CCRO Pilot Recover Concentrate Potable Reuse Ad 45 D03759 en

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Desalination 518 (2021) 115300

Contents lists available at ScienceDirect

Desalination
journal homepage: www.elsevier.com/locate/desal

Operational optimization of closed-circuit reverse osmosis (CCRO) pilot to


recover concentrate at an advanced water purification facility for
potable reuse
Han Gu a, *, Megan H. Plumlee a, Michael Boyd b, Michael Hwang c, James C. Lozier d
a
Orange County Water District, Research & Development Department, 18700 Ward Street, Fountain Valley, CA 92708, United States of America
b
Desalitech (DuPont Water Solutions), One Gateway Center, Suite 809, Newton, MA 02458, United States of America
c
Jacobs Engineering Group, 2600 Michelson Drive, Suite 500, Irvine, CA 92612, United States of America
d
Jacobs Engineering Group, 1501 West Fountainhead Parkway, Suite 401, Tempe, AZ 85282, United States of America

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Closed-circuit reverse osmosis (CCRO)


was piloted to treat RO concentrate.
• Pilot is operationally sustainable from a
two year study in a water reuse facility.
• Adaptive control strategies were
employed to manage fluctuations in
water quality.
• CCRO treating RO concentrate could
increase the overall RO recovery to
91%.

A R T I C L E I N F O A B S T R A C T

Keywords: Closed-circuit reverse osmosis (CCRO) was piloted to treat RO concentrate from a potable reuse facility to in­
Closed circuit reverse osmosis crease the RO recovery beyond 85%. The study determined optimum operating conditions and maintenance
Pilot study requirements for sustained performance at maximum recovery including flux, cross-flow velocity, and membrane
Operational optimization
cleaning intervals. The CCRO pilot included a “side conduit” to displace spent concentrate without depressu­
Fouling and mineral scaling mitigation
Water and wastewater treatment
rizing the membrane elements. Performance was evaluated in terms of recovery, clean-in-place (CIP) frequency,
Potable water reuse and permeate quality. Adaptive control strategies were implemented to manage feed water quality fluctuations
by operating in variable recoveries where cycle-to-cycle recovery was controlled by concentrate conductivity,
feed pressure and volumetric recovery. An important contribution of this study is the long-term pilot dataset
collected over two years of operation, which showed the treatment of RO concentrate by CCRO to be technically

Abbreviations: AWPF, Advanced Water Purification Facility; CIP, Clean-In-Place; CCRO, Closed-Circuit Reverse Osmosis; ED, Electrodialysis; FO, Forward
Osmosis; FR, Flow Reversal; GPM, Gallons Per Minute; GWRS, Groundwater Replenishment System; MD, Membrane Distillation; MPV, Membrane Pressure Vessel;
MF, Microfiltration; MGD, Million Gallons per Day; OC San, Orange County Sanitation District; OCWD, Orange County Water District; PF, Plug Flow; PV, Pressure
Vessel; RO, Reverse Osmosis; ROF, Reverse Osmosis Feed; ROC, Reverse Osmosis Concentrate; SC, Side Conduit.
* Corresponding author.
E-mail address: hgu@ocwd.com (H. Gu).

https://doi.org/10.1016/j.desal.2021.115300
Received 19 April 2021; Received in revised form 8 August 2021; Accepted 9 August 2021
Available online 16 August 2021
0011-9164/© 2021 Elsevier B.V. All rights reserved.
H. Gu et al. Desalination 518 (2021) 115300

feasible and operationally sustainable. The pilot operated continuously with a CIP interval greater than two
months and produced permeate that met potable reuse requirements. At theoretical full scale, CCRO could in­
crease the facility RO recovery from 85% to 91% (92% was demonstrated in a short-term run). At the future
expanded plant capacity of 130 million gallons per day (MGD) (5.7 m3/s), this corresponds to a production
increase to 139 MGD (6.1 m3/s).

1. Introduction reset the mineral salt “crystallization induction clock” and thus prevent
mineral scaling [13,14]. Permeate flushing of the RO membranes is used
Reverse osmosis (RO) is a widely used membrane treatment process when the feed water is supersaturated [18–20]. In PFRO, the RO
to purify municipal wastewater for potable reuse [1–3]. Operated in concentrate is discharged once every few seconds in intensive short
multistage configuration, RO can achieve up to 85% recovery in potable pulses with high shear forces [15]. The membrane cleaning effect comes
reuse applications. Constraints in mineral scaling and electrical energy from a combination of shearing velocity, vibrations and osmotic back­
consumption at a typical advanced treatment facility prevent higher wash, driven by changing osmotic and gauge pressures [15,21].
recovery rates [4–6]. The rejected concentrate contains inorganic salts, CCRO is a patented process by Desalitech (DuPont Water Solutions)
organics, and microbes that must be discharged via permit to inland that utilizes standard RO components in a single-stage semi-batch design
discharge sites, evaporation ponds, deep well injection, or ocean outfall and a unique control methodology [22,23]. Conventional multi-stage
[2,7,8]. Disposal can be costly, particularly for inland facilities. Alter­ RO configurations use membrane-in-series design to achieve high re­
natively, the RO concentrate could be treated further to generate more covery, subjecting the lead elements in the first stage to high flux and the
product water and simultaneously minimize the volume of the concen­ tail elements in the last stage to low permeate flux and low crossflow
trate waste stream, with the potential to increase the overall recovery of conditions. This often leads to biofouling in the first stage and mineral
a potable reuse facility to greater than 90–95% [2,8]. Water recovery precipitation (scaling) in the last stage [24,25]. Unlike the steady-state
from concentrate is becoming more economically favorable as the cost of single-pass configuration of a multi-stage RO system, the single stage
membrane treatment technologies has dropped and the value of water CCRO primarily operates in a closed-circuit mode, at 100% permeate
has increased due to greater demand resulting from population growth production while recirculating the concentrate back to the feed in a
and water scarcity associated with climate change [9–11]. semi-batch process [26]. The recirculation in closed circuit mode con­
Increasing overall RO recovery can help maintain permeate pro­ tinues for minutes to a few hours until a given set-point is reached (based
duction when less wastewater effluent is available to treat due to on recovery, pressure and/or conductivity threshold) and then switches
drought conditions or water conservation. For example, the Orange to plug flow mode during which the concentrate is flushed from the
County Water District (OCWD) (Fountain Valley, CA, USA) Ground­ system. Unlike conventional RO where the recovery, crossflow velocity
water Replenishment System (GWRS) currently treats 100% of the sec­ and permeate flux are correlated, in CCRO these set-points can be
ondary wastewater effluent available from a wastewater treatment changed independently. Recovery is achieved in time, crossflow is
facility operated by the Orange County Sanitation District (OC San) adjusted using a circulation pump, and permeate flux is controlled by
(Fountain Valley, CA), approximately 118 million gallons per day the speed of a high-pressure pump [16,27,28]. Under this unique
(MGD) (~5.2 m3/s). Given OCWD’s scheduled final GWRS expansion configuration, CCRO systems can operate with a lower lead element flux
which will increase the plant advanced treatment capacity from 100 and higher crossflow velocity, which provide better control of fouling
MGD (4.4 m3/s) to 130 MGD (5.7 m3/s), OCWD will begin relying on an and scaling than traditional multi-stage RO systems. Frequent feed
effluent supply from a second OC San facility due to lack of sufficient flushing is thought to help limit or mitigate scaling, as the concentrate is
flows from the first facility because of increased water conservation over flushed before the induction period for mineral precipitation [26].
recent years. Further, OCWD is facing some uncertainty in the avail­ CCRO technology has been piloted at multiple municipal reuse fa­
ability of sufficient flows from the second facility (~153 MGD [6.7 m3/ cilities in California with positive results (Table 1). In January 2014, the
s] total requirement). If the addition of a concentrate treatment system first municipal reuse CCRO pilot was successfully commissioned by the
after the primary 3-stage RO were able to increase the overall recovery Los Angeles County Sanitation Districts to treat tertiary effluent and
from 85% to 91%, the District could generate 9 MGD (0.4 m3/s) of provided a sustained RO system recovery of 93% [29]. The City of Los
additional RO permeate (an increase from 130 MGD [5.7 m3/s] to 139 Angeles [30] and the Padre Dam Municipal Water District [31,32]
MGD [6.1 m3/s]) and reduce the concentrate disposal from 23 MGD to subsequently commenced similar pilots in 2015 and 2016, respectively,
13.8 MGD (1 to 0.6 m3/s) (Fig. S1). In other words, the plant could still that demonstrated more than 95% recovery was sustainable by incor­
maintain 130 MGD (5.7 m3/s) of permeate production even if the porating CCRO to treat tertiary effluent for potable reuse. A key differ­
wastewater source (influent to GWRS) were to drop to 143 MGD (6.3 ence between the CCRO pilot in the present study compared to these
m3/s), ensuring a more resilient treatment capacity (Fig. S1). previous municipal potable reuse pilots is they treated RO concentrate
Addition of a fourth RO stage to treat RO concentrate is not without derived from micro/ultrafiltered nitrified/denitrified effluent at a pri­
challenges. Recovery beyond the optimal level of the applied RO feed mary RO system recovery of 75 to 80%, while the CCRO pilot in the
water antiscalant can result in concentrations of mineral salts beyond present study featured a more challenging feed water quality treating
their solubility limits and beyond the ability of the antiscalant to inhibit RO concentrate derived from microfiltered partially-nitrified effluent at
precipitation onto the membrane surface and feed spacer (i.e. mineral a primary RO recovery of 85% (i.e., CCRO serving as a ‘fourth stage’ RO
scaling) [4,6,12]. unit) (Table 1).
Recently, several RO-based batch and semi-batch technologies have Despite the high recovery rate achieved in these studies, the CCRO
been successfully demonstrated for high recovery operation in industrial technology has some limitations. Lee et al. [33] has found in a recent
wastewater and municipal water reuse applications. These include flow experimental study with a semi-batch RO system (same design as a
reversal (FR)-RO, pulse flow RO (PFRO), and closed-circuit reverse CCRO system [17]) treating a gypsum model solution that even with a
osmosis (CCRO) [13–16]. In these systems, the RO membranes switch flushing period three times longer than the filtration time, complete
between periods of filtration mode and periods of flushing mode removal of surface scale was not possible. Furthermore, they found that
[15,17]. The FR-RO technology is based on the principle of periodically any fragments of crystals that remain on the membrane surface can serve
reversing the feed flow direction within the pressure vessel (flow as sites for further crystal growth in subsequent cycles [33]. In other
tangential to the membrane surface along the membrane element) to words, although CCRO can reduce fouling and scaling, it cannot

