以混合模板剂合成TS—1分子筛及其性能研究

以四丁基溴化铵（ＴＢＡＢｒ）＋四乙基氢氧化铵（ＴＥＡＯＨ，ｎ（ＴＢＡ＾＋）／ｎ（ＴＥＡ＾＋）＝１）或以四丙基溴化铵（ＴＰＡＢｒ）＋ＴＥＡＯＨ为模板剂，钛酸四丁酯和正硅酸乙酯为原料，于１７０℃水热合成出ＴＳ－１分子筛。对合成的ＴＳ－１样品进行了ＸＲＤ，ＦＴ－ＩＲ，ＳＥＭ和ＢＥＴ比表面积分析，证实了样品中钛已进入Ｓｉｌｉｃａｌｉｔｅ－１骨架。选择戊烷氧化为探针反应，考察了ＴＳ－１的催化活性。结果表明以     

STUDIES ON THE SYNTHESIS OF TRACHYLOBAGIBBERELLINANALOGUE(Ⅱ)SYNTHESIS OF DIMETHYLESTER OF 3-HYDROXY-△1_10-12,16-CYCLOGIBBERELLIN 12

ＳＴＵＤＩＥＳ　ＯＮ　ＴＨＥ　ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＴＲＡＣＨＹＬＯＢＡＧＩＢＢＥＲＥＬＬＩＮＡＮＡＬＯＧＵＥ（Ⅱ）ＳＹＮＴＨＥＳＩＳ　ＯＦ　ＤＩＭＥＴＨＹＬＥＳＴＥＲ　ＯＦ　３－ＨＹＤＲＯＸＹ－△１_１０－１２，１６－ＣＹＣＬＯＧＩＢＢＥＲＥＬ?..     

ELECTRODEPOSITION OP Ba－K－Bi－O AND Ba－K－M－Bi－O （M＝Rb， Pb AND La） SINGLE CRYSTALS

ＥＬＥＣＴＲＯＤＥＰＯＳＩＴＩＯＮＯＰＢａ－Ｋ－Ｂｉ－ＯＡＮＤＢａ－Ｋ－Ｍ－Ｂｉ－Ｏ（Ｍ＝Ｒｂ，ＰｂＡＮＤＬａ）ＳＩＮＧＬＥＣＲＹＳＴＡＬＳ￥ＬｉａｎｇＺｈｏｎｇＺＨＡＯ；ＪｉｎＢｉａｏＺＨＡＮＧ；ＷｅｉＨｕａＷＡＮＧＳｈｉＨｏｎｇＬＩＵ；ＤａｏＢｅ...     

THE SYNTHESIS OF 4，5－BIS（4＇－BROMOBENZYLTHIO）－1，3－DITHIOLE－2－THIONE WITH ONE DIMENSIONAL INTERMOLECULAR INTERACTIONS

ＴＨＥＳＹＮＴＨＥＳＩＳＯＦ４，５－ＢＩＳ（４＇－ＢＲＯＭＯＢＥＮＺＹＬＴＨＩＯ）－１，３－ＤＩＴＨＩＯＬＥ－２－ＴＨＩＯＮＥＷＩＴＨＯＮＥＤＩＭＥＮＳＩＯＮＡＬＩＮＴＥＲＭＯＬＥＣＵＬＡＲＩＮＴＥＲＡＣＴＩＯＮＳ￥ＦａｎｇＱＩ（Ｉｎｓｔｉｔｕｔｅｏ...     

杂原子B—ZSM—35沸石的干法合成,表征及CO＋H2反应性能的研究

首次利用吸附态模板剂在Ｎａ２Ｏ－ＳｉＯ２－Ｂ２Ｏ３－ＤＥＡ干粉体系中合成了杂原子Ｂ－ＳＺＭ－３５沸石，ＸＲＤ，ＳＥＭ，ＩＲ，及ＣＯ加氢反应研究了其物理化学特性。结果表明，Ｂ原子同晶取代Ａｌ原子进入ＺＳＭ－３５沸石骨加。     

SYNTHESIS OF PHOSPHONO-DIPEPTIDES BY MANNICH-TYPE AND ARBUZOV-TYPE REACTIONS

ＳＹＮＴＨＥＳＩＳＯＦＰＨＯＳＰＨＯＮＯ－ＤＩＰＥＰＴＩＤＥＳＢＹＭＡＮＮＩＣＨ－ＴＹＰＥＡＮＤＡＲＢＵＺＯＶ－ＴＹＰＥＲＥＡＣＴＩＯＮＳ￥ＲｕＹｕＣＨＥＮ；ＱｉｎｇＤＡＩ（ＩｎｓｔｉｔｕｔｅｏｆＥｌｅｍｅｎｔｏ－ＯｒｇａｎｉｃＣｈｅｍｉｓｔｒｙ，Ｎ...     

