Determination of ambroxol in syrups using diffuse reflectance spectroscopy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Determination of herbicides residues in soil by small scale extraction

Herbicidas tais como trifluralina, simazina, atrazina, metribuzina e metolaclor são usados na agricultura brasileira. A eficiência de um método em pequena escala para a determinação destes herbicidas e dois produtos de degradação em amostras de solo foi avaliada. Os compostos foram extraídos das amostras de solo (5 g) com 20 ml de acetato de etila em agitador mecânico por 50 min. Após a extração, o sobrenadante foi filtrado em sulfato de sódio anidro, concentrado e analisado por cromatografia a gás de alta resolução com detector termiônico específico. Valores médios de recuperação obtidos de amostras de solo fortificadas em três níveis diferentes variaram de 81 a 115 % com valores de desvio padrão relativo entre 1,2 e 12,7 %. Os limites de detecção do método variaram de 0,01 a 0,06 mg kg-1. A metodologia foi aplicada a amostras de solo de fazendas localizadas próximas à cidade de Araraquara, estado de São Paulo, Brasil.

Gravimetric determination of soil organic matter

Avaliou-se o método de determinação gravimétrica da matéria orgânica do solo pela perda de massa por incineração a 300ºC e comparou-se com o carbono determinado pelo método Walkley-Black. Os dois métodos foram correlacionados positivamente com a seguinte equação de regressão linear: y = 3,720x + 0,2914. r = 0,937. O coeficiente. 3,720 foi maior do que os encontrados na literatura. que variaram de 1,68 a 2,13. Esta diferença foi atribuída ao maior grau de oxidação da matéria orgânica dos solos das regiões tropicais. O método de incineração é aplicável para determinação do C do solo em rotina. O método não contamina o meio ambiente com metal tóxico (Cr6+) e não oferece riscos aos analistas com o uso de ácido sulfúrico concentrado.

Determination of a point sufficiently close to the asymptote in nonlinear growth functions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Cathodic stripping voltammetric determination of ceftazidime in urine at a hanging mercury drop electrode

A method was developed for the differential-pulse cathodic stripping voltammetric determination of ceftazidime with a hanging mercury drop electrode using its reduction peak at -0.43 V in Britton-Robinson buffer pH 4.0. The optimum accumulation potential and time were -0.15 V and up to 60 s, respectively. Linear calibration graphs were obtained from 1 x 10(-8) M and 1.5 x 10(-7) M. The limit of determination was calculated to be 5 x 10(-9) M. The coefficient of variation was 4% (n = 7) at 1 x 10(-7) M ceftazidime. The effect of various components of urine on the voltammetric response was studied, and creatinine, uric acid, urea, and glucose were shown to interfere in the method. Ceftazidime bound to human albumin gives a unique stripping peak at -0.48 V. Recoveries of 87% +/- 2% of the ceftazidime (n = 5) were obtained from urine spiked with 1.27 mu g ml(-1) using C-18 solid phase extraction cartridges. (C) 1997 Academic Press.

Rapid determination of furanocoumarins in creams and pomades using SPE and GC

A solid-phase extraction and chromatography-flame ionization detection (GC-FID) method has been developed for the routine analysis of psoralen, bergapten, isopimpinellin and pimpinellin in creams and pomades employed in Brazil for the treatment of vitiligo. The calibration curve for psoralen was linear in the range 10-100 mu g ml(-1), for bergapten 5-90 mu g ml(-1), for pimpinellin 10-90 mu g ml(-1) and for isopimpinellin 5-100 mu g ml(-1). The best recoveries of the furanocoumarins in the creams analysed were 94-97%, whereas in the pomades, recoveries were 94-96%. The R.S.D. of the quantitative analysis of the furanocoumarins in the products analyses were within 5%. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Asymmetrical penetration of microwave in a conducting media and determination of microwave conductivity for very thin samples using electron spin resonance

Dyson's theory of conduction electron spin resonance (CESR) has been used in the limit d less than or equal to delta (d being the thickness of the sample and delta the skin depth of the microwave field) to obtain the microwave conductivity from the (A/B) ratio of the CESR absorbed power derivative. In this work we calculate the CESR absorbed power derivative using Kaplan's approach and show that the (A/B) ratio can be enhanced if asymmetrical penetration of microwave is used, which means that the microwave field enters into the sample from one of the faces. Therefore, the determination of the microwave conductivity from the (A/B) ratio of the CESR line can be performed for thinner samples. Experimentally, asymmetrical penetration can be obtained if one of the sample's faces is covered with a thin gold layer. The determination of microwave conductivity in conducting polymers films is among the possible applications of this method. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Colorimetric determination of formaldehyde in air using a hanging drop of chromotropic acid

