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Eingeladener Vortrag
- nein (138)
Separation of hydrophobic pulmonary surfactant proteins using preparative HPLC with UV detection
(2000)
Characterization of silicon polymers by coupling of liquid chromatographic methods with MALDI-TOF-MS
(2000)
Liquid adsorption chromatography at critical conditions (LACCC) in normal and in reversed-phase modes provides independent information on the molar mass distributions of both blocks of poly(methyl methacrylate)-block-poly(tert-butyl methacrylate), even if no information about the precursor is available. In addition, the amount of unreacted precursor can be determined, even if its molar mass is comparable to that of the total block copolymer. The reversal of elution order by changing of stationary and mobile phases makes it possible to independently characterize each block in the SEC mode of the LACCC system. Thus, complete structural information is obtained even without using two-dimensional chromatographic techniques.
We prepared 2,2-dibutyl-2-stanna-1,3-dithiacycloalkanes from dibutyltin oxide and ,-dimercaptoalkanes. Heterocycles with five-, six-, seven-, or nine-ring members were used as bifunctional monomers for polycondensations with aliphatic dicarboxylic acid chlorides. These polycondensations conducted in bulk were highly exothermic and yielded poly(thio ester)s with number average molecular weights (Mn's) in the range of 5000-30,000 Da. These poly(thio ester)s proved to be rapidly crystallizing materials with melting temperatures in the range of 90-150 °C. In addition to the success of the new synthetic approach, two interesting and unpredictable results were obtained. All volatile species detectable by matrix assisted laser desorption induced-time of flight (MALDI-TOF) mass spectrometry were cyclic oligo- and poly(thio ester)s. Second, several polyesters showed a reversible first-order change of the crystal modification as identified by differential scanning calorimetry measurements and X-ray scattering with variation of the temperature. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 3656-3664, 2000
2,2-Dibutyl-2-stanna-1,3-dioxepane (DSDOP) was polycondensed with bis(4-chlorothiophenyl) suberat under various reaction conditions, but only moderate molecular weights (Mn 10000) were obtained. The MALDI-TOF mass spectrosmetry revealed the formation of cyclic oligo- and polyesters in addition to linear species having OH, CO2H, and unreacted 4-chlorothiophenyl ester endgroups.
Furthermore, -Caprolactone (-CL) was polymerized with DSDOP as the initiator at monomer/initiator (M/I) ratios of 20 and 50. The resulting tin-containing macrocyclic polylactones were reacted with sebacic acid bis(4-thiocresyl)ester at three different temperatures and with different reaction times. Analogous polycondensations were conducted with suberic acid bis(4-chlorothiophenyl) ester. The presence of thioarylester endgroups in the isolated polyesters was checked by 1H NMR spectroscopy. The highest conversions were found at long reaction times (24 or 72 hours), or after the addition of pyridine and N,N-dimethylaminopyridine as catalysts. Despite high conversions, the number average molecular weights (Mn's) did not exceed values around 20000. Even in the samples having the highest molecular weights, unreacted 4-chlorothiophenylester endgroups were detected by GPC measurements evaluated with a UV-detector. It is concluded that both factors, cyclization and incomplete conversion, contribute to the limitation of the chain growth.
Chemical heterogeneities and molecular weight distributions of poly(ethylene oxide) (PEO)-co-polymethylene (PM) model oligomers, which are relevant to the synthesis of commonly used tensides, were investigated. For analytical characterization, the well-known principle of liquid adsorption chromatography at 'critical conditions' (LACCC) was modified. Near the critical conditions of adsorption of the PEO unit, e.g., at slight adsorption conditions of PM, the copolymers could be separated according to their PM chain length. The eluates were separated and single fractions of each peak were continuously transferred onto the MALDI target by means of a commercially available device. Simultaneously, the MALDI matrix solution was continuously added with a second pump. This procedure offers the possibility of the formation of homogeneous matrix-polymer textures. By MALDI-MS a complete characterization of the chemical composition (PEO and PM chain length) of each peak could be achieved. The obtained MALDI mass spectra of the eluates at different retention times could be used for the molecular weight calibration of the LAC system. In this way, an additional application of SEC, as in conventional 2D-chromatography, was avoided by using the MALDI method as quasi chromatographic separation
The curing conditions play an important role in the quality assurance of composite products.
