Journal of Occupational and Environmental Hygiene, 8: 573579 ISSN: 1545-9624 print / 1545-9632 online Copyright c 2011 JOEH, LLC

DOI: 10.1080/15459624.2011.613346

Comparison of Toluene Adsorption Among Granular Activated Carbon and Different Types of Activated Carbon Fibers (ACFs)
Jo Anne G. Balanay,1 Shaun A. Crawford,2 and Claudiu T. Lungu2
1 2

Environmental Health Sciences Program, East Carolina University, Greenville, North Carolina Department of Environmental Health Sciences, University of Alabama at Birmingham, Birmingham, Alabama

Activated carbon ber (ACF) has been demonstrated to be a good adsorbent for the removal of organic vapors in air. Some ACF has a comparable or larger surface area and higher adsorption capacity when compared with granular activated carbon (GAC) commonly used in respiratory protection devices. ACF is an attractive alternative adsorbent to GAC because of its ease of handling, light weight, and decreasing cost. ACF may offer the potential for short-term respiratory protection for rst responders and emergency personnel. This study compares the critical bed depths and adsorption capacities for toluene among GAC and ACF of different forms and surface areas. GAC and ACF in cloth (ACFC) and felt (ACFF) forms were challenged in stainless steel chambers with a constant concentration of 500 ppm toluene via conditioned air at 25 C, 50% RH, and constant airow (7 L/min). Breakthrough data were obtained for each adsorbent using gas chromatography with ame ionization detector. Surface areas of each adsorbent were determined using a physisorption analyzer. Results showed that the critical bed depth of GAC is 275% higher than the average of ACFC but is 55% lower than the average of ACFF. Adsorption capacity of GAC (with a nominal surface area of 1800 m2/g) at 50% breakthrough is 25% higher than the average of ACF with surface area of 1000 m2/g, while the rest of ACF with surface area of 1500 m2/g and higher have 40% higher adsorption capacities than GAC. ACFC with higher surface area has the smallest critical bed depth and highest adsorption capacity, which makes it a good adsorbent for thinner and lighter respirators. We concluded that ACF has great potential for application in respiratory protection considering its higher adsorption capacity and lower critical bed depth in addition to its advantages over GAC, particularly for ACF with higher surface area. Keywords activated carbon ber, adsorption, critical bed depth, granular activated carbon, toluene

INTRODUCTION ranular activated carbon (GAC) has been the standard adsorbent used in respirators for several gases and vapors, including volatile organic compounds (VOCs), because of its efciency, low cost, and available technology. However, GAC has some drawbacks, including poor selectivity, high pressure drop through the packed media, and requirement for containment. Activated carbon ber (ACF) is an alternative adsorbent that could overcome some of the drawbacks of GAC. It is obtained from the carbonization and activation of polymeric bers and has a narrow pore size distribution in the micropore range.(1) The advantages of ACF over GAC include larger surface area, comparable or larger adsorption capacities, and ease in handling due to its form.(2,3) Because of these advantages, one can envision for the future a thin respirator that is easy to wear and can ensure adequate protection, at least for a limited amount of time. Such a device of reduced size, complexity, and cost would be extremely useful in situations when a very toxic gas or vapor would be dispersed accidentally in a workplace or, intentionally, as a consequence of a terrorist attack. ACFs may therefore be used for short-term respiratory protection by rst responders, emergency personnel, and the public in case of a catastrophic event. Several studies have been conducted to assess ACF in air pollution control devices, usually in the form of xed bed reactors.(49) In such applications, ACFs have been shown to be very effective adsorbents to capture and/or recover water vapor and organic vapors, such as methyl ethyl ketone (MEK), benzene, toluene, xylene, cyclohexanone, tetrachloroethylene, acetone, isopropanol, ethyl acetate, isobutane, and dichloromethane, from gas streams at a wide range of concentrations.(1013) Filters composed of a mat of ACFs have also been applied in the capture of toxic gases emanating

Correspondence to: Claudiu T. Lungu, Department of Environmental Health Sciences, RPHB 530, 3rd Ave. S., Birmingham, AL 35294; e-mail: clungu@uab.edu.

