Search results for "deviation"
showing 10 items of 367 documents
Flow analysis-spectrophotometric determination of ?-dopa in pharmaceutical formulations by reaction with p-Aminophenol
1994
Abstract A new method has been developed for the spectrophotometric determination of l -dopa in pharmaceutical formulations. The method is based on the reaction between the open-chain quinone of l -dopa, obtained in NaOH, and the benzoqinoneimine form of p-aminophenol, in the presence of KIO4. The reaction product is determined at 574 nm by using both alternately procedures, one based on the stopped-flow and another on a flow injection approach. Under the best experimental conditions L-dopa can be determined with a limit of detection of 52 ng/ml and a relative standard deviation of 0.2% for three replicate measurements of a solution containing 4 μg/ml.
Rapid microwave assisted hydrolysis of formetanate
1993
Abstract A fast microwave-assisted hydrolysis procedure has been developed for the derivatization of formetanate previously to the flow-injection spectrophotometric determination of m -aminophenol by reaction with p -aminophenol. Formetanate is quantitatively hydrolyzed with 0.1 M NaOH in 150 s using a closed polyetrafluoroethylene reactor with 115 ml internal volume and a radiation power of 390 W. The above procedure has been applied, as a previous step, for the flow-injection spectrophotometric determination of formetanate in spiked water samples and accurate and precise results have been found. The method permits to obtain a limit of detection of 0.025 mg 1 −1 of formetanate. The relativ…
HPLC determination of oxadiazon in commercial pesticide formulations
2008
A simple, fast and precise high performance liquid chromatographic (HPLC) procedure has been developed for the determination of oxadiazon in emulsifiable concentrated pesticide formulations. 20 µL of diluted sample in acetonitrile were injected in a Kromasil C18 (250 ×am injetados em uma coluna Kromasil C18 4.6 mm, 5 µm) column, using acetonitrile:water (80:20) as mobile phase at 1 mL min-1 flow rate and oxadiazon determined by absorbance measurement at 292 nm. A theoretical limit of detection of 0.02 µg mL-1, a limit of quantification of 0.047 µg mL-1, corresponding to a 0.02 and 0.07% m/v in the original sample, and a relative standard deviation of 0.08% for three replicate analysis of sa…
Simultaneous determination of hydride and non-hydride forming elements by inductively coupled plasma optical emission spectrometry
2011
e percentagens de recuperacao entre 97 e 103%. A aplicabilidade do sistema foi demonstrada na determinacao simultânea de Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Zn, As, Bi, Sb, Se e Te em amostras certificadas para elementos tracos, NIST 1549 (leite em po desnatado), NIST 1570a (folhas de espinafre), DORM-2 (musculo de cacao) e TORT-2 (hepatopâncreas de lagosta). Os resultados obtidos foram concordantes com os teores certificados. The operating characteristics of a dual nebulization system were studied including instrumental and chemical conditions for the hydride generation and analytical figures of merit for both, hydride and non hydride forming elements. Analytical performance of the neb…
Non-chromatographic speciation of mercury in mushrooms
2016
A fast, sensitive and cheap procedure has been developed for the determination of inorganic mercury (i-Hg) and organic mercury (o-Hg) in mushroom samples. The procedure is based on the use of cold vapour atomic fluorescence spectrometry (CV-AFS). The method involves the extraction of total mercury (t-Hg) with diluted HCl, followed by measurements of the corresponding Hg vapour under two different conditions: (i) directly to determine i-Hg, and (ii) after oxidation with a mixture KBr/KBrO3 to determine t-Hg. o-Hg was estimated from the difference between t-Hg and i-Hg. Previous studies were focused on the assessment of different reagents for mercury extraction and breakdown of organomercury …
Vanadium and molybdenum concentrations in particulate from Palermo (Italy): analytical methods using voltammetry
2014
The main purpose of this work was to develop a reliable method for the determination of vanadium (V) and molybdenum (Mo) in atmosphere particles or aerosols because they can not be readily measured using conventional techniques. For this research, 30 particulate samples were collected from five different stations located at Palermo, Italy. We used the catalytic adsorptive stripping voltammetry and differential pulsed voltammetry to measure Vand Mo in atmospheric particulate, respectively. The represented method includes advantages of high sensitivity, high selectivity, simplicity, reproducibility, speed and low costs. The quantification limits for V and Mo are, respectively, 0.57 and 0.80 n…
Multi-pumping mechanised determination of selenium in natural waters by light emitting diode (LED) spectrometry
2009
It has been developed a fully mechanised procedure for the determination of selenium in waters employing a LED based spectrometer and solenoid multi-pumps as solution propelling devices. The proposed method is based on the reaction of selenium with potassium iodide in an acidic medium to liberate iodine, which oxidizes Variamine Blue to form a violet-colour species which absorb at 530 nm. The system was mechanised using the multicommutation process and a stopped flow strategy in the final step reaction. The analytical curve was linear between 0.010 and 0.500 mg L-1, with an equation ΔA = 0.501 (± 0.004) C and r = 0.999. The limit of detection (3σ/S) obtained for the proposed method was 0.00…
Analysis of insoluble silicate: Decomposition with molten sodium hydroxide and determination of Zr(IV) with chloranilic acid in medium-strong acid
1983
A rapid, accurate and precise method for the determination of zirconium in silicates is proposed. Insoluble or sparingly soluble samples are decomposed by means of molten sodium hydroxide. Chloranilic acid is employed as reagent for the spectrophotometric determination of Zr(IV). The limit of detection is 1.2×10−7 M and the relative standard deviation is 0.24%.
A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos.
2005
Abstract A FTIR methodology has been developed for the simultaneous determination of Cypermethrin and Chlorpyrifos in pesticide commercially available formulations. The method involves the extraction of both active principles with CHCl3 and direct measurement of the peak area values between 1747 and 1737 cm−1 corrected with a baseline defined at 2000 cm−1 for Cypermethrin and peak height values established at 1549 cm−1 corrected using a baseline situated at 1650 cm−1 for Chlorpyrifos. The limits of detection achieved were of the order of 0.7 and 0.4% (w/w), and the relative standard deviation 0.4 and 0.2% for Cypermethrin and Chlorpyrifos, respectively. The developed procedure provided stat…
Determination of As, Sb, Se, Te and Bi in milk by slurry sampling hydride generation atomic fluorescence spectrometry
2003
A simple and fast analytical procedure has been developed for the determination of As, Sb, Se, Te and Bi in milk samples by hydride generation atomic fluorescence spectrometry (HG-AFS). Samples were treated with aqua regia for 10min in an ultrasound water bath and pre-reduced with KBr for total Se and Te determination or with KI and ascorbic acid for total As and Sb, the determination of Bi being possible in all with or without pre-reduction. Slurries of samples, in the presence of antifoam A, were treated with NaBH(4) in HCl medium to obtain the corresponding hydrides, and AFS measurements were processed in front of external calibrations prepared and measured in the same way as samples. Re…