PAHs Removal from Urban Storm Water Runoff byDifferent Filter Materials

Krishna R. Reddy, F.ASCE1; Tao Xie2; and Sara Dastgheibi3

Abstract: Urban storm water runoff is contaminated as deleterious materials wash from roadways, parking lots, and open spaces, and thesubsequent discharge into surface water sources, such as lakes, can pose adverse effects on public health and the environment. Oil leaks andspills on roadways and parking lots can contain toxic polycyclic aromatic hydrocarbons (PAHs) that can be washed by storm water runoff.Although many best management practices have been developed to treat urban storm water, in-ground filter systems can be best suited inurban site-constrained settings. This paper investigates the effectiveness of different permeable inorganic materials as filter media for theremoval of PAHs from storm water runoff. Several series of batch experiments were conducted using four different filter media (calcite,zeolite, sand, and iron filings) and synthetic storm water containing representative PAHs (naphthalene or phenanthrene) at different initialconcentrations. The PAH removal and system chemistry in terms of pH, oxidation-reduction potential (ORP), and electrical conductivity (EC)were determined. All of the filter media possessed porous structure and surface characteristics that allowed adsorption and removal of theselected PAHs from the storm water runoff to more than 90%. Calcite and zeolite increased the pH and reduced the ORP and EC significantlyas compared with sand and iron filings. Overall, this study demonstrated that the selected filter media have great potential to remove PAHsfrom urban storm water runoff. DOI: 10.1061/(ASCE)HZ.2153-5515.0000222. © 2014 American Society of Civil Engineers.

Author keywords: Storm water runoff; Polycyclic aromatic hydrocarbons; Filter materials; Adsorption.

Introduction

Nonpoint source pollution such as urban storm water runoff gen-erated from residential, industrial, and commercial areas, highways,parks, parking lots, and open spaces is a leading cause of the deg-radation of nearby water bodies such as lakes. Contaminantsaccumulated on the surface of these areas wash off during rainfalland reach bodies of water, causing major water-quality problems(Tsihrintzis and Hamid 1997). The U.S. Environmental ProtectionAgency (USEPA) stated in a 1988 report to the U.S. Congress thatthe third and fourth largest sources of water-quality problems inrivers and lakes in the United States is urban storm water runoff(USEPA 1990). The degree of the storm water runoff pollutionis highly dependent on the rainfall patterns and intensity, numberof dry days, drainage system, and land use (Chui et al. 1982).

Polycyclic aromatic hydrocarbons (PAHs) are typical carcino-genic and mutagenic pollutants found in urban storm water runoffthat result from the incomplete combustion of fossil fuel, motor ve-hicle operation, spillage of oil, vehicle tire wear, and asphalt roadsurface materials [Agency for Toxic Substances and Disease Registry(ATSDR) 1995; Hwang and Foster 2006; Brown and Peake 2006].Brown and Peake (2006) investigated PAH concentration in the

suspended solids component of urban runoff from two storm watercatchments in Dunedin, New Zealand, over seven storm events from1998 to 2000. They found that the level of Σ16PAH in the runofffrom 100% urban catchment ranged from 1.2 to 11.6 μg=g of roaddebris and contained ten-fold greater levels of Σ16PAH than therunoff from a largely rural catchment (20% urban).

The development of best management practices (BMPs) haspaved the way to manage the different types of storm water pollu-tion (Urbonas and Stahre 1993; USEPA 2013). Storm water treat-ment BMPs consist of several methods and tools that allow theremoval of pollutants and particulates (Lynch and Corbett 1990;USEPA 2013). Bioretention is a well-known BMP; it is usuallysized at approximately 2–5% of the drainage area, which includesa mixed layer of soil and sand planted with appropriate vegetation(Diblasi et al. 2009). Diblasi et al. (2009) reported an average PAHmass load reduction of 87% to the discharging watershedafter passing through a bioretention cell. However, the specifica-tions on vegetation type and for the size of the bioretention cellneed to be carefully optimized. Besides, in urban areas, it maynot be possible to implement bioretention methods because ofunsuitable weather conditions or a lack of adequate area in that lo-cation. Under such situations, in-ground filter systems that consistof adsorptive/reactive permeable media have great potential to beeffective and practical.