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TABLE I. Denotation of ACF Types Based on ACF Surface Area and Form Nominal Surface Area, m2/g Form Cloth Felt 1000 ACFC10 ACFF10 1500 ACFC15 ACFF15 1800 ACFF18 2000 ACFC20

als.(5,6,8,9,12,21) Toluene was purchased from Fisher Scientic (Waltham, Mass.) and used in the experiments without further purication. Characterization of Adsorbent Surface Area and Porosity The surface area, pore area, pore volume, and pore size of the adsorbent samples were measured by nitrogen adsorption at 77 K in the range of relative pressure from 0.02 to 1.0, using a Micromeritics ASAP 2020 automatic physisorption analyzer (Micromeritics Corp., Norcross, Ga.). Ultra-high purity nitrogen (99.99%) (Airgas, Inc., Radnor, Pa.) was used in the measurement. All samples were degassed before the measurement at 300 C for 1 hr. All samples underwent both the degassing and analysis processes in the physisorption analyzer. Breakthrough Determination A dynamic adsorption experiment was used to characterize the adsorption of test materials. The materials were challenged with toluene at a concentration of 500 ppm in air in a stainless steel adsorption chamber at a constant airow (7 L/min), air temperature (25 C), and relative humidity (50%). The toluene concentration was in parts per million by volume (ppmv), but will be expressed in ppm going forward. The 500 ppm challenge concentration was chosen because we intended to test the adsorbents at the immediately dangerous to life and health (IDLH) concentration of toluene. Air temperature and relative humidity conditions are similar to those used by the National Institute of Occupational Safety and Health (NIOSH) in testing respirators for organic vapors, as well as in previous studies on ACF testing.(5,8,22) The 7 L/min airow rate through the system was selected as roughly corresponding to the air velocity through a cartridge during normal breathing conditions, and it also represented the maximum airow that we could condently control in our experimental setup. The chamber was immersed in a water bath to maintain constant temperature throughout the experiment. Four different bed depths were used for each challenge concentration. The mass of the adsorbent beds was determined before the challenge by using a Denver Model APX-100 analytical balance (Denver Instrument, Denver, Colo.). The adsorbent bed depth was measured using a caliper. Toluene vapor was generated by injecting a pre-calculated constant ow of liquid toluene using an Aladdin-1000 automated syringe pump (World Precision Instruments, Sarasota, Fla.) into a preconditioned stream of air of constant ow. Air was dried by passing through a Hankison air drying machine (Hankison, Canonsburg, Pa.) and a Drierite gas drying unit (W.A. Hammond Drierite Co. Ltd., Xenia, Ohio). Temperature and relative humidity of the air were controlled prior to mixing with toluene using a Miller-Nelson Model HCS401 instrument (Assay Technology, Inc., Livermore, Calif.). A Smart-Trak mass ow controller (Sierra Instruments, Inc., Monterey, Calif.) was used to regulate the ow of the airstream. Breakthrough of the adsorbent samples for toluene was determined by gas chromatography using an Agilent Model
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from industrial processes and gasoline vapors from automobile tanks.(14) These lters have been extensively used for capture of other gaseous compounds, such as freon.(15) Applications of ACF include environmental cleaning, recovery of sulfur dioxide and nitric oxide in ue gas, energy saving, and storage, such as methane storage, carbon dioxide (CO2 ) capture, and air separation.(1619) However, studies on the application of ACF for respiratory protection in the literature are non-existent to date. The assessment of the characteristics of ACFs is very crucial in determining if these materials may be used for respiratory protection. Given their advantages, ACFs have great potential in the development of better respirators in terms of efciency in the removal of VOCs and in comfort and ease of use because of lighter weight and less bulk. The purpose of this study was to compare the adsorption capacities and critical bed depth between one type of GAC and different types of ACF for toluene as a representative VOC and to determine if the ACF may serve as an alternative adsorbent in respirators. METHODS Materials GAC and ACF were the two main types of carbon adsorbents used in the study. The ACF was of two forms: woven cloth and unwoven felt. For each form, three manufacturespecied surface areas (1000, 1500, and 1800, or 2000 m2/g) were tested. Thus, six types of ACFs were analyzed. Table I shows the denotation of each ACF based on its form and surface area. The GAC used was the RVG-C 80 1220 (Calgon Carbon Corporation, Pittsburgh, Pa.). ACFC15, ACFF15, and ACFC20 were manufactured by American Kynol, Inc., Pleasantville, New York, and ACFC10, ACFF10, and ACFF18 by Beijing Evergrow Resources Co., Beijing, China. Adsorbents were treated in an oven (Thermo Electron Corporation, Waltham, Mass.) at 200 C overnight prior to testing to eliminate moisture and any volatile impurities from the adsorbent materials. The adsorbate used to challenge the adsorbents was toluene (laboratory grade) as the representative VOC because it is one of the most common VOCs in the workplace and is one of the major and most often reported indoor organic vapors.(20) It is often considered a representative for the VOC group in several studies involving the testing of ACF materi574