Especially as composite materials are widely used in high tech areas so that they are required to fulfil high quality Standards. Some problems which occur during curing, for instance undercuring, can hardly be detected using Standard NDT investigations, mainly because they are manifested only at high temperatures, particularly close to glass-rubber-transition. On-line eure monitoring has the outstanding advantage that it can monitor the material parameters even at the highest temperatures possible.
In recent years eure monitoring with ultrasonic methods has become more populär. In comparison to dielectric methods mechanical parameters are measured directly. The quantities to be measured are the velocity and the attenuation of the sound wave. On this basis the storage and loss modulus can be calculated. Depending on the form of excitation with longitudinal or transversal waves these moduli are referred to as long wave or shear modulus.
Well developed Computer based technology and sensor materials are available in the non-destructive testing (NDT) market. The measuring equipment employed a commercial NDT System, which worked computer-aided. With a special Software the demands of automatic Operation under industrial conditions was accomplished. This measurement equipment was tested on composites. Its structure, performance and some practical results will be presented in the following paper.
Indolizines, known as a useful class of fluorophores, were bridged yielding biindolizines. We intended to obtain long wavelength absorbing and emitting fluorescent systems suitable for fluorescence labeling of biomolecules. The influence of the different kinds of coupling on the absorption and fluorescence behaviour of the resulting biidolizines was studied. The new fluorophore systems were characterized spectroscopically by their absorption and emission maxima and their quantum yields.
Several series of crown fluoro-chromo-ionophores covering a broad spectral range are investigated experimentally and compared to their theoretically studied dimethylamino (DMA) analogues. It is shown that the logarithm of the complex stability constants log KS for NaI and CaII ions do not correlate with the observed complexation-induced shift. Likewise, an unsatisfactory correlation is found between the local charge density on the amino nitrogen of the DMA dyes and log KS. However, using the charge of the whole dimethylamino group instead strongly improves this correlation. This can be understood by considering pyramidalization and hyperconjugation effects on the amino nitrogen. The observed correlation allows a novel approach to the design of fluoroionophores with optimized properties.
Syntheses and photophysical properties of a series of cation-sensitive polymethine and styryl dyes
(2000)
The syntheses and photophysical properties of 20 cation-sensitive fluoroionophores carrying the tetraoxa monoaza 15-crown-5 receptor are described and discussed. Whereas complexation induces only weak effects for the positively charged hemicyanine probes, the closely related styryl dyes show stronger changes in their photophysical properties upon cation binding in the analytically advantageous near-infrared (NIR) region. The strongest effects in both cation-induced spectral effects and complex stability constants are observed for the uncharged probes of styryl base-type, but these probes usually absorb and emit at shorter wavelengths in the UV/VIS region. For both styryl dyes and styryl bases, in some cases cation-induced fluorescence enhancement or quenching is found.
The photophysical properties of several newly synthesized 1-benzothiazole-3-(4-donor)-phenyl-substituted prop-2-en-1-ones (substituted chalcones) are studied as a function of solvent polarity, temperature, and metal ion by employing steady-state and time-resolved spectroscopy. To investigate the effect of bulkiness and donor strength of the anilino moiety on the spectroscopic properties of these dyes, the spectroscopic behavior of the 4-N-dimethylamino (DMA), the 4-N-tetraoxa-monoaza-15-crown-5 (A15C5), and the 4-N-tetrathia-monoaza-15-crown-5 (AT415C5) derivatives as well as the 3-julolidino (Jul) analogue is compared. Absorption and fluorescence measurements reveal that the strength of the intramolecular charge transfer (ICT) process increases on the order of AT415C5 < A15C5 ~ DMA < Jul. The slight but significant differences between the two crowned dyes are well-supported by the results of the X-ray structure analysis, where oxa aza and thia aza crowns show essentially different geometries. For both fluoroionophores, this variation of heteroatom substitution pattern of the receptor induces specific cation selectivities. The spectroscopic effects accompanying complexation and the different binding sites are studied by steady-state and time-resolved optical spectroscopy as well as NMR spectroscopy. Whereas the probe carrying a tetraoxa monoaza 15-crown-5 receptor shows cation-induced fluorescence enhancement in the presence of alkali and alkaline-earth metal ions, its tetrathia analogue binds selectively to HgII, AgI, and CuII in acetonitrile. Moreover, an increase in fluorescence is observed for the latter probe even upon coordination to the widely known fluorescence quencher HgII. Besides receptor complexation, chelate formation in the benzothiazole-carbonyl acceptor part of these intrinsic fluorescent probes is possible, leading to a chromoionophoric signaling behavior in the near-infrared (NIR).
