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  • Chemistry  (407,083)
  • 04. Solid Earth::04.04. Geology::04.04.09. Structural geology
  • Wiley-Blackwell  (407,088)
  • AGU
  • Geological Society of America
  • MDPI Publishing
  • Nature Publishing Group
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Publisher
Years
  • 1
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    Coseismic recrystallization during shallow earthquake slip (2015)
    Geological Society of America
    Details
    Publication Date: 2020-11-26
    Description: Solidified frictional melts, or pseudotachylytes, remain the only unambiguous indicator of seismic slip in the geological record. However, pseudotachylytes form at 〉5 km depth, and there are many rock types in which they do not form at all. We performed low- to high-velocity rock friction experiments designed to impose realistic coseismic slip pulses on calcite fault gouges, and report that localized dynamic recrystallization may be an easy-to-recognize microstructural indicator of seismic slip in shallow, otherwise brittle fault zones. Calcite gouges with starting grain size 〈250 μm were confined up to 26 MPa normal stress using a purpose-built sample holder. Slip velocities were between 0.01 and 3.4 m s−1, and total displacements between 1 and 4 m. At coseismic slip velocities ≥0.1 m s−1, the gouges were cut by reflective principal slip surfaces lined by polygonal grains 〈1 μm in size. The principal slip surfaces were flanked by 〈300 μm thick layers of dynamically recrystallized calcite (grain size 1–10 μm) containing well-defined shape- and crystallographic-preferred orientations. Dynamic recrystallization was accompanied by fault weakening and thermal decomposition of calcite to CO2 + CaO. The recrystallized calcite aggregates resemble those found along the principal slip surface of the Garam thrust, South Korea, exhumed from 〈5 km depth. We suggest that intense frictional heating along the experimental and natural principal slip surfaces resulted in localized dynamic recrystallization, a microstructure that may be diagnostic of seismic slip in the shallow crust.
    Description: Published
    Description: 63-66
    Description: 4T. Fisica dei terremoti e scenari cosismici
    Description: JCR Journal
    Description: reserved
    Keywords: Rock mechanics ; shallow earthquales ; 04. Solid Earth::04.01. Earth Interior::04.01.04. Mineral physics and properties of rocks ; 04. Solid Earth::04.04. Geology::04.04.06. Rheology, friction, and structure of fault zones ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 2
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    Mirror-like faults and power dissipation during earthquakes (2015)
    Geological Society of America
    Details
    Publication Date: 2021-05-17
    Description: Earthquakes occur along faults in response to plate tectonic movements, but paradoxically, are not widely recognized in the geological record, severely limiting our knowledge of earthquake physics and hampering accurate assessments of seismic hazard. Light-reflective (so-called mirror like) fault surfaces are widely observed geological features, especially in carbonate-bearing rocks of the shallow crust. Here we report on the occurrence of mirror-like fault surfaces cutting dolostone gouges in the Italian Alps. Using friction experiments, we demonstrate that the mirror-like surfaces develop only at seismic slip rates (∼1 m/s) and for applied normal stresses and sliding displacements consistent with those estimated on the natural faults. Under these experimental conditions, the frictional power density dissipated in the samples is comparable to that estimated for natural earthquakes (1–10 MW/m2). Our results indicate that mirror-like surfaces in dolostone gouges are a signature of seismic faulting, and can be used to estimate power dissipation during ancient earthquake ruptures.
    Description: Published
    Description: 1175-1178
    Description: 4T. Fisica dei terremoti e scenari cosismici
    Description: JCR Journal
    Description: reserved
    Keywords: Earthquakes ; Faults ; Carbonates ; Rock Mechanics ; 04. Solid Earth::04.01. Earth Interior::04.01.04. Mineral physics and properties of rocks ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.01. Earthquake faults: properties and evolution ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 3
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    Dynamic feeder dyke systems in basaltic volcanoes: the exceptional example o fthe 1809 Etna eruption (Italy) (2015)
    Nature Publishing Group
    Details
    Publication Date: 2017-04-04
    Description: In this paper, we describe the 1809 eruption of Mt. Etna, Italy, which represents one historical rare case in which it is possible to observe details of the internal structure of the feeder system. This is possible thanks to the presence of two large pit craters located in the middle of the eruptive fracture field that allow studying a section of the shallow feeder system. Along the walls of one of these craters, we analysed well-exposed cross sections of the uppermost 15–20 m of the feeder system and related volcanic products. Here, we describe the structure, morphology and lithology of this portion of the 1809 feeder system, including the host rock which conditioned the propagation of the dyke, and compare the results with other recent eruptions. Finally, we propose the dynamic model of the magma behaviour inside a laterally-propagating feeder dyke, demonstrating how this dynamic triggered important changes in the eruptive style (from effusive/Strombolian to phreatomagmatic) during the same eruption. Our results are also useful for hazard assessment related to the development of flank eruptions, potentially the most hazardous type of eruption from basaltic volcanoes in densely urbanized areas, such as Mt. Etna.
    Description: Published
    Description: 1-11
    Description: 2T. Tettonica attiva
    Description: 2V. Dinamiche di unrest e scenari pre-eruttivi
    Description: 3V. Dinamiche e scenari eruttivi
    Description: 4V. Vulcani e ambiente
    Description: 6A. Monitoraggio ambientale, sicurezza e territorio
    Description: N/A or not JCR
    Description: open
    Keywords: feeder dyke ; basaltic volcanoes ; flank eruptions ; Etna ; volcanic hazards ; sill ; volcanic rift ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics ; 04. Solid Earth::04.08. Volcanology::04.08.99. General or miscellaneous ; 04. Solid Earth::04.08. Volcanology::04.08.03. Magmas ; 04. Solid Earth::04.08. Volcanology::04.08.04. Thermodynamics ; 04. Solid Earth::04.08. Volcanology::04.08.05. Volcanic rocks ; 04. Solid Earth::04.08. Volcanology::04.08.08. Volcanic risk ; 05. General::05.02. Data dissemination::05.02.03. Volcanic eruptions
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 4
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    The seismogenic structure of the 2013–2014 Matese seismic sequence, Southern Italy: implication for the geometry of the Apennines active extensional belt (2015)
    Wiley-Blackwell
    Details
    Publication Date: 2017-04-04
    Description: Seismological, geological and geodetic data have been integrated to characterize the seismogenic structure of the late 2013-early 2014 moderate energy (maximum local magnitude MLmax = 4.9) seismic sequence that struck the interior of the Matese Massif, part of the Southern Apennines active extensional belt. The sequence, heralded by a ML = 2.7 foreshock, was characterized by two main shocks with ML = 4.9 and ML = 4.2, respectively, which occurred at a depth of ∼17–18 km. The sequence was confined in the 10–20 km depth range, significantly deeper than the 1997–1998 sequence which occurred few km away on the northeastern side of the massif above ∼15 km depth. The depth distribution of the 2013–14 sequence is almost continuous, albeit a deeper (16–19 km) and a shallower (11–15 km) group of events can be distinguished, the former including the main shocks and the foreshock. The epicentral distribution formed a ∼10 km long NNW–SSE trending alignment, which almost parallels the surface trace of late Pliocene–Quaternary southwest-dipping normal faults with a poor evidence of current geological and geodetic deformation. We built an upper crustal model profile for the eastern Matese massif through integration of geological data, oil exploration well logs and seismic tomographic images. Projection of hypocentres on the profile suggests that the seismogenic volume falls mostly within the crystalline crust and subordinately within the Mesozoic sedimentary cover of Apulia, the underthrust foreland of the Southern Apennines fold and thrust belt. Geological data and the regional macroseismic field of the sequence suggest that the southwest-dipping nodal plane of the main shocks represents the rupture surface that we refer to here as the Matese fault. The major lithological discontinuity between crystalline and sedimentary rocks of Apulia likely confined upward the rupture extent of the Matese fault. Repeated coseismic failure represented by the deeper group of events in the sequence, activated in a passive fashion the overlying ∼11–15 km deep section of the upper crustal normal faults. We consider the southwest-dipping Matese fault representative of a poorly known type of seismogenic structures in the Southern Apennines, where extensional seismogenesis and geodetic strain accumulation occur more frequently on NE-dipping, shallower-rooted faults. This is the case of the Boiano Basin fault located on the northern side of the massif, to which the 1997–1998 sequence is related. The close proximity of the two types of seismogenic faults at the Matese Massif is related to the complex crustal architecture generated by the Pliocene–early Pleistocene contractional and transpressional tectonics.
    Description: Published
    Description: 823-837
    Description: 2T. Tettonica attiva
    Description: JCR Journal
    Description: partially_open
    Keywords: Seismicity and tectonics ; Continental tectonics: extensional ; Crustal structure ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.06. Surveys, measurements, and monitoring
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 5
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    The stress field in Europe: optimal orientations with confidence limits (2013)
    Wiley-Blackwell
    Details
    Publication Date: 2017-04-04
    Description: This article has been accepted for publication in Geophysical Journal International ©: The Authors 2003. Published by Oxford University Press on behalf of The Royal Astronomical Society. All rights reserved.
    Description: In this study, we modify and extend a data analysis technique to determine the stress orientations between data clusters by adding an additional constraint governing the probability algorithm. We apply this technique to produce a map of the maximum horizontal compressive stress (S_Hmax) orientations in the greater European region (including Europe, Turkey and Mediterranean Africa). Using the World Stress Map dataset release 2008, we obtain analytical probability distributions of the directional differences as a function of the angular distance, θ. We then multiply the probability distributions that are based on pre-averaged data within θ〈3° of the interpolation point and determine the maximum likelihood estimate of the S_Hmax orientation. At a given distance, the probability of obtaining a particular discrepancy decreases exponentially with discrepancy. By exploiting this feature observed in the World Stress Map release 2008 dataset, we increase the robustness of our S_Hmax determinations. For a reliable determination of the most likely S_Hmax orientation, we require that 90% confidence limits be less than ±60° and a minimum of three clusters, which is achieved for 57% of the study area, with small uncertainties of less than ±10° for 7% of the area. When the data density exceeds 0.8×10^-3 data/km2, our method provides a means of reproducing significant local patterns in the stress field. Several mountain ranges in the Mediterranean display 90° changes in the S_Hmax orientation from their crests (which often experience normal faulting) and their foothills (which often experience thrust faulting). This pattern constrains the tectonic stresses to a magnitude similar to that of the topographic stresses.
    Description: This work was supported by the DPC-INGV 2008-2010 S1 project, the EU-FP7 project “Seismic Hazard Harmonization in Europe” (SHARE; Grant agreement no. 226967), and project MIUR-FIRB "Abruzzo" (code: RBAP10ZC8K_003).
    Description: Published
    Description: 3.1. Fisica dei terremoti
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: 4.2. TTC - Modelli per la stima della pericolosità sismica a scala nazionale
    Description: JCR Journal
    Description: partially_open
    Keywords: Neotectonics ; Seismicity and tectonics ; Fractures and faults ; Intra-plate processes ; Plate motions ; Dynamics: gravity and tectonics ; 04. Solid Earth::04.03. Geodesy::04.03.01. Crustal deformations ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.05. Stress ; 05. General::05.02. Data dissemination::05.02.99. General or miscellaneous
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  • 6
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    New kinematic constraints of the western Doruneh fault, north-eastern Iran, from interseismic deformation analysis (2013)
    Wiley-Blackwell
    Details
    Publication Date: 2017-04-04
    Description: We used the SBAS DInSAR analysis technique to estimate the interseismic deformation along the western part of the Doruneh fault system (DFS), northeastern Iran. We processed 90 ENVISAT images from four different frames from ascending and descending orbits. Three of the ground velocity maps show a significant interseismic signal. Using a simple dislocation approach we model 2-D velocity profiles concerning three InSAR data set relative to the western part of the DFS, obtaining a good fit to the observations. The resulting model indicates that a slip rate of ∼5mmyr−1 accumulates on the fault below 10 km depth, and that in its western sector the Doruneh fault is not purely strike-slip (left-lateral) as in its central part, but shows a significant thrust component. Based on published geological observations, and assuming that all interseismic deformation is recovered with a single event, we can estimate a characteristic recurrence interval between 630 and 1400 yr.
    Description: Published
    Description: 622-628
    Description: 1.10. TTC - Telerilevamento
    Description: 3.2. Tettonica attiva
    Description: JCR Journal
    Description: restricted
    Keywords: Image processing; Satellite geodesy; Seismic cycle; Radar interferometry; Seismicity and tectonics; Continental tectonics: strike-slip and transform. ; 04. Solid Earth::04.03. Geodesy::04.03.01. Crustal deformations ; 04. Solid Earth::04.03. Geodesy::04.03.06. Measurements and monitoring ; 04. Solid Earth::04.03. Geodesy::04.03.07. Satellite geodesy ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.03. Earthquake source and dynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.02. Geodynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 7
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    Modeling the interseismic deformation of a thrust system: seismogenic potential of the Southern Alps (2013)
    Wiley-Blackwell
    Details
    Publication Date: 2022-05-24
    Description: This article focuses on the Montello thrust system in the Eastern Southern Alps as a potential seismogenic source. This system is of particular interest because of its lack of historical seismicity. Nevertheless, the system is undergoing active deformation. We developed a finite-element model using visco-elasto-plastic rheology. The free parameters of the model (essentially, the locking status of the three thrusts included in the study), were constrained by matching the observed horizontal GPS and vertical levelling data. We show that the amount of interseismic fault locking, and thus the seismic potential, is not necessarily associated with the fastest-slipping faults. More specifically, the locked Bassano thrust has a greater seismic potential than the freely slipping Montello thrust. The findings suggest that faults with subtle evidence of Quaternary activity should be carefully considered when creating seismic hazard maps.
