Development of a finite-element analysis methodology for the propagation of delaminations in composite structures

Analysing the collapse of skin-stiffened structures requires capturing the critical phenomenon of skin-stiffener separation, which can be considered analogous to interlaminar cracking. This paper presents the development of a numerical approach for simulating the propagation of interlaminar cracks in composite structures. A degradation methodology was introduced in MSC.Marc, which involved the modelling of a structure with shell layers connected by user-defined multiple-point constraints (MPCs). User subroutines were written that employ the virtual crack closure technique (VCCT) to determine the onset of crack growth and modify the properties of the user-defined MPCs to simulate crack propagation. Methodologies for the release of failing MPCs are presented and are discussed with reference to the VCCT assumption of self-similar crack growth. The numerical results obtained by using the release methodologies are then compared with experimental data for a double-cantilever beam specimen. Based on this comparison, recommendations for the future development of the degradation model are made, especially with reference to developing an approach for the collapse analysis of fuselage-representative structures. Russian translation published in Mekhanika Kompozitnykh Materialov, Vol. 43, No. 1, pp. 15–42, January–February, 2007.     

Evaluation of different tubing geometries for high-speed counter-current chromatography

Different tubing geometries were evaluated for use in high-speed counter-current chromatography. Standard round tubing was compared to rectangular and twisted rectangular tubing. The number of theoretical plates for a standard anthocyanin mixture from black currant was determined for each experiment. The results of twisted rectangular tubing were superior to a standard setup.     

A chiral 28-membered macrocycle with symmetry and structure similar to that of trans-cyclooctene

[reaction: see text] A bridged N,N-di(aryl)-1,2,4,5-benzenediimide was synthesized in which restricted rotation led to two diasteriomeric conformations at room temperature. The more stable syn-macrocycle is achiral, whereas the strained anti-macrocycle possesses planar chirality similar to that of trans-cyclooctene. The structure was characterized by X-ray crystallography, and the enantiomers were resolved by chiral chromatography.     

Optical clock with ultracold neutral atoms

We demonstrate how to realize an optical clock with neutral atoms that is competitive to the currently best single ion optical clocks in accuracy and superior in stability. Using ultracold atoms in a Ca optical frequency standard, we show how to reduce the relative uncertainty to below 10(-15). We observed atom interferences for stabilization of the laser to the clock transition with a visibility of 0.36, which is 70% of the ultimate limit achievable with atoms at rest. A novel scheme was applied to detect these atom interferences with the prospect to reach the quantum projection noise limit at an exceptional low instability of 4 x 10(-17) in 1 s.     

Isolation of the lignan secoisolariciresinol diglucoside from flaxseed (Linum usitatissimum L.) by high-speed counter-current chromatography

High-speed counter-current chromatography was successfully used for the isolation and purification of secoisolariciresinol diglucoside, a bioactive lignan from flaxseed (Linum usitatissimum L.). The solvent system consisted of tert.-butylmethyl ether-n-butanol-acetonitrile-water (1:3:1:5). The purity and identity of the isolated compound was checked by high-performance liquid chromatography analysis in combination with mass spectrometry and NMR measurements.     

Improvement of the fractional uncertainty of a neutral-atom calcium optical frequency standard to 2×10-14

We have investigated the two major effects that limit the accuracy of an optical frequency standard based on laser-cooled neutral calcium atoms, i.e. the residual Doppler shift and atomic collisions. A new correction method was applied to reduce the contribution of the residual Doppler effect to the total fractional uncertainty to 1×10^-14. Measurements of the shift of the clock transition frequency due to cold collisions allowed us to reduce their contribution to 4×10^-15. With these improvements we have reduced the total fractional frequency uncertainty of the standard by nearly an order of magnitude to 2×10^-14. Received: 9 August 2002 / Revised version: 16 November 2002 / Published online: 26 February 2003 RID="*" ID="*"Permanent address: Russian Academy of Sciences, P.N. Lebedev Physical Institute, Samara Branch, Novo-Sadovaya st. 221, Samara 443011, Russia RID="**" ID="**"Corresponding author. Fax: +49-531/592-4305, E-mail: uwe.sterr@ptb.de     

