MICROWAVE REFLECTION AND DIELECTRIC PROPERTIES OF MORTAR EXPOSED PERIODICALLY TO 2% CHLORIDE SALT SOLUTION AND COMPRESSION FORCE J.T. Case1, E. Gallaher1, S. Peer1, R. Zoughi1, and K.E. Kurds2 Applied Microwave Nondestructive Testing Laboratory (amntl), Electrical and Computer Engineering Department, University of Missouri-Rolla, Rolla, MO 65409, USA 2 School of Civil and Environmental Engineering, Georgia Institute of Technology, Atlanta, GA 30332, USA ABSTRACT. The corrosion of reinforcing steel in a concrete structure may compromise the strength, stiffness, impermeability, and long-term performance of the structure. Near-field microwave nondestructive testing (NDT) techniques are believed to offer an alternative to many existing destructive methods for chloride detection. To assess the potential of microwave NDT for this purpose, mortar cubes were produced and were cyclically exposed to a 2% NaCl solution, and their daily near-field microwave reflection properties were measured for three cycles each lasting 110 days. In an effort to investigate the combined effects of loading and environmental exposure, one of the samples was periodically exposed to compression loading. Details of the measurement approach and the results are presented in this paper. INTRODUCTION Corrosion of steel compromises the strength and integrity of reinforced concrete structures, and the presence of chlorides is known to be the predominant cause of damage [1]. Techniques exist to detect chloride and its migration into concrete structures, however many are destructive and time consuming. In recent years, near-field microwave nondestructive testing (NDT) techniques have been used to evaluate properties of cement based materials [2]. It has also been shown that these same techniques can detect the presence of chlorides that have penetrated into these materials [3-5]. In the present investigation, four mortar cubes were prepared all with the same constitutes. One was soaked in a salt solution and loaded to simulate the combinations of environmental exposure and loading to be expected in service. One was soaked in the salt solution and not loaded. One was soaked in distilled water to provide a comparison to the previous cubes. The last cube was kept in ambient conditions and was neither soaked nor loaded to serve as the reference. Soaking was administered cyclically for three cycles to further simulate the real environment and promote chloride ingress. Throughout the experiment, microwave reflection properties of the cubes were measured at S (2.6-3.95 GHz) and X (8.2-12.4 GHz) bands. Also, masses of the cubes were monitored daily to provide a CP657, Review of Quantitative Nondestructive Evaluation Vol. 22, ed. by D. O. Thompson and D. E. Chimenti © 2003 American Institute of Physics 0-7354-0117-9/03/$20.00 1132 comparison to the microwave data. This paper presents the results of these measurements along with a discussion of the results. EXPERIMENT Four 8"x8"x8" mortar cubes were prepared with water-to-cement (vv/c) ratio of 0.5 and sand-to-cement ratio (s/c) of 2.5 using Type I/II Portland cement. All cubes were allowed to cure in a hydration room for one day and subsequently stored in ambient conditions for 11 months. Subsequently, the top surface of each cube was ground to evenness using a 6" flat rotating disk grinder to allow even distribution of the loading, to be described later. Microwave reflection properties of the cubes were monitored at S(2.6-3.95 GHz / 4 points per side) and X- (8.2-12.4 GHz / 9 points per side) microwave bands using open-ended rectangular waveguide probes and a calibrated vector network analyzer (HP8510C) for three soaking cycles. Probes were placed flush against the surface of the cube for each measurement. Each cycle included soaking two cubes in a 2% sodium chloride solution and one in distilled water for 72 hours in three individual covered containers. Each cube was placed on small spacers supporting the corners to allow unimpeded water ingress into the bottom. Also, the top one centimeter of the cube was not submerged. The fourth cube was kept in ambient conditions and never exposed to any solution or loading, serving as the reference cube. This cube may also serve to provide information concerning the influence of ambient conditions (i.e., variations in relative humidity and temperature). After soaking, the microwave reflection properties of all four cubes were measured immediately and then daily for 110 days. During this time, mass of the cubes and ambient conditions were also monitored and recorded. The second and third cycles differed from the first in that one of the cubes previously soaked in salt solution was loaded hours before soaking. Loading was administered using a 120,000 Ib capacity Tinius and Olson testing machine to load the cube at a rate of 300 Ib/s (136 kg/s) to approximately half of its compressive strength (1400 psi or 9.65 MPa). The cube was then immediately unloaded