FLUORESCENCE STUDIES ON SELF－ASSEMBLING BEHAVIOR OF AMPHIPHILES WITH NAPHALENE－1，5－DIOXY GROUP

ＦＬＵＯＲＥＳＣＥＮＣＥ　ＳＴＵＤＩＥＳ　ＯＮ　ＳＥＬＦ－ＡＳＳＥＭＢＬＩＮＧ　ＢＥＨＡＶＩＯＲ　ＯＦ　ＡＭＰＨＩＰＨＩＬＥＳ　ＷＩＴＨ　ＮＡＰＨＡＬＥＮＥ－１，５－ＤＩＯＸＹ　ＧＲＯＵＰＦＬＵＯＲＥＳＣＥＮＣＥＳＴＵＤＩＥＳＯＮＳＥＬＦ－ＡＳＳＥＭ...     

SYNTHESIS OF 5－SUBSTITUTED－2－CHLORO－6－METHYL－4， 7－DIOXOBENZOTHIAZOLE DERIVATIVES

ＳＹＮＴＨＥＳＩＳ ＯＦ ５－ＳＵＢＳＴＩＴＵＴＥＤ－２－ＣＨＬＯＲＯ－６－ＭＥＴＨＹＬ－４， ７－ＤＩＯＸＯＢＥＮＺＯＴＨＩＡＺＯＬＥ ＤＥＲＩＶＡＴＩＶＥＳ￥ＣｕｉＨｕａＬＩＵ；ＢｉｎＬＵ；ＪｉｎｇＬｉｎｇＺＨＡＮＧ（Ｉｎｓｔｉｔｕｔｅｏｆｏｒｇ...     

（E）－β，γ－UNSATURATED NITRILES FROM DIMETHYLSULFONIUM CYANOMETHYLIDE AND 9－ALKENYL－9－BORABICYCLO［3，3，1］NONANES

（Ｅ）－β，γ－ＵＮＳＡＴＵＲＡＴＥＤＮＩＴＲＩＬＥＳＦＲＯＭＤＩＭＥＴＨＹＬＳＵＬＦＯＮＩＵＭＣＹＡＮＯＭＥＴＨＹＬＩＤＥＡＮＤ９－ＡＬＫＥＮＹＬ－９－ＢＯＲＡＢＩＣＹＣＬＯ［３，３，１］ＮＯＮＡＮＥＳＮａｎＳｈｅｎｇＬＩ；ＭｉｎＺｈｉＤＥＮＧ；Ｙ...     

STUDIES ON THE PRENYLFLAVOIDS PART Ⅹ Ⅵ SYNTHESIS OF （±）－3＇， 4＇－METHYLENEDIOXYISODERICINE－A AND （±）－PONGAPINONE－B

ＳＴＵＤＩＥＳＯＮＴＨＥＰＲＥＮＹＬＦＬＡＶＯＩＤＳＰＡＲＴⅩⅥＳＹＮＴＨＥＳＩＳＯＦ（±）－３＇，４＇－ＭＥＴＨＹＬＥＮＥＤＩＯＸＹＩＳＯＤＥＲＩＣＩＮＥ－ＡＡＮＤ（±）－ＰＯＮＧＡＰＩＮＯＮＥ－Ｂ￥ＸｉａｎＹｏｎｇＢＵ；ＬｉａｎＹｕｎＺＨＡＯａｎ...     

Boltzmann statistical consideration on the excitation mechanism of iron atomic lines emitted from glow discharge plasmas

A Boltzmann plot for many iron atomic lines having excitation energies of 3.3–6.9 eV was investigated in glow discharge plasmas when argon or neon was employed as the plasma gas. The plot did not show a linear relationship over a wide range of the excitation energy, but showed that the emission lines having higher excitation energies largely deviated from a normal Boltzmann distribution whereas those having low excitation energies (3.3–4.3 eV) well followed it. This result would be derived from an overpopulation among the corresponding energy levels. A probable reason for this is that excitations for the high-lying excited levels would be caused predominantly through a Penning-type collision with the metastable atom of argon or neon, followed by recombination with an electron and then stepwise de-excitations which can populate the excited energy levels just below the ionization limit of iron atom. The non-thermal excitation occurred more actively in the argon plasma rather than the neon plasma, because of a difference in the number density between the argon and the neon metastables. The Boltzmann plots yields important information on the reason why lots of Fe I lines assigned to high-lying excited levels can be emitted from glow discharge plasmas.     

