Marine Georesources & Geotechnology ISSN: 1064-119X (Print) 1521-0618 (Online) Journal homepage: http://www.tandfonline.com/loi/umgt20 Cementation of Sand Due to Salt Precipitation in Drying Process Jia He & Jian Chu To cite this article: Jia He & Jian Chu (2016): Cementation of Sand Due to Salt Precipitation in Drying Process, Marine Georesources & Geotechnology, DOI: 10.1080/1064119X.2016.1168498 To link to this article: http://dx.doi.org/10.1080/1064119X.2016.1168498 Accepted author version posted online: 30 Mar 2016. Submit your article to this journal Article views: 4 View related articles View Crossmark data Full Terms & Conditions of access and use can be found at http://www.tandfonline.com/action/journalInformation?journalCode=umgt20 Download by: [Gazi University] Date: 05 April 2016, At: 10:26 Cementation of Sand Due to Salt Precipitation in Drying Process Jia He Lecturer, College of Civil and Transportation Engineering, Hohai University, Nanjing, China Downloaded by [Gazi University] at 10:26 05 April 2016 Jian Chu* Professor, School of Civil and Environmental Engineering, Nanyang Technological University, Singapore Abstract Salt in soil can cause cementation effect and increase the shear strength and stiffness of soil during the drying process. In this paper, an experimental study is presented to explore the strength, stiffness, and particle level structure of a salt-cemented sand at the dry state. Unconfined compression tests were carried out on sands with various amounts of precipitated dry salt. Scanning electric microscopic and elemental analysis were also conducted. The study shows that the strength and stiffness of sand can increase significantly with salt content. The strength versus salt content curve displays a convex shape, instead of a concave shape as found in cemented or biocemented sands. This implies that the effect of dry salt on soil strength is strong at low level of salt content. The microscopic and elemental analysis evidence that salt tends to precipitate at particle contacts and form bridges between particles at relatively low salt content. The results presented in the paper may explain why even small amount of salt can lead to an overestimation of soil strength. 1 Keywords: cementation, salt precipitation, sand INTRODUCTION Recently, there have been a lot of studies on the effect of biocementation on sand using the microbial induced carbonate precipitation (MICP) approach (Chu et al. 2013; DeJong et al. 2013; Li 2015). In the MICP method, calcium chloride salt is usually used as a regent. Past studies have indicated that the presence of salt can affect the strength of soil. When the salt used for the MICP Downloaded by [Gazi University] at 10:26 05 April 2016 process has not been fully consumed, the strength of the biocemented sand can be attributed to both biocementation and cementation by dry salt. For example, Li (2015) reported that, in the use of biocement for strengthening sands, residual calcium chloride in soils led to an overestimation of soil strength in the dry state, see Figure 1. It is also reported that a very small amount of salt (as low as 0.065%) can greatly change the small-strain stiffness of soil at dry state (Truong et al. 2012). Under these circumstances, it is of research interest to understand the effect of precipitated salt on the strength of soils. Another objective of this paper is related to the soil strength and slope stability in the seashore areas. At the water fluctuation zones of seashore areas, soil may undergo drying and wetting processes, which leads to the variations in the soil strength. This variations in the soil strength could be ascribe to several mechanisms: the change in the matric suction and osmotic suction, and the precipitation or dissolving of salt when soil dries or wets. The last mechanism has not been fully realized in the past. It is reported in limited studies that precipitated salt could be relevant to the weakening of loess and saline skbkha in a wetting process (Abduljauwad and AlAmoudi 1995; Rinaldi, Santamarina, and Redolfi 1998; Cho and Santamarina 2001). The overlook 2 of the effect of precipitated salt in soil may cause an overestimation of soil strength and slope stability, especially in seashore areas. Salt (either calcium chloride, sodium chloride or other salts) can affect the soil properties in different ways. When salts are dissolved in pore water, they will give rise to osmotic suction, which in turn alters the compression and swelling behavior, Atterberg limits, shear strength, and maximum dry density of soil (Mitchell and Soga 2004; Ajalloeian et al. 2013; Xu et al. 2014). Downloaded by [Gazi University] at 10:26 05 April 2016 Another way that ionic salts affect soil behavior is that, as soil is drying, ionic concentration in pore water