at the same rate. RESULTS Water has much higher dielectric properties than mortar and air [6]. Consequently, the magnitude of microwave reflection coefficient, henceforth referred to as |F|, is expected to be larger for moist samples compared to dry. This can be seen in the first cycle for S-band in Figure 1 where |F| for cubes following soaking is much greater than the reference cube. |F| for the second day after soaking is much lower than |F| for the first day, since during the first 24 hours of the drying cycle much of the surface moisture is lost to evaporation. As the cubes dry, one may notice that |F| for the cubes soaked in salt water decreases at a slower rate than the cube soaked in distilled water. This is believed to be due to the hygroscopic nature of salt, which tends to hold water, thereby reducing the rate of evaporation [3]. This phenomenon is also seen for phase of microwave reflection coefficient, henceforth referred to as (p, in Figure 2. Another reason that a separation exists in the (p of the salt water and distilled water soaked cubes is that the dielectric properties of the 2% sodium chloride solution are markedly different from those of distilled water. Salt water has a greater loss factor than distilled water, and as a result absorbs more microwave energy and also causes q> to be lower [6]. It is important to note that in Figure 2, (p for salt water soaked cubes dips at the beginning of the cycle and then increases. Since the cube soaked in distilled water also exhibits this behavior, the phenomenon for the salt water cannot solely be due to increasing salinity of the pore solution which causes the loss factor 1133 -water, no load —a—saltwater, loaded —A—saltwater, no load —0—reference 0.65 100 150 200 250 300 350 FIGURE 1. Magnitude of microwave reflection coefficient at S-band (3 GHz). - water, no load -saltwater, loaded - saltwater, no load —O— reference FIGURE 2. Phase of microwave reflection coefficient at S-band (3 GHz). to increase [6]. This dip has been attributed to the location of the peak of the water content inside the cube [7]. As expected at the end of the first cycle, |F| and (p are similar for salt water soaked cubes because no loading had yet taken place. It also can be seen that the soaked cubes had not fully dried during the cycle. Later cycles reveal similar traits. Noted exceptions are that |F| decreases more rapidly initially and the dip in (p becomes less prominent as a function of cycle number. Results at X-band contrast highly with those at S-band as seen in Figures 3 and 4. The most striking feature is that at X-band |F| for all soaked cubes drops immediately to a value lower than that for the reference cube and continues to decrease and then increases asymptotically to a final value. Although X-band has a shorter depth of penetration than S-band, the cubes cannot possibly appear drier than the reference at this frequency because phase information in Figure 4 reveals that the cubes are still moist. To explain this phenomenon, a simple computational experiment was carried out at X-band involving a rectangular waveguide aperture radiating into a dry layer of mortar backed by a moist layer 1134 - water, no load —a— saltwater, loaded —£— saltwater, no load —-0— reference 0.675 50 100 150 200 250 300 350 FIGURE 3. Magnitude of microwave reflection coefficient at X-band (10 GHz). - water, no load -saltwater, loaded —A— saltwater, no load - reference FIGURE 4. Phase of microwave reflection coefficient at X-band (10 GHz). of mortar [8]. Dielectric properties for the dry layer and the moist layer were calculated using reflection properties of the reference cube and first day of measurement of the water soaked cube, respectively [2]. The microwave reflection properties were then calculated for this setup over a range of thicknesses of the dry layer [8]. The results in Figure 5 show that indeed |F| can be lower than the reference even when the cube is still moist. Phase results are consistent, but not shown. This calculation was confirmed using multiple layers whose dielectric properties were estimated using a moisture profile, thereby proving that the cube during the active drying cycle is drier towards the surface. As mentioned earlier, the mass of each cube was recorded daily. The average additional mass per unit volume for each cube was calculated by subtracting the dry mass of the cubes from daily mass measurement and dividing that value by the total volume. Figure 6 shows the average additional mass per unit volume, hereafter referred to as additional mass, for all three cycles. It is readily apparent that additional mass behaves 1135 -simulated 1 2 - reference 3 4 Thickness (mm) FIGURE 5. Simulated results at X-band (10 GHz) as a function of dry layer thickness. —O— water, no load —O— saltwater, loaded —&— saltwater, no load - reference FIGURE 6. Additional Mass per unit volume. similarly to |F| for S-band, as shown in Figure 1. This is because