Name: Production of Synthetic Nuclear Melt Glass (Video) | JoVE Journal
Uploaded: 2016-01-04T13:00:01.000+00:00
Duration: 4 min 36 s
Description: Learn to produce synthetic nuclear melt glass for nuclear forensics research using quartz sand and high-temperature furnace methods. This protocol helps researchers create surrogate standards for analyzing post-detonation debris and improving mass spectrometry techniques.

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5 minutes

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 previously reported compositional data for trinitite.10 The mass fractions reported here were determined by averaging the mass fractions for several different trinitite samples.10 The "missing" mass (the fractions to not sum to unity) exists to allow for some flexibility when adding fuel, tamper, and other constituents. Our independent analysis of several trinitite samples suggests that quartz is the only mineral phase surviving in trinitite.5 Therefore, quartz is the only mineral included in our Standard Trinitite Formulation (STF). Although relic grains of other minerals have been reported in trinitite,11 these tend to be the exception, rather than the rule. In general, quartz is the only mineral found in the melt glass.10,12 Also, quartz sand is a common component of asphalt and concrete which will be important in the formation of urban nuclear melt glass.
<table fo:keep-together.within-page="1">
	<tbody>
		<tr height="41">
			<td colspan="2" height="41" style="height:42px;width:317px;">Averaged Trinitite Data</td>
			<td colspan="2" style="width:317px;">Standard Trinitite Formulation (STF)</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:159px;">Compound</td>
			<td style="width:159px;">Mass Fraction</td>
			<td style="width:159px;">Compound</td>
			<td style="width:159px;">Mass Fraction</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:159px;">SiO2</td>
			<td style="width:159px;">6.42x10-1</td>
			<td style="width:159px;">SiO2</td>
			<td style="width:159px;">6.42x10-1</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:159px;">Al2O3</td>
			<td style="width:159px;">1.43x10-1</td>
			<td style="width:159px;">Al2O3</td>
			<td style="width:159px;">1.43x10-1</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:159px;">CaO</td>
			<td style="width:159px;">9.64x10-2</td>
			<td style="width:159px;">CaO</td>
			<td style="width:159px;">9.64x10-2</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:159px;">FeO</td>
			<td style="width:159px;">1.97x10-2</td>
			<td style="width:159px;">FeO</td>
			<td style="width:159px;">1.97x10-2</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:159px;">MgO</td>
			<td style="width:159px;">1.15x10-2</td>
			<td style="width:159px;">MgO</td>
			<td style="width:159px;">1.15x10-2</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:159px;">Na2O</td>
			<td style="width:159px;">1.25x10-2</td>
			<td style="width:159px;">Na2O</td>
			<td style="width:159px;">1.25x10-2</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:159px;">K2O</td>
			<td style="width:159px;">5.13x10-2</td>
			<td style="width:159px;">KOH</td>
			<td style="width:159px;">6.12x10-2</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:159px;">MnO</td>
			<td style="width:159px;">5.05x10-4</td>
			<td style="width:159px;">MnO</td>
			<td style="width:159px;">5.05x10-4</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:159px;">TiO2</td>
			<td style="width:159px;">4.27x10-3</td>
			<td style="width:159px;">TiO2</td>
			<td style="width:159px;">4.27x10-3</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:159px;">Total</td>
