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Removal of trace organic chemical contaminants

by a membrane bioreactor

T. Trinh, B. van den Akker, R. M. Stuetz, H. M. Coleman, P. Le-Clech

and S. J. Khan

ABSTRACT

Emerging wastewater treatment processes such as membrane bioreactors (MBRs) have attracted a

significant amount of interest internationally due to their ability to produce high quality effluent

suitable for water recycling. It is therefore important that their efficiency in removing hazardous trace

organic contaminants be assessed. Accordingly, this study investigated the removal of trace organic

chemical contaminants through a full-scale, package MBR in New South Wales, Australia. This study

was unique in the context of MBR research because it characterised the removal of 48 trace organic

chemical contaminants, which included steroidal hormones, xenoestrogens, pesticides, caffeine,pharmaceuticals and personal care products (PPCPs). Results showed that the removal of most trace

organic chemical contaminants through the MBR was high (above 90%). However, amitriptyline,

carbamazepine, diazepam, diclofenac, fluoxetine, gemfibrozil, omeprazole, sulphamethoxazole and

trimethoprim were only partially removed through the MBR with the removal efficiencies of 2468%.

These are potential indicators for assessing MBR performance as these chemicals are usually

sensitive to changes in the treatment systems. The trace organic chemical contaminants detected in

the MBR permeate were 1 to 6 orders of magnitude lower than guideline values reported in the

Australian Guidelines for Water Recycling. The outcomes of this study enhanced our understanding

of the levels and removal of trace organic contaminants by MBRs.

T. Trinh

B. van den Akker

R. M. Stuetz

H. M. Coleman

S. J. Khan (corresponding author)

UNSW Water Research Centre,

School of Civil and Environmental Engineering,

University of New South Wales,

NSW, 2052,

Australia

E-mail: [email protected]

P. Le-Clech

UNESCO Centre for Membrane Science and

Technology,

School of Chemical Engineering,

University of New South Wales,

NSW, 2052,

Australia

Key words | decentralised treatment system, membrane bioreactor, pesticides, pharmaceuticals

and personal care products, steroidal hormones

INTRODUCTION

The presence of trace organic chemical contaminants such

as steroidal hormones, xenoestrogens, pesticides, pharma-

ceuticals and personal care products (PPCPs) in municipal

wastewater has been the subject of increasing concern

throughout recent decades (Jjemba ; Wright-Walters

& Volz ). Some of these trace organic chemical con-

taminants are known to have endocrine disrupting effects

on aquatic organisms at low concentrations and others

have been linked to ecological impacts due to acute and

chronic toxicity mechanisms (Purdom et al. ; Hotchkiss

et al. ). Investigating the removal of these trace organic

chemical contaminants through treatment processes and

assessing the risks associated with these chemicals to

public health and the surrounding environment are particu-

larly important for water reuse applications.

Recently, membrane bioreactors (MBRs) have attracted

a significant amount of interest internationally due to their

ability to produce high quality effluent over conventional

activated sludge systems (Coleman et al. ; Le-Minh

et al. ). MBRs comprise a combination of a conventional

activated sludge process with microfiltration/ultrafiltration

membrane separation, which enables these systems to pro-

duce effluents that could be recycled. In addition, this

combination has the advantage of a small footprint which

is favourable for small decentralised water reuse systems.

However, like centralised wastewater treatment systems,

there remains concern as to the fate and removal of trace

chemical contaminants by MBR treatment processes.

This research investigated the removal of a comprehen-

sive set of 48 trace organic chemical contaminants through a

1856 IWA Publishing 2012 Water Science & Technology | 66.9 | 2012

doi: 10.2166/wst.2012.374
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decentralised package-plant MBR treating municipal waste-

water in New South Wales, Australia. This research is

unique because it includes a wide range of studied trace

organic chemical contaminants covering steroidal hor-

mones, xenoestrogens, pesticides, caffeine and PPCPs.

MATERIALS AND METHODS

Description of the package MBR

Samples were collected from a decentralised full-scale MBR

plant (800 equivalent persons) located in Wolumla, Bega

Valley, New South Wales, Australia. A schematic diagram

of the MBR is presented in Figure 1, which summarises

the key components, flow direction and sample sites. The

treatment process comprises of a fine screen (3 mm), a bio-

reactor tank, two parallel-submerged membrane modules

and a medium pressure ultra-violet (UV) disinfection unit.

