Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination

In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results.

Simultaneous preconcentration of Cu(II), Cd(II) and Mn(II) on silica-polyethylene glycol and determination by flame atomic absorption spectrometry

A simultaneous solid phase extraction procedure for enrichment of Cu(II), Cd(II) and Mn(II) has been developed. The method is based on adsorption of Cu(II), Cd(II) and Mn(II) ions on polyethylene glycol-silica gel pre-conditioned with acetate buffer (pH 5.5). The adsorbed metal ions are eluted with nitric acid (1 mol L -1) and determined by flame atomic absorption spectrometry. The calibration graph was linear in the range of 2-140 ng mL-1 for Cu(II), 1-40 ng mL-1 for Cd(II) and 4-100 ng mL-1 for Mn(II). The limits of detection were 0.66, 0.33 and 1.20 ng mL-1 for Cu(II), Cd(II) and Mn(II), respectively.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

Application of cloud point preconcentration and flame atomic absorption spectrometry for the determination of cadmium and zinc ions in urine, blood serum and water samples

A simple, sensitive and selective cloud point extraction procedure is described for the preconcentration and atomic absorption spectrometric determination of Zn2+ and Cd2+ ions in water and biological samples, after complexation with 3,3',3",3'"-tetraindolyl (terephthaloyl) dimethane (TTDM) in basic medium, using Triton X-114 as nonionic surfactant. Detection limits of 3.0 and 2.0 µg L-1 and quantification limits 10.0 and 7.0 µg L-1were obtained for Zn2+ and Cd2+ ions, respectively. Relative standard deviation was 2.9 and 3.3, and enrichment factors 23.9 and 25.6, for Zn2+ and Cd2+ ions, respectively. The method enabled determination of low levels of Zn2+ and Cd2+ ions in urine, blood serum and water samples.

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.

Sugarcane yellow leaf virus infection leads to alterations in photosynthetic efficiency and carbohydrate accumulation in sugarcane leaves

Infection by Sugarcane yellow leaf virus (ScYLV) causes severe leaf symptoms in sugarcane (Saccharum spp.) hybrids, which indicate alterations in its photosynthetic apparatus. To gain an overview of the physiological status of infected plants, we evaluated chlorophyll a fluorescence and gas exchange assays, correlating the results with leaf metabolic surveys, i.e., photosynthetic pigments and carbohydrate contents. When compared to healthy plants, infected plants showed a reduction in potential quantum efficiency for photochemistry of photosystem (PSII) and alterations in the filling up of the plastoquinone (PQ) pool. They also showed reduction in the CO2 net exchange rates, probably as a consequence of impaired quantum yield. In addition, reductions were found in the contents of photosynthetic leaf pigments and in the ratio chlorophyll a/chlorophyll b (chla/chlb). Carbohydrate content in the leaves was increased as a secondary effect of the ScYLV infection. This article discusses the relation of virus replication and host defense responses with general alterations in the photosynthetic apparatus and in the metabolism of infected plants.

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.

Determination of Hg in water by CVAAS using 2-aminothiazole modified silica

This paper discusses a rapid and sensitive method developed to determine trace levels of mercury in natural water samples by cold vapor atomic absorption spectrometry using a preconcentration system composed by mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT) coupled on-line with the spectrometer's cold vapor generator system. The optimum preconcentration conditions are also described here. The preconcentrated Hg(II) ions were eluted directly from the column to the spectrometer's cold vapor generator system using 100 µL of 2 mol L-1 hydrochloric acid and the retention efficiency achieved exceeded 95%. The enrichment factors determined were 29, 38 and 46 using 3, 4 and 5 mL of preconcentrated aqueous solutions containing 400 ng L-1 of Hg. The detection limit calculated was 5 ng L-1. The preconcentration procedure was applied to determine trace level mercury in spiked river water samples.

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.

Efficiency of phylloplane bacteria in controlling aerial tomato diseases under field conditions

The capacity of two bacteria isolated from the tomato phylloplane to control late blight (Phytophthora infestans) was investigated in the field, and compared against the effectiveness of spraying with the fungicide chlorothalonil (1.5 g a.i. L-1) or water (control). A 55% reduction in late blight intensity was observed in the leaves of the middle of the plant and 62% in those of the upper leaves when using the antagonist UFV-STB 6 (Novosphingobium capsulatum) as compared to the control. Isolate UFV-IEA 6 (Bacillus cereus) was able to reduce disease intensity by 55%, but only in the upper leaves of the tomato plants. Treatment with isolate UFV-STB 6 also led to a significant reduction in the percentage of fruits with late blight symptoms. The results demonstrate the potential of these two bacteria in controlling this disease.