Peter Tremaine. Department of Chemistry, University of Guelph, Canada
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1 Speciation and Thermodynamic Stability of Boric Acid, Borate and Polyborates under PWR Primary Coolant Conditions by AC Conductivity and Raman Spectroscopy Peter Tremaine Department of Chemistry, University of Guelph, Canada OLI Simulation Conference Wyndham Hamilton Park Hotel & Conference Center 175 Park Avenue, Florham Park NJ 7932 USA 2526 October 216
2 Upper Fuel Rod Span Aqueous Boron Chemistry on PWR Fuel Surfaces Fuel Bundles 176 to 264 fuel rods Grid NiFe 2 O 4 SNB NiO NiFe 2 O 4 ZrO2 NiO NiFe 2 O 4 Boiling Chimneys NiO Flow Little or no deposits form immediately downstream of grids due to good mixing / turbulent flow Grid OLI Simulation Conference, 2526 October 216 2
3 Boron Behavior in Fuel Deposits Leads to Crud Induced Power Shifts (CIPS) Li + We seek: Better tools to predict CIPS Li + B(OH) 4 B 2 (OH) 7 Etc. B(OH) 4 B 2 (OH) 7 LiB(OH) 4 B(nonaq liquid) The Challenge: Industry models for boron hideout are based on polyborate data below 2 C LiBO 2(s) Or Li 2 B 4 O 7(s) LiBO 2(s) Li 2 B 4 O 7(s) B 2 O 3(s) Ni(BO 2 ) 2(s) Fe(BO 2 ) 2(s) Ni 2 FeBO 5(s) Current CIPS (AOA) Model Potential Species (Unknown) Closer to Reality OLI Simulation Conference, 2526 October 216 3
4 Thermodynamic Databases for Boron Chemical Equilibrium Models EPRI MULTEQ ChemWorks 4.2, Database Ver 8. OLI Analyzer Studio Wang et al. Pure Appl. Chem. 213, 85, Knowledge Gaps Boric acid ionization constants above 29 o C Polyborate speciation above 2 o C Lithium borate ion pairing above 6 o C Metaborate stability is not well characterized OLI Simulation Conference, 2526 October 216 4
5 Aqueous Boron Chemistry Metaborate Borates Polyborates BO(OH) B(OH) 3 B(OH) 4 B 2 (OH) 5 Ionization and Polyborate Reactions B(OH) H 2 O B(OH) 4 + H 3 O + 2 B(OH) 3 + H 2 O B 2 O(OH) 5 + H 3 O + OR 2 B(OH) H 2 O B 2 (OH) 7 + H 3 O + 3 B(OH) 3 B 3 O 3 (OH) 4 + H 3 O + + H 2 O 4 B(OH) 3 B 4 O 5 (OH) H 3 O + + H 2 O 5 B(OH) 3 B 5 O 6 (OH) H 3 O + OR 5 B(OH) 3 B 5 O 6 (OH) 4 + H 3 O H 2 O Metaborate Formation B(OH) 3 BO(OH) + H 2 O IonPair Formation M + + B(OH) 4 MB(OH) 4 with M = Li, Na or K OLI Simulation Conference, 2526 October 216 5
6 Research Targets For PWR Operating Conditions, 25 to 35 o C Part I: Borates Boric acid ionization constants Borate association constants with Li +, K + and Na + AC Conductivity Cell Part II: Polyborates Structures and speciation of polyborate species Sapphire Raman Cell Part III: Models Revise MULTEQ database for aqueous boron species Capillary Raman Cell OLI Simulation Conference, 2526 October 216 6
7 Part I: Boric Acid Ionization Constants and Ion Pairing by Flow AC Conductivity
8 Supercritical Conductivity Flow Cell Zimmerman et al., J. Phys. Chem Zimmerman, Arcis, Tremaine. J. Chem. Eng. Data 212 Capabilities: Stateoftheart operating range 4 o C, 28 MPa, 1 5 mol kg 1 Measures concentration of charged species B(OH) 3 + H 2 O B(OH) 4 + H + Li + + B(OH) 4 LiB(OH) Pump 1 Pump 2. Sample Loop O n kw nf 5 Hz Peristaltic Pump Ar Back Pressure Regulator Solution Water reservoir Waste Flow cell Waste OLI Simulation Conference, 2526 October 216 8
9 Experimental Challenges Ionization Constants Very weak ionization of B(OH) 3 B(OH) 3 + H 2 O B(OH) 4 + H + B(OH) 4 Limiting Conductivities Limited data above 6 C Ion Pair Formation Constants Competing equilibria are challenging B(OH) 4 B(OH) 3 + OH Li + + B(OH) 4 LiB(OH) 4 Li + + OH LiOH 2% LiOH New Measurements 38 solutions, 8 temperatures, AC impedance analysis for each 8% 7% 6% 5% 4% 3% 1% % Relative concentrations of Boron Species at 3 o C T = 3 o C.8 mol/kg LiB(OH) 4.15 mol/kg NaB(OH) 4 LiB(OH) 4 NaB(OH) 4 B(OH) 3 B(OH) 4 MB(OH) 4 B 2 (OH) 7 MOH OLI Simulation Conference, 2526 October 216 9
