Search results for "Analytical"
showing 10 items of 9586 documents
Effect of ramp size and sample spinning speed on CPMAS 13C NMR spectra of soil organic matter
2011
Abstract Cross polarization (CP) magic angle spinning (MAS) 13C NMR spectroscopy is a solid state NMR technique widely applied to study the chemical composition of natural organic matter. In high magnetic fields (>7 T), fast sample spinning is required in order to reduce the influence of spinning sidebands underlying other chemical shift regions. As the spinning speed increases, the Hartmann–Hahn matching profiles break down into a series of narrow matching bands. In order to account for this instability variable amplitude cross polarization techniques (e.g. VACP, ramp-CP) have been developed. In the present study, we experimentally verified the stability of the Hartmann–Hahn condition unde…
O-Alkylation of a lignite humic acid by phase-transfer catalysis
2006
A mild phase-transfer catalytic reaction has been conducted to O-alkylate the acidic functions of a lignite humic acid (HA), using tetrabutylammonium hydroxide as the phase-transfer catalyst. The HA acidic functional groups were made to react, in tetrahydrofuran, by nucleophilic substitution with several alkyl halides-methyl iodide, and ethyl, propyl, and butyl, and benzyl bromide. The occurrence of the O-alkylation reaction was assessed by elemental analysis and 1H NMR, CPMAS 13C NMR, and FTIR spectroscopy. Bonding of alkyl groups increased the carbon and hydrogen content and the H/C ratios of all the humic reaction products. Increased nitrogen in the reaction products suggested incomplete…
Small angle scattering study of the structure of isotactic polypropylene-hydrogenated oligo(cyclopentadiene) blends
1996
Abstract Blends of isotactic polypropylene ( i PP) and hydrogenated oligo cyclopentadiene (HOCP) have been studied by means of small angle X-ray scattering in the temperature range 70–160°C. The structure of blends containing less than 25% HOCP is very similar to the one of plain i PP, i.e. lamellae whose thickness increases by increasing the temperature. Blends containing more than 25% HOCP are characterized by two kinds of lamellae formed by layers of i PP and amorphous material rich in i PP and in HOCP, respectively. The crystallizable i PP present in both phases crystallizes from the melt, in analogy to what happens in HDPE/HOCP blends and in agreement with the values of the crystallini…
Some observations on the determination of sulfite by reduction to sulfide with sodium borohydride
1987
Abstract Sodium borohydride is studied as an agent for reducing sulfite to sulfide. Rapid reductions are attained with greater than 97% recovery in the range 700–1200 μg of S/50 ml. Sulfate is not reduced.
FT-IR and dielectric study of water/AOT liquid crystals
2000
Abstract In order to explore the influence of microwave radiation on highly viscous microheterogeneous systems, the evolution of structural and dynamical properties of the water/sodium bis(2-ethylhexyl) sulfosuccinate (AOT) liquid crystals as a function of the molar ratio R (R=[water]/[AOT]) has been investigated by FT-IR spectroscopy and time domain reflectometry. The study emphasises how the progressive hydration of the surfactant head groups is mainly responsible for the structural and dynamical evolution of water/AOT liquid crystals. In particular, it has been found that the state of water at lower R values is strongly perturbed, bulk-like water appears only at R>23 and the water/AOT in…
Temporal fatty acid profiles of human decomposition fluid in soil
2017
Abstract We studied the changes in concentration and relative abundance of human-derived fatty acids (FAs) in soil over a period of one year. The study is based on analysis of soil underneath a human body that lay on the soil surface for 18 days before it was discovered. Soil samples were taken when the body was removed, and also 358 days later. Large amounts of the total FA concentration at the start of the measurement period were still present one year after the removal of the body. The FA profile suggested that extensive saturated FA reduction occurred during the first 18 days after deposition. 10-Hydroxystearic acid and FA salts, which are characteristic of adipocere, were abundant in a…
Study of silica-structured materials as sorbents for organophosphorus pesticides determination in environmental water samples
2018
Abstract A novel sorbent based on a UVM-7 mesoporous silica doped with Ti has been synthesized and used for solid-phase extraction of several organophosphorus pesticides in environmental water samples followed by gas chromatography coupled to a nitrogen-phosphorus selective detector. Thus, mesoporous silica materials doped with Ti and Fe as well as immobilized cyclodextrin silica-based supports were prepared and morphologically characterized by several techniques such as transmission electronic microscopy, nitrogen adsorption-desorption and X-ray diffraction. These sorbents were comparatively evaluated, and Ti25-UVM-7 material was selected as the best solid phase. After optimization of extr…
Fluorescence excitation and emission spectroscopy on single MEH-PPV chains at low temperature.
2008
Fluorescence emission and excitation spectra of single MEH-PPV polymer molecules dispersed in thin PMMA films have been recorded at 1.2 and 20 K. We observe single as well as multichromophore emission in single chain emission spectra, whereby the relative fractions depend on the two different molecular weights (50 and 350 kDa) studied. The molecular weight also affects the distribution of peak emission maxima, which is monomodal (bimodal) for the low (high) molecular weight. The appearance of an additional "red" subpopulation for the high molecular weight sample is attributed to interactions of multiple chromophores from a sufficiently flexible single chain. The comparison of emission spect…
Rapid characterization of alkylpolyphosphonates by CZE with indirect photometric and mass spectrometric detection.
2006
Methods for the rapid characterization of industrial alkylpolyphosphonates (APPs) by infusion MS and CZE with indirect photometric (IPD) and MS detection are described. Technical-grade APPs, including alkylaminepolyphosphonates with 3-5 phosphonate groups and different hydrocarbon skeletons, hydroxyethyl-amino-bis(methylenephosphonic acid), hydroxyethylidene-diphosphonic acid, and 2-phosphonobutane-1,2,4-tricarboxylic acid, were examined. A 10 mM solution of adenosine triphosphate disodium salt at pH 2.2 was used as BGE. The nominal compounds of the industrial APPs and their impurities were well resolved in less than 15 min. The peaks were identified by using extracted ion electropherograms…
On the determination of underivatised fatty alcohol ethoxylates by electrospray ionisation–mass spectrometry
2006
Abstract The oligomers of fatty alcohol ethoxylates (FAEs) exhibit large sensitivity differences in mass spectrometry with electrospray ionisation (ESI–MS) and atmospheric pressure chemical ionization (APCI). Standards of the oligomers from m = 1 to 7 ethylene oxide units (EOs) and linear alkyl chains from n = 10 to 18 carbon atoms were infused to examine the relative sensitivities or response factors in several media. The response factors of the [M + H]+ and [M + Na]+ peaks in 9:1 acetonitrile/water and methanol/water media containing acid buffers increased following irregular patterns when n and m increased. In methanol/water the response factors depended on the parity of m, being larger …