Chemical Oxidation Using Fenton s Reagent: Lessons Learned

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1 Chemical Oxidation Using Fenton s Reagent: Lessons Learned Konrad J. Banaszak, Ph.D., L.P.G. KERAMIDA Environmental, Inc. 330 North College Avenue Indianapolis, Indiana Andrew A. Gremos, L.P.G., C.H.M.M. KERAMIDA Environmental, Inc. 330 North College Avenue Indianapolis, Indiana Stanley A. Hunnicutt, NRCC-EAC, C.H.M.M. KERAMIDA Environmental, Inc. 330 North College Avenue Indianapolis, Indiana KEYWORDS Fenton s, alkalinity, ISCO, chemical oxidation ABSTRACT The choice to employ Fenton s Reagent as the remedial alternative is based heavily on two factors, (1) the geology of the site, and (2) the chemistry of the aquifer. The geology must be appropriate to allow the dispersal of reagent, and the chemistry of the saturated zone must not overly deplete the oxidation potential of the reagent. Several pilot tests were conducted at the sites to evaluate the dispersal of reagents in the subsurface. The data show a marked heterogeneity in the effective dispersal of reagents in the subsurface. In addition, alkalinity of the subsurface water and soil is important to regulating whether the Fenton s reaction can take place. High alkalinity groundwater can negate the application of acid to reduce the groundwater ph. Data from sites indicated that the ph of the groundwater drops rapidly from 7.5 to approximately 6.0 and any additional acid is effectively buffered. 1. INTRODUCTION The Fenton s reaction was discovered in and has more recently been used for the degradation of organic compounds in soil and groundwater 2,3,4. Fenton s reaction is the addition of ferrous iron to hydrogen peroxide to produce a hydroxyl radical, a hydroxide ion, and ferric iron. H 2 O 2 + Fe 2+ OH + OH - + Fe 3+ Hydroxyl radicals (OH ) are known to be one of the most powerful oxidizing agents available to remediation scientists. This reaction produces hydroxyl radicals very efficiently when the ph is between 3 and 5. (Note that the product side of Fenton s reaction has hydroxide. That means that relatively high activities of hydroxide favor the reactant side, clearly working against the production of hydroxyl radicals.) The purpose of generating the oxidative power of the hydroxyl 1

2 radical is the destruction of organic contaminants through oxidation. This process has been proved to be effective on several occasions 2,3,4. However, Fenton s reaction has also been shown to be ineffective on several occasions. These occasions are not typically published due to their lack of success, but these apparent failures are caused by two factors: (1) applying the technology to sites where it is inappropriate and (2) inadequate concentrations or quantities of reagents. The first category of failures is applying the technology to sites where it is inappropriate. One situation where the technology has been misapplied is sites where the contamination is present in tight clays. When this is the case, distribution of the reagents is difficult and the chance of having all of the contaminants come in contact with reagent is very small. Another is applying the reagents to the wrong subsurface zone. Without careful planning of the application process, the reagents can be applied to an area where no contaminants exist. Furthermore, a poorly planned application can lead to pushing the contaminants around and expanding the plume rather than degrading it. The second category of failures is the use of inadequate concentrations or quantities of reagents. This can happen for two reasons. The first is a poorly designed bench test, which does not take into consideration the true site conditions. This can take place by omission of solid phase materials or ignoring the natural oxidant demand (NOD) present in the site soils and groundwater. The second reason for failure is improper scaling up of the bench test results to the full-scale application. An inadequate amount of reagent for the degradation of all organic contaminants at the site is the result. This paper discusses two sites where the hydrogeology and proper bench-scale tests indicated that Fenton s Reagent should work, but where factors beyond these lead to failure. 2. SITE A The first site that matches this description is an industrial facility in the Midwest (Site A). Site A was contaminated with high concentrations of chlorinated solvents such as 1,1,1-trichloroethane, 1,1-dichloroethane, and vinyl chloride. The contaminants were confined to a small area and were located within a sand and gravel zone, which varied from two to eight feet thick. This sand and gravel zone was confined above and below by tight clay loam zones. This situation seemed ideal for the application of Fenton s reagent. The reagent easily could be introduced to the subsurface zone with minimal surfacing due to the confining clay layer. In addition, the sand and gravel should be the best possible subsurface medium for the uniform distribution of the reagents. The application of Fenton s reagent at Site A was meticulously planned. A bench test was conducted using site soils and deionized water to prove that the technology would, in fact, destroy the contaminants located on the site. After the success of the bench test, a pilot test was conducted to test the results of the bench test under actual site conditions. Reagent concentrations were based on the bench test results and the reagents were applied in two areas of the site. Reagents were mixed in two 300-gallon polyethylene tanks: one with acid and ferrous iron and one with hydrogen peroxide. The reagents were then pumped to the distribution points by the use of two double diaphragm pumps and a manifold system, which allowed for distribution of each reagent or both reagents to up to four separate distribution points. The distribution points consisted of 1¼-inch diameter stainless steel rods advanced to the desired depth of application by the use of a Geoprobe push-probe rig. Each rod was fitted with a 2

