共查询到20条相似文献,搜索用时 78 毫秒
1.
2.
3.
气相色谱保留指数通用数据库的研究(三)不同柱温模式下保留指数的相互转换 总被引:2,自引:1,他引:2
由于升温模式(T_0,r)、色谱柱和操作参数(A,T_b,β)的差别,使得T_R不同而影响I_(TP)的可比性,其影响的大小随恒温保留指数RI的温度系数的增加而增加。同时,由于T_R与n偏离了线性关系,采用保留温度线性插值方法计算I_(TP),方法本身就在一定程度上会使I_(TP)的可比性差,即使恒温RI的温度系数为零,I_(TP)也会随GC条件而改变。根据恒温与线性程升的保留值方程建立的各种柱温模式下的保留指数相互转换方法能准确快速地预测不同柱温模式下的保留指数,以此来建立通用数据库以适应不同的分析条件的需要。 相似文献
4.
5.
GC/MS分析煤抽出物中的含硫多环芳香化合物 总被引:9,自引:3,他引:9
煤的索氏抽出物中的含硫多环芳香化合物(PASH)由硅胶柱色谱与配体交换薄层色谱(PdCl_2/SiO_2)两步分离,用毛细管气相色谱(FID与FPD)和色质联用仪分析其组成、结构。通过与文献的色谱保留指数相比较、质谱数据验证,鉴定出贵定煤含硫芳香化合物以三、四环结构为主,主要是二苯并噻吩及其C_1~C_3烷基取代物、苯并萘并噻吩及其烷基取代物,其它稠环含硫芳香化合物较少。 相似文献
6.
由于升温模式(T_0,r)、色谱柱和操作参数(A,T_b,β)的差别,使得T_R不同而影响I_(TP)的可比性,其影响的大小随恒温保留指数RI的温度系数的增加而增加。同时,由于T_R与n偏离了线性关系,采用保留温度线性插值方法计算I_(TP),方法本身就在一定程度上会使I_(TP)的可比性差,即使恒温RI的温度系数为零,I_(TP)也会随GC条件而改变。根据恒温与线性程升的保留值方程建立的各种柱温模式下的保留指数相互转换方法能准确快速地预测不同柱温模式下的保留指数,以此来建立通用数据库以适应不同的分析条件的需要,特别是从2种升温模式出发预测其它柱温模式下的保留值能更方便地对复杂样品的分离条件进行优化。 相似文献
7.
8.
9.
采用X射线衍射技术研究了Al_0.9Fe_0.1和Al_0.9Fe_0.05Ce_0.05合金的液态结构及Al_0.9Fe_0.05Ce_0.05合金的非晶结构,并采用DSC热分析研究了非晶合金的晶化行为.发现液态和非晶态合金的结构因子曲线上都存在明显的预峰,所对应的化学短程有序结构随温度降低,尺寸不断增大,但其结构单元的尺寸保持不变.Ce的加入使液态合金中化学短程有序及其结构单元的尺寸增大,并有利于原子间交互作用增强,从而提高非晶形成能力.预峰所对应的化学短程有序结构单元是以Fe原子为中心的二十面体准晶结构,这种结构在液态已形成,并保留在非晶中. 相似文献
10.
11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
12.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
13.
Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
14.
The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
15.
Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
16.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
17.
N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
18.
A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
19.
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
20.
A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献