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  • Analytical Chemistry and Spectroscopy  (4)
  • Inorganic Chemistry  (4)
  • 42.75
  • Atomic, Molecular and Optical Physics
  • General Chemistry
  • Surface physics, nanoscale physics, low-dimensional systems
  • 1990-1994  (8)
  • 1980-1984
  • 1915-1919
  • 1994  (8)
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Schlagwörter
Verlag/Herausgeber
Erscheinungszeitraum
  • 1990-1994  (8)
  • 1980-1984
  • 1915-1919
Jahr
  • 1
    Digitale Medien
    Digitale Medien
    Microcolumn liquid chromatography with thermionic detection of the enantiomers of O-ethyl S-2-diisopropylaminoethyl methylphosphonothioate (VX) (1994)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 95-97 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Chemical warfare agents ; Microcolumn liquid chromatography ; Enantiomeric separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: An improved interface for the on-line coupling of microcolumn liquid chromatography (micro-LC) with thermionic detection (TID) is described. Modifications have been made to enable separate adjustment of the eluent introduction and the detector flame temperature in order to improve the sensitivity and ease of use of the system.The micro-LC-TID was used for the chiral separation of the nerve agent O-ethyl S-2-diisopropylaminoethyl methylphosphonothioate (VX). Baseline separation for the enantiomers of VX was obtained on Chiralcel OD using 1% isopropanol in hexane as the eluent. The detection limit of VX using 60 nl injections is ca. 5 μg/ml (ppm range). However, when using large-volume injections (10 μl) the detection limit is ca. 25 ng/ml (ppb range).
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/jhrc.1240170210
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  • 2
    Digitale Medien
    Digitale Medien
    The determination of cyclophosphamide and its metabolites in blood plasma as stable trifluoroacetyl derivatives by electron capture chemical ionization gas chromatography/mass spectrometry (1994)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1994), S. 149-158 
    Details
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method is described for the determination of the antitumour drug cyclophosphamide and six stable metabolites in plasma of cancer patients, namely dechloroethyl-cyclophosphamide, 4-keto-cyclophosphamide, carboxy-phosphamide, alcophosphamide, nor-nitrogen mustard and the N-chloroethyl-1,3-oxazolidine-2-one, as methyl and/or trifluoroacetyl derivatives by single ion monitoring gas chromatography/mass spectrometry, mostly in the electron capture chemical ionization mode. The isolation of most metabolites was performed by solid-phase C-18 extraction in weakly acidic medium. The phosphoramide mustard isolated under these conditions decomposes readily to the nor-nitrogen mustard during derivatization. The original nor-nitrogen mustard and the chloroethyl-1,3-oxazolidine-2-one were isolated by liquid extraction with ethyl acetate in alkaline medium. Recoveries of 75-99% were measured using spiked blank plasma samples. Quantitation of metabolites in patient plasma samples was performed using two sets of calibration curves for the concentration ranges of 1-100 ng and 0.1-10 μg of metabolite per millilitre of original plasma.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/bms.1200230306
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  • 3
    Digitale Medien
    Digitale Medien
    Packed capillary supercritical fluid chromatography of organophorus pesticides: Selective detection and applications (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 55-62 
    Details
    ISSN: 1040-7685
    Schlagwort(e): supercritical fluid chromatography ; packed capillary columns ; thermionic detection ; organophosphorus pesticides ; vegetable extracts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Packed capillary supercritical fluid chromatography coupled with thermionic detection was used for the selective determination of nineteen organophosphorus pesticides in vegetable extracts. The chromatographic behavior of some pesticides was studied using seven different stationary phases. Addition of an organic modifier to carbon dioxide was needed to improve peak shape and reduce retention. Quantitation of organophosphorus pesticides in vegetable extracts showed good linearity. Extraction was performed in a one-step extraction procedure using a water-miscible solvent (acetone) and an organic solvent with limited water capacity (dichloromethane). Under these conditions a wide range of both polar and apolar pesticides can be recovered from vegetable extracts down to the 3-25 μg kg-1 level. The recoveries found ranged from 35 to 95% depending on the polarity of the pesticides.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/mcs.1220060111
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  • 4
