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Journal of Membrane Science 194 (2001) 185196

Beer clarification by microfiltration product quality control and


fractionation of particles and macromolecules
Q. Gan a, , J.A. Howell b , R.W. Field b , R. England b , M.R. Bird b ,
C.L. OShaughnessy c , M.T. MeKechinie c
a

Department of Chemical Engineering, The Queens University of Belfast, Stranmillis Road, Belfast BT9 5AG, UK
b School of Chemical Engineering, University of Bath, Claverton Down, Bath BA2 7AY, UK
c Brewing Research International, Lyttel Hall, Nutfield, Redhill, Surrey RH1 4HY, UK
Received 15 May 2000; received in revised form 21 May 2001; accepted 29 May 2001

Abstract
Beer clarification by microfiltration demands a finely balanced retention of colloidal particulates (yeast cells, chill haze
flocs, etc.) and transmission of soluble macromolecules including carbohydrates, proteins, flavour, and colour compounds
which give the whole some quality of a beer. The required porous transmission of these macromolecular species led to
an unavoidable, complex and dynamic in-pore membrane fouling in terms of fouling constituents, formation, structure and
kinetics, which are the main obstacles in obtaining an economically viable flux and consistency in permeate quality.
This experimental study was carried out with the aims of understanding the dynamic inter-relation between flux, fouling and
system selectivity during a cross-flow beer microfiltration process so that an effective operating strategy for flux optimisation
could be formulated in conjunction with the parallel objective of good product (permeate) quality control. Tubular ceramic
membranes (Ceramem) with nominal pore diameters of 0.2, 0.5, and 1.3 m were used. Simultaneous measurement of flux
and permeate qualities, such as specific gravity and chill haze level enabled identification of the effect of anti-fouling techniques, such as backflushing on transmission of essential beer components and on the filtered beer quality. The experimental
evidence lead to an understanding that the drastic flux enhancement achieved by employing backflushing at reversed membrane morphology was associated with enhanced solute transmission which could, without careful control, upset a balanced
transmission of essential beer components and the retention of unwanted chill haze components. Further operating parameters and varying system configurations were investigated over their effect on both flux performance and system selectivity.
These include membrane pore size, filtration temperature, and the addition of an amorphous silica particles as coagulation
agent for hydrophilic proteins. 2001 Elsevier Science B.V. All rights reserved.
Keywords: Beer microfiltration; Particle fractionation; Macromolecular transmission; Backflushing; Reversed membrane morphology

1. Introduction
Cross-flow microfiltration (CF-MF) is attracting
increasing technical and commercial interest as an

Corresponding author. Tel.: +44-1232-274-253;


fax: +44-1232-381-1753.
E-mail address: q.gan@qub.ac.uk (Q. Gan).

alternative method for fluid clarification/pasteurisation/


sterilisation in the beverage, brewing, and dairy industries [1]. The dairy industry uses CF-MF for milk
pasteurisation and ultrafiltration (UF) for separating
lipoproteins and whey protein fractions [24]. Wine
and vinegar producers have developed CF-MF for
simultaneous clarification and sterilisation with major
breakthrough [5,6]. The cider and fruit juice industry

0376-7388/01/$ see front matter 2001 Elsevier Science B.V. All rights reserved.
PII: S 0 3 7 6 - 7 3 8 8 ( 0 1 ) 0 0 5 1 5 - 4

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Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

