Search results for "Spectroscopy"
showing 10 items of 10293 documents
Flow injection flame atomic absorption analysis of Fe and Mn in cement samples
1993
A new procedure has been developed for the determination of Fe and Mn in cements. It consists in dispersing 50 mg of the solid sample in 25 ml of 0.15 mol/l HNO3 and 0.12 mol/l HCl solution. Acid slurries are heated at 50°C for 10 min and then different volumes of the slurry are injected into a water carrier stream. This previous acid treatment leaches the elements to be determined and permits the use of acid solutions as standards. For the Mn determination, the use of a single line flow injection manifold provides a limit of detection of 0.03 mgl−1 and a dynamic range up to 6 mgl−1. For the determination of Fe, the on-line dispersion of samples, using a well stirred mixing chamber, increas…
Optimization of a microwave-assisted extraction large-volume injection and gas chromatography–ion trap mass spectrometry procedure for the determinat…
2006
Abstract A sensitive and rapid method for the determination of polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs) and polychlorinated naphthalenes (PCNs) in sediment samples is proposed. The method involving microwave-assisted extraction (MAE) and large-volume injection (LVI) gas chromatography (GC)–ion trap mass spectrometry (ITMS), and the experimental conditions were optimized using the statistical design of experiments (DOE). A Plackett–Burman (P–B) design was chosen to estimate the influence of five factors, such as resonance excitation voltage (EV), isolation time (IT), excitation time (ET), ion source temperature (IST) and electron energy (EE) on the analytical r…
New flow-multicommutation method for the photo-chemiluminometric determination of the carbamate pesticide asulam
2004
This paper deals with a straightforward automated method for the determination of asulam in water based on the use of a flow manifold including three computer-controlled solenoid valves. The method involves irradiating on an aqueous solution of asulam in glycine buffer at pH 8.3 with UV light during 90 s, then follows the oxidation with potassium permanganate in a sulphuric medium and chemiluminescence-based detection of the resulting photoproducts. The limit of detection thus achieved is 40 mug l(-1). The detector response is linear up to a 5 mg l(-1) asulam concentration and the throughput is 30 samples h(-1). In parallel tests, oxidation with alkaline ferricyanide was also assessed and t…
The natural compound chrysosplenol-D is a novel, ultrasensitive optical sensor for detection of Cu(II)
2020
Abstract Herein, we introduce a novel, ultrasensitive optical sensor for determination of Cu(II) ions over the concentration range of 0 to 1 μM Cu(II). The optical sensor is based on the natural molecule chrysosplenol-D (Chp-D) extracted from the flowering plant Chiliadenus montanus (Vahl.) Brullo. Free Chp-D emits fluorescence at 566 nm when excited at 292 nm. Chp-D chelates Cu(II) ions to form a 1:1 (metal:ligand) complex, which quenches the fluorescence emission peak of the free probe at 566 nm. “Turn-off” luminescence could be easily determined and provided distinct proof of the chelation of Cu(II) ions by Chp-D. This novel optical sensor offers a considerable fluorescence mechanism (ch…
Improvement of the detection limit for determination of 129I in sediments by quadrupole inductively coupled plasma mass spectrometer with collision c…
2004
The previously developed sample introduction device for the hot extraction of iodine from environmental samples (soils or sediments) and on-line introduction of analyte via the gas phase in quadrupole inductively coupled plasma mass spectrometry with hexapole collision cell (ICP-CC-QMS) was equipped with a cooling finger, which allowed intermediate iodine enrichment and improved the detection limits for I-129 down to 0.4 pg g(-1) without any additional sample preparation. A mixture of oxygen and helium as reaction gases in the hexapole collision cell was used for reducing the disturbing background intensity of Xe-129(+). Oxygen was also used as the carrier gas for iodine thermal desorption …
Determination of chromium(III) and chromium(VI) in mineral water by bidirectional electrostacking and electrothermal atomic absorption spectrometry
2001
Abstract A feasibility investigation was carried out on the use of bidirectional electrostacking for simultaneous separation and pre-concentration of Cr(III) and Cr(VI) and their electrothermal atomic absorption spectrometry (ETAAS) determination. The bidirectional electrostacking manifold was improved, and the effects of sample tube cross-section and electrostacking time on the pre-concentration factor were investigated. Results indicate that the sample tube cross-section and electrostacking time are the main influence factors on the electrostacking pre-concentration, as well as the electric field strength and ionic mobility. The method developed was suitable for the simultaneous separatio…
Multicommutation Fourier transform infrared determination of benzene in gasoline
2004
A fully mechanized method to determine benzene in motor gasolines has been developed based on the use of Fourier transform infrared spectroscopy (FT-IR) and multicommutation. The flow network comprised a set of three-way solenoid valves and was controlled by means of a microcomputer furnished with an electronic interface and running by a software written in QUICK BASIC 4.5. The flow network and control software were designed to implement the multicommutation approach providing facilities to handle sample and reagent solutions, so that, sample dilution, external calibration and standard addition could be easily performed on-line. The method permits the direct determination of benzene without…
Determination of Concentration Profiles of Methyl Mercury Compounds in Surface Waters of Polar and other Remote Oceans by GC-AFD
1998
Abstract The concentration of monomethyl mercury (MeHg+) and dimethyl mercury (Me2Hg) was determined in surface sea-water samples of the Antarctic and Arctic Ocean as well as of other remote areas (South Atlantic and South Pacific) during expeditions of the German research vessel “Polarstern”. A purge and trap/gas chromatographic system, equipped with an atomic fluorescence detector (AFD), was used. For the analysis of MeHg+ conversion into the volatile methylethyl mercury by reaction with tetraethyloborate prior to the purging process was carried out. The detection limit for both methylated mercury compounds was 5 pg Hg/L, which allowed their determination in most ocean water samples even …
Atomic absorption spectrometric determination of molybdenum in lubricating oils with use of emulsions
1985
Abstract Samples (0.1 g) containing molybdenum disulphide are digested with aqua regia or with a (1 + 1) hydrofluoric/nitric acid mixture, without complete destruction of the matrix, and the molybdenum is determined in an air/acetylene flame, after emulsification with a non-ionic surfactant (Nemol K-39). The detection limit is ca. 30 μg Mo g−1, and the r.s.d. is 2.9% for 6 analyses of a sample containing 6.5 mg Mo g−1.
On-line microwave oven digestion flame atomic absorption analysis of solid samples
1990
Abstract A manifold has been developed for on-line microwave oven digestion and flame atomic absorption spectrometric (FAAS) determination of metallic elements in solid samples. The use of a closed flow system permits sample treatment before analysis by FAAS, the direct injection of slurries avoids a filtration step and the interconnection of two conventional rotary injection valves allows the rapid introduction of samples and standards. The determination of lead in sewage sludge was employed as a test system for the proposed on-line sample digestion manifold. The procedure has a limit of detection of 0.2 μg Pb g−1.