2
H. Gu et al. Desalination 518 (2021) 115300

completely eliminate scaling. Operating at high recoveries will still three-stage, 85% recovery RO system generates 18 MGD (0.79 m3/s) of
result in progressive membrane fouling, especially in the case of organic concentrate that is discharged via OC San’s 5-mile ocean outfall at no
and biofouling with simultaneous occurrence of mineral scaling cost to OCWD. Upon completion of the final GWRS plant expansion in
[26,28,31,33,34]. Another challenge is that due to the semi-batch na­ 2023, the full production capacity will increase from 100 to 130 MGD
ture of the CCRO, data collection and normalization of the CCRO system (5.7 m3/s) with disposal of 23 MGD (1.0 m3/s) of RO concentrate. To
is more complex compared with conventional RO systems; and there are further increase GWRS purified water production, OCWD is investi­
concerns regarding the robustness of the system, including the potential gating cost effective options to recover additional water from the RO
for the rapid pressure change during closed-circuit and purge sequences concentrate to generate a new water supply for the region.
to cause membrane integrity problems over long term operation. The purification process begins with the addition of sodium hypo­
In this study, CCRO treatment of GWRS RO feed water and RO chlorite (12.5% NaOCl, Gallade Chemical, Santa Ana, CA) to react with
concentrate was tested with a ReFlex™ Max CCRO pilot (Desalitech/ residual ammonia in the wastewater to form chloramines to reduce
Dupont, Newton, MA). The goal of the pilot study was to determine the membrane biofouling (Fig. S2). After MF, sulfuric acid (93%, Univar
feasibility of recovering more potable water from RO concentrate using Solutions Inc., Downers Grove, IL) is added with a targeted pH of 6.9 in
CCRO, recognizing that full-scale success would require a reasonable addition to 3.5 mg/L dose of antiscalant (AWC A-110, American Water
clean-in-place (CIP) interval (i.e., membrane cleanings ideally no more Chemicals, Plant City, FL) to control mineral scaling on the RO mem­
than monthly), suitable permeate water quality, and maximum recovery branes. In late March 2018, the antiscalant was switched to AWC A-108
to promote economic feasibility. Three alternative feed sources were at a dose of 2.5 mg/L. Thus, these same chemicals (sodium hypochlorite,
tested, Phase I: primary plant RO feed water (i.e., microfiltered partially- sulfuric acid, and antiscalant) were in the RO feed water (or RO
nitrified wastewater effluent) was used to fill both the pilot membrane concentrate) that was the influent to CCRO pilot (depending on testing
pressure vessel (MPV) and an empty pressure vessel – called the “side phase).
conduit” (SC); Phase II: RO concentrate from primary three-stage RO The full-scale RO plant provides the RO concentrate to CCRO pilot.
plant (at a RO recovery of 85%) was used for both MPV and SC; and The current RO recovery (85%) is limited by the traditional multi-stage
Phase III: RO concentrate was used to fill the MPV and microfiltration membrane array along with the saturation of sparingly soluble salts in
effluent (primary plant RO feed water) used to fill the SC. Three key the RO concentrate, namely calcium carbonate, calcium phosphate and
parameters were examined in order to optimize the operation, i) RO silica. For this study, a slipstream of RO concentrate from the AWPF
permeate flux, ii) permeate volumetric recovery per cycle (until SC process was plumbed to continuously supply the feed tank for the CCRO
flushing), and iii) CIP interval. In order to cope with this challenging pilot unit. Typical water quality of the RO feed and concentrate streams
wastewater source, a novel adaptive control strategy was developed to of the AWPF RO plant are shown in Table 2.
operate CCRO in a variable recovery mode whereby the start of each
cycle was triggered by key setpoints monitored in real time. 2.2. Pilot description

2. Materials and methods OCWD acquired a CCRO pilot system in 2017 and commenced a pilot
program to evaluate and demonstrate the system’s ability to enhance
2.1. OCWD advanced water purification facility (AWPF) for potable recovery at the GWRS Advanced Water Purification Facility (AWPF).
reuse The CCRO pilot comprises a high-pressure feed pump, single-stage MPV
with three 8-in. × 40-in. spiral wound RO elements (Hydranautics
The study was conducted at OCWD’s GWRS AWPF RO facility in ESPA2-LD, Oceanside, CA), a concentrate recirculation pump, and pro­
Fountain Valley, California. The GWRS is the world’s largest potable cess control valves (photograph of pilot in Fig. S3). Cartridge filters (1-
reuse facility and produces 100 MGD (4.4 m3/s) of potable water from a μm) (Fil-Trek Corporation KG-1-20-E5-BN, Cambridge, Ontario, Can­
secondary-treated municipal wastewater effluent. The purified water is ada) were installed on the pilot feed and SC feed lines to remove any
used for groundwater recharge to augment drinking water supply and suspended solids.
for injection into a coastal seawater intrusion barrier. The plant treats a CCRO systems alternate between two operational modes. In “closed-
blend of 25% trickling filter and 75% activated sludge effluent from OC circuit” (CC) mode, concentrate produced by the CCRO system is
San by full advanced treatment consisting of microfiltration (MF), RO, recirculated and blended with the pressurized feed water such that the
and an ultraviolet-advanced oxidation process (UV-AOP) with hydrogen feed water salinity increases continuously (Fig. 1a). This continues until
peroxide to create a high-quality product water (Fig. S2). The existing desired water production (volume of permeate) is reached based on one

