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Mechanochemistry has become a valuable method for the synthesis of new materials and molecules, with a particular strength for screening and preparing multicomponent crystals. In this work, two novel cocrystals of pyrazinamide (PZA) with pimelic acid (PA) were prepared mechanochemically. Their formation was monitored in real time by in situ synchrotron powder X-ray diffraction. Control over the polymorphic form was obtained through the selective choice of liquid additive via liquid assisted grinding. Slurry experiments and dispersion-corrected density functional theory calculations suggest that Form I is the thermodynamically stable form under ambient conditions. Upon aging, Form II converts to Form I. The stability of Form II upon aging was found to depend strongly on the milling duration, intensity, and material of the milling vessels. Longer or higher energy milling drastically increased the lifetime of the Form II product. For the first time, this work also demonstrates that the choice of milling jar can have a decisive effect on the aging stability of a bulk polymorphic powder. In contrast to material prepared in steel milling vessels, the preparation of Form II in Perspex (PMMA) vessels increased its lifetime 3-fold. These findings offer a new dimension to garnering control over mechanochemical cocrystallization and demonstrate the critical importance of the careful and timely ex situ screening of ball mill grinding reactions. This will be of importance for potential industrial applications of mechanochemical cocrystallization where understanding polymorph longevity is crucial for the development of a robust preparative protocol.
The far infrared refractive indices and the extinction coefficients of liquids can be obtained by means of spectroscopic ellipsometry in attenuated total reflection configuration. Such optical constants will contribute to a spectroscopic data base in the far infrared and terahertz spectral regions. The experimental implementation and the calibration procedure of the method are described in detail. The temperature dependency of the optical constants for water over a broad spectral range is exemplarily presented.
For the classification, safe handling and use of chemicals, special standardised test methods have been developed and are used worldwide. Safety experts must be able to fully rely on the precise execution of the respective laboratory tests and assessments. In this context interlaboratory tests (round robin tests, interlaboratory comparisons / intercomparisons) are a crucial element of both the further development and improvement of the methods and of a laboratory's quality system. Participation in interlaboratory tests is explicitly recommended by the standard ISO/IEC 17025. This document reports on the results of the interlaboratory test 2012-2013 on the test method EN 14522:2005 “Determination of the auto ignition temperature of gases and vapours“ / IEC 60079-201, part 7 ”Method of test for auto-ignition temperature”. The auto ignition temperature is an important safety characteristic for explosion protection and prevention. It is the basis for classifying substances and explosion protected equipment into temperature classes. Because safety characteristic data are not a pure substance constant but a figure which denotes a special property of the substance, the determination methods are standardised. Currently EN 14522 and IEC 60079-20-1, part 7 are under revision with the aim to combine both to a standard accepted worldwide. An important part of the standard is the laboratory’s verification of their apparatus and procedure. To base this forthcoming standard on reliable and up-to-date verification data an interlaboratory test appears as the method of choice. The verification data given in the recent issues of the standards are based on comparison measurements which date back to a long time ago and did not include automated apparatuses.
Short diffusion paths and high specific interfacial areas in microstructured devices can increase mass transfer rates and thus accelerate multiphase reactions. This effect can be intensified by the application of ultrasound. Herein, we report on the design and testing of a novel versatile setup for a continuous ultrasound-supported multiphase process in microstructured devices on a preparative scale. The ultrasonic energy is introduced indirectly into the microstructured device through pressurized water as transfer medium. First, we monitored the influence of ultrasound on the slug flow of a liquid/liquid two-phase system in a channel with a high-speed camera. To quantify the influence of ultrasound, the hydrolysis of p-nitrophenyl acetate was utilized as a model reaction. Microstructured devices with varying channel diameter, shape, and material were applied with and without ultrasonication at flow rates in the mL min-1 range. The continuous procedures were then compared and evaluated by performing a simplified life cycle assessment.
THz stand-off detection of explosives and other hazardous liquids in public areas becomes more and more relevant and with it the knowledge of their optical properties. We present here both the results of THz transmission spectroscopy measurements and spectroscopic ellipsometry measurements on liquids and their mixtures.
Dry friction and wear rates as under liquid lubrication of ceramic/carbon couples up to 450°C
(2004)
In a high temperature tribometer, stationary carbon has been tested against different rotating ceramics (SiC, Si3N4, Al2O3, WC-6Ni, MgO-ZrO2, (Ti, Mo)(C, N)) and stainless steel (DIN 1.4876). The rotating discs were grinded, polished and/or lapped. For most material combinations, the wear morphology is known from available literature. A transfer film with a typical wear pattern was found on the rotating disc. The combination of antimony graphite EK3245 against MgO-ZrO2 did not form carbonaceous transfer layer. Through advanced variation of the roughness up to Rpk=0.011?µm, the wear rate has been reduced to Kv 3.5×10-8?mm3/N?m at a stable coefficient of friction in a millirange of µ~0.008 for a sliding distance of 20.000?m.