A simple and sensitive method to determine parts per billion (ppb) of atmospheric formaldehyde in situ, using chromotropic acid, is described. A colorimetric sensor, coupled to a droplet of 15.5 muL chromotropic acid, was constructed and used to sample and quantify formaldehyde. The sensor was set up with two optical fibers, a right emitting diode (LED) and two photodiodes. The reference and transmitted light were measured by a photodetection arrangement that converts the signals into units of absorbance. Air was sampled around the chromotropic acid droplet. A purple product was formed and measured after the sampling terminated (typically 7 min). The response is proportional to the sampling period, analyte concentration and sample flow rate. The detection limit is similar to2 ppb and can be improved by using longer sampling times and/or a sampling flow rate higher than that used in this work, 200 mL min(-1). The present technique affords a simple, inexpensive near real-time measurement with very little reagent consumption. The method is selective and highly sensitive. This sensor could be used either for outdoor or indoor atmospheres.

Determination of brilliant blue FCF in the presence and absence of erythrosine and quinoline yellow food colours by cathodic stripping voltammetry

A study of the voltammetric behaviour of the food colours brilliant blue FCF (C.I. 42090), erythrosine (C. I. 45430) and quinolin e yellow (C. I. 47005) in the pH range 2-10 have been carried out by cathodic stripping voltammetry. At pH 4.5 (acetate buffer) with an accumulation potential of 0 V and accumulation time of 30 s, the voltammograms presented well-defined reduction peaks at potential - 0.76 V for brilliant blue FCF, - 0.85 V for quinoline yellow and - 0.54 V for erythrosine. Linear calibration graphs were obtained from 8 to 80 mug l(-1) brilliant blue, from 4 to 43 mug l(-1) quinoline yellow and from 10 to 70 mug l(-1) erythrosine. The method has been successfully applied to identify and quantify binary mixtures of these dyes and applied for determining brilliant blue FCF in commercial food products.

Cathodic stripping voltammetric detection and determination at a hanging mercury-drop electrode of dye contaminants in purified biomaterials: study of the human serum albumin and reactive dye 120 system

Procion red HE-3B (RR120) is an example of dye currently used in affinity purification. A method is described for determining trace amounts of RR120 dye contaminant in human serum albumin by cathodic stripping voltammetry. The method is based on a measure of a well-defined peak at -0.58 V, obtained when samples of HSA protein (0.01-2% w/v) containing dye concentrations are submitted to a heating time of 330 min at 80degreesC in NaOH, pH 12.0 and the samples are removed to a solution containing Britton-Robinson buffer, pH 4.0. Using an optimum accumulation potential and tune of 0 V and 240 s, respectively, linear calibration curves were obtained from 1.0 X 10(-9) to 1.0 X 10(-8) mol 1(-1) for RR120 dye. Leakage/hydrolysis of reactive red 120 from an agarose support (e.g. at pH 2 or 12) can also be conveniently determined at very low levels (sub-mug ml(-1)) by means of cathodic stripping voltammetry, which involves adsorptive accumulation of the dye onto the hanging mercury-drop electrode. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Evaluation and application of bismuth as an internal standard for the determination of lead in wines by simultaneous electrothermal atomic absorption spectrometry

