Engineering topics

Snell, Edward

Publications and source records attributed to Snell, Edward.

4 records

NASA NTRS2006

Thermal Imaging Applied to Cryocrystallography: Cryocooling and Beam Heating (Part I)

Thermal imaging provides a non-invasive method to study both the cryocooling process and the heating due to the X-ray beam interaction with a sample. The method has been used successfully to image cryocooling in a number of experimental situations, i.e. cooling as a function of sample volume and as a function of cryostream orientation. Although there are experimental limitations to the method, it has proved a powerful technique to aid cryocrystallography development. Due to the rapid spatial temperature information provided about the sample it is also a powerful tool in the testing of mathematical models. Recently thermal imaging has been used to measure the temperature distribution on both a model and typical crystal samples illuminated with an X-ray beam produced by an undulator. A brief overview of thermal imaging and previous results will be presented. In addition, a detailed description of the calibration and experimental aspects of the beam heating measurements will be described. This will complement the following talk on the mathematical modeling and analysis of the results.

Snell, Edward↗

NASA NTRS2006

Beam Heating of Samples: Modeling and Verification

Energy absorbed from the X-ray beam by the sample requires cooling by forced convection (i.e. cryostream) to minimize temperature increase and the damage caused to the sample by the X-ray heating. In this presentation we will first review the current theoretical models and recent studies in the literature, which predict the sample temperature rise for a given set of beam parameters. It should be noted that a common weakness of these previous studies is that none of them provide actual experimental confirmation. This situation is now remedied in our investigation where the problem of x-ray sample heating is taken up once more. We have theoretically investigated, and at the same time, in addition to the numerical computations, performed experiments to validate the predictions. We have modeled, analyzed and experimentally tested the temperature rise of a 1 mm diameter glass sphere (sample surrogate) exposed to an intense synchrotron X-ray beam, while it is being cooled in a uniform flow of nitrogen gas. The heat transfer, including external convection and internal heat conduction was theoretically modeled using CFD to predict the temperature variation in the sphere during cooling and while it was subjected to an undulator (ID sector 19) X-ray beam at the APS. The surface temperature of the sphere during the X-ray beam heating was measured using the infrared camera measurement technique described in a previous talk. The temperatures from the numerical predictions and experimental measurements are compared and discussed. Additional results are reported for the two different sphere sizes and for two different supporting pin orientations.

Kazmierczak, Michael↗

NASA NTRS2003

Finding the Cold Needle in a Warm Haystack: Infrared Imaging Applied to Locating Cryo-cooled Crystals in Loops

Thermally imaging the cryocooling processes of crystals has been demonstrated showing the progression of a cold wave through a crystal from the face closest to the origin of the coldstream ending at the point furthest away. During these studies large volume crystals were clearly distinguished from the loop holding them. Large volume crystals, used for neutron studies, were chosen deliberately to enhance the imaging. The different infrared transmission and reflectance properties of the crystal in comparison to the cryo-protectant are thought to be the parameter that produces the contrast making the crystal visible. As an application of the technology to locating crystals, more small crystals of lysozyme and a bFGF/dna complex were cryo-protected and imaged in large loops. The crystals were clearly distinguished from the vitrified solution. In the case of the bFGF/dna complex the illumination had to be carefully manipulated to enable the crystal to be seen in the visible spectrum. These preliminary results will be presented along with advantages and disadvantages of the technique and a discussion of how it might be applied.

Snell, Edward↗

NASA NTRS2002

The Development and Application of a Method to Quantify the Quality of Cryoprotectant Conditions Using Standard Area Detector X-Ray Images

An X-ray based method for determining cryoprotectant concentrations necessary to protect solutions from crystalline ice formation was developed. X-ray images from a CCD area detector were integrated as powder patterns and quantified by determining the standard deviation of the slope of the normalized intensity curve in the resolution range where ice rings are known to occur. The method was tested determining the concentrations of glycerol, PEG400, ethylene glycol and 1,2-propanediol necessary to form an amorphous glass at 1OOK with each of the 98 crystallization solutions of Crystal Screens I and II (Hampton Research, Laguna Hills, California, USA). For conditions that required glycerol concentrations of 35% or above cryoprotectant conditions using 2,3-butanediol were determined. The method proved to be remarkably accurate. The results build on the work of [Garman and Mitchell] and extend the number, of suitable starting conditions to alternative cryoprotectants. In particular, 1,2-propanediol has emerged as a particularly good additive for glass formation upon flash cooling.

McFerrin, Michael↗