Search results for "LIMIT"
showing 10 items of 2826 documents
ChemInform Abstract: Diels-Alder Reactions of in situ Generated N-Benzoylindolo-2,3- quinodimethane with Carbodienophiles.
2010
The indolo-2,3-quinodimethane (5), generated from 2,3-bis(bromomethyl)indole (4), was trapped with unsymmetrical carbodienophiles or N, N′-p-phenylenedimaleimide to furnish the 1,2,3,4-tetrahydrocarbazoles (6–9). [4 + 2]-Cycloaddition of 5 with tetracyanoethylene gave rise to the tetracyanocarbazole (10) and a subsequent product 11a or 11b. The Diels-Alder reaction of 5 with divinyl sulfone was regiospecific within the detection limits of HPLC analysis. Similarly, the reaction of 5 with N, N′-p-phenylenedimaleimide yielded solely the stereoisomer 9.
Determination of titanium by adsorption voltammetry with 4-(2-pyridylazo) resorcinol
1990
Titanium (IV) forms a complex with 4-(2-pyridylazo) resorcinol (PAR) in weakly acidic solutions. This complex can be used to determine titanium by adsorption voltammetry at a stationary Hg-electrode. The experimental conditions for the determination are described. The current-concentration curve is linear from 0.15–4.8 ng/g. Ti at a deposition time of 3 min, the detection limit lies at 0.1 ng/g. The influence of foreign ions was investigated. The determination can be carried out in the presence of a 1000-fold excess of iron by the standard addition method, albeit with decreased sensitivity.
Determination of organophosphorus pesticides in honeybees after solid-phase microextraction.
2001
A method based on solid-phase microextraction (SPME) followed by gas chromatography with nitrogen-phosphorus detection was developed for the purpose of determining 18 organophosphorus pesticide residues in honeybee samples (Apis mellifera). The extraction capacities of polyacrylate and poly(dimethylsiloxane) fibers were compared. The main factors affecting the SPME process, such as the absorption time profile, salt, and temperature, were optimized. The method involved honeybee sample homogenization, elution with an acetone:water solution (1:1) and dilution in water prior to fiber extraction. Moreover, the matrix effect on the extraction was evaluated. In samples spiked at the 0.2 mg kg(-1) …
Development of a new method for the separation of vanadium species and chloride interference removal using modified silica capillaries-DIN-ICP-MS
2004
Abstract A new on-line method for the separation of vanadium (IV) and vanadium (V) as well as for the removal of ClO+ mass spectral interference on vanadium determination by quadrupole-ICP-MS has been developed. The sample introduction system consists of a modified fused silica capillary coupled to a direct injection nebuliser (DIN), between the solvent delivery system and the ICP. Fused silica capillaries were treated with different anion and cation exchanger reagents and were tested for the retention of Cl− and the separation of vanadium ions at μg l−1 levels. A suitable strong anion exchanger functional group (3-aminopropyltrimethoxy silane) was selected. Chlorine anions were retained in…
Development of an ICP-IDMS method for accurate routine analyses of toxic heavy metals in polyolefins and comparison with results by TI-IDMS
2000
An inductively coupled plasma isotope dilution mass spectrometric (ICP-IDMS) method was developed as a suitable method - with respect to its sensitivity, precision, accuracy, and time-consumption - for the analysis of toxic heavy metal traces (Pb, Cd, Cr, and Hg) in polyolefins. Results for Pb, Cd, and Cr were compared with those obtained by thermal ionization isotope dilution mass spectrometry (TI-IDMS), which was used as a reference method. Because of its high first ionization potential and its high volatility mercury could not be determined by TI-IDMS. A multi-element spike solution, containing isotopically enriched 206Pb, 116Cd, 53Cr, and 201Hg, was used for the isotope dilution step. D…
Trace analysis of plutonium in environmental samples by resonance ionization mass spectroscopy (RIMS)
1998
Resonance ionization mass spectroscopy (RIMS) is well suited for trace analysis of long-lived radioisotopes in environmental, biological and technical samples. By multiple resonant laser excitation and ionization of the elemental atoms under investigation, an extremely high element selectivity can be achieved. In addition, isotope selectivity is obtained by subsequent mass analysis. The excellent sensitivity results from the large atomic cross-sections in the excitation–ionization process and the good detection efficiency for ions. The element selectivity of RIMS allows a simplified procedure for the chemical preparation of the samples compared to the requirements of thin sources for α-spec…
Ultratrace analysis and isotope ratio measurements of long-lived radioisotopes by resonance ionization mass spectrometry (RIMS).
2003
Resonance Ionization Mass Spectrometry (RIMS) is a sensitive and selective method for ultratrace analysis of long-lived radioisotopes and isotope ratio measurements. It provides extremely high isobaric suppression and good overall efficiency. The experimental limits of detection are as low as 10(6) atoms per sample and isotopic selectivities of 5x10(12) have been obtained. The widespread potential of RIMS, using different experimental arrangements, is demonstrated for the determination of the radiotoxic isotopes Pu-238 to Pu-244 and Sr-89/Sr-90 in various environmental samples as well as for Ca-41 in nuclear reactor components and biomedical samples.
Resonance ionization mass spectrometry for ultratrace analysis of plutonium with a new solid state laser system
2004
Abstract Resonance ionization mass spectrometry (RIMS) is well-suited for isotope selective ultratrace analysis of long-lived radioactive isotopes due to its high element and isotope selectivity and good sensitivity. For the analysis of plutonium with a pulsed RIMS apparatus, a powerful, reliable and easy to handle Nd:YAG pumped titanium–sapphire laser system has been developed and combined with a time-of-flight mass spectrometer. Spectroscopic measurements led to an efficient three step excitation and ionization scheme for plutonium with λ1 = 420.76 nm, λ2 = 847.28 nm, and λ3 = 767.53 nm. The isotope shifts in this scheme for the plutonium isotopes 238 Pu through 244 Pu have been determine…
Recent developments in isotope ratio measurements by resonance ionization mass spectrometry
2005
Resonance ionization mass spectrometry (RIMS) has become a sensitive and highly selective technique for the determination of extremely low elemental or isotopic abundances, involving isotope ratio measurements with dynamical ranges of 109 and beyond. The experimental detection limits are as low as 106 atoms per sample, and isotopic selectivities of up to 1013 have been achieved under optimal conditions. The potential of RIMS using different experimental systems is outlined in the determination of lowest abundances and isotope ratios of long-lived radioisotopes of general importance like Pu238–244, 41Ca, and 236U for studies in geosciences, environmental, bio-medical or fundamental research.
Optimization of sample preparation conditions for detecting trace amounts of β-tegafur in α- and β-tegafur mixture.
2012
We report a semiquantitative method for determining trace amounts (<1%) of thermodynamically stable forms in polymorphic mixtures, focusing on sample preparation ef- fects on solid phase transitions. Tegafur (5-fluoro-1-(oxolan-2-yl)-1,2,3,4-tetrahydropyrimidine- 2,4-dione) was used as a model material in this study. The amounts of the thermodynamically stable $ tegafur were increased to levels detectable by powder X-ray diffractometry by grind- ing the samples in a ball mill in the presence of water. The limit of detection for this method was as low as 0.0005% of $ tegafur in " and $ tegafur mixtures. The amount of $ tegafur after sample preparation was found to be proportional to the init…