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  • 1
    Electronic Resource
    Electronic Resource
    Monitoring the behaviour of 4-ketocyclophosphamide versus cyclophosphamide during capillary gas chromatography by mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 643-647 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary Gas Chromatography (CGC) is capable of determining underivatized cyclophosphamide (CPA) using SCOT OV 275 columns. Then CPA is subjected to in situ degradation resulting in formation of a cyclization product which can be determined selectively in biological fluids. In routine bioanalysis however cyclization products of CPA metabolites might interfere, e.g. 4-keto CPA. In the present study possible formation of cyclization products of 4-keto CPA similar to CPA was monitored by Mass Spectrometry. Cyclization of 4-keto CPA in situ was demonstrated to occur, resulting in a product similar to that of CPA. Both cyclization products could be determined selectively and it appeared that in situ cyclization of 4-keto CPA was negligible (〈5%), probably owing to extra stabilization of the CPA metabolite by keto-enol tautomerism as has been demonstrated by NMR.
    Additional Material: 14 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200141113
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  • 2
    Electronic Resource
    Electronic Resource
    A study of some deactivation methods for fused silica capillary columns by CP-MAS NMR and capillary gas chromatography (1985)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 664-672 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; CP-MAS NMR ; Deactivation methods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of deactivating a fused silica surface by silylation with 1,1,3,3-tetraphenyl-1,3-dimethylilazane (TPDMDS), triphenylsilylamine (TPSA), and octamethylcyclotetrasiloxane (D4) and by polydimethylsiloxane degradation (PSD) is studied. Rehydrated, dried, and deactivated Cab-O-Sil M5 samples are used as model materials for 29Si CP-MAS NMR analysis.At about 350 °C, TPDMDS yelds mainly diphenylmethylsiloxysilane, dimethyldisiloxysilane, and triphenylsiloxysilane groups. TPSA yields phenyltrisiloxysilane, diphenyldisiloxysilane, and triphenylsiloxysilane groups. At 400°C, the products formed initially are eventually replaced by methyltrisiloxysilane or phenyltrisiloxysilane groups, while a substantial number of silanol groups still remains. The possible consequences for wettability are discussed.D4 reacts with Cab-O-Sil even at 200°C, but a large number of silanol groups remains. This number decreases gradually at higher temperatures and becomes negligible above 400°C. The formation of methyltrisiloxysilane groups, which starts at 425°C, is predominant at 490°C.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240081005
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  • 3
    Electronic Resource
    Electronic Resource
    The radical initiation of vinyl polymerization by α.α.α′.α′-Tetrasubstituted dibenzyls (1972)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 157 (1972), S. 279-298 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Im Temperaturbereich von 60 bis 100°C wird die radikalische Polymerisation von Styrol, Methylmethacrylat und Acrylnitril von α.α′-Dicyanodibenzylen ausgelöst, die in α-und α′-Stellung mit Ester-, Nitril-, Amid- oder Phenylgruppen disubstituiert sind. Bei 100 bis 110°C ist auch das α.α.α′.α′-Tetracarboxymethyldibenzyl aktiv. Vinylacetat und Vinylchlorid werden durch diese Initiatoren kaum polymerisiert.Fur die Polymerisation des Styrols wurden die Bruttogeschwindigkeitskonstanten Kp, für viele Dibenzyle und fur Peroxide vergleichbarer Aktivitat dilatornetrisch bestirnrnt. Norrnalerweise sind die Zeit-Urnsatz-Kurven rnit den Dibenzylen und den Peroxiden vergleichbar; das Tetracyanodibenzyl allerdings bewirkt nur eine unvollstandige Polymerisation.Der große Einfiuß von Substituenten in α-Stellung oder in den Phenylringen der Dibenzyle auf die Polymerisation des Styrols wird diskutiert. Dabei ist auch die Stereochernie wichtig. Die meso-Form des Dinitrildiesters ergibt eine 2.5- bis 3.5 ma1 schnellere Polyrnerisation als das dl-Isornere.Die Dissoziationsgeschwindigkeitskonstanten kd der Initiatoren wurden NMR-spektroskopisch aus der Linienbreite bestirnmt. Die Dinitrildiester sind gute Initiatoren, wahrend die α.α′-Dicyanodibenzyle rnit weiteren Nitril- oder Phenylgruppen in α- und α′-Stellung wenig geeignet sind. SchlieBlich wurde die 1.2-Addition einiger der Dibenzyle an Styrol im Ternperaturbereich von 120 bis 150°C rnit der Methode der chernisch induzierten KernPolarisation (CIDNP) untersucht.