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HEPA Filter

Air Compressor

Temperature/ Humidity Controller

Gas Drying Units

Mass Flow Controller

Bypass Line Syringe Pump

Temp Controller

GC Sample Chamber Water Bath

FIGURE 1. Experimental setup for breakthrough determination.

He

H2

Air

6850 gas chromatograph (Agilent Techonologies, Alpharetta, Ga.) tted with a ame ionization detector (FID) for quantication. The analytical column used was an HP-1 (100% methyl siloxane) capillary column, 30.0 m 0.32 mm (I.D.) 0.25 m. The oven temperature was 230 C for 5 min, and the FID temperature was 250 C. The carrier gas was helium. A 5-point calibration curve was established using the external method. The experimental setup for breakthrough determination is shown in Figure 1. Determination of the Critical Bed Depth Critical bed depth is the minimum bed depth of the adsorbent that is required to obtain an acceptable chemical concentration at time zero. In this study, critical bed depth was specically dened as the minimum bed depth of the adsorbent that is required to reduce the challenge concentration of the chemical of interest by 90%. The time in minutes when 10% of the challenge concentration is breaking through the adsorbent material was determined for each breakthrough curve. The time (min) at 10% breakthrough of the chemical was plotted against the adsorbent bed depth (cm) to obtain a regression line for each adsorption at a certain concentration. The depth at which the regression line intersects the x-axis was determined to be the critical bed depth for the adsorbent.(23) The standard error of the critical bed depth was calculated based on the standard error of the estimate (SEy ). The upper condence limit of Y (ULy ) at 95% condence level was

calculated using the equation ULy = Y + t3 (SEy ), where Y = 0 and t3 = 3.182. The upper condence limit of X (ULx ) was then obtained using the equation ULx = (ULy b)/a where a is the slope of the line, and b is the y-intercept. Finally, the standard error of X, and thus the critical bed depth, was calculated using the equation SEx = (ULx CBD)/t3 where CBD is the critical bed depth.(24) Determination of the Adsorption Capacity Adsorption capacities of the adsorbents were investigated in this study because it gauges how much protection these adsorbents may provide against airborne toluene. These adsorption capacities were calculated at equilibrium conditions. The time (min) at 50% breakthrough was plotted against the adsorbent mass (g) to obtain a regression line for the calculation of the adsorption capacity (We ) of each adsorbent at 500 ppm of toluene using the modied Wheeler equation, as shown below: tb = where tb = breakthrough time (min) Cx = exit concentration (g/cm3) C0 = inlet concentration (g/cm3) Q = volumetric ow rate (cm3/min) W = weight of adsorbent (g)
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We B Q W ln (C0 /Cx ) C0 Q kv

