A fast, simple and inexpensive procedure is described for the determination of gossypol in cottonseed meal. The procedure is based on a flow injection analysis system and a complexation reaction with spectrophotometric detection at 620 nm. A fluidized bed column was used to implement the on line that was coupled to the extraction flow system in order to analyze the solid samples directly. A linear response was observed from 0.96 to 3.85 mmol L-1, and the detection limit, the coefficient of variation and the sampling rate were estimated at 100 µmol L-1 (99.7% confidence level), 1.90% (n = 20) and 30 h-1, respectively. The reagent consumption was 1.08 mg of Fe(NO3)3, with a volume of 20 mL of effluent per determination. Analyses of the results of commercial samples were consistent with through the official procedure of detoxification of cottonseed meal as described by American Oil Chemists’ Society (AOCS) at the 95% confidence level.

Soils with high levels of iron and aluminum, thus negatively the phosphorous availability, affecting crop yields. A prior determination of the soil capacity to adsorb phosphate is relevant to attaining good agricultural performance. To this end, a multi-pumping flow system with pulsed fluidization is proposed. The procedure takes into account the amount of remaining phosphorus (P-rem) in the solution after the adsorption step to indirectly estimate the soil retention capacity. A 1.0 mg L-1 P solution is passed through a fluidized bed column with 50 mg of soil (particles < 0.15 mm), where the analyte is adsorbed. P-rem was spectrophotometrically quantified by the molybdenum blue method. The coefficient of variation (n = 20), limits of detection and quantification (99.7% confidence level), and sampling rate were estimated as 1.54%, 17 and 51 µg L-1 P, and 87 h-1, respectively. Only 0.27 mg (NH4)6Mo7O24 and 0.10 mg SnCl2 were consumed per determination, generating 2.4 mL of waste. The results followed a linear relationship [y = 0.9702x + 1.483 (r = 0.9635; n = 20)] with the reference procedure. In comparison to the reference procedure, 100, 40 and 180-fold reductions in the required soil amount, waste generation and analytical time were attained.

A webcam is proposed as the detector in a flow system with multicommutation, and the feasibility of the approach is demonstrated in the determination of nitrate and nitrite in natural waters. The typical transient signal inherent to the flow system was obtained using a digital video and quantified by ImageJ software. The linear dynamics range for nitrite and nitrate determinations were 0.2 to 2.0 mg L-1 NO2− and 1.0 to 10.0 mg L-1 NO3−, with relative standard deviation < 2% for both analytes. The limits of detection were 0.01 and 0.04 mg L-1 for nitrite for nitrate, respectively, and the sampling rate were 80 and 103 h-1 for nitrite and nitrate, respectively. The use of webcams has a high potential for analysis in the visible region of the electromagnetic spectrum, and the proposed strategy constitutes a promising alternative to traditional absorbance measurements that depend on conventional equipment. The webcam detection system is attractive, especially in relation to field analysis.

Diante do extensivo uso de fertilizantes nitrogenados na agricultura e elevado potencial de lixiviação do nitrato, há uma demanda por fertilizantes de liberação lenta ou controlada. Os hidróxidos duplos lamelares (HDLs) sintéticos reúnem características que os qualifica para o uso como matrizes para fertilizantes de liberação lenta de íons nitrato. Os objetivos deste trabalho foram focados na síntese, caracterização e investigação do processo de liberação lenta de nitrato em um HDL contendo íons Mg2+ e Al3+ em sua estrutura. O HDL com a fórmula Mg0,83Al0,17(OH)2(NO3)0,17.0,56H2O foi sintetizado pelo método de coprecipitação em pH alcalino constante, separado por centrifugação e seco em estufa a vácuo. As análises de difração de raios-X, de espectroscopia vibracional na região do infravermelho com transformada Fourier e as análises térmicas comprovam a obtenção do composto contendo o íon nitrato hidratado intercalado, além da fórmula proposta. O composto foi submetido a testes de liberação de nitrato em solução de NaHCO3 tamponado a pH 6,5 e em água destilada. As curvas obtidas evidenciaram dois eventos complementares de liberação de nitrato, um evento inicial rápido e um outro lento e gradativo. O composto investigado neste trabalho demonstrou potencial para ser utilizado como matriz para fertilizante de liberação lenta de nitrato.