use MF for microbiological stability, clarification and


spent fluid recovery with improved product quality
[710]. Unfortunately low flux and unsatisfactory
separation properties with undesirable product characteristics has retarded application to brewing [11,12].
Beer clarification serves the objective of obtaining
beer stability which can be divided into three broad
aspects: microbiological, colloidal, and flavour stability. Microbiological stability is achieved through
the removal of active yeast cells. Colloidal stability is
achieved through the removal of other large particles,
especially flocs formed by the coagulation of polyphenolic and proteinaceous compounds which appear as
chill haze in the clarified beer at low temperature.
Flavour stability is achieved through retaining flavour
compounds and by minimising dissolved oxygen in
the clarified beer.
Conventional beer clarification process employs filter press or pressure vessel filters which are commonly
pre-coated with porous particles of diatomaceous
earth (DE) as the filter aids, which play an important
role not only in acting as a second filtration barrier, but
also in absorbing the chill haze components. Recent
research works on replacing the conventional process
with CF-MF have suggested that the new technology
holds a number of advantages, including the elimination of using filter aids and associated handling
and disposal problems [13,14], reduced beer losses
[15], high solids handling capacity, and the substitution of heat pasteurisation and, therefore, a better
product quality and cost saving [16,17]. However,
there still exist considerable technical and economical
barriers have restrained large scale operation. These
include severe membrane fouling, inconsistent product quality, uncertainty over productivity, and large
flux/quality variations among different beer brands
filtered on one membrane system [18,19].
In theory, beer stability can be achieved in a single
microfiltration process by retaining unwanted materials and transmitting essential beer components. Microbiological stability is readily achievable because yeast
cells with a size range of 510 m can be readily rejected by MF membranes with pore diameters
in the range of 0.21.3 m. Colloidal stability is a
difficult task since the membrane selectivity based
on size-exclusion is unable to discriminate against
hydrophobic proteins, which give the essential foam
properties, and hydrophilic proteins which give rise

to unwanted chill haze. The size range of these two


groups of protein molecules overlaps with molecules
in the hydrophobic group only slightly bigger than
those in the hydrophilic group [20]. With the variation of membrane pore size, system configuration and
operating conditions, there is always a risk of over
transmission of haze proteins or under transmission of
foam proteins, resulting in impaired product (permeate) quality. This delicate trade-off can be further
complicated by a dynamic and continuous membrane
fouling process which may alter selectivity and other
performance characteristics of a carefully pre-selected
membrane system.
Flux is largely an economical issue. The economical flux rates are reported to range between 10
and 100 kg h1 m2 usually based upon recirculation
experiments [11,21]. The assumptions of these economical calculations are rather roughly defined. In
this work, an average flux rate of 40 kg h1 m2 over
24 h continuous filtration is considered as being of
commercial interest.
Whilst the mechanisms of fouling and flux decline
in beer microfiltration are now better understood
and documented [12,22,23], there has been little
reported on a systematic analysis of the dynamic
and inter-dependent relationships between separation
characteristics, permeate quality, flux and membrane
fouling. There is especially a lack of understanding
of how flux and permeate quality are affected by the
mechanism of transport of macromolecule through
the micropore phase of a membrane. The rate of the
transport determines the permeation rate and permeate
quality, and depends primarily on the particle/pore size
ratio and complex particlepore interactions. A systematic understanding of these dynamic inter-relations
and finding an optimal fluxpermeate quality relationships should lead to important process improvements.
A previous study of beer microfiltration has been
conducted through a Link project involving BRF
International, Courage Brewing plc (now Scottish
Courage) and the University of Bath. We have already
reported the effects of membrane fouling [23], flux
enhancement techniques [24] and membrane cleaning
[25]. This paper reports on the analysis and optimisation of the relationship between flux and permeate
quality performance. It highlights specifically the
synergetic relationship existing between the nature of
membrane fouling and the permeate quality variations

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

under different system configurations and operating


regimes, especially with high frequency backflushing and reversed membrane morphology with which
dramatic flux improvement has been achieved. Most
importantly a high product quality has been achieved.

2. Experimental methods and materials


A schematic flow diagram is shown in Fig. 1. In
addition to the provision for conventional cross-flow,
special features of the experimental rig include (i)
techniques for enhancing surface hydrodynamics and
producing secondary flow through two-way reversing
flow pulsation; (ii) creation of helical flow patterns
through insertion of helical baffles within the flow
channel; and (iii) an automated multi-stage backflush
(BF) facility which generates backpulses of controllable frequency and strength.
Ceramic membranes (Ceramem Corporation,
Waltham, USA) with nominal pore diameters of 0.2,
0.5, 1.3 m and 12 4 mm 4 mm square-shaped flow
channels inside a ceramic monolith were used in this
work. Modules were 500 mm long and 50 mm diameter with an internal total surface of 0.096 m2 and