    Notes: The radical polymerization of styrene, methyl methacrylate and acrylonitrile is initiated by α.α′-dicyanodibenzyls α.α′-disubstituted with ester, nitrile, amide or phenyl groups in the temperature range 60 to 100°C and by α.α.α′.α′-tetracarboxymethyldibenzyl at 100 to 110°C. Vinylacetate and vinylchloride show a low reactivity.The overall polymerization rate constants Kp have been determined dilatometrically for styrene initiated by a large number of dibenzyls and comparable peroxides. The styrene polymerization curves are generally comparable with those of peroxides. A notable exception is tetracyanodibenzyl.The strong influence of α- and ring-substituents in the dibenzyls on the styrene polymerization rate is discussed. The stereochemistry is also important : the meso α.α′-dicyanodibenzyls α.α′-disubstituted with ester groups give a 2.5 to 3.5 fold faster polymerization than their dl isomers.The initiator efficiency is related to the kd values, determined from NMR line width measurements. The α.α′- dicyanodibenzyls α.α′-disubstituted with ester groups are good initiators, while those with phenyl groups and nitrile groups are inefficient.Relevant to initiation and termination, the 1.2-addition of some of the dimers to styrene at 120 to 150°C has been studied with chemically induced dynamic nuclear polarization (CIDNP).
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1972.021570128
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  • 4
    Electronic Resource
    Electronic Resource
    The use of colloidal metal particles in protein blotting (1987)
    Weinheim : Wiley-Blackwell
    Electrophoresis 8 (1987), S. 403-409 
    Details
    ISSN: 0173-0835
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Two procedures are described for staining the overall protein pattern on transfer membranes. Both methods involve the use of colloidal metal particles. AuroDye staining is based on the interaction of anionic colloidal gold particles with cationic proteins at low pH. The method is highly sensitive, but limited to nitrocellulose and polyvinylidene difluoride membranes. FerriDye comprises an incubation in a cationic iron (hydrous) oxide sol and subsequent intensification with potassium hexacyanoferrate in acidic medium. FerriDye is of intermediate sensitivity, but there are no limitations concerning membranes. It can be used on nitrocellulose-, nylon-and polyvinylidene difluoride-based membranes. An immunodetection procedure is described which uses colloidal gold-labelled secondary antibodies to visualize antigen-antibody interactions. This signal can be significantly enhanced by silver. The procedure explained uses a new light-insensitive and user-friendly silver enhancement system.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/elps.1150080907
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  • 5
    Electronic Resource
    Electronic Resource
    Isolation and Absolute Configuration of β,β-Carotene Diepoxide (1988)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 71 (1988), S. 31-32 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 5,6:5′,6′-diepoxy-5,6:5′,6;-tetrahydro-β,β-carotene, isolated from tubers of a white-fleshed variety of sweet potato (Ipomoea batatas LAM.) has been assigned the (5R,6S,5′R,6′S)-chirality on the basis of its HPLC, UV/VIS, and CD data.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19880710104
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  • 6
    Electronic Resource
    Electronic Resource
    Isolation and Characterisation of (5R, 6S,5′R,8′R)- and (5R,6S,5′R,8′S)-Luteochrome from Brazilian Sweet Potatoes (Ipomoea batatas LAM.) (1986)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 69 (1986), S. 1554-1558 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Luteochrome isolated from the tubers of a white-fleshed variety of sweet potato (Ipomoea batatas LAM.) has been shown by HPLC, 1H-NMR and CD spectra to consist of a mixture of (5R,6S,5′R,8′R)- and (5R,6S,5′R,8′S)- 5,6:5′,8′-diepoxy-5,6,5′,8′-tetrahydro-β,β-carotene (1 and 2, resp.). Therefore, its precursor is (5R,6S,5′R,6′S)-5,6:5′,6′-diepoxy-5,6,5′,6′-tetrahydro-β,β-carotene (4). This is the first identification of luteochrome as a naturally occurring carotenoid and, at the same time, gives the first clue to the as yet unknown chirality of the widespread β,β-carotene diepoxide. These facts demonstrate that the enzymic epoxidation of the β-end group occurs from the α-side, irrespective of the presence of OH groups on the ring.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19860690705
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  • 7
