Report. Development of a Mechanism to Explain the Action of EcSS 3000 Soil Stabilizer

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1 Report On Development of a Mechanism to Explain the Action of EcSS 3000 Soil Stabilizer By R. Malek Director, Particle Characterization Laboratory, Materials Research Institute, Pennsylvania State University, University Park, PA RQM@PSU.EDU (814) For Environmental Soil Stabilization, LCC Arlington, TX January 5, 2006

2 ABSTRACT The present study has proven that EcSS 3000 TM soil stabilizer alters the integrity of the expansive structure of montmorillonite. X-ray diffraction and NMR studies provide direct evidence and the other supportive studies (BET surface area, cation exchange capacity (CEC), Fourier Transfer Infra Red (FTIR) spectroscopy, zeta potential, thermal analysis, Atterberg limits, and swell test), confirm the action of Ecss 3000 TM soil stabilizer on expansive clays. The major objective of this research was to provide unambiguously direct evidence on the mechanism of action of EcSS 3000 TM soil stabilizer on expansive clay (montmorillonite). The montmorillonite was treated with the 300:1 (water: chemical) diluted soil stabilizer using an application rate in general accordance with that established and typically used by ESSL. The suspension was stirred at 48 o C for 24 hours then filtered, dried and tested. It was found that the interlayer spacing becomes smaller, Al-O-Si bonds are broken and amorphous silica and aluminum are separated. There is evidence that the water content in the interlayer as well as at the outer surface of montmorillonite particles is reduced. Thermal analysis, surface area and particle size measurements confirmed the separation of amorphous Si and Al salt from montmorillonite. The zeta potential was reduced after treatment. Montmorillonite (1) loses its plasticity and lowers its swell potential, and (2) increases its strength after treatment with EcSS 3000 TM. It appears that the mechanism of action of EcSS 3000 TM soil stabilizer on expansive clay can be explained through cation exchange with the interlayer cations, formation of flocs, and catalyzed hydrolysis leading to Si-O-Al bond breaking. This is an irreversible process which leads to stabilization of the soil and enhancement of its strength. BACKGROUND Montmorillonite is a stack of 1 nm thick sheets, where each sheet is composed of an octahedral layer of (Al +3 ) being sandwiched between two tetrahedral layers of Si +4. Montmorillonite particles are negatively charged due to the isomorphous substitution of Al for Si in the tetrahedral sheets and Fe and Mg for Al in the octahedral sheets. This negative charge is compensated for by interlayer cations. Water molecules migrate to hydrate cations causing expansion. There have been some difficulties in identifying unambiguously the mechanism of action of EcSS 3000 TM soil stabilizer due to several reasons unrelated to the actual treatment process. A) Identification of the structure of the treated and untreated soils by the classical X- ray diffraction was difficult due to the already existing high disorder structure in both forms. In addition, the presence of different other components such as silica and calcite makes it difficult to identify clearly the difference between treated and untreated soils.

3 B) Furthermore, it was not possible to determine, with high degree of certainty, the Si and Al distribution in the final product. The 29 Si and 27 Al magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR) which is sensitive for probing such disordered structures was ill defined due to the interference of highly magnetic nuclei (such as iron). C) The problem will be more complicated if the soil was previously treated with calcium compounds (cement, fly ash, lime, etc ) or sulfate compounds (gypsum). D) The hydrophobic properties of the EcSS 3000 TM have not been fully studied in a systematic way. The broad lines of the present research are concentrated around full characterization of pure single form of expansive clay mineral, montmorillonite. a) X-Ray Diffraction METHODS Finely ground powder montmorillonite samples were placed in an engraved, zero background sample holder. The surface of the powder was leveled using a glass slide. In order to avoid preferred orientation of particles, which may produce inaccurate intensity values, a filter paper was placed on the surface of the powder and lightly pressed. Experience has shown that the texture of the filter paper prevents preferred orientation of crystals. The sample holder was then placed in a Scintag X-ray diffractometer and analyzed between angles 2 o to 60 o at a rate of 2 o per minute. Identification of montmorillonite structure by X-ray diffraction is based on the fact that each solid substance has its own characteristic atomic structure which diffracts X-rays in a characteristic pattern. The recognition of the pattern establishes uniquely the diffracting substance. The X-ray reflection takes place from the lattice planes according to Bragg s law: where λ = 2d sin θ... (1) λ is the wave length. θ is the incident angle, and d is the distance between lattice planes. Use was made of the MRL Center for Diffraction Data for analysis of x-ray diffraction data through five databases: ICDD, JCPDS, NIST, FIZ, and NRC.

