Microscopy & Microtechniques 83 Temperature Controlled Stage Employed in Freeze Drying Characterisation


The University of Iowa Pharmaceuticals (UIP) has been developing formulations, manufacturing products, and conducting analytical testing in compliance with current Good Manufacturing Practices (cGMPs) for over 30 years. The facility is the only one of its kind offering the range and scope of services needed by commercial clients. One area of interest is the understanding of lyophilisation processes. Key to this is the characterisation instrumentation from Biopharma Technology Limited. Two systems are in use: The Lyotherm 2 provides integrated Differential Thermal Analyser (DTA) and electrical impedance


(Zsinφ) capability in a single instrument. The Lyotherm 2 is designed to measure glass transition (Tg'), eutectic (Teu) and melting (Tm) temperatures relevant to freeze-drying formulations. The Lyostat 2 is a fully integrated freeze-drying microscope, which incorporates a Linkam THMS 600 cryo temperature stage. This enables critical events such as collapse and melting to be observed in situ, as well as characteristics such as skin or crust formation to be observed and identified. The coupled Lyostat 2 and Lyotherm 2 units provide valuable information for both formulation and cycle development processes. With UIP's in-house expertise in lyophilisation, this combination will allow quicker and more efficient development of lyophilisation cycles.


The team is led by Professor Lee Kirsch of the College of Pharmacy. One of his team describes the main work with the Lyostat 2 system. “We use the system to find out the collapse temperature for various clients freeze drying formulations.” Until the arrival of the Lyostat 2, determining the collapse temperature would take hours in the lab in an attempt to understand the critical temperatures needed to produce the best product. The ability to provide accurate thermal characterisation right down to -196°C significantly reduced the time and complexity in the process enabling scientists to determine these key temperatures and so create the best product quickly and simply.


Circle no. 251 Modular Upright Research Microscopes for Bioscience and Medical Research


The Nikon evolution in upright biological microscopes has advanced with the new Eclipse Ni series. Using core technology from Nikon’s renowned Eclipse Ti inverted research microscope, the Eclipse Ni series offers multi-mode system expandability to meet the imaging needs of bioscience and medical research on one platform. The new Ni range also provides superior optical performance with new CFI Plan Apochromat Lambda series objectives, and the flexibility of assisted observation by motorisation. The range comprises the fully motorised Eclipse Ni-E flagship model with focusing nosepiece or focusing stage options, and the manual Eclipse Ni-U with motorisation upgrade capability.


Nikon’s highly acclaimed proprietary stratum structure in the Ni series opens up a vast range of imaging possibilities that can be upgraded at any time. Both models support research into the reactions and changes of stimulated cells with a newly developed photoactivation unit, a first for upright microscopes. The Eclipse Ni-E is also configurable for multiphoton imaging, as well as offering the option of fixed-stage configurations to meet the demands of experiments such as in vivo imaging for cardio vascular and neuroscience research applications.


The new Eclipse Ni microscopes use the latest version 4.0 release of NIS-Elements software enabling microscope, camera and confocal control, thereby removing the need for a laboratory to rely on separate software. Image acquisition and analysis is improved with over 100 new functions.


Superior optical performance is ensured through Nikon’s new CFI Plan Apochromat Lambda series objectives with Nano Crystal Coat technology. Transmission and chromatic aberration correction have been improved throughout the wide range of visible to near IR wavelengths (950nm), providing bright, high-contrast, high signal-to-noise ratio and multi-colour fluorescence images with no perceivable focus shift when used with any wavelength. A comprehensive range of high speed, motorised accessories, specifically configured according to application, augment the improved features to meet all research requirements.


Circle no. 252 Razor-sharp High Definition Thermal Imaging


The FLIR™ SC660 thermal imaging camera offers superior thermal and visual image quality, spot size resolution and temperature measurement accuracy. It is ideal for all types of engineering, laboratory or field application that may benefit from thermal analysis. The SC660 infrared camera is a science-grade infrared camera with a host of advanced features. The SC660's high definition 640 x 480 pixel infrared detector delivers exceptional sensitivity, resolution and the image quality allowing it to measure even the most demanding applications. Proprietary FLIR Dynamic Detail Enhancement (DDE) technology further improves sharpness of thermal images. The SC660 also includes an integrated 3.2 megapixel digital video camera to aid in data presentation. Infrared and visual images can be stores in standard jpeg formats. A 5.6-inch widescreen LCD allows easy on-camera viewing of images. Using a FireWire interface the SC660 can transfer 14-bit radiometric data directly onto high capacity SD-cards or a PC for real-time analysis of captured images. The user can save a full 60 seconds of digital voice and embed it with each IR image allowing a full description of the target and measurement conditions to be recorded. In addition, data from the in-built GPS system can be used to exactly denote the camera's location at the time of making a reading.


Drawing upon its long experience in thermal imaging - FLIR has included in the SC660 an abundance of features that enhance its ease of use, productivity and safety of operation. The SC660's ergonomic magnesium housing is designed for rugged portability and meets the IP54 standard, thereby protecting internal parts from shock, vibration, dust and water splash. The SC660 can run up to three hours on a single fully charged battery.


Included with the SC660 is ThermaCAM® Researcher™ - a powerful Windows-based infrared software package that provides detailed precision analysis and


measurement tools for capturing, recording, and studying extremely high-speed thermal events. Circle no. 253


AFM used to Better Characterise Graphenes Properties


JPK Instruments reports on a keynote paper in Nano Letters where Dr Nikolai Severin and his co-workers from the group of Professor Jürgen P. Rabe have applied JPK's NanoWizard®


II Ultra system to improve their understanding of the properties of graphene.


Within this group is Dr Nikolai Severin, recently the lead author of a paper in Nano Letters, which shows the use of AFM in the study of graphenes. The electronic properties of graphenes depend sensitively on their deformation, and therefore strain-engineered graphene electronics is envisioned. In order to deform graphenes locally, the group has mechanically exfoliated single and few layer graphenes onto atomically flat mica surfaces covered with isolated double stranded plasmid DNA rings. Using scanning force microscopy in both contact and intermittent contact modes, they have found that the graphenes replicate the topography of the underlying DNA with high precision. The availability of macromolecules of different topologies, for example, programmable DNA patterns render this approach promising for new graphene based device designs. Furthermore, the encapsulation of single macromolecules offers new prospects for analytical scanning probe microscopy techniques.


Dr Severin has seen that graphene provides enhanced protection of DNA molecules to shear forces exerted during scanning force microscopy in contact mode. In addition, graphene will act as a surface protective layer against the ambient, for example, against oxidation, since it is impermeable to gases. Taking into account both the high electric conductivity of graphene and its extremely small thickness, this offers new opportunities for scanning probe microscopies and spectroscopies, such as scanning tunneling or tip enhanced Raman spectroscopy for analyses of both locally deformed graphene and confined molecules. Summarising,


Dr Severin said: "We have successfully demonstrated that topography of graphenes can be controlled with the precision down to single molecules." Circle no. 254


INTERNATIONAL LABMATE - JANUARY/FEBRUARY 2012


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