    Description: Published
    Description: 221-227
    Description: 3.2. Tettonica attiva
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: JCR Journal
    Description: open
    Keywords: interseismic deformation ; Montello thrust ; Southern Alps ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.06. Rheology, friction, and structure of fault zones ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 8
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    Active extension in Val d’Agri area, Southern Apennines, Italy: implications for the geometry of the seismogenic belt. (2012)
    Wiley-Blackwell
    Details
    Publication Date: 2020-02-24
    Description: Integration of geologic, geomorphologic and seismologic data sets is used to reconstruct the recent tectonic evolution and active deformation pattern in the Val d’Agri area, located in the seismically active axial sector of the Southern Apennines (Italy). The western portion of the Apennines thrust belt has been affected by Pliocene–Quaternary extension during easterly roll-back and crustal delamination of the Adriatic slab. The bulk of Quaternary extension has been accommodated bySW-dipping oblique and normal faults,which have attained mature morphologic and structural features and, nowadays, separate mountain ranges from intermontane basins. However, in the present seismogenic belt, coseismic faulting locally occurs on NE-dipping structures, which might cut the inherited Pleistocene landscape. In theVal d’Agri basin, in spite of the large Early–Middle Pleistocene, displacement occurred on SW-dipping faults bordering its eastern flank, our investigations show that the recent basin evolution has been controlled by a NE-dipping fault system (Monti della Maddalena fault system, MMFS). This fault system cuts across the Monti della Maddalena range, west of the Agri valley and has not yet created an evident tectonic landscape. Notwithstanding, fault motion since the Middle Pleistocene might explain geomorphologic and hydrographic anomalies of the Agri river and its valley, where fault-controlled subsidence has captured the river course and produced an aggrading plain within a regional uplift context. Recent and ongoing motion is documented by fault scarplets in loose deposits, 14C ages of palaeosols and the spatial relation with low to moderate instrumental seismicity. Results from fault kinematic analysis are compatible with fault-plane solutions of local and regional seismic events, and indicate ∼NE–SW oriented extension. Recognition of the MMFS as a potential seismogenic fault increases the longitudinal extent of the NE-dipping, morphologically immature seismic sources in the Southern Apennines and argues against the range-bounding fault model for active extension in the region. The regional size of the NE-dipping seismogenic belt may result from impingement of a mantle wedge beneath the Apenninic chain and possibly track the external front of crustal delamination.
    Description: Published
    Description: 591-609
    Description: 3.2. Tettonica attiva
    Description: JCR Journal
    Description: reserved
    Keywords: active tectonics ; crustal deformation ; earthquakes ; geomorphology ; normal faulting ; Southern Italy ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.03. Geomorphology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 9
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    Introduction: The ANDRILL McMurdo Ice Shelf (MIS) and Southern McMurdo Sound (SMS) Drilling Projects (2012)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: No Abstract
    Description: Published
    Description: 546-547
    Description: 2.3. TTC - Laboratori di chimica e fisica delle rocce
    Description: 3.5. Geologia e storia dei vulcani ed evoluzione dei magmi
    Description: 3.8. Geofisica per l'ambiente
    Description: JCR Journal
    Description: restricted
    Keywords: Stratigraphic Drilling ; McMurdo Ice Shelf ; Chronostratigraphy ; Neogene ; Tectonics ; Ice Sheet history ; 04. Solid Earth::04.04. Geology::04.04.99. General or miscellaneous ; 04. Solid Earth::04.04. Geology::04.04.08. Sediments: dating, processes, transport ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.04. Geology::04.04.10. Stratigraphy
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 10
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    Neogene deformation and granite emplacement in the metamorphic units of northern Apennines (Italy): Insights from mylonitic marbles in the Porto Azzurro pluton contact aureole (Elba Island) (2012)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: In the northern Tyrrhenian Sea, late Miocene intrusions (Monte Capanne pluton and Porto Azzurro pluton) were emplaced at upper crustal levels (〈0.2 GPa) in the thrust systems of Elba Island. The emplacement of intrusive rocks is currently explained in the context of late Miocene extensional tectonics. New detailed structural data collected along a continuous natural cross section through the contact aureole of the Porto Azzurro pluton (eastern Elba) where strain localization has occurred within two west-dipping decameter-scale carbonate shear zones, namely the Calanchiole and Felciaio shear zones, are reported here. These shear zones, characterized by a lithological difference with calcite and dolomite marbles dominant in the Calanchiole and Felciaio shear zones, respectively, exhibit a similar rheological behavior. They represent two weakened layers in which west-dipping mylonitic foliation, sheath folds, boudinage structures, and upright folds developed within the contact aureole. Moreover, in correspondence with the Felciaio shear zone, the inversion of metamorphic facies occurs. Meso- and microstructural data give evidence that most of the deformation and displacement in the shear zones was coeval with contact metamorphism and developed under metamorphic conditions retrograde from pyroxene hornfels to hornblende-hornfels facies. Geometric and kinematic features indicate that both shear zones correspond to ductile thrusts, which led to internal stacking of the contact aureole. Therefore, at Elba Island, emplacement of intrusive rocks coeval with late Miocene crustal shortening gives a new perspective on relations between tectonics and magmatism in the northern Apennines.
    Description: Published
    Description: 470-490
    Description: 1.10. TTC - Telerilevamento
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: JCR Journal
    Description: restricted
    Keywords: granite emplacement ; contact aureole ; deformation and metamorphism ; Neogene ; northern Apennines ; Elba Island ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.02. Geodynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 11
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    Insights from the Mw 6.3, 2009 L?Aquila earthquake (central Apennines) - Unveiling new seismogenic sources through their surface signatures: the adjacent San Pio Fault (2011)
    Wiley-Blackwell
    Details
    Publication Date: 2017-04-04
    Description: We analyzed a broad region around L’Aquila in search of seismogenic faults similar to that responsible for the 6 April 2009 earthquake (Mw 6.3). Having the lessons learned from this earthquake in mind, we focused on adjacent areas displaying similar morphotectonic, geological and structural evidence. The basin running from Barisciano to Civitaretenga-Navelli, notably located near the southeastern edge of the 2009 aftershock pattern, appears to be one of such areas. We collected morphotectonic and structural data indicating that this basin is underlain by a major active normal fault (San Pio Fault). All the observations are very much reminiscent of the morphotectonic, geological and structural setting of area struck by the L’Aquila earthquake, suggesting that the newly identified fault has the potential for a Mw 6.2-6.4 shock.
    Description: Published
    Description: Pages: 108–115
    Description: 3.2. Tettonica attiva
    Description: JCR Journal
    Description: partially_open
    Keywords: Seismotectonics ; Morphotectonics ; Active fault ; San Pio basin ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.03. Geomorphology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology
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  • 12
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    Monogenetic vent self-similar clustering in extending continental crust: Examples from the East African Rift System (2011)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: The spatial clustering of fracture networks and vents in basaltic volcanic fields has been analyzed in three sectors of the East African Rift System, the classical example of an active continental rift. Fracture trace maps and monogenetic basaltic vents have been thus collected in the Afar Depression, in the Main Ethiopian Rift, and in the Virunga Belt (Western Rift). The mapped vents are generally younger than 2 Ma, and most are of Holocene age. All the analyzed fracture networks have self-similar clustering with fractal exponents (Df) varying in the 1.54−1.85 range. Also, vents show a self-similar clustering with fractal exponents (Dv) in the 1.17−1.50 range. For all the studied sectors, the relationship Df 〉 Dv has been observed. The fractal exponents for vents (Dv) of power-law distributions are computed in a range of lengths with a lower and an upper cutoff. The upper cutoff (Uco) for the fractal clustering of vents in the studied sectors of the East African Rift System are compared with the respective crust thickness derived by independent geophysical data. The computed Ucos for the studied sectors well match the crust thickness in the volcanic fields. A preliminary conceptual model to explain the relationships between the upper cutoffs of the fractal distribution of vents and the thickness of the crust in the volcanic fields is thus proposed in the light of the percolation theory.
    Description: Published
    Description: 1.10. TTC - Telerilevamento
    Description: 3.2. Tettonica attiva
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: JCR Journal
    Description: reserved
    Keywords: crustal thickness ; basaltic volcanic fields ; vent distribution ; EASR ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.05. Stress ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 13
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    Introduction: LASI III—Magma pulses and sheets in tabular intrusions (2011)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: The origins of granites and intrusive rocks have been widely discussed for a couple of centuries, and the way volcanoes work and their magma forms have attracted scientists, naturalists, and laymen since the dawn of humankind. However, shallow igneous intrusions, representing the obvious link between the hidden kingdom of Pluto and the fiery realm of Vulcanus, have been partly overlooked, leading to some lack of communication between “plutonic” and “volcanic” researchers. An effort devoted to heal this breach has been contributed to by the establishment of the LASI conferences (named after laccolith and sill, the main types of shallow igneous intrusions).
    Description: Published
    Description: 161-162
    Description: 3.2. Tettonica attiva
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: JCR Journal
    Description: reserved
    Keywords: upper crustal level intrusions ; emplacement of magma ; 04. Solid Earth::04.01. Earth Interior::04.01.05. Rheology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.04. Geology::04.04.12. Fluid Geochemistry
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  • 14
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    Unknown
    Revised slip rates for the Alpine fault at Inchbonnie: Implications for plate boundary kinematics of South Island, New Zealand (2010)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: The northeast-striking, dextral-reverse Alpine fault transitions into the Marlborough Fault System near Inchbonnie in the central South Island, New Zealand. New slip-rate estimates for the Alpine fault are presented following a reassessment of the geomorphology and age of displaced late Holocene alluvial surfaces of the Taramakau River at Inchbonnie. Progressive avulsion and abandonment of the Taramakau floodplain, aided by fault movements during the late Holocene, have preserved a left-stepping fault scarp that grows in height to the northeast. Surveyed dextral (22.5 ± 2 m) and vertical (4.8 ± 0.5 m) displacements across a left stepover in the fault across an alluvial surface are combined with a precise maximum age from a remnant tree stump (≥1590–1730 yr) to yield dextral, vertical, and reverse-slip rates of 13.6 ± 1.8, 2.9 ± 0.4, and 3.4 ± 0.6 mm/yr, respectively. These values are larger (dextral) and smaller (dip slip) than previous estimates for this site, but they refl ect advances in the local chronology of surfaces and represent improved time-averaged results over 1.7 k.y. A geological kinematic circuit constructed for the central South Island demonstrates that (1) 69%–89% of the Australian-Pacific plate motion is accommodated by the major faults (Alpine-Hope-Kakapo) in this transitional area, (2) the 50% drop in slip rate on the Alpine fault between Hokitika and Inchbonnie is taken up by the Hope and Kakapo faults at the southwestern edge of the Marlborough Fault System, and (3) the new slip rates are more compatible with contemporary models of strain partitioning presented from geodesy.
    Description: Published
    Description: 139-152
    Description: 3.2. Tettonica attiva
    Description: 4.2. TTC - Modelli per la stima della pericolosità sismica a scala nazionale
    Description: N/A or not JCR
    Description: reserved
    Keywords: Alpine fault ; plate boundary ; slip rate ; New Zealand ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.02. Geochronology ; 04. Solid Earth::04.04. Geology::04.04.03. Geomorphology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.01. Earthquake faults: properties and evolution ; 04. Solid Earth::04.07. Tectonophysics::04.07.02. Geodynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.04. Plate boundaries, motion, and tectonics ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 15
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    Unknown
    Possible causes of arc development in the Apennines, central Italy (2010)
    Geological Society of America
    Details
    Publication Date: 2022-06-14
    Description: In central Italy, the geometry, kinematics, and tectonic evolution of the late Neogene Umbrian Arc, which is one of the main thrusts of the northern Apennines, have long been studied. Documented evidence for orogenic curvature includes vertical axis rotations along both limbs of the arc and a positive orocline test along the entire arc. The cause of the curvature is, however, still unexplained. In this work, we focus our attention on the southern portion of the Umbrian Arc, the so-called Olevano- Antrodoco thrust. We analyze, in particular, gravity and seismic-reflection data and consider available paleomagnetic, stratigraphic, structural, and topographic evidence from the central Apennines to infer spatial extent, attitude, and surface effects of a midcrustal anticlinorium imaged in the CROP-11 deep seismic profile. The anticlinorium has horizontal dimensions of ~50 by 30 km, and it is located right beneath the Olevano- Antrodoco thrust. Stratigraphic, structural, and topographic evidence suggests that the anticlinorium produced a surface uplift during its growth in early Pliocene times. We propose an evolutionary model in which, during late Neogene time, the Olevano- Antrodoco thrust developed in an out-of sequence fashion and underwent ~16° of clockwise rotation when the thrust ran into and was then raised and folded by the growing anticlinorium (late Messinian–early Pliocene time). This new model suggests a causal link between midcrustal folding and surficial orogenic curvature that is consistent with several available data sets from the northern and central Apennines; more evidence is, however, needed to fully test our hypothesis. Additionally, due to the occurrence of midcrustal basement-involved thrusts in other orogens, this model may be a viable mechanism for arc formation elsewhere.
    Description: Published
    Description: 1409-1420
    Description: 3.3. Geodinamica e struttura dell'interno della Terra
    Description: JCR Journal
    Description: reserved
    Keywords: oroclines ; Apennines ; fold and thrust belts ; gravity anomalies ; seismic reflection profiles ; 04. Solid Earth::04.02. Exploration geophysics::04.02.02. Gravity methods ; 04. Solid Earth::04.02. Exploration geophysics::04.02.06. Seismic methods ; 04. Solid Earth::04.03. Geodesy::04.03.04. Gravity anomalies ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.05. Geomagnetism::04.05.06. Paleomagnetism
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  • 16
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    Simultaneous magma and gas eruptions at three volcanoes in southern Italy: an earthquake trigger? (2008)
    Geological Society of America
    Details
    Publication Date: 2017-04-03
    Description: In September 2002, a series of tectonic earthquakes occurred north of Sicily, Italy, followed by three events of volcanic unrest within 150 km. On October 28, 2002, Mt. Etna erupted; on November 3, 2002, submarine degassing occurred near Panarea Island; and on December 28, 2002, Stromboli Island erupted. All of these events were considered unusual: the Mt. Etna NE-rift eruption was the largest in 55 yr, the Panarea degassing was one of the strongest ever detected there, and the Stromboli eruption, which produced a landslide and tsunami, was the largest effusive eruption in 17 yr. Here, we investigate the synchronous occurrence of these clustered unrest events, and develop a possible explanatory model. We compute short-term earthquake-induced dynamic strain changes and compare them to long-term tectonic effects. Results suggest that the earthquake-induced strain changes exceeded annual tectonic strains by at least an order of magnitude. This agitation occurred in seconds, and may have induced fluid and gas pressure migration within the already active hydrothermal and magmatic systems.
