Concentration of Apple Juice by a Reverse

Osmosis/Nanofiltration Hybrid Process

Mariana Fonseca de Sousa

Thesis to obtain the Master of Science Degree in

Chemical Engineering

Supervisors:
Dr. Michael Harasek
Dra. Maria Norberta Correia de Pinho

Examination Committee
Chairperson: Dr. Francisco Manuel da Silva Lemos
Supervisor: Dr. Michael Harasek
Members of the Committee: Dr. Luís Miguel Minhalma

October 2015
Acknowledgments

There are a lot of people who deserve my gratitude for helping me with the elaboration of this
thesis. To both my coordinators, Professor Maria Norberta for her endless patience and readiness to
help me to do better and to Professor Michael Harasek for always being available to help and for making
my stay in TU Wien memorable. I could not have succeed in the aromatic analysis without Professor
Erwin Rosenberg from TU Wien and for that I am deeply grateful.
Also to the chairperson and supervisor of my thesis defence, Dr. Francisco Lemos and Dr. Luís
Miguel Milhalma for accepting to participate in my defence, for reading and helping it to improve.
I could never forget my family and friends. Particularly my sister that truly supported me
unconditionally.
At last, to the person who always helped and supported me. She dealt with all my neurosis and
was my mother away from home. So for Dr. Amal Ahmed, you have my profound appreciation and
gratitude.

2
Resumo

Palavras-chave: Concentração de sumo de maçã, Osmose Inversa, Nanofiltração, Ultrafiltração

O sumo de maçã é normalmente concentrado na última etapa do processo de produção num

evaporador de múltiplo efeito que apresenta diversas desvantagens. Os processos de separação com
membranas, nomeadamente conduzidos por pressão, podem ser uma alternativa à evaporação apesar
de apresentarem a limitação de não serem capazes de alcançar concentrações elevadas. Para
ultrapassar esta limitação, um novo conceito de processo híbrido combinando operações com
membranas, Nanofiltração/Osmose Inversa/Evaporação, foi estudado como uma possível substituição
à evaporação.
A membrana de osmose inversa da Alfa Laval, RO98pHt, foi capaz de concentrar o sumo de
maçã desde 9,7º até 20º Brix com um fluxo médio de 43 Kg/(h.m2) e uma rejeição ao açúcar de cerca
de 98%. A membrana DK da GE obteve o fluxo mais elevado e a rejeição ao açúcar mais baixa com
um fluxo médio de 10 Kg/ (h.m2) e uma rejeição de 80% para o segundo andar.
O efeito da ultrafiltração como pré-tratamento também foi avaliado conduzindo a que nas
operações com membranas subsequentes os fluxos de permeação sejam mais elevados.
Uma análise aromática foi efetuada a diversas amostras e foram verificadas perdas de
compostos aromáticos relevantes, principalmente com a ultrafiltração.
Uma avaliação económica foi efetuada para determinar a poupança energética do processo
híbrido proposto. A comparação com o processo tradicional de evaporação apresenta uma poupança
de 73%. A área total de membrana e o número de módulos a instalar foram calculados para uma
alimentação de 100 ton/h. Duas configurações de instalação de módulos foram sugeridas.

3
Abstract

Key words: Apple juice concentration, Reverse Osmosis, Nanofiltration, Ultrafiltration

Apple juice is normally concentrated in multi effect evaporators that present several
disadvantages. Membranes separation processes, namely pressure driven processes, can be an
alternative to evaporation although present other disadvantages like not being able to reach desired
concentrations.
To attempt to overcome this limitation, a new multistage membrane Nanofiltration/Reverse
Osmosis/Evaporation process was studied as a possible replacement to evaporation.
Reverse osmosis membrane from Alfa Laval, RO98pHt was able to concentrate apple juice from
9,7º to 20º Brix with an average flux of 43 Kg/(h.m2) and a rejection around 98%. Nanofiltration
membrane DK from GE obtained the highest flux and lowest rejection for the second stage with an
average flux of 10 Kg/(h.m2) and a rejection of 80%.
Ultrafiltration effect was also evaluated as a pre-treatment step obtaining higher permeate rates
in sequential steps.
Aromatic analysis was performed to several samples and there was some relevant aromatic
components loss.
An economic evaluation was performed to determine the energetic savings of the hybrid process
compared with the traditional process with a 73% energetic saving. Total area and module numbers
were calculated for a 100 ton/h feed. Two distinct installation module configurations were suggested.

