Search results for "Spectrometry"
showing 10 items of 3206 documents
Determination of selected polyaromatic hydrocarbons by gas chromatography–mass spectrometry for the analysis of wood to establish the cause of sinkin…
2014
Abstract The aim of this paper was to establish the cause of sinking of an old wooden vessel by polycyclic aromatic hydrocarbon (PAH) analyses because wood combustion is a source of PAHs. In particular, the molecular PAH patterns generated by each source are like fingerprints and it is possible to determine the processes that generate PAHs by studying their distribution in wood samples. The relative abundance of high molecular weight PAHs, together with the PAH compound ratios and with total index (proposed by us) has demonstrated that samples owe their PAHs in wood archaeological material to a predominant single mode of origin, i.e. combustion processes, therefore we can say that the sinki…
Determination of zirconium traces in polymers by ICP-IDMS - a powerful and fast method for routine testing of zirconium residues in polyolefins
1999
Zirconium trace analyses play an important role for polyolefins produced by modern catalytic processes with zirconium metallocenes. A reliable and fast routine testing method by inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) was therefore developed, which allows the determination of zirconium in polymers down to the low ng/g level. With respect to its precision, accuracy, and time-consumption this method is suitable for routine testing of production processes. A spike solution, enriched in the stable isotope 91Zr, was prepared and used for the isotope dilution procedure, which has the advantage of being an internal “one point” calibration method. The polyolefin sam…
The ion trap aerosol mass spectrometer: improved design, first field deployment, and the capability of differentiating organic compound classes via M…
2016
Abstract. Further development and optimisation of a previously described ion trap aerosol mass spectrometer (IT-AMS) are presented, which resulted in more reproducible and robust operation and allowed for the instrument’s first field deployment. Results from this 11-day long measurement indicate that the instrument is capable of providing quantitative information on organics, nitrate, and sulphate mass concentrations with reasonable detection limits (0.5–1.4 µg m−3 for 1 h averages), and that results obtained with the IT-AMS can directly be related to those from Aerodyne aerosol mass spectrometers. The capability of the IT-AMS to elucidate the structure of fragment ions is demonstrated via …
Characterization of industrial alkylpolyphosphonates by infusion electrospray ionization-ion trap mass spectrometry with identification of the impuri…
2005
Technical grade diethylene-triaminepentakis(methylenephosphonic acid) (I), dihexamethylene-triaminepentakis(methylenephosphonic acid) (II), ethylene-diaminetetrakis(methylenephosphonic acid) (III), hexamethylene-diaminetetrakis(methylenephosphonic acid) (IV), amino-tris(methylenephosphonic acid) (V), hydroxyethyl-aminobis(methylenephosphonic acid) (VI), 1-hydroxyethylidene-1,1-diphosphonic acid (VII), and 2-phosphonobutane-1,2,4-tricarboxylic acid (VIII) were characterized by ion trap mass spectrometry with electrospray ionization (ESI-ITMS). Using the negative ion mode and acid and alkaline media, peak series corresponding to the nominal compounds and to impurities with a lower number of p…
Direct pyrolysis in the mass spectrometer of aromatic polysulfonates and polythiosulfonates
1978
The thermal degradation mechanism of three aromatic polysulfonates and polythiosulfonates was investigated by direct pyrolysis in the ion source of a mass spectrometer. Thermal degradation reactions were followed directly by this method by detecting the thermal and electron impact induced fragments. The results obtained have provided evidence that sulfur dioxide extrusion from the polymer backbone takes place in these polymers above 300°C. The synthesis and molecular characterization of the polymers studied are reported in the text.
Mass spectrometric investigation of polymers: Thermal degradation of truxillic and truxinic polyamides
1975
The thermal degradation mechanism of four isomeric truxillic and truxinic polyamides were investigated by direct pyrolysis in the ion source of a mass spectrometer. Thermal degradation reactions were followed directly by this method by detecting the thermal and electron impact-induced fragments. The results obtained have shown that the thermal degradation products are sensibly different for the head-to-head (hh) and head-to-tail (ht) polymers and that the predominant pyrolytic process is the cyclobutane ring cleavage. In the hh isomers, both symmetrical and asymmetrical cyclobutane ring cleavage was detected, while in the ht isomers only symmetrical cleavage occurs; this explains the notice…
Binding abilities of new cyclodextrin-cucurbituril supramolecular hosts
2015
Various combined techniques (UV–vis spectrophotometry, isothermal titration calorimetry, thermogravimetry, ESI-MS mass spectrometry, polarimetry and 1H NMR spectroscopy) were used in order to study the interaction between a new combined supramolecular host, namely a bow-tie-structured cyclodextrin–cucurbituril association solely held by non-covalent interactions, and a suitably selected guest, namely the N-(p-nitrophenyl)-1,8-diaminooctane hydrochloride. In particular, the use of different techniques highlighted the peculiar features of the possible host–guest supramolecular interactions under different concentration conditions.
Enzymatic Resolution of 3-oxodicyclopentadiene on a Decagram Scale
2018
The chiral building block 3-oxodicyclopentadiene (1) can be readily resolved on a decagram scale by a short sequence consisting of (1) reduction to the corresponding endo-alcohol, (2) enzymatic oxidative resolution with a ketoreductase enzyme to give (+)-1 and the (+)-form of the endo-alcohol, and (3) reoxidation of the (+)-endo-alcohol with another ketoreductase to give (–)-1. With a selectivity factor of 310, the enantiomeric ratios of the resolved (+)-endo-alcohol and (+)-ketone are both >99:1. Both enzymatic oxidations could be performed with a at least 300:1 substrate/catalyst ratio (w/w).
Reliable and simple analytical methods for determination of citrulline and metabolically related amino acids by liquid chromatography after derivatiz…
2014
We describe the development of a high-performance liquid chromatography (HPLC) method for the determination of citrulline and other amino acids relevant to intestinal diseases. The amino acids were derivatized with 9-fluorenylmethylchloroformate (FMOC-Cl) and their derivatives were separated on two different columns, a core-shell column (Halo C18) and a silica-based monolith (Chromolith Performance RP-18). The derivatization reaction was optimized with respect to pH, buffer concentration and reproducibility. The optimal derivatization conditions were achieved with 0.4 M borate buffer at pH 9.20, a constant ratio of FMOC-Cl/total amino acids (10 : 1) and 75 mM tyramine after 1 min (quenching…
Distribution of volatile organic compounds in Sicilian groundwaters analysed by head space-solid phase micro extraction coupled with gas chromatograp…
2008
This work presents the results of an assessment of the existence and concentration of 13 volatile organic compounds (VOCs) in groundwaters from 14 hydrological basins in Sicily (25,710km (2)). On the basis of hydrological, hydrogeochemical and geological studies, 324 sampling points were selected. All groundwater sampled were collected twice, from October to December 2004 and from February to May 2005, and were analysed to determine the concentration and spatial distribution of the VOCs in the aquifers. The need to analyze a large number of samples in a short space of time so as to obtain quantitative analyses in trace concentration levels spurred us to create a new analytical method, both …