3 disposable tip. Once the desired depth was reached, the Fenton s pumps were connected to the stainless steel rod and reagent was introduced to the rod. The resultant pressure deployed the disposable point from the end of the rod and reagent flowed into the subsurface. Distribution points were installed on a grid with 3½ foot spacing within the pilot test areas. Each area of the pilot test was located around a monitoring well so that the results of the bench test could be assessed through sampling the monitoring wells. Favorable results were obtained from the pilot test including a 37% reduction of contaminant concentrations in the effected monitoring wells. The full-scale application was then planned to begin on the downgradient side of the plume and work upgradient, thus limiting the spreading of the plume by working against the groundwater gradient. The full-scale application used the same reagent mix, delivery methods, and distribution point spacing as the pilot test. However, the results of the full-scale application were mixed. Results indicate anywhere from a 52% decrease to a 48% increase in concentrations depending on the individual constituent and monitoring well. The 52% decrease was likely due to effective Fenton s reaction, as 37% could be expected. Large increases were likely due to pushing more highly contaminated groundwater into the monitoring points. The range from 52% reduction to no reduction is likely the result of an ineffective application for geochemical reasons, as the site material allowed easy injection. One piece of data that may provide part of the answer is the ph results for samples collected after application was complete. None of these ph results were below 6. This ph level is not sufficiently low to allow the Fenton s reaction to proceed efficiently. It was noted that Site A and many other sites where Fenton s technology has failed are located in the Midwest. This typically means that the aquifer alkalinity is very high. High alkalinity groundwater is a buffer solution, which effectively negates the application of acid to reduce the groundwater ph. Also interfering were percent levels of reactive carbonate, mostly calcite, in the solid that buffered the system despite reasonable additions of acid. Aquifer alkalinity refers to both the alkalinity of the groundwater and solid materials that compose the aquifer. The bench test and scale up were acceptable to general industry standards, but did not consider the heterogeneity in the field of conductance, of geochemistry, of the solid phases, of the actual chemistry of the groundwater, or of the likely equilibrium of the groundwater and solid in the aquifer. The physical heterogeneity likely led to uneven distribution of the reagent. Hence the areas of better and of worse than expected impact. The heterogeneity of the geochemistry likely exacerbated these outcomes. The bench test used deionized water, but the site groundwater was highly alkaline and reduced. Finally, the groundwater/solids equilibrium of the aquifer led to a system highly buffered in its redox and ph. This buffering, including reactions of carbonate and iron-bearing minerals with water, likely kept the geochemical conditions in redox and ph conditions unfavorable to Fenton s reaction. 3. SITE B These ideas were tested to some level at another facility. Site B is also an industrial facility located in the Midwest. It is contaminated with chlorinated solvents, which are present in a sand and gravel aquifer. In addition, this site has a high aquifer alkalinity very similar to that observed at Site A. A Fenton s pilot test was already planned for Site B based on similar prior testing, such as bench scale testing, as at Site A. This pilot test was modified to allow for monitoring of the aquifer ph. Field ph was monitored during two Fenton s pilot tests at Site B. The first pilot test was designed to monitor the horizontal distribution of the reagents and consisted of one injection 3

4 point surrounded by five monitoring points at distances of 5 to 28.5 feet from the injection point. The monitoring points were designated PZ-1, PZ-2, PZ-3, RW-3, and SVE-8. The injection points used in this pilot test were installed in the same manner as those used at Site A above. Field ph was monitored during the Fenton s applications by the use of a peristaltic pump and a Hydrolab Quanta G water quality meter with a flow cell. Disposable polyethylene tubing was installed in each monitoring point to the desired depth. The tubing was then run to a central location where the Hydrolab was set up. Each location was monitored in turn using the same Hydrolab so that instrument variation would not be a factor. As each monitoring point was sampled and the groundwater was allowed to fill the flow cell, the ph was measured and recorded. The results for the first pilot test are presented in Figure 1. Two separate injection points 8 34' 11:53-12: ' 12:35-13:15 Figure 1: Change in ph Over Time - Pilot Test #1 Injection 1 Injection 2 26' 14:35-15:05 33' 15:14-15: ' 16:04-16:55 25' 17:15-17: /28/03 7 3/19/ /12/03 PZ-1 (5') PZ-2 (9.5') PZ-3 (18') RW-3 (5') SVE-8 (28.5') Time were used and three different depths of injection were used for each injection point. The distances of the monitoring points from the injection points are shown in the legend after the monitoring point designation. It would be expected that the ph of groundwater with no buffer capacity would asymptotically approach that of the reagents (ph<2). However, in four out of five monitoring points, the ph of the groundwater drops rapidly from 7.5 to approximately 6.0. At this point the ph is buffered by the aquifer alkalinity. The ph does not drop any lower with the continued addition of reagent. In addition, groundwater samples collected from RW-3 at one, two, and three weeks following the pilot test showed an immediate rebound to preapplication levels of ph (Figure 1). Monitoring point RW-3 is the only true monitoring well used as a monitoring point. All other monitoring points are temporary wells with no screen packs. The fact that the ph of RW-3 is one full standard unit less than any other observation point implies that a preferential pathway exists to this monitoring point, possibly induced by the screen pack around the monitoring well. This is one possible reason why concentrations of contaminants have been observed to rebound to pre-application levels at some sites 5. It is possible that the reagents are preferentially treating the monitoring wells where samples are collected. This would result in samples collected immediately after completion of the application exhibiting much lower concentrations of contaminants. Then, after several months of equilibration in the subsurface environment, the concentrations return to pre-application levels due to the migration of virtually untreated groundwater flowing into the monitoring well. 4

