Publications

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High-fidelity detection of iodine species is of utmost importance to the safety of the population in cases of nuclear accidents or advanced nuclear fuel reprocessing. In this paper, we describe the success at using impedance spectroscopy to directly detect the real-time adsorption of I₂ by a metal–organic framework zeolitic imidazolate framework (ZIF)-8-based sensor. Methanolic suspensions of ZIF-8 were dropcast onto platinum interdigitated electrodes, dried, and exposed to gaseous I₂ at 25, 40, or 70 °C. Using an unoptimized sensor geometry, I₂ was readily detected at 25 °C in air within 720 s of exposure. The specific response is attributed to the chemical selectivity of the ZIF-8 toward I₂. Furthermore, equivalent circuit modeling of the impedance data indicates a >10⁵× decrease in ZIF-8 resistance when 116 wt % I₂ is adsorbed by ZIF-8 at 70 °C in air. This irreversible decrease in resistance is accompanied by an irreversible loss in the long-range crystallinity, as evidenced by X-ray diffraction and infrared spectroscopy. Air, argon, methanol, and water were found to produce minimal changes in ZIF-8 impedance. Finally, this report demonstrates how selective I₂ adsorption by ZIF-8 can be leveraged to create a highly selective sensor using >10⁵× changes in impedance response to enable the direct electrical detection of environmentally relevant gaseous toxins.

The removal of silica, ubiquitous in produced and industrial waters, by novel mixed oxides is investigated in this present study. We have combined the advantage of high selectivity hydrotalcite (HTC, (Mg6Al2(OH)16(CO3)·4H2O)), with large surface area of active alumina (AA, (Al2O3)) for effective removing of the dissolved silica from cooling tower water. The batch test results indicated the combined HTC/AA is a more effective method for removing silica from CTW than using each of HTC or AA separately. The silica uptake was confirmed by Fourier transform infrared (FTIR), and Energy dispersive spectroscopy (EDS). Results indicate HTC/AA effectively removes silica from cooling tower water (CTW), even in the presence of large concentrations of competing anions, such as Cl−, NO3− HCO3−, CO32− and SO42−. The Single Path Flow Through (SPFT) tests confirmed to rapid uptake of silica by combined HTC/AA during column filtration. The experimental data of silica adsorption fit best to Freundlich isotherm model.

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Water shortages are a growing global problem. Reclamation of industrial and municipal wastewater will be necessary in order to mitigate water scarcity. However, many operational challenges, such as silica scaling, prevent large scale water reuse. Previously, our team at Sandia has demonstrated the use of selective ion exchange materials, such as calcinated hydrotalcite (HTC, (Mg ₆ Al ₂ (OH) ₁₆ (CO ₃ )*4H ₂ O)), for the low cost removal of silica from synthetic cooling tower water. However, it is not currently know if calcinated HTC has similar capabilities in realistic applications. The purpose of this study was to investigate the ability of calcinated HTC to remove silica from real cooling tower water. This was investigated under both batch and continuous conditions, and in the presence of competing ions. It was determined that calcinated HTC behaved similarly in real and synthetic cooling tower water; the HTC is highly selective for the silica even in the presence of competing cations. Therefore, the data concludes that calcinated HTC is a viable anti-scaling pretreatment for the reuse of industrial wastewaters.

Silica is ubiquitous in produced and industrial waters, and plays a major disruptive role in water recycle. Herein we have investigated the use of mixed oxides for the removal of silica from these waters, and their incorporation into a low cost and low energy water purification process. High selectivity hydrotalcite (HTC, (Mg₆Al₂(OH)₁₆(CO₃)•4H₂O)), is combined in series with high surface area active alumina (AA, (Al₂O₃)) as the dissolved silica removal media. Batch test results indicated that combined HTC/AA is a more effective method for removing silica from industrial cooling tower wasters (CTW) than using HTC or AA separately. The silica uptake via ion exchange on the mixed oxides was confirmed by Fourier transform infrared (FTIR), and Energy dispersive spectroscopy (EDS). Furthermore, HTC/AA effectively removes silica from CTW even in the presence of large concentrations of competing anions, such as Cl^-, NO₃^- HCO₃^-, CO₃^2- and SO₄^2-. Similar to batch tests, Single Path Flow Through (SPFT) tests with sequential HTC/AA column filtration has very high silica removal too. Technoeconomic Analysis (TEA) was simultaneously performed for cost comparisons to existing silica removal technologies.

Securing additional water sources remains a primary concern for arid regions in both the developed and developing world. Climate change is causing fluctuations in the frequency and duration of precipitation, which can be can be seen as prolonged droughts in some arid areas. Droughts decrease the reliability of surface water supplies, which forces communities to find alternate primary water sources. In many cases, ground water can supplement the use of surface supplies during periods of drought, reducing the need for above-ground storage without sacrificing reliability objectives. Unfortunately, accessible ground waters are often brackish, requiring desalination prior to use, and underdeveloped infrastructure and inconsistent electrical grid access can create obstacles to groundwater desalination in developing regions. The objectives of the proposed project are to (i) mathematically simulate the operation of hollow fiber membrane distillation systems and (ii) optimize system design for off-grid treatment of brackish water. It is anticipated that methods developed here can be used to supply potable water at many off-grid locations in semi-arid regions including parts of the Navajo Reservation. This research is a collaborative project between Sandia and the University of Arizona.

Impedance spectroscopy was leveraged to directly detect the sorption of I 2 by selective adsorption into nanoporous metal organic frameworks (MOF). Films of three different types of MOF frameworks, respectively, were drop cast onto platinum interdigitated electrodes, dried, and exposed to gaseous I 2 at 25, 40, or 70 C. The MOF frameworks varied in topology from small pores (equivalent to I 2 diameter) to large pore frameworks. The combination of the chemistry of the framework and pore size dictated quantity and kinetics of I 2 adsorption. Air, argon, methanol, and water were found to produce minimal changes in ZIF-8 impedance. Independent of MOF framework characteristics, all resultant sensors showed high response to I 2 in air. As an example of sensor output, I 2 was readily detected at 25 C in air within 720 s of exposure, using an un-optimized sensor geometry with a small pored MOF. Further optimization of sensor geometry, decreasing MOF film thicknesses and maximizing sensor capacitance, will enable faster detection of trace I 2 .

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