Search results for "Spectroscopy"
showing 10 items of 10293 documents
A clean method for flow injection spectrophotometric determination of cyclamate in table sweeteners
2005
Abstract A flow system based on the multicommutation is proposed for fast and clean determination of cyclamate. The procedure exploits the reaction of cyclamate with nitrite in acidic medium and the spectrophotometric determination of the excess of nitrite by iodometry. The flow system was designed with a set of solenoid micro-pumps to minimize reagent consumption and waste generation. The detection limit was estimated as 30 μmol L −1 (99.7% confidence level) with linear response ranging up to 3.0 mmol L −1 . The coefficient of variation was estimated as 1.7% for a solution containing 2.0 mmol L −1 cyclamate ( n = 20). About 60 samples can be analyzed per hour, consuming only 3 mg KI and 1…
Direct derivative spectrophotometric determination of carbaryl and carbofuran in water samples
1990
Abstract Derivative absorption spectrophotometry has been applied to the direct determination of carbaryl and carbofuran in water samples. The use of the third derivative for carbaryl and the fourth derivative for carbofuran reduces the matrix effect and the seventh derivative provides, in both cases, accurate results for the determination of these pesticides, even working at low dilution levels of the samples. A limit of detection of 4 ppb and a variation coefficient of 0.1% have been obtained for the determination of carbaryl. Carbofuran can be determined with a limit of detection of 5 ppb and a variation coefficient of 0.02%.
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…
Extractive-spectrophotometric determination of amphetamine in urine samples with sodium 1,2-naphthoquinone 4-sulphonate
1993
Abstract Sodium 1,2-naphthoquinone 4-sulphonate (NQS) was tested as a reagent for amphetamine in order to develop an extractive-spectrophotometric method for the drug in urine samples. The standard additions method showed the absence of proportional bias error whereas the Youden method and the two standard addition plots method showed the presence of a constant bias error [total Youden blank (TYB)]. Acceptable results were obtained by evaluating the TYB error or by using a placebo (urine sample from a normal subject). The dynamic range of concentrations was 1.4–50 mg 1−1 in urine samples and the detection limit was 0.6 mg 1−1 when 10 ml of urine sample were taken.
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…
Determination of inorganic species by thermal lens spectrometry
1997
Abstract The application of thermal lens spectrometry (TLS) to the determination of inorganic species is reviewed. The requirements of a chromogenic reaction to be advantageously adapted to TLS detection, and the necessary conditions for reaching very low limits of detection are discussed. Methods for the determination of metals and P, Si, S and N compounds in several samples are examined. Flow-injection and extraction methods, associated photoinduced reactions and surface phenomena, speciation and equilibrium studies are discussed. Gas phase NO 2 methods are also commented upon. Trends are given.
DETECTION LIMITS FOR NATURAL CIRCULAR-DICHROISM OF CHIRAL COMPLEXES IN THE X-RAY RANGE
1993
Whereas both Magnetic Circular Dichroism and Faraday Rotation studies have been successfully carried out at the K-, L- and M-absorption edges of metal atoms in ferromagnetic systems, Natural optical activity of chiral complexes has not yet been detected quite unambiguously in the X-ray range. We review a number of theoretical arguments which confirm that the optical asymmetry factor gσ should be very small in the X-ray range for unoriented powdered samples, especially at the K-absorption edges. This stimulating challenge prompted us to start an intensive programme of measurements aimed at detecting natural circular dichroism in both the soft and “firm” X-ray ranges. Although some of our ex…
Derivatization of tertiary amphetamines with 9-fluorenylmethyl chloroformate for liquid chromatography: determination of N-methylephedrine.
2000
The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) was evaluated for the derivatization of tertiary amphetamines prior to liquid chromatographic analysis. Conditions for the derivatization were investigated, including the reaction time, the derivatization reagent concentration and the pH, using N-methylephedrine as a model compound. On the basis of these studies, a method for the quantification of N-methylephedrine is presented. The method involves derivatization with FMOC at ambient temperature and separation of the derivatives formed on a LiChrospher C18, 5 μm, 125 × 4 mm id column using acetonitrile–water gradient elution. The proposed procedure shows good linearity, accuracy…
Determination of mercury in dry-fish samples by microwave digestion and flow injection analysis system cold vapor atomic absorption spectrometry
1997
Abstract Flow injection analysis system cold vapor atomic absorption spectrometry (FIAS-CV-AAS) preceded by a wet digestion in a microwave oven, as a method for measuring mercury in fish was studied. The digestion process and conditions of the FIAS (carrier concentration: HCl 3% v v ; reducing agent: SnCl2 2% w v : filling and injection times: 8 and 25 min, respectively; and sample volumes) were optimized. The analytical parameters of the proposed method (detection limit = 7.7 ng/g; precision intraassay = 6.7%; interassay = 14.0%) demonstrates its adequacy and are similar to the ones (detection limit = 19.4 ng/g; precision intraassay = 11.2%; interassay = 15.9%) obtained using a conventiona…
Flow injection Fourier transform infrared determination of caffeine in coffee
1999
Abstract A fully automatized procedure has been developed for the Fourier transform infrared (FT-IR) spectroscopic determination of caffeine in coffee samples. The method involves the on-line extraction of caffeine with CHCl3. Samples, weighed inside empty PTFE cartridges of 0.5 cm internal diameter (i.d.) and 1.5 ml volume, were humidified with four drops of 0.25 M NH3. The cartridge was installed in a flow manifold, in which samples were extracted in a closed-flow system with 1 ml CHCl3 during 6 min. Four hundred microliters of the extract were introduced in a microflow cell and absorbance measured as a function of time at 1659 cm−1, with a baseline established between 1900 and 830 cm−1, …