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Title: Facile incorporation of technetium into magnetite, magnesioferrite, and hematite by formation of ferrous nitrate in situ: precursors to iron oxide nuclear waste forms

Abstract

The fission product, 99Tc, presents significant challenges to the long-term disposal of nuclear waste due to its long half-life, high fission yield, and to the environmental mobility of pertechnetate (TcO 4 ), the stable Tc species in aerobic environments. Here, the migration of 99Tc from disposal sites can potentially be prevented by incorporating it into durable waste forms based on environmentally stable minerals.

Authors:
ORCiD logo [1]; ORCiD logo [2]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
  2. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); USDOE Office of Environmental Management (EM)
OSTI Identifier:
1550810
Alternate Identifier(s):
OSTI ID: 1460584
Grant/Contract Number:  
[AC02-05CH11231; AC02-76SF00515; AC05-76RL01830]
Resource Type:
Accepted Manuscript
Journal Name:
Dalton Transactions
Additional Journal Information:
[ Journal Volume: 47; Journal Issue: 30]; Journal ID: ISSN 1477-9226
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE WASTES FROM NUCLEAR FACILITIES

Citation Formats

Lukens, Wayne W., and Saslow, Sarah A. Facile incorporation of technetium into magnetite, magnesioferrite, and hematite by formation of ferrous nitrate in situ: precursors to iron oxide nuclear waste forms. United States: N. p., 2018. Web. doi:10.1039/c8dt01356j.
Lukens, Wayne W., & Saslow, Sarah A. Facile incorporation of technetium into magnetite, magnesioferrite, and hematite by formation of ferrous nitrate in situ: precursors to iron oxide nuclear waste forms. United States. doi:10.1039/c8dt01356j.
Lukens, Wayne W., and Saslow, Sarah A. Tue . "Facile incorporation of technetium into magnetite, magnesioferrite, and hematite by formation of ferrous nitrate in situ: precursors to iron oxide nuclear waste forms". United States. doi:10.1039/c8dt01356j. https://www.osti.gov/servlets/purl/1550810.
@article{osti_1550810,
title = {Facile incorporation of technetium into magnetite, magnesioferrite, and hematite by formation of ferrous nitrate in situ: precursors to iron oxide nuclear waste forms},
author = {Lukens, Wayne W. and Saslow, Sarah A.},
abstractNote = {The fission product,99Tc, presents significant challenges to the long-term disposal of nuclear waste due to its long half-life, high fission yield, and to the environmental mobility of pertechnetate (TcO4–), the stable Tc species in aerobic environments. Here, the migration of 99Tc from disposal sites can potentially be prevented by incorporating it into durable waste forms based on environmentally stable minerals.},
doi = {10.1039/c8dt01356j},
journal = {Dalton Transactions},
number = [30],
volume = [47],
place = {United States},
year = {2018},
month = {7}
}

Journal Article:
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A critical study<span class="fa fa-external-link" aria-hidden="true"></span></a> <small class="text-muted" style="text-transform:uppercase; font-size:0.75rem;"><br/> <span class="type">journal</span>, <span class="date" data-date="2014-09-30">September 2014</span></small> </h2> <ul class="small references-list" style="list-style-type:none; margin-top: 0.5em; padding-left: 0; line-height:1.8em;"> <li> <span style="color:#5C7B2D;"> Cervellino, Antonio; Frison, Ruggero; Cernuto, Giuseppe</span> </li> <li> Journal of Applied Crystallography, Vol. 47, Issue 5</li> <li> <span class="text-muted related-url">DOI: <a href="https://doi.org/10.1107/S1600576714019840" class="text-muted" target="_blank" rel="noopener noreferrer">10.1107/S1600576714019840<span class="fa fa-external-link" aria-hidden="true"></span></a></span> </li> </ul> <hr/> </div></div> <div class="pagination-container small"> <a class="pure-button prev page" href="#" rel="prev"><span class="fa fa-angle-left"></span></a><ul class="pagination d-inline-block" style="padding-left:.2em;"></ul><a class="pure-button next page" href="#" rel="next"><span class="fa fa-angle-right"></span></a> </div> </div> </div> <div class="col-sm-3 order-sm-3"> <ul class="nav nav-stacked"> <li class="active"><a