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91.
The mass resolution of a time-of-flight (TOF) mass spectrometer is directly proportional to its total flight pathlength. Multi-turn or multi-passage ion optical geometries are necessary to obtain fight distances of sufficient length within reasonable size limitations. We have investigated ion optics for a multi-turn TOF mass spectrometer with electrostatic sectors. The concept of 'perfect' focusing conditions is introduced. Furthermore, a new type of multi-turn TOF mass spectrometer, the MULTUM Linear plus, was developed. It consists of four cylindrical electric sectors and 28 electric quadrupole lenses. It has a vacuum chamber 60 x 70 x 20 cm in size. Mass resolution is demonstrated to increase according to the number of ion cycles. A mass resolution of 350 000 (m/z = 28, FWHM) was achieved after 501.5 cycles. The MULTUM Linear plus analyzer is not simple, however; 28 electric quadrupole lenses are used. In order to reduce the number of ion optical parts, an improved multi-turn TOF mass spectrometer, the MULTUM II, consisting of only four toroidal electric sectors, was also developed. The possibility of tandem mass spectrometric applications using multi-turn TOF mass spectrometers is also discussed. 相似文献
92.
Krasnov V. P. Levit G. L. Korolyova M. A. Bukrina I. M. Sadretdinova L. Sh. Andreeva I. N. Charushin V. N. Chupakhin O. N. 《Russian Chemical Bulletin》2004,53(6):1253-1256
The influence of the reaction conditions (solvent, base) on the diastereoselectivity of acylation of (±)-3-methyl-2,3-dihydro-4H-1,4-benzoxazine with (S)-naproxen and N-tosyl-(S)-proline chlorides was studied. The highest diastereoselectivity was observed for the reaction carried out in benzene in the presence of aliphatic tertiary amines. 相似文献
93.
不动杆菌静息细胞催化拆分外消旋环戊酮醇乙酸酯反应条件的优化 总被引:4,自引:0,他引:4
考察了反应条件对不动杆菌Acinetobactersp.YQ231催化外消旋环戊酮醇乙酸酯对映选择性水解的反应速度和对映选择性的影响.确定的最佳酶反应条件为pH8.0,温度50℃.不同乳化剂对对映选择性的影响不同,以壬基酚聚氧乙烯醚的效果最好,当其加入量为15g/L时,反应的对映选择性最高.产物环戊酮醇对酶活性有显著的抑制作用.细胞中的酯酶优先水解(R)-环戊酮醇乙酸酯,生成(R)-环戊酮醇,在底物浓度为250mmol/L时,对映体比率(E值)可达50. 相似文献
94.
Kenji Maeda Ross A. Miller Ali Shafiee Joseph D. Armstrong III 《Tetrahedron letters》2005,46(9):1545-1549
Highly diastereoselective (>20:1) bromo-lactonization of N-sulfonyl-2-allyl-2-phenylglycine methyl ester (11) was observed. Successive treatment of the chiral lactone with MeONa gave the desired (2S,4R)-4-hydroxy-2-phenylproline derivative in high yield without erosion of the diastereoselectivity. The starting chiral non-racemic compound (5) was prepared from the racemic 2-phenylglycine using a classical kinetic resolution (crystallization), an asymmetric phase transfer alkylation, and an enzyme-catalyzed kinetic resolution. 相似文献
95.
Marti E. Kaisersberger E. Emmerich W.-D. 《Journal of Thermal Analysis and Calorimetry》2004,77(3):905-934
The definitions of the temperature resolution, the so-called resolution of DSC instruments given in literature are discussed.
