6 resultados para Ultra-trace analysis

em Universidad de Alicante


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This work explores the multi-element capabilities of inductively coupled plasma - mass spectrometry with collision/reaction cell technology (CCT-ICP-MS) for the simultaneous determination of both spectrally interfered and non-interfered nuclides in wine samples using a single set of experimental conditions. The influence of the cell gas type (i.e. He, He+H2 and He+NH3), cell gas flow rate and sample pre-treatment (i.e. water dilution or acid digestion) on the background-equivalent concentration (BEC) of several nuclides covering the mass range from 7 to 238 u has been studied. Results obtained in this work show that, operating the collision/reaction cell with a compromise cell gas flow rate (i.e. 4 mL min−1) improves BEC values for interfered nuclides without a significant effect on the BECs for non-interfered nuclides, with the exception of the light elements Li and Be. Among the different cell gas mixtures tested, the use of He or He+H2 is preferred over He+NH3 because NH3 generates new spectral interferences. No significant influence of the sample pre-treatment methodology (i.e. dilution or digestion) on the multi-element capabilities of CCT-ICP-MS in the context of simultaneous analysis of interfered and non-interfered nuclides was observed. Nonetheless, sample dilution should be kept at minimum to ensure that light nuclides (e.g. Li and Be) could be quantified in wine. Finally, a direct 5-fold aqueous dilution is recommended for the simultaneous trace and ultra-trace determination of spectrally interfered and non-interfered elements in wine by means of CCT-ICP-MS. The use of the CCT is mandatory for interference-free ultra-trace determination of Ti and Cr. Only Be could not be determined when using the CCT due to a deteriorated limit of detection when compared to conventional ICP-MS.

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The elemental analysis of Spanish palm dates by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry is reported for the first time. To complete the information about the mineral composition of the samples, C, H, and N are determined by elemental analysis. Dates from Israel, Tunisia, Saudi Arabia, Algeria and Iran have also been analyzed. The elemental composition have been used in multivariate statistical analysis to discriminate the dates according to its geographical origin. A total of 23 elements (As, Ba, C, Ca, Cd, Co, Cr, Cu, Fe, H, In, K, Li, Mg, Mn, N, Na, Ni, Pb, Se, Sr, V, and Zn) at concentrations from major to ultra-trace levels have been determined in 13 date samples (flesh and seeds). A careful inspection of the results indicate that Spanish samples show higher concentrations of Cd, Co, Cr, and Ni than the remaining ones. Multivariate statistical analysis of the obtained results, both in flesh and seed, indicate that the proposed approach can be successfully applied to discriminate the Spanish date samples from the rest of the samples tested.

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Participation trends in 6-hour ultra-marathons held word-wide were investigated to gain basic demographic data on 6-hour ultra-marathoners and where these races took place. Participation trends and the association between nationality and race performance were investigated in all 6-hour races held worldwide between 1991 and 2010. Participation increased linearly in both women and men across years. The annual number of finishes was significantly higher in men than in women (P=0.013). The male-to-female ratio remained stable at ~4 since 1991. Runners in age group 45-49 years showed the largest increase in participation for both men (800 participants in 18 years) and women (208 participants in 16 years). Europe attracted most of the runners from other continents (166 runners), more than all other continents combined (55 runners). European runners also showed the best top ten performances (73±3 km for women and 77±11 km for men), while African (with 65±9 km for men) and South American (54±4 km for women and 65±2 km for men) runners showed the weakest. To summarize, participation in 6-hour ultra-marathons increased across years. Most of the development took place in Europe and in athletes in the age group 45-49 years. Europe also attracted the most diverse field of athletes with runners from all other continents. European runners accounted for the most runners and achieved the best top ten performances.

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A rapid and efficient Dispersive Liquid–Liquid Microextraction (DLLME) followed by Laser-Induced Breakdown Spectroscopy detection (LIBS) was evaluated for simultaneous determination of Cr, Cu, Mn, Ni and Zn in water samples. Metals in the samples were extracted with tetrachloromethane as pyrrolidinedithiocarbamate (APDC) complexes, using vortex agitation to achieve dispersion of the extractant solvent. Several DLLME experimental factors affecting extraction efficiency were optimized with a multivariate approach. Under optimum DLLME conditions, DLLME-LIBS method was found to be of about 4.0–5.5 times more sensitive than LIBS, achieving limits of detection of about 3.7–5.6 times lower. To assess accuracy of the proposed DLLME-LIBS procedure, a certified reference material of estuarine water was analyzed.

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The Web 2.0 has resulted in a shift as to how users consume and interact with the information, and has introduced a wide range of new textual genres, such as reviews or microblogs, through which users communicate, exchange, and share opinions. The exploitation of all this user-generated content is of great value both for users and companies, in order to assist them in their decision-making processes. Given this context, the analysis and development of automatic methods that can help manage online information in a quicker manner are needed. Therefore, this article proposes and evaluates a novel concept-level approach for ultra-concise opinion abstractive summarization. Our approach is characterized by the integration of syntactic sentence simplification, sentence regeneration and internal concept representation into the summarization process, thus being able to generate abstractive summaries, which is one the most challenging issues for this task. In order to be able to analyze different settings for our approach, the use of the sentence regeneration module was made optional, leading to two different versions of the system (one with sentence regeneration and one without). For testing them, a corpus of 400 English texts, gathered from reviews and tweets belonging to two different domains, was used. Although both versions were shown to be reliable methods for generating this type of summaries, the results obtained indicate that the version without sentence regeneration yielded to better results, improving the results of a number of state-of-the-art systems by 9%, whereas the version with sentence regeneration proved to be more robust to noisy data.

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Activated carbon was prepared from date pits via chemical activation with H3PO4. The effects of activating agent concentration and activation temperature on the yield and surface area were studied. The optimal activated carbon was prepared at 450 °C using 55 % H3PO4. The prepared activated carbon was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer, Emmett, and Teller (BET) surface area. The prepared date pit-based activated carbon (DAC) was used for the removal of bromate (BrO3 −). The concentration of BrO3 − was determined by ultra-performance liquid chromatography-mass tandem spectrometry (UPLC-MS/MS). The experimental equilibrium data for BrO3 − adsorption onto DAC was well fitted to the Langmuir isotherm model and showed maximum monolayer adsorption capacity of 25.64 mg g−1. The adsorption kinetics of BrO3 − adsorption was very well represented by the pseudo-first-order equation. The analytical application of DAC for the analysis of real water samples was studied with very promising results.