Table 1
Summary of piloting of closed circuit reverse osmosis (CCRO) for potable reuse in North America.
Utility Facility name Pilot duration Description Effluent Primary RO Primary
pretreatment RO design

Tillman Advanced Water Pilot-testing CCRO as primary and


Nitrified/denitrified 2-stage RO
City of Los Angeles Purification Facility (AWPF) 2015 to 2017 secondary RO to provide overall RO Microfiltration
tertiary effluent R = 75%
Pilot Plant system recovery of 92 to 95%.
Los Angeles
Valencia Water Pilot-testing completed by LACSD
County 2014 (7 Microfiltration and
Reclamation Plant showed CCRO could increase facility Nitrified/denitrified 2-stage RO
Sanitation months pilot ultrafiltration
Advanced Water Treatment recovery to 93% when operated as either tertiary effluent R = 74%
Districts operation) (parallel)
Facility Pilot the primary or secondary RO.
(LACSD)
Side-by-side pilot to compare
Padre Dam East County Advanced 2-stage RO
2016 to conventional RO versus CCRO for third Nitrified/denitrified
Municipal Water Purification Ultrafiltration R = 75 to
present stage concentrate recovery; CCRO tertiary effluent
Water District Demonstration Facility 80%
sustained a recovery of 96%.
Groundwater
Pilot testing as primary RO and 75% (AS nitrified/
Replenishment System 3-stage RO
OCWD (this study) 2017 to 2019 secondary RO at 91% recovery with a denitrified), 25% TF Microfiltration
Advanced Water R = 85%
CIP interval of >2 months. secondary effluent
Purification Facility

Note: R = recovery, AS = activated sludge, TF = trickling filter.

3
H. Gu et al. Desalination 518 (2021) 115300

Table 2 consecutive sequences at five recovery set points between 85 and 92%
Average water quality (October 2018–February 2019) of the feed and concen­ and a permeate flux of 8.0 gallons/ft2/day (gfd) (which is equal to the
trate streams of the reverse osmosis (RO) plant at the Orange County Water 3rd stage flux in the AWPF primary RO) in a series of short-term fixed
District (OCWD) Groundwater Replenishment System (GWRS) Advanced Water recovery tests. The pilot was subsequently operated for extended runs at
Purification Facility (AWPF) operated at ~85% water recovery. the selected recovery for the remainder of the phase. This established the
Analyte Unit RO feed RO concentrate benchmark recovery for Phase II and III testing.
Mean % St. Mean % St. In Phase II, CCRO was operated as a ‘fourth’ RO stage treating AWPF
Dev.a Dev.a RO concentrate with the MPV and SC both fed with AWPF RO concen­
Aluminum μg/L 3.3 26 23.5 38 trate. The pilot was operated for an extended duration (~3 months) at
Barium μg/L 35.2 5 229 4 the target recovery determined in the previous phase. In Phase III, CCRO
Bicarbonate (as HCO3− ) mg/L 227 4 1451c 4 was operated as a ‘hybrid’ fourth RO stage still treating AWPF RO
Calcium mg/L 81 5 519 4 concentrate but RO feed water (MF filtrate) was used to fill the SC such
Chloride mg/L 340b 2035b
that this lower-salinity RO feed water entered the CCRO MPV at the start
– –
Electrical Conductivity μS/ 1744 2 – –
cm of each cycle.
Iron μg/L 108 11 708 10 During each phase, system performance was evaluated regarding the
Magnesium mg/L 26.5 6 175 6 following: i) CCRO volumetric recovery, ii) specific flux (normalized
Manganese μg/L 54.7 4 358 5
against temperature), iii) CIP frequency, and iv) permeate water quality
Orthophosphate (as mg/L 1.42 62 7.54 44
PO43− ) (determined by electrical conductivity). Additional water quality pa­
pH 6.9 1 7.6 1 rameters were measured including wastewater-derived organic con­
Potassium mg/L 19 5 124 4 taminants and reported by the authors for publication [35,36]. The
Silica (as SiO2) mg/L 21.4 4 124 13 operational metric for the extended testing was to demonstrate the
Sodium mg/L 235 4 1516 5
Sulfate mg/L 205 14 1334 15
CCRO system could operate for at least 30 days between CIP events
TDS mg/L 1029 2 6570 3 while achieving the following goals: (1) <60% decline of normalized
Total organic carbon mg/L 7.6 2 – – specific flux, (2) <30% increase of normalized salt rejection, and (3)
Zinc μg/L 18.4 10 95.2 10 <30% increase of normalized differential pressure.
a
% St. Dev. = standard deviation/mean × 100%.
b
Estimated based on charge balance. 2.4. CCRO recovery
c
Estimated based on feed concentration and water recovery data.
Two terms were used to calculate recovery of the CCRO system,
of the following set-points: i) the maximum volume recovered (i.e., different from a conventional RO system due to the semi-batch or “cy­
production volume of permeate), ii) concentrate conductivity attained, clic” nature of operation. The apparent volumetric recovery percentage
or iii) feed pressure attained. No concentrate is bled from the system (RCCRO) was defined as the ratio of the permeate volume to the total
during closed-circuit operation (i.e. 100% permeate recovery). In “plug volume, where the total volume is the CCRO permeate volume plus the
flow” (PF) mode, the concentrate is purged from the system when the waste stream volume, or the permeate volume plus the SC feed flowrate:
desired set point is reached and replaced with fresh feed water. The
Desalitech ReFlex™ Max pilot used in this study utilizes a side conduit RCCRO (%) =
CCRO Permeate Volume
× 100
(SC) to complete the PF mode in two steps, which is a key difference CCRO Permeate Volume + CCRO Concentrate Volume
compared to previously tested municipal potable reuse CCRO pilots (1)
[22]. The SC is a blank pressure vessel (i.e. no membrane elements RCCRO will increase with increasing time associated with each CCRO
installed) with a volume equal to the MPV. The pressurized CCRO cycle. Because the permeate produced by CCRO would add to the main
concentrate is first purged into the SC while fresh feed water (from the RO facility permeate in a full-scale implementation, the GWRS overall
last sequence) is simultaneously pushed to the front of the MPV recovery percentage (Roverall) was defined as the theoretical full-scale,
(Fig. 1b). The concentrate replacement pump then refills the SC with overall recovery of the entire AWPF system downstream of the MF
fresh feed water while flushing the concentrate to waste without processes based on the additional water produced by CCRO (i.e., ac­
depressurizing the membranes in MPV (as shown in Fig. 1c). counting for the additional recovery by CCRO), calculated as:
This exchange and flushing sequence is executed without stopping
AWPF RO Permeate + CCRO Permeate
the high-pressure feed pump, and the permeate production continues Roverall (%) = × 100 (2)
without stopping. The ReFlex™ Max pilot design also provides the MF Effluent Flow
flexibility to operate at shorter sequence times (as low as 90 s) compared
to the ReFlex™ design which requires a minimum sequence time of 6 2.5. Membrane clean-in-place (CIP) and autopsy
min. This allows the ReFlex™ Max to operate at recovery rates ranging
from 35% to 98%, providing flexibility in both brackish and seawater CIPs were performed when required due to a reduction in the
applications [22,23,28]. normalized specific flux (more than 60% decline from initial specific
flux), increase in feed pressure, and after each phase of testing. Each CIP
was intended to restore any loss of specific flux and/or significant
2.3. Experimental plan changes in salt passage and differential pressure. The CIP protocol
initially adopted was similar to that used by OCWD for cleaning all
The operational goal of the CCRO pilot testing was to evaluate the stages of the GWRS RO system given that fouling and scaling in the
performance of the ReFlex™ Max CCRO configuration for recovery of CCRO was anticipated to be similar to that in the GWRS RO system,
water from AWPF RO concentrate. The pilot testing was completed in particularly in the third stage. A 2.0% (wt/vol) sodium tripolyphosphate
three phases. In Phase I, CCRO was operated as a primary RO unit (STPP) (Brenntag Pacific, Santa Fe Springs, CA) and 0.20% (wt/vol)
treating the AWPF RO feedwater (chloraminated MF filtrate chemically sodium dodecylbenzenesulfonic acid (SDDBS) (Brenntag Pacific, Santa
conditioned by acidification and antiscalant addition). Phase I evaluated Fe Springs, CA) solution were made with RO permeate in a 120-gallon
CCRO as an alternative to conventional 3-stage RO for potable reuse. tank. The pH was raised to 11 with sodium hydroxide and maintained
Phase I commenced with a 100-h break-in period of operation at a between 30 and 35 ◦ C with a heating coil placed in the CIP tank. The
conservative recovery (85%), then the CCRO pilot was operated for two solution was recirculated through the pressure vessel for 30 min (20 gpm