(1)

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TABLE II. Surface Area and Porosity Characteristics by Adsorbent Type Adsorbent Type Parameters Nominal surface area (m2/g) BET surface area (m2/g) Micropore areaA (m2/g) % Micropore by area Total Pore volumeB (cm3/g) Micropore volumeA (cm3/g) % Micropore by volume Pore sizeC (nm) Density (g/mL)
ABy BSingle-point

GAC 1511.7 1148.8 75.99 0.7025 0.4604 65.54 1.86 0.411

ACFC10 1000 893.0 835.1 93.51 0.3864 0.3520 91.11 1.73 0.272

ACFC15 1500 1472.5 1334.2 90.61 0.6224 0.5425 87.16 1.69 0.272

ACFC20 2000 2059.2 1742.6 84.62 0.8732 0.6918 79.23 1.69 0.236

ACFF10 1000 999.4 899.1 89.96 0.4265 0.3649 85.56 1.71 0.077

ACFF15 1500 1419.1 1288.4 90.79 0.5935 0.5184 87.34 1.67 0.070

ACFF18 1800 1852.9 1092.9 58.98 0.8430 0.4400 52.19 1.82 0.056

t-plot method. adsorption total pore volume estimated at relative pressure 0.95. CAdsorption average pore width (4V/A by BET).

B = bulk density of packed bed (g/cm3) kv = rst order rate constant of adsorption (min1) We = kinetic adsorption capacity (g/g) Data at 50% breakthrough were chosen to determine the adsorption capacity to be more consistent throughout the experiment, since the lower (e.g., 10%) and the upper (100%) parts of the breakthrough curve have more variability in the breakthrough concentration data. The equation was transformed to the following: tb = We B We W ln (C0 /Cx ) . C0 Q k v C0 (2)

the ACFC20 and ACFF18 can be considered counterparts and may be compared against each other. Nitrogen Adsorption/Desorption Isotherms The adsorption/desorption isotherms for nitrogen of seven types of adsorbents using an automatic physisorption analyzer at a temperature of 77 K are shown in Figure 2. The shape of adsorption isotherms for all ACF types demonstrates that they are of Type I or the Langmuir-type form, indicating that the materials are mainly microporous.(27) Regardless of the ACF form, the greater the surface area of the ACF, the higher the quantity of nitrogen adsorbed. Generally, the ACF cloth has a higher nitrogen adsorption than the ACF felt, except for the ACFC10 and ACFF10, whereas the felt has a higher nitrogen adsorption than the cloth. On the other hand, the nitrogen isotherm of the GAC clearly exhibits a hysteresis loop, which is typical of mesoporous and macroporous materials with pores that are likely to have a wide range of sizes and shapes.(28) Comparing the GAC with ACF, the GAC has a lower nitrogen adsorption capacity than the ACFC20 and ACFF18, which have a higher surface area of 1800 m2/g or more. However, it is interesting to note that the GAC, ACFC15, and ACFF15 have crossover in their isotherms. Figure 3 shows the close-up of the isotherm crossover. The GAC has a lower nitrogen adsorption at lower relative pressures, but its isotherm crosses over that of ACFC15 at 0.06 relative pressure and that of ACFF15 at 0.11 relative pressure. This shows that the ACF types are better for nitrogen adsorption at lower concentrations, while the GAC is better at higher concentrations. Such
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The slope of the regression line, a = We C0 Q, was used to obtain an equation for calculating the adsorption capacity, We = aC0 Q. The standard error of the adsorption capacity was calculated based on the standard error of the slope.(25,26) RESULTS AND DISCUSSION Surface Area and Porosity Table II summarizes the surface area, pore area, pore volume, and pore size for the GAC and the six types of ACF. Results show that the GAC has similar surface area compared with ACFC15 and ACFF15 but has lower percentage of micropores by area and volume. Comparing the two forms of ACFs, the measured surface area of the ACF cloth is similar to its ACF felt counterpart (e.g., ACFC10 vs. ACFF10). Moreover, the ACFC20 has a measured surface area that is slightly higher than that of the ACFF18 but may still be comparable. Thus,
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FIGURE 2.