187

an external surface of 0.0785 m2 . In all experiments,


0.5 m pore diameter was selected except in the
experiment where the effect of pore sizes was investigated. Baffles were made of 0.1 mm stainless
steel wire helically wound and soldered to a core
wire of 0.25 mm diameter at a pitch of 21 mm. When
the baffles were inserted in the monolith, the central
core wires were individually tensioned and fixed at
both ends of the channel to control vibration. Fully
reversing pulsatile flow was provided by a modified air
driven double diaphragm pump (Wilden M1, Cheshire,
UK). This could be superimposed on the feed flow.
Fresh cold-conditioned rough beer, Beer A, was
supplied daily by Courage Brewing plc at its on-site
development brewery where this study was carried
out. It is a slightly different beer as that used in a previous study [23] as it was brewed in a small scale fermenter (10 m3 ) with a shorter cold conditioning time
in a smaller storage tank (10 m3 ). The beer has a typical suspended solids loading of 0.190.23 g l1 (dry
weight) and total dry solids content of 3.533.67 wt.%.
Mean yeast cell diameter measured by laser Mastersizer (Malvern Instrument, Malvern, UK) is
6.40.2 m. The feed was stored and filtered at 2.0
0.9 C except in the experiment where the effect of

Fig. 1. Schematic flow diagram.

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Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

Table 1
Measured beer qualities of the cold-conditioned rough beer (feed)
and the conventionally filtered beer according to the EBC standards

HRV (s)
Chill haze (EBC)
Present gravity (S)
Colour (EBC)
Bitterness (BU)
pH

EBC standards

Feed

Product of
DE filtration

>100
<0.80
12
12
16
4.1

128
9.5
12.5
14.8
17.2
4.1

112
0.54
12.2
12.3
16.1
4.1

temperature was tested. Measurement of beer quality


was conducted according to the protocols from European Brewery Convention (EBC) [20]. This included
the measurement of head retention value (HRV), chill
haze, present gravity, colour, bitterness, alcohol, and
pH. The measured qualities of the cold-conditioned
rough beer are listed in Table 1 along with the EBC
standards. For comparison, qualities of the clarified
beer filtered through the conventional filtration using
DE as the filter aids (DE filtration) are also listed in
Table 1. The HRV is an indicator of the concentration
of hydrophobic proteins/peptides giving the desirable foam properties. The chill haze level indicates
the concentration of hydrophilic proteins which are
precursors to form the polyphenolicproteinaceous
complexes presenting themselves as visible loosely
bound flocs (haze) in the beer at low temperature and
over long storage time.
2.1. Backflush programme
The principle aim in designing a good backflush
regime is to minimise the permeate usage as backflush
media whilst achieving the maximum pore clearance
within the shortest possible time. In this work, backflush was governed by a programmed multi-stage
backpulse routine with time varying frequency and
pulse strength. The variables are many and include
the CO2 pressure, the duration of the pulse, duration
between end of the pulse and opening the permeate
valve and cycle frequency. These variables influence
the membrane cleaning efficiency of the backpulse,
dead-time and the loss of permeate. The lost permeate is permeate recycled from the product to the
feed-side and so this portion does not contribute to
the net flux.

Loss of permeate and time during backflush may


take upto an equivalent 25% of total filtration time
[13,26], offsetting in some cases the advantageous
flux gain. The backflush regime we have developed
is fully automated and computer controlled. To save
the permeate loss, gas (CO2 ) was used as a complimentary backflushing media. The combined use of
permeate and gas had similar pore clearance effect
and reduced the permeate loss by 40%. The overall
backflush frequency in this work varied from 0.016
to 0.133 Hz. Details of the backflush methodology
and programme are reported in a previous study
[23].
2.2. Filtration with reversed membrane morphology
Experiments on reversed membrane pore morphology were carried out by changing the port configuration to feed the process fluid to the substructure
side of the membrane and taking out permeate from
the former retentate ports. The trans-membrane pressure gradient was, thus, applied in a reversed fashion.
The mechanical structure of the ceramic membrane
is strong and able to withstand 1.5 bar back pressure
pulse without any problem.
2.3. Membrane cleaning
An effective and fast membrane cleaning formula
was developed [25] by following a combined simultaneous caustic cleaning and oxidation procedure
carried out at 80 C using 0.3% w/w NaOH solution
with the addition of 5 g l1 H2 O2 as the oxidising
agent. This cleaning formula can rapidly break down
tenacious surface deposit and attack residual fouling
forming by strong surface adsorption. Whilst this
cleaning method is very powerful, it did not affect the
integrity of the ceramic membrane which was periodically cleaned after each beer filtration operation.

