Validation and quality assurance applied to goat milk chemical composition: minerals and trace elements measurements

In the present study, quality assurance programmes were implemented to validate and control the analytical methodologies used for the characterization of minerals and trace elements in goat milk from Portuguese breeds. With the exception of chloride that was determined by potentiometric titration, all the other elements were determined by spectroscopic techniques after different sample decomposition: P was measured by ultraviolet-visible molecular absorption spectrometry, Ca, Fe, K, Mg, Mn, Na and Zn by flame atomic absorption spectrometry and Cd, Co, Cr, Cu, Mo, Ni and Pb by electrothermal atomic absorption spectrometry. The methods performance characteristics, namely specificity, limit of detection, limit of quantification, working range, precision and trueness were evaluated. Measurement uncertainty was expressed in terms of precision and trueness. Precision under intralaboratory reproducibility conditions was estimated from triplicate analysis, and the trueness component was estimated in terms of overall recovery using either skim milk powder certified reference materials or spiked samples. The results obtained are discussed on the basis of the performance criteria required by EC regulations to verify when a method is suitable for food control. The methods used for the characterization of minerals and trace elements in goat milk complied with EC requirements since there was no matrix influence, the Horrat values were < 2.0, recoveries were within the interval 1.00 ± 0.10 for minerals and 1.00 ± 0.20 for trace elements and the combined uncertainty of the results were lower than the maximum standard uncertainty calculated using the uncertainty function approach. In relation to the limits of detection and quantification, the limits obtained for Pb were lower than those specified by EC regulation

Validation and setting up quality control for characterization of aluminum alloys in non‑ferrous fraction of auto‑shredders

ABSTRACT: The improvement of recycling rates of metal waste, namely those of end-of life vehicles, is nowadays becoming imperative. Aluminum and its alloys are the main metal components in non-ferrous fraction of auto-shredders separated out after sampling. Silicon, Mg, Cu, Zn, Mn, Ti, Fe and Cr are alloying elements, which allowed the identification and differentiation of Al alloys. Flame Atomic Absorption Spectrometry was used for quantification after HCl-HNO3 digestion, with the exception of Si, where HCl–HNO3–HF–H3BO3 digestion was used. Performance characteristics of measurement procedures, namely analytical dynamic ranges, limits of detection and quantification, precision and trueness were evaluated and measurement uncertainty estimated by applying an approach based on precision and trueness validation studies and quality control data. Target values, for repeatability, intermediate precision, trueness (recovery) and measurement uncertainty, were specified to differentiate Al alloys based on their own fit-for-purpose. Metrological traceability of the measurements results of the alloying elements was established by using certified values of British Chemical Standard (BCS) of Al alloys, BCS nº 181/1, BCS Nº 268. BCS Nº 300 and Standard Reference Material of Al-base alloy, SRM 87. The quantification of Si, Mg, Cu, Zn, Mn, Ti, Fe and Cr in aluminum alloys from the non-ferrous fraction of automatic crushers was determined successfully through the validated procedures.info:eu-repo/semantics/publishedVersio

Procedure validation and laboratory performance monitoring for the measurement of moisture, ash and volatile matter mass fractions in solid biofuels

Participation in interlaboratory comparisons is a requirement of the accreditation bodies for granting laboratory accreditation by EN ISO/IEC 17025:2005 as external quality control. Proficiency testing (PT) is used to demonstrate the individual performance of a laboratory for a specific test or measurement. Monitoring PT performance over time shows the continuing performance and allows the identification of potential problems related to random and systematic errors. In this study, it is shown that the procedures applied to measure mass fractions of moisture, ash and volatile matter in solid fuels fulfill the conditions stated in the European standards EN 14774-3, EN 14775 and EN 15148:2009 regarding target uncertainty, repeatability and reproducibility. Repeatability was assessed from sample duplicate analysis and combined standard uncertainty. Limits of detection and quantification were also estimated although no target values are stated. The obtained values fulfill the requirements for specifications and classes of solid biofuels. Laboratory performance over the time from 2011 to 2013 regarding such measurements was evaluated with 18 materials provided by WEPAL within the BIMEP program. Apart from monitoring the individual z-scores, their sequence was checked with summarizing parameters including the ‘rescaled sum z-scores’, RSZ, the ‘sum squared z-scores’, SSZ, and J-scores. For none of the analytes, the parameters indicated a trend over time and therefore it was not necessary to trigger any investigation or correcting procedure.

Exploring Graphics Processor Performance for General Purpose Applications

Abstract In our experiments we compare the execution on a midclass GPU (NVIDIA GeForce FX 5700LE) with a high-end CPU (Pentium 4 3.2GHz). The results show that to achieve high speedup with the GPU you need to: (1) format the vectors into two-dimensional arrays; (2) process large data arrays; and (3

Traceability statement for the determination of total chromium fraction in serpentine soils by atomic absorption spectrometry

The purpose of this work is to contribute for the metrological traceability statement of chemical measurements. Traceability statement for total chromium mass fraction in serpentine soils was developed. Accordingly, the quantity values requiring a high degree of control are calibration and quality control standard solutions, matrix certified reference material and the calibration curve model fit

Evaluation of acid matrix effects in the determination of major elements in biomass by atomic absorption spectrometry from an environmentally friendly point of view

The estimation of major element content in solid biofuels is required for prediction and prevention of eventual ash-related problems during combustion. These analyses have to be achieved with minimum impact on the environment. The quantitation of Al, Ca, Mg, Na, K, Fe, Si and Mn in biofuels was carried out according to EN 15290 using acid decomposition of solid samples followed by atomic absorption spectrometry (AAS). A microwave-assisted acid digestion with a HNO3/H2O2/HF mixture was used, followed by HF complexation using H3BO3. Due to the presence of tetrafluoroboric acid complex in the digestion solution, matrix effects were noticed during elemental quantification by AAS. Standard addition calibration methods did not compensate for this matrix effect. Matrix effects that constrain an analytical response may be overcome by applying the procedure used for samples to the calibration standards using the same reagents. However, this entails using large amounts of toxic reagents. In this work, the fluoric–boric acid matrix matching was assessed statistically using one-way ANOVA tests. For the seven groups of nitric acid and reagent blank (HNO3/H2O2/HF/H3BO3) mixtures used, ranging from 0 to 1 volume ratios, no significant differences were observed for Si, Al, Fe and Mn. The calculated F values were lower than the critical value, F 6,14 = 2.85 (p = 0.05). However, for Ca, Mg, Na and K, significant differences were observed. Tenfold dilution was used for samples where the mass fraction exceeded the analytical dynamic range of the AAS instrument. The calibration solutions were prepared using the reagent blanks in the same proportion thus decreasing the amount of acids used. The procedure was validated using SRM 1573a—tomato leaves—purchased from the National Institute of Standards and Technology. Target recoveries of (1 ± 0.1) were achieved

Potencialidades da espetrometria de fluorescência de raios x na área da energia

RESUMO: A espectrometria de fluorescência de raios X em dispersão de comprimentos de onda (FRX-DCO) é uma técnica analítica comparativa, não destrutiva, que permite uma abordagem expedita para elementos de número atómico entre 9 e 92, que apresenta um baixo risco de contaminação e que é aplicável a diversos tipos de matrizes.info:eu-repo/semantics/publishedVersio