Search results for "Spectroscopy"
showing 10 items of 10293 documents
Spark source mass spectrometric assessment of boron and nitrogen concentrations in crystalline gallium arsenide
1999
The residual or doped element concentration [E] in GaAs measured by SSMS is only accurate with respect to the relative sensitivity coefficient RSCE. For a trace element concentration, the RSCE = [E]SSMS/[E]TRUE is set to unity, if no reference material or method is available to approximate the concentration to the true value. For boron a relative sensitivity coefficient of RSCB = 0.94 ± 0.08 was obtained using TI-IDMS as a reference method. RSCN = 1 is used for nitrogen determinations. A boron and nitrogen detection limit of 4.4 × 1013 cm–3 is achieved. SSMS was used as reference method to calibrate the FTIR factor fE = [E] / Iα due to the integrated local vibrational mode absorption Iα of …
Direct FIA—AS determination of potassium and magnesium in cement samples by use of the slurries approach
1992
A direct procedure has been developed for the flame atomic determination of potassium and magnesium in cement samples. A 50-mg sample is dispersed in 25 ml of 0.13M nitric acid; 100 mul of this slurry is injected in a double channel FIA manifold simultaneously with 100 mul of a 10% (w/v) lanthanum solution. This procedure allows the rapid extraction of potassium and magnesium by leaching of the sample; nitric acid is not necessary if only potassium must be determined and the sample can be diluted with only distilled water. Aqueous standards are used. The manifold employed includes a well-stirred mixing chamber, which provides an adequate on-line dilution of the sample, in order to obtain em…
On-line gel permeation chromatography–attenuated total reflectance–Fourier transform infrared determination of lecithin and soybean oil in dietary su…
2007
Gel permeation chromatography (GPC) with attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectrometry detection has been proposed for the simultaneous determination of lecithin and soybean oil in dietary supplements. The method involves the extraction of analytes with dichloromethane in an ultrasound water bath and the injection of 2 ml of centrifuged and filtered extracts into the system integrated by two Envirogel GPC columns (19 mm x150 mm, 19 mm x 300 mm) coupled on-line. Dichloromethane was used as mobile phase. A method has been developed to select the most appropriated wavenumber to be used for the determination of each considered compound from the calculation of a…
Active alkaline traps to determine acidic-gas ratios in volcanic plumes: Sampling techniques and analytical methods
2014
In situ measurements have been the basis for monitoring volcanic gas emissions for many years and—being complemented by remote sensing techniques—still play an important role to date. Con- cerning in situ techniques for sampling a dilute plume, an increase in accuracy and a reduction of detection limits are still necessary for most gases (e.g., CO2, SO2, HCl, HF, HBr, HI). In this work, the Raschig-Tube tech- nique (RT) is modified and utilized for application on volcanic plumes. The theoretical and experimental absorption properties of the RT and the Drechsel bottle (DB) setups are characterized and both are applied simultaneously to the well-established Filter packs technique (FP) in the …
Atomic fluorescence determination of inorganic arsenic in soils after microwave-assisted distillation
2000
Abstract An inexpensive microwave-assisted distillation procedure has been developed for quantitative determination of inorganic arsenic in soils by atomic fluorescence spectrometry (AFS). After reduction of As(V) to its trivalent state with potassium iodide, inorganic arsenic was distilled as AsCl 3 that was finally determined by atomic fluorescence after hydride generation with NaBH 4 in HCl medium. The different parameters that control the distillation: concentration and volume of HCl, time of distillation, sample weight, and oven load, were studied. The methodology developed has a detection limit of 0.015 μg l −1 , which corresponds to a concentration of 0.006 μg of As per gram of soil,…
On-line bi-directional electrostacking for As speciation/preconcentration using electrothermal atomic absorption spectrometry.
2006
A method using bi-directional electrostacking (BDES) in a flow system is presented for As preconcentration and speciation analysis. Some parameters such as electrostacking time and applied voltage, support buffers and their concentrations were investigated. Boric acid plus sodium hydroxide at 0.1mol/l concentration was selected as support buffer to improve the pre-concentration factor (PF) for As(V). An analytical range from 2.0 to 50.0mugl(-1), and 0.35mugl(-1) as limit of detection, when applied 750V for 20min, were achieved. Under these conditions, a pre-concentration factor of 4.8 was obtained. The proposed method was applied to determine As(V) in mineral water and natural water samples…
Thermal lens spectrometric determination of cerium with oxine
1991
Abstract The spectrophotometric and photothermal (TLS) procedures for cerium determination using 8-hydroxyquinoline (oxine), after extraction into chloroform, are compared. Photothermal measurements are made using a coaxial pump/probe thermal lens spectrometer. The use of high-purity reagents at low concentrations permits a decrease in the TLS blank signal and noise, leading to a limit of detection of 9 × 10−9 M (cerium extract concentration), 40-fold lower than the spectrophotometric value. The dynamic range extended up to 6 × 10−7 M and the relative standard deviation for 5 × 10−7 M cerium was 3.9%.
Development and Optimization of Pre-Concentration Procedure of Rare-Earth Elements (REEs) in Their Minerals, Using Microwave - Assisted Sample Dissol…
2015
Abstract The aim of this research was to develop and optimize a procedure for determination of REEs in xenotime and monazite samples collected from Bangka Island, which were compared to Standard Monazite (71 AG) of Bureau of Analyzed Samples, London. ICP-OES method was used for the determination. The samples were dried and sterilized by heating for a week at 110 °C, before digesting with nitric acid and hydrofluoric acid, using a microwave-assisted digestion system. After a careful line selection, at the detection limits for all REEs in the ng/mL the REEs were reliably obtained at the 0.09 – 38% level.
Pulsed EPR determination of water accessibility to spin-labeled amino acid residues in LHCIIb.
2009
Membrane proteins reside in a structured environment in which some of their residues are accessible to water, some are in contact with alkyl chains of lipid molecules, and some are buried in the protein. Water accessibility of residues may change during folding or function-related structural dynamics. Several techniques based on the combination of pulsed electron paramagnetic resonance (EPR) with site-directed spin labeling can be used to quantify such water accessibility. Accessibility parameters for different residues in major plant light-harvesting complex IIb are determined by electron spin echo envelope modulation spectroscopy in the presence of deuterated water, deuterium contrast in …
X-ray structures of five variably tert-butoxycarbonyl-substituted adenines and their liquid and solid state NMR investigations
2009
Abstract Adenine reacts selectively with di- tert -butyldicarbonate in THF in the presence of NaOH to give N 9-monoBoc-adenine 1 . The molecular structure and crystal packing of this and four other variably substituted Boc-derivatives of adenine were determined in solid state by means of X-ray diffraction and CP/MAS NMR experiments and characterized in liquid state by 1 H, 13 C, and 15 N NMR spectroscopy as well. Additionally, crystal structure of inclusion compound between N 6 -monoBoc-adenine 5 and CHCl 3 is reported. Tautomeric equilibria of mono- and disubstituted derivatives 4 and 5 in liquid state were studied by VT NMR experiments.