An in-ground permeable filter system is proposed to treat theurban storm water runoff near the beaches along the Lake Michiganin Chicago, Illinois (Reddy 2013). The purpose of the filter systemis to remove a wide range of contaminants found in urban stormwater runoff, thereby preventing contamination of beaches andprotecting public and the environment. The media selected insuch filter systems should be permeable, environmentally benign,adsorptive/reactive, easily available, less costly, and easily re-placeable.

This study, which is part of that larger study, investigates fourpotential filter media (calcite, zeolite, sand, and iron filings) toremove PAHs, specifically, naphthalene and phenanthrene, from

1Professor, Dept. of Civil and Materials Engineering, Univ. of Illinois atChicago, 842 West Taylor St., Chicago, IL 60607 (corresponding author).E-mail: kreddy@uic.edu

2Visiting Doctoral Student, Dept. of Civil and Materials Engineering,Univ. of Illinois at Chicago, 842 West Taylor St., Chicago, IL 60607.E-mail: xietaothu@gmail.com

3Graduate Research Assistant, Dept. of Civil and Materials Engineer-ing, Univ. of Illinois at Chicago, 842 West Taylor St., Chicago, IL 60607.E-mail: sdastg2@uic.edu

Note. This manuscript was submitted on June 11, 2013; approved onNovember 13, 2013; published online on November 15, 2013. Discussionperiod open until June 23, 2014; separate discussions must be submitted forindividual papers. This paper is part of the Journal of Hazardous, Toxic,and Radioactive Waste, © ASCE, ISSN 2153-5493/04014008(6)/$25.00.

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urban storm water runoff. Several series of batch experiments wereconducted using each media with synthetic storm water containingnaphthalene or phenanthrene at different concentrations. These ex-periments allowed investigation of the extent of PAHs removal andthe effects of physicochemical parameters such as pH, oxidation-reduction potential (ORP), and electrical conductivity (EC) on thePAHs removal.

Materials and Methods

Filter Materials

On the basis of published literature and preliminary testing of severalmaterials, four filter materials were selected for this study: calcite(limestone), zeolite, sand, and iron filings (Reddy 2013). Calciteis a sedimentary rock (mostly mineral calcite) that consists ofdifferent crystal forms of calcium carbonate (CaCO3) (Aziz et al.2001). The calcite used for this study was obtained from DuPageWater Conditioning (West Chicago, Illinois). Natural zeolites areformed in basaltic lava, in specific rocks, which are subjected to mod-erate geologic temperature and pressure (Vaughn 1988). The sourceof zeolite used for this study was Bear River Zeolite Co., Inc. (Pres-ton, Idaho). The white Ottawa silica sand used in this study was pri-marily composed of silicon dioxide, or SiO2, and was obtained fromU.S. Silica Co. (Ottawa, Illinois). Iron filings are mostly a byproductof the grinding, filing, or milling of finished iron products, and it wasobtained from Connelly-GPM, Inc. (Chicago, Illinois).

The water content of the filter materials, as received from thesuppliers, was measured according to the ASTM D2216 (ASTM2012b). All four filter media were air dried first and then washedon sieve #200 (with an opening size of 0.075 mm) with deionizedwater to remove any very fine fraction present in them to avoid anypotential increase in the total suspended solids in the treated stormwater. The washed media were then placed in the oven overnight todry completely. The dry filter media were then tested to character-ize the physical and hydraulic properties based on ASTM standardtesting procedures (ASTM 2012a). The filter materials were com-pacted in a cylindrical Harvard Miniature Compaction (Humboldt,Schiller Park, Illinois) test mold, and the total mass of materialpresent in the known total volume of mold was measured to deter-mine the bulk density. The specific gravity was calculated from theratio of media solid density to the density of water according toASTM D854 (ASTM 2012g). Porosity was calculated accordingto the bulk density, specific gravity and phase relationships.Particle-size distribution of media was determined by mechanicalsieve analysis ASTM D422 (ASTM 2012d). Hydraulic conduc-tivity of media was determined using the constant-head permeabil-ity method ASTM D4972 (ASTM 2012e). A muffle furnace, set at440°C, was used to determine the organic content of media ASTMD2974 (ASTM 2012c), and standard methods were used to deter-mine the pH, ORP, and EC of the filter media ASTM D1293(ASTM 2012f). Scanning electron micrographs of the filter mate-rials were obtained to assess their morphology and pore structure.