href="" class="reference-type-filter tab-nav" data-tab="biblio-references" data-filter="type" data-pattern="*"><span class="fa fa-angle-right"></span> All References</a></li> <li class="small" style="margin-left:.75em; text-transform:capitalize;"><a href="" class="reference-type-filter tab-nav" data-tab="biblio-references" data-filter="type" data-pattern="conference"><span class="fa fa-angle-right"></span> conference<small class="text-muted"> (1)</small></a></li> <li class="small" style="margin-left:.75em; text-transform:capitalize;"><a href="" class="reference-type-filter tab-nav" data-tab="biblio-references" data-filter="type" data-pattern="journal"><span class="fa fa-angle-right"></span> journal<small class="text-muted"> (80)</small></a></li> </ul> <div style="margin-top:2em;"> <form class="pure-form small text-muted reference-search"> <label for="reference-search-text" class="sr-only">Search</label> <input class="search form-control pure-input-1" id="reference-search-text" placeholder="Search" style="margin-bottom:10px;" /> <fieldset> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="name" style="position:relative;top:2px;" id="reference-search-sort-name"><label for="reference-search-sort-name" style="margin-left: .3em;">Sort by title</label></div> <div style="margin-left:1em; font-weight:normal; line-height: 1.6em;"><input type="radio" class="sort" name="references-sort" data-sort="date" data-order="desc" style="position:relative;top:2px;" id="reference-search-sort-date"><label for="reference-search-sort-date" style="margin-left: .3em;">Sort by date</label></div> </fieldset> <div class="text-left" style="margin-left:1em;"> <a href="" class="filter-clear clearfix" title="Clear filter / sort" style="font-weight:normal; float:none;">[ × clear filter / sort ]</a> </div> </form> </div> </div> </div> </section> <section id="biblio-related" class="tab-content tab-content-sec " data-tab="biblio"> <div class="row"> <div class="col-sm-9 order-sm-9"> <section id="biblio-similar" class="tab-content tab-content-sec active" data-tab="related"> <div class="padding"> <p class="lead text-muted" style="font-size: 18px; margin-top:0px;">Similar Records in DOE PAGES and OSTI.GOV collections:</p> <aside> <ul class="item-list" itemscope itemtype="http://schema.org/ItemList" style="padding-left:0; list-style-type: none;"> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="1" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1482510-incorporation-technetium-spinel-ferrites" itemprop="url">Incorporation of Technetium into Spinel Ferrites</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Lukens, Wayne W.</span> ; <span class="author">Magnani, Nicola</span> ; <span class="author">Tyliszczak, Tolek</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - Environmental Science and Technology</span> </span> </div> <div class="abstract">Technetium ( <sup>99</sup>Tc) is a problematic fission product for the long-term disposal of nuclear waste due to its long half-life, high fission yield, and to the environmental mobility of pertechnetate, the stable species in aerobic environments. One approach to preventing <sup>99</sup>Tc contamination is using sufficiently durable waste forms. We report the incorporation of technetium into a family of synthetic spinel ferrites that have environmentally durable natural analogs. A combination of X-ray diffraction, X-ray absorption fine structure spectroscopy, and chemical analysis reveals that Tc(IV) replaces Fe(III) in octahedral sites and illustrates how the resulting charge mismatch is balanced. When a large<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> excess of divalent metal ions is present, the charge is predominantly balanced by substitution of Fe(III) by M(II). When a large excess of divalent metal ions is absent, the charge is largely balanced by creation of vacancies among the Fe(III) sites (maghemitization). In most samples, Tc is present in Tc-rich regions rather than being homogeneously distributed.