increases and eventually reaches the saturated state, leading to the precipitation and crystallization of salts. These dry salts tend to accumulate at particle contacts where water menisci dry out, bridge soil particles, and enhance greatly the shear strength and stiffness of soils. There were only limited research studies related to this topic in the past (Abduljauwad and Al-Amoudi 1995; Lin et al. 2005; Truong et al. 2010; Truong et al. 2012; Li 2015). In natural conditions especially arid regions, salts affect strongly the mechanical behavior of soil and influence related geotechnical problems. Abduljauwad and Al-Amoudi (1995) studied the behaviour of a salty soil under soaking and leaching conditions. The soil in the wetting process showed that percolation of clean water through the soil led to destruction of natural cementation, causing an increase in settlement and a reduction in bearing capacity of soil ground; percolation of brine water through the soil did not have major influence on the soil behaviour. Lin et al. (2005) reported that, sandstones that contain dissolved minerals such as chlorite can be weakened during a wetting process, due to the loss of dissolved components in the sandstones. Collins and Sitar (2009) showed that, weakly-cemented and moderately-cemented sands manifested considerable reduction in strength during wetting. Nowadays, chemical and biochemical modifications of soil are becoming widely used. Soluble salts used in the soil treatment processes may also affect the 3 soil behaviour (Li 2015). The abovementioned studies aimed at investigating the discrepancies of soil behaviour between dry and wet states. However the formation process of salt precipitation and the relationship between salt content and mechanical behaviour of soil is still not well understood. Studies on the properties of salt-cemented soil are still rare. A few published papers include Truong et al. (2012), who studied the small strain behaviour of salt-cemented sand using elastic wave methods. They concluded that salt-induced cementation can increase the small strain stiffness of Downloaded by [Gazi University] at 10:26 05 April 2016 sand even with a salt content as low as 0.065%. It is also interesting to note that methods have been proposed to preferably form cementing agents at particle contacts, and thereby cemented soil can be much stronger than those using conventional cementation methods. Valdes and Cortes (2014) proposed a method of using polymer to strengthen sand. In heating and cooling process, polymer tends to accumulate at sand particle contacts. The strength of such specimens is much higher than that of sand treated with Portland cement. In biocement methods, a common way to treat bulky soil is to percolate treatment liquid through soil body and cementation can be formed along flow path. It is concluded by Cheng et al. (2013) that, in the treatment process, if degree of saturation can be controlled at a low level, more calcite accumulates at particle contacts. The soil can be much stronger than that treated at fully saturated conditions. From these studies, we can see that the formation and the spatial distribution of cementing agents (either Portland cement, biocement, or precipitated salts) play an important role in the strength of cemented soils. So it is a practical need to study the behavior of cemented soil with cementing agents preferably formed at particle contacts. It is also deserve pointing out that, the type of cementing agent may affect the strength and stiffness of host soil, because of the difference in the strengths and the morphologies of cementing crystals. However, it is not in the scope of this study. 4 Although research evidences have shown that salt precipitation can play an important role in the strength of dry soil, a direct relationship between salt content and strength of host soil was not seen in the past. Salt is omnipresent in natural soils (but is usually overlook in geotechnical laboratories). This paper may shed light on the effect of salt on the variation of soil strength in natural conditions, especially oceanic environments. In this paper, an experimental study on the strength, stiffness, and particle level structure of salt-cemented sand was carried out. A series of cylindrical samples were prepared with different salt contents. Unconfined compression tests were Downloaded by [Gazi University] at 10:26 05 April 2016 conducted. Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray Spectroscopy (EDX) analysis was used to analyze particle level structure. TESTING METHODS River sand (W9 grade, Gs = 2.63, D50 = 0.25 mm, poorly graded, sub-rounded, quartz content > 99%) was used. Calcium chloride was used as the cementing agent. It is one of the chemicals used in MICP-based biocement. The specimens were prepared in cylindrical PVC tubes with rubber stoppers. The size of the PVC tubes was 3.8 cm in diameter and 7.6 cm in length. Brine water was prepared by dissolving calcium chloride in de-ionized water. The concentration of calcium chloride in brine water ranges from 6.5 ~ 37.5%. The specimens were prepared by depositing dry sand into brine water in the PVC tubes. The dry mass and volume of sand was controlled to be the same for all the specimens. Extra brine water above the sand surface was removed. The specimens prepared in this way had a void ratio around 0.69. Then the specimens were moved to an oven at a temperature of 60°C for 5 days. At this stage, the specimens were not completely dry, but cementation or capillary effects were formed and the specimens could stand without support. The PVC tubes were taken off. The specimens were oven dried at the temperature of 105°C until they were completely dried. The specimens were kept in a sealed container to avoid 5 moisture absorption. The determination of salt contents at different parts of one specimen showed that salt content in the specimen was relatively even and the specimen can be taken as a uniform piece. Unconfined compression tests were conducted. The strain rate was 1 mm/min. The tested specimens were then used to determine salt contents. Salt mass was determined by weighing the specimen before and after rinsing it in distill water. Some small pieces of the specimens were used Downloaded by [Gazi University] at 10:26 05 April 2016 for particle level structure and elemental analysis, using SEM and EDX apparatus. RESULTS AND DISCUSSIONS Strength Data of unconfined compression strength (UCS) versus salt content are plotted in Figure 2. Another two trend lines are also drawn in Figure 2. One is sand treated with Portland cement (Consoli et al. 2010), and another is sand treated with biocement using the MICP method (Li 2015). The sand used in this study and the study by Li (2015) is the same. The sand used by Consoli et al. (2010) is also a poorly-graded clean quartz sand. Its mean size (D50) is 0.16 mm, which is a little smaller than the size of the sand used in this study. The effective cementing agent in biocement is calcite, a mineral consisting of calcium carbonate. For salt-cemented specimens, the UCS increases with the salt content. Within the range of 1.9 ~ 15% salt content, the UCS increases from 0.05 to 9.1 MPa. The strength of cemented and biocemented sands also show an increasing trend as the cement content increases, but the strength is much lower in the same tested range. Within the range of cement content of 5 ~ 12%, the UCS of cemented and biocemented soils are only 1/2 to 1/4 of that of the dry salt-cemented specimens. Another difference is that the trend line of the UCS of the salt-cemented specimens manifests a convex shape, that is, adding salt is more 6 effective in the lower range of salt content in terms of strength improvement. The trend lines for the cemented and biocemented treated sand are concave. This is related to the spatial distribution of cementing agents in soils pores, which will be discussed later in the paper. Stiffness The stiffness of the specimens is evaluated using the Young’s modulus determined from the unconfined compression tests. The Young’s moduli versus salt content for all the tested Downloaded by [Gazi University] at 10:26 05 April 2016 specimens are plotted in Figure 4. As salt content increases from 1.9 to 15%, the Young’s modulus shows an ascending trend from 17 to 1,600 MPa. For relatively weak specimens (UCS < 0.2 MPa), the cementation effect in the specimens progressively fails during compression, which leads to soil-like the stress-strain curves, as shown in Figure 3a. The modulus is determined as the tangential gradient at the origin point. For relatively strong specimens (UCS > 0.8 MPa), the stress-strain curves display a rock-like pattern, showing an increasing trend in gradient in the initial part of the curves and becoming linear at the latter stage of compression, as shown in Figure 3b. This stress-strain pattern could be due to the compression of small pores in the specimens in the initial stage of compression (Hoek and Martin 2014). The modulus is determined using the gradient of the linear part of the stress-strain curve. The boundary of the two types of stress-strain curves is likely to be within 2.7–3.1% range of salt content. Particle Level Structure SEM and EDX images of some salt-cemented samples are presented in Figure 5. The SEM image of a specimen with 6.5% salt content is shown in Figure 5a. It can be seen that two sand particles are bridged by salt precipitation. The salt precipitation takes on the shape of a water meniscus. This particle level structure is evidenced by the EDX elemental analysis (Figure 5b), 7 which shows that salt (Ca and Cl elements) lies between two sand particles (Si and O elements). However, there are also some Ca and Cl elements on the particle surfaces. This could be due to the drying of absorbed water on sand particles. Figure 5c, d present two SEM images with 6.5% and 12.9% salt contents, respectively. The difference between the two images is that: the specimen with 6.5% salt content has a lot of pore voids; the specimen with 12.9% salt content manifests that salt precipitates distribute continuously among sand grains (although some voids may not be seen from the image). Such a phenomenon is related to the water content and the morphology of water Downloaded by [Gazi University] at 10:26 05 April 2016 phase when saline water reach its solubility and salt starts to precipitate. In an unsaturated soil, water will be accumulate at soil particle contacts and form water menisci at relatively low water contents (namely pendular stage). But at relatively high water contents, water phase will be continuous (namely funicular stage). It is also reported that salt precipitation tend to form at soil particle contacts at pendular stage and contribute greatly to the small-strain stiffness (Cho and Santamarina 2001). The particle level analysis given above can explain some strength and stiffness features of salt-cemented sand as displayed in Figures 2 and 4. As salt precipitation are preferably formed at soil particle contacts, its contribution to the strength is larger than other cementation methods, where cementing agents are more randomly distributed in soil pores. But when salt content increases, meniscus-shaped salt bridges between sand particles cannot be formed. In this range of salt content, the cementation effect of salt becomes weaker. This is why UCS-salt content relationship shows a convex shape. CONCLUSIONS 8 This paper presents an experimental study on the effect of salt precipitation on strength and stiffness of sand at dry state. Within a range of 1.9% to 15% salt content, the dry specimens show great increases in both strength and stiffness. The strength versus salt content curve displays a convex shape, instead of a concave shape as found in sands treated with Portland cement or biocement. The SEM images of salt-cemented sand reveal that, at a relatively low level of salt content, salt tends to precipitate at particle contacts and bridge sand particles together, while at a high salt content, salt precipitates tend to distribute continuously among sand particles. This Downloaded by [Gazi University] at 10:26 05 April 2016 explains why salt precipitation contributes greatly to the strength of salt-cemented sand, but the strength increasing trend becomes slower as salt content increases. Acknowledgements This work is supported by Jiangsu Science Foundation Project BK20150814, China Postdoctor Science Foundation Project 2015M581714, and Jiangsu Postdoctor Research Foundation Project 1501026C. References Abduljauwad, S. N., and O. S. B. Al-Amoudi. 1995. Geotechnical behaviour of saline sabkha soils. 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H. Eom, Y. H. Byun, and J. S. Lee. 2010. Characteristics of elastic waves according to cementation of dissolved salt. Vadose Zone Journal Soil Science Society of America 9 (3):662–69. doi:10.2136/vzj2009.0131 Truong, Q. H., C. Lee, Y. U. Kim, and J. S. Lee. 2012. Small strain stiffness of salt-cemented granular media under low confinement. Géotechnique 62 (10):949–53. doi:10.1680/geot.10.t.004 Xu, Y., G. Xiang, H. Jiang, T. Chen, and F. Chu. 2014. Role of osmotic suction in volume change of clays in salt solution. Applied Clay Science 101:354–61. doi:10.1016/j.clay.2014.09.006 Valdes, J., and D. Cortes. 2014. Heat-induced bonding of sands. In Proceedings of Geo-Congress 2014 Technical Papers, Atlanta, Georgia, USA, 3721–33. 10 Downloaded by [Gazi University] at 10:26 05 April 2016 Figure 1. UCS versus calcite content for biocemented sands at wet and dry conditions (data from Li 2015). 11 Downloaded by [Gazi University] at 10:26 05 April 2016 Figure 2. UCS versus content of cementing agents. 12 Downloaded by [Gazi University] at 10:26 05 April 2016 Figure 3. Unconfined compression curve of salt-cemented sand specimens with (a) 2.3% and (b) 3.7% salt content. 13 Downloaded by [Gazi University] at 10:26 05 April 2016 Figure 4. Stiffness of salt-cemented sand. 14 Downloaded by [Gazi University] at 10:26 05 April 2016 Figure 5. SEM and EDX analysis of salt-cemented sand (a) A SEM image of the specimen with 6.5% salt content (×800 magnification); (b) EDX analysis of Si, O, Ca and Cl elements on the specimen in (a); (c) A SEM image of the specimen with 6.5% salt content (×50 magnification); (d) A SEM image of the specimen with 12.9% salt content (×50 magnification). 15