A method for the direct determination of Pb in wines by simultaneous multi-element atomic absorption spectrometry (SIMAAS) using a transversely heated graphite atomizer, Zeeman-effect background corrector and internal standardization is proposed. Bismuth was used as an internal standard and Pd(NO3)(2) plus Mg(NO3)(2) as chemical modifier,to stabilize both the analyte and the internal standard. The implementation of two pyrolysis steps avoided any build-up of carbonaceous residues on the graphite platform. All diluted samples (1 + 1 v/v) in 0.2% v/v HNO3 and reference solutions (5.0-50 mug l(-1) Ph in 0.2% v/v HNO3) were spiked with 25 mug l(-1) Bi. For a 20 mul aliquot dispensed into the graphite tube, a good correlation (r = 0.9997) was obtained between the ratio of the analyte signal to the internal standard signal and the analyte concentration of the reference solutions. The electrothermal behaviour of Pb and Bi in red, white and rose wines were compared. In addition, absorbance variations due to changes in experimental conditions, such as atomizer temperature, integration time, injected sample volume, radiation beam intensity, graphite tube surface, dilution and sample composition, were minimized by using Bi as internal standard. Relative standard deviations of measurements based on integrated absorbance varied from 0.1 to 3.4% and from 0.5 to 7.3% (n = 12) with and without internal standard correction, respectively. Good recoveries (91-104%) for Pb spikes were obtained. The characteristic mass was 45 pg Pb and the limit of detection based on integrated absorbance was 0.9 mug l(-1) Pb. Internal standardization increased the lifetime of the tube by 25%. Direct determinations of Pb in wines with and without internal standardization approaches were in agreement at the 95% confidence level. The repeatability and the tube lifetime were improved when using Bi as internal standard. The improvement in accuracy using an internal standard was only observed when the analytical results were affected by errors.

Indirect cathodic-stripping voltammetric determination of ceftazidime as a mercury salt

At accumulation potentials close to +0.1 V at a hanging mercury drop electrode, ceftazidime is accumulated at pH 9.5, probably in a hydrolysed or otherwise chemically altered form, in an anodic process to give an adsorbed mercury salt. The accumulation of this mercury salt allows the indirect cathodic-stripping voltammetric determination of ceftazidime using the reduction peak of the mercury salt at -0.70 V. The high sensitivity of the method coupled with high sample dilution allows ceftazidime to be determined in milk samples at the 28 mu g ml(-1) level without prior separation. In order to determine lower levels of ceftazidime in milk (ca. 10 ng ml(-1)) a separation process would be required. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Flow-injection spectrophotometric determination of methyldopa in pharmaceutical formulations

A flow-injection spectrophotometric procedure is proposed for methyldopa determination in pharmaceutical preparations. The determination is based on formation of a yellow product (measured at 410 nm) after complexation of methyldopa with molybdate. Under optimal conditions, Beer's law is obeyed in a concentration range of 50-200 mg l(-1) methyldopa. Typical correlation between absorbance and analyte concentration was 0.9999. Usual excipients used as additives in pharmaceuticals do not interfere with the proposed method. The analytical frequency was 210 h(-1) and the relative standard deviation (R.S.D.) was <= 2% for sample solution containing 150 mg l(-1) methyldopa (n = 11). The analytical results obtained in commercial formulations by applying the proposed FIA method were in good agreement with labeled values and those obtained by the Brazilian Pharmacopoeia procedure at 95% confidence level. (C) 2005 Elsevier B.V. All rights reserved.

DIRECT EXPRESSIONS FOR OGATA LEAD-LAG DESIGN METHOD USING ROOT LOCUS

Direct expressions for the design of a lead-lag continuous compensator using the root locus method and the procedure described in the 1970 and 1990 books by Ogata are presented. These results are useful in the Ogata design method because they avoid the geometrical determination of poles and zeros, making it easier to create a computer-based design.

Electrothermal AAS determination of Ni in soft drinks using Co as the internal standard

A method for the direct determination of Ni in soft drinks by graphite furnace atomic absorption spectrometry using a transversely heated graphite atomizer (THGA), Zeeman-effect background corrector, and Co as the internal standard (IS) is proposed. Magnesium nitrate was used to stabilize both Ni and Co. All diluted samples (1+1) in 0.2% (v/v) HNO3 and reference solutions [5.0-50 mu g L-1 Ni in 0.2% (v/v) HNO3] were spiked with 50 mu g L-1 Co. For a 20-mu L sample dispensed into the atomizer, correlations between the ratio of absorbance of Ni to absorbance of Co and the analyte concentration were close to 0.9996. The relative standard deviation of the measurements varied from 0.5 to 3.4% and 1.0 to 7.0% (n=12) with and without IS, respectively. Recoveries within 98-104% for Ni spikes were obtained using IS. The characteristic mass was calculated as 43 pg Ni and the limit of detection was 1.4 mu g L-1. The accuracy of the method was checked for the direct determination of Ni in soft drinks and the results obtained with IS were better than those without IS.