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The Water–Iodine Oxide System: a Revised Mechanism for Hydration and Dehydration† Cite This: RSC Adv.,2017,7,10183 Dylan K

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The Water–Iodine Oxide System: a Revised Mechanism for Hydration and Dehydration† Cite This: RSC Adv.,2017,7,10183 Dylan K RSC Advances PAPER The water–iodine oxide system: a revised mechanism for hydration and dehydration† Cite this: RSC Adv.,2017,7,10183 Dylan K. Smith,a Michelle L. Pantoya,*a Jeffrey S. Parkeyb and Mehmet Kesmezb Iodic acids are widely studied in atmospheric and biological applications but their inherent hydrophilic properties introduce complexities that affect their functionality and reactivity. We have shown that iodic acid (HIO3) dehydrates directly into iodine pentoxide (I2O5) in contradiction to the generally accepted multi-step dehydration mechanism where HIO3 dehydrates into HI3O8 first, then dehydrates into I2O5. The generally accepted mechanism is used to determine the concentration of iodic acid by TGA and is only valid for special conditions. The revised mechanism allows for the determination of concentrations of iodic acids under all conditions, and the more specific conditions where the accepted mechanism is Received 6th December 2016 valid are shown. The determination of concentration of iodic acid with the revised dehydration Accepted 1st February 2017 mechanism is dependent on assumptions of residual water and initial concentration of HI3O8. The DOI: 10.1039/c6ra27854j validity of these assumptions is established by studying the absorption and hydration behavior of I2O5 rsc.li/rsc-advances from atmospheric water. These results will have an impact on the handling and use of iodine. Introduction absorption begins; variations in concentration of iodic acids (HIO3,HI3O8); crystal structure; onset temperature for dehy- Iodine(V) oxides have biocidal potential in neutralizing bacterial dration and decomposition; and, absorption rates. All of the agents released in certain weapon systems. Handling iodine(V) inconsistencies discussed below are affected by the hydration oxides is one of the biggest challenges toward their effective and dehydration mechanism. utilization in this application. Specically, iodine(V) oxides are The accepted mechanism for hydration of I2O5 into iodic hygroscopic to the point of being deliquescent. A pile of di- acids (i.e., HIO3 and HI3O8) and dehydration of iodic acids into 1 iodine pentoxide (I2O5) powder, for example, will absorb so I2O5 (i.e., HIO3 and HI3O8) was rst proposed by Selte et al. and 1 much water from the surrounding atmosphere over time, that shown in eqn (1a) and (1b), respectively. a puddle is produced. This property has limited iodine(V) oxides Hydration: usefulness in energetic applications because an abundance of 3I O +3HO / 2HI O +2HO / 6HIO water can greatly consume liberated energy from a chemical 2 5 2 3 8 2 3 (1a) reaction between iodine(V) oxide and a metal fuel, such as Dehydration: aluminum, thereby inhibiting combustion performance. Understanding, absorption, hydration, desorption and dehy- 6HIO3 / 2HI3O8 +2H2O / 3I2O5 +3H2O (1b) dration mechanisms associated with iodine(V) oxides may enable more tailored synthesis and control over this property In dehydration, six moles of iodic acid in the form of HIO3 for engineering future prompt-agent-defeat technologies (or form three moles of I2O5 and three moles of water with an bio-agent defeat systems). intermediate step involving the formation of two moles of Iodine(V) oxide water absorption behavior is studied exten- HI3O8. In this reaction, water comprises 5.11 wt% of the total sively with inconsistent results that may stem from a limited mass. The mass loss from dehydration of water at each step is understanding of the fundamental kinetics and dynamics of shown in eqn (2). water absorption and reaction with iodine(V) oxides. The inconsistencies highlighted here involve iodine(V) oxides reac- 3HIO3 / HI3O8 +H2O: 3.41% water (2a) tion with water and include: different humidity levels where 2HI3O8 / 3I2O5 +H2O: 1.76% water (2b) aDepartment of Mechanical Engineering, Texas Tech University, Lubbock, TX 79409, Using mass loss from water calculated from eqn (2a) and USA. E-mail: [email protected]; Tel: +1-806-834-3733 (2b), concentrations of iodic acids can be determined from bLynntech, Inc., College Station, TX 77845, USA thermal equilibrium analysis using differential scanning calo- 1,2 † Electronic supplementary information (ESI) available. See DOI: rimetry (DSC) and thermal gravimetric analysis (TGA). The 10.1039/c6ra27854j This journal is © The Royal Society of Chemistry 2017 RSC Adv.,2017,7,10183–10191 | 10183 RSC Advances Paper ff equations used to calculate concentration of HIO3 (XHIO3) and hydration mechanism in eqn (1a). They explain di erent V HI3O8 (XHI3O8) are shown in eqn (3a) and (3b), respectively. hydrated species of iodine( ) oxide can precipitate out when ML% exposed to water and recrystallize depending on impurities, rate HIO3 XHIO ¼ 2 3 3:46% (3a) of evaporation, and crystal structure. This