The sludge retention time (SRT) of the bioreactor was

1015 d, the hydraulic retention time (HRT) was 1 d and

the mixed liquor suspended solids (MLSS) concentration

was 7.58.5 g L1. The bioreactor tank was intermittently

aerated in 10 minute cycles (dissolved oxygen set-point of

1 mg L1) to achieve simultaneous nitrification and denitri-

fication. The submerged membrane modules were made of

hollow fibre membranes (Koch Puron), which have an effec-

tive pore size of 0.10.2 m and a surface area of 235 m2

(each). For cleaning, scour air was applied to the mem-branes using a positive displacement blower and

backwashing occurred every 360 seconds for a period of

60 seconds. Chemical backwashing occurred automatically

every three weeks, in accordance with the manufacturers

recommendations, to maintain a transmembrane pressure

of

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compounds including 31 PPCPs (amitriptyline, atenolol,

atorvastatin, carbamazepine, diazepam, DEET (N,N-Diethyl-

meta-toluamide), diclofenac, dilantin, enalapril, fluoxetine,

norfluoxetine,gemfibrozil, hydroxyzine,ibuprofen, ketoprofen,

meprobamate, metformin, naproxen, omeprazole, o-hydroxya-

torvastatin, p-hydroxyatorvastatin, paracetamol, primidone,simvastatin, simvastatin hydroxy acid, sulphamethoxazole,

triamterene, triclocarban, triclosan, trimethoprim, risperi-

done), two pesticides (atrazine, linuron), a xenoestrogen

(bisphenol A) and caffeine. For another xenoestrogen propyl-

paraben, no direct isotopically labeled analogue was able to

be found, therefore quantification for this compound was

based on external calibration only. 15N13C-paracetamol and

D5-diazepam werepurchased fromCambridgeIsotope Labora-

tories Inc., USA. D4-sulphamethoxazole, D6-trimethoprim,

D5-atorvastatin, D5-p-hydroxyatorvastatin, D5-o-hydroxyator-

vastatin, D4-risperidone, D5-enalapril, D6-simvastatin, D6-

simvastatin hydroxy acid, D3-triclosan, D5-triamterene, D3-

meprobamate and D8-hydroxyzine were purchased from Tor-

onto Research Chemicals Inc., Canada. D6-amitriptyline, D7-

atenolol, D5-atrazine, D7-bisphenol A, D9-caffeine, D10-carba-

mazepine, D4-DEET, D4-diclofenac, D10-dilatin, D6-

gemfibrozil, D5-fluoxetine, D5-norfluoxetine, D3-ibuprofen,

D3-ketoprofen, D6-linuron, D6-metformin, D3-naproxen, D3-

omeprazole, D5-primidone and D4-triclocarban were pur-

chased from Dr. Ehrenstorfer GmbH, Germany. Atorvastatin,

fluoxetine, norfluoxetine, o-hydroxyatorvastatin, p-hydroxya-

torvastatin, risperidone, simvastatin hydroxy acid were

purchased from Toronto Research Chemicals Inc., Canadaand other analytes were purchased from Sigma Aldrich. The

limit of quantification (LOQ) for all analytes is 1 ng L1.

Gas chromatography-tandem mass spectrometry

(GC/MS-MS) analysis

After analysis by LC-MS/MS, the same samples were pro-

cessed for GC-MS/MS analysis of steroidal hormones

using a previously published method (Trinh et al. b).

The studied steroidal hormones include seven estrogens

and five androgens. Direct isotopically labelled analogues

were used for eight hormones (17-estradiol, estrone,

17-ethynylestradiol, estriol, testosterone, etiocholanolone,

dihydrotestosterone, androstenedione) and satisfactory isotopestandards were applied for the remaining four hormones

(17-estradiol, mestranol, levonorgestrel and androsterone).

RESULTS AND DISCUSSION

Concentration of trace organic chemical contaminants

in raw sewage

Steroidal hormones

The concentrations of steroidal hormones in raw sewage

are presented in Figure 2. The natural estrogen, 17-estra-

diol and the main components of the contraceptive pills

(17-ethynylestradiol, mestranol and levonorgestrel) were

not detected. The estrogens that were detected included

the natural estrogen, 17-estradiol and its metabolised

products estrone and estriol. The results show that the

androgenic hormones were detected at higher concen-

trations than estrogenic hormones which may be due to

the higher excretion rates of androgens compared with

estrogens in humans (Leusch et al. ). Testosterone

and its metabolised products, androsterone, etiocholano-lone and dihydrotestosterone were all detected. In

general, the concentrations of steroidal hormones are

consistent with previous Australian studies; with the

exception of testosterone and dihydrotestosterone,

which were one to two orders of magnitude higher than

values reported in the literature (Coleman et al. ;

Le-Minh et al. ). This may be due to higher sensitivity

of the analytical method used here compared with

other studies (Coleman et al. , ; Le-Minh et al.