S-band detects the moisture inside the cube and additional mass is the mass of the solution inside the cube. The reason that the two plots do not look more similar is due to the fact that S-band microwave measurements can distinguish water distribution and additional mass cannot. Therefore, additional mass averages all moisture and cannot distinguish moisture at the core from moisture at the surface. On the other hand, S-band results are sensitive to moisture distribution, and |F| is especially high when moisture is near the surface. Still, the agreement between the two measurements stands as a confirmation of microwave measurement. Loading and salt deposition effects can unfortunately not be seen readily from the plots of microwave reflection properties at this time. Similar experiments in the past revealed both effects, so the records were checked. Indeed it was found that the salt water soaked cube that was not loaded dried in different conditions than the other cubes. This 1136 caused faster drying rates for the first quarter of the cycle especially towards the surface as shown in Figure 1. Since the drying of cubes is so dependent on ambient conditions, a good comparison between loaded and no load samples does not exist. In a previous experiment, loading effects could be seen as a decrease in |F| and an increase in (p [4]. This is because loading causes existing microcracks to propagate and new microcracks to form, which increases the effective porosity and permeability of the sample [1]. The loaded cube is then expected to dry faster as a function of cycle, thereby decreasing |F| and increasing (p. Additional mass is not as sensitive to surface conditions as microwave results are, and the present experiment agrees with similar experiments conducted in the past [4]. This is why at the end of each cycle additional mass for the cube exposed to load slowly decreases toward the cube not exposed to load as the number of cycles increases. It is believed that at the end of the fourth cycle, the additional mass for the cube exposed to load will actually be less than the cube not exposed to load, overcoming any initial difference between the two. Therefore, additional mass results in this experiment show effects of cyclical loading. However, at present, microwave results do not show loading effects as clearly as in the previous investigation and more study is necessary to better understand the obtained microwave results [4]. Salt ingress can be detected by comparing salt water and distilled water soaked cubes. Deposited crystalline salt and chemically bound chlorides fill the pores and substitute for air, thereby increasing the dielectric properties of the cube and causing |F| to increase with respect to the water soaked sample [9]. This is not evident in Figure 1. However, additional mass at the last day of the cycle for the salt water soaked sample increases compared to the distilled water soaked cube as a function of cycle. Further analysis of the data and a modeling effort are underway to better explain the microwave results as they pertain to loading and salt deposition. SUMMARY Results of daily microwave reflection measurements were presented for four mortar cubes. One was soaked in distilled water, one was left in ambient conditions, and two were soaked in 2% salinity NaCl solution, one of which was loaded to half of its compressive strength. The purpose of this experiment was to determine whether near-field microwave reflection properties could observe effects of a cyclical chloride exposure regimen combined with loading. S-band results show a significant difference between the water and the salt water soaked cubes, especially for the first cycle. Also, results at this frequency reveal sensitivity to moisture distribution, and X-band results are even more sensitive to layering due to its higher frequency. Features of additional mass were also correlated with S-band results. Loading and salt deposition analysis is still underway. It is important to note that microwave reflection properties for water and salt water soaked cubes are distinguishable and they are both substantially different from an unaltered specimen. However, further study is required to better relate the measurements to physical changes in the samples with loading and exposure; a modeling effort is underway. ACKNOWLEDGEMENT The funding for this work has been provided by the National Science Foundation Grant no. NSF CMS-0196158. 1137 REFERENCES 1. Mehta, P.K. and PJ.M. Monteiro, "Concrete: Structure, Properties, and Materials," 2nd Ed, Prentice Hall, Englewood Cliffs, New Jersey, 1993, pp. 160-176. 2. Bois, Karl, "Near-Field Microwave Inspection and Characterization of Cement Based Materials," Ph.D. Dissertation, Department of Electrical and Computer Engineering, Colorado State University, Fort Collins, CO 1999. 3. Case, J.T., R. Zoughi, K. Donnell, D. Hughes and K.E. 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