    Electronic Resource
    Electronic Resource
    Iminophosphorane-mediated synthesis of mesoionic 1,3,4-Oxadiazolo-[3,2-a]pyridinylium-2-aminides (1988)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 121 (1988), S. 1495-1500 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Iminophosphoran-vermittelte Syntheses von mesoionischen 1,3,4- Oxadiazolo[3,2a]pyridinylium-2-aminidenDas Iminophosphoran 2 reagiert mit Methylisocyanat zu dem mesoionischen 1,3,4-Oxadiazolo[3,2-a]pyridinylium-2-methylaminid 3, das durch CF3SO3CH3 zum 1,3,4-Oxadiazolo[3,2-a]-pyridinium-Kation 4 methyliert wird. Struktur 4 wurde durch Röntgenstrukturanalyse gesichert. Durch Einwirkung von Base lagert das mesoionische Aminid 3 zum isomeren mesoionischen 1,3,4-Triazolo[3,2-a]pyridinylium-2-olat 11 um. Verbindung 3 wird durch (Arylimino)triphenylphosphorane in die entsprechenden 1,3,4-Oxadiazolo[3,2-a]pyridinium-2-arylaminide 12 umgewandelt, die auch aus Iminophosphoran 2 und Hydroximoylchloriden zugänglich sind.
    Notes: Reaction of iminophosphorane 2 with methyl isocyanate yields the mesoionic 1,3,4-oxadiazolo[3,2-a]pyridinylium-2-methylamindie 3, which undergoes N-methylation with CF3SO3CH3 to give the 1,3,4-oxadiazolo[3,2-a]pyridinium cation 4. The structure of compound 4 has been established by means of X-ray crystallography. Mesoionic aminide 3 undergoes rearrangement by the action of base to give the isomeric mesoionic compound 1,3,4-triazolo[3,2-a]pyridinylium-2-olate 11. Compound 3 by the action of (arylimino)triphenylphosphoranes is converted into the corresponding 1,3,4-oxadiazolo[3,2-a]pyridinylium-2-arylaminides 12, which can be also prepared from iminophosphorane 2 and hydroximoyl chlorides.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19881210825
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  • 8
    Electronic Resource
    Electronic Resource
    Influence of chemical structure on glass transition temperatures of poly(propylene terephthalate) and poly(propylene isophthalate) (1988)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 189 (1988), S. 691-699 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly(propylene terephthalate)Systematic IUPAC name: poly(oxypropyleneoxyterephthaloyl). (PPTP) and poly(propylene isophthalate)Systematic IUPAC name: poly(oxypropyleneoxyisophthaloyl). (PPIP) were prepared by melt polycondensation. Different fractions with number-average molar masses in the range 5 000 - 20 000 g·mol-1 were obtained and their respective glass transition temperatures (Tg) determined by calorimetry. The solubility parameters of the polymers were obtained by viscosity measurements in different solvents and were found to be 9,4 and 9,5 cal1/2·cm-3/2 (19,2·103 and 19,4·103 J1/2·m-3/2) for PPIP and PPTP, respectively. The glass transition temperatures were compared with those reported for analogous polyesters and it was shown that intramolecular interactions highly influence the Tg of these polyesters, whereas the effect of intermolecular interactions seems to be less important.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1988.021890321
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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis and viscosity behavior of poly(γ-p-biphenylmethyl-L-glutamate) in benzene/dichloroacetic acid mixtures, a comparison with poly(γ-benzyl-L-glutamate) (1974)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 175 (1974), S. 3193-3206 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Darstellung von Poly(γ-p-biphenylmethyl-L-Glutamat), PBPLG, (Poly{L-imino-1-[2-(4-biphenylmethoxycarbonyl)äthyl]-2-oxoäthylen}), (1d) wird beschrieben. Das Viskositätsverhalten dieses Polymers in Mischungen aus Benzol und Dichloressigsäure (c=0,2.10 - 3 - 1,4.10 - 3g/cm3) bei 25°CC wird untersucht. Die Ergebnisse werden verglichen mit Messungen unter den gleichen Bedingungen an Poly(γ-benzyl-L-Glutamat),PBLG, (Poly[ L-imino-l-(2-benzyloxycarbonylathyl)-2-oxoathylen]), (lc). In beiden Fallenfindet ein zweistufiger Ubergang von einer starren, von Wasserstoffbrucken stabilisiertenHelix in ein statistisches, solvatisiertes Knduel statt : PBPLG (erste Stufe CrSSX,, zweite Stufe 55-100%, Dichloressigsaure und PBLG (erste Stufe 0-70%, zweite Stufe 70-100%,Dichloressigsaure)).Die Einfiihrung eines p-Phenylsubstituenten in PBLG fuhrt deshalb in Mischungen aus Benzol- und Dichloressigsaure zu einer weniger stabilisierten Helix.Die Stabilitat und das Viskositatsverhalten von PBLG in Mischungen aus Benzol und Dichloressigsaure (c=0,2.10-3 -14.10-3g/cm3) sind denjenigen von PBLG in Mi-schungen aus m-Kresol und Dichloressigslure ( c = 1,0.10-3-4,0. 10-3g/cm3) ähnlich.