4
H. Gu et al. Desalination 518 (2021) 115300

Fig. 1. Schematic of a CCRO pilot (Desalitech ReFlex™ Max) in (a) closed circuit mode, (b) purge mode and (c) during side conduit refill (image courtesy of
Desalitech/DuPont).

5
H. Gu et al. Desalination 518 (2021) 115300

[1.26 L/s] per pressure vessel), followed by a 1-h soak (repeated three Table 3
times), and ended with a 45-min flush with RO permeate. A specialty RO Water quality testing matrix over CCRO operating cycle at end of phase A.
cleaner (AWC C-227) was used during Phase II and III to improve CIP Parameter Stream
results (details are shown in Supplementary Text S1).
CCRO FEED CCRO-CONC. (diluted) CCRO-PERM
At the completion of Phase I and III, the tail (third) element from the
CCRO pilot was removed for performance testing and autopsy at the CB CE CB CE CB CM CE

AWC laboratory (Plant City, Florida). The tail element is subject to the RO parameters X X X X X X X
lowest cross flow velocity, permeation, and highest concentration po­ pH X X X X X X X
Conductivity X X X X X X X
larization effect, especially at the concentrate exit region of the element,
Temperature X X X X X X X
and thus has the highest scaling potential for various mineral salts.
Biological and organic fouling (including antiscalant fouling) can also Notes:
develop on the sites of mineral scaling [12]. The membrane surface was Water quality sampling for the extended test run was performed once on
February 6, 2018 during operation at 92% recovery. Operating conditions and
analyzed by scanning electron microscopy (SEM), x-ray spectroscopy
results are further described in Section 4.
(EDX), energy dispersive spectroscopy (EDS) with superimposed
CCRO-FEED = sampling port (S3) of system feed (before recirculation enters
elemental imaging (SEI), and Fourier transform infrared (FTIR) line).
spectroscopy. CCRO-CONC = sampling port (S4) of system with immediate dilution (100-mL
sample diluted with 1 L of distilled water).
2.6. Water quality analysis CCRO-PERM = product water sample port (S5) collected from line (i.e.,
changing quality; not permeate tank).
If CCRO is used to treat RO concentrate as a ‘fourth stage’ RO unit in CB, CM, CE = sample collected at cycle beginning, cycle middle, or cycle end.
a full-scale potable reuse application, CCRO permeate would ideally be X = one sample collected.
blended with permeate from the 3-stage (primary) RO system. OCWD RO parameters = various inorganic parameters generally used to assess or
GWRS permit requirements for RO permeate quality are limited to predict RO performance in term of containments removal: Ca, Mg, Na, K, Ba, Sr,
NH4 (via NH3), HCO3, CO3 (via alkalinity), Cl, SO4, F, NO3, PO4, SiO2, TDS.
turbidity (shall not exceed 0.2 Nephelometric Turbidity Units [NTU] for
more than 1.2 h in any one day period; and 0.5 NTU at any time) and
percent ultraviolet transmittance at 254 nm (%UVT254) (>90%) [37]. 3. Results and discussion
The plant must also demonstrate 2-log removal of total organic carbon
(TOC) by the RO system as a surrogate for pathogen (virus) removal Table 4 list the pilot test conditions (e.g. duration, recovery, and
which is measured by online RO feed and permeate TOC analyzers. flux) for Phase I, II, and III. To manage mineral precipitation in the full-
OCWD also observes an internal RO permeate critical control point limit scale GWRS RO system, feed water (MF effluent) was dosed with AWC A-
of less than 0.1 milligrams per liter (mg/L) TOC via the online permeate 110 antiscalant at 3.5 mg/L until late March 2018 (during Phase I and
analyzer as an indicator of normal operating conditions. The GWRS II), at which time the antiscalant was switched to AWC A-108 at a dose of
finished water (after UV/AOP, post-treatment decarbonation, and lime 2.5 mg/L (partway through Phase III). The projected scaling potential
addition) is subject to a TOC limit (<0.5 mg/L) and total nitrogen limit for sparingly soluble salts in the concentrate based on GWRS RO system
(<10 mg/L, <5 mg/L preferred) along with various other monitoring operation at 85% recovery and the use of both AWC A-110 and A-108
requirements for regulated drinking water quality parameters as well as are presented in Fig. S4a and b, as modeled by the AWC Proton software,
organic constituents dictated by the California Recycled Water Policy with the scaling potential at 92% recovery shown in Fig. S4c [39]. Silica
[37,38]. At this time, California has not established specific permitting and the antiscalant are the most likely scaling species in the feed (su­
requirements for CCRO for potable reuse. Recognizing the need to persaturated in concentrate).
achieve suitable water quality consistent with California potable reuse
requirements, an objective of the pilot study was to characterize the
quality of the CCRO permeate and how it varies during the closed-circuit
sequence.
During Phase I, one sampling event was conducted to profile the
quality of the CCRO feed, permeate, and concentrate at the beginning, Table 4
Duration, recovery, and flux test conditions and feed water source for each
middle, and end of the closed-circuit sequence. This event included
CCRO pilot test phase.
analysis of inorganic compounds (e.g. metals, anions, TOC and total
dissolved solid [TDS]) by standard methods at OCWD’s Philip L. An­ Parameter Pilot study phases
thony Water Quality Laboratory. Table 3 summarizes the water quality Phase I Phase II Phase III
sampling and analysis performed during a typical CCRO cycle at the end Feed water source Primary RO feed 3rd stage RO Diluted 3rd stage
of Phase I. The present study focuses on CCRO operational performance (membrane concentrate RO concentrate
and related key water quality indicators of performance; additional pressure vessel)
comprehensive water quality samplings were performed during all Feed water source Primary RO feed 3rd stage RO Primary RO feed
(side conduit) concentrate
phases (e.g., organic contaminants) and will be reported in a follow-up
Permeate flux (gfd) 8.0 gfd (13.6 6.4 (11.0 LMH) 6.4 (11.0 LMH)
publication [35]. LMH)/6.4 (11.0
Given the importance of TOC as a surrogate for pathogen removal at LMH)
the GWRS, online TOC measurements were taken for the CCRO feed and Pilot period 09/14/2017–02/ 3/2/2018–7/ 7/12/2018–2/
27/2018 11/2018 21/2019
permeate during select periods of the testing. The online TOC moni­
2/21/2019–11/
toring was performed using Suez (formerly GE) Sievers 900 TOC online 30/2019a
analyzers, programmed to report TOC data at 4-min intervals. This data Pilot duration (weeks) 27 19 31, 40
served to characterize real-time changes in TOC during a typical closed-
Notes:
circuit sequence and to calculate surrogate pathogen log removal values
gfd = gallon(s) per square foot per day.
(LRVs) by the CCRO system. LMH = liter(s) per square meter per hour.
a
Testing during this period was completed using DuPont Filmtec BW30XFRLE
RO membrane elements in the CCRO pilot. All other testing shown was
completed using Hydranautics ESPA2-LD RO membrane elements.

