Ligandless cloud point extraction of trace amounts of palladium and rhodium in road dust samples using Span 80 prior to their determination by flame atomic absorption spectrometry

In this study, a procedure is developed for cloud point extraction of Pd(II) and Rh(III) ions in aqueous solution using Span 80 (non-ionic surfactant) prior to their determination by flame atomic absorption spectroscopy. This method is based on the extraction of Pd(II) and Rh(III) ions at a pH of 10 using Span 80 with no chelating agent. We investigated the effect of various parameters on the recovery of the analyte ions, including pH, equilibration temperature and time, concentration of Span 80, and ionic strength. Under the best experimental conditions, the limits of detection based on 3Sb for Pd(II) and Rh(III) ions were 1.3 and 1.2 ng mL-1, respectively. Seven replicate determinations of a mixture of 0.5 µg mL-1 palladium and rhodium ions gave a mean absorbance of 0.058 and 0.053 with relative standard deviations of 1.8 and 1.6%, respectively. The developed method was successfully applied to the extraction and determination of the palladium and rhodium ions in road dust and standard samples and satisfactory results were obtained.

Coprecipitation of trace amounts of silicon with aluminum hydroxide and the determination by flame atomic absorption spectrometry

A simple preconcentration method of silicon based on coprecipitation with aluminum hydroxide prior to its flame atomic absorption (FAAS) determination was established. The recovery values of analyte ion was higher than 95%. The parameters including types of hydroxide ion source for precipitation, acid type for dissolution step, amount of aluminum ion as collector, pH, temperature, standing and centrifuge time, and sample volume were optimized for the quantitative recovery of the analyte. The influences of matrix ions were also examined. The relative standard deviation was found to be 3.2%. The limit of detection was calculated as (0.1 mg L-1). The preconcentration factor is 100 for (200 mL) solution. The proposed method was successfully applied for the determination of silicon in some water and alloy samples.

RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) followed by graphite furnace atomic absorption spectrometry (GFAAS). Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

Effect of Fusarium graminearum and infection index on germination and vigor of maize seeds

Pathogens in maize (Zea mays) seeds cause serious problems, such as the loss of their capacity to germinative. The objectives of this study were to identify the optimal period for infection of maize seeds on agar colonized by Fusarium graminearum, when incubated for 4, 8, 16 and 32 h, and to evaluate the effect of the fungus on the germination and vigor of seeds with different infection levels. After the respective incubation periods, the seeds were removed from the culture medium and submitted to the blotter test for 3 min with and without superficial disinfection with 1% solution of sodium hypochlorite. Once the optimal period for seed incubation was identified, seeds from the same sample were again placed on the colonized agar for infection. Germination and vigor tests (accelerated aging and cold test) were performed with a mixture of healthy seeds (placed on PDA medium) and inoculated seeds, resulting in seeds with 0, 20, 40, 60, 80 and 100% rates of infection. The results showed that a period of 32 h was long enough to obtain seeds infected by the pathogen. There were no significant effects of fungal infection on seed germination at any of the infection levels, probably due to the high vigor of the maize seed lot tested. Regarding vigor tests, infection levels differed significantly from the control (0% infection), but there were no significant differences among the infection levels.

Concentration of Pb (II) by adsorption and its atomic absorption spectrometric determination

A sorption concentration method using impregnated silica has been developed to determine small concentration of lead in water by Atomic Absorption Spectrometry.

Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

A flow-injection system with sample and reagent addition by the synchronous merging zones approach for calcium determination in milk by flame AAS is proposed. Main parameters were optimized using a factorial design with central point. The optimum conditions were 2.5% (m/v) for La concentration, 8 mL min-1 for the carrier flow-rate, 20 cm for coiled reactor and 250 ìL for sample volume. Different sample preparation procedures were evaluated such as dilution in water or acid and microwave-assisted decomposition using concentrated or diluted acids. The optimized flow system was applied to determine Ca in eleven commercial milk samples and two standard reference materials diluted in water. Similar calcium levels were encountered comparing the results obtained by the proposed method (dilution in water) with those obtained using microwave-oven digestion. Results obtained in two standard reference materials were in agreement at 95% confidence level with those certified. Recoveries of spiked samples were in the 93% - 116% range. Relative standard deviation (n = 12) was < 5.4% and the sample throughput was 150 measurements per hour, corresponding to a consumption of 250 µL of sample and 6.25 mg La per determination.