4 b) Magic Angle Nuclear Magnetic Resonance Spectroscopy The structural changes that occur in expansive clay/soil when treated with EcSS 3000 TM soil stabilizer were studied by using Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy (MAS NMR). As concluded in a previous study, there have been many difficulties in identifying, unambiguously, the structure of the treated clay by the classical methods (such as Transmission Electron Microscopy) due to the high disorder of the products. The 29 Si and 27 Al MAS NMR is superior to other techniques in probing, sensitively, of such disordered structures. It is a valuable technique that provides detailed information such as the length of the aluninosilicate layers and coordination of Al and Si. Therefore in the 29 Si spectra, it is expected to see one or a combination of the following peaks Si-0Al, Si-1Al, Si-2Al, Si-3Al, and Si-4Al, at chemical shifts of 99-93ppm, 90-85ppm, 86-84ppm, ~76ppm, and <76 ppm, respectively. The Si-3Al is expected to be present in abundance in the untreated samples, since it represents the structure of aluminosilicate sheets of the montmorillonite. On the other hand, the Si-0Al, Si-1Al peaks are expected to increase in intensity as the structure disintegrates into small fragments. Thus the MAS NMR is a powerful tool in identifying the structural characteristics of these materials. The 27 Al MAS NMR spectra determines the extent of partition of Al between tetrahedral layers and octahedral interlayer sites. Tetrahedrally coordinated Al should show single resonance characteristically at ppm whereas octahedrally coordinated aluminum gives rise to signals at ~0 ppm. It is expected to see an appreciable increase in the octahedral Al at the expense of the tetrahedral Al as the structure disintegrates. In sum, MAS NMR will enable the determination of the exact structure of the final products which is essential to ensure long term stability of the treated soil. c) Fourier Transfer Infra Red spectroscopy (FTIR) An important aspect of the present study is to determine the effect of EcSS 3000 TM soil stabilizer on the degree of hydration of montmorillonite surfaces. The degree of hydration is related to the magnitude and location of the layer charge (in the octahedral or tetrahedral layers). Montmorillonite has mostly octahedral and to a lesser extent a tetrahedral layer charge. FTIR is most suited for this investigation. Therefore a reduction in the Al-O-Si bonds is an evidence of bond breakage. d) Zeta potential: Clays consist mainly of plate-like particles, which when in contact with water, usually have negatively charged faces. The physical properties of montmorillonite-water systems such as swelling are extremely sensitive to the nature of the electric double layer around the particles. Zeta potential measurements provide particularly relevant information regarding swelling. Zeta potential was measured using the microelectrophoretic mobility technique where the speed and direction of moving particles, under the influence of an electric field, were measured and used to calculate the surface charge.

