Produção de sulfato de amônio duplamente marcado com os isótopos estáveis 15N e 34S

The purpose of this work was the production of ammonium sulfate double labeled with 15N and 34S ((15NH4)2(34)SO4)), employing the ion exchange technique in two different processes. The first one was carried out using Na2(34)SO4 and (15NH4)2SO4 previously enriched. It was possible to obtain about 54g of (15NH4)2(34)SO4 from 70.0g of Na2(34)SO4 and 64.2g of (15NH4)2SO4 . The second method involved the production of H2(34)SO4, by ion exchange, and its subsequent reaction with 15NH3(aq), using a distillation system, to yield 58 g of (15NH4)2(34)SO4 from 43.1 g of H2(34)SO4.

Influência do agente precipitante na preparação do óxido de nióbio (V) hidratado pelo método da precipitação em solução homogênea

This work reports the preparation, characterization and study of the ion exchange behavior of hydrous niobium oxide prepared by a homogeneous precipitation method. The precipitating agent was obtained in aqueous solution by thermal decomposition of urea or ammonium carbonate. The compounds were chemically and physically characterized by X-ray diffractometry, thermal analysis (TG/DTG), surface area measurements and ion exchange behavior with sodium. The materials prepared with ammonium carbonate presented a higher degree of crystallinity and better ion exchange capacity with sodium than materials prepared with urea. In the homogeneous precipitation method, materials were obtained with specific surface area of 123 - 224 m² g-1. A variation of the preparation process produced hydrous niobium oxide with a different degree of hydration and specific surface area. This provided materials with different physico-chemical properties.

Complexos metálicos com o herbicida glifosato: revisão

We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature.

Determinação das formas de nitrogênio e nitrogênio total em rochas-reservatório de petróleo por destilação com arraste de vapor e método do indofenol

Several extraction procedures are described for the determination of exchangeable and fixed ammonium, nitrate + nitrite, total exchangeable nitrogen and total nitrogen in certified reference soils and petroleum reservoir rock samples by steam distillation and indophenol method. After improvement of the original distillation system, an increase in worker safety, a reduction in time consumption, a decrease of 73% in blank value and an analysis without ammonia loss, which could possibly occur, were achieved. The precision (RSD < 8%, n = 3) and the detection limit (9 mg kg-1 NH4+-N) are better than those of published procedures.

Influência do pH sobre a estabilidade de suspensões de alumina estabilizadas eletroestericamente

In this work, aqueous suspensions of aluminas with different particle sizes were evaluated. The effect of pH on the electrosteric stabilization using PMAA-NH4 (ammonium polymethacrylate) as deflocculant was studied. The amount of deflocculant was optimized and rheologic properties were determined at four different pH values. Sedimentation was also evaluated. For suspensions with pH 4, an electrostatic mechanism of stabilization was observed, probably due to a flat adsorption of PMMA- on the alumina surface, leading to a small efficiency in relation to steric stabilization. For a suspension with pH 12, the steric mechanism of stabilization prevails. Suspensions with pH 7 and 9 present a higher flocculation degree. In relation to particle size, A-1000 samples present a smaller particle size, leading to a smaller interparticle distance (IPS), making stabilization more difficult.

Otimização do banho eletrolítico da liga Fe-W-B resistente à corrosão

A study on optimization of bath parameters for electrodeposition of Fe-W-B alloys from plating baths containing ammonia and citrate is reported. A 2³ full factorial design was successfully employed for experimental design analysis of the results. The corrosion resistance and amorphous character were evaluated. The bath conditions obtained for depositing the alloy with good corrosion resistance were: 0.01 M iron sulfate, 0.10 M sodium tungstate and 0.60 M ammonium citrate. The alloy was deposited at 12% current efficiency. The alloy obtained had Ecorr -0.841 V and Rp 1.463 x 10(4) Ohm cm². The deposit obtained under these conditions had an amorphous character and no microcracks were observed on its surface. Besides this, the bath conditions obtained for depositing the alloy with the highest deposition efficiency were: 0.09 M iron sulfate, 0.30 M sodium tungstate and 0.50 M ammonium citrate. The alloy was deposited at 50% current efficiency, with an average composition of 34 wt% W, 66 wt% Fe and traces of boron. The alloy obtained had Ecorr -0.800 V and Rp 1.895 x 10³ Ohm cm². Electrochemical corrosion tests verified that the Fe-W-B alloy deposited under both conditions had better corrosion resistance than Fe-Mo-B.

Determinação do teor de edta remanescente em soluções de limpeza de equipamentos industriais

Cleaning solutions containing EDTA are widely employed to remove incrustation despite of the costs involved. The free content of EDTA in commercial solutions may be determined by mixing an aliquot to ammonium oxalate and using a standard calcium solution as titrant. The end-point is detected by the formation of insoluble calcium oxalate after all EDTA is complexed. A system for turbidimetric detection of the end-point was envisaged to substitute the visual detection, which impaired the analyses of dark samples. The proposed method was tested with real samples and good accuracy and precision was obtained.

