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Influence of Membrane Surface Properties on Initial Rate of Colloidal Journal of Membrane Science 188 (2001) 115–128 Influence of membrane surface properties on initial rate of colloidal fouling of reverse osmosis and nanofiltration membranes Eric M. Vrijenhoek a, Seungkwan Hong b, Menachem Elimelech a,∗ a Department of Chemical Engineering, Environmental Engineering Program, Yale University, P.O. Box 208286, New Haven, CT 06520-8286, USA b Civil and Environmental Engineering Department, University of Central Florida, P.O. Box 162450, Orlando, FL 32816-2450, USA Received 28 November 2000; received in revised form 6 February 2001; accepted 9 February 2001 Abstract Recent studies have shown that membrane surface morphology and structure influence permeability, rejection, and colloidal fouling behavior of reverse osmosis (RO) and nanofiltration (NF) membranes. This investigation attempts to identify the most influential membrane properties governing colloidal fouling rate of RO/NF membranes. Four aromatic polyamide thin-film composite membranes were characterized for physical surface morphology, surface chemical properties, surface zeta potential, and specific surface chemical structure. Membrane fouling data obtained in a laboratory-scale crossflow filtration unit were correlated to the measured membrane surface properties. Results show that colloidal fouling of RO and NF membranes is nearly perfectly correlated with membrane surface roughness, regardless of physical and chemical operating conditions. It is further demonstrated that atomic force microscope (AFM) images of fouled membranes yield valuable insights into the mechanisms governing colloidal fouling. At the initial stages of fouling, AFM images clearly show that more particles are deposited on rough membranes than on smooth membranes. Particles preferentially accumulate in the “valleys” of rough membranes, resulting in “valley clogging” which causes more severe flux decline than in smooth membranes. © 2001 Elsevier Science B.V. All rights reserved. Keywords: AFM; Fouling; Flux decline; Membrane surface roughness; Colloidal fouling; Nanofiltration; Membrane surface properties 1. Introduction continues to be a serious problem, thus pointing out to the paramount importance of understanding the Successful utilization of membrane technology has fundamental physical and chemical mechanisms that been greatly limited by membrane fouling. Fouling in- govern colloidal fouling of membranes. creases operation and maintenance costs by deteriorat- Recent studies have shown that membrane sur- ing membrane performance and ultimately shortening face morphology and structure influence performance membrane life. Numerous studies in recent years have characteristics of membranes [1–9]. Hirose et al. [9] investigated the causes and control of membrane foul- suggested an approximately linear relationship bet- ing, and substantial progress has been made. However, ween membrane surface roughness and permeate flux in many applications colloidal fouling of membranes for crosslinked aromatic polyamide reverse osmosis (RO) membranes, where permeability increased with ∗ Corresponding author. Tel.: +1-203-432-2789; increasing surface roughness. The linear relationship fax: +1-203-432-2881. was attributed to surface unevenness of the RO mem- E-mail address: [email protected] (M. Elimelech). brane skin layer, which resulted in enlargement of the 0376-7388/01/$ – see front matter © 2001 Elsevier Science B.V. All rights reserved. PII: S0376-7388(01)00376-3 116 E.M. Vrijenhoek et al. / Journal of Membrane Science 188 (2001) 115–128 effective membrane area. Kwak et al. [4] showed that membrane surface properties. It was demonstrated substitution of bisphenol biphenyl rings with either that colloidal fouling of the RO and NF membranes methyl or halogen strongly influenced rejection and was strongly correlated only with membrane surface permeability of aromatic polyester RO membranes. roughness. A novel mechanistic explanation for the Higher flux and lower rejection were associated striking effect of membrane surface roughness on with the smoother membrane surfaces obtained from colloidal fouling behavior is proposed. methyl substitution, while lower flux and higher re- jection were associated with the rougher membrane surfaces resulting from halogen substitution. Addi- 2. Materials and methods tional work by Kwak and Ihm [5] coupling nuclear magnetic resonance (NMR) spectroscopy and atomic 2.1. Membranes force microscopy (AFM) has shown an important relationship between proton spin–lattice relaxation Four commercial RO/NF thin-film composite mem- times and RO permeability, regardless of surface mor- branes were used in this study. The RO membranes phological features. The latter two studies suggest were Hydranautics LFC-1 (Oceanside, CA) and