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <span class="fa fa-book text-muted" aria-hidden="true"></span> Cited by 14<div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1021/acs.est.6b04209" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1482510" data-product-type="Journal Article" data-product-subtype="AM" >10.1021/acs.est.6b04209</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1482510" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1482510" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="2" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1482527-aqueous-synthesis-technetium-doped-titanium-dioxide-direct-oxidation-titanium-powder-precursor-ceramic-nuclear-waste-forms" itemprop="url">Aqueous Synthesis of Technetium-Doped Titanium Dioxide by Direct Oxidation of Titanium Powder, a Precursor for Ceramic Nuclear Waste Forms</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Lukens, Wayne W.</span> ; <span class="author">Saslow, Sarah A.</span> <span class="text-muted pubdata"> - Chemistry of Materials</span> </span> </div> <div class="abstract">Technetium-99 (Tc) is a problematic fission product that complicates the long-term disposal of nuclear waste due to its long half-life, high fission yield, and the environmental mobility of pertechnetate, its stable form in aerobic environments. One approach to preventing Tc contamination is through incorporation into durable waste forms based on weathering-resistant minerals such as rutile (titanium dioxide). Here, the incorporation of technetium into titanium dioxide by means of simple, aqueous chemistry - direct oxidation of titanium powder in the presence of ammonium fluoride - is achieved. X-ray absorption fine structure spectroscopy and diffuse reflectance spectroscopy indicate that Tc(IV) replaces Ti(IV)<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> within the structure. Rather than being incorporated as isolated Tc(IV) ions, Tc is present as pairs of edge-sharing Tc(IV) octahedra similar to molecular Tc(IV) complexes such as [(H <sub>2</sub>EDTA)TcIV](μ-O) <sub>2</sub>. Technetium-doped TiO <sub>2</sub> was suspended in deionized water under aerobic conditions, and the Tc leached under these conditions was followed for 8 months. The normalized release rate of Tc (LR <sub>Tc</sub>) from the TiO <sub>2</sub> particles is low (3 × 10 <sup>-6</sup>g m <sup>-2</sup>d <sup>-1</sup>), which illustrates the potential utility of TiO <sub>2</sub> as waste form. However, the small size of the as-prepared TiO <sub>2</sub> nanoparticles results in an estimated retention of Tc of 10 <sup>4</sup> years, which is only a fraction of the half-life of Tc (2.1 × 10 <sup>5</sup> years).</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <span class="fa fa-book text-muted" aria-hidden="true"></span> Cited by 4<div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1021/acs.chemmater.7b03567" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1482527" data-product-type="Journal Article" data-product-subtype="AM" >10.1021/acs.chemmater.7b03567</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1482527" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1482527" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="4" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/pages/biblio/1529251-thermodynamic-parameters-complexation-technetium-iv-edta" itemprop="url">Thermodynamic parameters for the complexation of technetium(IV) with EDTA</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Journal Article</small><span class="authors"> <span class="author">Friend, Mitchell T.</span> ; <span class="author">Lledo, Cecilia Eiroa</span> ; <span class="author">Lecrivain, Lindsey M.</span> ; <span class="author">...</span> <span class="text-muted pubdata"> - Radiochimica Acta</span> </span> </div> <div class="abstract">Technetium-99 is a high yield (~6% fission yield) fission product and long-lived (2.13×10 <sup>5</sup>year half-life) component of nuclear waste that will be disposed of in a geological repository. Some <sup>99</sup>Tc has been released into the environment due to nuclear fuel and weapon production activities at sites such as Hanford, WA. Strongly complexing ligands such as ethylenediamine- <em>N</em>, <em>N</em>, <em>N</em>', <em>N</em>'-tetraacetic acid (EDTA) are known to increase Tc(IV) solubility and mobility in environmental systems and an accurate quantification of the complexation of Tc(IV) with EDTA is important