Fabrication of mesoporous metal chalcogenide nanoflake silica thin films and spongy mesoporous CdS and CdSe

Mesoporous silica metal oxide (ZnO and CdO) thin films have been used as metal ion precursors to produce the first examples of mesoporous silica metal sulfide (meso-SiO(2) @ZnS, meso-SiO(2) @CdS) or silica metal selenide (meso-SiO(2) @ZnSe, meso-SiO(2) @CdSe) thin films, in which the pore walls are made up of silica and metal sulfide or metal selenide nanoflakes, respectively. A gentle chemical etching with a dilute HF solution of the meso-SiO(2) @CdS (or meso-SiO(2) @CdSe) produces mesoporous cadmium sulfide (meso-CdS) (or cadmium selenide, meso-CdSe). Surface modified meso-CdS displays bright blue photoluminescence upon excitation with a UV light. The mesoporous silica metal oxides are formed as metal oxide nanoislands over the silica walls through a self-assembly process of a mixture of metal nitrate salt-two surfactants-silica source followed by calcination step. The reactions, between the H(2) S (or H(2) Se) gas and solid precursors, have been carried out at room temperature and monitored using spectroscopy and microscopy techniques. It has been found that these reactions are: 1)?taking place through the diffusion of sulfur or selenium species from the top metal oxide layer to the silica metal oxide interface and 2)?slow and can be stopped at any stage to obtain mesoporous silica metal oxide metal sulfide or silica metal oxide metal selenide intermediate thin films.     

Multi-elemental bio-imaging of rat tissue from a study investigating the bioavailability of bismuth from shotgun pellets

In recent years, bismuth has been promoted as a "green element" and is used as a substitute for the toxic lead in ammunition and other applications. However, the bioavailability and toxicity of bismuth is still not very well described. Following a hunting accident with bismuth-containing shots, a bioavailability study of bismuth from metal pellets inoculated into rat limb muscles was carried out. Bismuth could be found in urine and blood of the animals. Bio-imaging using laser ablation ICP-MS of thin sections of the tissue around the metal implant was carried out to find out more about the distribution of the metal diffusing into the tissue. Two laser ablation systems with different ablation cell designs were compared regarding their analytical performance. Low concentrations of bismuth showing a non-symmetrical pattern were detected in the tissue surrounding the metal implant. This was partly an artefact from cutting the thin sections but also bio-mobilisation of the metals of the implant could be seen. An accumulation of zinc around the implant was interpreted as a marker of inflammation. Challenges regarding sample preparation for laser ablation and bio-imaging of samples of diverse composition became apparent during the analysis.     

Rim formation on crystal faces growing in confinement

A crystal face growing from solution while exerting a normal force on a confining surface is often observed to develop a growth rim surrounding a hollow core. The interpretation has been that this is a manifestation of steady state growth due to the balance between the concentration gradient and stress gradient along the confined crystal surface. In this paper, we present experimental results which show that the growth rim is instead formed as a consequence of faceted growth on the confined surface. Steady state growth is not ensured by a gradient in normal stress, but rather a gradient in step density along the crystal face. The loaded crystal surfaces display a high degree of roughness, and the stress is not uniformly distributed across the surface, but transmitted at discrete asperities. We discuss the implications of these findings for the interpretation of previous experimental results, and for the thermodynamics of crystal growth subject to normal stress.     

Qualitative and quantitative determination of extractives in heartwood of Scots pine (Pinus sylvestris L.) by gas chromatography

A method for quantitative determination of extractives from heartwood of Scots pine (Pinus sylvestris L.) using gas chromatography (GC) with flame ionization detection (FID) was developed. The limit of detection (LOD) was 0.03 mg/g wood and the linear range (r = 0.9994) was up to 10 mg/g with accuracy within +/- 10% and precision of 18% relative standard deviation. The identification of the extractives was performed using gas chromatography combined with mass spectrometry (GC-MS). The yields of extraction by Soxhlet were tested for solid wood, small particles and fine powder. Small particles were chosen for further analysis. This treatment gave good yields of the most important extractives: pinosylvin, pinosylvin monomethyl ether, resin acids and free fatty acids. The method is used to demonstrate the variation of these extractives across stems and differences in north-south direction.     

The selective and efficient laser ion source and trap project LIST for on-line production of exotic nuclides

Laser ion sources based on resonant excitation and ionization of atoms are well-established tools for selective and efficient production of radioactive ion beams. A recent trend is the complementary installation of reliable state-of-the-art all solid-state Ti:Sapphire laser systems. To date, 35 elements of the Periodic Table are available at laser ion sources by using these novel laser systems, which complements the overall accessibility to 54 elements including use of traditional dye lasers. Recent progress in the field concerns the identification of suitable optical excitation schemes for Ti:Sapphire laser excitation as well as technical developments of the source in respect to geometry, cavity material as well as by incorporation of an ion guide system in the form of the laser ion source trap LIST.     

