scholarly journals Evaluation of microflow configurations for scale inhibition and serial X-ray diffraction analysis of crystallization processes

Lab on a Chip ◽  
2020 ◽  
Vol 20 (16) ◽  
pp. 2954-2964
Author(s):  
Mark A. Levenstein ◽  
Yi-Yeoun Kim ◽  
Liam Hunter ◽  
Clara Anduix-Canto ◽  
Carlos González Niño ◽  
...  

Exploration of crystal growth in microchannels led to effective scale inhibition, enabling time-resolved injector-based serial crystallography-on-a-chip.

2011 ◽  
Vol 248 (11) ◽  
pp. 2449-2453 ◽  
Author(s):  
Périne Landois ◽  
Stéphan Rouziére ◽  
Mathieu Pinault ◽  
Dominique Porterat ◽  
Cristian Mocuta ◽  
...  

2017 ◽  
Vol 9 (41) ◽  
pp. 36392-36399 ◽  
Author(s):  
Jun Luo ◽  
Francisco Javier Martinez-Casado ◽  
Olivier Balmes ◽  
Jiaojiao Yang ◽  
Cecilia Persson ◽  
...  

2019 ◽  
Vol 26 (3) ◽  
pp. 774-784 ◽  
Author(s):  
Sebastian J. Gurgul ◽  
Gabriel Seng ◽  
Gareth R. Williams

The conversion of CaSO4·0.5H2O to CaSO4·2H2O is of great importance industrially, being the reaction behind plasterboard production and the setting of medical plasters. A detailed kinetic and mechanistic study of this process was conducted using time-resolved synchrotron X-ray diffraction in this work. The CaSO4·2H2O product is very similar regardless of whether the α- or β-form of CaSO4·0.5H2O is used as the starting material, but the reaction process is very different. The induction time is usually shorter for α-CaSO4·0.5H2O than β-CaSO4·0.5H2O, and a greater conversion percentage is observed with the former (although in neither case does the reaction proceed to 100% completion). The temperature of the system, widely used in industry as an indirect measure of the extent of the hydration process, is found to be a poor proxy for this, with the maximum temperature reached well before the reaction is complete. The Avrami–Erofe'ev and Gualtieri models could both be fitted to the experimental data, with the fits being substantially closer in the case of α-CaSO4·0.5H2O. The rate of reaction in the Avrami model tends to increase with the amount of gypsum seeds added to accelerate the process, and the importance of nucleation declines. The Gualtieri analysis suggested that the rate of nucleation increases substantially with the amount of seeds added, while there are less distinct changes in the rate of crystal growth. At low seed concentrations (<0.5% w/w) the rate of crystal growth is greater than the rate of nucleation, but at concentrations above 0.5% w/w nucleation is faster. These findings represent the first synchrotron study of the conversion of CaSO4·0.5H2O to CaSO4·2H2O, and will be of importance to gypsum producers globally.


2018 ◽  
Vol 33 (4) ◽  
pp. 287-297 ◽  
Author(s):  
Kristina M. Peterson ◽  
Peter J. Heaney ◽  
Jeffrey E. Post

Synchrotron X-ray diffraction was used to monitor the hydrothermal precipitation of akaganeite (β-FeOOH) and its transformation to hematite (Fe2O3) in situ. Akaganeite was the first phase to form and hematite was the final phase in our experiments with temperatures between 150 and 200 °C. Akaganeite was the only phase that formed at 100 °C. Rietveld analyses revealed that the akaganeite unit-cell volume contracted until the onset of dissolution, and subsequently expanded. This reversal at the onset of dissolution was associated with a substantial and rapid increase in occupancy of the Cl site, perhaps by OH− or Fe3+. Rietveld analyses supported the incipient formation of an OH-rich, Fe-deficient hematite phase in experiments between 150 and 200 °C. The inferred H concentrations of the first crystals were consistent with “hydrohematite.” With continued crystal growth, the Fe occupancies increased. Contraction in both a- and c-axes signaled the loss of hydroxyl groups and formation of a nearly stoichiometric hematite.


2009 ◽  
Vol 104 (2) ◽  
pp. 105-109 ◽  
Author(s):  
Toru INOUE ◽  
Isamu YOSHIMI ◽  
Akihiro YAMADA ◽  
Takumi KIKEGAWA

2019 ◽  
Vol 75 (10) ◽  
pp. 937-946 ◽  
Author(s):  
Rebecka Andersson ◽  
Cecilia Safari ◽  
Petra Båth ◽  
Robert Bosman ◽  
Anastasya Shilova ◽  
...  

Serial crystallography is having an increasing impact on structural biology. This emerging technique opens up new possibilities for studying protein structures at room temperature and investigating structural dynamics using time-resolved X-ray diffraction. A limitation of the method is the intrinsic need for large quantities of well ordered micrometre-sized crystals. Here, a method is presented to screen for conditions that produce microcrystals of membrane proteins in the lipidic cubic phase using a well-based crystallization approach. A key advantage over earlier approaches is that the progress of crystal formation can be easily monitored without interrupting the crystallization process. In addition, the protocol can be scaled up to efficiently produce large quantities of crystals for serial crystallography experiments. Using the well-based crystallization methodology, novel conditions for the growth of showers of microcrystals of three different membrane proteins have been developed. Diffraction data are also presented from the first user serial crystallography experiment performed at MAX IV Laboratory.


1996 ◽  
Vol 35 (Part 1, No. 10) ◽  
pp. 5426-5427 ◽  
Author(s):  
Hiroyuki Okada ◽  
Miki Shibata ◽  
Hiroyoshi Onnagawa

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.


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