A time-resolved powder diffraction study of the crystallisation of porous metal organic framework materials with the CPO-27 structure ([M2(dhtp)(H2O)2]·8H2O where, dhtp=2,5-dioxoterephthalate) using the energy dispersive X-ray diffraction method is described. Crystallisation under solvothermal conditions is performed between 70 - 110 °C from clear solutions of metal salts (M=Co2+ or Ni2+) and 2,5-dihydroxyterephthalic acid in a mixture of THF-water in sealed reaction vessels, using both conventional and microwave heating. Integration of Bragg peak areas with time provides accurate crystallisation curves, which are modelled using the method of Gualtieri to determine rate constants for nucleation and for growth and then, by Arrhenius analysis, activation energies. Crystallisation is determined to be one-dimensional, consistent with the elongated morphology of the crystals produced in these reactions. With conventional heating the Co-containing CPO-27 crystallises more rapidly than the isostructural Ni-containing analogue and analysis of the kinetic parameters would suggest a complex multi-step crystallisation process. The effect of microwave heating is upon activation energies: the values for both nucleation and for crystal growth are lowered compared to reactions using conventional heating.

Artifacts are the nemesis of trace element analysis in electron-excited energy dispersive X-ray spectrometry. Peaks that result from nonideal behavior in the detector or sample can fool even an experienced microanalyst into believing that they have trace amounts of an element that is not present. Many artifacts, such as the Si escape peak, absorption edges, and coincidence peaks, can be traced to the detector. Others, such as secondary fluorescence peaks and scatter peaks, can be traced to the sample. We have identified a new sample-dependent artifact that we attribute to Compton scattering of energetic X-rays generated in a small feature and subsequently scattered from a low atomic number matrix. It seems likely that this artifact has not previously been reported because it only occurs under specific conditions and represents a relatively small signal. However, with the advent of silicon drift detectors and their utility for trace element analysis, we anticipate that more people will observe it and possibly misidentify it. Though small, the artifact is not inconsequential. Under some conditions, it is possible to mistakenly identify the Compton scatter artifact as approximately 1% of an element that is not present.

Two recent developments in X-ray spectrometer technology provide dramatic improvements in analytical capabilities that impact the frontiers of electron microscopy. Silicon drift detectors (SDD) use the same physics as silicon (lithium) energy dispersive spectrometers [Si(Li) EDS] but differ in design: only 10% of the thickness of the Si(Li) EDS with an anode area below 0.1 mm2 and a complex rear surface electrode pattern that creates a lateral internal charge collection field. The SDD equals or betters the Si(Li) EDS in most measures of performance. For output versus input count rate, the SDD exceeds the Si(Li) EDS by a factor of 5 to 10 for the same resolution. This high throughput can benefit analytical measurements that are count limited, such as X-ray mapping and trace measurements. The microcalorimeter EDS determines the X-ray energy by measuring the temperature rise in a metal absorber. Operating at 100 mK, the microcalorimeter EDS achieves resolution of 2–5 eV over a photon energy range of 200 eV to 10 keV in energy dispersive operation, eliminating most peak interference situations and providing high peak-to-background to detect low fluorescence yield peaks. Chemical bonding effects on low energy (<2 keV) peak shapes can be measured.