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101.
采用带八级杆碰撞/反应池(ORS)的电感耦合等离子体质谱法(ICP-MS),直接测定丙烯腈或乙腈产品中的Fe、Cu,标准加入法定量.结果表明,方法的线性范围宽,线性相关系数均大于0.999.2种元素的相对标准偏差均低于5%,加标回收率在90%~110%.该方法简便、快速、准确. 相似文献
102.
103.
本文在两次标准加入法[1]的基础上,提出了三组份同时测定的三次标准加入法,并应用于钼、钨和钛的流动注射同时测定。测定条件:[水杨基荧光酮(SAF)]=1.25 ×10-4mol/L,[溴化+六烷基三甲基铵(CTMAB)」=2.5×10-3mol/L,pH1.35,25℃,采样、进样时间分别为10s和18s,进样频率128次/h。为消除组份间协同作用引起的吸光度加合性的偏离,定义了三组份协同系数。将其引入三组份同时测定方法,补偿了吸光度对线性的偏离。补偿后钼、钨和钛的测定范围分别为0.05~0.35,0.25~1.00,0.025~0.30mg/L。测定了钢样及模拟样品中钼、钨和钛含量,结果较好。 相似文献
104.
R. De
Lisi G. Lazzara S. Milioto N. Muratore 《Journal of Thermal Analysis and Calorimetry》2007,87(1):61-67
Macromolecule/laponite nanomaterials were
studied by DSC and X-ray diffraction techniques. The matrices are poly(ethylene)
glycols at various molecular masses and poly(ethylene oxides)-poly(propylene
oxides)-poly(ethylene oxides) tri-block copolymers. The latter were tuned
by modulating the molecular masses, at constant hydrophilic/hydrophobic ratio,
and the hydrophilicity. For all the investigated systems, the enthalpy of
melting (ΔH
m)
is nearly constant up to a given composition thereafter it increases monotonically
reaching the value of the pure macromolecule. We proposed a model to interpret
the DSC data.
Briefly, it was invoked a mechanism of interaction
following which some segments of the adsorbed macromolecule are anchored to
the laponite (RD) particles and the remaining segments are radiating away
from the surface. The portion of the macromolecule in contact with RD does
not contribute to ΔH
m
whereas that radiating away from the clay does. Once that the RD surface is
saturated, the excess of the macromolecule behaves like the pure one. The
proposed model allowed to compute successfully the ΔH
m
values. The X-ray diffraction experiments ruled out the polymer intercalation
between the silicate sheets. 相似文献
105.
ICP-AES中内标法的应用研究 Ⅲ.用内标法校正基体干扰 总被引:1,自引:0,他引:1
通过观测基体对分析元素发射强度的干扰情况,分析干扰机制,从而确定用来校正基体干扰的内标元素与分析元素的匹配条件。实验结果表明,只要选择合适的内标元素,可以校正基体干扰。 相似文献
106.
Lebedev B. V. Kulagina T. G. Smirnova N. N. Shifrina Z. B. Averina M. S. Rusanov A. L. 《Journal of Thermal Analysis and Calorimetry》2003,74(3):735-748
In an adiabatic vacuum calorimeter, the temperature dependence of the heat capacity C
p of phenylated polyphenylene and initial comonomer 1,4-bis(2,4,5-triphenylcyclopentadienone-3-yl)benzene was studied between
6 and 340 K with an uncertainty of about 0.2%. In a calorimeter with a static bomb and an isothermal shield their energies
of combustion DUcomb were measured. From the experimental data, the thermodynamic functions C
p
0 (T), H
0(T)-H
0(0), S
0(T)-S0(0), G
0(T)-H
0(0) were calculated from 0 to 340 K, and standard enthalpies of combustion ΔH
comb
0 and thermodynamic parameters of formation-enthalpies ΔH
f
0, entropies ΔH
f
0, Gibbs functions ΔG
f
0 - of the substances studied were estimated at T=298.15 K at standard pressure. The results were used to calculate the thermodynamic characteristics (ΔH
f
0 ,ΔS
f
0, ΔG
f
0) of phenylated polyphenylene synthesis in the range from 0 to 340 K.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
107.