    Description: In press
    Description: 1.4. TTC - Sorveglianza sismologica delle aree vulcaniche attive
    Description: 1.5. TTC - Sorveglianza dell'attività eruttiva dei vulcani
    Description: 3.1. Fisica dei terremoti
    Description: 3.2. Tettonica attiva
    Description: 3.5. Geologia e storia dei sistemi vulcanici
    Description: 3.6. Fisica del vulcanismo
    Description: 4.2. TTC - Scenari e mappe di pericolosità sismica
    Description: 4.3. TTC - Scenari di pericolosità vulcanica
    Description: JCR Journal
    Description: open
    Keywords: earthquake trigger ; magma and gas eruptions ; 04. Solid Earth::04.01. Earth Interior::04.01.99. General or miscellaneous ; 04. Solid Earth::04.01. Earth Interior::04.01.02. Geological and geophysical evidences of deep processes ; 04. Solid Earth::04.04. Geology::04.04.99. General or miscellaneous ; 04. Solid Earth::04.04. Geology::04.04.01. Earthquake geology and paleoseismology ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.99. General or miscellaneous ; 04. Solid Earth::04.06. Seismology::04.06.04. Ground motion ; 04. Solid Earth::04.06. Seismology::04.06.08. Volcano seismology ; 04. Solid Earth::04.07. Tectonophysics::04.07.99. General or miscellaneous ; 04. Solid Earth::04.07. Tectonophysics::04.07.02. Geodynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.04. Plate boundaries, motion, and tectonics ; 04. Solid Earth::04.07. Tectonophysics::04.07.05. Stress ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics ; 04. Solid Earth::04.08. Volcanology::04.08.99. General or miscellaneous ; 04. Solid Earth::04.08. Volcanology::04.08.03. Magmas ; 04. Solid Earth::04.08. Volcanology::04.08.06. Volcano monitoring ; 04. Solid Earth::04.08. Volcanology::04.08.08. Volcanic risk ; 05. General::05.02. Data dissemination::05.02.03. Volcanic eruptions
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  • 17
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    Multidisciplinary study of flank instability phenomena at Stromboli volcano, Italy (2007)
    AGU
    Details
    Publication Date: 2017-04-04
    Description: This study concerns the unstable scarp named Sciara del Fuoco (SDF) at Stromboli volcano, merging geostructural observations, live-cam records in the visible and IR bands, analysis of vertical aerial photographs, and seismic records. These are used to assess morpho-structural changes between 2002 and 2004. The onset of the lava effusion on 28 December, 2002 preceded a gravitational collapse by two days, affecting a wide area of the SDF above and below sea level. We surmise that the collapse enhanced latent instability of the scarp. The 2002–2003 lava flows had a remarkable stabilizing effect on wide portions (〉50%) of the SDF, whilst erosive phenomena continued in the zone not covered by lava. This caused unrelenting regression of the upper landslide scarp toward the summit craters in the form of rockfalls and debris flows. If the crater conduit were involved in the sliding, then a change in eruptive behavior cannot be excluded.
    Description: Published
    Description: L09304
    Description: reserved
    Keywords: NONE ; 04. Solid Earth::04.02. Exploration geophysics::04.02.99. General or miscellaneous ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 18
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    Propagation of dikes at Vesuvio (Italy) and the effect of Mt. Somma (2007)
    AGU
    Details
    Publication Date: 2017-04-04
    Description: Dikes provide crucial information on how magma propagates within volcanoes. Somma-Vesuvio (Italy) consists of the active Vesuvio cone, partly bordered by the older Mt. Somma edifice. Historical chronicles on the fissure eruptions in 1694–1944 are matched with an analytical solution to define the propagation path of the related dikes and to study any control of the Mt. Somma relief. The fissures always consisted of the downslope migration of vents from an open summit conduit, indicating lateral propagation as the predominant mechanism for shallow dike emplacement. No fissure emplaced beyond Mt. Somma, suggesting that its buttressing hinders the propagation of the radial dikes. An analytical solution is defined to describe the mechanism of formation of the laterally propagating dikes and to evaluate the effect of topography. The application to Somma-Vesuvio suggests that, under ordinary excess magmatic pressures, the dikes should not propagate laterally at depths 〉240–480 m below the surface, as the increased lithostatic pressure requires magmatic pressures higher than average. This implies that, when the conduit is open, the lateral emplacement of dikes is expectable on the S, Wand E slopes. The lack of fissures N of Mt. Somma is explained by its buttressing, which hinders dike propagation. Citation: Acocella, V., M. Porreca, M. Neri, E. Massimi, and M. Mattei (2006), Propagation of dikes at Vesuvio (Italy) and the effect of Mt. Somma, Geophys. Res. Lett., 33, L08301, doi:10.1029/2005GL025590.
    Description: Published
    Description: L08301
    Description: reserved
    Keywords: NONE ; 01. Atmosphere::01.01. Atmosphere::01.01.03. Pollution ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 19
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    Fissure eruptions at Mount Vesuvius (Italy):insights on the shallow propagation of dikes at volcanoes (2007)
    Geological Society of America
    Details
    Publication Date: 2017-04-04
    Description: Fissure eruptions may provide important information on the shallow propagation of dikes at volcanoes. Somma-Vesuvius (Italy) consists of the active Vesuvius cone, bordered to the north by the remnants of the older Somma edifice. Historical chronicles are considered to define the development of the 37 fissure eruptions between A.D. 1631 and 1944. The 1631 fissure, which reopened the magmatic conduit, migrated upward and was the only one triggered by the subvertical propagation of a dike. The other 25 fissure eruptions migrated downward, when the conduit was open, through the lateral propagation of radial dikes. We suggest two scenarios for the development of the fissures. When the summit conduit is closed, the fissures are fed by vertically propagating dikes. When the summit conduit is open, the fissures are fed by laterally propagating dikes along the volcano slopes. Consistent behaviors are found at other composite volcanoes, suggesting a general application to our model, independent of the tectonic setting and composition of magma. At Vesuvius, the historical data set and our scenarios are used to predict the consequences of the emplacement of fissures after the opening of the conduit. The results suggest that, even though the probability of opening of vents within the inhabited south and west slopes is negligible, the possibility that these are reached by a lava flow remains significant.
    Description: Published
    Description: 673-676
    Description: reserved
    Keywords: fissures ; dike propagation ; conduit ; Vesuvius ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.02. Geodynamics ; 04. Solid Earth::04.07. Tectonophysics::04.07.05. Stress
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  • 20
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    Understanding shallow magma emplacement at volcanoes: orthogonal feeder dikes during the 2002-2003 Stromboli (Italy) eruption (2007)
    AGU
    Details
    Publication Date: 2017-04-04
    Description: Understanding how shallow magma is emplaced within volcanoes is crucial for hazard assessment. The 2002–2003 Stromboli eruption provides the opportunity to investigate shallow magma emplacement resulting from orthogonal feeder dikes and its possible effects. Stromboli erupted in 2002–2003, when effusive activity replaced Strombolian activity. On December 28, a NE-SW fissure propagated from the lava-filled northernmost summit crater. On December 29, a NW-SE fissure propagated north of the craters, feeding NW-SE aligned vents. On December 30, this area collapsed, reaching the sea and generating a tsunami. In mid February 2003, the NW-SE fissure became inactive, while the NE-SW effusive fissure continued until July. A model for shallow magma emplacement is proposed. The lateral propagation of a NE-SW dike from the northernmost crater was triggered. Below, a NW-SE dike, propagating from the magma-filled NE tip of the NE-SW elongated conduit, fed the NW-SE aligned vents. In February, the conduit periphery became solidified, freezing the NW-SE dike, and the transport of magma was limited to the central part, focusing its rise below the craters. This fed the NE-SW fissure until the supply decreased further (July), returning to the ordinary level sustaining Strombolian activity. Orthogonal dike emplacement followed the trajectories of the maximum (gravitational) stress s1, partly controlled by the irregular topography of the uppermost edifice. The emplacement of orthogonal dikes in a limited area is feasible at non-perfectly conical active volcanoes, where the maximum gravitational stress may show variations from a purely radial path.
    Description: Published
    Description: L17310
    Description: reserved
    Keywords: NONE ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.07. Tectonophysics::04.07.05. Stress ; 04. Solid Earth::04.07. Tectonophysics::04.07.07. Tectonics
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  • 21
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    Volcanic tremor location during the 2004 Mount Etna lava effusion (2007)
    AGU
    Details
    Publication Date: 2017-04-03
    Description: A lava emission started at Mt. Etna, Italy, on 7 September, 2004. Neither earthquake seismicity heralded or accompanied the opening of the fracture field from which the lava poured out, nor volcanic tremor changed in amplitude and frequency content at the onset of the effusive activity. To highlight long-term changes, we propose a method for the location of the tremor source based on a 3D grid search, using the amplitude decay of the seismic signal, from January to November 2004. We find the centroid of the tremor source within a zone close to and partially overlapped with the summit craters (pre-effusive phase), which extended up to 2 km south of them (effusive phase). The depths are of between 1698 and 2387 m a.s.l. We hypothesize the lava effusion stemmed from a degassed magma body, although we find evidence of temporary magma overpressure conditions, such as those documented on 25 September.
    Description: Published
    Description: L09304
    Description: reserved
    Keywords: NONE ; 04. Solid Earth::04.02. Exploration geophysics::04.02.99. General or miscellaneous ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.08. Volcano seismology
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  • 22
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    Reactive halogen chemistry in volcanic plumes (2007)
    AGU
    Details
    Publication Date: 2023-01-19
    Description: Bromine monoxide (BrO) and sulphur dioxide (SO2) abundances as a function of the distance from the source were measured by ground-based scattered-light Multi AXis Differential Optical Absorption Spectroscopy (MAX-DOAS) in the volcanic plumes of Mt. Etna on Sicily, Italy in August-October 2004 and May 2005 and Villarica in Chile in November 2004. BrO and SO2 spatial distributions in a cross section of Mt. Etna’s plume were also determined by Imaging DOAS. We observed an increase in the BrO/SO2 ratio in the plume from below the detection limit near the vent to about 4.5 x 10-4 at 19 km (Mt. Etna) and to about 1.3 x 10-4 at 3 km (Villarica) distance, respectively. Additional attempts were undertaken to evaluate the compositions of individual vents on Mt. Etna. Furthermore, we detected the halogen species ClO and OClO. This is the first time that OClO could be detected in a volcanic plume. Using calculated thermodynamic equilibrium compositions as input data for a one–dimensional photochemical model, we could reproduce the observed BrO and SO2 vertical columns in the plume and their ratio as function of distance from the volcano as well as vertical BrO and SO2 profiles across the plume with current knowledge of multiphase halogen chemistry, but only when we assumed the existence of an ”effective source region”, where volcanic volatiles and ambient air are mixed at about 600°C (in the proportions of 60% and 40%, respectively)
    Description: Published
    Description: D06311
    Description: 3V. Proprietà chimico-fisiche dei magmi e dei prodotti vulcanici
    Description: JCR Journal
    Description: open
    Keywords: Chemistry ; Volcanic Plumes ; 04. Solid Earth::04.08. Volcanology::04.08.01. Gases ; 04. Solid Earth::04.08. Volcanology::04.08.06. Volcano monitoring ; 04. Solid Earth::04.08. Volcanology::04.08.07. Instruments and techniques
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  • 23
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    High spatial resolution radon measurements reveal hidden active faults on Mt. Etna (2005)
    AGU
    Details
    Publication Date: 2017-04-04
    Description: Radon emissions are frequently monitored in volcanically and tectonically active areas in order to reveal changes in soil degassing, as radon acts a tracer for the more abundant CO2 degassing commonly observed in such areas. Between July 2002 and May 2003 a series of discrete measurements of radon concentrations in soil were made with high spatial resolution (∼5–100 m) in the Santa Venerina area on Mt. Etna. These measurements revealed well-defined linear anomalies that we interpret as being caused by active faults whose higher porosity than surrounding soils allows an increased CO2 flux, carrying radon from beneath. These faults were not visible at the surface and were therefore revealed at high spatial resolution by our radon survey. Our hypothesis that the positive anomalies are attributable to active faults was strengthened by the observation of concentrated damage along this geometry during the earthquakes that struck this area in late October 2003.
    Description: Published
    Description: 4
    Description: partially_open
    Keywords: Structural Geology: Role of fluids ; Structural Geology: Fractures and faults ; Structural Geology: Instruments and techniques ; Volcanology: Instruments and techniques ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology
    Repository Name: Istituto Nazionale di Geofisica e Vulcanologia (INGV)
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  • 24
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    Paroxysmal summit activity at Mt. Etna (Italy) monitored through continuous soil radon measurements (2005)
    AGU
    Details
    Publication Date: 2017-04-04
    Description: Soil radon emissions have been proved as a useful tool for predicting earthquakes and volcanic eruptions and furthermore aided in determining the location of active faults. Continuous radon monitoring was carried out near Southeast Crater of Mt. Etna in September–November 1998, during a period of frequent eruptive episodes at that crater. Radon anomalies were detected when eruptive episodes and the accompanying volcanic tremor became increasingly intense: no anomalies in radon activity were observed during the first five, and weaker, eruptive episodes, whereas significant spikes in radon activity preceded the latter five episodes by ≥46 hours. This probably reflects increased gas leakage through fractures intersecting the shallow plumbing system, as gas pressure in the Southeast Crater conduit became higher with time. Radon monitoring thus might serve to better understand eruptive mechanisms and possible precursors, making further studies in this field a promising perspective.
    Description: Published
    Description: 1-4
    Description: partially_open
    Keywords: Seismology: Volcano seismology ; Structural Geology: Role of fluids ; Volcanology: Volcano monitoring ; Volcanology: Instruments and techniques ; 04. Solid Earth::04.04. Geology::04.04.09. Structural geology ; 04. Solid Earth::04.06. Seismology::04.06.08. Volcano seismology ; 04. Solid Earth::04.08. Volcanology::04.08.06. Volcano monitoring ; 04. Solid Earth::04.08. Volcanology::04.08.07. Instruments and techniques
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  • 25
    Electronic Resource
    Electronic Resource
    Triphenylpyrylium Tetrafluoroborate-Sensitized Photochemistry of the Terpenes Sabinene, α-Phellandrene, and α- and γ-Terpinene (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1563-1567 
    Details
    ISSN: 1434-193X
    Keywords: Triplet recombination ; Electron transfer ; Radical ions ; Photochemistry ; Terpenes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The triphenypyrylium tetrafluoroborate (TPT)-sensitized reactions of several terpene donor molecules, including sabinene (1), α-phellandrene (4), α-terpinene (5) and γ-terpinene (6) give rise to significantly different products than reactions induced by other electron-transfer sensitizers, such as 1,4-dicyanobenzene (DCB). The divergent reactions require decidedly different key intermediates; the products obtained with TPT can be explained by dissociative recombination of the intermediate radical-radical cation pair in the triplet state, generating donor-derived biradicals.