			<td style="width:159px;">9.81x10-1</td>
			<td style="width:159px;">Total</td>
			<td style="width:159px;">9.91x10-1</td>
		</tr>
	</tbody>
</table>
Table 1. List of chemical compounds.
1. Preparation of the STF
Note: Equipment needed includes a microbalance, metal spatulas, a ceramic mortar and pestle, a chemical fume hood, latex gloves, a lab coat, and eye protection.
<ol>
	<li>Mixing of non-radioactive components
	<ol>
		<li>Acquire at least 65 g of quartz sand (SiO2), 15 g of Al2O3 powder, 10 g of CaO powder, 2 g of FeO powder, 2 g of MgO powder, 2 g of Na2O powder, 7 g of KOH pellets, 1 g of MnO powder and 1 g of TiO2 powder (compounds listed in Table 1).</li>
		<li>Use a microbalance and small spatula to precisely measure the mass fractions of each compound as listed in Table 1. For best results prepare 100 g of the non-radioactive precursor matrix at one time.</li>
		<li>Use a mortar and pestle to pulverize (to ~10-20 µm size granules) and thoroughly mix the compounds, forming a homogenous powder mixture containing 64.2 g of SiO2, 14.2 g of Al2O3, 9.64 g of CaO, 1.97 g of FeO, 1.15 g of MgO, 1.25 g of Na2O. 6.12 g of KOH, 0.0505 g of MnO, and 0.427 g of TiO2.</li>
		<li>Agitate the mixture, using a ball mixer, shortly before the next step is taken.</li>
	</ol>
	</li>
	<li>Mixing of STF with Uranium Nitrate Hexahydrate (UNH)
	<ol>
		<li>Acquire at least 1 g of UNH.</li>
		<li>Inside a fume hood, pulverize a few UNH crystals (using a mortar and pestle) to form a fine powder of 1-2 µm granules.</li>
		<li>Add 33.75 µg of UNH per gram of the non-radioactive precursor matrix (this ratio is appropriate for simulating a simple weapon with a yield of 1 kiloton).13</li>
		<li>Thoroughly mix the powder mixture, including the UNH, using a mortar and pestle. Complete final mixing shortly before the melting step.</li>
	</ol>
	</li>
</ol>
2. Production of 1-gram Melt Glass Sample
Note: Equipment needed includes an HTF rated at 1,600 °C or higher, high purity graphite crucibles, long stainless steel crucible tongs, heat resistant gloves, and eye protection. Heat resistant gloves and eye protection should be worn when introducing or removing samples from the furnace. Tinted safety goggles (or sun glasses) are useful as they reduce the glare from the furnace.
<ol>
	<li>Production of a non-radioactive sample
	<ol>
		<li>Fill a thick ceramic dish (such as a mortar) with ~100 g of pure quartz sand and maintain at RT near the location of the furnace where the samples will be melted.</li>
		<li>Preheat the HTF to 1,500 °C.</li>
		<li>Carefully measure 1.00 g of the non-radioactive powder mixture and place the powder in a high purity graphite crucible.</li>
		<li>Carefully place the crucible in the heated HTF (using a long pair of steel crucible tongs) and melt the mixture for 30 min.</li>
		<li>Remove the sample (again using the tongs) and pour the molten sample into the mortar filled with sand.</li>
		<li>Allow the glass bead to cool for 1-2 min before handling.</li>
		<li>Polish the bead to remove residual sand (if necessary).</li>
	</ol>
	</li>
	<li>Production of a radioactive sample
	<ol>
		<li>Repeat steps 2.1.1 and 2.1.2 above.</li>
		<li>Carefully measure 1.00 gram of the radioactive powder mixture (including UNH) and place the powder in a high purity graphite crucible using a separate spatula and microbalance to avoid cross contamination.</li>
		<li>Repeat steps 2.1.4 - 2.1.6 above.</li>
		<li>Monitor the area around the furnace (using a hand-held radiation detector and/or swipe assays) to check for radioactive contamination.</li>
