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Challenges of quantitative phase analysis of iron and steel slags: a look at sample complexity
- Jessica E. Lyza, Timothy G. Fawcett, Sarah N. Page, Kelly L. Cook
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- Journal:
- Powder Diffraction / Volume 38 / Issue 2 / June 2023
- Published online by Cambridge University Press:
- 26 May 2023, pp. 119-138
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Quantitative phase analysis (QPA) of slags is complex due to the natural richness of phases and variability in sample composition. The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in slag, as well as the mixture of crystalline and amorphous components specific to each slag type. Additionally, polymorphs are common because of the complexity of the steelmaking and slag cooling processes, such as the cation-doped calcium aluminum silicate (Ca3Al2O6, C3A, Z = 24) supercell in LMF slag. References for these doped variants may not exist or in many cases are not known in advance, therefore it is incumbent on the analyzer to be aware of such discrepancies and choose the best available reference. All issues can compound to form a highly intricate QPA and have prevented previous methods of QPA from accurately measuring phase components in slag. QPA was performed via the internal standard method using 8 wt% ZnO as the internal standard and JADE Pro's Whole Pattern Fitting analysis. For each phase, five variables (lattice parameters, preferred orientation, scale factor, temperature factor, and crystallite size) must be accounted for during quantitation, with a specific emphasis on not refining crystallite sizes for iron oxides and trace phases as they are inclined to over-broaden and interact with the background to improve the goodness of fit (R/E value). Preliminary investigations show somewhat reliable results with the use of custom file sets created within PDF-4+ specifically targeted toward slag minerals to further regulate and normalize the analysis process. The objective of this research is to provide a standard protocol for collecting data, as well as to update methodologies and databases for QPA, to the slag community for implementation in a conventional laboratory setting. Currently, Whole Pattern Fitting “Modified” Rietveld block refinement coupled with the addition of a ZnO internal standard gives the most accurate QPA results, though further research is needed to improve upon the complex issues found in this study of the QPA of slags.
Crystal structure of dutasteride (Avodart), C27H20F6N2O2
- James A. Kaduk, Cyrus E. Crowder, Kai Zhong, Timothy G. Fawcett, Matthew R. Suchomel
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- Journal:
- Powder Diffraction / Volume 29 / Issue 3 / September 2014
- Published online by Cambridge University Press:
- 13 August 2014, pp. 274-279
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Commercial dutasteride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.587 44(3), b = 9.960 80(5), c = 33.500 42(12) Å, V = 2531.862(17) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, Rietveld, and density functional techniques. The most prominent feature of the structure is a zigzag chain of strong N–H···O = C hydrogen bonds along the a-axis. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.
Crystal structure of atomoxetine hydrochloride (Strattera), C17H22NOCl
- James A. Kaduk, Cyrus E. Crowder, Kai Zhong, Timothy G. Fawcett, Matthew R. Suchomel
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- Journal:
- Powder Diffraction / Volume 29 / Issue 3 / September 2014
- Published online by Cambridge University Press:
- 16 June 2014, pp. 269-273
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Commercial atomoxetine hydrochloride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.362 554(12), b = 13.340 168(27), c = 16.701 887(33) Å, V = 1640.421(5) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, and Rietveld and density functional techniques. The most prominent feature of the structure is zigzag chains of N–H···Cl hydrogen bonds along the a-axis. The powder pattern has been submitted to the ICDD for inclusion in future releases of the Powder Diffraction File™.
