scholarly journals In Situ Observation of Stress Accumulation during Sub-Merged Arc Welding

2014 ◽  
Vol 996 ◽  
pp. 417-423 ◽  
Author(s):  
Arne Kromm ◽  
Thomas Kannengiesser
Keyword(s):  
Arc Welding ◽  
Large Scale ◽  
X Ray Diffraction ◽  
X Ray ◽  
Residual Stress State ◽  
Testing Facility ◽  
Large Scale Testing ◽  
The Impact ◽  
Stress Accumulation

Results obtained from laboratory tests mostly need to be verified under fabrication conditions in order to incorporate design specifics (joint configuration and restraint), which effect the residual stress state considerably. For this purpose, multi-pass sub merged arc welding was performed in a special large-scale testing facility. The impact of varying interpass temperatures could be proven in-situ by means of a pronounced stress accumulation during welding and subsequent heat treatment accompanied by stress determination using X-ray diffraction.

scholarly journals Lanthanoid Complexes Supported by Retro-Claisen Condensation Products of β-Triketonates

2018 ◽  
Author(s):  
Laura Abad Galán ◽  
Alexandre N. Sobolev ◽  
Eli Zysman-Colman ◽  
Mark Ogden ◽  
Massimiliano Massi
Keyword(s):  
Chelating Ligands ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Claisen Condensation ◽  
X Ray ◽  
Condensation Products ◽  
Complexation Reactions ◽  
The Impact ◽  
Low Solubility

<i>β</i>-Triketonates have been recently used as chelating ligands for lanthanoid ions, presenting unique structures varying from polynuclear assemblies to polymers. In an effort to overcome low solubility of the complexes of tribenzoylmethane, four <i>β</i>-triketones with higher lipophilicity were synthesised. Complexation reactions were performed for each of these molecules using different alkaline bases in alcoholic media. X-ray diffraction studies suggested that the ligands were undergoing decomposition under the reaction conditions. This is proposed to be caused by <i>in situ</i>retro-Claisen condensation reactions, consistent with two examples that have been reported previously. The lability of the lanthanoid cations in the presence of a varying set of potential ligands gave rise to structures where one, two, or three of the molecules involved in the retro-Claisen condensationreaction were linked to the lanthanoid centres. These results, along with measurements of ligand decomposition in the presence of base alone, suggest that using solvents of lower polarity will mimimise the impact of the retro-Claisen condensation in these complexes. <br>

In-Situ Diffraction Studies of Gas Storage Materials on a Laboratory X-Ray System

2013 ◽  
Vol 1544 ◽  
Author(s):  
Marco Sommariva ◽  
Harald van Weeren ◽  
Olga Narygina ◽  
Jan-André Gertenbach ◽  
Christian Resch ◽  
...  
Keyword(s):  
Large Scale ◽  
Fossil Fuels ◽  
Reaction Chamber ◽  
Hydrogen Gas ◽  
Gas Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Modifications ◽  
Model Studies

ABSTRACTThe sorption processes for hydrogen and carbon dioxide are of considerable, and growing interest, particularly due to their relevance to a society that seeks to replace fossil fuels with a more sustainable energy source. X-ray diffraction allows a unique perspective for studying structural modifications and reaction mechanisms that occur when gas and solid interact. The fundamental challenge associated with such a study is that experiments are conducted while the solid sample is held under a gas pressure. To date in-situ high gas pressure studies of this nature have typically been undertaken at large-scale facilities such as synchrotrons or on dedicated laboratory instruments. Here we report high-pressure XRD studies carried out on a multi-purpose diffractometer. To demonstrate the suitability of the equipment, two model studies were carried out, firstly the reversible hydrogen cycling over LaNi5, and secondly the structural change that occurs during the decomposition of ammonia borane that results in the generation of hydrogen gas in the reaction chamber. The results have been finally compared to the literature. The study has been made possible by the combination of rapid X-ray detectors with a reaction chamber capable of withstanding gas pressures up to 100 bar and temperatures up to 900 °C.