Avaliação da composição química de águas do Sistema Guarapiranga: estudo de caso nos anos de 2002 e 2003

The supply of drinking water in the Metropolitan Area of São Paulo City has been a great and serious challenge in the latest years. This work demonstrates the viability of the evaluation of the degree of contamination of the water reservoirs using analytical procedures, which allow the analysis of several compounds at relatively low cost: stripping square wave voltammetry (SSWV) and capillary zone electrophoresis with contactless conductivity detection (CZE-CCD). The results of ionic composition indicated significant contamination of the Guarapiranga water system by human activities on the reservoir banks. In fact, the Guavirutuba and Itupu streams presented high concentrations of phosphate and ammonium ions. This can be directly related to misuse and unruled occupation of the soil and precarious sanitary infrastructure.

Métodos de extração para quantificação de manganês disponível em fertilizantes

The solubility of Mn in different fertilizers (MnSO4.H2O-p.a., MnO2-p.a.+MnO-Ind., MnO2-Ind.+MnO-Ind., MnO2-p.a., MnO2-Ind. and MnO-Ind.) was determined using different methodologies: total content and soluble contents in water, 10% H2SO4, citric acid at 20 g L-1, diluted neutral ammonium citrate, (1+9) and DTPA at 0.005 mol L-1. The Mn solubilities in the latter three extractors were assessed after agitation of the sample for one hour and after boiling for 5 minutes. The extraction procedure using neutral ammonium citrate (1+9), at 1:100, with agitation for one hour, was shown to be the most adequate to assess the availability of Mn in fertilizers.

Teores de nitrato (NO3-) e amônio (NH4+) nas águas do aqüífero Barreiras nos bairros do Reduto, Nazaré e Umarizal - Belém/PA

This paper evaluates the occurrence of nitrate and ammonium in the Barreiras aquifer in the metropolitan area of Belém, Pará State, Brazil. The results show that some wells display ammonium and nitrate concentrations above or close to the limits of water potability regulations. The main cause of the pollution of these waters is related the local disposal of domestic effluents and/or leakage from pipes of old sewage systems.

Size distribution of atmospheric particulate ionic species at a coastal site in Portugal

A Berner impactor was used to collect size-differentiated aerosol samples from March to August 2003 in the city of Aveiro, on the Portuguese west coast. The samples were analysed for the main water-soluble ion species. The average concentration of sulphate, nitrate, chloride and ammonium was 6.38, 3.09, 1.67 and 1.27 µg m-3, respectively. The results show that SO4(2-) and NH4+ were consistently present in the fine fraction < 1 µm, which represents, on average, 72 and 89% of their total atmospheric concentrations, respectively. The NO3-particles were concentrated in the coarse size. Chloride presented the characteristic coarse mode for marine aerosols. During some spring/summer events, an ammonium surplus was observed (NH4+/SO4(2-) molar ratios > 2), possibly due to greater availability of ammonia coming from agricultural activities or from the neighbouring chemical industrial complex. During the remaining periods, the aerosol was found to be somewhat acidic and predominantly in the form of ammonium bisulphate (NH4+/SO4(2-) molar ratios = 0.5-1.25). Samples collected under a major or exclusive influence of maritime air masses were essentially constituted by coarse particles with enrichment in sea salt, while for air masses of continental origin the contribution of water-soluble ionic species in the fine mode was more pronounced.

Determinação de fármacos diuréticos em associação por cromatografia em camada delgada e espectrofotometria

A rapid, sensitive and reliable thin-layer chromatography/spectrophotometry screening procedure was developed for quantitative determination of diuretics associated in pharmaceutical dosage forms. The chromatographic method employed microcrystalline cellulose and butanol : acetic acid : water (4:1:1) or amilic alcohol : ammonium hydroxide 25% (9:1) as mobile phases and detection by U.V. light. The drugs were extracted using a simple procedure and were quantified by U.V. spectrophotometry. Results varied from 97.5 to 102.5% and are similar to those obtained by conventional methods. This method of quantification of diuretics is promising for quality control of drugs.

Análise multivariada de parâmetros físico-químicos em amostras de vinhos tintos comercializados na região metropolitana do Recife

The Brazilian legislation requires analysis of certain parameters to classify a wine and allow its commercialization. Some physico-chemical and some color parameters were determined in this work in samples of different red wines sold in the metropolitan area of Recife. Multivariate analysis comprising principal component analysis and hierarchical cluster analysis was employed to distinguish the analyzed wines. The results for pH, chloride concentration, color parameters and ammonium content were the most important variables for sample classification. It was also possible to classify the wines as soft or dry wines and amongst the soft wines we could determine two out of four winegrowing producers.

Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Determination of etoricoxib in human plasma using automated on-line solid-phase extraction coupled with LC-APCI/MS/MS

A liquid chromatography-tandem mass spectrometry method with atmospheric pressure chemical ionization (LC-APCI/MS/MS) was validated for the determination of etoricoxib in human plasma using antipyrin as internal standard, followed by on-line solid-phase extraction. The method was performed on a Luna C18 column and the mobile phase consisted of acetonitrile:water (95:5, v/v)/ammonium acetate (pH 4.0; 10 mM), run at a flow rate of 0.6 mL/min. The method was linear in the range of 1-5000 ng/mL (r²>0.99). The lower limit of quantitation was 1 ng/mL. The recoveries were within 93.72-96.18%. Moreover, method validation demonstrated acceptable results for the precision, accuracy and stability studies.