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  • 26
    Electronic Resource
    Electronic Resource
    Ring Expansion of 2-Alkylidenedihydroquinazolines to Iminodihydro-1,4-benzodiazepines by Methanesulfonyl and Trifluoromethanesulfonyl Azide (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1577-1587 
    Details
    ISSN: 1434-193X
    Keywords: Azides ; Cleavage reactions ; Cycloadditions ; Nitrogen heterocycles ; Polycycles ; Ring expansion ; Synthetic methods ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---2-Alkyl-1-methylquinazolinium hexafluorophosphates 9 are deprotonated by sodium or potassium hydride to afford solutions of 2-alkylidenedihydroquinazolines 10, which were investigated by NMR spectroscopy. Trapping with methanesulfonyl azide (5a) of 10 in situ or subsequent treatment with trifluoromethanesulfonyl azide (5b) gives mixtures of colourless (15) and intensely yellow N-sulfonylimino-1,4-benzodiazepines 16 along with products due to cleavage of the exocyclic double bond of 10, viz. 11 and 13. The ethylidene compound 10b yields the bicyclic products 18 and 19, apparently by complex sequences of reactions that are triggered by removal of the acidic proton at C-2 of 16b and 16f. The structures of the products are based on spectroscopic evidence and X-ray diffraction analyses performed on 15b, 16d, 16e, and 19.
    Additional Material: 6 Ill.
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  • 27
    Electronic Resource
    Electronic Resource
    Electrophilic Reactivity of a 2-Azaallenium and of a 2-Azaallylium Ion (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1589-1593 
    Details
    ISSN: 1434-193X
    Keywords: Azaallenium ions ; Azaallylium ions ; Iminium ion ; Kinetics ; Linear Free Energy Relationships ; Ab initio calculations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The rate constants for the reactions of the 2-azaallenium ion 1b+, the 2-azaallylium ion 2a+ and the iminium ion 3+ with different nucleophiles were determined by 1H NMR spectroscopy. By correlation with the Linear Free Enthalpy Relationship (LFER) lg k20°C = s (E + N), developed by Mayr and Patz, the electrophilicity parameters E(1b+) = -3.7, E(2a+) ≍ -16 and E(3+) = -10.43 were obtained. They show that the relative reactivities of these ions are approximately 1012:1:106. Quantum chemical calculations (ab initio, DFT) of the methyl anion affinities for the ions 1b+,2a+ and3+ are in agreement with the experimental E values. The X-ray structure of 3+·CF3SO3- is reported for the first time; it shows no strong interaction between the cation and the anion.
    Additional Material: 2 Ill.
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  • 28
    Electronic Resource
    Electronic Resource
    Oxazoline N-Oxide Mediated [3+2] Cycloadditions: Application to a Formal Synthesis of a (+)-β-Methylcarbapenem (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1595-1601 
    Details
    ISSN: 1434-193X
    Keywords: Oxazoline N-oxide ; Cycloadditions ; Cycloadditions ; Lactams ; Thienamycin ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---[3+2] Cycloaddition between a camphor-derived oxazoline N-oxide 9 and the γ,δ-unsaturated enamino ester 11 afforded the single adduct 6. A stereoselective reduction of the enamino ester side chain allowed the control of the absolute configuration of the two additional asymmetric centres. Nitrogen protection and oxidative hydrolysis of the resulting product 13, followed by further functional group manipulations, led to the β-lactam derivative 1, a known precursor of the β-methylthienamycin derivative2a.
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    A New Substitution Pattern in Subphthalocyanines: Regioselective Synthesis and Separation of “ortho” Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1603-1607 
    Details
    ISSN: 1434-193X
    Keywords: Boron ; Cyclotrimerizations ; Nitrogen heterocycles ; Macrocycles ; Subphthalocyanines ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The regioselective preparation of ortho-substituted subphthalocyanides was achieved employing 3-substituted phthalonitrile derivatives as starting materials. A mechanistic proposal has been outlined.Supporting information for this article is available on the WWW under //http://www.wiley-vch.de/contents/jc_2046/2000/99525_s.pdf or from the author.
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    A New Route to 2,7- and 7-Functionalized Labdanes (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1609-1615 
    Details
    ISSN: 1434-193X
    Keywords: Terpenoids ; Natural products ; Total synthesis ; Cyclizations ; Rearrangements ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A new route for the synthesis of 2,7- and 7-functionalized labdanes starts from (R)-carvone (1). 11-Nordrim-7-en-9-one (15) is an appropriate starting material for the total synthesis of hispanone (21), a biologically active furolabdane isolated from the Mediterranean medicinal plant Ballota saxatilis.
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    Preparation of Kingiside from Aucubin (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1623-1626 
    Details
    ISSN: 1434-193X
    Keywords: Iridoid glucoside ; (8S)-Kingiside ; (8S)-Loganin ; (8S)-7-Ketologanin ; Asymmetric synthesis ; Natural products ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The tetraacetyl derivative 8 of the naturally occurring kingiside (8a) was prepared from aucubin (1). Intermediates in the synthesis were (8S)-tetraacetyl loganin (6) and (8S)-tetraacetyl-7-ketologanin (7), whose free (8R)-epimers occur in many different plants (Caprifoliaceae, Loganiaceae). The 13C NMR spectrum allows the structure to be unequivocally identified.
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    Isomeric Tetrakis(dimethylamino)naphthalenes: Syntheses, Structure-Dependence of Basicities, Crystal Structures, and Physical Properties (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1617-1622 
    Details
    ISSN: 1434-193X
    Keywords: Tetrakis(dimethylamino)naphthalenes ; Basicity ; Hydrogen bonds ; Cyclicvoltammetry ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---For comparison to the recently described 2,3,6,7-tetrakis(dimethylamino)naphthalene (1) the three isomers 2,3, and 4 were synthesized. The basicities of this group of isomers are strongly dependent upon the different mutual orientations of the pairs of dimethylamino substituents: only the isomers 3 and, partially, 4, both with dimethylamino groups in adjacent peri-positions of the naphthalene, are strong “proton sponges”. For the isomers 1 and 2 with the same number and kind of twofold dimethylamino substituents in neighbouring ortho-positions, however, no significant basicity increase is observed. To explain this difference between the two groups of isomers it is suggested that in the ortho-pairs of 1 and 2 the C-N bonds diverge considerably, leading to an increased N···N distance and consequently to less stable [N···H···N]+ hydrogen bonds in contrast to the parallel C-N bonds in the peri-substituted isomers 3 and 4. X-ray crystal structure analyses of the bases and of some of the salts derived therefrom were solved and are discussed. Cyclic voltammetry indicates that 1 to 4 are strong electron donors, reacting easily to radical cations or dications which with suitable acids have been obtained as salts.
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    Ring Closure Reactions of Disubstituted 4-Penten-1-oxyl Radicals - Towards a Stereoselective Synthesis of allo-Muscarine (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1677-1683 
    Details
    ISSN: 1434-193X
    Keywords: Radicals ; Cyclizations ; Pyridinethione ; Tetrahydrofurans ; Asymmetric synthesis ; Thiazolethione ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The trisubstituted functionalized tetrahydrofurans 10, 11, 16, 18, and 19 were photochemically prepared from 2,3-syn- and 2,3-anti-configuredN-(3-benzoyloxy-5-hexen-2-oxy)thiazole-2(3H)-thione anti-6, pyridinethiones 7, anti-8, and BrCCl3. The formation of tetrahydrofurans was achieved by an efficient and highly regioselective alkoxyl radical cyclization (5-exo-trig). The 2,3-anti substituted intermediates 9 and 12 cyclize stereoselectively whereas a 2,3-syn-configured O-radical affords both possible diastereomeric addition products in equal amounts. The cyclized tetrahydrofuryl methyl radicals were trapped with the bromine atom donor BrCCl3 to afford the bromomethyl-substituted cyclic ethers 10, 11, 18, and 19 in excellent yields. The utility of this reaction was stressed by conversion of one of the newly prepared tetrahydrofurans in a two-step synthesis into (+)-allo-muscarine (+)-20.Supporting information for this article is available on the WWW under //http://www.wiley-vch.de/contents/jc_2046/2000/99590_s.pdf or from the author.
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    The Formation of 1,3-Dithiolanes from Aromatic Thioketones and Diazomethane - The Mechanism of the Schönberg Reaction (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1685-1694 
    Details
    ISSN: 1434-193X
    Keywords: Thioketones ; Thiocarbonyl ylides ; Cycloadditions ; Cycloreversions ; Sulfur heterocycles ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Reactions of diaryl thioketones with diazomethane at room temperature afford 4,4,5,5-tetraaryl-1,3-dithiolanes; the scope of this surprising 2:1 interaction has been studied for decades (Schönberg Reaction). The clue to the mechanism was our observation that the stoichiometry is 1:1 at -78 °C, and 2,5-dihydro-2,2-diaryl-1,3,4-thiadiazoles are formed as primary [2+3] cycloadducts. They lose N2 at -45 °C in first-order reactions generating diaryl thioketone S-methylides which can be intercepted by thioketones (→1,3-dithiolanes), multiple CC bonds, or acids HX. In the absence of trapping reagents, the elusive intermediates either dimerize furnishing 2,2,3,3-tetraaryl-1,4-dithianes or give rise to 2,2-diarylthiiranes by electrocyclization. Beyond thiobenzophenone and diazomethane, our main model reaction, the studies involve fluorene-9-thione, 4,4-dimethoxy- and 4,4-dichlorothiobenzophenone. The ring of 2,5-dihydro-2,2-diphenyl-1,3,4-thiadiazole (8) is opened by LDA at -78 °C and derivatives of anion 12 are obtained. - In summa: The Schönberg reaction consists of two 1,3-dipolar cycloadditions, linked by a 1,3-dipolar cycloreversion.
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    New Boronic-Acid- and Boronate-Substituted Aromatic Compounds as Precursors of Fluoride-Responsive Conjugated Polymer Films (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1703-1710 
    Details
    ISSN: 1434-193X
    Keywords: Conjugation ; Boron ; Sensors ; Cyclic voltammetry ; Polymers ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---New electropolymerizable aromatic compounds (i.e. pyrrole, thiophene, aniline) bearing boronic acid and ester substituents have been synthesized and their electrochemical behavior has been investigated. Functionalized polythiophene and polypyrrole films could be anodically generated in acetonitrile, whereas the polyaniline derivative was electroformed in an acidic aqueous solution. The electrochemical responses of some of these materials were changed when fluoride ions were added to the electrolytic solutions. The strongest modifications, caused by binding of fluoride by the immobilized boron, were observed for the polypyrrole derivative in hydroorganic media.
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    The Effect of the Carbon Ligand on the Reaction of Organozinc Reagents in the Synthesis of Substituted 2,5-Dihydrofurans: A Rare Example of An Uncatalysed Allylic-Substitution Reaction Involving Alkyl Zinc Halides (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1711-1718 
    Details
    ISSN: 1434-193X
    Keywords: Heterocycles ; Zinc ; Palladium ; Catalysts ; Sulfur ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Organozinc halides derived from Grignard reagents behave differently in their reaction with ethyl (±±)-(2RS,3SR)-tetrahydro-4-methylene-2-phenyl-3-(phenylsulfonyl)furan-3-carboxylate (3) according to the hybridisation of the carbon ligand. During the development of short multi-component reactions for the synthesis of diverse functionalized ethyl 2,5-dihydrofuran-3-carboxylates it was discovered that aryl and vinyl zinc halides undergo clean reaction with 3 in the presence of Pd(PPh3)4. In contrast, when alkyl zinc halides are reacted with 3 in the presence of Pd(PPh3)4, reductive desulfonation of 3 is observed. Remarkably, in the absence of a transition metal catalyst, the allylic substitution of 3 with alkyl zinc halides proceeds cleanly and in moderate to good yield.
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    Stable Heterotopic Noncovalent Resorcin[4]arene Assemblies (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1727-1734 
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    ISSN: 1434-193X
    Keywords: Self-assembly ; Vapor-pressure osmometry ; Resorcin[4]arenes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Resorcin[4]arene tetracarboxylic acids 5,6 (A) and resorcin[4]arene tetrapyridines 2,3 (P) self-assemble in chloroform solution to form stable heterotopic AP dimers. Data from NMR titration and dilution experiments, as well as from vapor-pressure osmometry (VPO), indicate that the AP dimer is formed with an association constant greater than 107 M-1. Solid-solution extraction experiments are indicative of the formation of a 2:1 trimer (A2P), while self-associated homotopic species (A2 and A3) can be detected by NMR and VPO. Analysis of the heterotopic noncovalent assembly process over a range of compositions shows that these other species are much less stable than the AP heterodimer, which is the exclusive species at an A/P concentration ratio of 1:1 (〉 99.7% of the total at 10 mM).
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    The LiClO4-Mediated Synthesis of β-(Dialkylamino) Sulfoxides and β-(Dialkylamino) Sulfones by Addition of α-Lithiated Salts of Sulfoxides and Sulfones to Aldehydes and (Trimethylsilyl)dialkylamines (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1735-1739 
    Details
    ISSN: 1434-193X
    Keywords: Sulfoxides ; β-Amino sulfones ; Mannich type reaction ; Lithium perchlorate ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The LiClO4-mediated one-pot reaction of aldehydes with (trimethylsilyl)dialkyl amines and the lithium salt of sulfoxides or sulfones, affords the corresponding β-(dialkylamino) sulfoxides and β-(dialkylamino) sulfones in high yields. The aminosulfoxidation reaction of aliphatic or aromatic aldehydes lacks diastereoselectivity, but the diastereomeric sulfoxides can be separated by HPLC or column chromatography for further use.
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    Synthesis of Heptano Bridged Pyranoside Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1741-1744 
    Details
    ISSN: 1434-193X
    Keywords: Bridged pyranose derivatives ; Ring enlargement ; Carbenes ; Glycosides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Addition of dichlorocarbene to the glycal (±±)-2 followed by cyclopropyl-allyl rearrangement leads to the chloro-2H-pyran (±±)-4. Oxidation of (±±)-4 and reduction of the obtained hydroxypyranone (±±)-5 gave the methyl pyranoside (±±)-6. The relative configuration of (±±)-6 was established by X-ray structural analysis of the corresponding acetate (±±)-7. The synthesis of the optically active starting materials (+)-2 and (-)-2 is also reported.