for predicting its behavior in a geological repository. A liquid–liquid extraction system utilizing 0.2<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> M TOPO in dodecane was used to measure the stability constants of Tc(IV)-EDTA in 0.50 <em>m</em> NaNO <sub>3</sub> at variable temperatures (14.0±0.1, 25.0±0.1, and 32.0±0.1°C). The acid dependence of the apparent stability constants in the p <em>C</em> <sub>H</sub> range of 2.00–2.70 indicated the formation of TcO(EDTA) <sup>2-</sup>(log <em>β</em> <sub>101</sub>=17.9±0.3, 25.0±0.1°C) and a protonated complex TcO(H)(EDTA) <sup>-</sup>(log <em>β</em> <sub>111</sub>=20.5±0.1, 25.0±0.1°C). The associated thermodynamic parameters Δ <sub>r</sub> <em>G</em> <sub>101</sub>=-101.7±0.4 kJ·mol <sup>-1</sup>, Δ <sub>r</sub> <em>H</em> <sub>101</sub>=-47±9 kJ·mol <sup>-1</sup>, Δ <sub>r</sub> <em>S</em> <sub>101</sub>=179±36 J·mol <sup>-1</sup>·K <sup>-1</sup>, Δ <sub>r</sub> <em>G</em> <sub>111</sub>=-117.2±0.3 kJ·mol <sup>-1</sup>, Δ <sub>r</sub> <em>H</em> <sub>111</sub>=-23±5 kJ·mol <sup>-1</sup>, and Δ <sub>r</sub> <em>S</em> <sub>111</sub>=315±63 J·mol <sup>-1</sup>·K <sup>-1</sup>(0.50 <em>m</em>NaNO <sub>3</sub>, 25.0±0.1°C) were determined by van’t Hoff analysis. The formation of each Tc(IV)–EDTA complex is exothermic and present favorable entropy terms.</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> <ul class="pure-menu-list"> <li class="pure-menu-item"><span class="item-info-ftlink">DOI: <a class="misc doi-link " href="https://doi.org/10.1515/ract-2018-2992" target="_blank" rel="noopener" title="Link to document DOI" data-ostiid="1529251" data-product-type="Journal Article" data-product-subtype="AM" >10.1515/ract-2018-2992</a></span></li> <li class="pure-menu-item"><span class="item-info-ftlink"><a class="misc fulltext-link " href="/pages/servlets/purl/1529251" title="Link to document media" target="_blank" rel="noopener" data-ostiid="1529251" data-product-type="Journal Article" data-product-subtype="AM" >Full Text Available</a></span></li> </ul> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="5" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/biblio/22224826-radiation-stability-benzyl-tributyl-ammonium-chloride-towards-technetium-extraction" itemprop="url">Radiation Stability of Benzyl Tributyl Ammonium Chloride towards Technetium-99 Extraction - 13016</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Conference</small><span class="authors"> <span class="author">Paviet-Hartmann, Patricia</span> ; <span class="author">Horkley, Jared</span> ; <span class="author">Campbell, Keri</span> ; <span class="author">...</span> <span class="text-muted pubdata"></span> </span> </div> <div class="abstract">A closed nuclear fuel cycle combining new separation technologies along with generation III and generation IV reactors is a promising way to achieve a sustainable energy supply. But it is important to keep in mind that future recycling processes of used nuclear fuel (UNF) must minimize wastes, improve partitioning processes, and integrate waste considerations into processes. New separation processes are being developed worldwide to complement the actual industrialized PUREX process which selectively separates U(VI) and Pu(IV) from the raffinate. As an example, the UREX process has been developed in the United States to co-extract hexavalent uranium (U) and hepta-valent technetium<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> (Tc) by tri-n-butyl phosphate (TBP). Tc-99 is recognized to be one of the most abundant, long-lived radio-toxic isotopes in UNF (half-life, t{sub 1/2} = 2.13 x 10{sup 5} years), and as such, is targeted in UNF separation strategies for isolation and encapsulation in solid waste-forms for final disposal in a nuclear waste repository. Immobilization of Tc-99 by a durable solid waste-form is a challenge, and its fate in new advanced technology processes is of importance. It is essential to be able to quantify and locate 1) its occurrence in any new developed flowsheets, 2) its chemical form in the individual phases of a process, 3) its potential quantitative transfer in any waste streams, and consequently, 4) its quantitative separation for either potential transmutation to