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991.
化学衍生-高效液相色谱法测定硫氰酸根阴离子 总被引:4,自引:0,他引:4
以α-溴-2,3,4,5,6-五氟甲苯作柱前衍生试剂,经优化衍生和色谱条件,实现了用高效液相色谱法测定硫氰酸根离子。在ODS柱上,用甲醇-水(80:20)作流动相,于254nm检测,得到线性关系良好的工作曲线,最小检测限为4.7ng。分析了吸烟者唾液样品,回收率为93.7%~101.4%。 相似文献
992.
2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺与铂(Ⅳ)显色反应的研究 总被引:8,自引:0,他引:8
研究了2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺(3,5-diCl-PADMA)与铂(Ⅳ)的显色反应及铂配合物的质子化行为。结果表明,在0.04~0.48mol/L的H2SO4溶液中,于加热的条件下,试剂可与铂(Ⅳ)形成稳定的1∶2绿蓝色PtL2H2+2配合物,其最大吸收波长位于634nm,表观摩尔吸光系数为9.73×104L·mol-1·cm-1,桑德尔灵敏度为0.002μg·cm-2。铂配合物的三级质子化常数分别为:lgKa1=3.91,lgKa2=-2.21,lgKa3=-3.37。较大量的常见金属离子及除钯、钌外的其它贵金属离子不干扰测定。利用Pt,Pd与试剂反应所需的温度差异,可以用差减法消除微量Pd的干扰.铂(Ⅳ)浓度在每10mL0~7.5μg范围内符合比尔定律。所拟方法用于二次合金管理样-88及催化剂中微量铂的测定,结果满意。 相似文献
993.
表面修饰纳米CdS制备中两个重要影响因素及结构表征 总被引:12,自引:0,他引:12
利用溶胶-凝胶法制备了PVP表面修饰的CdS纳米晶粒。考察了影响纳米CdS制备的两个重要因素Cd2+/S2-和PVP,及其作用机理。确证表面过剩S2-和PVP在反应体系中的作用是在较高浓度下制备纳米CdS的两个重要因素,进一步确定了PVP的最佳用量。通过TEM、ED、XRD、FT-IR等手段对合成的纳米粒子进行了结构表征,最小粒径为7~10nm,闪锌矿构型,粒子大小及形貌可通过改变Cd2+/S2-及反应物浓度来控制。最后给出了CdS/PVP纳米晶粒的结构模型。 相似文献
994.
Eric Monflier Sbastien Tilloy Georges Fremy Yves Castanet Andr Mortreux 《Tetrahedron letters》1995,36(52):9481-9484
Solvent free biphasic hydroformylalion of various water-insoluble terminal olefins can be achieved in high yields and sclcctivitics by using a water-soluble rhodium/triphenylphosphine trisulfonate catalyst and per(2,6-di-o-mclhyl)-β-cyclodcxtrin as inverse phase transfer catalyst. The catalytic activities were up to ten times higher than those observed without pcr(2,6-di-o-methyl)-β-cyclodextrin. 相似文献
995.
Roger Douillard 《Colloids and surfaces. B, Biointerfaces》1993,1(6):333-340
Knowledge of the equation of state of adsorbed or deposited layers of proteins at the air/water interface is of fundamental interest in the understanding of the surface activity of these molecules. Using scaling laws of current polymer theories, it has been shown that the equation of state of the interfacial layer in the semi-dilute regime should relate the surface pressure to the surface concentration through a power law. The exponent of this power law should reflect the quality of the solvent and the conformation of the adsorbed polypeptide chain. In the case of β-lactoglobulin layers, in the range of surface concentrations that should correspond to the semi-dilute regime, the relationship between surface pressure and surface concentration is expressed as a power law. The exponent of this power law is strongly influenced by the nature of the aqueous substrate and by the net charge of the protein molecule. The use of scaling laws gives a coherent view of the expansion of the polypeptide chain in the interfacial layer and of the relationship between surface concentration and surface pressure in the semi-dilute regime. This result favours a strong similarity between β-lactoglobulin and a polymer chain in the interfacial layer. It is concluded that current theories of polymer adsorption could be applied to interfacial protein layers. 相似文献
996.
Enthalpies of dilution of formamide, N-methylformamide, N-ethylformamide, N-propylformamide, N-butylformamide, N-pentylformamide, N,N-diethyl-formamide, N,N-dipropylformamide, N,N-dibutylformamide, and N,N-dipentyl-formamide dissolved in N,N-dimethylformamide as solvent have been measured calorimetrically at 25°C. The results are interpreted in terms of the McMillan-Mayer theory. Enthalpic interaction parameters are obtained for pairs, triplets, and in some cases, quadruplets of solute molecules. In general, the enthalpic pair interaction coefficients are negative, whereas the triplet coefficients are positive. The interaction enthalpies are positive only for N-methylformamide and formamide. The magnitudes of the enthalpic pair and triplet interaction coefficients increase with increasing number of C atoms in the N-alkyl groups. The results for the formamides presented in this paper are compared with those for corresponding acetamides published earlier. Although the trends are comparable, distinct differences are observed. The contribution of the -CH3 group at the CO side of the dialkylacetamides to the enthalpic interaction coefficients appears to be negligible. The same is true for -CH2 groups at the NH side of a number of amides and related compounds. The enthalpic pair interaction coefficients of the mono-N-alkylsubstituted formamides show a shift of about 100 J-kg-mol–2 as compared with isomeric N-alkylacetamides. This is discussed in terms of the difference in proton donating and accepting ability of several types of amide molecules. It is concluded that substitution effects should be incorporated in additivity models for these type of systems. 相似文献
997.
The rapid determination of protein in plant material based on spectrophotometric determination of amino acids in protein hydrolysates with trinitrobenzenesulfonic acid has been adapted to flow injection analysis. With the manifold described, a routine sampling rate of 120 samples/h is possible, though this, as well as sensitivity, can easily be varied. The method was calibrated against the Kjeldahl method and a good correlation was obtained between the two methods over a wide range of protein values for beans. 相似文献
998.
Pd(OAc)2/FePc催化环己烯氧化合成环己酮的研究 总被引:6,自引:0,他引:6
考察了几种Fe-大环配合物与Pd(OAc)2组成的双组分催化体系,在乙腈酸性水溶液中环己烯经合成环己酮的催化活性,实验结果表明,其中以酞菁失(FePc)与Pd(OAc)2组成的催化体系活性最高,而FeTPPCl与Pd(OAc)2催化体系,虽然催化活性较高,但催化剂的稳定性较低,各种因素对Pd(OAc)2/FePc催化活催化影响的研究结果指出,在无水和酸存在的非水溶液中,Pd(OAc)2/FePc对 相似文献
999.
The reactions of aliphatic β-amino-β-trifluoromethylvinyl ketones with an excess of ethylenediamine at room temperature afforded
the corresponding 2,3-dihydro-1H-1,4-diazepines or substituted 2-acetonyl-2-trifluoromethylimidazolidines (the latter were obtained when the approach to the
carbonyl group was sterically hindered).
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2305–2308, November, 1998. 相似文献
1000.
On the basis of copper sulphate pentahydrate thermal dissociation, for analyzed reactions I to IV, 6 thermokinetic equations was discussed. Arrhenius law parameters were determined and the isokinetic effect (IE) and Kissinger law appearing was analyzed. It was found that only dependence resulting from isokinetic effect, in the form k
m=q/T
m, relates to the suitable thermokinetic Eq. (2) and Kissinger law in modified form (14). The confirmation was made that the possibility of determining the averaged activation energy from thermokinetic equations using suitable correction coefficients exists.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献