    Digitale Medien
    Digitale Medien
    Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography II. Use of a solvent vapor exit to increase introduction volumes and introduction rates into the gas chromatograph (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 207-215 
    Details
    ISSN: 1040-7685
    Schlagwort(e): capillary GC ; reversed-phase LC ; on-line coupling ; solvent vapor exit ; pressure-balanced carrier gas system ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A large-volume introduction system for capillary gas chromatography (GC) is described which can be coupled on-line with reversed-phase liquid chromatography (LC) using 2 mm i.d. LC columns. An on-column interface with a special retention gap, coated with a very thin film (0.02 μm) of Carbowax was used. Insertion of a solvent vapor exit before the analytical gas chromatography column allowed the solvent evaporation rate for an azeotropic acetonitrile/water mixture (84:16, v/v) to increase from 20 to 175 μL min-1 at 91°C and 150 kPa inlet pressure. A volume of 200 μL of this mixture containing phenanthrene and the potential basic drug eltoprazine, could be injected into the retention gap at introduction rates up to 200 μL min-1, under partially concurrent solvent evaporation conditions. Repeatability (CV = 2.4%) and linearity (at least 10-1000 ng mL-1) were satisfactory. The Carbowax-coated retention gap has a relatively large retention power for the polar solute. This means that the solvent can be completely evaporated through the vapor exit without loss of analyte. With apolar solutes, losses will occur if evaporation is unduly prolonged. In order to allow the use of a nitrogen-phosphorus detector, a special pressure-balanced carrier gas circuit was designed and tested for total solvent-free performance of the detector. With this set-up, 150 μL injections of eltoprazine in the acetonitrile/water azeotrope were made at an introduction rate of 200 μL min-1. No traces of acetonitrile were detected, while analyte detectability was 20-fold higher than with the FID.Finally, the practicability of reversed-phase LC-GC was demonstrated by on-line heart-cutting of the phenanthrene-containing fraction from a 2 mm i.d. LC column using acetonitrile/water (84:16, v/v) as eluent, and analyzing it by capillary GC-FID.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/mcs.1220060303
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  • 5
    Digitale Medien
    Digitale Medien
    Ein Beitrag über Ba3Pt4HgO11: Das erste Erdkalimetall-Oxoplatinat(II,V)/Oxomercurat (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1471-1475 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Barium, mercury, platinum, oxide ; crystal structure ; high pressure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: A Contribution on Ba3Pt4HgO11: The First Alkaline-Earth Oxoplatinate(II,V)/OxomercurateSingle crystals of Ba3Pt4HgO11 were prepared by oxygen high pressure technique (4 200-3 600 bar) and investigated by X-ray methods. It crystallizes with hexagonal symmetry, space group D3h4—P62c, a = 6.021, c = 17.374 Å, Z = 2. Ba3Pt4HgO11 represents a new structure type, showing structural relationships to Ba2Hg3Pd7O14 and to the precious metal 6L-perovskites. The Hg2+ ions show dumb-bell like coordination, Pt2+ a square-planar surrounding and Pt5+ face shared double octahedra.
    Notizen: Ba3Pt4HgO11 wurde unter hohem Sauerstoffdruck (4 200-3 600 bar) einkristallin dargestllt und röntgenographisch untersucht. Die Verbindung kristallisiert hexagonal, Raumgruppe D3h4—P62c mit a = 6,021; c = 17,374 Å; Z = 2. Ba3Pt4HgO11 bildet einen neuen Strukturtyp, der kristallchemische Verwandtschaft zu Ba2Hg3Pd7O14 und den Edelmetall-6L-Perowskiten zeigt. Die Hg2+-Ionen weisen eine hantelförmige, Pt2+ eine quadratisch-planare Koordination auf. Pt5+ bildet mit O2- flächenverknüpfte Doppeloktaeder.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946200825
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  • 6
    Digitale Medien
    Digitale Medien
    CdHgO2: Ein Oxomercurat mit Verwandtschaft zur Crednerit-StrukturProfessor Wilhelm Preetz zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1137-1141 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Cadmium ; mercury ; oxide ; high pressure ; crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: CdHgO2: An Oxomercurate related to the Crednerite StructureSingle crystals of CdHgO2 were prepared by oxygen high pressure technique (600°C, 3900 bar) and investigated by X-ray technique. It crystallizes with monoclinic symmetry, space group C2h3-C2/m; a = 5.933, b = 3.452, c = 5.875 Å, β = 91.26°; Z = 2. The Hg2+ ions show dumb-bell like coordination, Cd2+ an octahedral one. CdHgO2 shows strong relationship to the Crednerite structure. The orientation of the O—Hg—O dump-bells to the CdO6 octahedra layers is discussed with respect to related oxomercurates.
