Chromatographic classification and comparison of commercially available reversed-phase liquid chromatographic columns using principal component analysis

A total of 135 commercially available alkyl, cyano, phenyl, perfluorinated, polar embedded, enhanced polar selectivity (i.e., polar/hydrophilic endcapped), "Aqua type" and a variety of novel phases including some non-silica based stationary phases have been characterised in terms of their surface coverage, hydrophobic selectivity, shape selectivity, hydrogen bonding capacity and ion-exchange capacity at pH 2.7 and 7.6. Principal component analysis has been used to provide a simple graphical comparison of the differences/similarities between columns in the entire database and differing subsets such as "Aqua type"/enhanced polar selectivity phases. The PCA has been correlated to the phase's ability to analyse a range of hydrophilic bases.     

Synthesis of R-(-)-imperanene from the natural lignan hydroxymatairesinol

A convenient and high yielding method for the synthesis of R-(-)-imperanene, starting from the readily available natural lignan hydroxymatairesinol from Norway spruce, was developed. Hydroxymatairesinol was degraded in strongly basic aqueous conditions to (E)-4-(4-hydroxy-3-methoxyphenyl)-2-(4-hydroxy-3-methoxyphenylmethyl)but-3-enoic acid, which was esterified and then reduced by LiAlH(4) to afford R-(-)-imperanene. The configuration at the crucial stereocenter was preserved in the synthesis, and the obtained product was identified by optical rotation measurements and chiral HPLC analyses as the R-(-)-enantiomer (ee 86-92%).     

Characterisation of light emitting diodes (LEDs) for application in digital holographic microscopy for inspection of micro and nanostructured surfaces

Partial coherent light sources open up prospects for phase noise reduction in digital holographically reconstructed phase distributions by suppressing multiple reflections in the experimental setup. Thus, light emitting diodes (LEDs) are investigated for application in digital holographic microscopy. First, the spectral properties and the resulting coherence length of an LED are characterised. In addition, an analysis of dispersion effects and their influence on the hologram formation is carried out. The coherence length of LEDs in the range of a few micrometers restricts the maximum interference fringe number in off-axis holography for spatial phase shifting. Thus, the application of temporal phase-shifting-based digital holographic reconstruction techniques is compared to spatial phase-shifting-based methods. It is demonstrated that LEDs are applicable for digital holographic microscopy in connection with both spatial and temporal phase-shifting-based techniques for reduction of noise in comparison to a laser-light-based experimental setup.     

Benchmarking of maintenance performance: a case study in two manufacturers of furniture

When profit margins of a plant are decreasing, the need forreliable and efficient maintenance policy becomes more important.Measuring maintenance performance is important for companiesto recognize whether their planned goals are achieved or not.Also, such measurements can be utilized for benchmarking, whichis one of the tools for never-ending improvement. But, theseobjectives cannot be achieved without well-documented data ofthe relevant variables. Better data coverage and quality isnecessary for following maintenance performance developmentand it would, in many cases, clarify the ambiguity concerningthe main problem in the context, namely that neither the productionnor maintenance department can show what effect maintenancehas on profitability. A more effective maintenance policy indirectly implies improvementsin product quality and manufacturing process effectiveness.Elongation of the production time, i.e. reducing the downtimedue to failures, planned replacements and repair, in additionto the improvement in the total maintenance activities, arealso some of the results that can be expected when an efficientmaintenance policy is used. Measuring and monitoring maintenanceperformance measures is required partly for detecting, and eventuallytreating as soon as possible, undesirable changes and partlyto make benchmarking with the best in the branch, which savesappreciable economic losses for companies. In this paper, a model for how to identify the measurable variables,which are needed to develop measures for monitoring maintenanceperformance behaviour systematically, is developed. Five maintenanceperformance measures are proposed and applied. An additionalmodel for systematically analysing the trend of maintenanceperformance measures, for an overall assessment of the company'ssituation, is presented. Two case studies in manufacturers offurniture are conducted to verify these models.     

Die Konstitution der Melodinus-Alkaloide (+)-Meloscin, (+)-Epimeloscin und (+)-Scandin. 1. Mitteilung über Alkaloide aus Melodinus scandens FORST

For the alkaloids meloscine, epimeloscine and scandine, isolated from the Apocynacee Melodinus scandens FORST ., the structures 1, 10 and 11 , respectively, are deduced. Scandine is proved to possess the relative configuration as shown in 11 r. For meloscine and epimeloscine the relative configurations as depicted in 1 r and 10 r are discussed.     

Structure-acidity-IR spectra correlations for p-substituted N-phenylsulfonylbenzamides

The wavenumbers of the IR absorption bands of the C=O, S=O and N-H stretching vibrations for a series of p-substituted N-phenylsulfonylbenzamides were measured in trichloromethane. The bond orders, Mulliken charges, charge densities and heats of formation were calculated using the PM3 method. Fifty significant mutual mono parameter (MP) and six dual parameter (DP) correlations were found for the IR spectral, theoretical structural data, substituent constants and previously reported dissociation constants in five polar organic solvents. The transmission of the substituent effects has been discussed and the solvent effect on the slopes of some linear correlations was evaluated using different solvent parameters. The results showed that the factors describing the electronic structure and controlling the dissociation equilibrium and the IR spectra properties of p-substituted N-phenylsulfonylbenzamides must be the same.     

Amphiphilic polymer gel electrolytes. I. preparation of gels based on poly(ethylene oxide) graft copolymers containing different ionophobic groups

Amphiphilic graft copolymers were prepared via the radical copolymerization of poly(ethylene oxide) (PEO) macromonomers with fluorocarbon or hydrocarbon acrylates in toluene with 2,2′‐azobisisobutyronitrile (AIBN) as an initiator. ¹H NMR spectroscopy confirmed that the composition of the graft copolymers corresponded well to the monomer feed. For gel electrolytes prepared from the amphiphilic copolymers, the nature of the ionophobic parts of the amphiphilic graft copolymers had a great influence on the ion conductivity. Gel electrolytes based on graft copolymers containing fluorocarbon side chains showed significantly higher ion conductivity than electrolytes based on graft copolymers containing hydrocarbon groups. The ambient‐temperature ion conductivity was about 2.6 mS/cm at 20 °C for a gel electrolyte based on an amphiphilic graft copolymer consisting of an acrylate backbone carrying PEO and fluorocarbon side chains. Corresponding gels based on graft copolymers with PEO side chains and hydrocarbon groups showed an ambient‐temperature ion conductivity of about 1.2 mS/cm. The gel electrolytes contained 30 wt % copolymer and 70 wt % 1 M LiPF₆ in an ethylene carbonate/γ‐butyrolactone (2/1 w/w) mixture. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 2223–2232, 2001