5 e) Thermal Analysis A small portion of the clay samples were placed in the thermal analyzer and heated at a rate of 10 o C/min up to 1000 o C. The thermal analysis technique is used to characterize materials based on their behavior under various heat conditions. It includes Differential Scanning Calorimetry (DSC) which is used to measure the heat flows associated with physical and chemical changes during heating and Thermogravimetric Analysis (TGA) which is used to measure changes in weight of a sample with increasing temperature. f) BET Surface Area: BET surface area analysis, by gas adsorption, was used to measure the surface area of the clay mineral before and after treatment to determine effect of soil stabilizer on the surface area. The method is based on measuring the amount of nitrogen gas adsorbed (physically) on the surface of the clay mineral at o K (-196 o C) and calculates the surface area from the BET equation: V V m = (1 c( p ) po p )[1 + ( c 1) p ] p p o o Where: V is the volume of gas adsorbed at STP. V m is the volume of gas adsorbed for monolayer coverage p/p o is the relative pressure c is a constant g) Particle size analysis Particle size analysis in the nano size range of the treated and untreated montmorillonite mineral was made by using Photon Correlation Spectroscopy (PCS) which relies on measuring the Brownian motion of small particles and relating this to the hydrodynamic diameter of the particle. Malvern Nanosizer S (0.6 nm to 6 mm) was used. h) Uniaxial compression test (ASTM D 2435): A soil consolidation apparatus was used to measure the strain percent of montmorillonite as a function of applied load. The powder samples were mixed with silica sand (passing #40 sieve) in ratio of 20:80, montmorillonite: sand, before testing. The weight of the specimen was determined and placed in the compression cell and a continuously increasing load is applied. The corresponding change in sample height, after equilibrium, was measured (ASTM D 2435).

6 i) Swell test (ASTM D 4546): Unidimensional swell tests of the treated and untreated montmorillonite samples were measured using the consolidemeter (see h above) according to the ASTM method D The powder samples were mixed with silica sand (passing #40 sieve) in ratio of 20:80, montmorillonite: sand, before testing. j) Cation Exchange Capacity (CEC): An option is to determine the cation exchange capacity of the treated and untreated samples in order to determine the effect of the soil stabilizer on the amount of exchangeable cations. Cation exchange capacity (CEC) is the total amount of cations required to balance the negative charge on the montmorillonite mineral. It is utilized to verify the effectiveness of soil stabilizers. The CEC was measured on the montmorillonite samples without adjusting their ph values which is a more realistic procedure representing the soil in its natural environment.. The CEC was measured on the monmorillonite samples using 0.1M KCl solution at 25 o C. k) Atterberg limits (ASTM D 4318): The objective of the Atterberg limits test is to obtain basic information about the effect of EcSS 3000 TM soil stabilizer on the engineering characteristics of clay mineral. Three limits are tested: Liquid limit(ll): The liquid limit defines the boundary between plastic and viscous fluid states. It is determined using a standard "Liquid Limit Device," (ASTM D 4318) which drops a shallow cupful of soil 1 cm consistently. When a groove cut through the sample closes 1/2", the number of drops is recorded and the moisture content of the sample is calculated. Plastic limit (PL): The plastic limit defines the boundary between non-plastic and plastic states. It is determined simply by rolling a thread of soil and adjusting the moisture content until it breaks at 1/8 inch diameter (ASTM D 3418). Plasticity index (PI): The Plasticity index defines the complete range of plastic state and is equal to the difference between LL and PL. 1- Structure of Montmorillonite RESULTS AND DISCUSSION In order to understand the mechanism of action of EcSS 3000 TM in stabilizing montmorillonite, it is important to start with understanding its structure. Montmorillonite belongs to a group of clay minerals designated as 2:1 clays which generally consists of 1 nanometer thick, negatively charged sheets. In the dry state, the sheets stack by sharing charge-compensating cations (Fig. 1). Most of the negative charge in Montmorillonite results from the octahedral isomorphous substitution and to a lesser extent from the