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    Sialyltransferase Inhibitors Based on CMP-Quinic Acid (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1745-1758 
    Details
    ISSN: 1434-193X
    Keywords: CMP-Neu5Ac analogues ; Enzyme inhibitors ; Substrate analogues ; Transition state analogues ; Transferases ; Carbohydrates ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Quinic acid was transformed into phosphitamides 16, 25, and 36, which could be readily linked to 5′-O-unprotected cytidine derivative 17. Ensuing oxidation of the obtained phosphite triesters with tBuO2H and hydrogenolytic de-O-benzylation furnished the corresponding phosphate diesters 18, 26, and 38. Base catalyzed removal of acetyl protecting groups, and methyl ester hydrolysis furnished CMP-Neu5Ac analogues 1d, 1e, and 2. Quinic acid was also transformed into 1,2-unsaturated diallyl α-hydroxymethyl-phosphate derivatives (R)- and (S)-46, which on reaction with cytidine phosphitamide 47 afforded the phosphite triesters. Subsequent oxidation with tBuO2H and then treatment with NEt3 gave phosphate diester derivatives (R)- and (S)-48. Deallylation, acetyl group removal, and methyl ester hydrolysis furnished (R)- and (S)-3, respectively. Treatment of (R)- and (S)-48 with DBU as a base led to acetic acid elimination, thus yielding, after de-O-allylation, acetyl group cleavage, and ester hydrolysis, diene derivative (E)-4. Donor substrate analogues 1d and 1e exhibited good α(2-6)-sialyltransferase inhibition (Ki: 2.0·10-4 and 2.0·10-5 M). However, transition state analogues (R)-, and particularly (S)-3 showed excellent inhibition properties (Ki: 1.6·10-6 and 2.7·10-7 M).
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    Synthesis and α-Mannosidase Inhibitory Activity of Three Deoxy Derivatives of Mannostatin A (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1759-1765 
    Details
    ISSN: 1434-193X
    Keywords: Cyclitols ; Aminocyclitols ; Glycosidase inhibitors ; α-Mannosidase inhibitors ; Deoxygenation ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Three deoxy derivatives 2-4 of the α-mannosidase inhibitor mannostatin A (1) were synthesized, and their inhibition of Jack bean α-mannosidase was evaluated in order to elucidate the roles of each of the three hydroxyl groups of the inhibitor. The 1- and 2-deoxy derivatives 2 and 3 retained some inhibitory activity, although reduced by a factor of about 100 relative to the parent, whereas it was completely lost with the 3-deoxy derivative 4. Structure and activity relationships are discussed in the light of these findings.
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    A Circular Dichroism Approach to the Conformation of 1-Arylethylamino-Substituted 1,3,5-Triazine Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1767-1772 
    Details
    ISSN: 1434-193X
    Keywords: Circular dichroism ; Conformation analysis ; s-Triazines ; Chiral auxiliaries ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---CD data of the optically pure 2-[(R)-1-(9-anthryl)ethylamino]-4-chloro-6-[(R)-1-(1-naphthyl)ethylamino]-1,3,5-triazine, 2[(R)-1-(9-anthryl)ethylamino]-4,6-bis[(R)-1-(1-naphthyl)ethylamino]-1,3,5-triazine, 2,4-bis[(R)-1-(9-anthryl)ethylamino]-6-chloro-1,3,5-triazine are presented. The analysis of the CD spectra by means of the nonempirical DeVoe approach has afforded the complete conformational characterisation of the three s-triazine derivatives, allowing us to establish how the conformation of these derivatives depends on the nature of the substituent 1-arylethylamino groups.
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    α,β-Unsaturated Fischer Carbene Complexes vs. 1,3-Dipoles: Reactions with Nitrones and Nitrilimines (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1773-1783 
    Details
    ISSN: 1434-193X
    Keywords: Cycloadditions ; Carbenes ; Nitrones ; Nitrilimines ; Pyrazolines ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The reaction of tert-butylalkynyl chromium Fischer carbene complex 1 with nitrones 2 affords β-enamino-ketoaldehydes 4 by the light-promoted rearrangement of the corresponding [3+2] cycloadduct carbene complexes 3. On the other hand, [3+2] cycloaddition of chiral nonracemic Fischer alkenyl carbene complexes 19 with nitrilimines 10 yields enantiomerically pure Δ2-pyrazolines with high regio- and diastereoselectivity.
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    Increasing Enantioselectivities and Reactivities by Stereochemical Tuning: Fenchone-Based Catalysts in Dialkylzinc Additions to Benzaldehyde (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1785-1792 
    Details
    ISSN: 1434-193X
    Keywords: Asymmetric synthesis ; Zinc ; Transition structures ; QM/MM computations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Trimethylsilyl substitutions of the fenchyl alcohols [(1R,2R,4S)-exo-(2-Ar)-1,3,3-trimethylbicyclo[2.2.1]heptan-2-ol, Ar = 2-methoxyphenyl (1) and Ar = 2-(dimethylaminomethyl)phenyl (2)] yield the chiral ligands 3 [Ar = 2-methoxy-3-(trimethylsilyl)phenyl] and 4 [Ar = 2-(dimethylaminomethyl)3-(trimethylsilyl)phenyl]. Increased reactivities and enantioselectivities in diethylzinc additions to benzaldehyde are obtained from 3 (63% ee R) and 4 (93% ee S), relative to 1 (26% ee S) and 2 (73% ee S). X-ray crystal structures of 3 and of its methylzinc complex 3-Zn reveal out-of-plane bending of the methoxy groups as major geometrical consequences of the trimethylsilyl substitutions. Analyses of QM/MM ONIOM μ-O transition-structure models for 1, 2, 3, and 4 show that trimethylsilyl-induced distortions of methoxy and of dimethylaminomethyl groups explain the observed increased enantioselectivities.
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    Evidence of Formation of an exo-π-Allyl Complex Intermediate in the Pd0-Catalyzed Alkylation of a Bicyclic Allylic Diacetate with Stabilized Carbon Nucleophiles (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1799-1803 
    Details
    ISSN: 1434-193X
    Keywords: Palladium ; exo-π-Allylpalladium complexes ; Allylic alkylation ; Spiro compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The palladium(0)-catalyzed alkylation of 2,3-bis(acetoxymethyl)bicyclo[2.2.1]hepta-2,5-diene 1 with malonate-type enolates as nucleophiles is investigated. A monoalkylated product is formed first, and undergoes (depending on the nucleophile used) a second intramolecular reaction leading to spirocyclopropane-annulated bicyclo[2.2.1]heptene derivatives 5. The formation of endo spirobicyclic cyclopropanes adducts as major isomer is rationalized by assuming formation of an intermediate exo-(π-allyl)palladium complex.
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    Reductions of α,β-Unsaturated Ketones by NaBH4 or NaBH4 + CoCl2: Selectivity Control by Water or by Aqueous Micellar Solutions (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1793-1797 
    Details
    ISSN: 1434-193X
    Keywords: Ketones ; Reductions ; Micelles ; Cobalt ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Operationally simple and environmentally benign procedures have been developed to selectively reduce different α,β-unsaturated ketones, 4,4-dimethylcyclohex-2-ene-1-one (1), isophorone (2), benzylideneacetone (3), chalcone (4) by NaBH4 or by the system NaBH4 + CoCl2. Alternative reaction media to the extensively used MeOH have been explored, and new procedures take advantage of the acceleration and chemoselectivity induced by water or by aqueous micellar solutions. It was possible to selectively and quantitatively afford pure products of 1,2 and of 1,4 reduction as well as the totally reduced compounds (yield and selectivity 〉 90%) by simple changes in the experimental conditions.
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    Conformational Behavior of C-Glycosyl Analogues of Sialyl-α-(2→3)-Galactose (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1805-1813 
    Details
    ISSN: 1434-193X
    Keywords: C-Glycosides ; Conformation analysis ; Molecular dynamics ; Selectins ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The conformational behavior of the C-glycosyl analogue of sialyl-α-(2→3)-galactose, synthesized as a glycosidase inhibitor, has been studied using a combination of NMR spectroscopy (J and NOE data) and molecular dynamics calculations. The obtained results show that the population distribution of conformers with respect to the orientation about the pseudo-glycosidic linkages is mainly controlled by steric interactions. This is in contrast to findings made for O-glycosides. In these natural compounds, the conformational behavior about the glycosidic linkage Φ is mainly governed by the exo-anomeric effect.
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    Enantioselective Preparation of 2,4-Disubstituted Azetidines (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1815-1820 
    Details
    ISSN: 1434-193X
    Keywords: Asymmetric synthesis ; Palladium-catalysed couplings ; Palladacycles ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Chiral C2-symmetric N-benzylazetidines have been conveniently prepared from optically pure anti-1,3-diols without loss of enantiomeric purity. N-Debenzylation led to the corresponding N-unsubstituted azetidines, which were then subjected to palladium-catalysed coupling reactions with aryl bromides to afford chiral N-arylazetidines. (R,R)-N-Benzyl-2,4-dimethylazetidine has been employed in the synthesis of a new cyclopalladated complex, which can be used, for instance, as a chiral recognition agent for phosphorus ligands.
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    Deoxyhydantocidin: Synthesis by Base-Catalyzed Spiro Cyclization and Interconversion with the 1′-Epimer (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1831-1840 
    Details
    ISSN: 1434-193X
    Keywords: Cyclizations ; Spiro compounds ; Nucleosides ; Isomerizations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Syntheses of the spiro nucleosides 2′-deoxyhydantocidin 3a and its 1′-epimer 3b are described. The newly developed route involves a Horner-Wadsworth-Emmons condensation of the phosphonate 16 with the erythrose derivative 15 affording a mixture of six isomers which was fully assigned by NMR spectroscopy. The mixture was directly converted into the final compounds in an efficient base-catalyzed cyclization reaction. A base-catalyzed interconversion between the two isomers was observed.
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    1-Alkyl- and Azeto[1,2-a][1,5]benzodiazepine Derivatives in the Reaction of o-Phenylenediamine with 3-(Dimethylamino)propiophenones (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1973-1976 
    Details
    ISSN: 1434-193X
    Keywords: Benzodiazepines ; Heterocycles ; Azeto[1,2-a]-1,5-benzodiazepines ; Cyclizations ; Cycloadditions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The reaction of o-phenylenediamine (4) with one, two or three equivalents of p-substituted 3-dimethylaminopropiophenone hydrochlorides 5a-e was studied. 4-Aryl-2,3-dihydro-1H-1,5-benzodiazepine derivatives 6a-e were obtained in good yields, along with the 1:2-adducts 7c-e and the unexpected 1:3-adducts rac-8c-e. The type of adduct formed is determined by the molar ratio of the reactants 4 and 5 and by the nature of the substituent in the para position of the propiophenone 5.
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    Synthesis of Benzotri(benzonorbornadienes) (BTBNDs): Rigid, Cup-Shaped Molecules with High Electron Density within the Cavity (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1965-1971 
    Details
    ISSN: 1434-193X
    Keywords: Cup-shaped PAHs ; Host-guest compounds ; Host-guest chemistry ; Cyclizations ; Semiempirical calculations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Cyclotrimerisation of benzo-polycyclic bromostannylalkenes 8a-d with Cu(NO3)2·3H2O in THF affords benzotri(benzonorbornadienes) 3a-d as a mixture of the syn and anti isomers. The ratio of syn to anti is close to the 1:3 statistical value in most cases (i.e. in cyclotrimers 3a,b,d), but highly in favour of the anti isomer in 3c, where steric hindrance by the methoxy groups plays an important role in the stereochemistry of the cyclotrimerisation. The substrates for the cyclotrimerisation, i.e. the bromostannyl alkenes 8a-d, were prepared from bromoalkenes 7a-d by treatment with base (LDA) and quenching with trimethyltin chloride. In turn, bromoalkenes 7a-d were prepared from alkenes 5a-d by radical bromination-elimination. The reaction conditions used were designed to minimise Wagner-Meerwein rearrangements that would lead to unwanted bromo isomers. The cup-shaped syn cyclotrimers 3a-d exhibit high electron density within the cavity as determined by AM1 semiempirical calculations of their electrostatic potential surfaces and are valuable substrates for supramolecular chemistry. As an example, it is shown that fullerene C60 is drawn into solution in acetonitrile by complexation with both the syn and anti trimer of benzonorbornadiene 3a.
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    Determination of Pollutant Phenols by Capillary High-Performance Liquid Chromatography with UV Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 367-372 
    Details
    ISSN: 0935-6304
    Keywords: Capillary HPLC ; gradient elution ; temperature programming ; phenolic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This paper describes a liquid chromatographic method using a reversed phase capillary column coupled to an UV detector for the quantitation of thirteen pollutant phenols. Chromatographic separation was carried out with gradient elution at 25.0 ± 0.1°C. The two major anisocratic elution modes (gradient elution and temperature programming) were evaluated. The detection limit range was 10-81 pg (100 nL injected). The chromatographic method combined with liquid-liquid extraction was applied to analysis of these compounds in river water. Recoveries of 75-103% were achieved for most of them.
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    Use of Capillary Supercritical Fluid Chromatography in the Analysis of Zinc Dialkyldithiophosphates (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 389-392 
    Details
    ISSN: 0935-6304
    Keywords: Capillary SFC ; zinc dialkyldithiophosphates ; lubricating oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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    Application of Supercritical Fluid Chromatography to the Analysis of Waxes in Objects of Art (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 393-396 
    Details
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography (SFC) ; micropacked capillary columns ; waxes ; restoring ; objects of art ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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    Identification of Free and Glycosidically Bound Volatiles and Glycosides by Capillary GC and Capillary GC-MS in “Lulo del Chocó” (Solanum topiro) (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 379-385 
    Details
    ISSN: 0935-6304
    Keywords: Aroma ; “lulo del Chocó” ; Solanum topiro ; volatiles ; glycosidically bound volatiles ; glycoside TFA derivatives ; enantioselective gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The volatile constituents of lulo del Chocó (Solanum topiro) fruit pulp obtained by liquid-liquid extraction were analyzed by capillary GC and capillary GC-MS. In total, 30 components were identified with methyl salicylate, hexadecanoic acid, hexanal, guaiacol, ethyl butanoate, and ethyl acetate being the major components. Chirospecific MDGC analysis revealed the predominance of (R)-ethyl-3-hydroxybutanoate (ee 40%) and the presence of racemic mixtures both of δ-octalactone and of δ-decalactone. For γ-hexalactone, γ-octalactone, and γ-decalactone enantiomeric distributions of 22.4 : 77.6, 22.9 : 77.1, and 20.0 : 80.0, (R) : (S), respectively, were determined. Glycosidically bound aroma compounds were identified by capillary GC and capillary GC-MS after isolation of the glycosidic fraction obtained by Amberlite XAD-2 adsorption and methanol elution followed by hydrolysis with a commercial pectinase enzyme. In total 13 bound aroma compounds (aglycones) were identified. These aglycones mainly consisted of compounds exhibiting aromatic structures. Additionally, with the aid of capillary GC and capillary GC-MS (EI and NCI) of trifluoroacetylated derivatives we identified eight glucosides: the novel 3,6-epoxy-7-megastigmen-5,9-diol β-D-glucopyranoside and the hexyl, benzyl, linalyl oxide (furanic), 2-phenylethyl, vomifolyl (isomer 1), (6S,9R)-vomifolyl, and scopoletin β-D-glucopyranosides.