	</ol>
	</li>
</ol>
3. Sample Activation
Note: The equations that follow were derived assuming the use of weapons grade (enriched) uranium metal. The quantities of UNH or Uranium Oxide will need to be scaled according to the mass fraction of elemental uranium and the level of 235U enrichment.
<ol>
	<li>Activation of a Melt Glass Sample with Uranium Fue
	<ol>
		<li>Calculate the mass fraction of uranium metal required for the sample using the equation below13 (where mU represents the uranium mass fraction and Y represents the weapon yield): 
		<img alt="Equation for calculating \(m_u\) with division formula; research, mathematical concept." src="/files/ftp_upload/53473/53473eq1.jpg" data-altupdatedat="1787630408000" data-alt="Equation 1"></li>
		<li>Optional: Calculate the mass fraction of tamper (e.g., natural uranium, lead, tungsten) using the equation below:13 
		<img alt="Equation for calculating static equilibrium: m_Tamp = (3.2 × 10^-4) / Y; physics formula." src="/files/ftp_upload/53473/53473eq2.jpg" data-altupdatedat="1787630408000" data-alt="Equation 2"></li>
		<li>Calculate the target number of fissions in the sample using the following equation13 where Ms represents the mass of the sample in grams and Nf represents the number of fissions produced in the sample during irradiation: 
		<img alt="Static equilibrium equation for fissions per gram melt glass; formula representation." src="/files/ftp_upload/53473/53473eq3.jpg" data-altupdatedat="1787630408000" data-alt="Equation 3"></li>
		<li>Calculate the required irradiation time using the equation below13 where m235 represents the 235U mass fraction (enrichment level) and tirr is the irradiation time in seconds: 
		<img alt="Nuclear physics, irradiation time formula, equation analysis, scientific data interpretation." src="/files/ftp_upload/53473/53473eq4.jpg" data-altupdatedat="1787630408000" data-alt="Equation 4"></li>
		<li>Irradiate the sample for tirr seconds at a thermal neutron flux of 4.0 x 1014 n/cm2/sec. For example, a 60 sec irradiation in Pneumatic Tube 1 (PT-1) at HFIR (with a thermal to resonance ratio of 35) will produce approximately 1.1 x 1011 fissions in a sample containing 870 µg of UNH (equivalent to 410 µg of natural uranium, or 3.0 µg of 235U). This has been accomplished for one 0.433 g glass bead designed to simulate a melt glass sample produced by a weapon with a 0.1 kiloton yield. This sample has been thoroughly analyzed by Cook et al.14</li>
		<li>Follow applicable safety protocols for handling the radioactive sample post-irradiation. </li>
	</ol>
	</li>
	<li>Activation of a Melt Glass Sample with Plutonium Fuel (Planning Factors)
	<ol>
		<li>Calculate the mass fraction of plutonium metal required for the sample using the equation below13 where mPu represents the plutonium mass fraction and Y represents the weapon yield: 
		<img alt="Equation for calculating \( m_{pu} \), illustration of mathematical formula with variable \( Y \)." src="/files/ftp_upload/53473/53473eq5.jpg" data-altupdatedat="1787630408000" data-alt="Equation 5"></li>
		<li>Repeat Steps 3.1.2 and 3.1.3 above.</li>
		<li>Determine the irradiation time required to obtain the desired number of fissions in the melt glass sample. This time will depend on the composition and grade of the plutonium as well as the neutron energy spectrum.</li>
	</ol>
	</li>
</ol>
Note: Great care should be taken when dealing with plutonium and additional analysis will be required. As of this writing, only uranium has been used in the synthetic melt glass samples produced at UT and irradiated at HFIR.