Storm Water with Naphthalene or Phenanthrene

Naphthalene and phenanthrene, two well-known PAHs that arecommonly found in typical urban storm water runoff, were selectedfor this study. Concentrations of PAHs in urban storm water runoffare highly variable, and runoff is surface-dependent. In this study,concentrations of naphthalene and phenanthrene were chosenaccording to their maximum solubility in deionized water, and sev-eral orders of magnitude lower than these values were also consid-ered to assess the adsorption capacity of the filter media. Simulated

storm water was prepared by mixing known amounts of naphtha-lene or phenanthrene with deionized water to prepare storm waterwith different initial concentrations of these contaminants. Stormwater samples with naphthalene and phenanthrene concentrationsclose to their solubility limits were prepared first, and then thelower-concentration storm water samples were prepared by dilutingthe samples with deionized water. This study focused on testingindividual PAHs; a study of storm water with complex contaminantmixture of contaminants, including PAHs, metals, nutrients and E.coli in concentrations representative of typical urban storm waterrunoff, was also conducted and presented in Reddy (2013) andReddy et al. (2014a, b, c).

Batch Experimental Procedure

Batch experiments were performed to assess the ability of the filtermedia to adsorb and remove naphthalene or phenanthrene fromsynthetic storm water. The test procedure consisted of placing aknown dry mass of filter media into a 250-mL glass bottle contain-ing a known volume of prepared storm water with a known initialconcentration of naphthalene or phenanthrene. The experimentswere conducted using synthetic storm water with different initialconcentration of naphthalene or phenanthrene (C0). The sampleswere shaken for 24 h in a mechanical tumbler at room temperatureto reach equilibrium concentration. The supernatant was separatedby filtration, and the concentration of naphthalene or phenanthrene(Ceq) was determined. The difference in the initial and final solu-tion concentrations at equilibrium condition was used to determinethe percent contaminant removal by each medium for different con-centrations, as represented by the following:

Contaminant removalð%Þ ¼�C0 − Ceq

C0

�× 100 ð1Þ

where C0 = initial concentration of naphthalene or phenanthrene(mg=L) in synthetic storm water; Ceq = final (equilibrium) concen-tration of the naphthalene or phenanthrene (mg=L) in the superna-tant; and the percent contaminant removal shows the amount ofnaphthalene or phenanthrene adsorbed and removed from stormwater by filter medium.

The filter media to contaminated storm water (naphthalene orphenanthrene solution) ratio of 1∶10was selected for all of the batchexperiments. Naphthalene solutions with four concentrations of0.9, 1.8, 6.7, and 43 mg=L were used, and phenanthrene solutionsof four concentrations of 0.03, 0.14, 0.53 and 1.9 mg=L were used.These concentrations were selected on the basis of the maximumaqueous solubility of the contaminants. For each test, 100 mL ofprepared contaminant solution was transferred into a wide-mouthglass bottle containing 10 g of the selected dry filter media.Samples were prepared and labeled with the filter medium, contam-inant type, and contaminant concentration. Bottles were sealed withscrew caps and shaken in a tumbler at room temperature for 24 h.Afterward, the samples were filtered through a Whatman glass mi-crofiber filter (Grade GF/C) (Sigma-Aldrich, St. Louis, Missouri)(45 μm), and the filtrates were transferred to the empty glass bot-tles. The contaminant concentrations of filtrates were thenanalyzed to quantify the percent removal under each of the initialconcentrations of the contaminant for each filter media. The filtratewas also analyzed for pH, ORP, and EC. Control samples with onlystorm water samples (naphthalene or phenanthrene solution)exclusive of filter media and blank samples that only containedeach filter media in distilled water without any contaminants werealso tested. All batch tests were performed in duplicate.