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    System Peaks of Cyclodextrins in Capillary Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 409-412 
    Details
    ISSN: 0935-6304
    Keywords: Cyclodextrin ; capillary electrophoresis ; system peak ; CHES 1 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using a running buffer containing cyclodextrins (CDs) and 2-[N-cyclohexylamino]-ethanesulfonic acid (CHES), positive system peaks were observed in the analysis of a ganglioside mixture by CE-UV. These system peaks were related to CDs in the running buffer because these peaks were also detected when a plug of solution devoid of CDs but having the same CHES concentration and pH as the running buffer was injected. Neutral CDs were separated owing to the formation of inclusion complexes with the anionic CHES ion. One possible explanation for the positive system peaks is that the anionic CD-CHES inclusion complex is displaced by co-ions with higher UV absorptivity.
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    Liquid Chromatography of Unstable Zinc Dithiocarbamates. Application to Rubber Gloves Analysis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 565-566 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; zinc dithiocarbamate ; vulcanization accelerator ; rubber gloves ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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    Characteristic Stationary Phase Constants for Two Popular Open-Tubular Column Stationary Phases for Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 603-608 
    Details
    ISSN: 0935-6304
    Keywords: Solvation parameter model ; ystem constants for poly(dimethyldiphenylsiloxane) HP-5 and poly(ethylene glycol) HP-INNOWax stationary phases ; temperature ; molecular interaction ; retention models ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Determination of Cinnamomi Constituents by High-performance Liquid Chromatography and Capillary Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 561-564 
    Details
    ISSN: 0935-6304
    Keywords: Retention factors ; Cinnamomi ramulus ; high-performance liquid chromatography ; capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Ion Chromatography of Inorganic Anions on Graphitic Carbon as the Stationary Phase (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 590-594 
    Details
    ISSN: 0935-6304
    Keywords: Ion chromatography ; graphitic carbon stationary phases ; anions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Inorganic anions could be separated on porous graphitic carbon stationary phases in ion chromatography. Ion exchange between eluent anions and sample anions on the stationary phase was confirmed by the retention behavior and the possibility of indirect photometric detection. The elution order of anions was different from that observed for commercially available anion exchangers. Chloride, nitrate, and sulfate contained in tap water could be determined in 7 min.
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    Solid-Phase Microextraction of Pyrethroid Pesticides from Water at Low and Sub-ppt Levels at Different Temperatures (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 485-488 
    Details
    ISSN: 0935-6304
    Keywords: Pyrethroids ; solid-phase microextraction ; water analysis ; temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Synthetic pyrethroids are increasingly being used for insect control on field crops because of their advantageous environmental properties such as short field life, broad spectrum of insecticide activity, and relatively low mammalian toxicity. In the present work, experimental conditions were optimized for trace analysis of pyrethroids in water by using solid-phase microextraction followed by capillary gas chromatography. Effects of temperature, SPME-fiber diameter, and matrix were studied. SPME used off-line with a gas chromatograph electron-capture detection (GC-ECD) showed a linear response over a wide concentration range. Our results showed a strong temperature effect on pyrethroid extraction yield. The detection limit after 5 min of SPME-fiber exposure to the samples changed from 1 ppb (at 30°C) to 0.1 ppt (at 90°C), which is a 10000 increase in pyrethroid detection. The standard deviations of the analyte peak area ratios were typically in the range of 1-7% at 30°C and of 3 to 15% at 90°C. Best conditions for pyrethroids analysis were achieved using high temperature solution and a 100 μm polydimethylsiloxane fiber. No matrix (river water) influence was observed on detection of the investigated pyrethroids.
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    Microfabricated Monolith Columns for Liquid Chromatography. Sculpting Supports for Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 19-26 
    Details
    ISSN: 0935-6304
    Keywords: Microfabrication ; monolith ; electrochromatography ; peptides ; reactive ion etching ; reversed phase ; nanocolumns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monolith columns are generally fabricated by polymerization of monomers within a column. This paper reviews an alternative strategy in which the bed is microfabricated in an inorganic material by ablation. Channels of 1.5 μm width and 10 μm depth were sculpted in quartz by deep reaction ion etching. Using this approach chromatographic beds were constructed in which cubic support structures were created and arranged in rows to mimic particles in a conventional column. Beds ranging from hundreds of thousands to millions of “particles” with volumes of 15 nL to 15 μL were produced. Columns that had been derivatized with an octadecyl silane stationary phase were used to separate both low molecular weight analytes and peptides in the CEC mode. Plate height in the CEC mode was 1.2 μm at maximum efficiency.
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    Dynamic Capacity Studies of CIM (Convective Interaction Media)® Monolithic Columns (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 39-43 
    Details
    ISSN: 0935-6304
    Keywords: Monoliths ; CIM® monolithic column ; dynamic binding capacity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characterization of CIM® DEAE monolithic columns in terms of dynamic binding capacity is presented in this paper. Breakthrough experiments were performed for capacity determination. Bovine serum albumin (BSA) was used as a model protein. It is shown that CIM® monolithic columns have good batch-to-batch reproducibility as well as long-term stability. The experiments performed under different linear velocities demonstrated that the dynamic capacity is unaffected at least up to a linear velocity of 2450 cm/h. Furthermore, the breakthrough curve slope is constant, indicating that the capacity would remain constant at even higher linear velocities. The adsorption isotherm of BSA dissolved in 20 mM Tris-HCl buffer shows a constant capacity of around 30 mg/mL of support down to a concentration of 20 μg/mL. The capacity is substantially influenced by the ionic strength; however, 20% of the maximal capacity is still preserved at 0.3 M NaCl.
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    Affinity Chromatography of Human Blood Coagulation Factor VIII on Monoliths with Peptides from a Combinatorial Library (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 47-58 
    Details
    ISSN: 0935-6304
    Keywords: Monolith ; factor VIII ; affinity chromatography ; combinatorial peptide library ; peptide synthesis ; recombinant proteins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: FVIII is a very complex molecule of great therapeutic significance. It is purified by a sequence of chromatographic steps including immunoaffinity chromatography. A peptide affinity chromatography method has been developed using peptides derived from a combinatorial library. Spot technology using cellulose sheets has been applied for this purpose. The dual positional scanning strategy was used for identification of the amino acids in random positions. Approximately 5000 possible candidates found in the first screening round were reduced to a panel of 36. Six candidates have been selected empirically. Five peptides seem to be directed against the light chain of FVIII, one peptide seems to be directed against the heavy chain. The peptides have been immobilized on conventional beaded material and CIM polymethacrylate monoliths. Much better performance with respect to capacity and selectivity has been observed with the monolithic material. Exposure of the ligand and its ensuing accessibility are responsible for these properties.
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    Capillary Electrochromatography with Monolithic Poly(styrene-co-divinylbenzene-co-methacrylic acid) as the Stationary Phase (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 67-72 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; monolithic column ; electroosmotic flow ; retention mechanism ; aromatic compound ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new kind of monolithic capillary electrochromatography column with poly(styrene-co-divinylbenzene-co-methacrylic acid) as the stationary phase has been developed. The stationary phase was found to be porous by scanning electron microscopy and the composition of the continuous bed was proved by IR spectroscopy to be the ternary polymer of styrene, divinylbenzene, and methacrylic acid. The effects of operating parameters, such as voltage, electrolyte, and organic modifier concentration in the mobile phase on electroosmotic flow were studied systematically. The retention mechanism of neutral solutes on such a column proved to be similar to that of reversed-phase high performance liquid chromatography. In addition, fast analyses of phenols, chlorobenzenes, anilines, isomeric compounds of phenylenediamine and alkylbenzenes within 4.5 min were achieved.
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    Continuous-Bed Columns Containing Sol-Gel Bonded Packing Materials for Capillary Electrochromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 73-80 
    Details
    ISSN: 0935-6304
    Keywords: Continuous-bed ; sol-gel ; octadecylsilica ; mixed-mode stationary phase ; large-pore ; column technology ; capillary electrochromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Sol-gel bonded packing materials in continuous-bed columns have been prepared for capillary electrochromatography (CEC). Three packing materials were investigated: small-pore Spherisorb ODS1 (3 μm, 80 Å) with octadecyl as stationary phase, small-pore mixed-mode Spherisorb ODS/SCX (3 μm, 80 Å) with octadecyl and propyl sulfonic acid as stationary phases, and large-pore Nucleosil ODS (7 μm, 1 400 Å) with octadecyl as stationary phase. The characteristics of these columns were compared in terms of electroosmotic flow, efficiency, inertness, and retention factors. In contrast to columns containing sol-gel bonded ODS, columns containing sol-gel bonded mixed-mode ODS/SCX generated nearly pH independent electroosmotic flow (EOF) over pH 2-9. Columns containing sol-gel bonded large-pore ODS produced nearly three times lower reduced plate height than those containing small-pore ODS. Efficiencies of 220,000 plates per meter and 175,000 plates per meter were obtained from columns containing sol-gel bonded 7 μm, 1 400 Å ODS and columns containing sol-gel bonded 3 μm, 80 Å ODS, respectively, which are among the highest reported efficiencies for continuous-bed columns. In CEC, over one million plates per meter and pH independent EOF are expected from continuous-bed columns containing sol-gel bonded 1.5 μm particles with large pores and mixed-mode stationary phases.
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    Particle Loaded Monolithic Sol-Gel Columns for Capillary Electrochromatography: A New Dimension for High Performance Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 81-88 
    Details
    ISSN: 0935-6304
    Keywords: Monolithic chromatography columns ; capillary electrochromatography (CEC) ; micro high performance liquid chromatography ; sol-gel based columns for chromatography ; fritless capillary chromatography columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Particle-loaded (3 μm, octadecylsilica) monolithic sol-gel columns have been prepared and selected characteristics measured. Several electrical properties may be calculated from simple current measurements in the column as a whole. Resistivity in the packed segment is approximately three times that in open segments, resulting in a 60% increase in field strength in the packed regions compared to the capillary with no packing. The surprisingly high specific permeability of these sol-gel columns is characteristic of 8-μm particles, which allows their operation in the microLC mode at pressures as low as 69 kPa where their efficiency is about 50,000 plates per meter and in the CEC mode where efficiency is about 106,000 plates per meter at 5 kV. There is a relatively rapid loss of efficiency with increasing linear velocity beyond 0.2 mm/s in microLC mode, which may be due to additional diffusion processes in the inter-particulate voids. A rapid loss of efficiency above 0.5 mm/s is also observed in the CEC mode, for the same reasons. Chromatographic retention behavior in either separation mode is characteristic of conventional octadecylsilica particles, indicating that analytes have significant access to the surface within the pores of the immobilized bonded phase.
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    Preparation of Fritless Packed Silica Columns for Capillary Electrochromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 89-92 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; packed columns ; fritless columns ; stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Fritless packed silica gel columns were prepared using sol-gel technology. A part of a 75 μm i.d. fused silica capillary was filled with a mixture of tetramethoxysilane and poly(ethylene glycol). After gelling at 40°C and heating at 300°C, the resultant silica gel was derivatized with dimethyloctadecylchlorosilane. A scanning electron micrograph of a cross-section of the capillary column showed that the gel took the form of a spherical particle aggregate and adhered to the column inner wall. The column performance was evaluated for electrochromatography using acetonitrile-50 mM HEPES buffer (pH 6.6) (60/40 or 40/60, v/v) as the mobile phase. An electroosmotic flow of 1.0 mm/s was generated with (60/40, v/v) acetonitrile/HEPES buffer at a field strength of 546 V/cm. Using a sol-gel-derived packed column at an electroosmotic flow of 0.5 mm/s, efficiencies of up to 1.1×105 plates/m were obtained for retained solutes.
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    A New Monolithic-Type HPLC Column For Fast Separations (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 93-99 
    Details
    ISSN: 0935-6304
    Keywords: HPLC ; monolithic column ; silica rod column ; fast separations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The application of a new silica-based, monolithic-type HPLC-column for fast separations is presented. The column is prepared according to a new sol-gel process, which is based on the hydrolysis and polycondensation of alkoxysilanes in the presence of water soluble polymers. The method leads to “rods” made of a single piece of porous silica with a defined pore structure, i. e. macro- and mesopores. The main feature of silica rod columns is a higher total porosity, about 15% higher than of conventional particulate HPLC columns. The resulting column pressure drop is therefore much lower, allowing operation at higher flow rates including flow gradients. Consequently, HPLC analysis can be performed much faster, as it is demonstrated by various applications.
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    Monolithic Stationary Phases for Capillary Electrochromatography Based on Synthetic Polymers: Designs and Applications (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 3-18 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; monolithic columns ; synthetic polymers ; stationary phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monolithic materials have quickly become a well-established stationary phase format in the field of capillary electrochromatography (CEC). Both the simplicity of their in situ preparation method and the large variety of readily available chemistries make the monolithic separation media an attractive alternative to capillary columns packed with particulate materials. This review summarizes the contributions of numerous groups working in this rapidly growing area, with a focus on monolithic capillary columns prepared from synthetic polymers. Various approaches employed for the preparation of the monoliths are detailed, and where available, the material properties of the resulting monolithic capillary columns are shown. Their chromatographic performance is demonstrated by numerous separations of different analyte mixtures in variety of modes. Although detailed studies of the effect of polymer properties on the analytical performance of monolithic capillaries remain scarce at this early stage of their development, this review also discusses some important relationships such as the effect of pore size on the separation performance in more detail.