6
H. Gu et al. Desalination 518 (2021) 115300

3.1. CCRO treatment of RO feed water (Phase I) a reduced flux of 6.4 gfd (10.9 LMH) and increased recirculation flow
rate of 52 gpm (3.28 L/s) to maintain the same crossflow velocity as
3.1.1. Recovery optimization based on short and extended runs at fixed operation at 8 gfd (13.6 LMH) flux. Under these conditions, a maximum
recovery recovery of 92% was sustained, limited by amorphous silica scaling and
In Phase I, the CCRO ReFlex™ Max pilot was operated with AWPF fouling associated with silts/clays when operated with AWPF RO feed
RO feed water (i.e., microfiltration effluent) with the objective to water as the feed to the CCRO process. This established the benchmark
determine the maximum recovery rate (RCCRO) while meeting the operational recovery percentage for tests in Phase II and III.
operational metrics. Operation as a primary RO resulted in the longest The recovery and pressure profile of the CCRO pilot operated during
closed-circuit (CC) sequence times and the RO elements were exposed to Phase I at 92% recovery is shown in Fig. 2. As the salinity of the feed
the widest range of concentrate quality (i.e., TDS). Data collected during water increased due to recirculation of the CCRO concentrate, the
Phase I were used to generate the operational set-points for Phase II and pressure required to maintain specific flux increased. It is hypothesized
Phase III testing. A 100-h break-in period at 85% recovery and 8 gfd or that scaling was mitigated by operating the RO elements in CC-mode
13.6 L/min/h (LMH) permeate flux equal to the AWPF RO unit third with periodic SC flushing and refill.
stage permeate flux was completed to stabilize the RO elements on the An alternate operational strategy was also tested by application of
AWPF feed water. The operational data was normalized and the baseline periodic low recovery purge sequences or “mini-cleaning” periods be­
performance determined for specific flux, salt rejection, and trans­ tween high recovery CC sequences. In this mode, the CCRO pilot oper­
membrane pressure. ated at an elevated recovery of 94% for several CC sequences (~1.9 h/
The fixed-recovery optimization tests included a series of dual- sequence) followed by low recovery (50%) operation for three CC se­
sequence (two consecutive sequences) runs and extended runs encom­ quences (~0.05 h/sequence). This strategy appeared to achieve high
passing multiple sequences. The sequence times (CC + PF) and operating recovery for a few CCRO cycles (Figs. S8 and S9), but on close exami­
conditions for both the dual-sequence and extended runs are presented nation, the average recovery over extended operation only achieved
in Table 5. The dual-sequence runs were completed at five recoveries: approximately 89% (based on sequence timing).
85%, 87%, 89%, 90%, and 92%. For the first four targeted recovery Upon completion of Phase I, the tail element from the pilot unit was
setpoints, the normalized specific flux returned to the initial level. At removed for performance testing and membrane autopsy. The autopsy
92% recovery, the feed pressure rapidly reached approximately 250 psi, identified the primary foulants as silts/clays and organics (Supplemen­
which is relatively high and indicative of membrane scaling or fouling, tary Text S2). A CIP was performed on the remaining two elements using
precluding tests at higher recovery. Following these tests, the unit re­ the OCWD CIP protocol and the third element was replaced with a new
covery rate was temporarily reduced to 85% recovery, during which the element before beginning Phase II (Table 7).
maximum feed pressure at the end of an operating sequence/cycle
declined and stabilized at approximately 180 psi. 3.1.3. Permeate water quality during a closed circuit (CC) sequence
A longer test comprising eight sequences was performed at 90% re­ At the end of Phase I, sampling during a typical CCRO closed-circuit
covery at 8.0 gfd (13.6 LMH) for approximately 2.5 days (Fig. S5). sequence during operation at 92% recovery was conducted. Feed,
During this time, the feed pressure reached as high as 22.1 bar (330 psi) permeate, and concentrate samples were collected and analyzed at the
at the end of a cycle (Fig. S6). After a reduction in recovery to 85%, the beginning and end of a cycle, and permeate collected and analyzed in
run continued for another 5 days. At the reduced recovery, feed pressure the middle of the cycle (Fig. 3). The feed quality remained consistent
again declined and generally stabilized, demonstrating sustainable from beginning to end of the cycle (data not shown). Except for calcium,
operation. In another extended test, a recovery of 93% at 6.4 gfd (11.0 the results clearly illustrate how the concentration of each parameter
LMH) was attempted for 10 sequences, which resulted in a rapid and increased during the closed-circuit cycle. The increase in the permeate
substantial decline in specific flux (Fig. S7). Recovery was subsequently solute concentration ranged from 1×–7× by the end of the cycle as
reduced to 92%, after which stable performance was observed. Fast compared to a concentration factor of 1×–12.5× for constituents in the
specific flux recovery was observed when the recovery point was CCRO feed based on operation at 92% recovery. The percent rejection
deceased from 93% to 92% (Fig. S7) [40]. In summary, the short and for each parameter is shown at the beginning, middle, and end of the
extended runs shows that 90–92% is likely the maximum RCCRO range CCRO cycle in Fig. 3. An increase in permeate concentration was
the CCRO pilot can stably operate when treating AWPF RO feed (at a observed as the concentrations of constituents in the feed water
permeate flux of 11.0 LMH). increased during the cycle, although the amount of constituent increase
in the permeate and recovery loss varied based on constituent. Rejection
3.1.2. Stabilization and optimization of CCRO performance generally remains constant or slightly increase for most constituents and
During Phase I, several adjustments were made to the CCRO pilot only decreased for ammonia nitrogen and silica. Greater change was
operation to optimize the operation. These included reducing permeate observed for constituents having lower initial rejection (ammonia ni­
flux, increasing cross flow velocity, and optimizing the SC engagement trogen and boron,). Nonetheless, the total nitrogen was <5 mg/L as
volume required to adequately flush the CCRO unit during PF mode. nitrogen (N) and TOC < 0.5 mg/L as carbon (C) in the CCRO permeate
Feed water dosing of an organic dispersant (AWC A-132) at 5 and 8 mg/ which complied with the GWRS finished water requirements of <10 mg/
L was also attempted but yielded no noticeable changes in performance. L as N (with <5 mg/L as N preferred) and <0.5 mg/L as C.
Of these modifications, the most beneficial was operation of the pilot at The silica levels in the ‘end of cycle’ sample (279 mg/L, which

Table 5
Summary of sequence times for recovery optimization test period (Phase I).
Recovery (%) Part 1 – dual-sequence recovery testing Part 2 – multiple-sequence recovery testing

Number of sequences Sequence time (minutes) Run time (hours) Number of sequences Sequence time (minutes) Run time (hours)

85% 2 37 0.6 38 37 24
87% 2 60 1.0 N/A N/A N/A
89% 2 72 1.2 N/A N/A N/A
90% 2 81 1.4 64 81 87
92% 2 108 1.8 135 108 242
93% N/A N/A N/A 9 144 22

7
H. Gu et al. Desalination 518 (2021) 115300

Fig. 2. Phase I volumetric recovery and membrane feed/outlet array pressure operating at 92% recovery (data from 12/10/2017).