7 tetrahedral substitution. Water molecules migrate to hydrate cations causing expansion. Due to this negative charge, a double layer of water molecules builds up around clay particles. Exchange of water molecules takes place in the double layer surrounding the clay particles. Si sheet Isomorphous Substitution Al sheet Si sheet Interlayer space 2- Clays and their treatment Figure 1: Structure of Montmorillonite The clays used in this study were: Wyoming Montmorillonite (SWy-1), a synthetic clay- Barassym SSM-400 (Syn-1), and Arizona Montmorillonite (SAz-1). X-ray diffraction has shown that Wyoming Montmorillonite, a sodium montmorillonite, contain considerable amount of quartz and was excluded because of the potential of interfering with the NMR results. Barassym SSM-400 (Syn-1) forms a dense gel with water and some precursors from its synthesis were found remaining which can potentially interfere with the results of this study. Arizona Montmorillonite (SAz-1), a calcium montmorillonite, was found to be appropriate for the present investigation. SAz-1 is also similar to the calcium montmorillnite found in Texas. Ecss 3000 TM soil stabilizer, diluted at 300:1 (water: chemical), was added to SAz-1 montmorillonite using an application rate in general accordance with that established by ESSL. The suspension was stirred at 48 o C for 24 hours in a sealed container then filtered, dried at 50 o C and tested.

8 3- X-Ray Diffraction The influence of Ecss 3000 TM soil stabilizer on the integrity of the structure of Montmorillonite is confirmed by the XRD patterns before and after treatment (Figure 2). Arizona Montmorillonite exhibits a narrow intense d 001 reflection at A, which corresponds to the interlayer spacing. After treatment, this peak becomes broad with much smaller intensity and shifts to a smaller spacing of A. In addition, Gypsum was identified in the XRD pattern after treatment. The appearance of such broad, small intensity peak coupled with the shrinkage of the interlayer spacing and precipitation of gypsum is indicative of the leaching of interlayer cations and transformation to a non expansive structure. Figure 2: XRD of Arizona Montmorillonite before (red) and after (blue) treatment with Ecss 3000 TM soil stabilizer. 4- NMR The 29 Si spectrum of the untreated sample (Figure 3) is dominated by an intense peak at ppm, which is typical of Arizona Montmorillonite. This peak corresponds to Q 3 (0Al) configuration attributed to SiO 4 groups at the tetrahedral sheets branching sites, where silicon is connected to 3 other silicon tretrahedra. Because of the small number of

9 Al in the tetrahedral sheets, Q 3 (1Al) could not be detected relative to the intense Q 3 (0Al) peak. After treatment, the peak intensity decreases (Figure 4). In the meantime, a new peak appears at ppm, which corresponds to Q 4 (0Al) configuration attributed to pure silica, where silicon is connected to 4 other silicon tretrahedra. The broad nature of this peak is indicative of amorphous silica. Additionally, there is a low signal at 102 ppm that is indicative of a small number of (SiO) 3 SiOH localized on structural defects where bond breakage took place. Figure 3: Si NMR of Arizona Montmorillonite before treatment with Ecss 3000 TM soil stabilizer.

10 Figure 4a: Si NMR of Arizona Montmorillonite after treatment with Ecss 3000 TM soil stabilizer.

11 Figure 4b: Si NMR of Arizona Montmorillonite after treatment with Ecss 3000 TM soil stabilizer (Magnified).

12 The 27 Al spectrum of Arizona Montmorillonite (Figure 5) shows a dominant sharp resonance at 3.1 ppm which corresponds to octahedral Al and a very weak tetrahedral resonance at 62.2 ppm. The relative intensity of the Oh/Td Al signal is 46/1. After treatment, there is a shift in the tetrahedral and octahedral signals due to the change in bonding environment as a result of bond breakage (Figure 6). In addition, the octahedral peak seems composed of two peaks at 8.9 ppm and 5.3 ppm. After washing with water (Figure 7), the peak at 5.3 ppm shrinks relative to the peak at 8.9, which is indicative of the existence of a soluble form of Al that was not detected by the XRD. The separation of soluble Al salt is indicative of bond breakage and release of Al into solution. Figure 5: Al NMR of Arizona Montmorillonite before treatment with Ecss 3000 TM soil stabilizer.

