Name: production of synthetic nuclear melt glass
Uploaded: 2016-01-04T13:00:01
Description: Watch this Scientific Journal Video about Production of Synthetic Nuclear Melt Glass at JoVE.com

Portions of this study have been previously published in the Journal of Radioanalytical and Nuclear Chemistry.3,13 A patent is pending for this method.

Caution: The process outlined here includes the use of radioactive material (e.g., Uranium Nitrate Hexahydrate) and several corrosive substances. Appropriate protective clothing and equipment should be used (including a lab coat, gloves, eye protection, and a fume hood) during sample preparation. In addition, laboratory areas used for this work should be monitored regularly for radioactive contamination.
Note: The chemical compounds needed are listed in Table 1. This formulation was developed by examining pre...

<ol>
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J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+synthetic+nuclear+melt+glass+for+forensic+analysis.">Development of synthetic nuclear melt glass for forensic analysis.</a> J Radioanal Nucl Chem. 304 (3), 1293-1301 (2015).</li><li>Fluegel, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+of+Glass+Liquidus+Temperatures+using+Disconnected+Peak+Functions.">Modeling of Glass Liquidus Temperatures using Disconnected Peak Functions.</a> , (2007).</li><li>Oldham, C. J., Molgaard, J. J., Auxier, J. D., Hall, H. 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J., Simonetti, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nuclear+forensics:+searching+for+nuclear+device+debris+in+trinitite-hosted+inclusions.">Nuclear forensics: searching for nuclear device debris in trinitite-hosted inclusions.</a> J Radioanal Nucl Chem. 293 (1), 313-319 (2012).</li><li>Ross, C. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Optical Properties of Glass from Alamogordo, New Mexico. , (1948).</li><li>Giminaro, A. V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Compositional+planning+for+development+of+synthetic+urban+nuclear+melt+glass.">Compositional planning for development of synthetic urban nuclear melt glass.</a> J Radional Nucl Chem. , (2015).</li><li>Cook, M. T., Auxier, J. D., Giminaro, A. V., Molgaard, J. J., Knowles, J. R., Hall, H. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+comparison+of+gamma+spectra+from+trinitite+versus+irradiated+synthetic+nuclear+melt+glass.">A comparison of gamma spectra from trinitite versus irradiated synthetic nuclear melt glass.</a> J Radioanal Nucl Chem. , (2015).</li><li>Fahey, J., Zeissler, C. J., Newbury, D. E., Davis, J., Lindstrom, R. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Postdetonation+nuclear+debris+for+attribution.">Postdetonation nuclear debris for attribution.</a> Proc Natl Acad Sci U S A. 107 (47), 20207-20212 (2010).</li><li>Bellucci, J. J., Simonetti, A., Koeman, E. C., Wallace, C., Burns, P. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+detailed+geochemical+investigation+of+post-nuclear+detonation+trinitite+glass+at+high+spatial+resolution:+Delineating+anthropogenic+vs.+natural+components.">A detailed geochemical investigation of post-nuclear detonation trinitite glass at high spatial resolution: Delineating anthropogenic vs. natural components.</a> Chem Geol. 365, 69-86 (2014).</li><li>Donohue, P. H., Simonetti, A., Koeman, E. C., Mana, S., Peter, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nuclear+Forensic+Applications+Involving+High+Spatial+Resolution+Analysis+of+Trinitite+Cross-Sections.">Nuclear Forensic Applications Involving High Spatial Resolution Analysis of Trinitite Cross-Sections.</a> J Radioanal Nucl Chem. , (2015).</li><li>Eaton, G. F., Smith, D. 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Note regarding steps 1.2.2 and 1.2.3: The exact amount of UNH will vary depending on the scenario being simulated. The planning formulas developed by Giminaro et al. can be used to choose the appropriate mass of uranium for a given sample13 as discussed in the &#34;Sample Activation&#34; section of this paper. Also, Uranium Oxide (UO2 or U3O8) may be used in place of UNH, if available, and the mass fraction of 235U in the compound (whether UNH or Uranium Oxi...