10 Experimental Measurement of Borate Limiting Conductivities: 25 to 3 o C Experimental Limiting Conductivities of Borate: λ o [B(OH) 4 ] vs. T Simultaneous Regression Determines λ o [B(OH) 4 ] and K A Below 25 o C, Values for KB(OH) 4 are best less competition from KOH Above 3 o C: Extrapolate using difference fit to triflate ion as a model system: First accurate limiting conductivity data for borate to 3 o C OLI Simulation Conference, 2526 October 216 1
11 Experimental Borate IonPairs Formation Constants: 25 to 35 o C Borate IonPair Formation Constants Log K vs. Temperature (T / K) M + + B(OH) 4 MB(OH) 4 LiB(OH) 4 KB(OH) 4 NaB(OH) 4 35 o C IonPair Formation: At 25 C K A [Li] > K A [K] K A [Na] Above15 C: K A [Li] K A [K] K A [Na] 25 o C 175 o C This work Pokrovski et al. (1995) Corti et al. (198) Density model: Fitted with a density model : b f log KA a c T e T T log w Association constants for LiB(OH) 4, NaB(OH) 4 and KB(OH) 4 are the same to within the experimental uncertainty under PWR coolant conditions OLI Simulation Conference, 2526 October
12 Experimental Boric Acid Ionization Constants: 25 to 35 o C B(OH) 3 : K 11 vs. Temperature 5 o C B(OH) 3 + OH B(OH) 4 Mesmer et al. (1972) This Work 35 o C Experimental Ionization Constants B(OH) 3 + OH B(OH) 4 B(OH) 3 : K 11, 275 to 35 o C Palmer 2 MPa, p sat 275 o C New experimental values Consistent with extrapolations of Oak Ridge density model by Palmer et al. (2) Ionization constants agree within ±1% 2 MPa, p sat This work Guelph (215) Sirota et al. (198) Mesmer et al. (1972) Tremaine and Bulemela (26) 35 o C OLI Simulation Conference, 2526 October
13 Summary Boric Acid Ionization Constants and Ion Pairing Limiting Conductivity of B(OH) 4 Direct measurements from 25 to 3 o C IonPair Formation Constants: LiB(OH) 4, KB(OH) 4 and NaB(OH) 4 Direct measurements from 25 to 35 o C First experimental values for Li + above 4 o C K A [LiB(OH) 4 ] K A [KB(OH) 4 ] K A [NaB(OH) 4 ] under PWR coolant conditions Ionization Constants: B(OH) 3 + H 2 O B(OH) 4 + H + First accurate experimental data above 3 o C Consistent with extrapolated Oak Ridge density model (Palmer et al. 2) OLI Simulation Conference, 2526 October
14 Part II: Polyborate Speciation by Raman Spectroscopy
15 Low and High Temperature Raman Cells Raman spectroscopy sees the characteristic vibrations of each species using polarized light I I 4/3I iso Quartz tube Macro chamber Sapphire flow cell 2 o C, p sat 3 o C, 2 MPa OLI Simulation Conference, 2526 October
16 High Temperature Raman Cells Quartz Capillary Cell: 5 o C, 3 MPa Capillary Cell O.D. 36 μm I.D. 2 μm Fused Silica Capillary Cell and Ferrule Holding Mount Optical Window Silver Heating Block OLI Simulation Conference, 2526 October
17 Ab Initio Borate Species and Polyborates BO(OH) Ion Pairs Borate species LiB(OH) 4 NaB(OH) 4 KB(OH) 4 Solventseparated No Raman spectrum Maya, Inorg. Chem (1976) Zhou et al., Spectrochim. Acta A, (211) This work, Applegarth et al., J. Phys. Chem. B (submitted) Not in the databases OLI Simulation Conference, 2526 October
18 Polyborates Characterization by Raman Spectroscopy at 25 and 8 o C Reduced Isotropic Raman Spectra for Concentrated NaB(OH) 4 Solutions at 25 and 8 o C Total Experimental Matrix 17 solutions at 25 and 8 o C Na/B ratios (R buffer ) from to 2 These spectra: Na/B ratios from. to.9 Concentration Dependence Confirms OLI model for major species at 25 & 8 o C Yields temperatureindependent relative scattering coefficients for polyborates Is pentaborate B 5 O 6 (OH) 6 3 OR B 5 O 6 (OH) 4? OLI Simulation Conference, 2526 October
19 Pentaborate Species from Ab Initio Calculations Cory Pye Dept. of Chemistry, St. Mary s University, Halifax B 5 O 6 (OH) 4 Symmetry: D 2d B 5 O 6 (OH) 6 3 A Symmetry: C 2 Theoretical Frequency 545 cm 1 Strong B Confirmed by Observed Frequency 53 cm 1 Strong HF Basis sets 631G* Also done with B3LYP & MP2; basis sets 631+G*, 6311+G* Theoretical Frequencies: 52 cm 1 Medium 547 cm 1 Weak 56 cm 1 Medium 68 cm 1 Medium OLI Simulation Conference, 2526 October
