Pyrohydrolysis of carbon nanotubes for Br and I determination by ICP-MS

Bromine and iodine determination was performed in carbon nanotubes (CNTs) by inductively coupled plasma mass spectrometry (ICP-MS) after sample preparation using pyrohydrolysis. Samples of CNTs (up to 500 mg) were mixed with 750 mg of V₂O₅ and heated at 950 °C during 12.5 min in a quartz tube under water vapor and air. The main operational conditions of pyrohydrolysis (carrier gas, absorbing solution, heating time, sample mass and use of V₂O₅) were evaluated. Accuracy was evaluated using certified reference materials (CRM) with similar matrix and also by comparison of results obtained after digestion of samples by microwave-induced combustion (MIC) and determination by ICP-MS. Agreement with CRM values was higher than 97% for Br and better than 96% in comparison with reference values (MIC/ICP-MS) of Br and I in CNTs samples. The limit of detection of the method for Br and I determination by ICP-MS was 0.05 and 0.004 μg g^? 1, respectively. Using a relatively simple and low cost pyrohydrolysis apparatus up to four samples can be processed per hour. The pyrohydrolysis sample preparation procedure is easy to be performed and provide a clean solution for analysis by ICP-MS, which is very attractive for Br and I control in CNTs.     

Exclusive \eta production in pp reactions

Angular distributions for the exclusive reaction observed via the decay channel have been measured at GeV, 2.50 GeV and 2.85 GeV (excess energies Q = 324 MeV, 412 MeV and 554 MeV). The polar angle of the shows an anisotropy with respect to the beam direction for the lowest energy, which vanishes for the higher energies. The anisotropy of the pp polar angle increases slightly with the beam energy.Received: 30 September 2002, Published online: 22 October 2003PACS: 13.75.Cs Nucleon-nucleon interactions (including antinucleons, deuterons, etc.) - 14.40.Aq , K, and mesons - 25.40.Ve Other reactions above meson production thresholds (energies > 400 MeV)Y. Bedfer: Present address: DAPNIA/SPhN, CEA Saclay, France.A. Brenschede: Present address: Syngenio AG, StuttgartF. Brochard: Present address: LPHNHE, Ecole Polytechnique 91128 Palaiseau, France.Seonho Choi: Present address: Temple University, Philadelphia, PA, USA.R. Dressler: Present address: Paul Scherrer Institut, Villigen, CH-5232.J. Foryciarz: Present address: Motorola Polska Software Center, Kraków, Poland.H.-W. Pfaff: Present address: d-fine GmbH, Eschborn.     

The EF and GK1Σg+ states of hydrogen: Calculation of nonadiabatic coupling

The mutual vibronic coupling between the EF and GK states of hydrogen has been computed in an adiabatic basis of electronic-vibrational states. The electronic matrix elements 〈EF|?_R|GK〉 and 〈EF|Δ_R|GK〉 are presented over the relevant range 2.0 ≤ R ≤ 4.0 a.u. and the vibronic coupling matrix is displayed for H₂. Nonadiabatic vibroic energies and B values are calculated for H₂, HD, and D₂ and compared with experimental data. The irregularities of the observed vibronic EF and GK progressions are well reproduced by the calculation. The remaining errors of the calculated energies grow systematically as the dissociation limit is approached, indicating the importance of additional nonadiabatic interactions with higher states and possibly of R-dependent errors of the Born-Oppenheimer energies of the EF and GK states at R values far from the potential minima.     

