METHODS FOR MOUNTING RADIOACTIVE POWDERS FOR XRD ANALYSIS
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1 54 METHODS FOR MOUNTING RADIOACTIVE POWDERS FOR XRD ANALYSIS Leah N. Squires, Robert D. Mariani, Thomas Hartmann* and J. Rory Kennedy Idaho National Laboratory, Fuel Fabrication and Characterization Department, Idaho Falls, Idaho and University of Nevada at Las Vegas, Nuclear Technology Programs Department, Las Vegas, Nevada 89154* ABSTRACT The preparation of powdered radioactive materials for analysis by X-ray diffraction presents a unique set of challenges. Since these materials are easily dispersed, it is not possible to prepare them for analysis in a standard laboratory fume hood or on a laboratory bench top. The materials must be contained to ensure that no radioactive contamination is released during the preparation of the specimen as well as during analysis in the diffractometer. A simple and inexpensive method was developed by which air sensitive, radioactive powder samples can be prepared in a highly contaminated radioactive glovebox then removed from the glovebox and placed in a specially designed sample containment chamber with a Kapton window. The chamber can then be completely decontaminated before it is placed in the diffractometer. The design of the chamber allows samples to be analyzed using a Bruker D8 Discover with microfocus optics or a PANalytical Empyrean. INTRODUCTION The study of nuclear fuel and related materials at the atomic level is important for understanding the physical and thermal properties of these materials. Knowledge about these properties allows for improvements in the design and efficiency of nuclear fuel. X-ray diffraction is an important tool in this process because it provides phase identification and a better understanding of the changes these materials undergo during irradiation. Sample preparation for these materials is challenging due to the necessity to avoid radioactive contamination of the instrument or laboratory personnel. Caution must be used when preparing samples, especially in the powder form because most powder samples are easily dispersed and therefore it is not possible to prepare them in a fume hood or on a bench top due to the potential for the powder to become airborne thus spreading radioactive contamination throughout the lab. For this reason most of the fuel
2 This document was presented at the Denver X-ray Conference (DXC) on Applications of X-ray Analysis. Sponsored by the International Centre for Diffraction Data (ICDD). This document is provided by ICDD in cooperation with the authors and presenters of the DXC for the express purpose of educating the scientific community. All copyrights for the document are retained by ICDD. Usage is restricted for the purposes of education and scientific research. DXC Website ICDD Website -
3 55 samples analyzed are in the solid form as cast rods cut to fit inside a mount. However, situations arise when it is necessary to analyze a radioactive sample in the powder form. Powder containment mounts were first designed to allow for the removal of radioactive powders from an inert atmosphere glovebox into the laboratory for analysis via XRD. The first design was then improved upon for use as primary containment of radioactive samples, both powder and solid. POWDER MOUNT FOR SCINTAG X-RAY DIFFRACTOMETER Development of a powder XRD mount began after two pieces of solid radioactive material were removed from an inert atmosphere glovebox for analysis and reacted with air before they reached the XRD instrument. These samples were a mixture of metal and metal oxide and in the glovebox they appeared solid. Figure 1a shows the samples under inert atmosphere inside the glovebox. Figure 1b shows the samples after they were removed from the glovebox and opened in a fume hood. As these figures illustrate the material underwent a reaction when not in inert atmosphere which made a highly dispersive powder that could not be analyzed with the XRD containment capabilities available. a. b. Figure 1: a. Under inert atmosphere in the glovebox samples of radioactive metal/metal oxide were solid pieces as shown. When they were placed in the sample mount shown in b and removed from the glovebox the samples reacted with air to form a powder. b. This photograph shows the samples once they reacted with air and formed a powder.