<ol><li>Carnesdale, A. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aCarnesdale%2C+A+%22Nuclear+Forensics%3A+A+Capability+at+Risk+%28Abbreviated+Version%29%22">Nuclear Forensics: A Capability at Risk (Abbreviated Version)</a>. , Committee on Nuclear Forensics, National Research Council of the National Academies. Washington, D.C. (2010).</li>
<li>Garrison, J. R., Hanson, D. E., Hall, H. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Monte+Carlo+analysis+of+thermochromatography+as+a+fast+separation+method+for+nuclear+forensics%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">Monte Carlo analysis of thermochromatography as a fast separation method for nuclear forensics.</a> J Radioanal Nucl Chem. 291 (3), 885-894 (2011).</li>
<li>Molgaard, J. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Development+of+synthetic+nuclear+melt+glass+for+forensic+analysis%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">Development of synthetic nuclear melt glass for forensic analysis.</a> J Radioanal Nucl Chem. 304 (3), 1293-1301 (2015).</li>
<li>Fluegel, A. Modeling of Glass Liquidus Temperatures using Disconnected Peak Functions. ACerS 2007 Glas Opt Mater Div Meet, , (2007).</li>
<li>Oldham, C. J., Molgaard, J. J., Auxier, J. D., Hall, H. L. Comparison of Nuclear Debris Surrogates Using Powder X-Ray Diffraction. Southeastern Undergraduate Research Conference, , (2014).</li>
<li>Liezers, M., Fahey, A. J., Carman, A. J., Eiden, G. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((The+formation+of+trinitite-like+surrogate+nuclear+explosion+debris+%28+SNED+%29+and+extreme+thermal+fractionation+of+SRM-612+glass+induced+by+high+power+CW+CO+2+laser+irradiation%5BTitle%5D)+AND+%22J+Radional+Nucl+Chem%22%5BJournal%5D)">The formation of trinitite-like surrogate nuclear explosion debris ( SNED ) and extreme thermal fractionation of SRM-612 glass induced by high power CW CO 2 laser irradiation.</a> J Radional Nucl Chem. 304 (2), 705-715 (2015).</li>
<li>Harvey, S. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Porous+chromatographic+materials+as+substrates+for+preparing+synthetic+nuclear+explosion+debris+particles%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">Porous chromatographic materials as substrates for preparing synthetic nuclear explosion debris particles.</a> J Radioanal Nucl Chem. 298 (3), 1885-1898 (2013).</li>
<li>Hanni, J. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Liquidus+temperature+measurements+for+modeling+oxide+glass+systems+relevant+to+nuclear+waste+vitrification%5BTitle%5D)+AND+%22J+Mater+Res%22%5BJournal%5D)">Liquidus temperature measurements for modeling oxide glass systems relevant to nuclear waste vitrification.</a> J Mater Res. 20 (12), 3346-3357 (2005).</li>
<li>Weber, W. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Radiation+Effects+in+Glasses+Used+for+Immobilization+of+High-Level+Waste+and+Plutonium+Disposition%5BTitle%5D)+AND+%22J+Mater+Res%22%5BJournal%5D)">Radiation Effects in Glasses Used for Immobilization of High-Level Waste and Plutonium Disposition.</a> J Mater Res. 12 (8), 1946-1978 (1997).</li>
<li>Eby, N., Hermes, R., Charnley, N., Smoliga, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Trinitite-the+atomic+rock%5BTitle%5D)+AND+%22Geol+Today%22%5BJournal%5D)">Trinitite-the atomic rock.</a> Geol Today. 26 (5), 180-185 (2010).</li>
<li>Bellucci, J. J., Simonetti, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Nuclear+forensics%3A+searching+for+nuclear+device+debris+in+trinitite-hosted+inclusions%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">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://scholar.google.com/scholar?hl=en&safe=off&q=author%3aRoss%2C+CS+%22Optical+Properties+of+Glass+from+Alamogordo%2C+New+Mexico%22">Optical Properties of Glass from Alamogordo, New Mexico</a>. , (1948).</li>
<li>Giminaro, A. V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Compositional+planning+for+development+of+synthetic+urban+nuclear+melt+glass%5BTitle%5D)+AND+%22J+Radional+Nucl+Chem%22%5BJournal%5D)">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/pubmed?term=((A+comparison+of+gamma+spectra+from+trinitite+versus+irradiated+synthetic+nuclear+melt+glass%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">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/pubmed?term=((Postdetonation+nuclear+debris+for+attribution%5BTitle%5D)+AND+%22Proc+Natl+Acad+Sci+U+S+A%22%5BJournal%5D)">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/pubmed?term=((A+detailed+geochemical+investigation+of+post-nuclear+detonation+trinitite+glass+at+high+spatial+resolution%3A+Delineating+anthropogenic+vs.+natural+components%5BTitle%5D)+AND+%22Chem+Geol%22%5BJournal%5D)">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/pubmed?term=((Nuclear+Forensic+Applications+Involving+High+Spatial+Resolution+Analysis+of+Trinitite+Cross-Sections%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">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. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Aged+nuclear+explosive+melt+glass%3A+Radiography+and+scanning+electron+microscope+analyses+documenting+radionuclide+distribution+and+glass+alteration%5BTitle%5D)+AND+%22J+Radioanal+Nucl+Chem%22%5BJournal%5D)">Aged nuclear explosive melt glass: Radiography and scanning electron microscope analyses documenting radionuclide distribution and glass alteration.</a> J Radioanal Nucl Chem. 248 (3), 543-547 (2001).</li>
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</ol>