Fig. 3. Phase I CCRO permeate water quality at the beginning, middle, and end of a CCRO cycle operating at 92% recovery. The percent rejection is shown at the top
of the bars (data from 2/6/2018).

corresponds to the CCRO concentrate) were slighter greater than the potential for establishing 2-log credit using TOC (based on primary RO
level assumed in the Proton antiscalant projection (274 mg/L). None­ feed compared to blended RO permeate). Further, other pathogen sur­
theless, the silica concentration did not result in silica scaling at 92% rogates with greater log removal could be utilized in place of TOC,
recovery, which was the primary consideration for the maximum RCCRO including strontium which has demonstrated >3-log removal by CCRO
that could be sustainably achieved. in other studies [41].
The online TOC data was collected over an approximately 7-h period
during Phase I (Fig. S10). The feed TOC varied from 7.2 to 8.2 mg/L
during this period, while permeate TOC exhibited cyclic levels that 3.2. CCRO treatment of RO concentrate with concentrate SC flush (Phase
varied from 0.110 to 0.180 mg/L. The cyclical behavior was consistent II)
with the results of permeate grab sampling and reflected the increase in
TOC concentration in the CCRO feed water (via recirculation loop) over In Phase II, the CCRO pilot unit was operated to treat and recover
the course of a closed-circuit cycle. LRVs for TOC ranged from 1.68 to water from a portion of the concentrate from the AWPF RO system, with
1.87 (see Fig. S10). This is less than the 2-log removal required for the the objective of determining the CIP interval while achieving an Roverall
primary RO system at GWRS to be granted 2 LRV credit for pathogens by of 92% that was demonstrated in Phase I. The only difference between
the State of California Division of Drinking Water (DDW) [37]. The operating as a primary RO compared to operating as a fourth stage RO
primary RO system of GWRS consistently achieves 2-log or more of was the amount of time the CCRO pilot was in CC mode to achieve the
pathogen credit based on online TOC monitoring (LRVs range from 45% target RCCRO. The pilot test conditions (e.g. duration, recovery, and
2.0–2.8 annually, with greater than 2.3 LRV 90% of the time) However, flux) are listed in Table 4. A reduction in specific flux to 0.04 gfd/psi
if CCRO was implemented at full scale (such as the case in Fig. S1), the (0.998 LMH/bar) triggered a CIP.
relatively small flow of CCRO permeate (20 MGD) would be blended Rapid specific flux (permeability) decline, 60% loss within 3 weeks,
with the much larger permeate flow from the primary RO system was observed during the first run shown in Fig. 4. The recirculation
(119.25 MGD), resulting in flow-weighted log removal in the range of velocity was increased from 40 to 65 gpm in the second and third run by
2.14 to 2.48. Thus, depending on the regulator-determined approach for increasing the recirculation rate of the pilot. The higher velocity of water
crediting a CCRO-based ‘fourth’ stage treatment system, there is flow was thought to mitigate deposition of foulants and formation of
scalants on the membrane surface through increased turbulence over the

8
H. Gu et al. Desalination 518 (2021) 115300

Fig. 4. Phase II CCRO pilot average specific flux, feed pressure, normalized pressure drop across MPV, and membrane salt rejection based on EC measurements
where AWPF primary RO concentrate was the feed water to CCRO and side conduit. CIP trigger was the normalized specific flux of 0.04 gfd/psi (0.998 LMH/bar).

feed spacers. However, this change did not increase run time between
Table 6
CIPs. Finally, reducing the RCCRO from 45% to 40% (91% Roverall) then to
Apparent CCRO recovery and GWRS overall recovery using AWPF RO feed and
36.5% (90.5% Roverall) while increasing the crossflow rate (velocity) to
RO concentrate for CCRO side conduit (SC) feed.
65 gpm in the third run was able to achieve a run time of 26 days (Fig. 4).
An autopsy following completion of Phase II was not considered Case AWPF Apparent GWRS overall recovery (RO system)
primary RO CCRO
necessary given the sustainable operation of the CCRO unit. recovery recovery
CCRO SC supply = CCRO SC
AWPF RO supply =
concentrate AWPF RO feed
3.3. CCRO treatment of RO concentrate with primary RO feed water side 1 85.0% 40.0% 91.0% 81.6%
conduit (SC) flush (Phase III) 2 85.0% 45.0% 91.8% 84.5%
3 85.0% 57.5% 93.6% 90.0%
4 85.0% 60.5% 94.1% 91.1%
During Phase III the CCRO unit continued to operate as a ‘fourth
5 85.0% 61.0% 94.2% 91.2%
stage’ treating AWPF RO concentrate but in this phase the SC was filled 6 85.0% 66.0% 94.9% 92.8%
with AWPF RO feed (ROF) instead of RO concentrate. The CCRO pilot
was operated to determine if the use of ROF to flush the CCRO pressure
vessel would reduce the rate of specific flux decline during normal op­ Fluctuations in RO concentrate water quality created a major chal­
erations. The ROF flush had two potential benefits. First, the undersat­ lenge for maintaining RO membrane performance in Phase II. Diurnal
urated (in sparingly soluble salts) ROF water introduced to the CCRO variations in the electrical conductivity (EC) of the AWPF ROC water
feed at the beginning of the CC mode could potentially act as a “mini- was mirrored in the CCRO recirculation loop (Fig. S11). The ROC EC
clean” to dissolve any scale or crystals already formed on the membrane varied from 8200 to 12,000 μs/cm with an estimated TOC between 40
surface. Second, it increased the duration of the CC sequence, exposing and 54 mg/L that represented a significant load of organic fouling po­
the membrane to a pressure and salinity ‘swing’ that could help to tential. In addition to diurnal variations, AWPF ROC conductivity was
reduce biological fouling [26]. However, if the SC is filled with ROF observed to be lower on Sundays and Mondays and vary hourly
from the AWPF, this source water is no longer available for treatment in (sometimes dropped to below 2 mS due to intrusion of CIP rinse water
the primary RO system, which must be accounted for in the determi­ from RO plant) (Fig. S11).
nation of overall recovery of a plant as it reduces the calculated recovery In order to mitigate the impacts of feed water quality changes on
of the primary RO. pilot performance, an adaptive control strategy was implemented at the
Six different recovery scenarios using either the AWPF ROF or RO beginning of Phase III. Instead of initiating the purge mode (PF) once a
concentrate for the SC supply are listed in Table 6. The derivation based fixed maximum recovery was achieved (volumetric) for every sequence,
on mass balance around the CCRO and the AWPF (three-stage RO) + the pilot was operated in a variable recovery mode where the command
CCRO (as ‘fourth’ stage RO) is shown in the Supplementary Text S3. The for entering the purge mode was triggered when one of the three
data illustrate that higher RCCRO is required (~61%) to obtain 91% thresholds was met. The first trigger for activating the purge mode was
Roverall, when using the AWPF ROF as feed for the SC flush. A 40.0% the CCRO concentrate EC measured prior to entering the circulation
RCCRO is required to obtain 91% overall recovery, when using the AWPF pump (see Fig. 1), which represents the point of highest EC at any given
RO concentrate as feed for the SC flush. As noted in Section 2.4 (Eq. (2)), time during CC operation. The rate of membrane fouling was noted to
the Roverall is the hypothetical recovery for the entire system—AWPF and increase as indicated by initial pressure at the start of a CC sequence
CCRO combined. It assumes all the AWPF RO concentrate is treated by when CCRO concentrate conductivity exceeded 16.5 mS (tests were
the CCRO system. Therefore, Roverall would be less if all RO concentrate conducted up to a conductivity of 19.5 mS). Using this trigger, the CCRO
was not treated by the CCRO system. pilot adapted to the changes in the CCRO concentrate (and feed)