Localization of carboxyl groups at surface layer of carboxylated polymer emulsion particles by alkali treatment

For the purpose of localizing carboxyl groups from inside to particle surface, styrene — butyl acrylate — methacrylic acid (74.3/17.0/8.7, mol ratio) terpolymer emulsion was kept under pH 9 at different temperatures. The amount of carboxyl groups at the particle surface, As, was remarkably increased by the alkali-treatment above 35 °C. On the other hand, As value of the alkalitreated emulsion was decreased by keeping under ph 3 above 45 °C, although in the case of the original emulsion without the alkalitreatment, it was not changed by the acid-treatment. These results suggest that a part of polymer segments which have ionized carboxyl groups is dragged out at the surface by an increase in the affinity of the groups against water, and the dragged segments turn back into the inside again when the carboxyl groups are deionized.Part 97 of the series Studies on Suspension and Emulsion.     

Digestion of biological materials using the microwave-assisted sample combustion technique

In this study a procedure for sample digestion based on sample combustion assisted by microwave radiation is proposed. Combustion is started by microwave radiation in the presence of oxygen under pressure using ammonium nitrate as aid for ignition. The system was adapted in a microwave oven with quartz closed vessels. A quartz piece is used simultaneously as a sample holder and as protection to the cap of quartz vessel from the flame generated in the combustion process. Sample was pressed into a pellet and placed on a disc paper in the holder and 50 μl of 50% m/v ammonium nitrate solution was added. The influence of the absorption solution (diluted and concentrated nitric acid or water) on the recoveries for Cu and Zn was evaluated. About 3 s of microwave irradiation was necessary to start the combustion. The combustion process was evaluated in relation to the influence of sample mass on the ignition time, combustion time and maximum operation pressure. Bovine liver, milk powder and oyster tissue certified reference materials were used to evaluate the accuracy of the procedure for determination of copper and zinc. Good agreement for zinc (96% to 103%) was obtained from bovine liver certified reference material when microwave combustion and microwave combustion followed by reflux were used to sample decomposition, even if water was used for absorption of analyte. For copper, the combustion followed by reflux of 5 min allows an agreement from 96% to 100%. Similar results were obtained for oyster tissue samples. However, for milk powder good agreement close to 100% was obtained only if 4 mol l^− 1 HNO₃ was used with a reflux step. Results from the proposed procedure were also compared to those from conventionally used procedures for biological samples decomposition, such as wet digestion in open vessels and microwave-assisted digestion in closed vessels. The advantages of this procedure include the complete sample decomposition in less time than other procedures and the acid consumption was always lower than 2%. Another advantage is the low residual carbon content, less of 1.4% without reflux and less than 0.3% with the reflux step and the possibility of use of diluted acid as absorbing solution. Moreover, the new holder allows an effective protection of the vessel cap to burnt high masses.     

Destruction of Organic Compounds in a High-Frequency Discharge Plasma at Reduced Pressure

Plasma Chemistry and Plasma Processing - Conditions of the destruction of organic compounds in a hf discharge plasma at reduced pressure and parameters of this plasma type are determined. The...     

Simultaneous determination of thirteen plant alkaloids in a human specimen by SPE and HPLC

A new screening method for the simultaneous determination of thirteen plant alkaloids (aconitine, anabasine, atropine, brucine, colchicine, cotinine, cytisine, harmine, ibogaine, nicotine, scopolamine, strychnine, yohimbine) in a human specimen was developed based on solid-phase extraction and reversed-phase liquid chromatography with photodiode array detection. The validated method enables selective identification as well as accurate and sensitive quantification. The analysis of forensic and clinical samples emphasizes the applicability for intoxications and drug abuse, as well as for compliance control.     

Electro-optical properties of excitons in polydiacetylene chains

We show how to compute the optical functions (reflectivity, transmission, and absorption) of polydiacetylene chains diluted in their monomer matrix exposed to a uniform electric field in the chain direction, in the excitonic energy region. Adopting a model electron-hole potential, we derived an analytical expression for the effective chain susceptibility, which gives the optical functions. The resulting absorption shows excitonic peaks below the gap and Franz-Keldysh oscillations above the gap. The method has been applied for a 3BCMU polydiacetylene chain, showing a good agreement with experimental spectra. Received 5 November 1998 and Received in final form 23 February 1999