A new definition of the resolution for DSC instruments is presented and outlined. The main characteristic introduced in this
new definition is a minimum between two caloric events as a prerequisite of an existing resolution. Possible candidates of
test substances have been evaluated. The oligomer n-hexatriacontane is revealing an interesting phenomenon, namely a lambda
transition which is in the peak temperature only 2 K lower than the melting temperature of 76°C. The substance was selected
as an ideal test substance for the quantification of the resolution of DSC instruments. The lambda transition is a second
order process which may reach under certain conditions the saturation of the occurring molecular dislocation within 0.2 K,
and after saturation the heat flow rate drops sharply down. Investigations concerning the main characteristics of n-hexatriacontane
in respect to the temperatures of transition (lambda transition and melting), to the involved enthalpies, and to the resolution
factors were performed as functions of the sample mass and the heating rate. The importance of relevant evaluation procedures
increasing the resolution factors of DSC curves are discussed and these procedures are integrated into the testing of the
resolution. The necessity for widening the experimental scope from instruments to evaluation procedures is forced by the existence
of instruments with built-in signal treatments based on electronic devices and software procedures. A comparison with literature
data is outlined for all of the mentioned characteristic values of n-hexatriacontane.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
96.
压力流驱动电色谱分析方法及其若干色谱行为 总被引:1,自引:0,他引:1
压力流驱动电色谱分析方法是一种新型色谱技术。它组合了HPLC和电泳两种技术,为分离提供了更多可控制的因素。介绍了压力流驱动电色谱的装置和毛细管电色谱柱的装置方法,从理论上讨论了影响电色谱分离的因素并用实验数据加以证明。最后尝试性地将电色谱法用于测定香蕉样品中萨索啉(Salsolinol)等的含量。 相似文献
97.
PengWANG ShuRenJIANG ZhiQiangZHOU 《中国化学快报》2004,15(12):1457-1460
Cellulose-tris(3,5-dimethylphenylcarbamate)(CDMPC) were synthesized as highperformance liquid chromatography (HPLC) chiral stationary phase(CSP). The successful resolution of four chiral pesticides on the CSP was realized and the influence of the temperature on the separation was studied. 相似文献
98.
Y. Akiyama F. Mizukami H. Izutsu M. Sato K. Maeda Y. Kiyozumi K. Sakaguchi 《Journal of Sol-Gel Science and Technology》1998,13(1-3):421-425
A novel organic-inorganic composite was prepared by a sol-gel process using hydrolysis and condensation of tetraethoxysilane (TEOS) reacted with a saccharide. During the process, ethoxy groups of the TEOS were replaced with hydroxyl groups of the saccharide and, consequently, saccharide molecules were combined with silica through their hydroxyl groups. Samples obtained under different reaction conditions were used for optical resolution of a metal chelate compound. The resolution ability of the composites was affected by the amount of water added for hydrolysis and of the saccharide. In particular, the amount of water drastically influenced the optical resolution performance. Composites obtained at the lower H2O/TEOS ratio gave the metal chelate compound a higher optical rotation. Three types of composites with the same composition were prepared by kneading, impregnation and by the sol-gel method, and were compared. The sol-gel composite showed the best optical resolution ability. It was concluded that the optical resolution ability was closely related to dispersibility of saccharide in the silica matrix. 相似文献
99.
J. Díaz-Ferrero M.C. Rodríguez-Larena L. Comellas B. Jiménez 《Trends in analytical chemistry : TRAC》1997,16(10):1865-573
The usual methods for determining polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF) and polychlorinated biphenyls (PCB) are generally expensive and time consuming. This fact has favored the development of faster and cheaper techniques, based on immunoassays and bioassays. This paper reviews these bioanalytical methods and their analytical importance at the present moment. 相似文献
100.
《Surface and interface analysis : SIA》2004,36(1):92-95
By using modern XPS systems it is possible to obtain spectra with well‐resolved spin orbit, multiplet and field splitting even with powder samples mounted using adhesive tape. Measurement of Cr2O3 powder with the latest generation of XPS spectrometers, which are able to analyse non‐conductive powders with ultimate energy resolution, revealed multiplet splitting features and satellite emission in the Cr 2p spectrum. Therefore, peak‐fit analysis of Cr 2p XPS spectra of Cr(III) compounds requires a more appropriate approach and common practice has to be reconsidered. One possible way to analyse this spectrum is proposed, based on the experimental and theoretical work of other authors. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献