13 Figure 6: Al NMR of Arizona Montmorillonite after treatment with Ecss 3000 TM soil stabilizer.

14 5- FTIR Figure 7: Al NMR of Arizona Montmorillonite after treatment with Ecss 3000 TM soil stabilizer then washed with water. The FTIR spectra of the treated and untreated samples are presented in Figure 8. A clear diminution in the intensity of the 916 cm -1 (AlAl-OH), 840 cm -1 (AlMg-OH), and 520 cm -1 (Al-O-Si) bands is reflecting the reduction of octahedral cations and the breakage of Al-O-Si bonds. The persistence of the 520 cm -1 band indicates that not all the Al-O-Si linkages were removed, but the changes in the Si bonding environment makes it susceptible to further removal by prolonged exposure or reexposure to the acidic chemical. But clear evidence on the effect of the chemical on water content in the interlayer is the noticeable decrease in the peak of water at 3627 cm -1. It has been established that water in the interlayer or surrounding the montmorillonite particles are in

15 SAz %T SAz-1-treated %T Wavenumbers (cm-1) Figure 8: FTIR of Arizona Montmorillonite before and after treatment with Ecss 3000 TM soil stabilizer (Magnified). an immobile state and are characterized by the 3627 cm -1 band. The reduction in the intensity of this band after treatment is indicative of the lower water content in the interlayer as well as at the outer surface of montmorillonite particles and of the release of water that was originally bound in the soil-water matrix. 6. Thermal Analysis Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) of Arizona Montmorillonite are presented in Figure 9. The general features are an endothermic peak around 110 o C, and the corresponding weight loss (6.168%) is due to the elimination of physically adsorbed water. Elimination of OH groups (dehydroxylation) appeared at o C (weight loss of 3.797%). An exothermic peak was observed at 862 o C attributed to an exothermic reaction and another exothermic peak at 962 o C due to crystallization of mullite (3AL2O3.2SiO2). After treatment (Figure 10), the physically adsorbed water increases to 10.98% due to the presence of amorphous silica and water of crystallization of the Al salt. In addition, a new endothermic peak (and corresponding weight loss) appears at o C attributed to the decomposition of Al salts.

16 Sample: SAz-1' Size: mg DSC-TGA File: G:\SAz-1'.001 Operator: Malek Run Date: 20-Dec :38 Instrument: 2960 SDT V3.0F % (1.292mg) C 95 Heat Flow (W/g) C C Weight (%) % (0.7411mg) C Exo Up Temperature ( C) Universal V4.1D TA Instruments Figure 9: TGA/DSC of Arizona Montmorillonite before treatment with Ecss 3000 TM soil stabilizer. 7. Zeta potential: Clays consist mainly of plate-like particles, which when in contact with water, usually have negatively charged faces. As a result, water molecules arrange themselves to form a layer around the clay particle. The surface charge decreases gradually as we go towards the bulk liquid. Water molecules arrange themselves in a rather less bound fashion than the first layer forming a diffuse layer. This whole arrangement is termed the electric double layer. At a certain distance from the particle surface there exists a plane of the closest approach between particles. The charge at this plane is known as the zeta potential. The physical properties of clay-water systems such as swelling are extremely sensitive to the nature of the electric double layer around the particles. Zeta potential was measured using the microelectrophoretic mobility technique where the speed and direction of moving particles, under the influence of an electric field, were measured and used to calculate the surface charge. Zeta potential was found to be mv before treatment and it dropped to mv after treatment.

17 Sample: SAz-1-Treated2 Size: mg DSC-TGA File: G:\SAz-1-Treated2.001 Operator: Bo Yi Run Date: 19-Dec :57 Instrument: 2960 SDT V3.0F % (1.623mg) C C 90 Heat Flow (W/g) % (0.8404mg) Weight (%) % (0.4770mg) C Exo Up Temperature ( C) Universal V4.1D TA Instruments Figure 10: TGA/DSC of Arizona Montmorillonite after treatment with Ecss 3000 TM soil stabilizer. 8. Particle size analysis Particle size analysis in the nano size range of the treated and untreated clay mineral was made by using Photon Correlation Spectroscopy (PCS) which relies on measuring the Brownian motion of small particles and relating this to the hydrodynamic diameter of the particle. A Malvern Nanosizer S (0.6 nm to 6 mm) was used. It was noticed that the average particle size shifts to a smaller value after treatment due to the formation of amorphous silica. 9. Surface area: Gas adsorption technique (at o K [-196 o C]) was used to determine effect of EcSS 3000 TM soil stabilizer on the surface area of montmorillonite. The surface area of untreated Arizona Montmorillonite is m 2 /g. After treatment with EcSS 3000 TM, the surface area decreases to m 2 /g. due to the flocculation of small particles into flocs.

