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Title: PERMEABILITY OF SALTSTONE MEASUREMENT BY BEAM BENDING

Abstract

One of the goals of the Saltstone variability study is to identify (and, quantify the impact of) the operational and compositional variables that control or influence the important processing and performance properties of Saltstone mixes. A performance property for Saltstone mixes that is important but not routinely measured is the liquid permeability or saturated hydraulic conductivity of the cured Saltstone mix. The value for the saturated hydraulic conductivity is an input into the Performance Assessment for the SRS Z-Area vaults. Therefore, it is important to have a method available that allows for an accurate and reproducible measurement of permeability quickly and inexpensively. One such method that could potentially meet these requirements for the measurement of saturated hydraulic conductivity is the technique of beam bending, developed by Professor George Scherer at Princeton University. In order to determine the feasibility of this technique for Saltstone mixes, a summer student, David Feliciano, was hired to work at Princeton under the direction of George Scherer. This report details the results of this study which demonstrated the feasibility and applicability of the beam bending method to measurement of permeability of Saltstone samples. This research effort used samples made at Princeton from a Modular Caustic sidemore » solvent extraction Unit based simulant (MCU) and premix at a water to premix ratio of 0.60. The saturated hydraulic conductivities for these mixes were measured by the beam bending technique and the values determined were of the order of 1.4 to 3.4 x 10{sup -9} cm/sec. These values of hydraulic conductivity are consistent with independently measured values of this property on similar MCU based mixes by Dixon and Phifer. These values are also consistent with the hydraulic conductivity of a generic Saltstone mix measured by Langton in 1985. The high water to premix ratio used for Saltstone along with the relatively low degree of hydration for MCU based mixes leads to high total and capillary porosities. These two conditions generally lead to higher permeabilities as has been well documented in the literature for typical cementitious pastes in water. Therefore, it is not unexpected that the hydraulic conductivities of these Saltstone mixes are relatively high.« less

Authors:
; ;
Publication Date:
Research Org.:
SRS
Sponsoring Org.:
USDOE
OSTI Identifier:
923832
Report Number(s):
WSRC-TR-2007-00437
TRN: US0802190
DOE Contract Number:
DE-AC09-96SR18500
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
12 MANAGEMENT OF RADIOACTIVE WASTES, AND NON-RADIOACTIVE WASTES FROM NUCLEAR FACILITIES; 36 MATERIALS SCIENCE; RADIOACTIVE WASTES; HYDRAULIC CONDUCTIVITY; PERMEABILITY; MEASURING METHODS; FEASIBILITY STUDIES; PERFORMANCE

Citation Formats

Harbour, J, Tommy Edwards, T, and Vickie Williams, V. PERMEABILITY OF SALTSTONE MEASUREMENT BY BEAM BENDING. United States: N. p., 2008. Web. doi:10.2172/923832.
Harbour, J, Tommy Edwards, T, & Vickie Williams, V. PERMEABILITY OF SALTSTONE MEASUREMENT BY BEAM BENDING. United States. doi:10.2172/923832.
Harbour, J, Tommy Edwards, T, and Vickie Williams, V. 2008. "PERMEABILITY OF SALTSTONE MEASUREMENT BY BEAM BENDING". United States. doi:10.2172/923832. https://www.osti.gov/servlets/purl/923832.
@article{osti_923832,
title = {PERMEABILITY OF SALTSTONE MEASUREMENT BY BEAM BENDING},
author = {Harbour, J and Tommy Edwards, T and Vickie Williams, V},
abstractNote = {One of the goals of the Saltstone variability study is to identify (and, quantify the impact of) the operational and compositional variables that control or influence the important processing and performance properties of Saltstone mixes. A performance property for Saltstone mixes that is important but not routinely measured is the liquid permeability or saturated hydraulic conductivity of the cured Saltstone mix. The value for the saturated hydraulic conductivity is an input into the Performance Assessment for the SRS Z-Area vaults. Therefore, it is important to have a method available that allows for an accurate and reproducible measurement of permeability quickly and inexpensively. One such method that could potentially meet these requirements for the measurement of saturated hydraulic conductivity is the technique of beam bending, developed by Professor George Scherer at Princeton University. In order to determine the feasibility of this technique for Saltstone mixes, a summer student, David Feliciano, was hired to work at Princeton under the direction of George Scherer. This report details the results of this study which demonstrated the feasibility and applicability of the beam bending method to measurement of permeability of Saltstone samples. This research effort used samples made at Princeton from a Modular Caustic side solvent extraction Unit based simulant (MCU) and premix at a water to premix ratio of 0.60. The saturated hydraulic conductivities for these mixes were measured by the beam bending technique and the values determined were of the order of 1.4 to 3.4 x 10{sup -9} cm/sec. These values of hydraulic conductivity are consistent with independently measured values of this property on similar MCU based mixes by Dixon and Phifer. These values are also consistent with the hydraulic conductivity of a generic Saltstone mix measured by Langton in 1985. The high water to premix ratio used for Saltstone along with the relatively low degree of hydration for MCU based mixes leads to high total and capillary porosities. These two conditions generally lead to higher permeabilities as has been well documented in the literature for typical cementitious pastes in water. Therefore, it is not unexpected that the hydraulic conductivities of these Saltstone mixes are relatively high.},
doi = {10.2172/923832},
journal = {},
number = ,
volume = ,
place = {United States},
year = 2008,
month = 1
}