).

Xenoestrogens, pesticides, caffeine and PPCPs

The concentrations of xenoestrogens, pesticides, caffeine

and PPCPs that were detected in raw sewage are shown

in Figure 2. Of the 36 studied chemicals, 12 were not

detected in the raw sewage. These included 10 PPCPs (dila-

tin, enalapril, norfluoxetine, hydroxyzine, meprobamate,

primidone, simvastatin, simvastatin hydroxy acid, triamter-

ene, risperidone) and two pesticides (atrazine, linuron).

Table 1 | Quality of raw sewage and MBR permeate (mean values reported, n 6)

Quality parameters Raw sewage MBR permeate

DOC (mg L1) 147.1 14.9

NH3 (mg L1) 22.4 0.10

Total N (mg L1) 71.6 1.9

Total P (mg L1) Unavailablea 2.7

pH 7.0 7.7

aTotal P was not measured in raw sewage as the colourimetric method used onsite was

not suitable for such coloured samples.

1858 T. Trinh et al. | Removal of trace organic chemical contaminants by MBR Water Science & Technology | 66.9 | 2012
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Caffeine was found at concentrations of up to 40.5 g L

1

which was four times higher than values reported in raw

sewage in the literature (Kim et al. ). Pharmaceuticals

including ibuprofen, metformin, naproxen and paraceta-

mol were all detected in the raw sewage at

concentrations in the range of 18.359.5 g L1, which

was not surprising given that these pharmaceuticals are

used extensively in Australia (Khan & Ongerth ).

The concentrations of carbamazepine, diclofenac and sul-

phamethoxazole are consistent with published Australian

data while ketoprofen was found to be five times higher

(Al-Rifai et al. , Le-Minh et al. ). The remaining

pharmaceuticals (trimethoprim, fluoxetine, omeprazole,amitriptyline, gemfibrozil and diazepam) were found in

the raw sewage at concentrations of less than 100 ng L1.

High day-to-day variability in concentrations of some

chemicals, including gemfibrozil, omeprazole and sulpha-

methoxazole was observed. Such variability may be the

expected result for relatively low prescription rate drugs

in a very small wastewater catchment (800 equivalent

persons).

Removals of trace organic chemical contaminants bythe package MBR

Removal of steroidal hormones

The percentage removal of steroidal hormones through the

package MBR is presented in Figure 3. Results from this study

show that steroidal hormones were effectively removed by

the package MBR, with the removal efficiencies in the order

of 97100%. These results are consistent with previous studies

on MBRs (Kim et al. ; Spring et al. ; Lee et al. ;

Coleman et al. ; Le-Minh et al. ; Trinh et al. ).

The mechanisms responsible for removing these steroidal hor-mones in MBR plants typically include particulate adsorption

and biodegradation (Ternes et al. ; Servos et al. ;

Leusch et al. ; Abegglen et al. ; Coleman et al. ).

Removal of xenoestrogens, pesticides, caffeine and PPCPs

The removal of xenoestrogens, pesticides, caffeine and

PPCPs through the package MBR is presented in Figure 3.

Figure 2 | Concentrations of trace organic contaminants in raw sewage.

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Most of these chemicals were effectively removed by thepackage MBR. Removal efficiencies of bisphenol A, propyl-

paraben, atenolol, atorvastatin, DEET, ibuprofen,

ketoprofen, metformin, naproxen, o-hydroxyatorvastatin,

p-hydroxyatorvastatin, paracetamol, triclosan and caffeine

were between 90 and 100%. Previous studies on MBRs

reported similar removal efficiencies for bisphenol A, ibu-

profen, triclosan and caffeine (Clara et al. ; Kim et al.

; Radjenovic et al. ; Coleman et al. ; Radjeno-

vic et al. ). These trace chemical contaminants are

typically removed by MBRs via biodegradation and sorption

to biomass (Cirja et al. ). Studies have shown that ateno-

lol, ibuprofen, naproxen, paracetamol and caffeine arereadily biodegradable (Abegglen et al. ; Radjenovic

et al. ) while triclosan can absorb to biomass (Coleman

et al. ). For bisphenol A, both sorption to biomass and

biodegradation are significant (Hu et al. ). The high

removal efficiencies noted here can be attributed to the

high SRT and MLSS concentration in the MBR (Clara

et al. ; Chen et al. ; Coleman et al. ). Amitripty-

line, gemfibrozil, omeprazole and sulphamethoxazole were

moderately removed by the MBR with removal effi

cienciesbetween 59 and 68%. Conversely, carbamazepine, diaze-

pam, diclofenac, fluoxetine and trimethoprim were not

effectively removed through the MBR with removal

efficiencies of 2447%. Carbamazepine, diclofenac and tri-

methoprim have been identified as persistent compounds

that are difficult to be removed through MBRs with various

removal efficiencies in the literature ranging from 0 to 50%.