20 Normalized Raman intensity Reduced Isotropic Raman Spectra of Aqueous Polyborates to 3 o C Reduced Isotropic Raman Spectra of BoricAcidRich Aqueous Sodium Borate from 25 to 3 o C B 5 O 6 (OH) 4 B 3 O 3 (OH) 4 B(OH) 4 3 C B(OH) 3 Total Experimental Matrix 3 solutions from 25 and 3 o C Na/B ratios from.1 to Wavenumber (cm 1 ) 25 C ClO 4 This Spectrum Na/B ratio R buffer =.13 Total boron, m B tot =.847 m.5. R buffer =.13, m B tot =.847 m B 3 O 3 (OH) 4 B(OH) 4 Major (Poly)Borates in Solution B(OH) 4 B 3 O 3 (OH) 4 B 5 O 6 (OH) 4 (trace) Wavenumber (cm 1 ) B 3 O 3 (OH) 4 OLI Simulation Conference, 2526 October 216 2
21 Normalized Intensity Raman (a.u.) intensity Boric Acid under NearCritical Conditions Speciation and Phase Behaviour Raman Spectra Isotropic Spectra of ~.9 Molal Boric Acid with Perchlorate (Internal Standard) Phase Behaviour Boiling of ~.9 Molal Boric Acid at Fixed Pressures 15 MPa 347. o C degrees 1 degree 15 degree 2 degree 25 degree 3 degree B(OH) 3 3 o C 25 o C Shows no metaborate! B(OH) 3 ClO 4 ClO 4 Liquid Phase 2 MPa 38.7 o C Gas Phase Wavenumber (cm 1 1 )) OLI Simulation Conference, 2526 October
22 Summary Borate Speciation and Phase Behavior Low Temperature Measurements (t < 1 o C) Observe SIX polyborate species in solution Structures confirmed by ab initio calculations Pentaborate species is B 5 O 6 (OH) 4 not B 5 O 6 (OH) 3 6 LiB(OH) 4 ion pairs cannot be observed Sapphire Flow Cell Measurements up to 3 o C, 2 MPa Confirm triborate species B 3 O 3 (OH) 4 in buffers, < Na/B < 1 Quartz Capillary Cell Measurements up to 5 o C, 3 MPa Confirmed boric acid species is B(OH) 3 not metaboric acid BO(OH) No liquidliquid phase separation observed Experiments limited by precipitation at 25 o C OLI Simulation Conference, 2526 October
23 Part III: Update of the MULTEQ Database for Aqueous Boron species
24 Proposed Update of the Aqueous Boron Databases Ionization Constants for Boric Acid Equations for Log K from Palmer et al. (2) fully compatible with experiments Revised Entries for Borate and Hydroxide Ion Pairs B(OH) 3, B(OH) 4, Minor change LiB(OH) 4, KB(OH) 4 and NaB(OH) 4 Based on these experimental data up to 35 o C LiOH, KOH and NaOH Based on recent Oak Ridge data New fit for LiOH might impact predicted ph values Revised Entries for Polyborate Species B 2 (OH) 7, B 3 (OH) 1, and B 4 (OH) 14 2 taken from Palmer et al. (2) Based on Mesmer potentiometric titrations up to 2 o C Pentaborate inconsistent with Raman studies B 5 O 6 (OH) 4 should be included New values for limiting conductivities at 25 o C Measurements continue to quantify polyborates above 2 o C OLI Simulation Conference, 2526 October
25 Acknowledgements Project Staff Conductivity Measurements Dr Hugues Arcis, PhD student Jane Ferguson, Prof. Greg Zimmerman Raman Spectroscopy and ab initio Calculations Dr. Lucas Applegarth, Dr. Swaroop Sasidharanpillai, Prof Cory Pye, Dr. Jenny Cox EPRI Project Managers Dr. Daniel M. Wells; Dr. Dennis Hussey Funders EPRI: Agreement EPP43257/C18781 OLI Systems: Software Donation Dr. Peiming Wang, Dr. Andrzej Anderko Canadian Foundation for Innovation OLI Simulation Conference, 2526 October
26 The Hydrothermal Chemistry Group University of Guelph, 216 OLI Simulation Conference, 2526 October
27 Future Work Update of the Aqueous Boron MULTEQ Database Polyborate Species Should be revised based on their correct structures B 2 O(OH) 5, B 3 O 3 (OH) 4 and B 4 O 5 (OH) 4 2 NOT B 2 (OH) 7, B 3 (OH) 1, and B 4 (OH) 14 2 Must characterize the new unknown species observed by Raman spectroscopy Include pentaborate B 5 O 6 (OH) 4 in the database Refit data from Mesmer and Baes and from Weres Including: ALL correct polyborate species New hydroxide ion pairs New borate ion pairs Revised the activity coefficient model for neutral borate species Not consistent with the revised boron database by Guelph OLI Simulation Conference, 2526 October
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