Technical Report:

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  • The Engineering Process Development Group (EPD) of the Savannah River National Laboratory (SRNL) prepared simulated saltstone core samples to evaluate the effect of sample collection by coring on the permeability of saltstone. The Environmental Restoration Technology Section (ERTS) of the SRNL was given the task of measuring the permeability of cores of simulated saltstone. Saltstone samples collected from Vault 4 Cell E using both dry and wet coring methods were also submitted for permeability analysis. The cores from Vault 4 Cell E were in multiple pieces when they were recovered (Smith, 2008 Cheng et.al, 2009). Permeability testing was only performedmore » on the portions of the core sample that were intact, had no visible fractures or cracks, and met the specifications for 'undisturbed specimens' identified in Method ASTM D5084-03 Standard Test Methods for Measurement of Hydraulic Conductivity of Saturated Porous Materials Using a Flexible Wall Permeameter that was used for the testing. Permeability values for cores of simulated saltstone compared with values from permeability tests conducted on molded saltstone samples by an independent laboratory using the same method. All hydraulic conductivity results for Vault 4 samples exceeded results for both molded and cored saltstone simulant samples. The average hydraulic conductivity result for Vault 4 Cell E samples of 3.9 x 10{sup -7} cm/sec is approximately two orders of magnitude greater than that of the simulated saltstone with an average of 4.1 x 10{sup -9} cm/sec. Numerical flow and transport simulations of moisture movement through saltstone performed for the performance assessment of the Saltstone Disposal Facility (SDF) used 2.0 x 10{sup -9} cm/sec for the hydraulic conductivity of saltstone (Flach et al, 2009). The results for simulated versus actual saltstone were further compared using non-parametric statistics. The results from non-parametric statistical analysis of results indicate that there is at least a 98% probability that the hydraulic conductivity of saltstone samples collected from Vault 4 Cell E saltstone is greater than that of the baseline simulant mix.« less
  • This report focuses on the impact of curing temperature on the performance properties of simulated Saltstone mixes. The key performance property of interest is saturated liquid permeability (measured as hydraulic conductivity), an input to the Performance Assessment (PA) modeling for the Saltstone Disposal Facility (SDF). Therefore, the current study was performed to measure the dependence of saturated hydraulic conductivity on curing temperature of Saltstone mixes, to correlate these results with measurements of Young's moduli on the same samples and to compare the Scanning Electron Microscopy (SEM) images of the microstructure at each curing temperature in an effort to associate thismore » significant changes in permeability with changes in microstructure. This work demonstrated that the saturated liquid permeability of Saltstone mixes depends significantly on the curing temperature. As the curing temperature increases, the hydraulic conductivity can increase over three orders of magnitude from roughly 10{sup -9} cm/sec to 10{sup -6} cm/sec over the temperature range of 20 C to 80 C. Although an increased aluminate concentration (at 0.22 M) in the ARP/MCU waste stream improves (decreases) saturated permeability for samples cured at lower temperatures, the permeabilities for samples cured at 60 C to 80 C are the same as the permeabilities measured for an equivalent mix but with lower aluminate concentration. Furthermore, it was demonstrated that the unsaturated flow apparatus (UFA) system can be used to measure hydraulic conductivity of Saltstone samples. The permeability results obtained using the UFA centrifuge system were equivalent within experimental error to the conventional permeameter results (the falling head method) obtained at MACTEC. In particular the UFA technique is best suited for the range of hydraulic conductivities between 10{sup -10} cm/sec to 10{sup -6} cm/sec. Measurements of dynamic Young's moduli (E) for these mixes revealed a correlation between E and hydraulic conductivity. Therefore, it is possible to use E values to estimate the values of hydraulic conductivity. Measurement of Young's modulus is much easier than the measurement of permeability of Saltstone mixes and facilitates the measurement of the time dependence hydraulic conductivity. The results presented in this report show that changes in permeability as a function of curing temperature appear to be related to microstructural changes in the cured Saltstone mixes. Backscattered electron microscopy images revealed significant differences between the samples cured at different temperatures.« less