Kémiai Adatbázisok
(2000)
The fundamental quantities in the depth sensing hardness test are force and displacement. The penetration depth used for the calculation of a certain hardness parameter (for instance HU, Eq. (1)) makes it necessary to determine the contact point. As shown in the paper, fitting of the forcedisplacement curve, F(h), by a second order polynomial and extrapolating to F=0 is not always the right way to achieve a sufficiently small uncertainty of depth. The feature of that procedure is analysed by a simple mathematical model. In dependence of the testing force, the scatter of the experimental data, and the required limit of depth uncertainty, a profound selection of the fitting range, the fitting function, and the extrapolation function should be done.
In der vorliegenden Arbeit wird die sicherheitstechnische Eigenschaft "Entzündlichkeit" von
Gasen und Gasgemischen vorgestellt. Die Definitionen und Prüfverfahren in den
unterschiedlichen technischen Rechtsbereichen werden erläutert. Zur Klassifizierung von
Gasgemischen in kleineren Mengen ist sowohl im europäischen Gefahrstoff-, als auch im
Gefahrgutrecht ein Rechenverfahren nach ISO 10156, Nr. 4.6, zulässig. Für die Anwendung
des Rechenverfahrens benötigt man Stoffkenngrößen (Tci, Kk), die im Anhang zur ISO 10156
für einige Stoffe aufgelistet sind. Im Rahmen einer Forschungskooperation wurden im
europäischen Kernforschungszentrum (CERN) in Genf, an der Uni-GH Paderborn und in der
BAM Explosionsbereiche von Dreistoffsystemen (Brenngas, Inertgas, Luft) nach DIN 51649
bestimmt, aus denen sich Tci- sowie KK-Werte berechnen lassen. Die so mit einheitlichen
Apparaturen und Prüfverfahren ermittelten Werte weichen z.T. erheblich von den Angaben
der ISO 10156 ab. Im letzten Abschnitt dieser Arbeit werden Druck- und Temperatureinfluss
auf die Entzündlichkeit diskutiert.
Chemie
(2000)
Four ISO/IEC-test charts have been defined in ISO/IEC 15775 (1999) to specify image reproduction of
colour copiers. Corresponding test charts have been defined in DIN 33866-1 to 5 (in print) to specify
image reproduction of colour copiers, printers, scanners and monitors. All colours of all test charts are
defined in CIELAB coordinates. In applications the devices including software are used for test chart
input and output in the three different combinations "analog - analog" (copiers), "digital - analog"
(printers, monitors) and "analog - digital" (scanners, Photo-CD-systems).
This paper uses mainly ISO/IEC-test colours of a 16 step grey scale (defined by olv*-coordinates
according to the standard) in the original scene to calibrate the variable (photographic and Photo-CD)
analog-digital process. The relative digital olv*-input data and the digital olv*'-output data are used to
get approximately the same digital output (image file) independent of exposure (e. g. between -1 stop
under to +2 stop over exposure for slide or negative film) and other variables, e. g. the digitizing Photo-
CD-process. This "direct" colour management method adds a new method compared to the ICC colour
management method which fails to handle variable processes and can not manage the variable data of
original scenes taken by the photographic process.
The committees ISO/IEC JTC1/SC28 and DIN-NI-28 "Information technology, Office equipment" have
worked together to develop the International Standard ISO/IEC 15775. The new national standards
DIN 33866-1 to 5 (in print, drafts May to Nov. 1999) and the International Standard ISO/IEC 15775
are based on equivalent colour series. Both use the same colour series both in digital and analog test
charts and approximately the same layout.
New colorimetric technologies of Germany and Japan have been used to produce the four DIN- and
ISO/IEC-test charts in offset printing (3600 dpi) which are in application for colour devices now.
The different productions will be shown, e. g. in halftone and continuous tone and in reflectance and
transmittance mode. Some problems of measurement (e. g. fluorencent photographic material) and the
accuracy of production is important for applications.
A flat area lamp which is shown at the conference has the chromaticity of D65. With transparent ISO/IEC-test chart material on top this equipment defines a reference monitor for comparison with display
output. For additional information see the URL: www.ps.bam.de