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The present study was conducted to investigate the molecular absorption by AlCl in a carbon rod furnace for determination of chlorine in organic compounds, by using the lead atomic line at 261.418 nm emitted from a Pb-hollow cathode lamp. A deuterium lamp was used for the simultaneous background correction. The method enables rapid and accurate determination of trace chlorine in varying organic samples with good precision. The method was tested on different organic chloro-coumpounds and α-pinene products. 相似文献
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Kütt A Movchun V Rodima T Dansauer T Rusanov EB Leito I Kaljurand I Koppel J Pihl V Koppel I Ovsjannikov G Toom L Mishima M Medebielle M Lork E Röschenthaler GV Koppel IA Kolomeitsev AA 《The Journal of organic chemistry》2008,73(7):2607-2620
A general route to functionalized pentakis(trifluoromethyl)phenyl (C6(CF3)5) derivatives, promising building blocks for designing novel stable carbenes, radical species, superacids, weakly coordinating anions and other practically and theoretically useful species, is presented. This pertrifluoromethylation route proceeds via conveniently pregenerated (trifluoromethyl)copper (CF3Cu) species in DMF, stabilized by addition of 1,3-dimethyl-2-imidazolidinone (DMI). These species react with hexaiodobenzene at ambient temperature to give the potassium pentakis(trifluoromethyl)phenoxide along with hexakis(trifluoromethyl)benzene and pentakis(trifluoromethyl)benzene in a combined yield of 80%. A possible reaction pathway explaining the formation of pentakis(trifluoromethyl)phenoxide is proposed. Pentakis(trifluoromethyl)phenol gives rise to easily functionalized pentakis(trifluoromethyl)chlorobenzene and pentakis(trifluoromethyl)aniline. Pertrifluoromethylation of pentaiodochlorobenzene and pentaiodotoluene allows straightforward access to pentakis(trifluoromethyl)chlorobenzene and pentakis(trifluoromethyl)toluene, respectively. XRD structures of several C6(CF3)5 derivatives were determined and compared with the calculated structures. Due to the steric crowding the aromatic rings in all C6(CF3)5 derivatives are significantly distorted. The gas-phase acidities (Delta Gacid) and pKa values in different solvents (acetonitrile (AN), DMSO, water) for the title compounds and a number of related compounds have been measured. The origin of the acidifying effect of the C6(CF3)5 group has been explored using the isodesmic reactions approach. 相似文献
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Abnormal inversion splitting in NH2D: rotational analysis of the nu5 bending vibrational band system
A high-resolution Fourier transform infrared spectrum of the nu(5) bending vibrational band system region of the partially deuterated ammonia molecule NH(2)D has been measured and rotationally analyzed. The spectrum consists of strong a-type transitions between the states of same vibrational symmetry and weaker c-type transitions between the states of different vibrational symmetry. The Hamiltonian model used includes interaction terms between the rotational states of both upper and lower inversion doublets. The vibrational term values for the symmetric and the antisymmetric component of the upper-inversion doublet are 1,605.637 965(620) cm(-1) and 1,590.993 82(100) cm(-1), respectively, where the numbers in parentheses are one-standard deviations in the least significant digit. These figures are close to the corresponding values 1,605.62 cm(-1) and 1,590.72 cm(-1) obtained recently from results based on high-level ab initio calculations. The order of the vibrational term values is abnormal in the ammonia family, as typically the symmetric state is lower in wavenumber than the antisymmetric one. 相似文献
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In this work, the mechanochemical synthesis of a moderately agglomerated tin oxide (SnO2) powders and the subsequent preparation of semiconductor gas sensors as prototypes, were studied. Tin (II) chloride (SnCl2) powder was milled with calcium hydroxide (Ca(OH)2) and potassium carbonate, (K2CO3) powder, respectively, in a ball mill at room temperature and in an air atmosphere. Heat treatment of milled mixtures at 400 °C resulted in the formation of a tetragonal phase, confirmed by X-ray diffraction (XRD). During milling in the presence of water, a high number of hydroxide (OH) groups are formed at the surface. When SnCl2 was milled with K2CO3, no water was produced and the Fourier-transform infrared spectrum (FT-IR) of the powder has no surface hydroxyl deformations. On exposure to hydrogen sulfide (H2S) gas, the particles, prepared from anhydrous powder, have higher sensitivity than these, prepared from hydrated powder. The SnO2 thick film, prepared from anhydrous powder may be successfully applied to a H2S gas sensor. 相似文献
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Toom L Kütt A Kaljurand I Leito I Ottosson H Grennberg H Gogoll A 《The Journal of organic chemistry》2006,71(19):7155-7164
Basicity constants for a series of 3,7-diazabicyclo[3.3.1]nonane derivatives in acetonitrile with a variation over 13 orders of magnitude have been determined using a spectrophotometric titration technique. An excellent correlation between basicity and calculated proton affinities obtained at PCM-B3LYP/6-31+G(d)//B3LYP/6-31G(d) level was found. The results are discussed in terms of substituent effects and compared to (15)N NMR chemical shifts. 相似文献
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Birgit Maaten Lauri Loo Alar Konist Andres Siirde 《Journal of Thermal Analysis and Calorimetry》2018,131(3):2087-2091
Four oil shale samples with different amounts of organic and mineral matter were analysed through non-isothermal thermogravimetric analysis using a heating rate of 50 °C min?1 in nitrogen. The goal of the paper is to study the supposed catalytic effect of the indigenous and removed minerals. The samples contained 30, 49, 70 and 90% of organic matter, respectively. X-ray diffraction analysis was used to identify the minerals in the samples. Thermal analysis experiments were carried out up to temperatures of 850 °C in pyrolysis conditions. The mass loss data were used to study the variations in the conversion profiles of the organic matter depending on the content of the mineral matter. The obtained data and the comparison of the sample composition show that the effect of the mineral matter amount on the course of the pyrolysis processes is insignificant. 相似文献
20.
The preparation and H2S sensing potential of thick‐films of a mixed oxide, Fe2O3? Fe2(MoO4)3, were investigated. A Fourier‐transform infrared (FTIR) study confirmed the existence of sulfur species at the surface after the interaction of H2S gas with the mixed oxide. The starting material, β‐FeMoO4, was synthesized by a solvothermal method, followed by supercritical drying. Heat treatment of this material (oxidation) above 500 °C resulted in the formation of Fe2O3? Fe2(MoO4)3 mixed oxide, where Fe2O3 was a by‐product. An increase in the conductivity of the films in the presence of H2S gas (concentration range 1–20 ppm in air) was observed with the simultaneous formation of water and sulfide ions at 225 °C. An improvement of the H2S sensing potential is obtained, using an intermediate short heat treatment at higher temperature (500 °C) in the beginning of recovery (desorption) phase. This intermediate high temperature, used before every expected exposure to H2S gas, may contribute the formation of an initial surface coverage of O2?. 相似文献