Ultra-trace monitoring of copper in environmental and biological samples by inductively coupled plasma atomic emission spectrometry after separation and preconcentration by using octadecyl silica membrane disks modified by a new schiff's base

Ultra-trace amounts of Cu(II) were separated and preconcentrated by solid phase extraction on octadecyl-bonded silica membrane disks modified with a new Schiff,s base (Bis- (2-Hydroxyacetophenone) -2,2-dimethyl-1,3-propanediimine) (SBTD) followed by elution and inductively coupled plasma atomic emission spectrometric detection. The method was applied as a separation and detection method for copper(II) in environmental and biological samples. Extraction efficiency and the influence of sample matrix, flow rate, pH, and type and minimum amount of stripping acid were investigated. The concentration factor and detection limit of the proposed method are 500 and 12.5 pg mL-1, respectively.

Identificação e quantificação do cristal violeta em aguardentes de mandioca (tiquira)

Tiquira is a traditional homemade alcoholic distillate produced in the Maranhão State (Brazil), gotten from cassava (Manihot esculenta, Crantz.). It can be normally found on street markets. Due to the addition of tangerine leaves, the original tiquira has a bluish color. Samples of this beverage were acquired in the local trade and analyzed from the spectroanalytical point of view. The results indicated that these drinks had been adulterated by the addition of crystal violet, a potencialy hazardous compound. The identification and quantification of crystal violet in 10 spiked samples was accomplished by UV-Vis spectrophotometry through the standard addition method. In order to verify the efficiency of the proposed method, experiments on the quantification and recovery were carried out and the results indicated a content of crystal violet in the 10-6 to 10-7 mol L-1 range.

Bauer-7-en-3beta-yl acetate: a major constituent of unusual samples of Brazilian propolis

The pentacyclic triterpenoid bauer-7-en-3beta-yl acetate was obtained from the chloroform extract of an unusual sample of propolis from southeast Brazil with the yield of 7%. The compound was identified by comparison of IR, MS and NMR analysis with published data.

Removal of chromium (vi) in aqueous environments using cork and heat-treated cork samples from quercus cerris and quercus suber

Chromium (VI) removal and its reduction to chromium (III) from aqueous solution by untreated and heat-treated Quercus cerris and heat-treated Quercus suber black agglomerate cork granules was investigated. Initial screening studies revealed that among the sorbents tested, untreated Q. cerris and Q. suber black agglomerate are the most efficient in the removal of Cr(VI) ions and were selected for adsorption essays. Heat treatment adversely affected chromium adsorption and chromium (VI) reduction in Q. cerris cork. The highest metal uptake was found at pH 3.0 for Q. cerris and pH 2.0 for black agglomerate. The experimental data fitted the Langmuir model and the calculated qmax was 22.98 mg/g in black agglomerate and 21.69 mg/g in untreated Q. cerris cork. The FTIR results indicated that while in black agglomerate, lignin is the sole component responsible for Cr(VI) sorption, and in untreated Q. cerris cork, suberin and polysaccharides also play a significant role on the sorption. The SEM-EDX results imply that chromium has a homogenous distribution within both cork granules. Also, phloemic residues in Q. cerris granules showed higher chromium concentration. The results obtained in this study show that untreated Q. cerris and black agglomerate cork granules can be an effective and economical alternative to more costly materials for the treatment of liquid wastes containing chromium

Determination of chemical elements in africanized Apis mellifera (Hymenoptera: Apidae) honey samples from the State of Piauí, Brazil

Honey is a food used since the most remote times, appreciated for its characteristic flavor, considerable nutritional value and medicinal properties; however, little information exists about the presence of chemical elements in it. The objectives of this work were to determine the chemical elements present in 38 honey samples, collected directly from beekeepers from the State of Piauí, Brazil and to verify whether they presented any contamination. The chemical elements were determined by means of Total Reflection X-ray Fluorescence. The means of three replicates were: K (109.671 ± 17.487), Ca (14.471 ± 3.8797), Ti (0.112 ± 0.07), Cr (0.196 ± 0.11), Mn (0.493 ± 0.103), Fe (1.722 ± 0.446), Co (0.038), Ni (0.728 ± 0.706), Cu (0.179 ± 0.0471), Zn (0.967 ± 0.653), Se (not detected), Br (not detected), Rb (0.371 ± 0.097), Sr (0.145 ± 0.45), Ba (11.681), Hg (not detected), and Pb (0.863) µg g-1.