Nitrogen adsorption/desorption isotherms at 77K by adsorbent type.

observation may be attributed to the amount of micropores in the adsorbent. As shown in Table II, ACFC15 and ACFF15 have a greater percentage of micropores by area and volume compared with the GAC. Micropores are preferentially lled at lower concentrations due to the greater energy potential in these micropores, which is attributed to the proximity of the pore walls and overlapping potential elds.(27,29,30) Critical Bed Depth Critical bed depth is dened in this study as the minimum bed depth of the adsorbent required to reduce the concentration of toluene by 90%. This bed depth is required to prevent immediate breakthrough of toluene at the start of the challenge.

The lower the critical bed depth, the better the adsorbent because it takes a smaller depth of the material to adsorb a certain amount of chemical, and thus making a thinner respirator. The critical bed depths for GAC, ACF cloth, and ACF felt are shown in Figure 4. Critical bed depth of GAC for 500 ppm toluene (0.2 0.1 cm) is higher than those of the ACF cloth types (0.03 0.1 to 0.08 0.02 cm) but is lower compared with those of the ACF felt types (0.30 0.03 to 0.55 0.06 cm). Critical bed depth of GAC is 275% higher than the average critical bed depth of ACF cloth but is 55% lower than the average critical bed depth of ACF felt. This indicates that the ACF cloth may be used at a thinner bed depth as compared with the GAC and, thus, may be developed into a thinner respirator.

450

Quantity Adsorbed (cm 3/g STP)

400 350

0.7 0.6

250 200 150 100 50 0 0.00 0.02 0.04 0.06 0.08 0.10

ACFC15 ACFF15

Critical Bed Depth (cm)

0.14

300

GAC

0.5 0.4 0.3 0.2 0.1

0.12

0 GAC ACFC10 ACFC15 ACFC20 ACFF10 ACFF15 ACFF18

Relative Pressure (P/Po)

Adsorbent Type

FIGURE 3. Nitrogen adsorption isotherms for GAC, ACFC15, and ACFF15 at 77K.

FIGURE 4.

Critical bed depth by adsorbent type.

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Comparing the two ACF forms, the ACF cloth has a 7394% lower critical bed depth than the ACF felt with comparable surface area. On average, the ACF cloth has an 88% lower critical bed depth compared with the ACF felt. Critical bed depth of the ACF cloth is equivalent to approximately 1 layer of the cloth, while that of the ACF felt is equivalent to 13 layers of the felt material. This may be explained by the fact that a single layer of ACF cloth is thinner and denser than a layer of ACF felt, which is more spongy in nature. As shown in Table II, the ACF cloth on average is 3.8 times denser than the ACF felt. Thus, ACF cloth has more mass per bed depth, thus more bers, and more available adsorption sites for toluene molecules. Critical bed depth depends on the physical form of the ACF and is affected mainly by the density and thickness of the material. Based on critical bed depth alone, the ACF cloth is a better adsorbent than the ACF felt, making ACF cloths good candidates for the development of thinner respirators. Critical bed depth is dependent on the challenge concentration of the inuent. Theoretically, a higher initial toluene concentration will result in a higher critical bed depth. This effect is caused by the presence of more toluene molecules to be adsorbed in the pores of activated carbon, thus requiring more adsorbent materials to reduce the concentration to 90%. This is important to consider in real-life scenarios where the concentration of the pollutant changes with time. However, it is unlikely that toluene concentrations higher than 500 ppm will be encountered in most workplaces; thus, the critical bed depth determined in this study will be representative of a worst-case scenario. Adsorption Capacity The calculated adsorption capacities for GAC, ACF cloth, and ACF felt are shown in Figure 5. Adsorption capacity of GAC (392 0.02 mg/g), with a surface area of approximately 1500 m2/g, for 500 ppm toluene is 25% higher than the average adsorption capacity of the ACF types with a surface area of 1000 m2/g (335 0.07 and 293 0.03 mg/g for ACFC10 and ACFF10, respectively). This may be explained by the

