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  • 1
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Möglichkeit der quantitativen Bestimmung von Iod als Routinemessung mittels AES-ICP wird vorgestellt. Die empfindlichsten Iodemissionslinien werden bezüglich Nachweisgrenzen, Untergrundäquivalenzwerten sowie chemischen und spektralen Interferenzen unter Standardbedingungen getestet. Geeignete Methoden zur Herstellung stabilier Eichlösungen und zur Präparation von Probenlösungen aus iodhaltigen organischen und anorganischen Substanzen werden erläutert, sowie Ergebnisse von Testanalysen mitgeteilt.
    Notes: Summary The possibility of quantitative determination of iodine as a conventional measurement by AES-ICP is introduced. The most sensitive iodine emission lines are investigated, referring to detection limit, background equivalation concentration, as well as the chemical and spectral interferences for standard conditions. Appropriate methods for the preparation of stable calibration solutions, and the preparation of sample solutions of iodic organic and inorganic samples are discussed, as well as the results of the test analyses.
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  • 3
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 46 (1990), S. 1982-1984 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
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  • 4
    ISSN: 1573-4811
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 5
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The crystal structure of a Cu-richβ-phase in the system Cu-In-Se with the composition Cu14.0In16.7Se32 quenched from 750° C, has been determined with single crystals. The investigated single crystal of this Cu-richβ-phase has the composition Cu14In16.7Se32 and crystallizes witha = 1.1534(4) nm in the space groupP−43m. The cations are statistically distributed together with vacancies, but show strong preferences for distinct positions. The number of vacancies is estimated from the crystal structure analyses and is found to be much less than in the Cu-poorβ-phase. The crystal structure is compared with that of an ordered Cu-richβ-phase.
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  • 6
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract To investigate how the local symmetry of the Sm3+ ion affects the fluorescence of a samarium metaphosphate glass of composition (Sm2O3)0.248(P2O5)0.752, the temperature and pressure dependences of its laser induced fluorescence spectrum are compared with those of a samarium pentaphosphate crystal (SmP5O14). Findings include: (i) The crystal field splitting of the energy levels responsible for fluorescence in SmP5O14 at room temperature is consistent with the local symmetry of oxygen atoms of the phosphate cage around the Sm3+ ions being quite close to cubic – in accord with crystal structure. At 12 K there is a systematic disappearance of the shortest wavelength lines of each fluorescence band attributable to a decreasing population of higher crystal field levels, which are occupied at ambient temperature. (ii) The (Sm2O3)0.248(P2O5)0.7520.248 glass fluorescence spectrum forms five bands, which can be related to that of the crystal but with inhomogeneous line broadening; the short wavelength edges sharpen at low temperatures, also attributable to a decreasing population of higher crystal field levels at lower temperatures. (iii) The shifts (dλ/dp) in the wavelengths of the fluorescence peaks of the SmP5O14 crystal induced by pressure up to 50 kbar in a diamond anvil cell are small but measurable at room temperature, being about +0.03 nm kbar−1 (+0.3 Å kbar−1). Application of pressures up to 50 kbar to the (Sm2O3)0.248(P2O5)0.752 glass did not alter the positions of the bands within the error in the fluorescence wavelength measurements. Neither the SmP5O14 crystal nor the metaphosphate glass showed any indication of undergoing a phase transition up to the highest pressure reached. A low frequency Raman mode has been observed, which softens with reducing temperature, indicating softening of the associated optical mode and suggesting that, like other RP5O14 crystals, SmP5O14 undergoes a ferroelastic phase transition.
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  • 7
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Decompositions of inorganic and organic materials can be carried out within a few minutes by means of the microwave technique. For dissolving substances with volatile components in the microwave oven, low pressure containers were developed from microwave transparent materials and an excess pressure security system. Results and limitations of the method are explained by examples.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 440 (1978), S. 171-182 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structures of the Heptahetero-Nortricyclenes P7(Sime3)3 and P4(Sime2)3Tris(trimethylsilyl)heptaphospha-nortricyclene P7(Sime3)3 1 and Hexamethyl-trisila-tetraphospha-nortricyclene P4Si3me6 2 are structural analogons to the hetero-nortricyclenes P73- and P4S3. 1 crystallizes in the space group P21 with a = 965.7 pm, b = 1746.5 pm, c = 693.3 pm, β = 99.61° and Z = 2 formula units. In the P7 system tge P—P bond lengths differ functionally, namely 221.4 pm in the three-membered ring, 219.2 pm at the ring atoms and 217.9 pm at the bridgehead atom. The P—Si and Si—C bond lengths are 228.8 pm and 187.8 pm respectively. 2 crystallizes in the space group R3 with aR = 1129.3 pm, αR = 50.01° (hexagonal axes: a = 954.7 pm, c = 2956.9 pm) and Z = 2 formula units. In the P4Si3 systems the bond lengths are P—P = 220.2 pm, P—Si = 228.3 pm and 224.7 pm (to the bridgehead atom). The Si—C bond lengths are 187.3 pm. The structures are discussed with related compounds.