3. Results and discussion


3.1. Flux, fouling, and product quality at
conventional cross-flow filtration
Fouling was severe and complex in conventional
cross-flow filtration of the cold-conditioned beer,

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196


Table 2
The 24 h average fluxes at steady cross-flow filtration conditionsa
TMP (bar)

24 h average flux (kg h1 m2 )

0.4
0.8
1.2

3.8
4.9
4.6
a

Re = 1552, T = 2.0 0.9 C.

causing rapid flux reduction (>95%) in the first hour


of filtration. Steady flux, defined as the flux value at
which further flux reduction due to fouling is less
than 2% per hour, was less than 5 kg h1 m2 under
conventional cross-flow filtration conditions. It took
more than 5 h to reach the steady-state. It is also
noted that the performance of the cold-conditioned
beer used in this study behaved very differently to
the beers used in some other studies [11,22,26] as the
rough beer was undiluted and has a higher specific
gravity and total solids concentration.
Extended 24 h filtration operations were carried out
to assess the long run flux performance. The average
fluxes under three different trans-membrane pressures
are shown in Table 2.
Enzymatic analysis in a stirred cell apparatus had
been carried out to identify specific classes of membrane foulants [23]. Carbohydrates were important,
in particular pentosans, glucans and hydrophilic haze
proteins. Trace minerals (Ca2+ , Cu2+ ) also played an
important bridging role in the surface complexion of
the key membrane foulants.
The formation of the fouling structure can be
subdivided into three major types: (i) the cake
layer consisting of a compact deposit of yeast cells,

189

debris, and coagulated materials, e.g. chill haze;


(ii) discrete particles blocking the pore entrances and
plugging pore pathways; (iii) soluble macromolecules
adsorbed to the membrane surface and inner pore
walls.
The in-pore membrane fouling has been identified
as the most predominant flux reduction factor. The
presence of chill haze may also played an important role in flux reduction, and more importantly,
in changing the membrane systems selectivity as
the formation of a tenacious and compressible layer
of chill haze materials on the membrane surface
may have acted as a secondary barrier. The formation of chill haze is a temperature-dependent and
reversible process. The large colloidal aggregates may
re-dissolve into the beer when temperature rises above
4 C.
The continuous in-pore fouling caused a gradual reduction of the effective pore size leading to
further flux decline and change of selectivity. The
transmission of essential beer components was hindered which adversely affected the permeate quality.
Colour, HRV and present gravity gradually declined
to a level below the required EBC quality standard
(Table 3). On the other hand, the decreased transmission of protein molecules also reduced the level
of chill haze. Transmission of bitterness, alcohol,
and pH were little affected during the filtration as
these beer qualities are constituted by very small
molecules.
The time dependence of the permeate qualities
during the microfiltration compares unfavourably
with the traditional DE filtration process which has
only very small filtrate quality fluctuation.

Table 3
Measured permeate beer qualities against filtration time at steady cross-flow filtration conditionsa
Filtration time (h)

Colour (EBC)

Present gravity (S)

0.05
0.3
2.5
10.0
17.0
24.0

14.8
11.9
12
10.9
10.1
9.5

12.5
12.0
11.8
9.9
9.2
8.6

Average

10.4 0.4

EBC standard

11.5

9.8 0.3
12.0

Re = 1552, TMP = 0.8 bar, T = 2.0 0.9 C.