Selective and sensitive trace analysis of sulfur mustard with thermal desorption and two-dimensional gas chromatography-mass spectrometry

An improved method is presented for the trace analysis of sulfur mustard (HD) in biological samples, such as blood and tissue from laboratory animals. Using the internal standard method and liquid-liquid extraction with ethyl acetate, up to 400 microL of the extract was injected by thermal desorption from Tenax and analyzed by two-dimensional GC-MS/EI in SIM mode. The analysis was compared with a direct GC injection. Reversed thermal desorption was used as a tool for handling heavily contaminated (fat) samples, thus preventing contamination of the injection system and pre-column. A successful analytical configuration has been set up for the bioanalysis of HD at the low, toxicologically relevant pM level. A detection limit of 10 pg mL(-1) blood or pg g(-1) tissue of sulfur mustard (S/N=3) was established by using this configuration.     

Determination of vitamin B12 in infant formula and adult nutritionals using HPLC after purification on an immunoaffinity column: first action 2011.09

During the "Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting," on June 29, 2011, the method "Determination of vitamin B12 in infant formula and adult nutritionals using HPLC after purification on an immunoaffinity column" was recommended by an Expert Review Panel and adopted as AOAC Official First Action status. The method is applicable for the determination of vitamin B12 in milk-based infant formula. Vitamin B12 is extracted from the sample in sodium acetate buffer in the presence of potassium cyanide. After purification and concentration with an immunoaffinity column (IAC), vitamin B12 is determined by LC with UV detection (361 nm). Data supplied by CLF demonstrated linear response over a wide range of concentrations (1.4-39 microg/100 mL). The analytical range is 0.2-10 microg/100 g, depending on the capacity of the IACs (0.01-0.5 microg), the input weight, and dilutions. Recovery rates were assessed using National Institute of Standards and Technology SRM 1849, and determined to be 95.1%, with SD of 0.34 and CV of 9.0. Measurement uncertainty (UE) was 0.8 microg/100 g, which was calculated from the validation data. It is an expanded measurement uncertainty and was obtained through multiplication with a coverage factor k. LOQ values were reported as 0.10 microg/100 g. The performance characteristics of the method met the standard method performance requirements set forth by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals; thus, the method was determined to be appropriate for First Action status.     

Effect of changes in the deuterium content of drinking water on the hydrogen isotope ratio of urinary steroids in the context of sports drug testing

The hydrogen isotope ratio (HIR) of body water and, therefore, of all endogenously synthesized compounds in humans, is mainly affected by the HIR of ingested drinking water. As a consequence, the entire organism and all of its synthesized substrates will reflect alterations in the isotope ratio of drinking water, which depends on the duration of exposure. To investigate the effect of this change on endogenous urinary steroids relevant to doping-control analysis the hydrogen isotope composition of potable water was suddenly enriched from -50 to 200 ‰ and maintained at this level for two weeks for two individuals. The steroids under investigation were 5β-pregnane-3α,20α-diol, 5α-androst-16-en-3α-ol, 3α-hydroxy-5α-androstan-17-one (ANDRO), 3α-hydroxy-5β-androstan-17-one (ETIO), 5α-androstane-3α,17β-diol, and 5β-androstane-3α,17β-diol (excreted as glucuronides) and ETIO, ANDRO and 3β-hydroxyandrost-5-en-17-one (excreted as sulfates). The HIR of body water was estimated by determination of the HIR of total native urine, to trace the induced changes. The hydrogen in steroids is partly derived from the total amount of body water and cholesterol-enrichment could be calculated by use of these data. Although the sum of changes in the isotopic composition of body water was 150 ‰, shifts of approximately 30 ‰ were observed for urinary steroids. Parallel enrichment in their HIR was observed for most of the steroids, and none of the differences between the HIR of individual steroids was elevated beyond recently established thresholds. This finding is important to sports drug testing because it supports the intended use of this novel and complementary methodology even in cases where athletes have drunk water of different HIR, a plausible and, presumably, inevitable scenario while traveling.