    Notes: Tris(trimethylsilyl)-heptaphospha-Nortricyclen P7(Sime3)3 und Hexamethyl-trisila-tetraphospha-Nortricyclen P4Si3me6 2 sind strukturelle Analoga zu den Hetero-Nortricyclenen P73- und P4S3. 1 kristallisiert in der Raumgruppe P21 mit a = 965,7 pm, b = 1746,5 pm, c = 693,3 pm, β = 99,61° und Z = 2 Formeleinheiten. Im zentralen P7-System sind die P—P—Abstände funktionell verschieden: 221,4 pm im Dreiring, 219,2 pm am Dreiring und 217,9 pm am Brückenkopfatom. Die P—Si-Abstände betragen 228,8 pm, die Si—C—Abstände 187,8 pm.  - 2 kristallisiert in der Raumgruppe R3 mit aR = 1129,9 pm, αR = 50,01° und Z = 2 Formeleinheiten (hexagonale Achsen: a = 954,7pm, c = 2956,9 pm). Im P4Si3—System sind die Bindungsabstände P—P =220,2 pm und P—Si = 228,3 bzw. 224,7 pm (zum Brückenkopfatom). Die Abstände Si—C betragen 187,3 pm. Die Strukturen werden im Zusammenhang mit anderen Verbindungen diskutiert.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Organosilicon Compounds. 83. Formation, Reactions, and Structure of Ylides Generated from Perchlorinated CarbosilanesThe CCl-moiety in perchlorinated carbosilanes as (Cl3Si)2 a, Cl3Si—CH2—SiCl2—CCl2—SiCl3 b, (Cl3Si—CCl2)2SiCl2 c or (Cl2Si—CCl2)3 d, e.g., cleaves the Si—P bond of me3Si—Pme2 e (me = CH3); and by subsequent rearrangement ylides are formed. Such, treating e with a yields (Cl3Si)2CPme2Cl 1, which also results from the reaction of me2P—Pme2 with a. The ylides also can be obtained by means of treating the carbosilanes a, b, c or d with LiPme2. Thus, c with one mole of LiPme2 yields Cl3Si—CCl2—SiCl2—C(Pme2Cl)—SiCl3 or Cl3Si—C(Pme2Cl)—SiCl2—C(Pme2Cl)—SiCl3, resp., with two moles of LiPme2. The corresponding Si-methylated derivates do not form ylides; (me3Si)2CCl2, e.g., with e in benzene yields me3Si—CH(Pme2)—Sime3. One mole of Lime methylates 1 to yield (Cl3Si)2CPme3 11. With either LiPme2, me3Si—Pme2 or Me2P—Pme2 1 forms (Cl3Si)2CPme2-Pme2. Reacting 1 with CH3OH/(C2H5)2NH, (Cl3Si)[SiCl2(OCH3)]CPme2(OCH3) is formed. Ylides also result from the reactions of partially C-chlorinated 1,1,3,3,5,5-hexachloro-1,3,5-trisilacyclohexanes with me3Si—Pme2, (Cl2Si—CCl2)3 with three moles of me3Si—Pme2 or LiPme2, resp., yields (Cl2Si—CPme2Cl)3 16, the 1,1,3,3,5,5-Hexachlor-2,4,6-tris(chlordimethylphosphoranyliden)-1,3,5-trisilacyclohexan, which crystallizes with one mole of monoglyme. X-ray structure determinations revealed that 1, 11 and 16 are planar. As well the (P—C) as the (Si—C) bond lengths are remarkably shortened; in 1 (P—C) to 173.3 pm, (Si—C) to 173.3 pm, (Si—C) to 179.5 pm, in 16 (P—C) to 168.7 pm, (Si—C) to 180 pm. The (Si—C) and (P—C) bond orders amount to about 1.33, and are relatively equally distributed. Therefore, the charge of the formal carbanion is equally distributed, which shall be expressed by means of the following kind of writing for 1 and 16 see “Inhaltsübersicht”.