4
Contents

List of Figures ........................................................................................................................................ 7

List of Tables ......................................................................................................................................... 8
List of Graphs ........................................................................................................................................ 9
List of abbreviations ........................................................................................................................... 10
1. Introduction .................................................................................................................................. 12
1.1. Membrane Technology ...................................................................................................... 12
1.1.1. Membrane processes................................................................................................. 12
1.1.2. Pressure Driven Membrane Processes .................................................................. 15
1.2. Apple Juice Industry, Traditional Process and Constitution ......................................... 18
1.2.1. Apple Juice Industry ................................................................................................... 18
1.2.2. Apple Juice .................................................................................................................. 19
1.2.3. Traditional apple juice production ............................................................................ 21
1.3. Membrane Application in Apple Juice Industry .............................................................. 22
1.4. Concept of a Multistage Membrane Process ................................................................. 24
2. Scope and Research Approach ............................................................................................... 26
3. Experimental Set up and Procedure ........................................................................................ 27
3.1. Experimental Set Up .......................................................................................................... 27
3.2. Experimental Procedure .................................................................................................... 28
4. Experiments and Results........................................................................................................... 30
4.1. UF membrane K328 from KOCH ..................................................................................... 30
4.2. RO membrane RO98pHt from ALFA LAVAL ................................................................. 35
4.3. NF membranes ................................................................................................................... 40
4.3.1. MPF 34 membrane from KOCH ............................................................................... 40
4.3.2. NF270 membrane from FILMTEC............................................................................ 41
4.3.3. MPF36 membrane from KOCH ................................................................................ 44
4.3.4. Nadir membrane from Microdyn Nadir .................................................................... 46
4.3.5. DK membrane from GE ............................................................................................. 47
4.4. Membrane Comparison ..................................................................................................... 49
4.4.1. First Stage.................................................................................................................... 49
4.4.2. Second stage............................................................................................................... 50
4.4.3. Mass balance .............................................................................................................. 50
4.5. Conductivity ......................................................................................................................... 51
4.6. pH .......................................................................................................................................... 52
4.7. Aroma Analysis ................................................................................................................... 53
5
5. Energy consumption and Saving Estimation .......................................................................... 57
5.1. Membrane Energy Consumption ..................................................................................... 57
5.2. Evaporators Energy Consumption ................................................................................... 58
5.3. Energy consumption: Design Comparison ..................................................................... 59
6. Area and Module Configuration ................................................................................................ 61
6.1. Membrane Area and Number of modules....................................................................... 61
6.2. First arrangement: equal number of parallel modules .................................................. 61
6.3. Second Arrangement: Tapered Design........................................................................... 62
7. Conclusions and further work ................................................................................................... 64
Bibliography ......................................................................................................................................... 65
Annex.................................................................................................................................................... 69

6
List of Figures

Figure 1: Schematic membrane cross flow mode diagram with permeate and retentate movement
representation ........................................................................................................................................ 12
Figure 2: Typical UF flux curves evolution [3] ......................................................................................... 15
Figure 3: Example of an apple juice production process ...................................................................... 21
Figure 4: New integrated process purposed by Alvarez et al. (2000) ................................................... 23
Figure 5: Traditional multistage membrane concentration diagram ...................................................... 24
Figure 6: New multistage membrane concentration diagram ................................................................ 25
Figure 7: Experimental set up diagram ................................................................................................. 27
Figure 8: Experimental set up image ..................................................................................................... 27
Figure 9: Permeate and retentate samples of experiences with UF membrane K328 from KOCH ...... 31
Figure 10: Diagram of UF pre-treatment with K328 from KOCH membrane ........................................ 31
Figure 11 : Membrane K328 after use ................................................................................................... 32
Figure 12: Permeate and retentate image of experiment J ................................................................... 36
Figure 13: Diagram of reverse osmosis with Ultrafiltration pre treatment ............................................. 37
Figure 14: RO98pHt permeate and retentate with UF pre treatment .................................................... 38
Figure 15: MPF 34 membrane after use ............................................................................................... 41
Figure 16: MPF 34 permeate and retentate .......................................................................................... 41
Figure 17: Diagram of a reverse osmosis membrane process followed by a nanofiltration membrane 42
Figure 18: NF270 membrane after experiments ................................................................................... 43
Figure 19: Permeate and retentate samples image with NF270 membrane ........................................ 43
Figure 20: Membrane MPF36 after use ................................................................................................ 45
Figure 21: Final diagram for an apple juice concentration diagram with a first and second stage ....... 51
Figure 22: Aroma analysis ..................................................................................................................... 54
Figure 23: Multi effect evaporator diagram [27] ....................................................................................... 58
Figure 24: Diagram of the first module arrangement ........................................................................... 61
Figure 25: Diagram of second module arrangement ............................................................................. 62