Measurement of the properties of a CO2 laser induced air-plasma by double floating probe and spectroscopic techniques

The laser-induced breakdown spark has recently been advanced as a method for real-time, in-situ spectrochemical analysis of gases. Many of these analyses take place in ambient air. To better characterize this source, we have measured the temporal variation of temperature and electron density in an air plasma induced by a CO₂ laser operating at 0.5 and 0.8 J/pulse. The electron temperature was measured by the double floating-probe technique (DFP). An excitation temperature for oxygen atoms was determined spectroscopically by Boltzmann plots. Electron density in the plasma was measured from the Stark broadening of the 715.6-nm line of 01. At 0.5 J/pulse, the DFP temperature ranged from 175000 K at 5 μs to less than 10000 K at 25 μs, while the 01 excitation temperature ranged from 19000 K at 1 μs to above 11 000 K at 25 μs. The excitation temperature and electron density agree with values calculated by others from local thermodynamic equilibrium models of an air plasma. While the electron temperature from the DFP method is much higher than the excitation temperature at 5 μs, at times greater than 25 μs the two have converged, implying thermodynamic equilibration between the species.     

Rotational temperatures and LTE in argon ICP

Rotational temperatures deduced from OH molecular spectra have been studied in an analytical argon inductively coupled plasma for various operating conditions. The Boltzmann plots are often curved and temperatures are very different from those deduced from atomic Boltzmann plots or from other molecular species like N₂. Generally non-equilibrium is deduced from these observations. But thermal stability of OH and local gradient in the droplet surroundings can to a great part explain these phenomena. Complex simulations seem useful for a satisfactory explanation.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

A Comparative Study of Calibration Free Methods for the Elemental Analysis by Laser Induced Breakdown Spectroscopy

We have used two calibration free laser induced breakdown spectroscopy (CF-LIBS) methods for the quantitative analysis of Pb–Sn alloys with different compositions. The first method is based on Boltzmann plots where the elemental concentration is determined from the intercept along the y-axis whereas the second method is the electron density conservation method, in which elemental compositions are determined by comparing the experimentally measured number density with the theoretical results obtained by CF-LIBS. The neutral spectral lines of lead and tin have been used for the estimation of plasma temperature by the Boltzmann plot method whereas the Saha–Boltzmann equation has been used to calculate the electron number density. By comparing the results of both CF-LIBS methods, it is concluded that the CF-LIBS (electron number density conservation) method is more appropriate than the CF-LIBS (Boltzmann plot method) for the quantitative elemental analysis.     

Characterization of a laser-induced plasma by spatially resolved spectroscopy of neutral atom and ion emissions.: Comparison of local and spatially integrated measurements

The local values of the parameters that characterize a laser-induced plasma (temperature, electron density, relative number densities of neutral atoms and ions) have been obtained by spatially resolved emission spectroscopy, including the deconvolution of the measured intensity spectra. The plasma has been generated using a Nd:YAG laser with a Fe–Ni alloy in air at atmospheric pressure, and the emission in the time window 3.0–3.5 μs has been detected. The temperature values obtained from neutral atom and ion emissions have been compared in the cases of local and spatially-integrated measurements. Local Boltzmann and Saha–Boltzmann plots with high correlation to linear fittings have been obtained using two broad sets of optically thin neutral atom and ion lines (21 Fe I lines and 15 Fe II lines), resulting in local values of the electronic temperature that coincide within the error. These results of local measurements contrast with those of spatially integrated measurements, for which two different temperatures are obtained from the Boltzmann plots of neutral atoms (9100±150 K) and ions (13 700±300 K). This difference is explained according to the measured distributions of the electronic temperature and the neutral atom and ion number densities, that result in separated emissivity (or population) distributions of neutral atom and ion lines, leading to different neutral atom and ion apparent temperatures (population-averages of the local electronic temperature). Local values of the plasma parameters have been obtained at all the positions with significant emission, including the determination of the electronic temperature from Saha–Boltzmann or Boltzmann plots. The ionization degree is high- and low-varying at the inner part of the plasma, decaying only near the plasma front. The maximum of the ion density does not coincide with the temperature maximum; on the contrary, the axial variation of both the neutral atom and ion densities (that decrease towards the sample surface) is opposite to that of the temperature, a behaviour that is interpreted to result from the plasma expansion process.     