Solid phase extraction of zinc with octadecyl silica membrane disks modified by N,N'-disalicylidene-1,2-phenylendiamine and determination by flame atomic absorption spectrometry

A procedure for separation and preconcentration of trace amounts of Zn(II) from aqueous media is proposed. The procedure is based on the adsorption of Zn2+ on octadecyl bonded silica membrane disk modified with N,N'-disalicylidene-1,2-phenylendiamine at pH 7. The retained zinc ions were then stripped from the disk with a minimal amount of 1.5 mol L-1 hydrochloric acid solution as eluent, and determined by flame atomic absorption spectrometry. Maximum capacity of the membrane disk modified with 5 mg of the ligand was found to be 226 µg Zn2+. The relative standard deviation of zinc for ten replicate extraction of 10 µg zinc from 1000 mL samples was 1.2%. The limit of detection of the proposed method was 14 ng of Zn2+ per 1000 mL. The method was successfully applied to the determination of zinc in natural water samples and accuracy was examined by recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry (GFAAS).

Mathematical equation correction to spectral and transport interferences in high-resolution continuum source flame atomic absorption spectrometry: determination of lead in phosphoric acid

In this work, a new mathematical equation correction approach for overcoming spectral and transport interferences was proposed. The proposal was applied to eliminate spectral interference caused by PO molecules at the 217.0005 nm Pb line, and the transport interference caused by variations in phosphoric acid concentrations. Correction may be necessary at 217.0005 nm to account for the contribution of PO, since Atotal217.0005 nm = A Pb217.0005 nm + A PO217.0005 nm. This may be easily done by measuring other PO wavelengths (e.g. 217.0458 nm) and calculating the relative contribution of PO absorbance (A PO) to the total absorbance (Atotal) at 217.0005 nm: A Pb217.0005 nm = Atotal217.0005 nm - A PO217.0005 nm = Atotal217.0005 nm - k (A PO217.0458 nm). The correction factor k is calculated from slopes of calibration curves built up for phosphorous (P) standard solutions measured at 217.0005 and 217.0458 nm, i.e. k = (slope217.0005 nm/slope217.0458 nm). For wavelength integrated absorbance of 3 pixels, sample aspiration rate of 5.0 ml min-1, analytical curves in the 0.1 - 1.0 mg L-1 Pb range with linearity better than 0.9990 were consistently obtained. Calibration curves for P at 217.0005 and 217.0458 nm with linearity better than 0.998 were obtained. Relative standard deviations (RSD) of measurements (n = 12) in the range of 1.4 - 4.3% and 2.0 - 6.0% without and with mathematical equation correction approach were obtained respectively. The limit of detection calculated to analytical line at 217.0005 nm was 10 µg L-1 Pb. Recoveries for Pb spikes were in the 97.5 - 100% and 105 - 230% intervals with and without mathematical equation correction approach, respectively.

Determination of copper at wide range concentrations using instrumental features of high-resolution continuum source flame atomic absorption spectrometry

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324.754 nm, 327.396 nm, 222.570 nm, 249.215 nm and 224.426 nm were evaluated and main figures of merit established. Absorbance measurements at 324.754 nm, 249.215 nm and 224.426 nm allows the determination of Cu in the 0.07 - 5.0 mg L-1, 5.0 - 100 mg L-1 and 100 - 800 mg L-1 concentration intervals respectively with linear correlation coefficients better than 0.998. Limits of detection were 21 µg L-1, 310 µg L-1 and 1400 µg L-1 for 324.754 nm, 249.215 nm and 224.426 nm, respectively and relative standard deviations (n = 12) were £ 2.7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.