Concerns over the potential malicious use of nuclear weapons by terrorists or rogue nations have highlighted the importance of nuclear forensics analysis for the purpose of attribution.1 Rapid post-detonation analysis techniques are desirable to shorten the attribution timeline as much as possible. The development and validation of such techniques requires realistic nuclear debris samples for testing. Nuclear testing no longer occurs in the United States and nuclear surface debris from the testing era is not readily available (with the exception of trinitite - the melt glass produced by the first nuclear test at the trinity site) and therefore realistic surrogate debris is needed. 
The primary goal of the method described here is the production of realistic surrogate nuclear debris similar to trinitite. Synthetic nuclear melt glass samples which are readily available to the academic community can be used to test existing analysis techniques and to develop new methods such as thermo-chromatography for rapid post-detonation analysis.2 With this goal in mind the current study is focused on producing samples which mimic trinitite but do not contain any sensitive weapon design information. The fuel and tamper components within these samples are completely generic and the comparison to trinitite is based on chemistry, morphology, and physical characteristics. The similarities between trinitite and the synthetic nuclear melt glass produced in this study have been previously discussed.3
The purpose of this article is to outline the details of the production process used at the University of Tennessee (UT). This production process was developed with two key parameters in mind: 1) the composition of material incorporated into nuclear melt glass, and 2) the melting temperature of the material. Methods exist for estimating the melting temperature of glass forming networks4 and these techniques have been employed here, along with additional experimentation to determine the optimal processing temperature for the trinitite matrix.5
Alternative methods for surrogate debris production have been published recently. The use of high power lasers has the advantage of creating sufficiently high temperatures to cause elemental fractionation within the target matrix.6 Porous chromatographic substrates have been used to produce small particles similar to fallout particles using condensed phase methods7. The latter method is most useful for producing particulate debris (nuclear fallout) and has been demonstrated with natural metals. The advantages of the method presented here are 1) simplicity, 2) reproducibility, and 3) scalability (sample sizes can range from tiny beads to large chunks of melt glass). Also, this method is expandable both in terms of production output and variety of explosive scenarios covered, and it has already been demonstrated using radioactive materials. A sample has been successfully activated at the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL). Natural uranium compounds were added to the matrix prior to melting and fission products were produced in situ by neutron irradiation. 
Methods within the glass making industry and those employed for the purpose of radioactive waste immobilization8 have been consulted in the development of the method presented here. The unique effects of radiation in glasses are of inherent interest9 and will constitute an important area of study as this method is further developed. 
The method described below is appropriate for any application where a bulk melt glass sample is desired. These samples most closely resemble the material found near the epicenter of a nuclear explosion. Samples of various sizes can be produced, however, methods employing plasma torches or lasers will be more useful for simulating fine particulate debris. Also, commercial HTFs do not reach temperatures high enough to cause elemental fractionation for a wide range of elements. This method should be employed when physical and morphological characteristics are of primary importance.

<table border="0" cellpadding="0" cellspacing="0" width="1019">
	<tbody>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">High Temperature Furnace (HTF)</td>
			<td style="width:200px;">Carbolite</td>
			<td style="width:119px;">HTF 18</td>
			<td style="width:469px;">1800C HTF used to melt samples</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">High Temperature Drop Furnace</td>
			<td style="width:200px;">CM Inc.</td>
			<td style="width:119px;">1706 BL</td>
			<td>1700C Drop Furnace used to melt samples</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Graphite Crucibles</td>
			<td style="width:200px;">SCP Science</td>
			<td style="width:119px;">040-060-041</td>
			<td>27 mL high purity graphite crucibles (10 pack)</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Crucible Tongs</td>
			<td style="width:200px;">Grainger</td>
			<td style="width:119px;">5ZPV0</td>
			<td>26 in, stainless steele tongs for handling crucibles</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Heat Resistent Gloves</td>
			<td style="width:200px;">Grainger</td>
			<td style="width:119px;">8814-09</td>
			<td>Gloves used to protect hands from heat during sample intro/removal</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Mortar &#38; Pestle</td>
			<td style="width:200px;">Fisherbrand</td>
			<td style="width:119px;">S337631</td>
			<td>300 mL, Ceramic mortar and pestle for powdering and mixing</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Micro Balance</td>
			<td style="width:200px;">Grainger</td>
			<td style="width:119px;">8NJG2</td>
			<td>220g Cap, high precision scale for measuring powder mass</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Spatulas</td>
			<td style="width:200px;">Fisherbrand</td>
			<td style="width:119px;">14374</td>
			<td>Metal spatulas for measure small quantities of powder</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">SiO2</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">274739-5KG</td>
			<td>Quartz Sand&#160; CAS Number: 14808-60-7</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Al2O3</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">11028-1KG</td>
			<td>Aluminum Oxide Powder&#160; CAS Number: 1344-28-1</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">CaO</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">12047-2.5KG</td>
			<td>Calcium Oxide Powder&#160; CAS Number: 1305-78-8</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">FeO</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">400866-25G</td>
			<td>Iron Oxide Powder&#160; CAS Number: 1345-25-1</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">MgO</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">342793-250G</td>
			<td>Magnesium Oxide Powder&#160; CAS Number: 1309-48-4</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">Na2O</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">36712-25G</td>
			<td>Sodium Oxide Powder&#160; CAS Number: 1313-59-3</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;">KOH</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">278904-250G</td>
			<td>Potasium Hydroxide Pellets&#160; CAS Number: 12030-88-5</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">MnO</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">377201-500G</td>
			<td>Manganese Oxide Powder&#160; CAS Number: 1344-43-0</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:27px;width:231px;">TiO2</td>
			<td style="width:200px;">Sigma-Aldrich</td>
			<td style="width:119px;">791326-5G</td>
			<td>Titanium Oxide Beads&#160; CAS Number: 12188-41-9</td>
		</tr>
	</tbody>
</table>

