Time and temperature induced phase transformation in L‐isoleucine hydrochloride monohydrated crystal

Semi organic crystals have been intensively studied aiming applications in nonlinear optical (NLO). Such applicability requires crystals with both high quality and thermal stability, which make the full characterization of this material a topic issue. In this paper, single crystals of L‐isoleucine hydrochloride monohydrated (L‐Ile.H2O.HCl) was synthesized by slow evaporation technique and characterized by thermal analysis and X‐ray diffraction (XRD) measurements. XRD results at 298 K showed that the sample crystallize with the orthorhombic structure, and the lattice parameters obtained by Rietveld refinement were a = 5.873(3) Å, b = 24.814(4) Å, and c = 6.873(5) Å. Thermal analysis measurements shows four decomposition stages between 328 ‐480 K which were associated with loss of water by desolvation, loss crystallization water and decomposition of L‐Ile.HCl. XRD measurements as a function of temperature up to 428 K show an irreversible phase transformation. This transformation was obtained after 32 hours keeping the L‐Ile.HCl.H2O sample at 413 K. The analysis shows that phase transformation occurs due to water and chlorine losses without destroy the amino acid carbon chain and in the end of transformation only the precursor amino acid remains. L‐Ile.HCl.H2O present low thermal stability and the phase transformation is time and temperature dependent.     

Sequential reactions from catalytic hydroformylation toward the synthesis of amino compounds

Different families of new amino compounds were efficiently synthesized, through optimized sequential processes, involving rhodium catalyzed hydroformylation as the key step. The selection of appropriate hydroformylation catalytic systems and reaction conditions allowed obtaining aldehydes derived from several n-alkyl olefins, cholest-4-ene and 3-vinyl-1H-indole, which were subsequently transformed, in one-pot, in to α-amino acids via hydroformylation/Strecker reaction, and in to tertiary amines via hydroaminomethylation, with excellent yields.     

Reversible coordinative chain transfer polymerization of styrene by rare earth borohydrides,chlorides/dialkylmagnesium systems

The ability of various rare earth borohydride and chloride complexes/n‐butylethylmagnesium systems to operate styrene chain transfer polymerization in mild conditions has been assessed. Thirteen precatalysts have been considered: the rare earth trisborohydrides Ln(BH₄)₃(THF)_x (x = 3, Ln = Nd (1), La (2), Sm (3), x = 2, Ln = Y (4), Sc (5)), the rare earth chlorides LnCl₃(THF)_x (x = 3, Ln = Nd (6), La (7), Sm (8), Y (9), x = 2, Ln = Sc (10)), the mixed La(BH₄)₂Cl(THF)_2.6 (11) and the half‐lanthanidocenes Cp*Ln(BH₄)₂(THF)₂ (Ln = Nd (12), La (13)). Six systems were found to be active precatalysts for the polymerization of styrene. 1 , 2 , and 11 led to an efficient transmetalation of the growing polystyrene chain with the simultaneous occurrence of βH elimination, whereas 7 , 12 , and 13 led to catalyzed chain growth behavior. It is noteworthy that the catalyzed chain growth obtained with 12 and 13 occurs with significant stereoselectivity. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 802–814, 2010     

Microwave-assisted synthesis of 3-hydroxy-4-pyridinone/naphthalene conjugates. Structural characterization and selection of a fluorescent ion sensor

Two novel 3-hydroxy-4-pyridinone/naphthalene conjugates (L1 and L2) with different distances between the chelating and the fluorescent moieties were synthesized using conventional heating and microwave irradiation achieving a shorter reaction time. The structure of both compounds was confirmed by X-ray crystallography, revealing that these compounds were isolated as hydrochloride salts in dihydroxypyridinium forms. In solution and in the presence of a base, the tautomeric keto forms may be obtained as it was elucidated by NMR analysis. The dihydroxypyridinium form of L1 exhibits fluorescence at 450 nm, both in ACN and DMSO, whereas the corresponding keto form exhibits fluorescence at 365 nm. In contrast, the dihydroxypyridinium form of L2 only fluoresces in DMSO, exhibiting a band at 340 nm, while the keto form is non-fluorescent. These distinct fluorescent behaviors reveal that the tautomeric form in which the ligands are isolated and the distance between the chelating and fluorescent functions strongly influences their fluorescence properties. Ligand L1 exhibits better fluorescence properties and its fluorescence intensity is quenched in the presence of variable concentration of Cu²⁺, Zn²⁺, and Fe³⁺, thus making it suitable to be used as ion sensor.     