Contributor affiliations
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- By Frank Andrasik, Melissa R. Andrews, Ana Inés Ansaldo, Evangelos G. Antzoulatos, Lianhua Bai, Ellen Barrett, Linamara Battistella, Nicolas Bayle, Michael S. Beattie, Peter J. Beek, Serafin Beer, Heinrich Binder, Claire Bindschaedler, Sarah Blanton, Tasia Bobish, Michael L. Boninger, Joseph F. Bonner, Chadwick B. Boulay, Vanessa S. Boyce, Anna-Katharine Brem, Jacqueline C. Bresnahan, Floor E. Buma, Mary Bartlett Bunge, John H. Byrne, Jeffrey R. Capadona, Stefano F. Cappa, Diana D. Cardenas, Leeanne M. Carey, S. Thomas Carmichael, Glauco A. P. Caurin, Pablo Celnik, Kimberly M. Christian, Stephanie Clarke, Leonardo G. Cohen, Adriana B. Conforto, Rory A. Cooper, Rosemarie Cooper, Steven C. Cramer, Armin Curt, Mark D’Esposito, Matthew B. Dalva, Gavriel David, Brandon Delia, Wenbin Deng, Volker Dietz, Bruce H. Dobkin, Marco Domeniconi, Edith Durand, Tracey Vause Earland, Georg Ebersbach, Jonathan J. Evans, James W. Fawcett, Uri Feintuch, Toby A. Ferguson, Marie T. Filbin, Diasinou Fioravante, Itzhak Fischer, Agnes Floel, Herta Flor, Karim Fouad, Richard S. J. Frackowiak, Peter H. Gorman, Thomas W. Gould, Jean-Michel Gracies, Amparo Gutierrez, Kurt Haas, C.D. Hall, Hans-Peter Hartung, Zhigang He, Jordan Hecker, Susan J. Herdman, Seth Herman, Leigh R. Hochberg, Ahmet Höke, Fay B. Horak, Jared C. Horvath, Richard L. Huganir, Friedhelm C. Hummel, Beata Jarosiewicz, Frances E. Jensen, Michael Jöbges, Larry M. Jordan, Jon H. Kaas, Andres M. Kanner, Noomi Katz, Matthew S. Kayser, Annmarie Kelleher, Gerd Kempermann, Timothy E. Kennedy, Jürg Kesselring, Fary Khan, Rachel Kizony, Jeffery D. Kocsis, Boudewijn J. Kollen, Hubertus Köller, John W. Krakauer, Hermano I. Krebs, Gert Kwakkel, Bradley Lang, Catherine E. Lang, Helmar C. Lehmann, Angelo C. Lepore, Glenn S. Le Prell, Mindy F. Levin, Joel M. Levine, David A. Low, Marilyn MacKay-Lyons, Jeffrey D. Macklis, Margaret Mak, Francine Malouin, William C. Mann, Paul D. Marasco, Christopher J. Mathias, Laura McClure, Jan Mehrholz, Lorne M. Mendell, Robert H. Miller, Carol Milligan, Beth Mineo, Simon W. Moore, Jennifer Morgan, Charbel E-H. Moussa, Martin Munz, Randolph J. Nudo, Joseph J. Pancrazio, Theresa Pape, Alvaro Pascual-Leone, Kristin M. Pearson-Fuhrhop, P. Hunter Peckham, Tamara L. Pelleshi, Catherine Verrier Piersol, Thomas Platz, Marcus Pohl, Dejan B. Popović, Andrew M. Poulos, Maulik Purohit, Hui-Xin Qi, Debbie Rand, Mahendra S. Rao, Josef P. Rauschecker, Aimee Reiss, Carol L. Richards, Keith M. Robinson, Melvyn Roerdink, John C. Rosenbek, Serge Rossignol, Edward S. Ruthazer, Arash Sahraie, Krishnankutty Sathian, Marc H. Schieber, Brian J. Schmidt, Michael E. Selzer, Mijail D. Serruya, Himanshu Sharma, Michael Shifman, Jerry Silver, Thomas Sinkjær, George M. Smith, Young-Jin Son, Tim Spencer, John D. Steeves, Oswald Steward, Sheela Stuart, Austin J. Sumner, Chin Lik Tan, Robert W. Teasell, Gareth Thomas, Aiko K. Thompson, Richard F. Thompson, Wesley J. Thompson, Erika Timar, Ceri T. Trevethan, Christopher Trimby, Gary R. Turner, Mark H. Tuszynski, Erna A. van Niekerk, Ricardo Viana, Difei Wang, Anthony B. Ward, Nick S. Ward, Stephen G. Waxman, Patrice L. Weiss, Jörg Wissel, Steven L. Wolf, Jonathan R. Wolpaw, Sharon Wood-Dauphinee, Ross D. Zafonte, Binhai Zheng, Richard D. Zorowitz
- Edited by Michael Selzer, Stephanie Clarke, Leonardo Cohen, Gert Kwakkel, Robert Miller, Case Western Reserve University, Ohio
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- Book:
- Textbook of Neural Repair and Rehabilitation
- Published online:
- 05 May 2014
- Print publication:
- 24 April 2014, pp ix-xvi
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Contributor affiliations
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- By Frank Andrasik, Melissa R. Andrews, Ana Inés Ansaldo, Evangelos G. Antzoulatos, Lianhua Bai, Ellen Barrett, Linamara Battistella, Nicolas Bayle, Michael S. Beattie, Peter J. Beek, Serafin Beer, Heinrich Binder, Claire Bindschaedler, Sarah Blanton, Tasia Bobish, Michael L. Boninger, Joseph F. Bonner, Chadwick B. Boulay, Vanessa S. Boyce, Anna-Katharine Brem, Jacqueline C. Bresnahan, Floor E. Buma, Mary Bartlett Bunge, John H. Byrne, Jeffrey R. Capadona, Stefano F. Cappa, Diana D. Cardenas, Leeanne M. Carey, S. Thomas Carmichael, Glauco A. P. Caurin, Pablo Celnik, Kimberly M. Christian, Stephanie Clarke, Leonardo G. Cohen, Adriana B. Conforto, Rory A. Cooper, Rosemarie Cooper, Steven C. Cramer, Armin Curt, Mark D’Esposito, Matthew B. Dalva, Gavriel David, Brandon Delia, Wenbin Deng, Volker Dietz, Bruce H. Dobkin, Marco Domeniconi, Edith Durand, Tracey Vause Earland, Georg Ebersbach, Jonathan J. Evans, James W. Fawcett, Uri Feintuch, Toby A. Ferguson, Marie T. Filbin, Diasinou Fioravante, Itzhak Fischer, Agnes Floel, Herta Flor, Karim Fouad, Richard S. J. Frackowiak, Peter H. Gorman, Thomas W. Gould, Jean-Michel Gracies, Amparo Gutierrez, Kurt Haas, C.D. Hall, Hans-Peter Hartung, Zhigang He, Jordan Hecker, Susan J. Herdman, Seth Herman, Leigh R. Hochberg, Ahmet Höke, Fay B. Horak, Jared C. Horvath, Richard L. Huganir, Friedhelm C. Hummel, Beata Jarosiewicz, Frances E. Jensen, Michael Jöbges, Larry M. Jordan, Jon H. Kaas, Andres M. Kanner, Noomi Katz, Matthew S. Kayser, Annmarie Kelleher, Gerd Kempermann, Timothy E. Kennedy, Jürg Kesselring, Fary Khan, Rachel Kizony, Jeffery D. Kocsis, Boudewijn J. Kollen, Hubertus Köller, John W. Krakauer, Hermano I. Krebs, Gert Kwakkel, Bradley Lang, Catherine E. Lang, Helmar C. Lehmann, Angelo C. Lepore, Glenn S. Le Prell, Mindy F. Levin, Joel M. Levine, David A. Low, Marilyn MacKay-Lyons, Jeffrey D. Macklis, Margaret Mak, Francine Malouin, William C. Mann, Paul D. Marasco, Christopher J. Mathias, Laura McClure, Jan Mehrholz, Lorne M. Mendell, Robert H. Miller, Carol Milligan, Beth Mineo, Simon W. Moore, Jennifer Morgan, Charbel E-H. Moussa, Martin Munz, Randolph J. Nudo, Joseph J. Pancrazio, Theresa Pape, Alvaro Pascual-Leone, Kristin M. Pearson-Fuhrhop, P. Hunter Peckham, Tamara L. Pelleshi, Catherine Verrier Piersol, Thomas Platz, Marcus Pohl, Dejan B. Popović, Andrew M. Poulos, Maulik Purohit, Hui-Xin Qi, Debbie Rand, Mahendra S. Rao, Josef P. Rauschecker, Aimee Reiss, Carol L. Richards, Keith M. Robinson, Melvyn Roerdink, John C. Rosenbek, Serge Rossignol, Edward S. Ruthazer, Arash Sahraie, Krishnankutty Sathian, Marc H. Schieber, Brian J. Schmidt, Michael E. Selzer, Mijail D. Serruya, Himanshu Sharma, Michael Shifman, Jerry Silver, Thomas Sinkjær, George M. Smith, Young-Jin Son, Tim Spencer, John D. Steeves, Oswald Steward, Sheela Stuart, Austin J. Sumner, Chin Lik Tan, Robert W. Teasell, Gareth Thomas, Aiko K. Thompson, Richard F. Thompson, Wesley J. Thompson, Erika Timar, Ceri T. Trevethan, Christopher Trimby, Gary R. Turner, Mark H. Tuszynski, Erna A. van Niekerk, Ricardo Viana, Difei Wang, Anthony B. Ward, Nick S. Ward, Stephen G. Waxman, Patrice L. Weiss, Jörg Wissel, Steven L. Wolf, Jonathan R. Wolpaw, Sharon Wood-Dauphinee, Ross D. Zafonte, Binhai Zheng, Richard D. Zorowitz
- Edited by Michael E. Selzer, Stephanie Clarke, Leonardo G. Cohen, Gert Kwakkel, Robert H. Miller, Case Western Reserve University, Ohio
-
- Book:
- Textbook of Neural Repair and Rehabilitation
- Published online:
- 05 June 2014
- Print publication:
- 24 April 2014, pp ix-xvi
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- Chapter
- Export citation
A new “chain” of events: polymers in the Powder Diffraction FileTM (PDF®)
- Stacy D. Gates, Thomas N. Blanton, Timothy G. Fawcett
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- Journal:
- Powder Diffraction / Volume 29 / Issue 2 / June 2014
- Published online by Cambridge University Press:
- 09 April 2014, pp. 102-107
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Developments in X-ray analysis, and advances in scientific research, have dramatically influenced the types of data now considered suitable for inclusion in the Powder Diffraction FileTM (PDF®). Initially, the PDF was geared towards the identification of unknown crystalline materials by comparison of d-spacings and peak intensities. Today, the International Centre for Diffraction Data (ICDD) maintains and continuously enhances the quality and content of the PDF database to better provide customers and scientists with a comprehensive reference source that supports their needs, and interests. The events that initially led to the inclusion of crystalline polymer data to the PDF have recently been amended to also encompass semi-crystalline and amorphous polymeric materials as well. This paper discusses the resultant updates being made to the PDF in support of this new data form, and also highlights several features and benefits of providing this data to PDF users.
Study of Model Copper-Based Catalysts by Simultaneous Differential Scanning Calorimetry, X-Ray Diffraction and Mass Spectrometry
- Robert A. Newman, Joseph A. Blazy, Timothy G. Fawcett, Larry F. Whiting, Robert A. Stowe
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- Journal:
- MRS Online Proceedings Library Archive / Volume 111 / 1987
- Published online by Cambridge University Press:
- 28 February 2011, 405
- Print publication:
- 1987
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Recently, a new materials characterization instrument and technique employing simultaneous differential scanning calorimetry/X-ray diffraction/mass spectrometry (DSC/XRD/MS) have been developed at Dow. Use of this technology can be illlustrated by the study of various materials such as polymers, organics/pharmaceuticals, inorganics, and catalysts.
Presented here is the use of the DSC/XRD/MS instrument to study the thermostructural behavior of four model copper-based catalyst systems during activation and regeneration. The instrument allows simultaneous generation of thermal, structural and chemical data in real-time during temperature programmed analysis and provides useful insights into the chemical and physical processes occurring. In addition, the calorimetry data yield qualititative information on the magnitude and rate of heat flow, while the diffraction data provide structural dynamics of reduction, oxidation and crystallite growth.
The results of this study conclusively show cuprous oxide as an intermediate in the reduction of the copper oxide portion of each of the model catalysts. However, such features as the onset temperature and copper surface area varied widely among the four catalysts in response to the same chemical event conducted under similar experimental conditions. On the other hand, oxidation runs on the reduced catalysts were all similar to each other, first producing cuprous oxide from copper metal over a broad range of temperature, followed by the oxidation of cuprous oxide to copper oxide at even higher temperatures.