González-Pérez A. Galán J. J. Rodríguez J. R. 《Journal of Thermal Analysis and Calorimetry》2003,72(2):741-749
The specific conductivities of dodecyldimethylbenzylammonium bromide (C12BBr) have been determined in aqueous butanol and
aqueous benzyl alcohol solutions in the temperature range of 5-40°C. From these data the temperature dependent critical micelle
concentration (cmc) was determined. The molar fraction of alcohol in the micelle was estimated using the theory suggested by Motomura et al. for surfactant binary mixtures. The thermal properties such as standard Gibbs free energy, enthalpy and entropy of solubilization
of alcohols in the micelles were estimated for the phase separation model. The change in heat capacity upon solubilization
of alcohol in the micelle has been estimated form the above properties.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
108.
This paper reports our results for the direct experimental determination of the equilibrium constant for the hydrogen-isotope-exchange
reaction, 1/2D2(g)+HCl(hexOH)=1/2H2(g)+DCl(hexOD), where hexOH isn-hexanol and hexOD isn-hexanol with deuterium substitution in the alcohol function. The reaction was studied in electrochemical double cells without
liquid junction for which the net cell reaction is the above isotope-exchange reaction. The experimentally determined value
of ε° (296.0°K) for this cell is 4.03±0.95 mV (strong electrolyte standard states, mole-fraction composition scale); the value
of the equilibrium constant for the reaction is 1.17±0.05. The contributions of isotope-exchange and transfer effects to the
magnitude of the standard Gibbs energy change for the above reaction and for the analogous reaction 1/2D2(g)+HCl(aq)=DCl(daq)+1/2H2(g) are considered. Our results support the conclusion of Heinzinger and Weston that the formulation of the solvated proton
in water as H3O+, as opposed to H9O4
+, is sufficient for the interpretation of the thermodynamics of hydrogen-isotope-exchange reactions in water. We also find
that the formulation of the solvated proton inn-hexanol as ROH
2
+
is sufficient for the interpretation of our results on the thermodynamics of hydrogen-isotope-exchange inn-hexanol. 相似文献
109.
Z. H. Zhang Z. J. Ku H. R. Li Y. Liu S. S. Qu 《Journal of Thermal Analysis and Calorimetry》2005,79(1):169-173
The solid-state ternary complex of terbium chloride with L-tyrosine and glycine, [Tb(Tyr)(Gly)3Cl3·3H2O], was synthesized and characterized. Using a solution-reaction isoperibol calorimeter, the enthalpy of reaction for the following reaction, TbCl3·6H2O(s)+Tyr(s)+3Gly(s)=Tb(Tyr)(Gly)3Cl3·3H2O(s)+3H2O(l), was determined to be (5.1±0.6) kJ mol-1. The standard enthalpy of formation of Tb(Tyr)(Gly)3Cl3-3H2O at T=298.15 K has been derived as -(4267.3±2.3) kJ mol-1. The thermal decomposition kinetics of the complex was studied by non-isothermal thermogravimetry in the temperature range of 325-675 K. Two main mass loss stages existed in the process of the decomposition of the complex, the kinetic parameters for the second stage were analyzed by means of differential and integral methods, respectively. Comparing the results of differential and integral methods, mechanism functions of the thermal decomposition reaction for its second stage were proposed. The kinetic equation can be expressed as: d/dt=Aexp(-E/RT)(1-)2. The average values of the apparent activation energy E and pre-exponential factor A were 213.18 kJ mol-1 and 2.51·1020 s-1, respectively. 相似文献
110.
Yu H. G. Yu Dong J. X. Qin C. Q. Liu Y. Qu S. S. 《Journal of Thermal Analysis and Calorimetry》2004,75(3):807-813
The energy of combustion of crystalline 3,4,5-trimethoxybenzoic acid in oxygen at T=298.15 K was determined to be -4795.9±1.3 kJ mol-1 using combustion calorimetry. The derived standard molar enthalpies of formation of 3,4,5-trimethoxybenzoic acid in crystalline
and gaseous states at T=298.15 K, ΔfHm
Θ (cr) and ΔfHm
Θ (g), were -852.9±1.9 and -721.7±2.0 kJ mol-1, respectively. The reliability of the results obtained was commented upon and compared with literature values.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献