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Analytical Methods

The naphthalene and phenanthrene concentrations in blank, con-trol, and media-contacted filtered samples were determined usinga liquid-liquid extraction procedure in accordance with USEPAtest method 3520C (USEPA 2007). This was followed by a gaschromatography analysis that used an Agilent Model 6890 gaschromatography (GC) (Agilent Technologies, Santa Clara,California) equipped with a flame ionization detector (FID) andColumn J&W Scientific DB (Agilent Technologies, Santa Clara,California), 30 m × 0.32 mm × 25 μm. The carrier gas was heliumat a constant pressure of 121.4 kPa (17.61 psi), and the oventemperature was ramped from 100 to 285°C at 20°C=min for9 min and then held at 285°C until the end of the run time.

Standard solutions containing naphthalene or phenanthrene ofincreasing concentration levels were prepared from naphthaleneor phenanthrene salts in 1 mL of methylene chloride (MeCl). 2-fluorobiphenyl standard solutions with different concentrations werealso prepared in acetone to determine extraction efficiency. Samplesof 38.7 mL were transferred into the 40-mL bottle, and the septa capwas tightened completely. 1.3 mL of MeCl and known volume of the200-mg=L 2-fluorobiphenyl solution were gently injected into thebottle through the cap. The samples were then shook by hand for5 min to ensure that all of the contaminant was transferred to theMeCl. After being allowed to settle for 5 min, the MeCl at the bottomof the bottle was extracted and transferred into the 2-mL amber vialby using a 1-mL syringe. 1 μL of the extracted MeCl was injectedinto the GC port and run on the GC. The final concentrations of thenaphthalene or phenanthrene were determined according tothe extraction efficiencies, which were calculated according to the2-fluorobiphenyl concentrations obtained from the GC.

The pH, ORP, and EC of the filtered samples were measured inaccordance with ASTM D1293 (ASTM 2012f), ASTM D1125(ASTM 2009), and ASTM D1498 (ASTM 2008), respectively.The pH meter used was Orion Model 720A (Fisher Scientific, Pitts-burgh, Pennsylvania) that was calibrated using pH 7 and 10 buffers.The probe was placed inside the samples, and the pH value was re-corded after the electrode stabilized. The ORP and EC of the sampleswere measured in the same manner with the appropriate electrodes.

Results and Discussion

Filter Materials Properties

Table 1 summarizes the properties of the filter media. The results ofthe grain-size distribution analysis of the filter media, shown inFig. 1, indicates that the filter media mostly consisted of coarseparticle sizes, which varied between 10 and 0.5 mm. Zeolitehad the largest particle-sizes distribution, followed by iron filings,calcite, and sand. The effective particle size (D10), however, wasapproximately the same for the four filter media. Zeolite had adry density of 1 g=cm3, whereas calcite and sand had similardry densities ranging from 1.6 to 1.8 g=cm3. Iron filings had a veryhigh density of 2.3 g=cm3. The density of the filter media is an

important consideration to ensure physical stability of the full-scalefilter infrastructure under field conditions. Iron filings also had thehighest porosity of 66%, followed by zeolite with 55%, calcitewith 44%, and sand with 34%. The high porosity and approxi-mately the same effective particle size resulted in approximatelythe same high hydraulic conductivity of 0.3 to 0.6 cm=s for allof the filter media. Hydraulic conductivity is a decisive character-istic of the filter media, necessary to achieve the desired hydrauliccapacity of the whole filter system under typical storm events.

The scanning electron micrographs shown in Fig. 2 depict themorphology of the filter media. These micrographs provide funda-mental insight into the filter media structure, which is of great im-portance for understanding their reaction mechanism and theirstructure-function relationship. The porous, rough structure offilter media, an essential property for capturing of contaminants,is visible in these images.

Naphthalene and Phenanthrene Removal

Fig. 3 shows the percent removal of naphthalene and phenanthreneunder different initial concentration conditions by the four filtermedia in the batch experiments. These results are obtained by test-ing with naphthalene and phenanthrene solutions separately; thus,synergistic effects that occur if they coexist in the storm water ontheir removal behavior was not studied. In general, the researchshows that each filter media nearly completely removed the naph-thalene and phenanthrene from the storm water. The final pH, ORP,and EC values of the storm water solutions at equilibrium conditionfor each filter media, with different initial naphthalene and phenan-threne concentrations, are presented in Figs. 4 and 5.