This work was performed under grant number DE-NA0001983 from the Stewardship Science Academic Alliances (SSAA) Program of the National Nuclear Security Administration (NNSA).

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><tbody><tr><td>High Temperature Furnace (HTF)</td><td>Carbolite</td><td>HTF 18</td><td>1,800 &amp;#176;C HTF used to melt samples</td></tr><tr><td>High Temperature Drop Furnace</td><td>CM Inc.</td><td>1706 BL</td><td>1,700 &amp;#176;C Drop Furnace used to melt samples</td></tr><tr><td>Graphite Crucibles</td><td>SCP Science</td><td>040-060-041</td><td>27 ml high purity graphite crucibles (10 pack)</td></tr><tr><td>Crucible Tongs</td><td>Grainger</td><td>5ZPV0</td><td>26 in., stainless steele tongs for handling crucibles</td></tr><tr><td>Heat Resistent Gloves</td><td>Grainger</td><td>8814-09</td><td>Gloves used to protect hands from heat during sample intro/removal</td></tr><tr><td>Mortar &amp;amp; Pestle</td><td>Fisherbrand</td><td>S337631</td><td>300 ml, Ceramic mortar and pestle for powdering and mixing</td></tr><tr><td>Micro Balance</td><td>Grainger</td><td>8NJG2</td><td>220 g Cap, high precision scale for measuring powder mass</td></tr><tr><td>Spatulas</td><td>Fisherbrand</td><td>14374</td><td>Metal spatulas for measure small quantities of powder</td></tr><tr><td>SiO&lt;sub&gt;2&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>274739-5KG</td><td>Quartz Sand&amp;nbsp; CAS Number: 14808-60-7</td></tr><tr><td>Al&lt;sub&gt;2&lt;/sub&gt;O&lt;sub&gt;3&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>11028-1KG</td><td>Aluminum Oxide Powder&amp;nbsp; CAS Number: 1344-28-1</td></tr><tr><td>CaO</td><td>Sigma-Aldrich</td><td>12047-2.5KG</td><td>Calcium Oxide Powder&amp;nbsp; CAS Number: 1305-78-8</td></tr><tr><td>FeO</td><td>Sigma-Aldrich</td><td>400866-25G</td><td>Iron Oxide Powder&amp;nbsp; CAS Number: 1345-25-1</td></tr><tr><td>MgO</td><td>Sigma-Aldrich</td><td>342793-250G</td><td>Magnesium Oxide Powder&amp;nbsp; CAS Number: 1309-48-4</td></tr><tr><td>Na&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>36712-25G</td><td>Sodium Oxide Powder&amp;nbsp; CAS Number: 1313-59-3</td></tr><tr><td>KOH</td><td>Sigma-Aldrich</td><td>278904-250G</td><td>Potasium Hydroxide Pellets&amp;nbsp; CAS Number: 12030-88-5</td></tr><tr><td>MnO</td><td>Sigma-Aldrich</td><td>377201-500G</td><td>Manganese Oxide Powder&amp;nbsp; CAS Number: 1344-43-0</td></tr><tr><td>TiO&lt;sub&gt;2&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>791326-5G</td><td>Titanium Oxide Beads&amp;nbsp; CAS Number: 12188-41-9</td></tr></tbody></table>

production of synthetic nuclear melt glass

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...