7
List of Tables

Table 1: Main modular membrane arrangement characteristics ........................................................... 13

Table 2: Membrane separation processes classified by phase, driving force and permeate state ...... 14
Table 3: Pressure driven membrane processes classification by particle size and applied pressure .. 15
Table 4: Example of NF processes in several industries [5] ................................................................... 17
Table 5: Apple juice average composition in USA [13] ........................................................................... 20
Table 6: Example of apple juice aroma composition, main components and molecular weight [14] ...... 20
Table 7: K328 UF membrane characterization summary...................................................................... 30
Table 8: Operating conditions for UF membrane K328 from KOCH and for experiments from A to G 31
Table 9: Operating conditions for experiments A-G with membrane K328 ........................................... 32
Table 10: RO98pHt membrane from ALFA LAVAL characterization .................................................... 35
Table 11: Operatory conditions for experiences J to P performed with membrane RO98pHt from ALFA
LAVAL.................................................................................................................................................... 35
Table 12: MPF34 membrane characterization ...................................................................................... 40
Table 13: Experimental conditions of Exp. Q with membrane MPF34 .................................................. 40
Table 14: NF270 membrane from FILMTEC characterization .............................................................. 41
Table 15: Operational conditions of experiences R and S for NF270 membrane ................................. 42
Table 16: MPF36 membrane characterization ...................................................................................... 44
Table 17: Operational conditions of experiments T,U,W,X and Y with membrane MPF 36 ................. 44
Table 18: Nadir membrane characterization ......................................................................................... 46
Table 19: Operational conditions of experiments Z with membrane Nadir ........................................... 46
Table 20: DK membrane characterization ............................................................................................. 47
Table 21: Operational conditions of experiments AA, AB and AC with membrane DK ....................... 47
Table 22: Mass Balance values for the proposed diagram ................................................................... 51
Table 23: Sample ID .............................................................................................................................. 53
Table 24: Calculations of membrane energy consumption for a feed of 100 ton/h............................... 58
Table 25: Evaporator energy consumption for the traditional ad proposed hybrid process .................. 59
Table 26: Membrane and Evaporation energy consumption comparison ............................................. 59
Table 27: Hybrid Process monetary savings in Portugal and Austria ................................................... 60
Table 28: Membrane area calculations ................................................................................................. 61
Table 29: First module arrangement ..................................................................................................... 62
Table 30: First and Second stage consecutive modules for each parallel module ............................... 63