HRV (s)
128
112
111
97
84
63
74 2
>100

Haze (EBC)
9.53
0.49
0.49
0.48
0.44
0.39
0.46 0.02
<0.8

Bitterness (BU)
17.4
16.7
16.6
16.8
16.2
16.1
16.8 0.4
16.1

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Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

3.2. Effect of flow hydrodynamics on


flux and permeate quality
Flux improvement through employing hydrodynamic techniques, such as superimposed flow pulsation and a helical flow has been effective in a number
of microfiltration applications for solids concentration and separation where particle fractionation and
transmission of macromolecular species through the
pore phase are not demanding [2729].
However, the hydrodynamic techniques had only
limited flux improving effect in the beer microfiltration in which pore phase transport of large amount of
macromolecules is required. By creating a two-way
reversing flow oscillation, the presence of a highly enhanced flow turbulence and unsteady flow conditions
failed to produce a meaningful flux improvement
(Table 4). It suggests that the increase in bulk flow
turbulence did not produce a sufficient shear stress
close to the membrane surface which is critical in
removing particle deposit.
Further attempts to improve flux by modifying
surface hydrodynamic conditions were made through
creating a helical flow pattern accompanied by a superimposed secondary flow. This was done by installing
helically wound baffle inserts inside the tubular flow
channel. The combined effect of the two-way reversing
flow pulsation and baffle inserts was also investigated.
The 24 h average flux improved by 48% by using the
baffle inserts at steady cross-flow. By using the baffle
inserts under two-way reversing pulsatile flow conditions with a peak Reynolds number Rep = 4950, a
maximum 57% flux improvement was obtained.

Permeate quality had very minor change as a result


of changing flow hydrodynamics. Quality analysis
of permeate collected over 24 h filtration is given
in Table 5. This indicates that in-pore fouling was
dominant and insensitive to the conditions of surface hydrodynamics. It also suggests that bulk fluid
hydrodynamic conditions had little influence on the
transmission of macromolecular species through the
membrane pores. The pore flow of a permeate stream
containing large solutes may have to overcome a
much greater frictional force than flow of pure liquid
as the steric drag and electrostatic force on the solutes
can be highly significant. The transport mechanism of
solutes through cylindrical pores has been reviewed
by Deen [30]. More recently, the coupled liquid/solute
flow through micropores was extensively studied by
Bowen and co-workers [3133] which shows that the
critical velocity of the solute and the overall permeation rate depends heavily on electrostatic interaction
as well as steric frictional forces.
3.3. Effect of backflush
The improved flux after adopting the hydrodynamic techniques is still too low to be considered
of commercial significance. Backflush has shown to
be a more effective way in unravelling the fouling
structure of steric pore entrance blocking and pathway
plugging since the formation of this type of fouling is largely reversible [34,35]. It is also noted that
backflushing was not so effective in reducing fouling caused by surface adsorption of macromolecular
species.

Table 4
Steady-state flux at different feed flow hydrodynamic conditionsa
Filtration time (h)

5
10
15
20

Steady-state flux (kg h1 m2 )


CF, Re = 1552

CF + PUL, Re = 1552,
Rep = 3400

CF + BFL, Re = 1552,
Rep = 4950

CF + PUL + BFL,
Re = 1552, Rep = 4950

7.6
5.8
4.6
4.3

7.7
5.7
4.8
4.6

10.7
8.1
7.3
6.9

11.1
8.8
7.6
7.3

a CF: conventional cross-flow filtration; CF + PUL: cross-flow filtration with two-way reversing flow pulsation; CF + BFL: cross-flow
filtration with superimposed helical flow pattern; CF + PUL + BFL: cross-flow filtration with combined flow pulsation and a superimposed
helical flow pattern; Re: bulk fluid Reynolds number; Rep : peak fluid Reynolds number under flow pulsation and at helical flow pattern;
TMP = 0.8 bar, T = 2.0 0.9 C.

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196


Table 5
Quality analysis for permeate collected over 24 h filtration at different flow hydrodynamic conditionsa
Quality parameters

Operational mode
CF + BF

CF
Colour (EBC)
Present gravity (S)
HRV (s)
Haze (EBC)
Bitterness (BU)
a

10.4
9.8
74
0.46
16.8

0.3
0.2
1
0.03
4

10.5
10.0
78
0.49
16.7

0.4
0.2
3
0.04
0.4

CF + PUL
+ BF
10.5
10.1
81
0.47
17.1

0.5
0.2
3
0.04
0.4

TMP = 0.8 bar, T = 2.0 0.9 C.