Prediction of collective characteristics for ion ensembles in quadrupole ion traps without trajectory simulations

Fundamental aspects are presented of a two-temperature moment theory for quadrupole ion traps developed via transformation of the Boltzmann equation. Solutions of the moment equations correspond to changes in the ensemble average for any function of ion velocity, because the Boltzmann equation reflects changes to an ion distribution as a whole. The function of primary interest in this paper is the ion effective temperature and its behavior during ion storage and resonance excitation. Calculations suggest that increases in ion effective temperature during resonance excitation are due primarily to power absorption from the main RF trapping field rather than from the dipolar excitation signal. The dipolar excitation signal apparently serves mainly to move ions into regions of the ion trap where the RF electric field, and thus ion RF heating, is greater than near the trap center. Both ideal and non-ideal ion trap configurations are accounted for in the moment equations by incorporating parameterized variables a and q , which are modified versions of the commonly used forms for the DC and AC ring voltages, and b and d , which are new forms that account for the voltages applied to the endcaps. Besides extending the applicability of the moment equations to non-ideal quadrupole ion traps, the modified versions of the parameterized variables can have additional utility. Calculation of the spatial dependence of ion secular oscillation frequencies is demonstrated as an example.     

Spectroscopic Diagnostics of Enhanced Magnetron and Mesh Separation Effects in Cyclonic Atmospheric Pressure Plasma Surface Modification of Polyethylene Terephthalate

The correlation of plasma surface modification consequence and the electron characteristics in plasma state with the enhanced magnetron source and metal mesh screen are studied by cyclonic-atmospheric-pressure plasma on polyethylene terephthalate (PET) surface. The contact angle measurement is employed to examine the plasma modified PET surface hydrophilicity. Optical emission spectroscopy is used to detect the electronic excitation temperature and electron density in cyclonic atmospheric pressure plasma. The electronic excitation temperature and the electron density are measured as the operational conditions of adding magnetron source and metal mesh separation. Boltzmann plot method is employed to estimate the electronic excitation temperature whereas electron density measurement by the Voigt profile. The results show that both electronic excitation temperature and electron density have similar trend i.e., both increasing with the enhanced magnetron source while decreasing trend is observed with passing through the metal mesh.     

An isocratic fluorescence HPLC assay for the monitoring of l-asparaginase activity and l-asparagine depletion in children receiving E. colil-asparaginase for the treatment of acute lymphoblastic leukaemia

A novel assay for the determination of l-asparaginase activity in human plasma is described that is based on the HPLC quantitation of l-aspartic acid produced during enzyme incubation. Methods for monitoring l-asparagine depletion are also described. Chromatography of l-aspartic acid, l-asparagine and l-homoserine (the internal standard) involved derivatization with o-pthaldialdehyde, then separation from other amino acids on a Phenomenex Luna C(18) column using a 1 mL/min flow rate and a mobile phase consisting of di-potassium hydrogen orthophosphate propionate buffer, pH 6, with 10% methanol and 10% acetonitrile. Fluoresence detection was at excitation/emission wavelengths of 357/455 nm. Under these conditions l-aspartic acid, l-asparagine and l-homoserine had retention times of 3.5, 9.8 and 17.7 min, respectively. The l-asparaginase assay was linear from 0.1 to 10 U/mL activity and interday precision and accuracy were less than 13%. The limit of quantitation was approximately 0.03 U/mL. The assay utility was established in 12 children who received E. coli l-asparaginase as treatment for acute lymphoblastic leukaemia.     

Consideration on excitation mechanisms in a high-power two-jet plasma

The study of excitation mechanisms in the region before the jet confluence of a high-power two-jet plasma used for analysis of different powders has been undertaken. Distribution of excited levels of Fe atoms and ions according to the Boltzmann population was found. Measuring Fe atomic and ionic excitation temperatures showed their considerable difference (≈ 2000–2500 K). The effect of argon on line intensities of a wide range of elements was investigated by the experiment with argon covering. A negligible effect of argon covering on line intensities of atoms with ionization energy of < 8 eV allows one to assume their predominant excitation by electron impact. The argon participation in excitation of atoms having ionization energy of > 8 eV was revealed. This is likely to be due to Penning ionization by metastable argon followed by ion recombination with an electron and stepwise de-excitations. A more pronounced effect of argon covering was observed for ionic lines of investigated elements with total excitation energy ranging from 11 to 21 eV. Penning ionization followed by electron impact is believed to be a probable mechanism for ion excitation. The contribution of metastable argon to excitation processes results in departure from local thermodynamic equilibrium and different atomic and ionic excitation temperatures.