8
List of Graphs

Graph 1: Millions of fruit juice produced for several fruits between 2008-2013 .................................... 18
Graph 2: Circular chart of the distribution of the different fruit juices consumption in 2013 [9] ............... 19
Graph 3: Circular chart of apple juice production countries in EU [9] ..................................................... 19
Graph 4: Permeate flux evolution through time for UF membrane K328 at ambient temperature and 6
bar.......................................................................................................................................................... 32
Graph 5: Flux influence on time for membrane K328 at different temperatures ................................... 33
Graph 6: Sugar rejection evolution through time for membrane K328 at different temperatures and 6
bar.......................................................................................................................................................... 33
Graph 7: Permeate Brix evolution with time for membrane K328 at different operatory conditions ..... 34
Graph 8: Feed Brix influence on permeate flux for membrane RO98pHt at 50 bar and ambient
temperature ........................................................................................................................................... 36
Graph 9: Flux influence on feed Brix of RO98pHt under different operational conditions .................... 36
Graph 10: Rejection influence on feed Brix of RO98pHt under different operational conditions .......... 37
Graph 11: Feed Brix influence on flux evolution with membrane Ro98pHt with and without pre-
treatment with UF .................................................................................................................................. 38
Graph 12: Flux evolution with applied pressure for different Brix.......................................................... 38
Graph 13: Van’t Hoff osmotic pressure ................................................................................................. 39
Graph 14: Dow/Filmtec osmotic pressure ............................................................................................. 39
Graph 15: Feed Brix influence on permeate flux and rejection in membrane MPF 34 ......................... 41
Graph 16: Flux and rejection evolution with feed Brix for NF270 membrane ....................................... 43
Graph 17: Flux influence on feed Brix of membrane MPF36 ................................................................ 45
Graph 18: Flux influence on concentration of membrane MPF36 with or without pre-treatment.......... 45
Graph 19: Flux influence on sugar concentration of experience Z with membrane Nadir .................... 46
Graph 20: Sugar concentration influence on permeate flux levels for experiments AA and AB with DK
membrane.............................................................................................................................................. 47
Graph 21: Sugar concentration influence on sugar rejection coefficients for experiments AA, AB and
AC with membrane DK .......................................................................................................................... 48
Graph 22: Flux evolution with time with membrane DK with and without UF pre-treatment ................. 48
Graph 23: Feed Brix influence on permeate flux for first stage membranes ......................................... 49
Graph 24: Feed Brix influence on sugar rejection coefficients for first stage membranes .................... 49
Graph 25: Feed Brix influence on flux for second stage membranes ................................................... 50
Graph 26: Feed Brix influence on sugar rejection coefficients for second stage membranes .............. 50
Graph 27: Conductivity evolution with feed Brix in retentate samples .................................................. 52
Graph 28: Conductivity evolution with feed Brix in permeate samples ................................................. 52
Graph 29: pH versus sugar concentration of the feed in the retentate ................................................. 53
Graph 30: pH versus sugar concentration of the feed for permeate ..................................................... 53
Graph 31: Ethyl and CO2 expression on permeate and retentate samples .......................................... 55
Graph 32: Permeate and Retentate area values for known compounds .............................................. 56
9
List of abbreviations

µ - Viscosity
A - Membrane area
AT – Austria
C - Consumption of thermal primary energy
CA- solute A concentration
CAa - concentration of the solute on the feed
CAM - concentration of solute adjacent to the membrane surface
CAP - concentration of solute in the permeate
CF – Feed Brix
CP – Permeate Brix
CR – Retentate Brix
CS - substitution coefficient
DAW - diffusion coefficient of the solute in a free solution
E - Consumption of electrical energy
E.C. – Energy Consumption
Ep – Power
G- Gas phase
i - Van’t Hoff factor
J- Permeate flux
L- Liquid phase
M - Molecular mass
MF - Microfiltration
mj - Sum of molality concentration of constituent j
ms - Mass flow rate of steam
MWCO – Molecular Weight Cut Off
NF- Nanofiltration
PT – Portugal
PV- Pervaporation
q - Thermal power
qv - Volumetric flow rate
R - Rejection of the sugar compounds
Re- Reynolds number
RGC- Ideal Gas Constant
RO- Reverse osmosis
Rt - Total membrane resistance.
SPME - Headspace solid phase micro extraction

10
T – Temperature
ΔP - transmembrane pressure
UF- Ultrafiltration
δ - Thickness of a volume adjacent to membrane layer
Δm - Mass difference
ΔP - Pressure applied
Δt - Time interval
η – Efficiency
λ - Water latent heat
Π – Osmotic pressure

11
1. Introduction

1.1. Membrane Technology

Membrane process developments have given this technology a place in industry. Its implementation
has optimized processes through benefits like high efficiency, small footprint, less use of space and
energy consumption among many others advantages. This benefits have led to a gradual replacement
of membranes over conventional technology like evaporation or freezing/crystallization.

1.1.1. Membrane processes

Membranes function on a physical process, not relying on heat as a driving force. One stream
enters the module, the feed, and flows tangentially to the membrane surface. Permeable compounds
will pass through the membrane and leave the module in one stream, designated as permeate, while
the non-permeable, rejected by the membrane, will leave in another stream designated retentate.
A schematic representation of a selective permeable membrane is represented in figure 1.
Solutes with higher affinity to the membrane (blue dots) are preferably permeated while others (orange
dots) are rejected, enriching the feed in these solutes. In figure 1 the feed flow travels tangentially to
the membrane. This type of filtration is known as cross flow mode.