  • Radioactive liquid effluent from the In Tank Precipitation Process is mixed with Portland cement, flyash and furnace alag to form Saltstone. The Saltstone is poured into vaults at Z Area for long term disposal. A transient heat transfer model of the Saltstone pouring process was previously written to determine whether the Saltstone temperature would exceed the Technical Specification Limit of 95 degrees C. The present work was performed to provide Saltstone density, heat capacity, heat of hydration and thermal conductivity for inclusion in the model.
  • This report provides initial results on the measurement of heat of hydration of Saltstone mixes using isothermal calorimetry. The results were obtained using a recently purchased TAM Air Model 3116 Isothermal Conduction Calorimeter. Heat of hydration is an important property of Saltstone mixes. Greater amounts of heat will increase the temperature of the curing mix in the vaults and limit the processing rate. The heat of hydration also reflects the extent of the hydraulic reactions that turn the fluid mixture into a ''stone like'' solid and consequently impacts performance properties such as permeability. Determining which factors control these reactions, asmore » monitored by the heat of hydration, is an important goal of the variability study. Experiments with mixes of portland cement in water demonstrated that the heats measured by this technique over a seven day period match very well with the literature values of (1) seven day heats of hydration using the standard test method for heat of hydration of hydraulic cement, ASTM C 186-05 and (2) heats of hydration measured using isothermal calorimetry. The heats of hydration of portland cement or blast furnace slag in a Modular Caustic Side Solvent Extraction Unit (MCU) simulant revealed that if the cure temperature is maintained at 25 C, the amount of heat released over a seven day period is roughly 62% less than the heat released by portland cement in water. Furthermore, both the blast furnace slag and the portland cement were found to be equivalent in heat production over the seven day period in MCU. This equivalency is due to the activation of the slag by the greater than 1 Molar free hydroxide ion concentration in the simulant. Results using premix (a blend of 10% cement, 45% blast furnace slag, and 45% fly ash) in MCU, Deliquification, Dissolution and Adjustment (DDA) and Salt Waste Processing Facility (SWPF) simulants reveal that the fly ash had not significantly reacted (undergone hydration reactions) after seven days (most likely less than 5%). There were clear differences in the amount of heat released and the peak times of heat release for the three different simulants. It turns out that SWPF simulant mixes give off greater heat than does MCU and DDA simulant mixes. The temperature dependence of the heat of hydration was measured by carrying out these measurements at 25, 40 and 55 C. In general, the peak times shifted to shorter times as the isothermal temperature increased and the amount of heat released was independent of temperature for DDA and MCU but slightly higher at higher temperatures for SWPF. The goal of this study is to apply this technique to the measurement of the heat of hydration of mixes that will be made as part of the variability study. It is important to understand which variables will impact (and to what extent) the amount of heat generated and the peak times for the heat release. Those variables that can be controlled can then be tuned to adjust the heat of hydration as long as the other properties are still acceptable. The first application of heat of hydration measurements to the variability study was completed and the results presented in this report. These measurements were made using Phase VI mixes (SWPF simulants) following a statistical design that included variation in the compositional and operational variables. Variation in both the amount of heat released and the peak times for the heat release were observed. The measured ranges were 23 Joules per gram of premix for the heat release