X射线荧光分析中熔融制样条件的研究

本文研究了熔融制样时熔融温度、熔融时间和脱模剂的加入量对分析结果的影响。研究结果表明,随着熔融温度的升高和熔融时间的加长,分析结果的总值将随之增大。相反,脱模剂量的增加会使分析结果降低。通过对熔融样品时产生的升华物的研究,发现在熔触过程中,四硼酸锂比样品以更大的比例逸出熔融体,从而造成了样品在分析圆片中的相对浓缩。而且在高温熔融时,钾和钠比样品中的其他元素例如硅、铝、铁、钛、钙、镁等更易于逸失。制样条件的不同引起样品和熔剂逸失的比例会有变化,它直接影响测定的结果,这证明了在X射线荧光光谱分析中保持制样条件一致的重要性。     

The crystallinity of polyaryl ether ether ketone

Measurement of the degree of crystallinity of the polymer matrix in a composite is complicated by the presence of the reinforcing additive. This is particularly the case in APC-2 in which as much as 70% can be carbon fibre. A First Law procedure, developed for determining the degree of crystallinity of PEEK, which involves direct measurement of the enthalpy changes associated with melting, crystallization and heat capacity changes, has found to be an effective method for the determination of the crystallinity of the PEEK matrix. The procedure has been applied to carbon fibre and glass fibre PEEK composites.     

Enthalpies of Phase Transitions and Heat Capacity of TbCl3 and Compounds Formed in TbCl3–MCl Systems (M=K, Rb, Cs)

The molar enthalpies of the solid–solid and solid–liquid phase transitions were determined by differential scanning calorimetry for pure TbCl₃ and KTb₂Cl₇, RbTb₂Cl₇, CsTb₂Cl₇, K₃TbCl₆, Rb₃TbCl₆ and Cs₃TbCl₆ compounds. Both types of compounds, i.e. M₃TbCl₆ and MTb₂Cl₇ (M=K, Rb, Cs) melt congruently and show additionally a solid–solid phase transition with a corresponding enthalpy Δ_trs H ⁰ of 6.1, 7.6 and 7.0 kJ mol^–1 for potassium, rubidium and caesium M₃TbCl₆ compounds andΔ_trs H ⁰ of 17.1 (rubidium) and of 12.1 and 10.9 kJ mol^–1 (caesium) for MTb₂Cl₇ compounds, respectively. The enthalpies of fusion were measured for all the above compounds with the exception of Rb₃TbCl₆ and Cs₃TbCl₆. The heat capacities of the solid and liquid compounds have been determined by differential scanning calorimetry (DSC) in the temperature range 300–1100 K. The experimental heat capacity strongly increases in the vicinity of a phase transition, but varies smoothly in the temperature ranges excluding these transformations. C _p data were fitted by an equation, which provided a satisfactory representation up to the temperatures of C _p discontinuity. The measured heat capacities were checked for consistency by calculating the enthalpy of formation of the liquid phase, which had been previously measured. The results obtained agreed satisfactorily with these experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of the enthalpy of fusion of K3TaF8 and K3TaOF6

The areas of the fusion and crystallization peaks of K₃TaF₈ and K₃TaOF₆ have been measured using the DSC mode of the high-temperature calorimeter (SETARAM 1800 K). On the basis of these quantities and the temperature dependence of the used calorimetric method sensitivity, the values of the enthalpy of fusion of K₃TaF₈ at temperature of fusion 1039 K: Δ_fusH_m(K₃TaF₈; 1039 K) = (52 ± 2) kJ mol⁻¹ and of K₃TaOF₆ at temperature of fusion 1055 K: Δ_fusH_m(K₃TaOF₆; 1055 K) = (62 ± 3) kJ mol⁻¹ have been determined.     

Comment on papers by K. Shanahan that propose to explain anomalous heat generated by cold fusion

Dr. Shanahan has published two papers (Thermochim. Acta 428 (2005) 207, Thermochim. Acta 382 (2002) 95) in which he argues that excess heat claimed to be produced by cold fusion is actually caused by errors in heat measurement. In particular, he proposes that unrecognized changes in the calibration constant are produced by changes in the locations where heat is being generated within the electrolytic cell over the duration of the measurement. Because these papers may lend unwarranted support to rejection of cold fusion claims, these erroneous arguments used by Shanahan need to be answered.     

Heteroatom derivatives of indene: V. Vibrational spectra of benzimidazole

Infrared and Raman measurements for benzimidazole are presented and discussed, including its argon-matrix infrared spectrum. To assist in the assignment, benzimidazole's harmonic force fields for the 321G* and 631G* levels were scaled by scaled factors derived by fitting the respective computed force fields of other indene derivatives to previously reported experimental vibrational frequencies. Comparison to the best set of experimental wavenumbers, usually taken from the matrix, shows mean 321G* and 631G* deviations of 7.0 and 5.8 cm⁻¹ for the planar modes, and 14.0 and 6.8 cm⁻¹ for the nonplanar modes, respectively, with much of the error residing in imino-hydrogen group modes. Standard entropies are derived with the matrix wavenumbers and the methods of statistical mechanics. An attempt to determine standard entropies by calorimetric methods was unsuccessful. The triple-point temperature T_tp and enthalpy of fusion Δ¹_crH_m only are reported.     

Structural, spectral and thermal studies of N-2-(4-picolyl)- and N-2-(6-picolyl)-N′-(2-chlorophenyl)thioureas and N-2-(6-picolyl)-N′-(2-bromophenyl)thiourea

N-2-(4-picolyl)-N′-2-chlorophenylthiourea, 4PicTu2Cl, monoclinic, P2₁/c, a=10.068(5), b=11.715(2), β=96.88(4)°, and Z=4; N-2-(6-picolyl)-N′-2-chlorophenylthiourea, 6PicTu2Cl, triclinic, P-1, a=7.4250(8), b=7.5690(16), c=12.664(3) Å, =105.706(17), β=103.181(13), γ=90.063(13)°, V=665.6(2) ų and Z=2 and N-2-(6-picolyl)-N′-2-bromophenylthiourea, 6PicTu2Br, triclinic, P-1, a=7.512(4), b=7.535(6), c=12.575(4) Å, a=103.14(3), β=105.67(3), γ=90.28(4)°, V=665.7(2) ų and Z=2. The intramolecular hydrogen bonding between N′H and the pyridine nitrogen and intermolecular hydrogen bonding involving the thione sulfur and the NH hydrogen, as well as the planarity of the molecules, are affected by the position of the methyl substituent on the pyridine ring. The enthalpies of fusion and melting points of these thioureas are also affected. ¹H NMR studies in CDCl₃ show the NH′ hydrogen resonance considerably downfield from other resonances in their spectra.     

脑信息特征的评价分类方法

对脑信息处理的能力特征量和总体偏离度特征量进行了确定性评价分类.在分类数上,提出了common分类法,以一般人的特征作为分类基准,在common两边展开,以确定分类数.在分类边界上,提出了根据特征量的正态分布确定分类边界的方法.若特征量分布不是正态分布,则采用了博克斯和考克斯变换将其变为正态分布,最终得到能力特征量和总体偏离度特征量的分类规则.由于人的行为是脑信息处理在宏观上的表现,所以其研究成果可直接用来评价人的能力和行为特征.