FEED RETENTATE

PERMEATE

Figure 1: Schematic membrane cross flow mode diagram with permeate and retentate movement representation

For industrial use, membranes are arranged into module configurations characterized by a large
ratio of membrane surface area per unit volume. These have high processing capacity in adequate
hydrodynamic pressure conditions of operation. Easy cleaning and maintenance are also desired.
The four modular configurations most common are tubular, hollow fiber, flat sheet and spiral
wound. Table 1 synthetizes the arrangements and characteristics of each modular configuration.

12
 Table 1: Main modular membrane arrangement characteristics
Tubular Hollow Fiber Flat Sheet Spiral- wound
These modules
Modules are
comprise a
composed of a Modules are thin In these modules
selective flat
number of tubular membranes two membrane
sheet
Arrangement membrane tubes in compact sheets are
membrane on
assembled into modules. separated by a
the top and a flat
shell-and- tube mesh.
plate on the
arrangement
bottom
-Are recommended
to work with Re
-Are easily cleaned
between -The pressure
by mechanical or
500<Re<3000 drop is high due
chemical methods
-Have low energy -Re numbers are to the feed
-They need large
consumption and in the laminar spacers drag
operating space
highest surface flow region -Have the lowest
Characteristics due to high hold ups
area-to-volume ratio investment and
volume of tubular
-The good high surface
modules and the
backwash capacity area-volume
lowest surface
makes them easy to ratio
area-to-volume
clean
ratio
-Susceptible to get
blocked

Membrane processes can also be classified upon the state of the phase of the streams and by
the driving force that forces the passage through the membrane. Table 2 summarizes these processes
indicating the phases and the driving force involved. The focus of this work will be pressure driven
processes in liquid phase.

13
 Table 2: Membrane separation processes classified by phase, driving force and permeate state
Membrane Phase Driving Force Permeate
Process Feed/permeate
Forward osmosis Liquid/Liquid Concentration Solvent
Difference
RO, NF, UF and Liquid/Liquid Pressure Solvent
MF Difference
Dialysis Liquid/Liquid Concentration Solute
Difference
Electrodialysis Liquid/Liquid Electrical potential Solute
Gas permeation Gas/Gas Partial pressure Preferably
Difference permeating
component
Pervaporation Liquid/Gas Partial pressure Preferably
difference permeating
component
Membrane Liquid/Gas Partial pressure Solvent
Distillation difference
Osmotic Liquid/Gas Partial pressure Solvent
distillation difference

There are several advantages and disadvantages in membrane processes. Before choosing, a
comparative assessment should be made between membrane processes and traditional separation
methods. Below are listed the advantages and disadvantages of membrane processes.[1]

Advantages:
- The solute size range of separation is very broad, this means that theoretically
membrane processes can please a high number of separations needed.
- Most membrane processes do not need a change in physical state, leading to less
energy spent and are appropriate to deal with components sensible to phase changes.
- Membrane processes are simple, easy to operate and have low maintenance operation.
- They can be designed to achieve high selectivity, being able to recover components
with low presence but high value.
- The use of “simple” and non-toxic materials as well as lower energy costs makes
membranes environmental friendly.
Disadvantages:
- In most cases, membrane processes cannot separate two pure products. One of the
outcome stream has minor amounts of the second component.
- Membranes can react negatively with solutions that contain for example high organic
compounds.
- The temperature application range can limit membrane applicability.
- Larger feeds have to be divided in several parallel modules.
- Fouling can occur restricting permeation rates.

14
 1.1.2. Pressure Driven Membrane Processes

Pressure driven membrane processes, as mentioned in table 2, have as driving force the
pressure difference between feed and permeate to instigate the permeate flow through the membrane.
These processes are normally divided into four main groups based on membrane pore size and
transmembrane pressure (ΔP). In table 3 it is summarized the separation size ranges and applied
pressure range. In fact, only in Microfiltration (MF) the separation membrane is controlled by sieving
effects. Ultrafiltration (UF) is determined both by sieving and physical-chemical effects. In Nanofiltration
(NF) and Reverse Osmosis (RO) the membrane-solvent-solute interactions are usually described by the
solution-diffusion theory.
Molecular weight cut-off (MWCO) is a concept often used to characterize membranes. Feed solutes
with molecular weight superior to the MWCO have a high probability to be rejected by the membrane.