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    Preparative Monolithic Silica Sorbents (PrepRODs™) and Their Use in Preparative Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 100-105 
    Details
    ISSN: 0935-6304
    Keywords: Preparative chromatography ; silica monoliths ; PrepROD™ ; productivity ; SMB-chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The use of monolithic silica sorbents for the isolation of substances by preparative liquid chromatography is demonstrated. Preparative liquid chromatography is recognized as a valuable technique for the isolation and purification of substances in the pharmaceutical and fine chemicals industry. The system technology has meanwhile reached a high standard, and the greatest future improvements are expected to arise from new and improved adsorbents. Monolithic silica sorbents offer some unique features for preparative liquid chromatography. They exhibit high efficiencies even at high flow rates due to their fast convective mass transfer and can therefore be used at very high mobile phase velocities, leading to high productivity and hence to maximum process economy. The benefits of this new type of adsorbent are illustrated for an example in batch-chromatographic mode and an example using the continuous simulated moving bed (SMB) technology.
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    Tailoring Mesopores in Monolithic Macroporous Silica for HPLC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 106-110 
    Details
    ISSN: 0935-6304
    Keywords: Silica ; monolithic column ; aging ; mesopores ; pore size distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Mesopore formation in silica gels having continuous macropores has been investigated. The macroporous wet silica gel prepared by the sol-gel process including phase separation was aged in a basic solvent making use of hydrolysis of urea in a closed condition. The mesopore structure was finally obtained by subsequent evaporation drying of solvent and heat-treatment at 600°C for 2 h. The dissolution-reprecipitation kinetics at the interfaces between wet gel skeletons and an external solvent affected the size and volume of pores formed within the skeletons. Below 120°C, mesopores suitable for various chromatographic applications have been formed typically within 24 h. On the other hand, at 200°C, the pore size attained the macropore dimensions (〉50 nm), and the whole macroporous morphology was significantly modified.
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    Monolithic Silica Columns for HPLC, Micro-HPLC, and CEC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 111-116 
    Details
    ISSN: 0935-6304
    Keywords: Monolithic column ; silica monolith ; HPLC ; capillary liquid chromatography ; capillary electrochromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Two types of monolithic silica columns derivatized to form an ODS phase, one prepared in a fused silica capillary (SR-FS) and the other prepared in a mold and clad with an engineering plastic (poly-ether-ether-ketone) (SR-PEEK), were evaluated. The column efficiency and pressure drop were compared with those of a column packed with 5-μm ODS-silica particles and of an ODS-silica monolith prepared in a mold and wrapped with PTFE tubing (SR-PTFE). SR-FS gave a lower pressure drop than a column packed with 5-μm particles by a factor of 20, and a plate height of 20 μm at a linear velocity below 1 mm/s. SR-PEEK showed higher flow-resistance than the other monolithic silica columns, but they still showed a minimum plate height of 8-10 μm and a lower pressure drop than popular commercial columns packed with 5-μm particles. The evaluation of SR-FS columns in a CEC mode showed much higher efficiency than in a pressure-driven mode.
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    Note on the Net Retention Volume in Chromatography with a Real Gas as a Carrier (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 119-126 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; retention volume ; real gas carrier ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The problem of the calculation and interpretation of the net retention volume with a real gas as carrier is revisited. The properties of the carrier are described by a first order virial equation of state. The net retention volume of a solute is related to the mean flow rate of the carrier, therefore determination of the mean flow rate of a real gas carrier is reviewed. It is shown that the mean flow rate cannot be calculated from the mean column pressure. With a real gas carrier the local capacity factor depends on the local pressure of the real gas. The basic relationship between the net retention volume and the function describing this pressure dependence is also reviewed. Precise formulae as well as practical approximations are presented for the calculation of the mean flow rate, of the mean column pressure, and of a representative pressure related to the mean capacity factor.
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    Detection of Polyols by HPLC Coupled with an On-Line Photochemical Oxidation Reactor and Chemiluminescence Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 127-130 
    Details
    ISSN: 0935-6304
    Keywords: Chemiluminescence ; diol compound ; oxalate ; post-column reaction ; ruthenium complex ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In this paper we propose a new post-column detection method for polyols containing 1,2-diol, 1,3-diol, and saccharides. The polyols are oxidized in a photochemical reactor to yield oxalate with subsequent chemiluminescence detection using [Ru(III)(bpy)3]3+. A mixing solution of eluate and oxidizing reagent is delivered to a reaction coil, which is then irradiated with ultraviolet light to promote the oxidation reaction. The detection limits for 1,2-ethanediol (ethylene glycol) and 1,3-propanediol were 38 pmol and 23 pmol, respectively.
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    Coupled LC-GC-NPD for Determination of Carbazole-Type PANH and Its Application to Personal Exposure Measurement (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 131-137 
    Details
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; nitrogen selective detection ; NPD ; carbazoles ; PANH ; personal exposure measurement ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A coupled LC-GC method for the analysis of carbazole-type PANH has been developed and evaluated. Group separation and isolation of carbazoles from interfering acridines in a complex sample matrix was accomplished by using a back-flush technique and an in situ end-capped dimethylaminopropyl silica column in the HPLC part of the system. On-line injection of the carbazole fraction into the GC column was performed with a loop-type interface utilizing concurrent solvent evaporation technique. An LOD of 1-3 pg of individual carbazole compounds was achieved by nitrogen selective detection using an NPD. The method is shown to be robust and is demonstrated by application to personal exposure measurement in an aluminum reduction plant.
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    Fast Separation of Nucleosides by Capillary Electrochromatography on Non-Endcapped Phenyl-Bonded Silica Phase Using Short-End Injection Method (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 138-142 
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    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; nucleosides ; short-end injection ; phenyl-bonded silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The influence of several experimental parameters (pH, ionic strength, organic modifier content of hydro-organic buffer) upon EOF, migration time, and retention factor has been studied in CEC with a phenyl-bonded silica column on a model mixture of five nucleosides. This paper illustrates the current interest in CEC as a method of resolving complex mixtures of neutral and ionic solutes and demonstrates the potential of the short-end injection method as a means of reducing analysis time.
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    Separation of Anthraquinones by Capillary Electrophoresis and High-Performance Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 143-148 
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    ISSN: 0935-6304
    Keywords: Analysis of anthraquinones ; capillary electrophoresis ; high-performance liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The separation and determination of twelve anthraquinones, viz. anthraquinone 1, chrysphanol 2, aloe-emodin 3, alizarin 4, anthraquinone-2-carboxylic acid 5, purpurin 6, sennoside B 7, sennoside A 8, emodin 9, quinalizarin 10, rhein 11, and anthraflavic acid 12, were achieved by capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC). Detection at 260 nm with a buffer solution containing 30 mM sodium borate (adjusted to pH = 10.56 with 0.05N NaOH) and acetonitrile (9 : 1) in CE or with a linear gradient elution containing 20 mM KH2PO4 with 0.05% phosphoric acid (pH = 2.91) and methanol in HPLC was found to be the most suitable approach for this separation. Contents of six components (2, 3, 7, 8, 9, 11) in crude Rhei Rhizoma extract could easily be determined within 39 min by CE or 63 min by HPLC. The effects of buffers on this separation and the validation of the two methods were studied.
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    Capillary Gas Chromatography of Trichlorophenols Using Ammonia as Carrier Gas (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 156-157 
    Details
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; trichlorophenols ; ammonia ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Large Volume Injection in Fast Gas Chromatography with On-Column Injector (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 149-155 
    Details
    ISSN: 0935-6304
    Keywords: Capillary GC ; fast GC ; on-column injection ; narrow-bore column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In this work a fast gas chromatography set-up with on-column injection was optimized and evaluated with a model mixture of C8-C28 n-alkanes. Usual injection volumes when using narrow-bore (e. g., 0.1 mm i.d.) analytical columns are ca. 0.1 μL. The presented configuration allows introduction of 10-30-fold larger sample volumes without any distortion of peak shapes. In the set-up a normal-bore retention gap (1 m×0.32 mm i. d.) was coupled to a narrow-bore (4.8 m×0.1 mm i. d.×0.4 μm film thickness) analytical column using a low dead volume column connector. The effects of the experimental conditions such as inlet pressure, sample volume, initial injection temperature, and oven temperature on a peak focusing are discussed. H-u curves for helium and hydrogen are used to compare their suitability for high speed gas chromatography and to show the dependence of separation efficiency on the carrier gas velocity at high inlet pressures. In the fast gas chromatography system a baseline separation of C10-C28 n-alkanes was achieved in less than 3 minutes.
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    Proper Tuning of Comprehensive Two-Dimensional Gas Chromatography (GC×GC) to Optimize the Separation of Complex Oil Fractions (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 182-188 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional gas chromatography ; GC×GC ; thermal modulation ; oil analysis ; petroleum analysis ; analysis of middle-distillate oil fractions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Comprehensive two-dimensional gas chromatography (GC×GC) is an utterly suitable separation technique for the analysis of complex samples, such as oil fractions. Once the two columns and the operating conditions are properly tuned, the technique is able to provide a detailed characterization of such materials. Some considerations applying to the tuning of a GC×GC system for a specific separation are presented and discussed. The authors present a number of different column sets and conditions which allow the separation of a non-aromatic hydrocarbon solvent, a kerosene, the light end of a crude oil, and an olefinic fraction, respectively. The highly structured GC×GC chromatograms, together with chemical knowledge about the samples, provide a much more comprehensive characterization of the samples than hitherto possible.
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    Comprehensive Two-Dimensional Gas Chromatography with a Rotating Thermal Desorption Modulator and Independently Temperature-Programmable Columns (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 189-196 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional gas chromatography ; thermal desorption modulator ; temperature programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In comprehensive two-dimensional gas chromatography, two individual separations are coupled by means of a rotating thermal desorption modulator interface. The injection pulse introduced via the interface onto the second column should be as short as possible. Parameters affecting the modulator operation are studied. In the set-up used in this study, the temperature of the second column can be programmed independently from that of the first column. Optimization of the second-dimension separation to minimize peak broadening and maximize resolution is discussed and an elegant approach to determine second-dimension retention times using a non-constant modulation frequency is demonstrated. The high separation power of the comprehensive system is demonstrated by the analysis of technical and biota samples containing chlorinated biphenyls and toxaphene.
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    Determination of Oxygenates in Gasoline by GC×GC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 197-201 
    Details
    ISSN: 0935-6304
    Keywords: Multidimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC×GC ; oxygenates ; MTBE ; reformulated gasoline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Comprehensive two-dimensional gas chromatography (GC×GC) has been applied to the quantitation of oxygenates in reformulated gasoline. Target oxygenates were C1-C4 alcohols, tert-pentanol, methyl tert-butyl ether (MTBE), diisopropyl ether (DIPE), ethyl tert-butyl ether (ETBE), and tert-amyl methyl ether (TAME). These were separated from the gasoline matrix using a volatility-based selectivity in the first chromatographic dimension, followed by a mixed-phase polarity/shape selectivity in the second dimension. The high resolving power of this stationary phase combination completely separated all oxygenates except DIPE, ETBE, and TAME, which exhibited coelution with other nonpolar gasoline components. Oxygenates quantitation was achieved with the use of an internal standard, an FID detector, and calibration curves. Quantitation results are in good agreement with ASTM and EPA standard methods. When coupled with our previous method for BTEX and aromatics, a single GC×GC method can now quantitate MTBE, alcohols, BTEX, and aromatics in a one-hour analysis.
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    Biodegradation of Pharmaceutical Residues Investigated by SPE-GC/ITD-MS and On-Line Derivatization (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 474-478 
    Details
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Solid-phase extraction, on-line derivatization, and measurement by ion trap mass spectrometry (ITD-MS) were used to investigate the biological degradation of pharmaceutical residues (clofibric acid, ibuprofen, diclofenac). The results of the single steps of sample pretreatment and analytical determination are reported. MS/MS measurements were performed on an ITD-MS by selecting collision induced dissociation of the molecular ions (M+) as parent ions to defined daughter ions. A pilot sewage plant and biofilm reactors operating under oxic and anoxic conditions were run as model systems with synthetic sewage water containing 10 to 50 mg/L dissolved organic carbon (DOC) and pharmaceuticals in concentrations of 10 μg/L. Clofibric acid displayed its persistent character in all cases. The pilot sewage plant and the oxic biofilm reactor showed comparable results for diclofenac and ibuprofen, which both were partly degraded. These results can explain the occurrence of these substances in sewage effluents and in the aquatic environment. A high degree of degradation was found especially for ibuprofen in the oxic biofilm reactor, which was attributed to adaptation of the biofilm to the residue. Two metabolites of ibuprofen could be identified on the basis of their mass spectra and comparison with literature data, viz. hydroxyibuprofen and carboxyibuprofen.
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    Characterization of Polydimethylsiloxanes Using an Off-Line Combination of Supercritical Fluid Chromatography with Matrix-Assisted Laser Desorption Ionization Mass Spectrometry (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 502-506 
    Details
    ISSN: 0935-6304
    Keywords: Silicone oil ; supercritical fluid chromatography (SFC) ; micropacked columns ; MALDI-TOF ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Separation and Detection of Metal Ions in Ecological Samples by Capillary Zone Electrophoresis with Indirect UV Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 511-514 
    Details
    ISSN: 0935-6304
    Keywords: CZE ; indirect UV detection ; metal ions ; ecological samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Solventless Sample Preparation Techniques in Environmental Analysis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 297-303 
    Details
    ISSN: 0935-6304
    Keywords: Sample preparation ; gas extraction techniques ; membrane-type techniques ; water analysis ; soil analysis ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This review focuses on the role of so-called solventless methods of sample preparation in contemporary environmental analysis. The basic classification of this group of methods as well as the principal features and advantages of the techniques in current use are discussed.
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    Comparison of Thermal Sweeper and Cryogenic Modulator Technology for Comprehensive Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 253-258 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive gas chromatography ; cryogenic modulation ; semi-volatile aromatics ; thermal sweeper ; peak widths ; peak asymmetries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The two current technologies for achieving comprehensive gas chromatography (GC×GC) - the thermal sweeper and the cryogenic modulator - are compared in an interlaboratory study using a multicomponent semi-volatile aromatic compound sample. The same column set (phases, film thickness, dimensions of columns) and conditions of oven temperature program were used. Carrier gas flow settings however were different for the data reported here. The thermal sweeper has a longer overall length due to the extra ca. 30 cm length of narrow bore tubing used for the modulator/accumulator section. Data reveal that the two methods behave in an analogous manner in respect of delivering GC×GC results, with key peak parameters of peak widths and symmetry measures showing good correlation. Retention time dissimilarity on the first dimension columns in the two systems arises from different flow rates used, however the second column retention is similar, and this is due to the resulting different elution temperatures that peaks elute on the first dimension in each system. Overall, the two approaches to GC×GC appear to produce equivalent results within the scope of the application studied. Each system does have its experimental limitations; the thermal sweeper has what may be called a ‘thick film effect’, where at high temperature it can be difficult to sufficiently trap the migrating bands in the accumulator column, and the pulsing of solutes in the cryogenic system may suffer from a ‘thick wall effect’ if a column with too thick a wall dimension is used at low oven temperature.