9
H. Gu et al. Desalination 518 (2021) 115300

conductivity in real time, thereby optimizing the overall pilot system


recovery while avoiding the point of failure identified as a CCRO
concentrate EC > 16.5 mS.
The second trigger to activate the purge mode was the apparent
CCRO recovery. Recovery set points at 61.0, 61.5%, 62.0%, 62.5%, and
63.0% were tested with an EC set point of 16.5 mS/cm, where each point
was tested for one to three days. The feed pressure and average specific
flux of the membranes were closely monitored. If there was rapid initial
feed pressure increase at the beginning of a CC cycle (>10 psi), the re­
covery set point was too high. To recover the system, the recovery set
point was lowered to 50%, so that the pressure could drop slowly over
time by the flush mode. A RCCRO of 61.0% was determined to be most
suitable given weekly episodes of low conductivity that exhibited higher
fouling potential, as operating >16.5 mS in the concentrate on these
‘low conductivity’ days resulted in fouling of the membranes. Fig. 5
shows the evolution of feed and recirculation concentrate EC and RCCRO
for several CCRO sequences controlled by the maximum recovery trigger
in the case of treating feed water with a low EC (~9 mS). In Fig. 6, Fig. 6. Illustration of adaptive operation of CCRO pilot under conditions of
adaptive operation is shown in the case of high feed EC (~12 mS), the high feed EC. The CCRO purge mode was triggered when the CCRO concentrate
purge mode was triggered when the CCRO concentrate EC reach 17 mS EC reached 17 mS. The dashed line indicates the initial (lowest) EC in the CCRO
(set based on scaling potential). concentrate during purge of PV with GWRS ROF. Permeate flux: 6.4 gfd (11.0
LMH). CCRO sequence duration: 9.5–12 min. Data from 4/17/2019.
Lastly, a high feed pressure of 220 psi (15.2 bar) was the third trigger
to enter purge mode. If the pilot operates in CC mode for too long, the
pressure will build up quickly in the MPV due to the increase in feed
water salt concentration. High feed pressure in RO MPV typically in­
dicates severe membrane fouling or scaling and a CIP is required to
restore performance. Although triggering a purge mode won’t replace a
CIP, by limiting CCRO operation to this pressure, the filtration time will
be shortened, and the degree of fouling/scaling (measured by specific
flux decline) could be reduced by SC flushing before the application of a
CIP. Fig. 7 illustrates the adaptive control strategies for the CCRO pilot
over a 9-day period.
After switching the feed source to the side conduit from AWPF RO
concentrate to ROF in Phase III, together with the programming changes
to trigger the purge mode when one of three setpoints was reached, the
CCRO was successfully operated for 55 days before a CIP was required.
The specific flux and feed pressure for the first run are shown in Fig. 8. In
the next run, also shown in Fig. 8, 62 days of operation was achieved
before a CIP was required. These runs illustrated that the programming
changes enabled optimum operation of the pilot unit. The RCCRO ranged Fig. 7. Demonstration of Phase III adaptive control strategies of the CCRO pilot
from 59.0–61.0%, corresponding to a theoretical Roverall between 90.6 over a 9-day period. The CCRO pilot enters purge mode when one of three
and 91.2%. Upon successful completion of the two extended runs, the setpoints (recirculation EC, volumetric recovery, and feed pressure) was
reached. The CCRO feed EC is shown for reference.

Hydranautics ESPA2-LD elements were removed from the CCRO and the
tail element was tested for performance and an autopsy performed.
DuPont Filmtec BW30 XFRLE-400/34 RO elements were then
installed in the CCRO unit and further runs were completed (see Fig. 8)
due to some concern that the Hydranautics membranes had inadver­
tently exceeded pressure recommendations (potential compaction)
during the early multi-phase trials and to test a different manufacturer’s
membrane. The DuPont Filmtec membrane was selected based on suc­
cessful performance in the GWRS AWPF and ability to maintain stable
salt rejection following repeated CIPs.
As shown in Fig. 8, the CCRO pilot loaded with DuPont elements was
operated continuously using the same programming setpoints described
above at 59.0–61.0% apparent CCRO recovery for 71 days prior to
requiring a CIP. Specific flux was restored by the CIP after which a
second run was completed for 73 days, demonstrating that CCRO
operation is sustainable at ~60% recovery (Table 7). After the second
CIP, a third run was initiated at 59–61% recovery. After 30 days, re­
Fig. 5. Illustration of adaptive operation of CCRO pilot under conditions of low
covery was increased to 66%, corresponding to a theoretical GWRS
feed EC. The CCRO purge mode was triggered when CCRO apparent recovery
overall recovery of 92.8%, and the unit was operated for an additional
reached 61%. The lower dashed line indicates the initial (lowest) EC in the
CCRO concentrate during purge mode of PV with GWRS ROF. Permeate flux:
33 days (63 days total). At the higher recovery, the feed pressure
6.4 gfd (11.0 LMH). CCRO sequence duration: 9.5–12 min. Data collected: 4/ increased and specific flux decreased at greater rates, indicating a
15/2019. greater rate of fouling similar to operation at 93% recovery observed in

10
H. Gu et al. Desalination 518 (2021) 115300

Fig. 8. Phase III daily average of specific flux and feed pressure of the CCRO pilot illustrating completion of membrane CIPs whenever the feed pressure reaches
trigger of 15.2 bar. CCRO R% = CCRO apparent recovery; overall R% = GWRS overall recovery.

Table 7
Summary of CIP events.
Phase Date Membrane CIP regime Average conditions over three CIP Pre-CIP Post-CIP
circuits

pHa Temperature Cross flow Feed Normalized specific Feed Normalized specific
(◦ C)b (gpm)c pressure flux (gfd/psi) pressure flux (gfd/psi)
(psi) (psi)

I 2/27/ ESPA2-LD 2% STPP/ 11.62 26.8 21.9 260 0.023 73 0.132


2018 0.20% SDDBS
II 4/24/ ESPA2-LD 2% STPP/ 11.40 26.3 23.0 244 0.043 172 0.076
2018d 0.20% SDDBS
II 5/7/ ESPA2-LD 2% AWC C- 12.04 23.3 30.0 207 0.057 117 0.110
2018 227
II 5/30/ ESPA2-LD 2% AWC C- 12.29 31.4 46.7 256 0.036 126 0.100
2018 227
II 6/28/ ESPA2-LD 2% AWC C- 12.21 31.0 50.0 236 0.040 95.3 0.086
2018 227
III 11/8/ ESPA2-LD 2% AWC C- 11.97 27.7 52.0 213 0.055 85 0.112
2018 227
III 11/20/ ESPA2-LD 2% AWC C- 12.24 31.0 52.0 206 0.054 103 0.090
2018 227
III 5/22/ BW30- 2% AWC C- 12.08 33.9 49.0 220 0.044 120 0.100
2019 XFRLE 227
III 9/12/ BW30- 2% AWC C- 11.91 38.0 48.0 225 0.045 120 0.120
2019 XFRLE 227
a
pH adjustment achieved with sodium hydroxide. Target pH was 11 for 2% STPP/0.20% SDDBS and 12 for 2% AWC C-227.
b
Target temperature was 30–35 ◦ C for 2% STPP/0.20% SDDBS and 35–39 ◦ C for 2% AWC C-227.
c
Target cross flow was 20 gpm for 2% STPP/0.20% SDDBS and 50 gpm for 2% AWC C-227.
d
CIP on 4/24/2018 with 2% STPP/0.20% SDDBS was ineffective and resulted in switch to 2% AWC C-227 for next CIP on 5/7/2018.

