Time-resolved synchrotron X-ray

Dhavan, G.M. Chance, M.R. Brenowitz, M. Kinetics analysis of DNA-protein interactions by time-resolved synchrotron X-ray footprinting. Kinet. Anal. Macromol. 2003, 75-86. 

Chance, M.R. Sclavi, B. Woodson, S.A. Brenowitz, M. Examining the conformational dynamics of macromolecules with time-resolved synchrotron X-ray footprintmg . Structure 1997, 5, 865—869. 

Sclavi, B., Woodson, S., Sulhvan, M., Chance, M. R., and Brenowitz, M. (1997). Time-resolved synchrotron X-ray footprinting , a new approach to the study of nucleic acid structure and function Application to protein-DNA interactions and RNA folding. J. Mol. Biol. 266, 144-159. 

Figure 22.6. (A) Temperature variation profile during, and (B) three-dimensional plots of the results obtained from, a time-resolved synchrotron X-ray diffraction experiment on SOS (1,3-distearoyl-2-oleoyl-.sn-glycerol) without annealing, a and (3 polymorphic forms LC1 liquid crystalline structure 1. (Reproduced with permission from Sato et al., 1999.)...

From the analysis of the data in the LIPID AT database (41), more than 150 different methods and method modifications have been used to collect data related to the lipid phase transitions. Almost 90% of the data is accounted for by less than 10 methods. Differential scaiming calorimetry strongly dominates the field with two thirds of all phase transition records. From the other experimental techniques, various fluorescent methods account for 10% of the information records. X-ray diffraction, nuclear magnetic resonance (NMR), Raman spectroscopy, electron spin resonance (ESR), infrared (IR) spectroscopy, and polarizing microscopy each contribute to about or less than 2-3% of the phase transition data records in the database. Especially useful in gaining insight into the mechanism and kinetics of lipid phase transitions has been time-resolved synchrotron X-ray diffraction (62,78-81). 

Fig. 1. Simultaneous DSC/WAXS/SAXS design. Experimental setup of the microcalorimeter cell in the time-resolved synchrotron X-ray diffraction environment The cell is positioned with sample-containing capillary perpendicular to the beam in such a way that the diffraction patterns are recorded in the vertical plane including the beam by one or two one-dimensional proportional detectors (Position Sensitive Linear Detector 1 and LD2). Counting Electronic (Counting Elect.), Nanovoltmeter (mVter), and Temperature Controller (T Ctrl) are all monitored by the same PC Computer (PC Comp.). Temperature-Controlled Bath (TCB) is kept at constant temperature (e.g., 20°C). Figure is adapted from Reference 3.

Lasocha W, Schenk H (1997) A simplified, textirre-based method for intensity determination of overlapping reflectiorts in powder diffraction. J Appl Crystallogr 30 561-564 Lee Y, Cahill C, Hanson J, Parise JB, Carr S, Myrick ML, Preckwinkel UV, Phillips JC (1999) Characterization of K -ion exchange into Na-MAX using time resolved synchrotron X-ray powder diffraction and rietveld refinement. In 12th Int l Zeolite Assoc Meeting, Baltimore, Maryland, IV 2401-2408... 

Ralston CY, Sclavi B, SuUivan M, et al. Time-resolved synchrotron X-ray footprinting and its application to RNA folding. Methods Enzymol. 2000 317 353-368. von Sonntag C. The Chemical Basis ofRjodiation Biology. London Taylor Francis 1987. Pogozelski WK, McNeese TJ, TuUius TD. What species is responsible for strand scission in the reaction of Fe EDTA and H2O2 with DNA J Am Chem Soc. 1995 117 6428-6433. 

Schneider, K et al. (2006). The Study of Cavitation in HDPE Using Time Resolved Synchrotron X-ray Scattering During Tensile Deformation, Macromolecular Symposia Vol.236 (2006), 241-248... 

Y. Akpalu, L. Kielhorn, B.S. Hsiao, R.S. Stein, T.P. RusseU, J. van Egmond and M. Muthukumar, Structure development during crystaUization of homogeneous copolymers of ethene and 1-octene Time-resolved synchrotron X-ray and SALS measurements, Macromolecules 32, 765-770 (1999). 

Coppens P, Gerlits O, Vorontsov II et al (2004) A very large Rh-Rh bond shortening on excitation of the [Rh2(l,8-diisocyano-p-menthane)4] ion by time-resolved synchrotron X-ray diffraction. Chem Comm 2144-2145... 

Joe Wong, T, Ressler and J.W. Elmer, Dynamics of phase transformations and microstructure evolution in carbon-manganese steel arc welds using time-resolved synchrotron x-ray diffraction, J. Synchrotron Rad. (2002) submitted. 

An interesting experiment of real-time growth process of LAO/STO was performed by time-resolved surface X-ray diffraction (SXRD) on the beamline 33-ID at the advanced photon source (APS) synchrotron in Argonne, showing the formation and evolution of the LAO epitaxial layers [62]. 

Time-Resolved Crystallography. Time-resolved crystallography (TC) uses an intense synchrotron X-ray source and Laue data collection techniques to greatly reduce crystallographic exposure times. Normal time resolution for X-ray... 

Time-resolved x-ray crystallography (TC) is a more recent advanced application of x-ray crystallography. It uses an intense synchrotron x-ray source and data collection methods to reduce crystallographic exposure times. This allows multiple exposures to be taken over time at near-physiological, crystalline conditions to determine the structures of intermediates. A typical problem with this method is that the existence of the intermediates is brief, resulting in difficulty in interpreting the resulting electron density maps. 

Microscopic time-resolved measurements of the hydrate phase during gas hydrate formation, decomposition, and inhibition began only in the mid-1990s. These techniques include in situ synchrotron x-ray diffraction (Koh et al., 1996 Klapproth et al., 2003 Uchida et al., 2003), neutron diffraction (Henning et al., 2000 Koh et al., 2000 Halpern et al., 2001 Staykova et al., 2003), Raman spectroscopy (Subramanian and Sloan, 2002 Komai et al., 2004), and NMR spectroscopy (Moudrakovski et al., 2001 Kini et al., 2004 Gupta et al., 2007). 

Figure 17. Time-resolved synchrotron radiation X-ray diffraction patterns of concentration ratio LLL/PPP = 60/40. At left is the temperature change with time (unit nm).

Detectors used for time resolved non-crystalline diffraction experiments on a synchrotron X-ray source should have most if not all of the following characteristics ... 

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