Physicochemical composition of Apis mellifera honey samples from São Paulo State, Brazil

This research, developed with Apis mellifera honey samples from producers of São Paulo State, Brazil, has the objective of verifying how eucalyptus, wild flower, and orange honey samples would be clustered, based on physicochemical characteristics. All the orange honey samples and some wild flower ones formed distinct groups, thus confirming that the floral source interferes with honey characteristics. Eucalyptus and some of the wild flower honey samples were clustered together because of the great floral source variation in the latter ones. The characteristics that influence sample clustering are acidity and electric conductivity on the X axis, and total sugars and pH on the Y axis.

Determinação da diferença entre o valor real e o teórico do triglicerídeo ECN 42 para a detecção de adulteração em azeites de oliva comercializados no Brasil

The difference between the actual ECN 42 triacylglyceride content in vegetable oils, obtained by HPLC analysis, and the theoretical value calculated from the fatty acid composition was applied to detect the addition of seed oils with high contents of linoleic acid to olive oils commercialized in Brazil. The results indicate that samples analyzed were probably adulterated with low commercial value seed oils, rich in linoleic acid, like soybean, sunflower or corn.

Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU), copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4) of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH) in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(a)pyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

Stability of antioxidants vitamins in bee pollen samples

This study evaluated the stability of vitamins C, E and β-carotene in six samples of bee pollen after their process, and in a one-year period of storage. After the pollen's process, there was a 67.1% increase for vitamin C (p <0.05), an 18.7% loss for vitamin E and 15.6% for β-carotene. Storage in freezer was the most efficient condition for the vitamins conservation; the loss in storage at room temperature (exposed or protected from light) was similar. Vitamin E appears to be better preserved during storage when compared to vitamin C and β-carotene.

Determination of aluminum in food samples after preconcentration as aluminon complex on microcrystalline naphthalene by spectrophotometry

A sensitive preconcentration procedure for spectrophotometeric determination of aluminum was developed. Aluminum as aluminon complex is adsorbed on microcrystalline naphthalene. The naphthalene containing the complex is dissolved in 3 mL of acetone and its absorbance is measured at 544 nm. The effect of various factors on the preconcentration of aluminum was investigated. The calibration graph was linear in the range of 1-60 mg L-1. The limit of detection was 0.52 mg L-1 and relative standard deviation for the determination of 5 mg L-1 was 2.65%. The proposed solid phase extraction procedure was applied to determination of aluminum in food samples.

Determination of traces of nitrate in water samples using spectrophotometric method after its preconcentration on microcrystalline naphthalene

Nitrate is quantitatively retained with 2,6-bis(4-methoxyphenyl)-4-phenyl pyrylium perchlorate (PPP) on microcrystalline naphthalene in the pH range of 6.5-9.0 from a large volume of aqueous solutions of various samples. The method was based on the complexation between PPP and nitrate and then, extraction of the resulted complex from aqueous solution by microcrystalline naphthalene. The solid mass consisting of the nitrate complex and naphthalene was then dissolved in dimethyl formamide (DMF) and absorption of the resulted solution was obtained at 328 nm. The linear calibration range for the determination of nitrate was 15-135 μg L-1 with the detection limit of 10 μg L-1.

Ion pair-dispersive liquid-liquid microextraction of trace amount of rhodium ion in water and road dust samples prior to flame atomic absorption spectrometry determination

A simple ion pair-dispersive liquid-liquid microextraction method was proposed for preconcentration trace amounts of rhodium. An ion association complex of RhCl4- and tetradecyldimetylbenzylamonium was extracted into cholorobenzene. The volume and the type of extractive and dispersive solvents, the extraction time and the pH of the aqueous solutions were optimized. The calibration curve was linear in the range of 0.6-500 ng mL-1 of rhodium. The limit of detection was 0.10 ng mL-1 in initial solution and preconcentration factor was 40. The proposed method was successfully applied to the extraction and determination of rhodium in road dust and water samples.

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.