomised was in the range 0.250-0.660 mg+/-30%. The relative sampling error found for the CRM investigated varied from 15-34%. Calculated relative homogeneity constants of the order of 4-21 mg(1/2) were obtained, and were reduced considerably by reduction of the particle size. The minimum sample sizes representative of the CRM were, with one exception, much lower (11-75 mg) than those recommended in the documentation accompanying the standards (100-200 mg). In a Chinese hair reference sample Cr data were normally distributed but the presence of nuggets was observed for Cd and Pb; this was associated with severe radial and longitudinal gradients of these elements in hair.
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