Due to the extensive use of nitrogen fertilizers in the agriculture e due to the elevate potential of nitrate leaching, there is a great demand for slow or controlled release fertilizers. Synthetic layered double hydroxides (HDLs) combine the characteristic that qualifies them to be used as matrixes for nitrate slow release fertilizers. The objectives of the present work are focused in the synthesis, characterization and investigation of the slow release of nitrate process in one structure of a HDL containing ions Mg2+ and Al3+ in its structure. The HDL with the formula Mg0,83Al0,17(OH)2(NO3)0,17.0,56H2O was synthesized by the co-precipitation method at constant alkaline pH, isolated by centrifugation and dried in an vacuum oven. Measurements of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and thermal analysis (TGA/DTA) confirmed the obtaining of the compound containing the intercalated hydrated nitrate anions and the proposed formula. The compound was tested for release nitrate NaHCO3 solution buffered to pH 6.5, and distilled water. The representative curves demonstrated two complementary behaviors nitrate release a fast initial and a slow gradual. The compound investigated in this study demonstrates the potential to be used as a matrix for slow release fertilizer nitrate. The compound was submitted to the nitrate release tests using a NaHCO3 solution buffered at pH 6.5 and in distilled water. The obtained curves have shown two complementary events of nitrate release, one fast initial event and another slow and gradual. The compound investigated in the present work has shown a potential to be used as matrix for nitrate slow release fertilizers.

This paper describes the use of the open source hardware platform, denominated "Arduino", for controlling solenoid valves for solutions handling in flow analysis systems. System assessment was carried out by spectrophotometric determination of iron (II) in natural water. The sampling rate was estimated as 45 determinations per hour and the coefficient of variation was lower than 3%. Per determination, 208 µg of 1-10-phenanthroline and ascorbic acid were consumed, generating 1.3 mL of waste. "Arduino" proved a reliable microcontroller with low cost and simple interfacing, allowing USB communication for solenoid device switching in flow systems.

This paper describes a homemade autosampler for flow injection analysis (FIA), constructed with two step motors from old floppy disk drives (5¼-inch). The autosampler was connected to a computer through the parallel port and the sampling process was controlled by software in Quick Basic. The performance of the system was assessed by the determination of ammonium, based on the gaseous diffusion into a bromocresol purple solution, following the spectrophotometric determination of change in absorbance. The easy and simple construction is the main characteristics of this equipment and analytical results with RSD lower than 1% were obtained.

No estudo da dinâmica de solutos num meio poroso, é de suma importância o conhecimento das propriedades do meio e dos líquidos percolantes, bem como de fatores externos. Um fator externo relevante é a temperatura e, nesse sentido, teve-se como objetivo determinar os parâmetros de transporte dos íons potássio e nitrato para diferentes valores de temperatura em experimentos de deslocamento miscível. Os parâmetros avaliados foram o fator de retardamento (R), o coeficiente de difusão/dispersão (D) e a dispersividade (λ ), e as temperaturas utilizadas foram a ambiente (25 a 28 ºC), 40 ºC e 50 ºC. Os sais utilizados foram nitrato de potássio e cloreto de potássio, preparados em solução composta de 50 ppm de nitrato e 2.000 ppm de potássio, sendo o meio poroso um Latossolo Vermelho-Amarelo, textura média. A temperatura apresentou influência positiva na velocidade da solução no meio poroso e no coeficiente de dispersão.

When doing researches on solute dynamics in porous medium, the knowledge of medium characteristics and percolating liquids, as well as of external factors is very important. An important external factor is temperature and, in this sense, our purpose was determining potassium and nitrate transport parameters for different values of temperature, in miscible displacement experiments. Evaluated parameters were retardation factor (R), diffusion/dispersion coefficient (D) and dispersivity, at ambient temperature (25 up to 28 ºC), 40 ºC and 50 ºC. Salts used were potassium nitrate and potassium chlorate, prepared in a solution made up of 5 ppm nitrate and 2.000 ppm potassium, with Red-Yellow Latosol porous medium. Temperature exhibited a positive influence upon porous medium solution and upon dispersion coefficient.

Quantitative analysis of colored substances is generally performed using a spectrophotometer for detection of radiation. However, the combination of digital images and mathematical conversion of colors is an alternative for quantitative procedures based on colored chemical reactions. This work proposes a didactic experiment using a scanner for determination of ascorbic acid in medicines based on the formation of the Prussian blue complex. Results were in good agreement with a conventional spectrophotometer method and the procedure is attractive for instrumental analysis undergraduate courses.

The objective of this study was to develop a method for the direct determination of residual CO3(2-) in acid soil using a flow system coupled with pervaporation. The gas released from the acidified sample was separated though a hydrophobic membrane and detected by conductivimetry. The detection limit was 0.054 mmol c kg-1 for CO2/CO3(2-) with relative error of 3.1%. The analytical frequency was 20 samples per hour. The method is recommended for studying the reactions and kinetics of lime applied in acid soils.