Phase I. implementation of CCRO as a ‘fourth’ stage RO, primary RO feed must


The four extended runs conducted with the Hydranautics and be diverted to the installed CCRO system and the volume used for
DuPont membranes demonstrated that the theoretical Roverall can be flushing CCRO is no longer available to feed the primary RO system. This
sustained near 91% and that 92% could be achieved while meeting the must be accounted for to determine overall system recovery as it results
30-day minimum preferred CIP interval. A greater than 2-month CIP in a reduction in the primary system volumetric production and an
interval is more attractive from an operational perspective. All CIPs equivalent increase in the required CCRO capacity (or CCRO recovery)
performed during Phase III used the modified CIP protocol (Supple­ to achieve the same overall system recovery. In the case of an existing
mentary Text S1 and Table 7). The pilot was able to maintain high primary RO plant now oversized, the reduction in water produced by the
average normalized salt rejection and normalized differential pressure primary RO can be addressed in one of two ways: 1) reduce the average
for the two membranes tested (Fig. 9). flux of the existing RO units and, thus, their permeate production; 2)
Although Phase III was successful in which primary RO feed water remove one or more trains from service and rotate trains in operation.
(microfiltration effluent) was used to fill the SC, the use of primary RO Both options have the advantage of reduced fouling and CIPs for the
feed water for CCRO PV flush does have disadvantages. In a full-scale existing RO units and the second option has the advantage of

11
H. Gu et al. Desalination 518 (2021) 115300

Fig. 9. Phase III daily average of normalized salt rejection and normalized differential pressure during CCRO pilot testing.

maintaining current train operating conditions but will result in the organic fouling. This is an important point as it differs the results of this
need for train flushing when removed from service. The water displaced testing from other CCRO pilots where scaling (silica or calcium phos­
during flushing could be used as make-up to the CCRO system, although phate) was responsible for flux loss and what limit sustainable recovery.
a means to capture, store, and transfer this water would be required. Deposition of silts and clays were not anticipated given the use of MF
pretreatment (0.1 μm nominal pore size), however the age of the MF
3.3.1. Chemical water quality assessment for Phase III membranes most likely allowed for passage of such particulates into the
There was a noticeable difference in CCRO permeate water quality AWPF RO feed and their concentration in the CCRO feed. In the second
between the start of a cycle and end of a cycle that was expected due to and third phases, the pilot was operated as a “fourth stage” RO treating
the recirculation of the concentrate through the CCRO process (see RO concentrate directly, where the salinity is near supersaturation. The
Figs. 3 and S8). The concentration of select water quality parameters and SC enables shorter filtration duration (filtration time as short as 1.5
inorganic constituents in CCRO permeate are shown in Fig. S12 and min), and thus a greater recovery range (low to high) is feasible. An
compared to the primary RO system (GWRS AWPF) permeate for operation flux of 6.4 gfd (11.0 LMH) and a MPV crossflow velocity ≥ 60
reference. The two permeates were comparable, notably considering the gpm (0.23 m3/min) were demonstrated to best minimize the accumu­
more challenging RO concentrate feed of the CCRO pilot. The CCRO lation of silts/clays and dissolved organics at the membrane surface and
permeate generally met permit limits for the OCWD AWPF finished minimize the decline in specific flux. Under these conditions, and sup­
water. The average CCRO permeate TOC was low at 0.17 ± 0.049 mg/L plying the side conduit of the pilot with AWPF RO feed water rather than
but slightly higher than the 6-month average GWRS AWPF RO permeate RO concentrate, the pilot demonstrated sustainable operation at a re­
TOC of 0.11 ± 0.03 mg/L. The CCRO permeate was still below the AWPF covery range of 57–61% (RCCRO) over a long-term run (up to 66% re­
finished water permit limit for TOC < 0.5 mg/L and in a theoretical full- covery in a short-term run). This corresponds to an overall theoretical
scale application, could be reduced significantly through blending with GWRS recovery of 90–92% at full-scale (i.e., assuming all primary sys­
the primary RO system permeate. The average TDS of the CCRO tem RO concentrate is treated by CCRO and the CCRO permeate blended
permeate was 50.5 ± 28.9 mg/L, higher than the 6-month average with primary RO permeate to increase production), while allowing for
AWPF RO permeate TDS of 17.0 ± 8.0 mg/L, but well below the AWPF CCRO operation with a CIP frequency to between 63 and 73 days, two
finished water permit requirement of <500 mg/L. All sulfate (SO42− ) times greater than the 30-day minimum CIP interval recommended by
concentrations were below the detection limit of 0.5 mg/L except for plant managers. These operations were accomplished without
one sample of CCRO permeate (0.7 mg/L) on 2/21/19, which was well increasing antiscalant or acid dosing to the AWPF RO feedwater for
below the permit requirement of 100 mg/L. The average CCRO control of fouling/scaling.
permeate chloride (Cl− ) concentration was 30.9 ± 35.7 mg/L that was In order to cope with fluctuating feed water quality, an adaptive
higher than the 6-month average AWPF RO permeate Cl− concentration control strategy was implemented as an alternative to operation at a
of 5.0 ± 0.98 mg/L. Finally, the nitrate in the CCRO permeate was low preset maximum recovery, in which the pilot operated in a variable
(9.1 ± 4.1 mg/L), though higher than AWPF RO permeate, but well recovery mode where the CCRO cycle trigger was controlled by the
below the GWRS-FPW permit requirement of 45 mg/L as NO3. maximum CCRO concentrate conductivity, maximum recovery setpoint
and the maximum feed pressure. Additional information regarding
4. Conclusions CCRO permeate water quality and estimated theoretical full-scale
implementation costs compared to FO-RO will be reported in a future
Two years of pilot testing demonstrated the sustainable use of CCRO follow-up publication.
for RO concentrate treatment. The testing focused on operational opti­ Water recovery from concentrate is becoming more feasible as the
mization and treatment of concentrate from the RO process of a full- cost of membrane treatment technologies has dropped and the value of
scale potable reuse facility, the OCWD GWRS AWPF, to recover addi­ water has increased. Piloting promising technologies using real facility
tional potable quality water to increase the overall system recovery source waters and operational preferences over longer timescales is
above current 85%. In the first phase of testing, a maximum pilot re­ critical to advancing technology adoption to improve water security.
covery of 92% was achieved from an MF effluent feedwater to the CCRO This comprehensive long-term pilot dataset collected over a two-year
process. Although considered the a priori limit to maximizing recovery, period has not been previously presented in the literature. With the
mineral scaling was not thought as the constraint but rather silt and current interest in increasing RO recoveries and minimizing discharge of

12
H. Gu et al. Desalination 518 (2021) 115300

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Declaration of competing interest 10.1016/j.desal.2020.114336.
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lationships which may be considered as potential competing interests: osmosis (SBRO) desalination, J. Membr. Sci. 588 (2019), https://doi.org/10.1016/
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[18] M. Uchymiak, A.R. Bartman, N. Daltrophe, M. Weissman, J. Gilron, P.
declare that they have no conflict of interest. Michael Boyd is a current D. Christofides, W.J. Kaiser, Y. Cohen, Brackish water reverse osmosis (BWRO)
employee of DuPont Water Solutions. operation in feed flow reversal mode using an ex situ scale observation detector
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