Cyclic homo and block copolymers through sequential double click reactions

Well‐defined linear α‐anthracene‐ω‐maleimide functionalized polystyrene (l‐Anth‐PS‐MI) and linear α‐alkyne‐ω‐maleimide functionalized poly(tert‐butyl acrylate) (l‐alkyne‐PtBA‐MI) homopolymers, and linear α‐anthracene‐ω‐maleimide functionalized PS‐b‐PtBA (l‐Anth‐PS‐b‐PtBA‐MI) and linear α‐anthracene‐ω‐maleimide functionalized PS‐b‐poly(ε‐caprolactone) (PCL) (l‐Anth‐PS‐b‐PCL‐MI) block copolymers were obtained via combination of atom transfer radical polymerization (ATRP)/ring opening polymerization (ROP) and azide‐alkyne click reaction strategy. Subsequently, these linear homo and block copolymers were efficiently clicked via Diels‐Alder reaction to give their corresponding cyclic homo and block copolymers at reflux temperature of toluene for 48 h under 7–4 × 10^?5 M conditions. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2010     

Synthesis,characterization, and antioxidant activity of heterocyclic Schiff bases

Schiff base derivatives have gained great importance due to revealing a great number of biological properties. Schiff bases were synthesized by treatment of 4-amino-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one ( 1 ) with various aldehydes in methanol at reflux. In addition, diamine was reacted with an aldehyde to yield the corresponding Schiff bases. The structures of synthesized Schiff bases were elucidated by spectroscopic methods such as microanalysis, ¹H-NMR, ¹³C-NMR, and FTIR. Antioxidant activities of synthesized Schiff bases were carried out using different antioxidant assays such as 1,1-diphenyl-2-picryl-hydrazyl free radical (DPPH^•) scavenging, 2,2′-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) radical scavenging, and reducing power activity. (E)-4-((1H-indol-3-yl)methyleneamino)-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one ( 3 ), (E)-1,5-dimethyl-4-((2-methyl-1H-indol-3-yl)methyleneamino)-2-phenyl-1H-pyrazol-3(2H)-one ( 5 ), (E)-1,5-dimethyl-2-phenyl-4-(thiophen-2-ylmethyleneamino)-1H-pyrazol-3(2H)-one ( 7 ), (E)-1,5-dimethyl-2-phenyl-4-(quinolin-2-ylmethyleneamino)-1H-pyrazol-3(2H)-one ( 9 ), (1S,2S,N1,N2)-N1,N2-bis((1H-indol-3-yl)methylene)cyclohexane-1,2-diamine ( 11 ), and (1S,2S,N1,N2)-N1,N2-bis((2-methyl-1H-indol-3-yl)methylene)cyclohexane-1,2-diamine ( 12 ) were synthesized in high yields. Compound 5 displayed a good ABTS^•+ activity. Compound 3 revealed the outstanding activity in all assays. Compound 7 has the best-reducing power ability in comparison to other synthesized compounds. Although compounds 5, 11, 12 are new, compounds 3, 7, 9 are known. Due to revealing a good antioxidant activity, the synthesized compounds ( 3, 5, 7 ) have the potential to be used as synthetic antioxidant agents.     

Three‐arm star ring opening metathesis polymers via alkyne‐azide click reaction

The click chemistry strategy is successfully applied for the preparation of three‐arm star (A₃) ring opening metathesis polymers. A well‐defined monoazide end‐functionalized poly(N‐ethyl oxanorbornene) and a poly(N‐butyl oxanorbornene) obtained via ring opening metathesis polymerization using first generation Grubbs' catalyst are simply clicked with the trisalkyne core affording the synthesis of target star polymers. The obtained star polymers are characterized via nuclear magnetic resonance spectroscopy and gel permeation chromatography (GPC). The deconvolution analyses of GPC traces reveal that the click reaction efficiency for the star formation strongly depends on the chemical nature and the molecular weight of ROM polymers. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 2344–2351, 2009     

Identification of aerosol particle sources in semi‐rural area of Kwabenya,near Accra,Ghana, by EDXRF techniques

Small aerosol particles have for a long time been known to be harmful to humans, and are today regarded to cause a larger number of deaths than traffic accidents globally. Energy dispersive x‐ray fluorescence (EDXRF) is a well known method that has been used for identification of toxic as well as non‐toxic elements in the particles. The combination of elements will together with other information help to identify the sources and predict the effects of particles on environment and human health. The present work was conducted in Kwabenya, a suburb of the capital Accra of Ghana, which is frequently exposed to Harmattan dust from the Sahara–Sahel region. In total 171 filters each of PM2.5 and PM(2.5–10) were collected during 1 year. Levels of elements, black carbon (BC) and mass, were determined for both particle sizes. Principal component analysis (PCA) was performed on the datasets from Harmattan and non‐Harmattan periods. The daily average of PM10 was very high, 179 µg m^?3 and the BC contents were 4 µg m^?3. The presence of crustal elements was large in PM(2.5–10) as well as in PM2.5, and had a more than tenfold increase in PM(2.5–10) during the Harmattan period. Major characteristic elements for different sources were identified from correlation coefficients and regression analysis of the data. Sahara sand aerosol was the major source in both study periods, but influence from biomass burning, sea‐spray and metal industries was also observed. Copyright © 2009 John Wiley & Sons, Ltd.