A study of the removal of selenite and selenate from aqueous solutions using a magnetic iron/manganese oxide nanomaterial and ICP-MS

Selenium (Se) is naturally occurring in the environment and is an essential nutrient in mammals. However, environmental Se can be increased to toxic levels through different industrial practices. The potential adsorption of the Se oxoanions, selenite and selenate, from aqueous solutions onto nanosynthesized MnFe₂O₄ was investigated using batch techniques and DRC-ICP-MS spectroscopy. The nanomaterial (NM) was laboratory synthesized through slow titration of a mixture of Fe²⁺ and Mn²⁺ ions. X-ray diffraction and Scherrer's equation were used to determine the phase of the material and crystallite size, respectively. The effects of pH, reaction time, competitive anions, and the adsorption capacity of the synthesized NM to bind selenite and selenate were investigated. The Langmuir isotherm was used to determine the binding capacity of the NM. Results showed that the phase of the nanomaterial was similar to Jacobsite with a size of 27.5 nm. Results also showed that the sorption of either 100 ppb of selenite or selenate was pH independent in the pH range 2 to 6 and occurred within 5 min of contact time. The introduction of Cl⁻ and NO₃⁻ anions individually added to solution had no significant effect on the sorption of either selenite or selenate. However, it was found that the addition of SO₄²⁻ had a competitive effect only on the sorption of selenate, first seen at 10 ppm and more pronounced at 100 ppm of SO₄²⁻. In the presence of 100 ppm of PO₄³⁻, the adsorption of selenate decreased to 87% while selenite sorption decreased to 20%. From the Langmuir isotherm equation it was determined that the nano-Jacobsite had a selenite and selenate binding capacity of 6573.76 and 769.23 mg Se/kg of NM, respectively.     

Measurement of the B(+) production cross section in pp collisions at sqrt[s]=7 TeV

Measurements of the total and differential cross sections dσ/dp(T)(B) and dσ/dy(B) for B(+) mesons produced in pp collisions at sqrt[s]=7 TeV are presented. The data correspond to an integrated luminosity of 5.8 pb(-1) collected by the CMS experiment operating at the LHC. The exclusive decay B(+)→J/ψK(+), with J/ψ→μ(+)μ(-), is used to detect B(+) mesons and to measure the production cross section as a function of p(T)(B) and y(B). The total cross section for p(T)(B)>5 GeV and |y(B)|<2.4 is measured to be 28.1±2.4±2.0±3.1 μb, where the first uncertainty is statistical, the second is systematic, and the last is from the luminosity measurement.     

Measurement of the t-channel single top quark production cross section in pp collisions at √s=7 TeV

Electroweak production of the top quark is measured for the first time in pp collisions at √=7 TeV, using a data set collected with the CMS detector at the LHC and corresponding to an integrated luminosity of 36 pb?1. With an event selection optimized for t-channel production, two complementary analyses are performed. The first one exploits the special angular properties of the signal, together with background estimates from the data. The second approach uses a multivariate analysis technique to probe the compatibility with signal topology expected from electroweak top-quark production. The combined measurement of the cross section is 83.6±29.8(stat+syst)±3.3(lumi) pb, consistent with the standard model expectation.     

Search for stopped Gluinos in pp collisions at square root s=7 TeV

The results of the first search for long-lived gluinos produced in 7 TeV pp collisions at the CERN Large Hadron Collider are presented. The search looks for evidence of long-lived particles that stop in the CMS detector and decay in the quiescent periods between beam crossings. In a dataset with a peak instantaneous luminosity of 1×10(32) cm-2 s-1, an integrated luminosity of 10 pb-1, and a search interval corresponding to 62 hours of LHC operation, no significant excess above background was observed. Limits at the 95% confidence level on gluino pair production over 13 orders of magnitude of gluino lifetime are set. For a mass difference mg - mχ1(0) >100 GeV/c2, and assuming BR(g→gχ1(0))=100%, mg < 370 GeV/c2 are excluded for lifetimes from 10 μs to 1000 s.     

Study of Z Boson Production in PbPb Collisions at √S(NN)=2.76 TeV

A search for Z bosons in the μ(+)μ(-) decay channel has been performed in PbPb collisions at √S(NN)=2.76 TeV with the CMS detector at the LHC, in a 7.2 μb(-1) data sample. The number of opposite-sign muon pairs observed in the 60-120 GeV/c(2) invariant mass range is 39, corresponding to a yield per unit of rapidity (y) and per minimum bias event of [33.8±5.5(stat)±4.4(syst)]×10(-8), in the |y|<2.0 range. Rapidity, transverse momentum, and centrality dependencies are also measured. The results agree with next-to-leading order QCD calculations, scaled by the number of incoherent nucleon-nucleon collisions.