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.

production-of-synthetic-nuclear-melt-glass

Research

JoVE Journal

Engineering

We present the high-temperature synthesis of intermetallic precursors K4Ge9, their dissolution in ethylenediamine to form Ge94- deltahedral Zintl ions, and the reaction of the clusters with alkynes to form organo-Zintl ions.  The latter are characterized by  electrospray mass spectrometry in solutions and by single-crystal X-ray diffraction in the solid state.

Synthesis of Nine-atom Deltahedral Zintl Ions of Germanium and their Functionalization with Organic Groups

An indirect additive manufacturing method combining a 3D printing of polymers with a centrifugal casting is outlined for manufacturing 3D octet truss metals (Al and Cu alloys) having a unit cell length of 5 mm with a wall thickness of 0.5 mm.

Indirect Fabrication of Lattice Metals with Thin Sections Using Centrifugal Casting

We present experiments in which real nuclear fuel, cladding, and containment materials are laser heated to temperatures beyond 3,000 K while their behavior is studied by radiance spectroscopy and thermal analysis. These experiments simulate, on a laboratory scale, the formation of a lava-phase following a nuclear reactor core meltdown.

Laser-heating and Radiance Spectrometry for the Study of Nuclear Materials in Conditions Simulating a Nuclear Power Plant Accident

This manuscript proposes a soft-chemistry method to synthesize superhydrophobic, TiO2-coated hollow glass microspheres (HGM) with high IR-reflective properties.

TiO2-coated Hollow Glass Microspheres with Superhydrophobic and High IR-reflective Properties Synthesized by a Soft-chemistry Method

This protocol describes the fabrication of optical-quality glass surfaces adsorbed with compounds containing long-chain hydrocarbons that can be used to monitor macrophage fusion of living specimens and enables super-resolution microscopy of fixed specimens.

Fabricating Optical-quality Glass Surfaces to Study Macrophage Fusion

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of Mössbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Key procedures to optimize the sealing process and achieve real-time monitoring of the metal-to-glass seal (MTGS) structure are described in detail. The embedded fiber Bragg grating (FBG) sensor is designed to achieve online monitoring of temperature and high-level residual stress in the MTGS with simultaneous environmental pressure monitoring.

Optimized Sealing Process and Real-Time Monitoring of Glass-to-Metal Seal Structures

Here, we present a protocol to synthesize two types of UTe2 crystals: those exhibiting robust superconductivity, via chemical vapor transport synthesis, and those lacking superconductivity, via molten metal flux synthesis.

Comparison of Two Different Synthesis Methods of Single Crystals of Superconducting Uranium Ditelluride

A protocol is presented for the synthesis of persistent luminescent nanomaterials (PLNPs) and their potential applications in rewritable displays and artistic processing utilizing the afterglow effect under ultraviolet light (365 nm) irradiation.

Synthesis of Persistent Luminescent Nanoparticles for Rewritable Displays and Illumination Applications

Fluid-cell Raman Spectroscopy (FCRS) enables in operando observations of reaction and transport phenomena during the aqueous corrosion of silicate glasses at a microscopic level, at elevated temperatures, and in real-time. Without interrupting ongoing processes, FCRS provides information about reaction mechanisms, kinetics, and transport processes.

Fluid-cell Raman Spectroscopy for operando Studies of Reaction and Transport Phenomena during Silicate Glass Corrosion

Learn to produce synthetic nuclear melt glass for nuclear forensics research using quartz sand and high-temperature furnace methods. This protocol helps researchers create surrogate standards for analyzing post-detonation debris and improving mass spectrometry techniques.

Production of Synthetic Nuclear Melt Glass

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