Determination of cobalt in biological materials by RNAA via induced short-lived 60mCo

A chemiluminescence (CL) micro-flow system is presented for rapid determination of chemical oxygen demand (COD) in water at room temperature. In this system, potassium dichromate is reduced to Cr³⁺ in 2 mol L⁻¹ H₂SO₄ during the chemical oxidation of COD substances in the sample, and Cr³⁺ can be measured with the help of the luminol-H₂O₂ CL system. The polymethyl methacrylate micro-flow chip with discrete microdroplet sampling was used here. Effects on COD determination (such as pH, concentrations, the channel length, and interference) were investigated. The linear range for COD determination was 0.27–10 g L⁻¹, and the detection limit was 100 mg L⁻¹. The method was successfully applied to the determination of COD in wastewater samples. The data obtained with the present method were in fairly good agreement with those obtained by the titrimetric method. Correspondence: Zhujun Zhang, Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry and Materials Science, Shaanxi Normal University, Xi’an 710062, P.R. China; Department of Chemistry, Institute of Analytical Science, Southwest University, Beibei, Chongqing 400715, P.R. China     

Manipulation of dielectric,ferroelectric and magnetic anomalies in multiferroic,morphotropic phase boundary quenched BiFeO3-0.35PbTiO3 solid solutions

The effect of thermal quenching on physical properties of morphotropic phase boundary BiFeO₃-0.35PbTiO₃ composition, composed of Pnma, R3c and P4mm phases, has been investigated in detail. We detected and quantified role of quenching through investigation of magnetic, dielectric and ferroelectric anomalies. Quenching significantly i) enhances the tetragonal phase percentage (hence affects domain structure), ii) reduces domain wall clamping with a large increase in electrical polarization, iii) increases magnetization at the structural phase transition temperature (tunable magneto-electric coupling), iv) magnifies intrinsic property i.e. intra grain relaxation dynamics (which are otherwise suppressed due to the pinning of the defect dipoles), etc. All these findings clearly verify the role of quenching which noticeably enhances multiferroic properties at the well-known morphotropic phase boundary.     

Octupole-deformed molecular bands in 21Ne

Cluster states up to 12 MeV in the stable light nucleus ²¹Ne, based on the ¹⁶O + n + α molecular configurations, have been populated in the incomplete-fusion reaction ¹⁶ ₈O(⁷₃Li, np)²¹₁₀Ne at 29.4 MeV. The observation of both intra- and inter-band transitions leads to a re-interpretation of some levels in the K^π = ^- and K^π = ^- bands. The implications of this re-ordering on the octupole doublet bands are examined. The data allow a more accurate determination of some previously uncertain level energies. The “missing” I^π = ^- level is also discussed.     

Tandem on-line continuous separations for atomic spectroscopic indirect analysis: Iodide determination by ICP-AES

A sensitive and selective indirect determination of iodide by inductively coupled plasma emission spectrometry (ICP-AES) based on the principle of tandem on-line continuous separations as an alternative means of introducing samples into plasmas is proposed. Iodide is continuously extracted as an ion-pair into xylene by mixing the sample with Hg(II) and dipyridil solutions. The organic phase (containing the analyte in [Hg(Dipy)₂]I₂ form) is on-line continuously mixed with NaBH₄ (in DMF) and acetic acid solutions. Mercury vapour continuously generated from this organic phase is separated in a classical U-type gas-liquid separation device. The system has been optimized for the continuous extraction of KI, for the direct generation of cold mercury vapour from xylene and for the final ICP-AES determination of mercury. The optimised method has been applied to the determination of iodide (detection limit 20 ng/ml of iodide) in table salt and in synthetic samples. Very good agreement between found and certified results was observed. The usefulness and convenience of such alternative sample chemical pretreatment/presentation to the ICP is thus demonstrated for indirect determinations to be carried out by atomic spectroscopy methods.     

Gamma-Ray Transitions Induced in Nuclear Spin Isomers by X-Rays

Because of the high density of energy storage and the large cross section for its release, nuclear spin isomers have attracted considerable recent interest. The triggering of induced gamma emission from them has encouraged efforts to develop intense sources of short-wavelength radiation. One of the more interesting examples is the 16⁺ 4-qp isomer of ¹⁷⁸Hf which stores 2.445 MeV for a half-life of 31 years meaning that as a material, such isomeric ¹⁷⁸Hf would store 1.3 GJ/g. Recently, a sample containing 6.3×10¹⁴ nuclei of the isomer of ¹⁷⁸Hf was irradiated with X-ray pulses derived from a device operated at 15 mA to produce bremsstrahlung radiation with end point energies set to values between 60 and 90 keV. Emission of gamma radiation from the sample was increased by 1–2% above the quiescent value of spontaneous emission. Such an accelerated decay of the ¹⁷⁸Hf isomer is consistent with an integrated cross section of 2.2×10⁻²² cm² keV if the resonant absorption of the X-rays takes place below 20 keV as indicated by the use of selective absorbing filters in the irradiating beam. The work reported here describes the current experimental focus and results recently obtained with the use of coincident detection of emitted gamma photons by several detectors. This revised version was published online in July 2006 with corrections to the Cover Date.     

Are liquid chromatography/electrospray tandem quadrupole fragmentation ratios unequivocal confirmation criteria?

Multiple reaction monitoring (MRM) ratios as provided by tandem mass spectrometers are used to confirm positive residue findings (e.g. veterinary drugs or pesticides). The Commission Decision 2002/657/EEC defines tolerance levels for MRM ratios, which are intended to prevent the reporting of false positives. This paper reports findings where blank sample extracts have been spiked by a drug (difloxacin) and the corresponding measured MRM ratios significantly deviated from MRM ratios observed in matrix‐free solution. The observation was explained by the formation of two different [M+H]⁺ analyte ions within the electrospray ionization (ESI) interface. These two ions vary only by the site of analyte protonation. Since they are isobaric, they are equally transmitted through the first quadrupole, but are differently fragmented in the collision chamber. The existence of two isobaric ions was deduced by statistical data and the observation of a doubly charged analyte ion. It was hypothesized that the combined presence of [M+H]⁺ and [M+2H]²⁺ implies the existence of two different singly charged ion species differing only by the site of protonation. Low‐ and high‐energy interface‐induced fragmentation was performed on the samples. The surviving precursor ion population was mass selected and again fragmented in the collision chamber. Equal product ion spectra would be expected. However, very different product ion spectra were observed for the two interface regimes. This is consistent with the assumption that the two postulated isobaric precursor ions show different stability in the interface. Hence the abundance ratio among the two types of surviving precursor ions will shift and change the resulting product ion spectra. The existence of the postulated singly charged ions with multiple chargeable sites was finally confirmed by successful ion mobility separation. Copyright © 2009 John Wiley & Sons, Ltd.     

Bioenergetics of the growth of the lactobacillus culture on various nutrient media

The energy (enthalpy) of the multiplication of lactobacilli on various nutrient media was measured on a DAK-1-1 differential microcalorimeter. Cultivation of lactobacilli on the nutrient media studied was accompanied by a release of energy. The time dependences of heat evolution were similar in shape to the curves of the growth of the microorganism population. The conclusion was drawn that the quantity of the evolved energy depended on the type of the nutrient medium.