Table 3: Pressure driven membrane processes classification by particle size and applied pressure
Particle Size ΔP
(nm) (bar)
MF: Microfiltration 100-10.000 0,1-1
UF: Ultrafiltration 1-100 1-10
NF: Nanofiltration 0,5-10 10-30
RO: Reverse Osmosis <0,5 35-100

Typical flux curves are divided in 3 regions. The first region is characterized by a fast accentuated
decrease of the flux that can be connected to the solute adsorption or blocking of the membrane pores.
In the initial moments, the pores are clean and the flux has the highest value. However, soon the
membrane begins to be fouled by the solutes in the feed and the flux decreases. These same reasons
are also associated to the increase in the rejection coefficients. After the initial period, the flux still
decreases and eventually a cake layer may be formed.[3]

Figure 2: Typical UF flux curves evolution [3]

15
 As a result of a pressure gradient, perpendicular to membrane surface, the feed permeates through
the membrane with partial or total rejection of the solutes. In steady state, the convective flux towards
the membrane results in a balance between the solute flux through the membrane and the diffusive
solute flux from membrane surface to the feed bulk. A concentration polarization profile is developed in
the boundary layer adjacent to the membrane.
A mass balance to a differential element volume in the layer adjacent to the membrane of thickness
δ, is presented in equation (1). CA represents the solute concentration, J the flux and D AW the diffusion
coefficient of the solute in a free solution.

dCA
J. CA − DAW . = J. CAp (1)
dx

x = 0 CA = CAa (2)
x=δ CA = CAm (3)

The integration of equation (1) with the boundary conditions of equation (2) which refers to the
concentration of the solute on the feed (CAa), and equation (3) which refers to the concentration of solute
adjacent to the membrane surface (CAM), results in the mass balance equation (4).
J.δ
CAm −CAp
= eDAW (4)
CAa −CAp

Although concentration polarisation can be reversible, it can lead to loss of performance due to
the introduction of an additional resistance to flow and a precursor of membrane fouling. Several
parameters like nature, concentration of solutes and solvents, membrane type, pore size distribution,
surface characteristics, membrane material and feed flow hydrodynamics influence fouling formation.

Ultrafiltration

UF processes remove high molecular-weight solutes, colloidal materials, organic and inorganic
polymeric molecules. The low molecular-weight organics and ions such as sodium, calcium, magnesium
chloride, and sulphate are not removed by UF processes. Because only high-molecular weight species
are removed, the osmotic pressure differential across the UF membrane surface is negligible [2]. The
osmotic pressure (π) is the necessary pressure to the water chemical potential in the feed solution to
be elevated to the value of pure water at atmospheric pressure.

In UF, the flux is dependent of the applied pressure. This dependency is described by Darcy
Law, equation 5, where µ stands for viscosity and Rt for total membrane resistance. The decrease in
flux is translated by the increase in the parameter Rt and in the solution viscosity.
∆𝑃
J= (5)
μ.Rt

Ultrafiltration is mainly used in the manufacturing processes in chemical and pharmaceutical

industries. It is also used in waste water treatment, food and beverage processing.[4]

16
Nanofiltration

NF membranes are somewhere between UF and RO membranes. They often offer a

compromise between high rejection coefficients and low applied pressures. NF membranes differ from
RO membranes in the way NF membranes distinguish between mono and bivalent salts while RO
membranes rejects everything.
In NF and RO processes, the osmotic pressure difference between permeate and retentate
cannot be neglected therefore equation (5), for the permeation flux, takes the form of equation (6).

∆P− ∆π
Jv = μ.Rt
(6)

Nanofiltration is gaining more and more importance mainly in the field of drinking water
purification where nanofiltration steps are used to remove organic substances as micro pollutants and
multivalent ions [5]. More recently, NF is being applied in food processing industries for concentration and
demineralisation. Table 4 resumes other uses of nanofiltration in diverse industries.