As shown in Fig. 3(a), all four filter media had excellent naph-thalene removal efficiency, reaching more than 90%, even underhigh initial concentration. The highest naphthalene concentration

Table 1. Properties of Filter Materials

Filter material

Effectiveparticle size,D10 (mm)

Average particlesize, D50 (mm)

Dry density(g=cm3)

Organiccontent (%) pH

Oxidation-reduction

potential (mV)

Electricalconductivity(mS=cm)

Hydraulicconductivity,K (cm=s)

Calcite 0.5 0.7 1.6 0.0 9.0 −117.1 0.01 0.3Zeolite 0.6 1.2 1.0 6.8 7.8 −58.0 0.10 0.4Sand 0.5 0.6 1.8 0.3 8.4 −95.3 0.02 0.3Iron filings 0.5 0.9 2.3 0.0 5.3 87.6 30.5 0.6

Particle Size (mm)

.01.1110

Per

cent

Fin

er

0

20

40

60

80

100

CalciteZeoliteSandIron Filings

Fig. 1. Particle-size distribution of filter materials

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solution reflects the maximum solubility in deionized water, whichis the highest concentration that can be expected in storm waterrunoff. The high removal efficiencies imply that there are still moreavailable active sites on the surface of filter media to adsorb morenaphthalene. The removal of phenanthrene by the filter media fordifferent initial concentrations is similar to that of naphthalene, asshown in Fig. 3(b). Phenanthrene removal efficiencies were veryhigh, almost 100%. Zeolite had the lowest removal efficiency ofall of the media at lower initial phenanthrene concentration; how-ever, as the phenanthrene concentration increased, its removal ef-ficiency increased as well. The results show that these four mediahave excellent potential for the removal of phenanthrene and naph-thalene, and potentially other PAHs, from urban storm water runoff.

pH, ORP, and EC Changes

Fig. 4 shows the pH of the different concentrations of naphthalenesolutions and shows how pH changes because of contact with thefilter media. The initial pH value of naphthalene concentrationswithout any filter media was approximately 6. When the filtermedia was added, the pH increased irrespective of the concentra-tion of naphthalene. The calcite, zeolite, and iron filings increasedthat pH value to greater than 9, 8, and 7, respectively. The presenceof carbonate (HCO3) in calcite may be responsible for the highestpH increase. As the naphthalene concentration increased, the pHslightly increased when the filter medium was calcite or zeolite,whereas the change in pH level found with sand and iron filingswas insignificant. As shown in Fig. 5, the pH values of the initialphenanthrene solutions with different concentrations were slightlyacidic, with pH of approximately 6. Because of existence ofcarbonates, the final solutions in contact with calcite were alkaline,and their pH values increased to greater than 9 (Fig. 5). Zeolitealso increased the pH values of the solutions to greater than 8.Iron filings and sand increased the solution pH slightly toapproximately 6.5.

The ORP tests show the tendency of chemical species in a sol-ution to be reduced and to gain electrons. As the positive ORPvalue increases, the tendency to attract electrons in a solution in-creases. The high positive values of ORP in the initial naphthalene

Filter Material

Calcite Zeolite Sand Iron Filings

Nap

htha

lene

Rem

oval

Eff

icie

ncy

(%)

(a)

(b)

80

100

0.91.86.743

Filter Material

Calcite Zeolite Sand Iron Filings

Phe

nant

hren

e R

emov

al E

ffic

ienc

y (%

)

60

80

100

0.030.140.531.9

Fig. 3. Removal of (a) naphthalene and (b) phenanthrene usingdifferent filter materials

Fig. 2. Scanning electron micrographs of filter materials

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and phenanthrene solutions without filter media (Figs. 4 and 5)demonstrate that oxidizing conditions existed, whereas the ORPof the final naphthalene and phenanthrene solutions in contactwith filter media are reduced. The ORP values for solutions in con-tact with calcite had the lowest values, which ranged from −151.5to −173.6 mV and demonstrated a decreasing trend as the initialconcentration increased. A similar trend was observed for zeolitewith the ORP reduced from−50.7 to−90.2 mV. In the case of sand,the very low ORP values changed from negative to positive with anincrease in the phenanthrene or naphthalene concentration. In gen-eral, iron filings resulted in low negative ORP values for all concen-trations of naphthalene solutions but changed to slightly positivevalues with the increase in concentration for the phenanthrene.