    Notes: The synthesis of poly(γ-p-biphenylmethyl-L-glutamate), PBPLG, (poly{L-imino-1-[2-(4-biphenylylmethoxycarbonyl)ethyl]-2-oxoethylene}), (1d) is described. The viscosity behavior of this polymer in benzene/dichloroacetic acid mixtures (c=0,2.10 - 3 - 1,4.10 - 3 g/cm3) at 25°CC is investigated. The results are compared with measurements on poly(γ-benzyl-L-glutamate), PBLG, (poly[L-imino-1-(2-benzyloxycarbonylethyl)-2-oxoethylene]), (1c) under the same conditions. A transition from a rigid hydrogen bonded helix to a random solvated coil occurs in two stages for both: PBPLG (first stage 0 - 55%, second stage 55 - 100% dichloroacetic acid) and PBLG (first stage 0 - 70%, second stage 70 - 100% dichloroacetic acid).Therefore, the introduction of a p-phenyl substituent in PBLG leads to a less stable helix in benzene/dichloroacetic acid mixtures.The stability and viscosity behavior of PBLG in benzene/dichloroacetic acid mixtures (c=0,2.10 - 3 - 1,4.10 - 3g/cm3) is quite similar to the behavior of PBLG in m-cresol/dichloroacetic acid mixtures (c=1,0.10 - 3 - 4,0.10 - 3 g/cm3).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1974.021751113
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  • 10
    Electronic Resource
    Electronic Resource
    Short fiber-reinforced thermoplastic elastomers from blends of natural rubber and polyethylene (1986)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 32 (1986), S. 5123-5146 
    Details
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Thermoplastic elastomer blends of natural rubber (NR) with high density polyethylene (HDPE) and with low density polyethylene (LDPE) were reinforced with short silk fiber. Processing characteristics such as torque and temperature developed during mixing and the effect of processing parameters such as nip gap and number of passes in the mill necessary to secure maximum orientation of the fibers in the blends were studied. A small nip gap and a single pass in the mill were found to give best results. Of the different mixing sequences studied, the sequence where short fibers followed by rubber were added to the molten thermoplastic was found to give a uniform dispersion of fibers. Fiber breakage and the change in aspect ratio of the fibers after mixing were also examined. It was observed that, as a direct consequence of the mixing sequence, each fiber was coated with a layer of thermoplastic. Although the properties improved on the addition of the dry bonding system of silica-resorcinol-hexamethylenetetramine, the comparatively long curing time required for full development of adhesion between the fibers and the matrix proved to be a major disadvantage associated with the incorporation of the bonding system. The tensile and tear properties were substantially enhanced, but the ultimate elongation decreased sharply with increasing loading of short fibers in the blends. The effect of fiber orientation and the development of anisotropy in the properties was also noted. Scanning electron microscopy (SEM) studies of the benzene-extracted surfaces of the NR/HDPE (high density polyethylene) blends substantiated the theory of fibers behaving like “mechanical anchors” between the rubber and thermoplastic phase. The effect of fiber loading on the tear and tensile properties of the blends of NR/LDPE with varying blend ratios was studied. Most pronounced improvement in the properties on the addition of short fibers was observed in the high rubber blends. As the plastic content in the blends increased, the short fibers were found to have a lesser influence on the properties. SEM photomicrographs of the tensile and tear fracture surfaces indicated the fiber orientations and the effect of orientation, fiber loading, and blend ratios on the nature of fracture.
    Additional Material: 31 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/app.1986.070320530
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