    Notizen: CdHgO2 wurde mit Sauerstoff-Hochdrucktechnik (600°C, 3900 bar) einkristallin dargestellt und röntgenographisch untersucht. Es kristallisiert monoklin, Raumgruppe C2h3-C2/m mit a = 5,933, b = 3,452, c = 5,875 Å, β = 91,26° und Z = 2. Die Hg2+-Ionen zeigen eine hantelförmige, Cd2+ eine oktaedrische Koordination. CdHgO2 zeigt große Ähnlichkeit zur Crednerit-Struktur. Die Anordnung der O—Hg—O-Hanteln zu den CdO6-Oktaederschichten wird unter Bezug auf verwandte Oxomercurate diskutiert.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946200702
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  • 7
    Digitale Medien
    Digitale Medien
    Bis(cyclopentadienyl)methan-verbrückte Zweikernkomplexe. VIII. Zweikernige Cobaltkomplexe mit dem Dianion des Bis(cyclopentadienyl)methans und des Bis(tetramethylcyclopentadienyl)dimethylsilans als BrückenligandenProfessor Gerhard Fritz zum 75. Geburtstag gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 2053-2063 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Dinuclear cobalt complexes ; oxidative addition and substitution reactions ; formation of dinuclear and chiral complex salts ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Bis(cyclopentadienyl)methane-bridged Dinuclear Complexes. VIII. Dinuclear Cobalt Complexes with the Dianion of Bis(cyclopentadienyl)methane and Bis(tetramethylcyclopentadienyl)dimethylsilane as Bridging LigandsThe dinuclear cobalt complex [CH2(C5H4)2][Co(CO)2]2 (4) which is obtained from [Co(CO)4I] (2) and Li2[CH2(C5H4)2] (3) in 75% yield reacts with PMe3, PiPr3, P2Me4, Me2PCH2CH2PMe2 and (EtO)2POP(OEt)2, to the compounds 5-9 substituting one CO ligand per cobalt atom. Oxidative addition of CH3I to [CH2(C5H4)2][Co(CO)(PMe3)]2 (5) leads to the formation of the dinuclear cobalt(III) complex [CH2(C5H4)2][Co(COCH3)(PMe3)I]2 (11). The reaction of 4 with iodide generates [CH2(C5H4)2][Co(CO)I2]2 (12) which with PMe3, P(OMe)3, P(OiPr)3, and CNMe reacts under CO substitution to [CH2(C5H4)2][Co(L)I2]2 (13-16) and with PMe2H to {[CH2(C5H4)2][Co(PMe2H)3]2}I4 (17). The electrophilic addition reactions of NH4PF6 and CH3I to [CH2(C5H4)2][Co(PMe3)2]2 (20) produce the complex salts {[CH2(C5H4)2][CoR(PMe3)2]2}X2 (21: R = H; 22: R = CH3). From 22a (X = I) and LiCH3 the dinuclear tetramethyldicobalt compound [CH2(C5H4)2] · [Co(CH3)2(PMe3)]2 (23) is obtained which further reacts, via the intermediate 24, to the chiral complex {[CH2(C5H4)2] · [CoCH3(PMe3)P(OMe)3]2}(PF6)2 (25). The reaction of 20 with C2(CN)4 and E- or Z-C2H2(CO2Me)2 gives the olefin(trimethylphosphine) cobalt(I) derivatives 26 und 27. The synthesis of the dinuclear compounds 31-38 with [Me2Si(C5Me4)2]2- as the bridging unit is also described.