    Notes: Die CCl-Gruppe in perchlorierten Carbosilanen wie (Cl3Si)2CCl2a, Cl3Si—CH2—SiCl2—CCl2—SiCl3 b, (Cl3Si—CCl2)2SiCl2 c, (Cl2Si—CCl2)3 d spaltet die Si-P-Bindung im me3Si—Pme2 e und durch anschließende Umlagerung entstehen Ylide. So bildet a mit e (Cl3Si)2-CPme2Cl 1 (me = CH3). 1 entsteht auch aus a mit me2P—Pme2. Die Bildung des Ylids bleibt bei entsprechenden Si-methylierten Derivaten aus; (me3Si)2CCl2 bildet mit e in Benzol me3Si—CH(Pme2) - Sime3. Entsprechende Ylide werden aus den Carbosilanen a, b, c, d auch durch Umsetzung mit LiPme2 erhalten. So reagiert c mit einem Mol LiPme2 zu Cl3Si—CCl2—SiCl2—C(Pme2Cl)—SiCl 3 und mit zwei Mol LiPme2 zu Cl3Si—C(Pme2Cl)—SiCl2—C(Pme2Cl)— SiCl3. 1 wird mit einem Mol Lime zu (Cl3Si)2CPme3 11 methyliert. 1 reagiert mit LiPme2, me3Si—Pme2 und me2P—Pme2 zum (Cl3Si)2-CPme2Pme2. Mit CH3OH/(C2H5)2NH bildet 1 (Cl3Si)[SiCl2(OCH3)]CPme2(OCH3). Die Ylidbildung erfolgt auch bei der Umsetzung von C-teilchlorierten 1,1,3,3,5,5-Hexachloro-1,3,5-trisilacyclohexanen mit me3Si—Pme2. (Cl2Si—CCl2)3 bildet mit drei Mol me3Si—Pme2 bzw. LiPme2 das(Cl2Si—CPme2Cl)3 16, das mit einem Mol Monoglym kristallisiert. 16 ist das 1,1,3,3,5,5-Hexachlor-2,4,6-tris(chlordimethylphosphoranyliden)-1,3,5- trisilacyclohexan. Nach der Röntgenstrukturuntersuchung sind die Verbindungen 1, 11, 16 eben. Sowohl die (P—C)- als auch die (Si—C)-Bindungen sind deutlich verkürzt; in 1 (P—C) auf 173,3 pm; (Si—C) auf 179,5 pm; in 16 (P—C) auf 168,7 pm, (Si—C) auf 180 pm. Die höheren Bindungsordnungen der (Si—C)- und (P—C)-Bindungen betragen∼1,33 und sind relativ gleichmäßig verteilt. Die Ladung des formalen Carbanions ist demnach gleichmäßig verteilt, was in der folgenden Schreibweise für 1 und 16 ausgedrückt wird.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 543 (1986), S. 161-168 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of LiInSe2The crystal structure of LiInSe2 has been determined from single crystal data (β-NaFeO2 type, space group Pna21 (No. 33), a = 718.3(2), b = 839,8(3), c = 678.1(2) pm; 375 hkl, R = 0.032; R(w) = 0.029). The mean values 253.6 pm of the bond distances Li—Se are larger than calculated, the distances In—Se (256.8 pm) are equal with the calculated values. The structure is discussed in relation to the analogous LiBIIIC2VI compounds.
    Notes: Die Kristallstruktur von LiInSe2 wurde aus Einkristalldaten bestimmt (β-NaFeO2-Typ, Raumgruppe Pna21 (Nr. 33), a = 718,3(2), b = 839,8(3), c = 678,1(2) pm; 375 hkl, R = 0,032; R(w) = 0,029). Die gemittelten Abstände Li—Se sind mit 253,6 pm gröΒer, die Abstände In—Se mit 256,8 pm ungefähr gleich den berechneten Werten. Die Struktur wird im Zusammenhang mit analogen LiBIIIC2VI-Verbindungen diskutiert.
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