In Situ Time-Resolved X-Ray Diffraction Investigation of the ω→ψ Transition in Al-Cu-Fe Quasicrystal-Forming Alloys

2007 ◽  
Vol 558-559 ◽  
pp. 943-947 ◽  
Author(s):  
E. Otterstein ◽  
R. Nicula ◽  
J. Bednarčík ◽  
M. Stir ◽  
E. Burkel
Keyword(s):  
Large Scale ◽  
Applied Pressure ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
In Situ Xrd ◽  
Kinetics Of

Quasicrystals are aperiodic long-range ordered solids with a high potential for many modern applications. Interest is nowadays paid to the development of economically viable large-scale synthesis procedures of quasicrystalline materials involving solid-state transformations. The kinetics of the high-temperature phase transition from the complex ω-phase to the icosahedral quasicrystalline (iQC) ψ-phase in AlCuFe nanopowders was here examined by in-situ time-resolved X-ray diffraction experiments using synchrotron radiation. In-situ XRD experiments will allow insight on the influence of uniaxial applied pressure on the kinetics of phase transitions leading to the formation of single-phase QC nanopowders and further contribute to the optimization of sintering procedures for nano-quasicrystalline AlCuFe alloy powders.

Photo-mechanical azobenzene cocrystals and in situ X-ray diffraction monitoring of their optically-induced crystal-to-crystal isomerisation

2014 ◽  
Vol 5 (8) ◽  
pp. 3158-3164 ◽  
Author(s):  
Oleksandr S. Bushuyev ◽  
T. Christopher Corkery ◽  
Christopher J. Barrett ◽  
Tomislav Friščić
Keyword(s):  
Large Scale ◽  
Thermochemical Properties ◽  
Crystal Shape ◽  
X Ray Diffraction ◽  
X Ray ◽  
Optically Induced

We demonstrate the first supramolecular cocrystallisation strategy for generating crystalline azobenzene materials with a range of photo-mechanical and thermochemical properties: from those that exhibit isomerisation without any change in crystal shape to those that undergo a crystal-to-crystal cis–trans isomerisation accompanied by large scale bending.

scholarly journals Lanthanoid Complexes Supported by Retro-Claisen Condensation Products of β-Triketonates

2018 ◽  
Author(s):  
Laura Abad Galán ◽  
Alexandre N. Sobolev ◽  
Eli Zysman-Colman ◽  
Mark Ogden ◽  
Massimiliano Massi
Keyword(s):  
Chelating Ligands ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Claisen Condensation ◽  
X Ray ◽  
Condensation Products ◽  
Complexation Reactions ◽  
The Impact ◽  
Low Solubility

<i>β</i>-Triketonates have been recently used as chelating ligands for lanthanoid ions, presenting unique structures varying from polynuclear assemblies to polymers. In an effort to overcome low solubility of the complexes of tribenzoylmethane, four <i>β</i>-triketones with higher lipophilicity were synthesised. Complexation reactions were performed for each of these molecules using different alkaline bases in alcoholic media. X-ray diffraction studies suggested that the ligands were undergoing decomposition under the reaction conditions. This is proposed to be caused by <i>in situ</i>retro-Claisen condensation reactions, consistent with two examples that have been reported previously. The lability of the lanthanoid cations in the presence of a varying set of potential ligands gave rise to structures where one, two, or three of the molecules involved in the retro-Claisen condensationreaction were linked to the lanthanoid centres. These results, along with measurements of ligand decomposition in the presence of base alone, suggest that using solvents of lower polarity will mimimise the impact of the retro-Claisen condensation in these complexes. <br>

scholarly journals The impact of pressure on β-Cyclodextrin·acetaminophen inclusion complexes

2014 ◽  
Vol 70 (a1) ◽  
pp. C264-C264 ◽  
Author(s):  
Sofiane Saouane ◽  
Wolfgang Morgenroth ◽  
Hanns-Peter Liermann ◽  
Carsten Paulmann ◽  
Francesca Fabbiani
Keyword(s):  
High Pressure ◽  
Inclusion Complex ◽  
Aqueous Solubility ◽  
Crystal Form ◽  
Model Systems ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
The Impact

Cyclodextrins (CDs) have attracted considerable interest as model systems in supramolecular host-guest chemistry. They are described as hollow truncated cones with a hydrophilic outer surface and a nonpolar inner cavity suitable for small molecules' encapsulation.[1] By virtue of their character, CDs are used as excipients to improve the aqueous solubility of active pharmaceutical ingredients (APIs). High-pressure crystallisation techniques have been established as a suitable tool for exploring the phenomenon of polymorphism and solvate formation of pharmaceutical compounds throughout numerous examples reported in the literature.[2] Thus, exploring the inclusion-complex formation and the polymorphic behaviour of CDs with APIs at high pressure would be an interesting extension of the technique. The present work describes the attempt of an in-situ crystallisation of β-CD·acetaminophen inclusion complex and compression studies of the known β-CD·acetaminophen complex[3] in different crystallisation media at pressures up to 1.0 GPa. A new high-pressure crystal form observed at 0.8 GPa as well as unexpected results are presented herein. The crystals have been characterised by means of polarised optical microscopy, Raman spectroscopy and single-crystal X-ray diffraction using both home and synchrotron sources.