lower surface areas of these ACF types compared with the GAC. The rest of the ACF types, however, have adsorption capacities (429 0.01 to 720 0.03 mg/g) higher than the GAC. The adsorption capacity of the GAC is 28% lower than the average adsorption capacity for the rest of the ACF with surface area of 1500 m2/g or more. This indicates that the ACF with similar or greater surface area than the GAC may provide greater protection against toluene when used in a respirator. A study by Lorimier et al.(8) determined the adsorption capacities of ACF cloth and felt for toluene. When the results of this current study and Lorimiers on the adsorption capacities of ACF cloth and felt with comparable surface areas are compared, both ACF forms in this study have higher adsorption capacities. For ACF cloths with approximate surface areas of 1000 m2/g, the present study and Lorimiers obtained an adsorption capacity of 549 and 270 mg/g, respectively, for 500 ppm toluene. For ACF felts with approximate surface areas of 1500 m2/g, the present study and Lorimiers obtained an adsorption capacity of 616 and 430 mg/g, respectively. Among the ACF types, the adsorption capacity has an increasing trend as the surface area increases, regardless of the ACF form. This can be explained by the amount of available adsorption sites at a given ACF mass, which is obviously less in low-surface area ACFs; the higher the surface area, the more available adsorption sites for capturing toluene molecules. Previous studies have demonstrated similar results for other VOCs, where a linear relationship was found between the adsorption capacities of organic compounds and the surface areas of adsorbents, independent of the type of adsorbent.(31,32) Comparing the two ACF forms, the adsorption capacity of ACF cloth is 1435% higher than that of ACF felt with a comparable surface area. On average, the ACF cloth has a 24% higher adsorption capacity compared with the ACF felt. Therefore, based on adsorption capacity alone, the ACF cloth is a better adsorbent than the ACF felt, particularly the ACFC20 with the highest surface area.

SUMMARY AND CONCLUSION

800 700

600 500 400 300 200 100 0 GAC ACFC10 ACFC15 ACFC20 ACFF10 ACFF15 ACFF18

Adsorbent Type

FIGURE 5.

Adsorption capacity by adsorbent type.

ritical bed depth and adsorption capacity of the GAC for 500 ppm of toluene were compared with those of six different types of ACFs to determine if the ACFs can be used as an alternative adsorbent in respirators. The ACF cloth was shown to have a lower critical bed depth compared with the GAC, making the ACF cloth a good candidate for the development of thinner respirators. Moreover, the ACF cloth and felt types with surface areas similar or greater than that of the GAC (1500 m2/g) have higher adsorption capacities compared with the GAC, making them good adsorbents against airborne toluene. Considering their critical bed depth and adsorption capacities, both the ACF cloth and felt forms used in this study have good potentials for use as adsorbents in thinner and lighter respirators that may be more comfortable to wear. Given its advantages over the GAC, the ACF shows promise in the
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Adsorption Capacity (mg/g)

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development of disposable respirators or masks for short-term protection against toluene, and probably other VOCs. Future studies are needed to determine the critical bed depth and adsorption capacities of different types of ACFs at different toluene concentrations, as well as against other VOCs and other gases, such as sulfur dioxide and chlorine. Other factors such as relative humidity and pressure drop across the ACF materials will be investigated to determine if these adsorbents are appropriate materials for respiratory protection. ACKNOWLEDGMENT

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he authors acknowledge funding support from the National Institute for Occupational Safety and Health (ROI grant # OH 008080). REFERENCES
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