Deformation der Mikrofibrillen von Baumwoll-und Bakterien-Cellulose

Ohne Zusammenfassung     

A magic-angle rotor for NMR using a forced gas bearing

A new design for a rotor system to achieve spinning rates of the order of 3 kHz is presented. The design uses a simple cylindrical rotor, and involves a forced air bearing over the whole cylindrical surface. The jets of gas which make this bearing also cause the spinning. Powder-filled hollow rotors spin smoothly, and are convenient to make and use. The whole system is suitable for magic angle rotation, such as is needed to obtain high-resolution NMR spectra of solids. Examples of spectra obtained using the device are illustrated and discussed.     

Amino Acid Sequence of N-Terminal Peptide of Normal Human Serum Albumin

From the peptic digest of normal human serum albumin., the N-terminal peptide comprising 24 amino acid residues was obtained by means of peptide mapping. Combined uses of trypsin, α-chymotrypsin, thermolysin, carboxypeptidase A and Dansyl-Edman technique resulted in the elucidation of amino acid sequence of no. 1 to no. 24 as follows: NH₂-Asp-Ala-His-Lys-Ser-Glu-Val-Ala-His-Arg-Phe-Lys-Asp-Leu-GIy-Glu-Glu-Asn-Phe-Lys-Ala-Leu-Val-Leu-COOH These sequence results agree completely with those recently published by other workers.     

热轧带钢层流冷却设定模型的开发与实现

分析了热轧带钢层流冷却的传热过程,基于传热过程给出了冷却控制的空冷和水冷温降计算模型,该模型为线性回归模型,不同于理论的指数温降模型,回归数据取自于现场,更具有实用性,具有模型结构简单、精度高的特点·对层流冷却的设定计算(预设定和修正设定计算)的程序实现方法进行了详细描述,讨论了层流冷却系统中的组别划分,并给出了冷却控制系统的数据流程·本系统的冷却能力强,具有较宽的冷却速率调整范围,运行情况以及使用控制效果良好,能满足现场生产以及新品种开发的要求·     

N‐[1‐(Penta­fluoro­phenyl)­ethyl]­acetamide

The title compound, C₁₀H₈F₅NO, crystallizes as a racemate with four symmetry‐independent mol­ecules in the asymmetric unit. The four mol­ecules form two hydrogen‐bonded pairs. Each pair is a building unit of an independent C(4) chain propagating parallel to the ab plane.     

Evaluation of the stability and selectivity for various adjustable stationary phases using zirconium oxide supports in high-performance liquid chromatography

The selectivity and retention properties of a zirconia stationary phase were reversibly altered using various ligands containing Lewis base functional groups. A simple loading procedure allowed a variety of ligands to be attached to the zirconia surface via Lewis interactions. The resulting stationary phases were shown to be stable and produced different selectivity and retention properties from the native zirconia material. The metal oxide adsorbent was converted to a diol-type stationary phase using glucose-6-phosphate for use under normal-phase conditions. Reversed-phase supports were produced by loading either octyl- or octadecylphosphonic acid onto the native zirconia support. The properties of these new phases were then compared to commercially available bonded silica analogs. Ligands bound to the surface in this manner were effectively removed and the native zirconia was regenerated using a dilute base wash procedure.     

Mechanistic studies on the B(C(6)F(5))(3) catalyzed allylstannation of aromatic aldehydes with ortho donor substituents

Mechanistic studies on the B(C(6)F(5))(3) catalyzed allylstannation of isomeric substituted benzaldehydes are reported. Confirming a report by Maruoka et al., good (5:1) to excellent (>20:1) selectivities for ortho over para isomers are observed when 1:1 mixtures (X = OMe, Cl, F, OTBS) are allylstannated with C(3)H(5)SnBu(3) in the presence of B(C(6)F(5))(3) (2.5% per CHO). The best selectivities are observed for the anisaldehydes. Multinuclear NMR studies on solutions of B(C(6)F(5))(3) and C(3)H(5)SnBu(3) (1:1 to 1:5) show that the borane abstracts the allyl group from the organotin reagent, forming an adduct (C(6)F(5))(3)B...CH(2)CHCH(2)SnBu(3), 1, or ion pair [(C(6)F(5))(3)BCH(2)CH=CH(2)](-)[Bu(3)SnCH(2)CHCH(2)SnBu(3)](+), 2, depending on the reagent ratio. These compounds are important in the mechanism of Lewis acid catalyzed 1,3-isomerization of substituted allyl stannanes. When allyltin reagent is added to solutions of B(C(6)F(5))(3) and ortho-anisaldehyde (1:5) at -60 degrees C, conversion to the stannylium ion pair [Bu(3)Sn(ortho-anisaldehyde)(2)](+)[o-ArCH(allyl)OB(C(6)F(5))(3)](-), o,o-4, is observed. The structure of this species was confirmed by (1)H, (11)B, (19)F, and (119)Sn NMR spectroscopy and by forming related ion pairs (o-5 and o,o-5) utilizing the [B(C(6)F(5))(4)](-) counteranion via reaction of [Bu(3)Sn](+)[B(C(6)F(5))(4)](-) with aldehyde. The anion in o,o-4 is formed via direct allylation of the ortho-anisaldehyde/B(C(6)F(5))(3) adduct o-3, while the cation arises upon aldehyde ligation of the resulting tributylstannylium ion. The crystal structure of the related derivative ortho-C(6)H(4)(OMe)CHO x SnMe(3)BF(4), 6, showed that the aldehyde binds the tin nucleus only through the carbonyl oxygen. Similar reactions using para-anisaldehyde show that formation of p,p-4 occurs at a much slower rate, again demonstrating the preference for the ortho substituted substrates. For similar experiments using benzophenone, however, formation of the ion pair [Bu(3)Sn(Ph(2)CO)(2)](+)[(C(3)H(5))B(C(6)F(5))(3)](-), 8, was observed, illustrating the differences subtle changes in substrate can bring. Ion pair 8 is formed via the trapping of 1 by the benzophenone substrate. In the presence of excess aldehyde and allyltin reagent, ion pair o,o-4 catalyzes the allylstannation of aldehyde to give the product stannyl ether. Several lines of experimental evidence suggest this is the true catalyst in the system. The chemoselectivity observed thus does not rely on classical chelation control in any way. Rather, we propose that the ortho donor group stabilizes the developing positive charge at the beta carbon of the allyl group and the tin atom during the allylation event. This stabilization renders the ortho substituted substrates kinetically favored toward allylation irrespective of the Lewis acid employed.