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    Is Multidimensional High Performance Liquid Chromatography (HPLC) an Alternative in Protein Analysis to 2D Gel Electrophoresis? (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 259-265 
    Details
    ISSN: 0935-6304
    Keywords: Proteomics ; protein analysis ; multidimensional HPLC ; ion-exchange chromatography ; reversed phase chromatography ; comprehensive HPLC ; two-dimensional HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The interactive modes of High Performance Liquid Chromatography (HPLC) of proteins provide a platform for the construction of a multidimensional HPLC system coupled to mass spectrometry. We present a system composed of both anion and cation exchanger columns, in the first dimension, and n-octadecyl bonded 1.5 μm nonporous silica columns in the second dimension. Both columns are operated under gradient conditions. A system suitability test with standard proteins showed that the total analysis can be performed within about 20 minutes. The fractions taken from the ion exchanger column are directly analyzed within one minute on the reversed phase column at a high flow rate. Two reversed phase columns are applied and operated alternatively: while the first column performs the separation within one minute, the analytes leaving the first dimension are enriched in an on-column focusing mode on top of the second column. The sample clean-up and enrichment is performed on a novel type of restricted access cation exchanger column with internal sulfonic acid groups and external diol groups. The columns exhibit a molecular weight exclusion limit for globular proteins of about 15 kDa. Our next studies will be directed towards the analysis of proteins and peptides from extracts of fibroblasts.
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    Fiber Conditioners for Solid Phase Microextraction: Design, Testing, and Application (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 343-347 
    Details
    ISSN: 0935-6304
    Keywords: SPME ; desorption ; fiber conditioning ; field sampling ; sample preparation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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    Silver Ion High-Performance Liquid Chromatographic Separation of Conjugated Linoleic Acid Isomers, and other Fatty Acids, after Conversion to p-Methoxyphenacyl Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 348-352 
    Details
    ISSN: 0935-6304
    Keywords: Silver ion high-performance liquid chromatography (Ag-HPLC) ; conjugated linoleic acid (CLA) ; p-methoxyphenacyl derivatives ; single-column Ag-HPLC ; fatty acid analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Seed Oil Fatty Acids of Mongolian Compositae: The trans-Fatty Acids of Heteropappus hispidus, Asterothamnus centrali-asiaticus and Artemisia palustris (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 360-366 
    Details
    ISSN: 0935-6304
    Keywords: Artemisia palustris ; Asterothamnus centrali-asiaticus ; capillary gas liquid chromatography ; Compositae (Asteraceae) ; Heteropappus hispidus ; seed oil ; silver ion thin layer chromatography ; trans-fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Seed oils from the Compositae plant family are known to contain a variety of unusual fatty acids. Subsequent to the recent discovery of γ-linolenic acid in Saussurea and Youngia, further Mongolian Compositae species were investigated for their seed oil fatty acid composition. A number of δ3trans-fatty acids (16 : 1δ3t, 18 : 1δ3t and 18 : 3δ3t, 9c, 12c) were found in the seed oils of Heteropappus hispidus and Asterothamnus centrali-asiaticus. The latter fatty acid, but not the trans-monoenes, was also found in one species of Artemisia. These unusual fatty acid isomers were characterized by capillary gas-liquid chromatographic (GLC) separations in combination with other chromatographic techniques (analytical thin layer chromatography, TLC and preparative argentation TLC), and infrared spectrocsopy (IR). Their identity was further confirmed by co-chromatography with other seed oils known to contain these trans-fatty acids. The fact that within the Compositae plant family there are apparently two or three distinct groups of genera containing δ3trans-fatty acids is discussed.
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    2H/1H Ratio Analysis of Flavor Compounds by On-Line Gas Chromatography Pyrolysis Isotope Ratio Mass Spectrometry (HRGC-P-IRMS): Benzaldehyde (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 357-359 
    Details
    ISSN: 0935-6304
    Keywords: 2H/1H ratio analysis ; HRGC-P-IRMS ; stable isotopes ; benzaldehyde ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Isotope ratio monitoring gas chromatography-mass spectrometry of the 2H/1H ratio by pyrolysis isotope ratio mass spectrometry (P-IRMS) was used to analyze benzaldehyde originating from various sources. Based on the δ2HSMOW value of an authentic reference sample determined with an elemental analyzer (EA), the range of reproducibility and linearity was checked. Correct (EA related) and reproducible data were obtained for sample amounts 〉0.6 μg benzaldehyde (on column). In another series of experiments, the influence of sample preparation, i. e. simultaneous distillation-extraction (SDE) was found to be negligible. The following ranges of δ2HSMOW values were determined for benzaldehyde using five types of samples, i. e. (i) synthetic (δ2HSMOW -78 to -85‰, ex benzal chloride; +420 to +668‰, ex toluene) and ‘natural’ (including ‘ex-cassia’) references (δ2HSMOW -83 to -144‰); (ii) bitter almond oils (δ2HSMOW -113 to -148‰); (iii) fruits (δ2HSMOW -111 to -146‰); (iv) kernels (δ2HSMOW -115 to -188‰); and (v) leaves (δ2HSMOW -165 to -189‰).
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  • 94
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    Effects of Injected Volume and Applied Voltage on Column Efficiency in Capillary Electrochromatography with Open Tubular Columns of 10 μm i. d. (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 373-378 
    Details
    ISSN: 0935-6304
    Keywords: Open tubular columns ; capillary electrochromatography ; column efficiency ; injected volume ; applied voltage ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of some instrumental parameters on column efficiency in open tubular capillary electrochromatography (OTCEC) has been evaluated. First, it was investigated whether band broadening due to the sample injection process is within a tolerable range when an open tubular column (OTC) of about 10 μm i. d. is used. As a result of the small injection profile factor (K2 = 1.3), injected volumes must be sufficiently small (less than 10 pL) to avoid a significant efficiency loss (〉5%) when hydrodynamic injection by siphoning is employed. Secondly, the kinetic performance of OTCs in a CEC system was estimated from the variation of the reduced plate height (h) with the reduced linear velocity (ν) which was controlled by the voltage applied. Reasonable agreement was obtained between the theoretical h versus ν curve and the experimental values for a group of polycyclic aromatic hydrocarbons used as test compounds. Values of 0.25 for minimum h at an optimum ν of 16 are estimated, which permit separations with around 400,000 plates per meter to be obtained in less than 5 min. Finally, the possibility of estimating the diffusion coefficients of the solutes in the mobile phase from the plot of the height of a theoretical plate versus electroosmotic flow velocity is shown.
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  • 95
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    Separation of Enantiomers of Drugs by Capillary Electrophoresis with Permethyl-gamma-Cyclodextrin as Chiral Solvating Agent (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 413-429 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; enantiomer separation ; chiral drugs ; TM-γ-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---High-throughput screening is a promising new approach in analytical chemistry. Within the framework of an extended screening program (The German-Chinese Drug Screening Program), the enantioseparation of 86 drugs was investigated by capillary zone electrophoresis in the presence of the chiral solvating agent (CSA) octakis-(2,3,6-tri-O-methyl)-γ-cyclodextrin (TM-γ-CD). By this means, 15 drugs could be separated into enantiomeric pairs. Approximate measures for the degree of interaction (migration retardation factor, Rm) and for the degree of enantiomer recognition (migration separation factors, αm) revealed intriguing patterns that were compared with those found for native γ-cyclodextrin (γ-CD). Although there is a distinct influence of the analyte structure on the electrophoretic data, interpretation remains difficult. Most remarkably, permethylation of γ-CD leads neither to a higher affinity nor to better chiral recognition, in contrast to the findings with α-CD.
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  • 96
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    Retention Prediction System of O-Aryl,O-(1-methylthioethylidene-amino)phosphates on RP-HPLC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 445-448 
    Details
    ISSN: 0935-6304
    Keywords: O-Aryl,O-(1-methylthioethylideneamino)phosphates ; retention prediction ; quantitative structure-retention relationship (QSRR) ; reversed-phase HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Using factor analysis and stepwise linear regression methods, two parameters - CMR and ECCR - were selected from eight solute-related structure parameters as the most retention-influencing parameters. The relationships between the retention data (k ´) and the two structure parameters were established for 13 O-aryl,O-(1-methylthioethylideneamino)phosphate compounds under a wide range of experimental conditions. The retention data (k ´) of another seven compounds with similar structures were predicted using these QSRR equations. Good agreement was obtained between the experimental k ´ values and predicted ones.
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  • 97
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    Temperature-Programmed Packed Capillary Liquid Chromatography Coupled to Fourier-Transform Infrared Spectroscopy (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 525-530 
    Details
    ISSN: 0935-6304
    Keywords: Packed capillary liquid chromatography ; temperature programming ; Fourier-transform infrared spectroscopy ; polymer additives ; pneumatic nebulization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Temperature-programmed packed capillary liquid chromatography has been coupled off-line to Fourier-transform infrared spectroscopy, utilizing a commercially available interface with a pneumatic nebulizer rebuilt to handle low flow rates at elevated temperatures. The modified interface showed excellent performance with regard to non-aqueous reversed phase separations of polymer additives, resulting in constructed Gram-Schmidt chromatograms comparable to chromatograms obtained using UV detection. The spray of the in-house constructed nebulizer was not influenced by temperature changes of the column effluent, and hence temperature-programmed gradient separations could be used successfully. The relative standard deviation of peak height was 4.4% (n = 5) and the mass limit of detection was determined to be about 40 ng, using a polymer antioxidant as model compound. The present instrumental coupling has been used for characterization of the antioxidant Irgafos P-EPQ.
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  • 98
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    Separation of Enantiomers by On-Line Capillary Isotachophoresis-Capillary Zone Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 531-538 
    Details
    ISSN: 0935-6304
    Keywords: Capillary isotachophoresis ; capillary electrophoresis ; column-coupling electrophoresis ; enantiomers ; chiral ; amino acids ; tryptophan ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The ability of capillary zone electrophoresis (CZE) coupled on-line with capillary isotachophoresis (ITP) sample pretreatment in the column-coupling capillary electrophoresis equipment to separate trace enantiomers present in samples of complex ionic matrices and enantiomers present in their mixtures at significantly differing concentrations has been studied. Enantiomers of 2,4-dinitrophenyl labeled norleucine (DNP-Nleu) and tryptophan enantiomers were employed as model analytes in this work while urine and mixtures of tryptophan enantiomers of differing concentrations served as model samples. Experiments performed with urine samples spiked with the DNP-Nleu racemate at sub-μmol/L concentrations demonstrated excellent sample pretreatment capabilities of ITP (concentration of the analytes, in-column and post-column sample clean up) when coupled on-line with chiral CZE separations. In the CZE separations of enantiomers present in the samples at trace concentrations the sample pretreatment could be performed in both achiral and chiral ITP electrolyte systems. The use of a chiral electrolyte system was found to be essential in the ITP pretreatment of the samples containing the enantiomers at very differing concentrations. For example, a 2×10-7 mol/L concentration of L-tryptophan could be detected in the CZE separation stage of the ITP-CZE combination in samples containing about a 104 excess of D-tryptophan only when the ITP pretreatment was carried out in the electrolyte system providing the resolution of enantiomers (α-cyclodextrin served for this purpose in the present work). A post-column ITP sample clean up was found effective in enhancing the destacking rate of the trace enantiomer in the CZE stage when the migration configuration of the enantiomers was less favorable (the trace constituent migrating behind the major enantiomer).
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  • 99
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    Electronic Resource
    Characterization and Comparison of Tea Tree and Lavender Oils by Using Comprehensive Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 554-560 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive gas chromatography ; multidimensional gas chromatography ; essential oils ; coupled column analysis ; high resolution analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The essential oils from French lavender (Lavandula angustifolia) and tea tree (Melaleuca alternifolia) were separated by the two-dimensional GC technique of comprehensive gas chromatography. A coupled column combination of non-polar (5% phenyl equivalent) and polyethylene glycol phase columns was used to provide the desired resolution performance. By using a range of known standards, some of the peaks in lavender oil can be assigned. Some of these also occur in tea tree oil; however, from our knowledge of the major constituents in this oil and their relative retention behaviour, most of the major peaks may be tentatively assigned within the 2-dimensional separation space. There appear to be elution patterns within the 2-D space which should be useful in correlating retention with chemical and structural properties of the components, although this will require further evaluation. A range of coeluting peaks, which may not be so readily separated by using a single column capillary GC analysis, are resolved in the experiment described.
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  • 100
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    Gas Chromatographic Enantiomer Separation of Atropisomeric PCBs Using Modified Cyclodextrins as Chiral Phases (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 619-627 
    Details
    ISSN: 0935-6304
    Keywords: Enantiomer separation ; mixed chiral selectors ; modified cyclodextrins ; gas chromatography ; PCB ; o,p´-DDD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Columns containing different types of cyclodextrin derivatives have been evaluated for chiral gas chromatographic separation of atropisomeric PCBs, o,p´-DDT and o,p´-DDD. Separation was attempted on columns containing mixed chiral selectors, and the performance of two closely related selectors was also examined. The cyclodextrins were: permethylated-β-CD (PM-β-CD), heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)-β-CD (2,3-M-6-TBDMS-β-CD), heptakis(2,3-di-O-methyl-6-O-tert-hexyldimethylsilyl)-β-CD (2,3-M-6-THDMS-β-CD), and heptakis(2,3-di-O-ethyl-6-O-tert-hexyldimethylsilyl)-β-cyclodextrin (2,3-E-6-THDMS-β-CD). The cyclodextrins were dissolved in OV-1701 or in a dimethylsiloxane/silarylene copolymer containing 5% phenyl in the backbone. The application of mixed chiral selectors led to improved separations, however; at most eleven PCB congeners were separated on a single column. Chiral resolution of o,p´-DDD was achieved. The use of a dimethylsiloxane/silarylene copolymer as a matrix for the cyclodextrins is a promising approach. With such a matrix, blocking of the CD cavities by silicone substituent groups can be avoided, and a reasonable CD solubility can be provided. The selectivity of heptakis(2,3-di-O-ethyl-6-O-tert-hexyldimethylsilyl)-β-CD and heptakis(2,3-di-O-methyl-6-O-tert-hexyldimethylsilyl)-β-CD was quite different, the former selector could separate four congeners, while the latter separated ten congeners.
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