A combination of X-ray diffraction and computational techniques can determine unknown crystal structures in powder mixtures
The characterization of individual components in an unknown crystalline powder mixture is a challenge that has eluded scientists for many years. Now, A*STAR researchers have for the first time invented a methodology to accurately determine the crystal structures present in such mixtures1.
A new method that combines X-ray diffraction with computational analysis can be used to measure mixtures of unknown solids and identify their individual components.
© 2014 A*STAR Institute of Chemical and Engineering Sciences
Powder X-ray diffraction (PXRD) is a powerful tool used to determine the structure of crystalline solids. Every solid has its own unique crystal structure which, when hit by X-rays, produces a unique diffraction pattern — a ‘fingerprint’ from which the solid can then be identified and characterized through computational analysis.
However, traditional PXRD works best with pure single-component powders; mixed powders of unknown solids are far more difficult to analyze because the diffraction patterns overlap and are difficult to separate. Another complication is that individual solids can produce slightly different diffraction patterns depending on how the crystals are shaped and orientated in the powder samples.
Marc Garland and co-workers at the A*STAR Institute of Chemical and Engineering Sciences in Singapore have developed a new methodology, the PXRD-BTEM-Rietveld method, which combines two existing techniques to determine the individual crystal structures in a powder mixture.
“Many analytical problems in the chemical sciences involve mixtures of unknown solids,” explains Garland. “The extension of PXRD analysis to these mixtures opens up a myriad of new possibilities for the experimentalist because a purified single-component sample is no longer needed.”
First, Garland and his team used PXRD to obtain diffraction datasets from pre-prepared mixtures of several different powders. They then used their own algorithm, called band-target entropy minimization (BTEM), to sift through the entire dataset, looking for the simplest underlying patterns and to untangle overlapping diffraction patterns.
“BTEM is a blind separation technique,” explains Garland. “By searching for the simplest patterns — those with the smoothest profiles and the least signal disorder — we obtain accurate estimates of each pure component’s diffraction pattern.”
Garland and his team then used computational structure determination, including so-called Rietveld refinement, to obtain the crystal structures for each solid. This allowed the researchers to characterize the unknown components in the mixtures.
“One example of an application for our new technique could be investigating polymorphism in pharmaceuticals,” says Garland. “Each polymorphic pharmaceutical solid has a unique diffraction pattern resulting from its crystal structure, and it is incredibly important to the pharmaceutical industry to identify these from mixtures.”
The researchers plan to further refine their methodology, and hope to eliminate the problem of measuring irregularities due to crystal orientation.
Schreyer, M., Guo, L., Thirunahari, S., Gao, F. & Garland, M. Simultaneous determination of several crystal structures from powder mixtures: The combination of powder X-ray diffraction, band-target entropy minimization and Rietveld methods. Journal of Applied Crystallography 47, 659–667 (2014).
A*STAR Research | ResearchSEA
A better way to weigh millions of solitary stars
15.12.2017 | Vanderbilt University
A chip for environmental and health monitoring
15.12.2017 | Friedrich-Alexander-Universität Erlangen-Nürnberg
DNA molecules that follow specific instructions could offer more precise molecular control of synthetic chemical systems, a discovery that opens the door for engineers to create molecular machines with new and complex behaviors.
Researchers have created chemical amplifiers and a chemical oscillator using a systematic method that has the potential to embed sophisticated circuit...
MPQ scientists achieve long storage times for photonic quantum bits which break the lower bound for direct teleportation in a global quantum network.
Concerning the development of quantum memories for the realization of global quantum networks, scientists of the Quantum Dynamics Division led by Professor...
Researchers have developed a water cloaking concept based on electromagnetic forces that could eliminate an object's wake, greatly reducing its drag while...
Tiny pores at a cell's entryway act as miniature bouncers, letting in some electrically charged atoms--ions--but blocking others. Operating as exquisitely sensitive filters, these "ion channels" play a critical role in biological functions such as muscle contraction and the firing of brain cells.
To rapidly transport the right ions through the cell membrane, the tiny channels rely on a complex interplay between the ions and surrounding molecules,...
The miniaturization of the current technology of storage media is hindered by fundamental limits of quantum mechanics. A new approach consists in using so-called spin-crossover molecules as the smallest possible storage unit. Similar to normal hard drives, these special molecules can save information via their magnetic state. A research team from Kiel University has now managed to successfully place a new class of spin-crossover molecules onto a surface and to improve the molecule’s storage capacity. The storage density of conventional hard drives could therefore theoretically be increased by more than one hundred fold. The study has been published in the scientific journal Nano Letters.
Over the past few years, the building blocks of storage media have gotten ever smaller. But further miniaturization of the current technology is hindered by...
11.12.2017 | Event News
08.12.2017 | Event News
07.12.2017 | Event News
15.12.2017 | Power and Electrical Engineering
15.12.2017 | Materials Sciences
15.12.2017 | Life Sciences