This is because they are not easily biodegradable and adsorb

poorly to biomass (Clara et al. ; de Wever et al. ;

Kim et al. ; Radjenovic et al. ; Radjenovic et al.

). The trace organic chemical contaminants that are

partially removed through MBRs in normal operating con-ditions are potential indicators for assessing MBR

performance as these chemicals are usually sensitive to

changes in MBR treatment process performance (Drewes

et al. ).

Despite the high removal efficiencies for most of the

chemicals, estrone, caffeine and some PPCPs were

detected in the MBR permeate as shown in Figure 4.

The concentration of metformin in the MBR

Figure 3 | Removal of trace organic contaminants through the package MBR.

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permeate was up to 3.3 g L1. Atenolol, carbamazepine,

diclofenac, ibuprofen, ketoprofen, sulphamethoxazole,

triclocarban and trimethoprim were detected in the

permeate at concentrations of 66230 ng L1. Atorvasta-

tin, caffeine, DEET, omeprazole, o-hydroxyatorvastation,

p-hydroxyatorvastation, paracetamol and triclosan were

all detected in the MBR permeate at concentrations in

the range of 6.221.6 ng L1. Estrone was the only ster-

oidal hormone detected in the MBR permeate with a

concentration of 1.5 ng L1. These results were 16

orders of magnitude lower than Australian guideline

values for water recycling (Australian Guidelines for

Water Recycling ).

CONCLUSIONS

The results of this study showed that the removal of most of

the studied trace chemical contaminants through the pack-

age MBR was high (above 90%). However, amitriptyline,

carbamazepine, diazepam, diclofenac, fluoxetine, gemfibro-

zil, omeprazole, sulphamethoxazole and trimethoprim

were only partially removed through the MBR with removal

efficiencies of 2468%. These compounds are potential indi-

cators for assessing the MBR performance as these

chemicals are usually sensitive to changes in MBR treatment

process performance. The trace organic chemical contami-

nants detected in the MBR permeate were 16 orders of

magnitude lower than guideline values in the Australian

Guidelines for Water Recycling. These results enhance our

understanding of the levels and removal of a comprehensive

list of 48 trace chemical contaminants of concern through

MBR systems.

ACKNOWLEDGEMENTS

This work was supported by the Australian Research Coun-

cil Linkage Projects LP0989365 (with industry support from

MidCoast Water, Bega Valley Council, Hunter Water and

NSW Health). Trang Trinh was also supported by Water

Quality Research Australia. The authors thank Ken

McLeod, Chris Scharf and Tony Brown from Bega Valley

Council for their support during the sampling period. We

Figure 4 | Concentration of trace organic contaminants in MBR permeate.

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also thank Dr James McDonald for his technical support

with the undertaking of this work.

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disrupting chemicals and microbial indicators by a

decentralised membrane bioreactor for water reuse. Journal

of Water Reuse and Desalination 2 (2), 6773.

Trinh, T., van den Akker, B., Coleman, H. M., Stuetz, R. M.,

Le-Clech, P. & Khan, S. J. a Fate of

pharmaceuticals during wastewater treatment by

a membrane bioreactor. Gwf-Wasser/Abwasser 152

(S1/2011), 98102.

Trinh, T., Harden, N. B., Coleman, H. M. & Khan, S. J. b

Simultaneous determination of estrogenic and androgenic

hormones in water by isotope dilution gas chromatography-

tandem mass spectrometry. Journal of Chromatography A

1218 (12), 16681676.

Vanderford, B. J. & Snyder, S. A. Analysis of

pharmaceuticals in water by isotope dilution liquid

chromatography/tandem mass spectrometry. Environmental

Science and Technology 40 (23), 73127320.

Wright-Walters, M. & Volz, C. Municipal wastewater

concentrations of pharmaceutical and xeno-estrogens:

wildlife and human health implications. In: Proceedings of

the National Conference on Environmental Science and

Technology, Greensboro, North Carolina, USA, pp. 103113.

First received 27 February 2012; accepted in revised form 16 May 2012

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