Ru-100 or isolation and encapsulation in solid waste-forms for ultimate disposal. In addition, as a result of an U(VI)-Tc(VII) co-extraction in a UREX-based process, Tc(VII) could be found in low level waste (LLW) streams. There is a need for the development of new extraction systems that would selectively extract Tc-99 from LLW streams and concentrate it for feed into high level waste (HLW) for either Tc-99 immobilization in metallic waste-forms (Tc-Zr alloys), and/or borosilicate-based waste glass. Studies have been launched to investigate the suitability of new macro-compounds such as crown-ethers, aza-crown ethers, quaternary ammonium salts, and resorcin-arenes for the selective extraction of Tc-99 from nitric acid solutions. The selectivity of the ligand is important in evaluating potential separation processes and also the radiation stability of the molecule is essential for minimization of waste and radiolysis products. In this paper, we are reporting the extraction of TcO{sub 4}{sup -} by benzyl tributyl ammonium chloride (BTBA). Experimental efforts were focused on determining the best extraction conditions by varying the ligand's matrix conditions and concentration, as well as varying the organic phase composition (i.e. diluent variation). Furthermore, the ligand has been investigated for radiation stability. The ?-irradiation was performed on the neat organic phases containing the ligand at different absorbed doses to a maximum of 200 kGy using an external Co-60 source. Post-irradiation solvent extraction measurements will be discussed. (authors)</span><a href='#' onclick='$(this).hide().prev().hide().prev().show();return false;' style='margin-left:10px;display:none;'>« less</a></div><div class="metadata-links small clearfix text-muted" style="margin-top:15px;"> <div class="pure-menu pure-menu-horizontal pull-right" style="width:unset;"> </div> </div> </div> <div class="clearfix"></div> </div> </li> <li> <div class="article item document" itemprop="itemListElement" itemscope itemtype="http://schema.org/WebPage"><meta itemprop="position" content="6" /><div class="item-info"> <h2 class="title" itemprop="name headline"><a href="/biblio/4169469-accumulation-technetium-from-soil-plants-potential-mechanism-uptake-toxicity" itemprop="url">Accumulation of technetium from soil by plants: a potential mechanism for uptake and toxicity</a></h2> <div class="metadata"> <small class="text-muted" style="text-transform:uppercase;display:block;line-height:2.5em;">Conference</small><span class="authors"> <span class="author">Wildung, R E</span> ; <span class="author">Garland, T R</span> ; <span class="author">Cataldo, D A</span> <span class="text-muted pubdata"></span> </span> </div> <div class="abstract">The isotope<a href='#' onclick='$(this).hide().next().show().next().show();return false;' style='margin-left:10px;'>more »</a><span style='display:none;'> $sup 99$Tc (T $sup 1$/$sub 2$, 2.15 x 10$sup 5$ years) is produced by the spontaneous fission of $sup 238$U in nature and by the slow neutron fission of $sup 238$U in nuclear reactors. In the latter case, the potential exists for Tc entrance into the environment in emissions from nuclear reactors, nuclear fuel reprocessing plants, and other facilities which use Tc for commercial purposes. Results are reported from studies on Tc uptake by plants. The most stable chemical species of Tc in aqueous solution is the pertechnetate ion (TcO$sub 4$$sup -1$), and it is this form which is most likely to enter surface soils. Recent studies indicated that at least over the short term, pertechnetate is soluble and highly mobile in most soils and is sorbed in significant quantities only in high organic matter, low pH soils. Plant availability normally increases with increased ion solubility in soil provided the ion is not discriminated against at the plant root level. Furthermore, the aqueous chemistry of pertechnetate is similar in several respects to permanganate and molybdate, compounds of elements essential in plant nutrition. Experiments were undertaken to determine the uptake and distribution of Tc in plants as a function of time using soybeans (Glycine max) and $sup 99$Tc as a tracer. 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