that membrane performance (flux and rejection) is Trisep X-20 (Goleta, CA). The NF membranes were strongly influenced by the structure of the polymer Dow-FilmTec NF-70 (Minneapolis, MN) and Osmo- network which constitutes the thin-film active layer. nics HL (Minnetonka, MN). All membranes were Several fundamental investigations of membrane stored in deionized (DI) water at 5◦C with water fouling have explored the effects of membrane surface replaced regularly. The membranes were character- properties such as pore size and pore size distribution, ized for intrinsic physical and chemical properties surface roughness and structure, electrokinetic (zeta such as zeta potential, roughness (AFM), contact an- potential) characteristics, chemical properties (hydro- gle, chemical composition (XPS), and performance phobic/hydrophilic), and specific chemical structure (pure water flux and salt rejection). [1,3,6–8]. Various analytical techniques have been employed for elucidating specific physical and chem- 2.1.1. Membrane surface zeta potential ical surface properties of membranes, including Membrane surface zeta potential was determined Raman spectroscopy (structure) [1], electron spin res- by a streaming potential analyzer (EKA, Brookhaven onance (solute mobility in membrane polymer matrix Instruments Corp., NY) following the procedure de- and pores) [1], AFM (surface morphology, structure, scribed by Childress and Elimelech [11]. Three runs and pore size) [1–9], streaming potential (membrane on three separate days were performed for three dif- surface zeta potential) [10,11], NMR spectroscopy ferent samples of each membrane at an ionic strength (permeability) [5], contact angle [12], and X-ray of 0.01 M NaCl and pH ranging from 3 to 9. photoelectron spectroscopy (XPS) for surface chem- ical functional groups [13,14]. Despite these efforts, 2.1.2. Membrane AFM analysis however, the role of membrane surface properties in Membrane surface roughness was determined colloidal fouling of RO/NF membranes is still not by AFM imaging and analysis (Multi-Mode AFM, well understood. Digital Instruments, Santa Barbara, CA). Imaging This investigation relates several key membrane was performed in tapping mode with an etched sili- surface properties of four commercial RO/NF mem- con probe (TESP, Digital Instruments, Santa Barbara, branes to their initial colloidal fouling behavior CA). The TESP probes had a spring constant of during crossflow membrane filtration. The aromatic 20–100 N/m, resonant frequency of 200–400 kHz, polyamide thin-film composite membrane surfaces nominal tip radius of 5–10 nm, and cantilever length were characterized for morphological properties of 160 ␮m. Clean membrane coupons were removed (AFM), contact angle, zeta potential, and specific from storage in DI water and allowed to air dry be- chemical structure (XPS). Membrane fouling, deter- fore AFM scans were performed. Fouled membranes mined by percent of flux decline for a specific volume were removed from crossflow filtration devices fol- of permeate filtered, was correlated to the measured lowing each experiment, and immediately rinsed in a E.M. Vrijenhoek et al. / Journal of Membrane Science 188 (2001) 115–128 117 particle-free electrolyte solution similar to that used the membranes to equilibrate and attain steady-state in the corresponding fouling experiment before air performance. drying. After a constant flux was achieved at the starting pressure, operating pressure was decreased in incre- 2.1.3. Membrane contact angle measurement ments of 172 kPa (25 psi) down to 345 kPa (50 psi). Contact angle measurements were obtained via a At each pressure, flux was monitored for at least goniometer (Rame-Hart Inc., Mountain Lakes, NJ). 60 minutes, or until a satisfactory steady state was Three equilibrium contact angles as described by Mar- achieved. When flux at 345 kPa was maintained mur [15] were measured for each membrane. Each steady for at least 30 min, an appropriate volume of equilibrium contact angle was the average of the left premixed stock of NaCl solution was added to pro- and right contact angles, and the reported values are vide a 0.01 M (585 mg/l) salt concentration. After salt the average of three equilibrium contact angles. addition, the unit was allowed to equilibrate until a satisfactory steady-state flux was again reached. Per- 2.1.4. Membrane XPS analysis meate, retentate, and feed samples were drawn, and All XPS analyses were performed using a 5400 conductivity (YSI Inc., Yellow Springs, OH) and pH PHI ESCA spectrometer (Physical Electronics, Eden (Accumet 1500 pH Meter, Fisher Scientific, Pitts- Prarie, MN). A non-monochromated aluminum K␣ burgh, PA) were measured. Operating pressure was X-ray source (hν = 1486.6 eV) at a power of 250 W then increased in increments of 172 kPa (25
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