O problema da contaminação na determinação de traços de alumínio

The most common difficulties which occur in trace analysis are those which involve contamination, mainly when the measurement is at very low concentration of ubiquitous elements as aluminium. The worst situation is when a separation step is necessary, because it requires extra-manipulations of the sample. This article describes the degree of contamination and its control for the aluminium trace analysis in dialysis solutions, when aluminium content of about 15 µg/l must be determinated.

Síntese de β-cetoésteres cíclicos: novo procedimento para ciclizações de Dieckmann empregando ALCL3 e trietilamina

In this communication we describe a new methodology to Dieckmann cyclization of diethyl adipate (1) and diethyl pimelate (3) applying "push-pull" strategy using anhydrous aluminium trichloride and triethylamine in dichloromethane at room temperature. This method is very efficient, simple, safe and reproducible, giving the corresponding cyclic β-keto ester derivatives in 84% and 71% yield, respectively.

Preparación y propiedades de una arcilla montmorillonita pilareada con polihidroxicationes de aluminio

Montmorillonite clay from Brazil was pillared with aluminium polyhydroxications. The influence of Al/Mont ratio and calcination temperature in the properties of the prepared materials was studied. Results showed that the pillarization process increases the basal spaces of the natural clay from 9,7 to 18,5Å and the superficial area from 41 to ~230m2/g. The calcination process at different temperatures showed that the pillared material was stable until 600oC but the adequate temperature for calcination was 450oC. Materials prepared with different Al/Mont ratios showed the maximum Al incorporation for ratios >10meq Al/g and a good distribution for rations >15meq Al/g.

Uso do violeta de alizarina N (AVN) como reagente espectrofotométrico na determinação de alumínio

The present work proposes the application of the 4-Hidroxy-3-(2-hydroxynaphtylazo)-benzenesulphonic acid (C.I. 15670), Alizarine Violet N (AVN), as a reagent for direct aluminium determination using molecular absorption spectrophotometry in the presence of tensoatives. Al(III) cation reacts with AVN in pH 9.4, forming a red complex, stable for at least 24 hours, with absorption minimum at 607nm and, against a reagent blank, (epsiloncomplex - epsilonreagent) = -2.71x10(4) L.mol-1.cm-1. The reaction occurs in the presence of a Triton-X100 and CTAB tensoatives mixture, in the presence of EDTA. Al(III) determination is possible in the linear range of 50 up to 400ng.mL-1, with a detection limit of 41 ng.mL-1.

Safrol e eugenol: estudo da reatividade química e uso em síntese de produtos naturais biologicamente ativos e seus derivados

The chemical reactivity of safrole, eugenol, piperonal, vanillin and derivates toward ozone, aluminium chloride, brominating agents and butyl lithium was investigated. The synthesis of naturally occuring anthraquinones, furonaphthoquinones, naphthoquinones, lignans and pterocarpans from these easily available staring materials is also discussed.

Determinação espectrofotométrica de alumínio em concentrados salinos utilizados em hemodiálise empregando pré-concentração em fluxo

An automatic flow injection procedure for spectrophotometric aluminium determination in purified water and solutions containing high salts concentrations used for hemodyalisis treatment was developed. The method was base on reaction of Al3+ with cianine eriochrome R (ECR) after preconcentration using the AG50W-X8 cationic-exchange resin. Elution was carried out using a 1 % (m/v) calcium chloride solution. The manifold comprised an automatic proporcional injector controlled by a computer equipped with an eletronic interface and software written in QuicBASIC 4.5 with facilities to control the injector and perform data acquisition. Samples with concentration ranging from 4.96 to 19.90 µg L-1 Al were analyzed and recoveries between 88 and 113% were obtained by using the standard addition method. Other profitable analytical characteristics such as a relative standard deviation 1.3 % (n = 10) for a typical sample 14.5 µg L-1 Al, a linear response ranging up to 60.0 µg L-1Al, and a sampling throughput of 10 determinations per hour were achieved. A detection limit of 4.2 µg L-1 Al was estimated as suggested by IUPAC.

Recuperação de metais de catalisadores mássicos e monometálicos

This work presents a study on the dissolution of some commercial monometallic and non-supported deactivated catalysts in HF + H2O2 mixtures (and, eventually, other media) under mild experimental conditions, after a previous oxidation step. The samples were neither crushed nor grinded. The best experimental conditions were dependent on the nature of the support and of the active phase. For example, the Pt/Al2O3 catalyst was dissolved in about 10 minutes, without agitation and heating; however, dissolution of the Pd/Al2O3, Ni/Al2O3, Ni/SiO2, Cu/Al2O3 and V2O5 samples required a temperature of 60 ºC and an agitation of 400 rpm. A careful addition of a NaOH solution allowed a quantitative precipitation of aluminium as criolite (Na3AlF6) or precipitation of Si as Na2SiF6; NaF was obtained as a by-product. As expected, processing of Pd/C, V2O5 and CuO.Cr2O3 samples was relatively simple. Metals recovery from catalysts reached a quantitative level in all samples studied; it is particularly interesting that platinum and palladium could be easily recovered in a single step process, thus separing them from aluminium.