Table 4: Example of NF processes in several industries [5]

Industry Uses
Non-thermal solvent recovery and management
Fine chemistry and Pharmaceuticals
Room temperature solvent exchange
Oil and Petroleum chemistry Removal of tar components in feed
Purification of gas condensates
Bulk Chemistry Product Polishing
Continuous recovery of homogeneous catalysts
Natural Essential Oils and similar Fractionation of crude extracts
products Enrichment of natural compounds Gentle Separations
Medicine Is able to extract amino acids and lipids from blood and
other cell culture

Reverse Osmosis

Osmosis is the natural process when two solutions, with different concentrations of a solute, are
put into contact through a semi permeable membrane. In the search for equilibrium the solute passes
from the more concentrated solution to the lower to achieve equilibrium. RO process follows the opposite
movement by applying pressure to overcome the osmotic pressure and forces the solvent through the
membrane creating a dilute and a concentrated solution. The transport depends of the temperature, the
pressure and the concentration difference between permeate and retentate. An increase in the pressure
and temperature, results in an increase in the flux through the membrane although in different measures.

17
 Solute concentration also affects immensely the performance of the RO process. As the solute
concentration increases so does the osmotic pressure. This makes the amount of necessary applied
pressure, to reverse the natural direction of the flow to increase. This is one of the main limitations of
concentration with RO processes.
NF and RO are very promising membrane processes due to their wide range of applicability.
Even though they are not always the most economically viable options, the development of new
membranes and process improvements has decreased costs and therefore amplifying their range of
applicability.

1.2. Apple Juice Industry, Traditional Process and Constitution

1.2.1. Apple Juice Industry

The juice industry has seen a global decline in consume driven by the decline of orange juice
consumption, shown in graph 1, mostly due to the price increase, changes in traditional eating habits,
awareness and demand of lower sugar levels in drinks [6]. Even though orange juice leads the decline
in juice consumption due to the price increases, other fruit juices experience a growth in their
consumption like apple, grape and pineapple juice, associated with the newly trends and social
behaviours to experience a healthy life style achieved by the consumption of natural products.[7]
Graph 1 shows the evolution in the production of fruit juices in the last years.

4 000 Others
Millions of fruit juice production

Single citrus fruit

(excluding orange
3 000 and grapefruit)
Mixtures of fruit and
vegetable

Apple
2 000
Grape

1 000 Pineapple

Grapefruit
0
2008 2009 2010 2011 2012 2013 Orange

Year

Graph 1: Millions of fruit juice produced for several fruits between 2008-2013

In spite of the decline in consumption, in 2013, it can be noticed in graph 2, that the unconcetrated
orange juice is still the most produced juice with almost 30% of all juice production, followed by mixture
fruits with 23% and apple with 20%. With significantly lower percentages grape juice stands for 9%,
pineapple and citrus fruits with 3 % each.[9]

18
 Single citrus
Tomato fruit
(excluding
Others orange and
grapefruit)

Unconcentrated
Mixtures of
orange
fruit and
vegetable

Orange
Grapefruit
Grape
Apple
Pineapple

Graph 2: Circular chart of the distribution of the different fruit juices consumption in 2013[9]

Being recommended for young children due to the pleasing sweet taste and mild laxative effects,
apple juice benefits are varied helping relieving several symptoms associated with asthma,
arteriosclerosis among others like lung cancer prevention. The nutritional benefits include high levels of
vitamin A and C and a good source of potassium, calcium, iron and phosphorus.[8]
Graph 3 shows the division of the main apple juice producers in the EU. In Europe, apple juice has
its main producers in Germany, with almost half of the European production, followed by Poland and
United Kingdom with 18 and 10%, France, Italy and Spain have approximately 5 %.

Hungary Others France

Poland
Austria
Belgium Germany
Spain
Denmark United
Kingdom Italy

[9]
Graph 3: Circular chart of apple juice production countries in EU

In the world view, China is a major producer of apple juice being responsible for two thirds of USA
apple juice consumption. [11]
Even though the list of health benefits is quite extensive, apple juice has been under attack in USA
after being announced the existence of elevated levels of arsenic in a popular television talk show. After
the alarm raised, the Food and Drug Administration conducted studies on several apple juice samples
trying to educate the public by explaining the difference between organic and inorganic arsenic. [12]

1.2.2. Apple Juice

The concentration of apple juice components, diverges with the type of apples used. In average,
the major constituents of apple juice are fruit sugars like fructose, glucose and sucrose. The amount of
sugars in juices is usually measured in Brix. The Brix indicates the grams of sugar in 100 g of solution.
Acids are also present in lower concentrations, with malic acid being by far the main acid. Additionally

19
in residual concentrations, it was already mentioned potassium, phosphate and magnesium among
others. Table 5 exemplifies an apple juice concentration.