Electrical conductivity indicates the amount of dissolved ionsin an aqueous solution that relates to its capability to conductelectrical current. Higher initial EC values indicate higher dis-solved constituents in the storm water. Figs. 4 and 5 show thatthe EC values of the initial naphthalene and phenanthrenesolutions before contact with the filter media were high andranged from 3 to 10 mS=cm. However, after contact with thefilter media, the EC of the final solutions decreased significantlyin all cases and varied between 0.6 and 2.4 mS=cm. The ECwas approximately zero when the filter medium was calcite orzeolite as a result of the high pH conditions, which causedany dissolved substances to precipitate. The EC measured inthe final solutions in contact with were slightly higher thanthose determined for iron filings. Because either naphthaleneor phenanthrene was the only contaminant dissolved in the

Initial Naphthalene Concentration (mg/L)

Filter Material

None Calcite Zeolite Sand Iron Filings

pH

0

2

4

6

8

10

1200.91.86.743

Filter Material

None Calcite Zeolite Sand Iron Filings

OR

P (

mV

)

-150

-100

-50

0

50

Filter MaterialNone Calcite Zeolite Sand Iron Filings

EC

(m

S/cm

)

0

1

2

6

8

(a)

(b)

(c)

Fig. 4. pH, ORP, and EC variation in naphthalene batch experimentsusing different filter materials

Initial Phenanthrene Concentration (mg/L)

Filter MaterialNone Calcite Zeolite Sand Iron Filings

pH

0

2

4

6

8

10

12

00.030.140.531.9

Filter Material

None Calcite Zeolite Sand Iron FilingsO

RP

(m

V)

-150

-100

-50

0

50

Filter MaterialNone Calcite Zeolite Sand Iron Filings

EC

(m

S/cm

)

0

1

2

3

6

8

10

12

(a)

(b)

(c)

Fig. 5. pH, ORP, and EC variation in phenanthrene batch experimentsusing different filter materials

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deionized water, the EC values indicate the presence of traceionic species present in the deionized water used in this study.In the presence of filter media, some ionic species may haveadsorbed to the filter media or some species desorbed fromfilter media and released into the solution, affecting the final ECmeasurement.

Conclusions

This study quantified the extent of removal of naphthaleneand phenanthrene individually from storm water with four filtermedia (calcite, zeolite, sand, and iron filings). Several seriesof batch experiments were conducted using each filter mediawith naphthalene and phenanthrene solutions of differentinitial concentrations. The extent of the removal of the naphtha-lene and phenanthrene and changes in pH, ORP, and ECof the storm water were measured. The following conclusionscan be drawn:• None of the filter media reached their maximum adsorption

capacity, which implies that these media still have goodpotential to remove higher concentrations of naphthalene andphenanthrene.

• The naphthalene and phenanthrene removal efficiencies by cal-cite, zeolite, iron filings, and sand were very high, exceeding90% for all of the initial concentrations tested.

• Calcite, zeolite, and iron filings induced alkaline solutions,whereas sand was the only medium that did not alter the pHvalue of the storm water.

• Calcite and zeolite induced reducing conditions, whereas sandand iron filings induced oxidizing conditions. The electricalconductivity was reduced to almost zero in calcite and zeolite,and it was slightly reduced in sand and iron filings.

• Overall, the selected media demonstrated great potential toremove PAHs from storm water.

Acknowledgments

Financial support for this project is provided by the U.S. Environ-mental Protection Agency Great Lakes National Program Office(under Grant No. GL00E00526). The support for the second authoris provided by the China Scholarship Council. The assistance ofGiridhar Prabukumar, Krishna Pagilla, Preethi Chinchoud, PoupakYaghoubi, Alexander Hardaway, and Hanumanth Kulkarni is grate-fully acknowledged.

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