Design and implementation of a differential scanning calorimeter for the simultaneous measurement of small angle neutron scattering

For almost 30 years, at synchrotron facilities, it has been possible to perform small-angle x-ray scattering experiments whilst simultaneously measuring differential scanning calorimetry (DSC). However, a range of challenges exist to enable the collection of simultaneous small-angle neutron scattering (SANS) and DSC data associated not only with intrinsic flux limitations but also scattering geometry and thermal control. The development of a DSC (temperature range ca. −150 °C to 500 °C) suitable for SANS is detailed here and its successful use is illustrated with combined measurements on a binary blend of normal alkanes in which one component has been deuterium labelled.

[1]  Simultaneous measurements of small angle X-ray scattering, wide angle X-ray scattering and heat exchange during crystallization and melting of polymers , 1993 .

[2]  E. Gilbert The stability of binary alkane blends , 1999 .

[3]  Terry Noakes,et al.  ‘Quokka’—the small-angle neutron scattering instrument at OPAL , 2006 .

[4]  Elliot P. Gilbert Incommensurate modulation in phase separating binary paraffin mixtures , 1999 .

[5]  A. Donald,et al.  Gelatinisation of starch: a combined SAXS/WAXS/DSC and SANS study , 1998 .

[6]  Kiyotaka Sato,et al.  Simultaneous synchrotron radiation X-ray diffraction-DSC analysis of melting and crystallization behavior of trilauroylglycerol in nanoparticles of oil-in-water emulsion , 2003 .

[7]  Ingo Berndt,et al.  Doubly Temperature Sensitive Core−Shell Microgels , 2003 .

[8]  Philip A. Reynolds,et al.  Microphase separation in graphite-adsorbed paraffin solid solutions , 1996 .

[9]  Philip A. Reynolds,et al.  SMALL ANGLE X-RAY SCATTERING FROM PHASE SEPARATING N-PARAFFIN BINARY MIXTURES , 1997 .

[10]  E. Staples,et al.  A Couette shear flow cell for small-angle neutron scattering studies , 1990 .

[11]  April S. Brown,et al.  n-Paraffin solid solutions: modification of phase separation with carbon number , 1996 .

[12]  Tushar H. Gore,et al.  Self-Assembly of Model Collagen Peptide Amphiphiles , 2001 .

[13]  Anthony J. Ryan,et al.  The combination of thermal analysis and time-resolved X-ray techniques: a powerful method for materials characterization , 1995 .

[14]  T. Gutberlet,et al.  Neutron Scattering in Biology , 2006 .

[15]  A. Ryan,et al.  Sample environments and techniques combined with small angle X-ray scattering. , 1998, Advances in colloid and interface science.

[16]  Philip A. Reynolds,et al.  Microphase separation kinetics in n-alkane mixtures , 1999 .

[17]  Thomas P. Russell,et al.  Simultaneous differential scanning calorimetry and small-angle x-ray scattering† , 1985 .

[18]  E. Lang,et al.  Phase Separation in the Organic Solid State: The Influence of Quenching Protocol in Unstable n-Alkane Blends , 2005 .

[19]  R. G. Snyder,et al.  Microphase separation in paraffin solid solutions , 1990 .

[20]  S. R. Olsen,et al.  An in situ rapid heat–quench cell for small-angle neutron scattering , 2008 .

[21]  I. Grillo,et al.  Applications of stopped-flow in SAXS and SANS , 2009 .