No abstract

A spark discharge system was coupled to laser-induced breakdown spectroscopy (SD-LIBS) to improve sensitivity in the determination of P in fertilizers. A LIBS system consisting of a Q-switched Nd:YAG laser operating at 1064 nm and emitting pulses at 50 mJ with a fluence of 70 J cm −2 at the focal point was used. Results of preliminary experiments suggested that the most appropriate wavelength to measure P was the P (I) line at 214.9 nm, which did not show interferences by Fe, Cu and Zn. The electrical discharge was provided by a homemade highvoltage electronic circuit consisting of two cylindrical tungsten electrodes at the optimized output voltage of 4.5 kV, with tips arranged at the optimal distances of 4 mm between them and 2 mm above the sample surface. To minimize the expected matrix effects calibration standards of P 2 O 5 in the range of 4.8 and 33.3% were prepared by mixing various amounts of a phosphate rock reference material (SRM-120c) with a mixture of CaCO 3 , CaSO 4 , (NH 2 ) 2 CO and KCl at a 1:1:1:1 mass ratio. The calibration curves obtained at a 4.5 kV SD-LIBS output voltage showed correlation coefficients ≥0.993, RSD ≤8% and LOQ 5.3% (m/m) P 2 O 5 . Data obtained by analyzing commercial samples by the proposed system were in good agreement, at 95% confidence level, with those obtained by using high-resolution continuum-source flame atomic absorption spectroscopy.

Spectra of diatomic molecules are rich in fine structures which may be used for different analytical applications in high-resolution continuum source molecular absorption spectrometry (HR-CS MAS).

Establishing fast, simple, low-cost, and efficient sample preparation procedures to determine elements in foodstuffs is a relevant aspect for nutritional and health purposes. For this reason, the recently proposed closed-vessel conductively heated digestion system (CHDS) was evaluated for the digestion of milk powder, chocolate powder, and soluble coffee samples aiming for Ca, Cu, Fe, K, Mg, Mn, Na, and Zn determinations by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and Cd, Mo, and Se determinations by inductively coupled plasma mass spectrometry with tandem configuration (ICP-MS/MS). The accuracy was evaluated by analyzing two milk certified reference materials digested by the CHDS and a microwave oven for comparison. When using the CHDS, recoveries for the analytes varied from 91 to 104 %. For microwave digestions, recoveries within the 94-109 % intervals were obtained. The method was then applied to the samples. For comparative purposes, the analytes were also determined in the samples after microwave digestion, and the results between the two digestion systems showed no differences based on a paired t test at a 95 % confidence level. Similar analytical blanks were obtained because quartz digestion tubes were used in both digestion systems. The CHDS with quartz tubes is an interesting alternative for laboratories dedicated to large-scale routine analysis because volatile elements usually found in very low concentrations in food samples such as Cd and Se can also be determined.

No abstract

This work describes the application of standard dilution analysis (SDA) in Raman spectroscopy, demonstrating the versatility of this new calibration method. A flow system (FA) was developed for ethanol determination in gasoline employing liquid-liquid extraction (LLE) and acetone as the internal standard (IS). Applying LLE eliminated the intense fluorescence background, allowing for ethanol determination using a portable 785-nm-laser Raman system. The SDA-LLE-FA method was applied to commercial gasoline samples and the results were compared with values obtained using the ABNT NBR 13992 reference method. No statistically significant differences were observed for ethanol concentrations determined using the two methods (paired t-test at the 95% confidence level). SDA's accuracy was also evaluated by comparing results from analyses using the same LLE-FA system combined with the traditional calibration methods of matrix matching (MM), standard additions (SA) and internal standardization (IS). Recoveries from spike experiments were in 98.6-104.1% (SDA-LLE-FA), 94.7-171.1% (ABNT NBR 13992), 106.8-114.1% (MM-LLE-FA), 103.7-108.4% (IS-LLE-FA), and 114.7-125.8% (SA-LLE-FA) range. The relative standard deviation (RSD, n = 12, 25.5% v/v −1 ethanol in gasoline), limits of detection and quantification calculated for the SDA-LLE-FA method were 2%, 0.5% and 1.8% (v/v −1 ), respectively.

No abstract

In this work, an improved conductively heated digestion system (CHDS) with closed vessels, which provides simpler, easier and safer digestion of raw chicken, beef and pork meat samples aiming at Ca, Cu, Fe, K, Mg, Mn, Na, P, S, and Zn determinations by ICP OES and As, Cd, Cr, Mo, Pb and Se by ICP-MS/MS, was evaluated.