Large-scale synthesis of Li1.15V3O8 nanobelts and their lithium storage behavior studied by in situ X-ray diffraction

2012 ◽  
Vol 22 (7) ◽  
pp. 3035 ◽  
Author(s):  
Jie Shu ◽  
Miao Shui ◽  
Dan Xu ◽  
Yuanlong Ren ◽  
Dongjie Wang ◽  
...  
Keyword(s):  
Large Scale ◽  
X Ray Diffraction ◽  
Lithium Storage ◽  
X Ray ◽  
Storage Behavior ◽  
Large Scale Synthesis

scholarly journals Lanthanoid Complexes Supported by Retro-Claisen Condensation Products of β-Triketonates

2018 ◽  
Author(s):  
Laura Abad Galán ◽  
Alexandre N. Sobolev ◽  
Eli Zysman-Colman ◽  
Mark Ogden ◽  
Massimiliano Massi
Keyword(s):  
Chelating Ligands ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Claisen Condensation ◽  
X Ray ◽  
Condensation Products ◽  
Complexation Reactions ◽  
The Impact ◽  
Low Solubility

<i>β</i>-Triketonates have been recently used as chelating ligands for lanthanoid ions, presenting unique structures varying from polynuclear assemblies to polymers. In an effort to overcome low solubility of the complexes of tribenzoylmethane, four <i>β</i>-triketones with higher lipophilicity were synthesised. Complexation reactions were performed for each of these molecules using different alkaline bases in alcoholic media. X-ray diffraction studies suggested that the ligands were undergoing decomposition under the reaction conditions. This is proposed to be caused by <i>in situ</i>retro-Claisen condensation reactions, consistent with two examples that have been reported previously. The lability of the lanthanoid cations in the presence of a varying set of potential ligands gave rise to structures where one, two, or three of the molecules involved in the retro-Claisen condensationreaction were linked to the lanthanoid centres. These results, along with measurements of ligand decomposition in the presence of base alone, suggest that using solvents of lower polarity will mimimise the impact of the retro-Claisen condensation in these complexes. <br>

scholarly journals Control of Pharmaceutical Cocrystal Polymorphism on Various Scales by Mechanochemistry: Transfer from the Laboratory Batch- to the Large-Scale Extrusion Processing

2018 ◽  
Author(s):  
Tomislav Stolar ◽  
Stipe Lukin ◽  
Martina Tireli ◽  
Irena Sović ◽  
Bahar Karadeniz ◽  
...  
Keyword(s):  
Vitamin C ◽  
Mechanochemical Synthesis ◽  
Large Scale ◽  
Antioxidant Properties ◽  
In Situ Monitoring ◽  
Human Consumption ◽  
Continuous Manufacturing ◽  
X Ray Diffraction ◽  
X Ray

<p>We demonstrate a controllable mechanochemical synthesis of cocrystal polymorphs of ascorbic acid (vitamin C) and nicotinamide (vitamin B3) on different scales and without using bulk solvents. Next to the previously described polymorph of the 1:1 cocrystal, which is one of the first cocrystals approved for human consumption, we report here a new, thermodynamically more stable polymorph detected during in situ synchrotron powder X-ray diffraction monitoring of milling reactions. The new polymorph is currently available exclusively by mechanochemical synthesis, and its crystal structure was determined from powder X-ray diffraction data. Laboratory in situ monitoring by Raman spectroscopy provided direct insight into the cocrystals formation and was further used to optimize the manufacturing procedure. Sub-gram synthesis using laboratory mixer mill was transferred to the 10 g scale on a planetary ball mill and continuous manufacturing using a twin-screw extruder. Both cocrystal polymorphs perform excellently in tableting, thus alleviating the notoriously poor compactible properties of vitamin C, while the mechanochemical cocrystallization does not harm its antioxidant properties.<b></b></p>

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