18 10. Cation exchange capacity (CEC): Cation exchange capacity (CEC) is the total amount of cations required to balance the negative charge on the montmorillonite mineral. It is utilized to verify the effectiveness of soil stabilizers. The CEC was measured on the monmorillonite samples using 0.1M KCl solution at 25 o C. The CEC of Arizona Montmorillonite was found to be 154 meq/100g and after treatment with EcSS 3000 TM chemical, it drops to 92 meq/100g. This is an indication of the decrease of expansive power after treatment with EcSS 3000 TM soil stabilizer. 11. Atterberg limits: Arizona Montmorillonite before treatment: Liquid limit (LL): 106% Plastic limit (PL); 45% Plasticity Index (PI): 61%. Arizona Montmorillonite after treatment with EcSS 3000 TM soil stabilizer: Liquid limit (LL): 63% Plastic limit (PL); 36% Plasticity Index (PI): 37%. The Atterberg limits were found to be reduced after treatment indicating reduced plasticity, swell potential and compressibility. 12. Swell test: Unidimensional swell tests of the treated and untreated montmorillonite samples were measured using the consolidemeter according to the ASTM method D The unidimensional increase for the untreated montmorillonite was found to be 8.85%, and after treatment with EcSS 3000 TM soil stabilizer, it dropped to 1.48%. 13. Uniaxial compression test (ASTM D 2435): The results of the unidirectional compression tests of the treated and untreated montmorillonite samples are shown in figure 11. It is clear that the two curves are parallel. But the treated sample shows a much less strain percent indicating increase in strength of the montmorillonite as a result of treatment with EcSS 3000 TM soil stabilizer.

19 Strain(%) Treated Untreated Stress (KPa) Figure 11: Stress-strain curves of the treated and untreated montmorillonite samples. SUMMARY AND CONCLUSONS When montmorillonite is treated with EcSS 3000 TM observed: soil stabilizer, the following is The treatment processes are irreversible and do not cause preswelling of the clay. The interlayer spacing is reduced and the interlayer cations are exchanged. Si-O-Al bonds are broken resulting in the separation of amorphous silicon and soluble aluminum from the structure. The surface charge (zeta potential) is reduced. Water originally bound by the clay particles, and within the mineral interlayer is released. Particle size is reduced and surface area is reduced due to flocculation. Cation exchange capacity (CEC) is reduced. Liquid limits (LL), Plasticity limit (PL) and Plasticity index are reduced indicating lower plasticity, swelling and compressibility characteristics. The extent of swelling is greatly reduced. Uniaxial compression test shows an increase in strength of montmorillonite as a result of the treatment with EcSS 3000 TM soil stabilizer.

20 It appears that the mechanism of action of EcSS 3000 TM soil stabilizer can be explained as follows: When EcSS 3000 TM solution is added to clay or soil, it has an immediate effect on the properties of the soil as cation exchange begins to take place between interlayer cations and hydrogen ions in solution. This reduces the density of the electrical charge around the clay particles which leads to them being attracted closer to each other to form flocs, the process is termed flocculation. It is this process which is primarily responsible for the modification of the engineering properties of the clay. So, montmorillonite loses its plasticity immediately. In the meantime, a catalyzed attack on the Si-O-Al bonds in the tetrahedral sheets takes place (organic sulfonate acts as catalyst) causing disintegration and separation of amorphous Si into the floc making them dense and impermeable. These two processes are responsible for the enhanced strength, reduced CEC and stopping expansion.

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