4 56 Until this point radioactive samples were analyzed as solid pieces and the containment was a modified environmental chamber purchased with the Scintag XRD instrument which is shown in Figure 2. Samples were mounted in a glovebox in a holder similar to the one shown in Figure 1b, then removed from the glovebox and placed in a hood where they could be loaded into the environmental chamber. In order to load these samples into the environmental chamber it was necessary for laboratory personnel to handle the exposed samples in fume hood for a short period of time. Therefore, this technique could not be used for the samples shown in Figure 1. A second challenge associated with these samples was their apparent reactivity with air. Design of a new mount that could be loaded under inert atmosphere and transferred into the environmental chamber was necessary. Figure 2: A modified environmental chamber with a beryllium window was used for radioactive sample containment. The mount design consisted of two pieces of polycarbonate which formed a top and bottom. The pieces were threaded to fit securely together. Beryllium foil was attached in the top of the mount using epoxy to serve as window for x-rays. A well in the bottom of the mount was filled with vacuum grease to allow the powder to adhere. Once the powder (and internal standard) was
5 57 sprinkled onto the vacuum grease the lid of the mount was screwed down. This mount is shown in Figure 3a. It was quickly discovered that these mounts would need to be disposable due to the levels of contamination on the inside and on the underneath side of the beryllium. Since beryllium is difficult to dispose of it was replaced with Mylar. The Mylar presented difficulty when attempts were made to hold it in place with epoxy. Therefore the epoxy was replaced with an o-ring to hold the Mylar window in place in the top of the mount and also to ensure a good seal was formed between the bottom and top of the mount to make the mount as airtight as possible. Figure 3b shows the mount with the Mylar window held in place with an o-ring. In order to use this mount the samples shown in Figure 1a were powdered in the inert atmosphere glovebox using a mortar and pestle. The powder was then sprinkled onto the vacuum grease filling the well in the bottom of the mount. The lid was screwed onto the bottom (finger tight to allow the o-ring to properly seal). The mount was subsequently wiped down with a chelating agent while still inside the glovebox to remove most loose contamination. It was transferred out of the glovebox into the fume hood where it underwent additional decontamination before it was loaded into the environmental chamber shown in Figure 2 for analysis in the Scintag diffractometer. a. b. Figure 3: a. The first prototype used a beryllium window held in place with epoxy. b. The second prototype used a Mylar window held in place with an o-ring which allowed for a better seal between the top and bottom of the mount and also for easier disposability of the mount.
6 58 RADIOACTIVE SAMPLE CONTANMENT FOR BRUKER D8 DISCOVER AND PANALYTICAL EMPYREAN When two new instruments, a PANalytical Empyrean and a Bruker D8 Discover with microfocus capabilities, were purchased it became necessary to find a way to contain radioactive samples for analysis on these instruments and ensure that the instruments themselves were not contaminated. The previously described sample mounts became the starting point for the design of sample containment for these new instruments. The containment chamber was designed to the more rigid size requirements of the PANalytical and made of stainless steel to allow the magnetic spinning mechanism on the PANalytical spinner stage to operate properly. The Mylar window was replaced with a Kapton window which was found to be easier to manipulate. An o-ring was used to hold the window in place and to seal the chamber. The sample was placed in the center holder in a glovebox then bagged into a fume hood where it was placed inside the containment chamber. After the lid was securely screwed onto the bottom of the mount it was decontaminated with a chelating agent. In all cases the containment mount has been successfully decontaminated using this process so that it could be removed from the fume hood as radiologically clean (i.e. no loose or outside contamination). Figure 4 shows the assembly of these mounts. a. b. c. Figure 4: a. The Kapton window is placed inside the lid of the containment chamber using an o- ring to hold it in place. b. The sample is place in the bottom of the containment chamber (a small amount of LaB 6 shown here). c. The lid is screwed onto the bottom and the entire chamber is decontaminated with a chelating agent prior to radiological survey. A sample chamber that surveys clean can be removed from the fume hood and place on the instrument.
7 59 RADIOACTIVE POWDER SAMPLE CONTAINMENT IN NEWLY DESIGNED MOUNT The final challenge arose when powdered radioactive samples were presented for analysis. Since the environmental chamber was no longer an option and restrictions prohibited the manipulation of loose radioactive powders in a fume hood for reasons already discussed, it became necessary to develop a method whereby radioactive powders could be fixed in a glovebox and removed for analysis. For this zero diffraction plates (24.6 mm in diameter x 1 mm thick) were obtained from MTI Corporation. These zero diffraction plates were taken into the glovebox where a slurry of LaB 6, PuO 2 powder and an ethyl acetate based fixative (clear nail polish) was made. A thin layer of this slurry was then painted onto the zero diffraction plate as shown in Figure 5 and allowed to dry. Figure 5: A slurry of PuO 2 powder, LaB 6 internal standard and clear nail polish was painted onto the zero diffraction plate and allowed to dry. Once dry the zero diffraction plate was decontaminated using a chelating agent prior to removal from the glovebox to remove any loose contamination. It was then transferred to a fume hood where it loaded into the containment chamber using the method shown in Figure 4. The addition of the zero diffraction plate greatly reduced the background from the use of the polycarbonate sample holder by itself. CONCLUSIONS A powder mount was designed to allow for the successful analysis of radioactive XRD samples in the powder form on a Scintag XRD. It was then modified for use in the analysis of solid radioactive samples on two new instruments, a PANalytical Empyrean and a Bruker D8 Discover which were later acquired. Finally the same sample containment chamber design was modified again to be used for the analysis of radioactive powder samples in these two new instruments.
8 60 The design offers protection of the instruments from sample contamination, a reusable outer chamber and an inexpensive and easily disposable window and internal sample holder. To date the containment chambers have always been cleaned and re-used with only the internal holder, o- ring and Kapton window being disposed of as waste.
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