Incidência de patógenos e vigor de sementes de milho doce submetidas a danos mecânicos

Com o objetivo de avaliar a incidência de patógenos e o vigor de sementes de milho doce de diferentes classes de tamanhos submetidas a diferentes níveis de danos mecânicos, sementes do híbrido 'SWB551' Dow AgroSciences® foram classificadas em peneiras com crivos de diferentes tamanhos e formas (RG, RM1, RM2 e RP com crivos circulares de 8,7; 7,9; 7,1 e 6,4 mm de diâmetro, respectivamente, e CG, CM e CP com crivos oblongos com dimensões de 8,7 x 19,0, 7,9 x 19,0, 6,4 x 19,0 mm, respectivamente), submetidas a impactos contra uma placa metálica de maneira que fossem obtidos tratamentos com diferentes intensidades de danos mecânicos (0, 1, 3, 5 e 7 impactos) e armazenadas por 5 meses em ambiente com temperatura de 20ºC e 50-60% de umidade relativa do ar. Foi utilizado o delineamento inteiramente casualizado, com quatro repetições, perfazendo um fatorial 7 x 5 (7 peneiras x 5 intensidades de danos), totalizando 35 tratamentos. Foram realizadas as avaliações de teor de água das sementes, teste de danos mecânicos (tintura de iodo), teste de germinação, teste de frio e teste de sanidade. Foram evidenciadas variações nos níveis de incidência de patógenos entre as sementes de milho doce com diferentes tamanhos e formas. O aumento da intensidade dos danos mecânicos não favoreceu o aumento da incidência de patógenos nas sementes, mas reduziu o vigor das mesmas.

Influência da minieataquia seriada no vigor de minicepas de clones de Eucalyptus grandis

Neste estudo objetivou-se avaliar a influência dos subcultivos de miniestaquia seriada na capacidade de produção, vigor e sobrevivência das minicepas de quatro clones de Eucalyptus grandis, nas sucessivas coletas de miniestacas. O jardim miniclonal foi localizado em ambiente coberto por plástico transparente e conduzido em sistema de hidroponia em calhetão. A sobrevivência das minicepas foi superior a 96% após as sete coletas de brotações, para todos os clones e subcultivos. Em relação à produtividade e ao vigor das minicepas, ocorreram variações entre os clones e as coletas estudadas e, de modo geral, a miniestaquia seriada não proporcionou efeitos significativos.

Efeitos do envelhecimento precoce no vigor de sementes de Chorisia speciosa St. Hil. - Bombacaceae

O objetivo deste trabalho foi avaliar a influência do envelhecimento precoce no vigor de sementes de paineira (Chorisia speciosa St. Hil. - Bombacaceae). Adotou-se o método da câmara de envelhecimento (45ºC e 100% de umidade relativa), sendo utilizadas para cada período de envelhecimento (0, 24, 48, 72, 96, 120 e 144 horas) quatro subamostras de 50 sementes, distribuídas em caixas tipo ";gerbox";. Decorridos os períodos de envelhecimento, as sementes foram submetidas às seguintes avaliações: teste de germinação (27 ºC), teste de condutividade elétrica e avaliação de plântulas. Os resultados foram submetidos à análise de variância e ao teste de Tukey. Nos períodos de 48, 72, 96 e 120 horas de envelhecimento, foram obtidos valores estatisticamente inferiores de porcentagem de germinação em relação ao experimento-controle. A permanência das sementes por 144 horas em câmara de envelhecimento levou à perda total da viabilidade. O decréscimo na germinação foi diretamente proporcional ao aumento na lixiviação eletrolítica dos solutos celulares das sementes. A partir de 72 horas de envelhecimento precoce, detectou-se redução significativa na porcentagem de plântulas emergidas. O período de 72 horas de envelhecimento mostrou-se adequado para ser utilizado em trabalhos futuros de avaliação de vigor de sementes de paineira, pois é possível detectar diferenças significativas, em relação ao experimento-controle (sementes não envelhecidas), dos parâmetros porcentagem de germinação, porcentagem de plântulas emergidas e condutividade elétrica.