and 23 hours for the peak time of heat release at 25 C. Linear models with high R{sup 2} values and no statistical evidence for lack of fit were developed that relate the amount of heat release and the peak time for heat release for the Phase VI mixes to certain variables. The amount of heat released was a function of the aluminate and portland cement concentrations as well as the temperature of mixing. The peak time for heat release was a function of aluminate, portland cement and total nitrate plus nitrite concentrations. A comparison was made of the measured values of heat release by isothermal calorimetry to a previous study of the measurement of the heat of hydration using adiabatic calorimetry by Steimke and Fowler. After 80 hours of reaction time, the two techniques provided heat release results that were roughly in the same range. However, additional experiments at higher isothermal temperatures will be required to see how well the two measurements agree for longer times. This is due to the higher temperatures that are experienced in adiabatic calorimetry ({approx}105 C).« less
  • One of the goals of the Saltstone Variability Study is to identify the operational and compositional variables that control or influence the important processing and performance properties of Saltstone mixes. One of the key performance properties is porosity which is a measure of the volume percent of a cured grout that is occupied by salt solution (for the saturated case). This report presents (1) the results of efforts to develop a method for the measurement of porosity of grout samples and (2) initial results of porosity values for samples that have been previously produced as part of the Saltstone Variabilitymore » Study. A cost effective measurement method for porosity was developed that provides reproducible results, is relatively fast (30 to 60 minutes per sample) and uses a Mettler Toledo HR83 Moisture Analyzer that is already operational and routinely calibrated at Aiken County Technology Laboratory. The method involves the heating of the sample at 105 C until no further mass loss is observed. This mass loss value, which is due to water evaporation, is then used to calculate the volume percent porosity of the mix. The results of mass loss for mixes at 105 C were equivalent to the results obtained using thermal gravimetric analysis. The method was validated by comparing measurements of mass loss at 105 C for cured portland cement in water mixes to values presented in the literature for this system. A stereopycnometer from Quantachrome Instruments was selected to measure the cured grout bulk densities. Density is a property that is required to calculate the porosities. A stereopycnometer was already operational at Aiken County Technology Laboratory, has been calibrated using a solid stainless steel sphere of known volume, is cost effective and fast ({approx}15 minutes per sample). Cured grout densities are important in their own right because they can be used to project the volume of waste form produced from a given amount of salt feed of known composition. For mixes made from either Modular Caustic Side Solvent Extraction Unit (MCU) or Salt Waste Processing Facility (SWPF) simulants in premix, the porosities averaged near 62 % with an uptake of water through hydration reactions equivalent to a water to cementitious materials ratio (w/cm) of 0.04. For a mix made from a Deliquification, Dissolution and Adjustment (DDA) simulant and premix, the porosity is slightly lower at 57 % with an uptake of water through hydration reactions equivalent to a w/cm ratio of 0.07. Data are presented which demonstrate that porosity is inversely related to the heat of hydration, a measure of the extent of the hydration reactions. Modeling of porosities from three of the statistically designed phases of the Saltstone Variability Study demonstrated that the data could be fit to a linear model with an R2 of 0.74 and no statistical evidence for a lack of fit. The model revealed that w/cm ratio plays a significant role in the total porosity with porosity increasing as the w/cm ratio increases. Other elements of the model include positive correlations with the free hydroxide ion concentration and the total nitrate plus nitrite ion concentration. For a series of mixes in which the composition of the salt solution remained constant (MCU baseline) the porosity increased from {approx}60 to 65 % as the w/cm ratio increased from 0.55 to 0.65.« less