production of synthetic nuclear melt glass

Realistic surrogate nuclear debris is needed within the nuclear forensics community to test and validate post-detonation analysis techniques. Here we outline a novel process for producing bulk surface debris using a high temperature furnace. The material developed in this study is physically and chemically similar to trinitite (the melt glass produced by the first nuclear test). This synthetic nuclear melt glass is assumed to be similar to the vitrified material produced near the epicenter (ground zero) of any surface nuclear detonation in a desert environment. The process outlined here can be applied to produce other types of nuclear melt glass including that likely to be formed in an urban environment. This can be accomplished by simply modifying the precursor matrix to which this production process is applied. The melt glass produced in this study has been analyzed and compared to trinitite, revealing a comparable crystalline morphology, physical structure, void fraction, and chemical composition.

The non-radioactive samples produced in this study have been compared to trinitite and Figures 1-3 show that the physical properties and morphology are indeed similar. Figure 1 provides photographs that reveal the similarities in color and texture which are observed at the macroscopic level. Figure 2 shows Scanning Electron Microscope (SEM) Secondary Electron (SE) images which reveal similar features at the micron level. SEM analysis was performed using a SEM and SEM sof...

Watch this Scientific Journal Video about Production of Synthetic Nuclear Melt Glass at JoVE.com

Production of Synthetic Nuclear Melt Glass

A protocol for the production of synthetic nuclear melt glass, similar to trinitite, is presented.

Realistic surrogate nuclear debris is needed within the nuclear forensics community to test and validate post-detonation analysis techniques. Here we ...

The overall goal of this procedure is to make surrogate nuclear melt glass to prepare materials that can be used as standards for the nuclear forensics community. The method that you're going to see today can help answer key questions in nuclear forensics field, such as challenges in analyzing nuclear melt glass and the effects that interfere with mass spectrometry techniques. The main disadvantage of this technique is that it cannot simulate the pressures found in nuclear weapon detonations.In the video today, you are going to see my graduate students, Andrew Giminaro and Jonathan Gill as they demonstrate how to make a synthetic nuclear melt glass. First, acquire the requisite quantities of quartz sand and additional components as indicated in the text protocol. Use a microbalance and small spatula to precisely measure the mass fractions of each compound as listed here.Next, use the mortar and pestle to pulverize and thoroughly mix the compounds, forming a homogenous powder mixture. Agitate using a ball mixer immediately prior to the next step. Following this, acquire a few medium sized crystals of UNH.Inside a fume hood pulverize the UNH crystals using a mortar and pestle to form a fine powder of one to two micron granules. Add 33.75 micrograms of UNH per gram of the non-radioactive precursor matrix. Thoroughly mix the powder mixture, including the UNH, using a mortar and pestle.At this point, fill a thick ceramic dish such as a mortar with approximately 100 grams of pure quartz sand and maintain at room temperature near the location of the furnace where the samples will be melted. Preheat the high temperature furnace to 1, 500 degrees Celsius. After carefully measuring one gram of the radioactive powder mixture, place it in a high purity graphite crucible.Following this, carefully place the crucible in the heated high temperature furnace using a long pari of steel crucible tongs. After melting the mixture for 30 minutes, remove the same from the furnace and pour it into mortar filled with sand. Photographs reveal the similarities in color and texture of the non-radioactive samples and trinitite produced in this study, which are observed at the macroscopic level.Scanning electron microscopes secondary electron images, which reveal similar features at the micron level are displayed here. Numerous voids are observed and the defects and heterogeneity are similar in both trinitite and the synthetic samples. A comparison of powder x-ray defraction spectra for trinitite and the synthetic samples is shown here.Quartz is the only mineral present in both cases and the peak intensities are similar, suggesting a comparable degree of amorphousness. Once mastered, this technique can be done in four hours if done properly. When performing this method, it's very important to be very cautious about the high temperatures that are used in this procedure.Following this procedure, other methods like the development of urban melt glass can be performed in order to answer additional questions, such as the differences between morphologies and cities. After its development, this technique paved the way for researchers in the field of nuclear forensics to explore the possible deficiencies and analytical techniques required to perform analysis on post-detonation debris. After watching this video, you should have a good understanding on how to produce and analyze surrogate nuclear debris that closely resembles the debris found in the trinity test.When working with high temperature furnaces, this can be extremely hazardous and precautions such as wearing appropriate eyewear and temperate-rated personal protective equipment should always be taken when performing this method.

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