Our backflush programme was optimised in terms


of backpulse frequency, back pressure, and the duration of each pulse. By applying the multi-stage,
high frequency backflush programme using CO2 as
the complimentary flush media, the 24 h average flux
was increased to 21.6 kg h1 m2 , a 442% increase
compared to normal cross-flow filtration [23].
Analysis of the permeate quality showed that the
large flux increase was accompanied by a higher transmission of total soluble beer components reflected
by increased specific gravity, HRV, chill haze and
colour of the permeate (Table 6). This synergetic relationship between flux improvement and increased
transmission of macromolecules suggests that the
pore clearing effect of backflush is beneficiary to
both flux and solutes transmission. The results also
show that whilst the permeate quality was improved
on the measures of increased HRV value, gravity, and
colour, it also had the side effect of a large increase in
chill haze level. This again demonstrates the inability
of the size-exclusion mechanism in discriminating
haze-forming hydrophilic proteins and foam-forming
hydrophobic proteins.
In general, it has been shown that backflushing was
a more effective flux and quality improving technique
than enhanced surface hydrodynamics.

191

3.4. Effect of temperature


Fermented beer has a high concentration of suspended solids which may quickly saturate the filter
medium in the conventional dead-end DE filtration.
A pre-filtration cold conditioning process is necessary to reduce the suspended solids concentration
by storing the beer at a temperature below 4 C to
allow the coagulation and subsequent sedimentation
of cells, flocs of chill haze and other large particles.
The cold conditioning process requires large storage
vessels placed in a temperature controlled space and
normally takes place for more than 72 h.
Unlike the traditional filtration operating in a
dead-end mode, CF-MF is capable of handling a high
loading of suspended solids. There is a growing interests in eliminating the cold conditioning process by
direct cross-flow filtration of fermented rough beer.
Provided the small compromise in flavour is acceptable, great cost saving could be achieved by taking
out the entire cold conditioning process. This has
been considered feasible with certain types of light
lager beer.
Since the formation of flocs of chill haze is temperature-dependent, beer filtration normally operates at
a low temperature similar to that of the cold conditioning process so that chill haze can be filtered out as
large aggregate particles. The temperature effect was
studied in this work by filtering the cold-conditioned
beer at two different temperatures of 2 and 10 C.
Backflush was also applied. The data of steady-state
flux are given in Table 7, and the time profile of the two
quality parameters in Fig. 2. The 24 h average flux improved by 34 and 41%, respectively, at the two different operational mode when the filtration temperature
increased from 2 to 10 C. The permeate HRV value
benefited from the increase in filtration temperature,
but still gradually declined to a level below the EBC
standards because of continuous fouling. The effect of

Table 6
Quality analysis for permeate collected over 24 h filtration with backflushinga
Quality parameters

Present gravity (S)

Colour (EBC)

Chill haze (EBC)

HRV (s)

24 h average value
Percentage increase over conventional
cross-flow filtration without backflushing

10.2 0.3
+4.3

10.8 0.4
+3.8

0.53 0.04
+15.1

83 2
+12.0

Re = 1552, TMP = 0.8 bar, T = 2.0 0.9 C.

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Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

Table 7
Steady-state flux at different temperature with or without backflusha
Temperature ( C)

2.0

Operational mode
(kg h1

m2 )

Flux at 10th hour


Flux at 20th hour (kg h1 m2 )
24 h average flux (kg h1 m2 )
a

10.0

CF

CF + BF

CF

CF + BF

5.8
4.3
4.9

27.2
17.5
21.6

7.7
5.9
6.6

37.4
26.7
30.5

Re = 1552, TMP = 0.8 bar.