Eletrodo íon-seletivo para determinação potenciométrica de alumínio(III) em meio de fluoreto

The construction and analytical evaluation of a coated graphite Al(III) ion-selective electrode, based on the ionic pair formed between the Al(F)n3-n anion and tricaprylylmethylammonium cation (Aliquat 336S) incorporated on a poly(vinylchloride) (PVC) matrix membrane are described. A thin membrane film of this ionic pair and dibutylphthalate (DBPh) in PVC was deposited directly on a cylindric graphite rod (2 cm length x 0.5 cm diameter) attached to the end of a glass tube using epoxy resin. The membrane solution was prepared by dissolving 40% (m/m) of PVC in 10 mL of tetrahydrofuran following addition of 45% (m/m) of DBPh and 15% (m/m) of the ionic pair. The effect of membrane composition, fluoride concentration, and several concomitants as potential interferences on the electrode response were investigated. The aluminium(III) ion-selective electrode showed a linear response ranging from 1.4 x 10-4 to 1.0 x 10-2 mol L-1, a detection limit of 4.0 x 10-5 mol L-1, aslope of -54.3±0.2mV dec-1 and a lifetime of more than 1 year (over 3000 determinations for each membrane). The slope indicates that the ion-selective electrode responds preferentially to the Al(F)4- species. Application of this electrode for the aluminium(III) determination in stomach anti-acid samples is reported.

Óxido misto de ítrio-alumínio dopado com Eu(III)

In this work, we report the synthesis and the photoluminescence features of Eu(III)-doped yttrium-aluminium oxide obtained by non-hydrolytic sol-gel routes. After heating the powders above 600 ºC the XRD patterns show the presence of the Y4Al2O9 (YAM) and Y3Al5O12 (YAG) phases. At 800 and at 1500 ºC the PL spectra display the Eu(III) lines characteristic of the YAM monoclinic phase. The 5D0->7F2 transition is favored relatively to the 5D0->7F1 lines. However, at 1100 ºC the cubic YAG is the preferential phase and the 5D0->7F1 transition dominates the spectrum. The Eu(III) ions lie in a centrosymmetrical site. The different solvents used in the sol-gel synthesis also change the relative proportion between these two phases. This is monitored analyzing the modifications in the relative intensity between the 5D0->7F2 and the 5D0->7F1 transitions.

Pilarização de uma argila brasileira com poliidroxications de alumínio: preparação, caracterização e propriedades catalíticas

Montmorillonite clay from Brazil was pillared with aluminium polyhydroxications. The influence of aging of the pillaring solution and the concentration of the clay suspension on the properties of the prepared materials was studied. The materials were characterized by chemical analysis, XRD and pore analysis by N2 adsorption. The catalytic properties were evaluated in the cumene cracking reaction. Results showed that the pillarization process increases the basal spaces of natural clay from 9.7 to 18.5 Å and the surface area from 41 to 300 m²/g.

Adsorção de glifosato sobre solos e minerais

Glyphosate, an enzyme inhibitor herbicide, has been widely used around the world in agriculture. Dr. John Franz from Monsanto Corporation (USA) discovered glyphosate in 1970. It has been showed that glyphosate is strongly adsorbed by inorganic soil components especially aluminium and iron oxides, and the phosphate group is involved in this interaction. The inactivation of glyphosate in soils can last for days or even months depending on soil characteristics. The addition of phosphate from fertilizers can displace glyphosate from the soils and this could be the cause of decreased productivity of some crops.

A qualidade de água como indicador de uso e ocupação do solo: bacia do Gama - Distrito Federal

The spread of Brasília isn't accompanied by correct support of land occupation, situation that is reflected in water quality. Under the optics of land use and occupation, working with multivariate statistics as main tool, water physical and chemical quality of Gama Catchment were assessed. During two years samples were collected and analyzed for 24 parameters. The statistical analysis showed the influence of civil buildings, agricultural activities and the best statistical parameters to a quickly assessment: nitrate, ammonia, suspended solids and aluminium.

Estudio preliminar sobre la determinación de elementos traza en cervezas venezolanas por ICP-OES

The levels of several chemical elements were determined simultaneously in ten different beers of the Venezuelan market by ICP-OES. With the exception of chromium, beer does not provide important amounts of nutritional oligoelements. The average chromium content found (33 µg/L) is higher than one reported for USA's beer (10 µg/L) but smaller than another reported for Brazilian beer (66 µg/L). The average percentage of chromium RDA by beer consumption found for Venezuela (6.3%) is similar to that reported for Belgium (5%). Regarding toxic elements, one of the samples contained an elevated amount of aluminium, probably dissolved from the aluminium can.

Tratamento do efluente do biodiesel utilizando a eletrocoagulação/flotação: investigação dos parâmetros operacionais

Electrocoagulation/flotation process was applied to treat biodiesel wastewater using aluminium electrodes. Firstly, a literature survey was conducted to choose the process variables and then, operational parameters including initial pH, electrode distance and reaction time were tested. Experimental results showed the best parameter that can be used in a factorial design for further studies. The results indicate that electrocoagulation/flotation is very efficient to reduce oil and grease, the effluent was very clear after treatment and small amount of sludge was produced.

Synthesis, characterization and thermal studies of solid state 4-methylbenzylidenepyruvate of some trivalent metal ions

Solid state compounds of 4-methylbenzylidenepyruvate with Al(III), Ga(III), In(III) and Sc(III) have been synthesized. Complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA) have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition of these compounds.