5 The second pilot test, also conducted at Site B, consisted of three injection points arranged around a single monitoring point. The injection points were installed in the same manner as the pilot test described above and the monitoring point was a monitoring well (MW-2) in which samples were collected from two distinct depths in an effort to evaluate the vertical distribution of the reagents. The results of the second pilot test are presented in Figure 2. Two separate monitoring points were located in the same Figure 2: Change in ph Over Time - Pilot Test # ph Time ph (23') ph (26') ph (3/12-3/28) monitoring well at different depths. The depths are indicated in the legend. It is again observed that the ph of the groundwater drops rapidly from 7.5 to approximately 6.2. At this point the ph is again buffered by the aquifer alkalinity and does not drop any lower with the continued addition of reagent. The extremely low value at 12:13 is attributed to the brief incursion of raw reagent to the monitoring well. 4. RETURN TO SITE A The third pilot test consisted of four injection points arranged around one monitoring point. The injection points were installed in the same manner as the previous pilot tests and the monitoring point was a monitoring well in which samples were collected from only one depth. This test was undertaken to determine whether the use of high volumes of concentrated acid would overcome the alkaline buffer system. In order to test this theory, the normal use of citric acid was replaced with 10% sulfuric acid. The results of the third pilot test (Figure 3) indicate that the same phenomenon is occurring at both sites. 5

6 Figure 3: Change in ph Over Time - Pilot Test # ph 5.00 ph Time In addition, the use of sulfuric acid did not allow for the aquifer alkalinity to be overcome. Approximately 500 gallons of 10% sulfuric acid were injected into the subsurface at four points located within two feet of the monitoring point. The net result was that the ph did not drop below 5. This ph effectively stops the Fenton s process because the optimum ph for the Fenton s reaction is between 3 and DISCUSSION In conclusion, the use of the traditional Fenton s reaction in high alkalinity systems is not feasible. Even if enough acid could be introduced to overcome the alkalinity and lower the ph below 5, it would be cost prohibitive. In order for Fenton s reaction to be effective in these systems, a catalyst would be needed to accelerate the reaction at neutral ph. This may be the case in several proprietary approaches 6. 6

7 REFERENCES 1. Luong, H. V.; Lin, H. K. Anal. Lett. 2000, 33(14), DeHgi, B.; Hodges, A. In Remediation of Chlorinated and Recalcitrant Compounds 2002; Gavaskar, A. R.; Chen, A. S. C., Ed.; Proceedings of the Third International Conference on the Remediation of Chlorinated and Recalcitrant Compounds; Batelle Press: Columbus, OH, Plaisier, W.; Pancras, T. In Remediation of Chlorinated and Recalcitrant Compounds 2002; Gavaskar, A. R.; Chen, A. S. C., Ed.; Proceedings of the Third International Conference on the Remediation of Chlorinated and Recalcitrant Compounds; Batelle Press: Columbus, OH, Shiple, J.; Coons, M.; Campbell, R. E.; Collins, W. E.; Abedi, H. In Remediation of Chlorinated and Recalcitrant Compounds 2002; Gavaskar, A. R.; Chen, A. S. C., Ed.; Proceedings of the Third International Conference on the Remediation of Chlorinated and Recalcitrant Compounds; Batelle Press: Columbus, OH, Roberts, E. P.; Bauer, N. In Remediation of Chlorinated and Recalcitrant Compounds 2000; Wickramanayake, G. B.; Gavaskar, A. R.; Chen, A. S. C., Ed.; Proceedings of the Third International Conference on the Remediation of Chlorinated and Recalcitrant Compounds; Batelle Press: Columbus, OH, 2000; pp Levin, R.; Wilson, J.; Ware, L.; Findley, J.; Baehr, J. In Remediation of Chlorinated and Recalcitrant Compounds 2000; Wickramanayake, G. B.; Gavaskar, A. R.; Chen, A. S. C., Ed.; Proceedings of the Third International Conference on the Remediation of Chlorinated and Recalcitrant Compounds; Batelle Press: Columbus, OH, 2000; pp

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