3.5. Filtration at reversed membrane


morphology

Fig. 2. Effect of temperature on the transmission of HRV and chill


haze; Re = 1552, TMP = 0.8 bar.

temperature on chill haze is more pronounced leaving


a chill haze value above the EBC standard at the end
of the 24 h operation.
The chill haze at 0 C is fairly constant which is in
contrast to its time dependence at 10 C, suggesting
a consistent cut-off of a proportion of hydrophilic
proteinaceouspolyphenolic species existing in a
physical form of large aggregates at a temperature below 4 C. The colloidal particles may have re-dissolved
at higher temperatures with a consequence of a higher
transmission of the haze components in the form of
individual molecules.

Flux increase was dramatic and more sustainable


when the membrane was mounted in a reversed configuration (RV mode) to feed the process fluid to the
open substructure of the membrane and withdraw the
permeate from the former feed side. In the combined
cross-flow + backflush + reversed pore morphology
(CF + BF + RV) operational mode, 24 h average flux
was in excess of 42.7 kg h1 m2 which is considered
economically significant. The flux increase and fouling mechanism at reversed membrane morphology is
to be reported in a separate paper [24].
Analysis of permeate quality revealed that the flux
increase was accompanied by a corresponding large
increase of HRV and chill haze level in the permeate (Table 8). The 24 h average chill haze value at
the RV mode almost doubled that at normal membrane installation, and just exceeded the stipulated
EBC standard (<0.8 EBC). The simultaneous increase
in flux and transmission of macromolecular species
suggests that the improved transport of large solutes
through the reversed membrane structure is the main
cause of the large flux increase. The dirt holding
and realising mechanism at reversed membrane morphology [24] is an effective mechanism in preventing
large particles to reach and block the membrane pores.
Flux is also more responsive to backflushing at the
RV set-up.

Table 8
Permeate quality analysis (24 h average) at reversed membrane installation with backflushinga
Present gravity (S)

Colour (EBC)

HRV (s)

Chill haze (EBC)

Bitterness (BU)

pH

11.31 0.4

12.9 0.4

116 2

0.86 0.02

17.0 0.5

4.1 0.01

Re = 1552, TMP = 0.8 bar, T = 2.0 0.9 C.

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

193

3.6. Effect of membrane pore size


Membrane properties including surface charge,
pore size and pore structure strongly influence flux,
fouling and separation characteristics in most microfiltration processes. However, it is not well established
how these properties influence the rate at which fine
colloids and single macromolecular species are transported through the micropores. In the case of beer
microfiltration, it is difficult to predict the fractionation and transport of particles/macromolecules based
solely on the relative particle/pore size ratio since
a pre-selected size ratio may immediately start to
change with the onset of fouling, and continue to
change because of the reduction of effective convective pore diameter caused by dynamic and continuous
fouling. Most reported data so far on the effect of
membrane pore size in beer microfiltration are system
specific and lack in consistency across the spectrum
of different membranes, mode of operation and beer
brands [16,19,21].
Nonetheless, membrane pore size is still recognised
as the single most important membrane parameter in
designing and selecting a MF membrane system. The
effects of pore size were investigated in our experiments using three different pore diameters of 0.2, 0.5,
1.3 m. Fig. 3 shows that at conventional cross-flow
conditions, 24 h average flux decreased with increasing pore diameter. Flux at 1.3 m pore diameter was
26% lower than that obtained at 0.2 m pore diam-

Fig. 3. Effect of pore diameter on 24 h average fluxes; Re = 1552,


TMP = 0.8 bar, T = 2.0 0.9 C.

Fig. 4. Effect of pore diameter on transmission of HRV; Re = 1552,


TMP = 0.8 bar, T = 2.0 0.9 C.

eter. This is contrary to expectation and the cause is


attributed to a greater degree of pore entrance blockage and entrapping of large particles at 1.3 m pore
diameter. Flux reduction by these mechanisms was
reversible as Fig. 3 also shows that flux responded
more favourably to the anti-fouling techniques (backflush and reversed pore morphology) at the larger
pore sizes.
Analysis also showed that transmission of both
hydrophilic and hydrophobic proteins increased with
increasing pore diameter, especially under the combined CF + BF + RV operating mode, resulting in
higher permeate HRV and chill haze level at larger
pore diameters (Figs. 4 and 5). Chill haze at 1.3 m
pore diameter exceeded the EBC standard, a potential

Fig. 5. Effect of pore diameter on transmission of chill haze;


Re = 1552, TMP = 0.8 bar, T = 2.0 0.9 C.