nding is in contrast 1 to Selte et al., where all samples were exclusively HIO3. Little ML% 2 HI3O8 et al. note that multiple iterations of this method produced XHI O ¼ (3b) 3 8 1:76% varying concentrations of iodic acid. Also, a threshold value of 60% RH was found by Little et al.2 to hydrate commercially In eqn (3), ML% is measured mass loss from TGA. The mass available samples without dissolving the solid in water and recrystallization. When commercially available samples are loss percent is divided by the calculated maximum mass loss exposed to air above 60% RH threshold, the product is HIO3 and from eqn (2a) and (2b) for HIO3 and HI3O8 respectively, to obtain the concentration of each iodic acid. The DSC/TGA data when exposed to air below 60% RH, no hydration is observed. Because the commercial sample was entirely HI3O8, a threshold shows an endotherm and mass loss at 110 C, where HIO3 of 60% RH was assumed to be the RH that HI3O8 started dehydrates into HI3O8, followed by an endotherm and mass loss 2 absorbing water. To obtain I2O5, a sample initially HI3O8 was at 210 C, where HI3O8 dehydrates into I2O5. Dehydration of ball milled, and produced a sample 75 wt% I2O5 and 25 wt% HI3O8 has always been observed when HIO3 dehydration was 2 HI3O8. For hydration from I2O5 to HI3O8, Little et al. exposed observed, indicating an intermediate step where HIO3 dehy- 1,2 1 the ball milled samples to 40% RH over a period of several days. drates into HI3O8. In Selte et al. and multiple references within, determination of iodic acid concentration by TGA is The TG analysis indicated increased mass loss at 210 C such conrmed with XRD analysis. The temperatures where the that samples with higher concentrations of I2O5 were hydrated at 40% RH. It is interesting to note that the observation of an onset of iodic acid dehydration begins is widely varied and o en overlooked. endotherm with an onset temperature of 170 C remained constant with increased hydration. An endotherm with an onset A review of the publications over the thermochemical prop- erties of iodine oxides3 summarized data available for reported temperature of 170 C is outside of the range of generally onset temperatures of each dehydration step and decomposi- accepted dehydration temperatures for hydrated species of iodine oxides. Over time with exposure to 40% RH, the endo- tion of I2O5. The onset temperatures reported for I2O5 decom- position are between 300 and 450 C.3 Selte et al. report a lower thermic peak indicating HI3O8 increased and formed a double peak. Commercially available I2O5 was used to study the onset temperature of 280 C for amorphous I2O5, with onset 1 hydration step from HI3O8 to HIO3 (eqn (1a)). No hydration was temperatures between 300 and 420 C for crystalline I2O5. Iodic seen below 50% RH over a period of weeks, however, hydration acids such as HI3O8 onset temperatures are reported between 1 was seen when RH increased to 70% RH. Hydration rates were 195 and 220 C (ref. 1) and between 100 and 130 C for HIO3. The reason for the variation in temperature is not known. measured at 70% RH for HI3O8 to HIO3 (eqn (1a)) and at 40% Formation of hydrated species of iodine oxides is a complex, RH for I2O5 to HI3O8 (eqn (1a)). At 40% RH, the hydration rate went to 0 before 80 wt% of the sample was HI O , but at 70% RH dynamic process that can depend on variables such as relative 3 8 humidity (RH), particle size, hydration and desorption rates, hydration continued until the sample was solely HIO3.In available water, and crystal structure. These variables can be summary, a discrepancy from previous research is that water dependent on each other and could affect properties of the nal absorption thresholds for any iodic acid widely range from 0 to material including dehydration temperature. 85% RH. The reason for the dramatic variation may be due to Relative humidity (RH) has a signicant inuence on the limited understanding of the fundamental mechanism of 1 hydration and dehydration. A better understanding of the oxidation state and kinetics of iodine(V) oxides. Selte et al. fundamental hydration and dehydration kinetics is needed to report that crystalline HI3O8 powder can be stored in open reconcile these discrepancies. vessels for an indenite period independent of atmospheric humidity but ne-powdered samples completely convert to Our goal is to improve the fundamental mechanism of 4 hydration and dehydration of I2O5 by studying hydration and HIO3 in moist air. Kumar et al. studied the deliquescence and ffl dehydration from atmospheric water (i.e. relative humidity). e orescence behavior of I2O5 and HIO3. They describe deli- quescence as the transformation from a solid crystal phase to The objectives are to understand the fundamental absorption an aqueous solution and efflorescence as the reverse, when an mechanism of I2O5; understand how I2O5 reacts with water to aqueous solution crystallizes to a solid phase; and, dene these form iodic acids; and, identify how the reactions between I2O5 ff differences by changes in the optical properties of the sample.
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