Influência da miniestaquia seriada no vigor radicular de clones de Eucalyptus grandis

O presente estudo teve por objetivo avaliar a influência da técnica de miniestaquia seriada no vigor radicular das mudas de quatro clones de Eucalyptus grandis. Após a realização de sete subcultivos de miniestaquia, as miniestacas foram enraizadas em condições de casa de vegetação (25 dias), com aclimatação de 10 dias em casa de sombra e avaliação final das mudas realizada aos 50 dias de idade, em pleno sol. De modo geral, os subcultivos de miniestaquia seriada promoveram aumento no número de raízes e proporcionaram maior vigor radicular inicial nos clones de menor potencial de enraizamento, indicando efeito positivo da miniestaquia seriada em clones de Eucalyptus com relação às características.

Vigor de sementes armazenadas de ipê-amarelo Tabebuia serratifolia (Vahl.) Nich

O objetivo deste trabalho foi determinar as melhores condições e períodos de armazenamento adequados a tipos de conservação do vigor das sementes de ipê-amarelo. O experimento foi instalado no Laboratório de Análise de Sementes do CCA/UFPB, seguindo-se um delineamento inteiramente casualizado. Os tratamentos constituíram-se de sementes de ipê-amarelo acondicionadas em dois tipos de embalagens (papel e polietileno); três condições de armazenamento (câmara, laboratório e geladeira); e seis períodos de armazenamento (0, 30, 60, 90, 120 e 150 dias). As características avaliadas foram: teor de água, Índice de Velocidade de Germinação (IVG) e comprimento e massa seca de plântulas. Os resultados de IVG, comprimento e massa seca de plântulas foram submetidos à análise de regressão polinomial. As sementes de ipê-amarelo acondicionadas na embalagem de papel apresentaram maior teor de água ao longo do armazenamento, nos ambientes de câmara e condições normais de laboratório. Em geral, as sementes acondicionadas nas embalagens de papel e polietileno e armazenadas no ambiente de laboratório perderam mais rapidamente o vigor ao longo do armazenamento.

Influência do tamanho e da procedência de sementes Mimosa caesalpiniifolia Benth. Sobre a germinação e vigor

Mimosa caesalpiniifolia Benth. é uma planta nativa da Região Nordeste que vem sendo progressivamente cultivada do Maranhão ao Rio de Janeiro. A planta apresenta grande potencial para arborização, cerca viva e produção de madeira. O presente trabalho teve como objetivo avaliar a influência da procedência e tamanho das sementes sobre a germinação e vigor. Para tanto, realizou-se um experimento no Laboratório de Análise de Sementes do Centro de Ciências Agrárias da Universidade Federal da Paraíba (CCA-UFPB), em Areia, PB, em delineamento experimental inteiramente casualizado com os tratamentos distribuídos em esquema fatorial 3x3, com os fatores procedência (Areia, Usina e Arara) e classes de tamanho (sementes pequenas, médias e grandes), em quatro repetições de 25 sementes. Foram analisadas as seguintes características: peso de 100 sementes, dimensões das sementes (comprimento, largura e espessura), porcentagem, primeira contagem e velocidade de germinação, comprimento e massa seca da raiz primária e hipocótilo e massa seca dos cotilédones. Constatou-se que a germinação não foi influenciada pelo tamanho das sementes, no entanto, ela foi significativamente influenciada pela procedência. Os testes de primeira contagem e de velocidade de germinação não se mostraram adequados para avaliação do vigor das sementes, sendo este mais bem avaliado pela massa seca dos cotilédones e hipocótilo. O vigor das sementes, apresentou relação direta com o seu tamanho, justificando-se a adoção de classes de tamanho para a formação de mudas.