194

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

Fig. 6. Effect of the addition of silica gel on flux and transmission of chill haze; Re = 1552, TMP = 0.8 bar, T = 2.0 0.9 C.

problem of colloidal instability. On the other hand,


the 0.2 m pore diameter seems too small to allow
the passage of sufficient proteinaceous components
to give an acceptable HRV value.
3.7. Effect of silica gel as a processing aid
Amorphous silica particles are sometimes used as a
processing aid for beer stabilisation in circumstances
where the beer bas a high content of proteinaceous
and polyphenolic compounds. The silica particulates
used in this work have equivalent spherical diameters ranging from 5 to 15 m. The stabilising effect
stems from the silicas ability in selective adsorption
of hydrophilic haze forming proteins. This mechanism
involves hydrogen bonding between protein carbonyl
groups and silanol hydroxyl groups.
The effect of using silica in beer microfiltration was
investigated by mixing amorphous silica particles to
a concentration of 500 ppm in cold-conditioned beer
which was left at 2 C for 12 h for the adsorption and
sedimentation (of the silica particles) to take place.
The treated beer, with much reduced concentration
of hydrophilic proteins, was then filtered using the
0.5 m membrane at different operating modes. Flux
showed a general increase at all operating conditions
(Fig. 6) and chill haze level was substantially reduced.
Even with the combined CF + RV + BF operational
mode which normally promotes high solutes trans-

mission, a 0.53 EBC chill haze value was recorded


which is significantly below the stipulated EBC limit.
Whilst there was a great reduction in the chill haze
level, HRV values at all three operating modes only
marginally decreased in comparison to the values obtained at the same operational conditions without use
of the silica particles.
The results show that selective use of processing
aids before microfiltration had a very positive effect on subsequent flux performance and resultant
permeate quality. It is suggested that similar experimental assessment should be performed for some
advanced synthetic processing aids (Nylon 66, PVPP,
etc.) which have selective adsorption properties towards polyphenols. This is beyond the scope of this
study. The potential advantage of on-line addition of
the processing aid during microfiltration may be also
worthy of investigation.

4. Conclusions
The consistency of permeate beer quality depends
critically on a carefully controlled retention of colloidal micro particles and consistent transmission of
macromolecular solutes. A finely balanced particle
fractionation and solute transmission are susceptible to
alteration by the dynamic membrane fouling process
and the techniques employed for flux improvement

Q. Gan et al. / Journal of Membrane Science 194 (2001) 185196

during a continuous beer microfiltration process. This


inter-relationship between fouling, flux and permeate
quality flux has important implications in optimising
operating strategies for flux enhancement and product quality control. Given the evidence that in-pore
membrane fouling is the predominant cause of flux
decline and selectivity change, backflush at reversed
membrane morphology was shown to be a much more
effective technique for promoting flux and preserving
system selectivity. The experimental results have also
shown that although it was difficult to obtain a consistent permeate HRV and specific gravity throughout
the 24 h beer filtration, it was possible to obtain an
average permeate quality better the EBC standards.
Enhanced surface hydrodynamics had very limited effect on improving flux and maintaining system
selectivity as the surface flow conditions had little influence over the dominant in-pore fouling and on the
transmission of macromolecular solutes. The success
of backflush at reversed membrane morphology was
attributed to the pore clearing and particle-holding
effect of the open membrane substructure. At this
operating mode transmission of both hydrophilic and
hydrophobic proteins was enhanced as the microfiltration membrane was unable to discriminate against
these two groups of proteins of similar size range.
This predicament can be largely rectified by using
hydrophilic silica particles as the processing aids to
absorb specifically the hydrophilic or charged protein
molecules.
High temperature had a beneficial effect on flux
and HRV, but was detrimental to the permeate quality
with respect to the increased chill haze level. Pore
size was a major flux and quality control parameter.
The optimised nominal pore diameter is 0.5 m which
gave a more balanced flux and selectivity performance
in comparison to the 0.2 and 1.3 m pore diameters.
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