    Notizen: Der Cobalt-Zweikernkomplex [CH2(C5H4)2] · [Co(CO)2]2 (4), der aus [Co(CO)4I] (2) und Li2[CH2(C5H4)2] (3) mit 75%iger Ausbeute entsteht, reagiert mit PMe3, PiPr3, P2Me4, Me2PCH2CH2PMe2 und (EtO)2POP(OEt)2 unter Substitution je eines CO-Liganden pro Cobaltatom zu den Verbindungen 5-9. Aus [CH2(C5H4)2][Co(CO)(PMe3)]2 (5) und CH3I erhält man durch oxidative Addition den zweikernigen Cobalt(III)-Komplex [CH2(C5H4)2][Co(COCH3)(PMe3)I]2 (11). Die Umsetzung von 4 mit Iod liefert die Verbindung [CH2(C5H4)2][Co(CO)I2]2 (12), die mit PMe3, P(OMe)3, P(OiPr)3 und CNMe unter CO-Verdrängung zu [CH2(C5H4)2] · [Co(L)I2]2 (13-16) und mit PMe2H zu {[CH2(C5H4)2] · [Co(PMe2H)3]2}I4 (17) reagiert. Die Umsetzungen von [CH2(C5H4)2][Co(PMe3)2]2 (20) mit NH4PF6 und CH3I führen unter elektrophiler Addition zu den Komplexsalzen {[CH2(C5H4)2][CoR(PMe3)2]2}X2 (21: R = H; 22: R = CH3). Aus 22a (X = I) und LiCH3 ist die zweikernige Tetramethyldicobalt-Verbindung [CH2(C5H4)2][Co(CH3)2(PMe3)]2 (23) und daraus über die Zwischenstufe 24 der chirale Komplex {[CH2(C5H4)2][CoCH3(PMe3)P(OMe)3]2}(PF6)2 (25) zugänglich. Aus 20 und C2(CN)4 und E- oder Z-C2H2(CO2Me)2 erhält man die Olefin(trimethylphosphan)cobalt(I)-Derivate 26 und 27. Die Synthese der Zweikernkomplexe 31-38 mit [Me2Si(C5Me4)2]2- als verbrückender Einheit wird ebenfalls beschrieben.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946201207
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  • 8
    Digitale Medien
    Digitale Medien
    Einkristallzüchtung und Röntgenstrukturanalyse von CoSO4 · Pyrazin · 6 H2O (I) und (CoSO4)2 · Pyrazin · 12 H2O (II) (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1750-1754 
    Details
    ISSN: 0044-2313
    Schlagwort(e): Cobalt Complexes ; Pyrazine ; Gel Crystallization ; Structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Crystal Growth and Structure of CoSO4 · Pyrazine · 6 H2O (I) and (CoSO4)2 · Pyrazine · 12 H2O (II)Single crystals of μ-pyrazino-bis[pentaquacobalt(II)]-sulfate-dihydrate CoSO4(pz) · 6 H2O and Tetraqua-μ-pyrazino-cobalt(II)sulfate-dihydrate (CoSO4)2(pz) · 12 H2O were grown by using gel methods and investigated by X-ray analysis. CoSO4(pz) · 6 H2O (I) shows monoclinic symmetry, space group C2/c; a = 1006.4(4) pm, b = 1026.9(4) pm, c = 1261.5(2) pm; β = 104.01(4)°; Z = 4. (CoSO4)2(pz) · 12 H2O (II) shows orthorhombic symmetry, space group Pbam; a = 1262.3(4) pm, b = 1231.3(4) pm, c = 684.1(2) pm; Z = 2. CoSO4 and Pyrazine crystallize in a polymeric (I) as well as in a dimeric (II) compound. In the polymeric compound the molecules are bonded by pyrazine to form alternating linear chains. The dimer is a dinuclear complex with a bridging pyrazine molecule.
    Notizen: μ-Pyrazino-bis[pentaquacobalt(II)]sulfatdihydrat (CoSO4 · Pyrazin · 6 H2O) und Tetraqua-μ-pyrazino-cobalt(II)sulfat-dihydrat ((CoSO4)2 · Pyrazin · 12 H2O) wurden mittels der Gelmethode synthetisiert und röntgenographisch untersucht. CoSO4 · Pz · 6 H2O (I) kristallisiert monoklin, Raumgruppe C2/c, a = 1006,4(4) pm, b = 1026,9(4) pm, c = 1261,5(2) pm; β = 104,01(4)°; Z = 4. (CoSO4)2 · Pz · 12 H2O (II) kristallisiert orthorhombisch, Raumgruppe Pbam, a = 1262,3(4) pm, b = 1231,3(4) pm, c = 684,1(2) pm; Z = 2. Zwischen CoSO4 und Pyrazin läßt sich neben einer polymeren (I) auch eine dimere Verbindung (II) kristallisieren. Der polymeren Verbindung liegen lineare, in ihrer Richtung alternierende Ketten zugrunde. Das Dimere liegt als pyrazinverbrückter Zweikernkomplex vor.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1002/zaac.19946201015
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