[13]
Table 5: Apple juice average composition in USA
Component Concentration Component Concentration
Sucrose (g/100mL) 2,16 Sodium (ppm) 11,8
Glucose (g/100mL) 2,01 Potassium (ppm) 1511
Fructose (g/100mL) 5,69 Magnesium (ppm) 64,9
Sorbitol (g/100mL) 0,45 Calcium (ppm) 41,9
Quinic (mg/100mL) 41,8 Iron (ppm) 0,1
Malic (mg/100mL) 847,7 Chloride (ppm) 1,4
Isocitric (mg/100mL) 3,8 Phosphate (ppm) 252,1
Shikimic (mg/100mL) 1,4 Chlorogenic (ppm) 70,7
Citric (mg/100mL) 11,9 Catechin (ppm) 1,2
Fumaric (mg/100mL) 0,14 Caffeic (ppm) 4,9
Epicatechin (ppm) 16,6
p- Coumaric (ppm) 4,9
Ferulic (ppm) 0,3
Rutin (ppm) 8,2
Phloridzin (ppm) 26,1

Aroma composition also differs according to the type of apples used. Additionally, this
components are not originally present in apples only formed after the beginning of apple juice
production[14]. The identification of these components is complex due to their multitude and due to the
aromatic nature of apples. In table 6, an example is advanced of an apple juice aroma composition. The
major components present are butanol, isobutanol, isopentanol and ethyl acetate.

[14]
Table 6: Example of apple juice aroma composition, main components and molecular weight
Compound Concentration (ppm) Molecular weight
Ethyl acetate 150 88,11
Ethyl butanoate 90 116,16
Ethyl-2-methyl butanoate 70 130,19
Isopentyl acetate 70 130,19
Hexyl acetate 20 144,22
Hexanal 70 100,2
Isobutanol 180 74,12
Butanol 200 74,12
Isopentanol 170 88,15
Hexanol 40 102,18

20
 Fermentation can change apple juice composition and aroma constitution. Yeasts are
microorganisms present in juice, responsible for the fermentation process. Most yeasts require oxygen
and a basic substrate such as sugar. Some yeasts can ferment sugars to alcohol and carbon dioxide in
the absence of air. They produce ethyl alcohol and carbon dioxide from simple sugars such as glucose
and fructose as portrayed by equation 7.[15]

C6H12O6 → 2C2H5OH + 2CO2 (7)

Glucose yeast ethyl alcohol + carbon dioxide

Fermentation is sometimes difficult to avoid due to the broad range of operatory conditions in
which yeasts are active. They can prosper in the range of 0 to 50ºC and are acid tolerant. Solutions
containing 40% of sugar, create a favourable environment for yeasts to grow. There are only a few
yeasts that can tolerate sugar concentrations of 65-70% and these grow very slowly in these conditions
(Board, 1983). [15]
After alcohol is formed and if the solution is exposed to an oxygen source, acetic acid (vinegar)
can be formed.
In fermented juices, the main aroma compounds were studied to be 2-hydroxyethylhydrazine,
3-methyl-1-butanol, hexanoic acid ethyl ester and acetic acid hexyl ester [14].

1.2.3. Traditional apple juice production

Fruit
Washing Sorting Milling
Reception

Aroma
Depectinization Press
Concentrate

Floculation Centrifugation

Concentration

Figure 3: Example of an apple juice production process

The traditional process for juice concentration, resumed in figure 3, starts with washing, sorting
followed by milling and pressing of the apples until pulp. After milling, pectolytic enzymes are added to

21
the mixture to break down the fibres and facilitate the pressing process. After being pressed for the
extraction of all possible liquid, the solid residues are normally used for animal consumption. The juice
is then extracted and goes through clarification for the removal of components responsible for the juice
cloudiness like pectins. This clarification is achieved with the addition of pectolytic enzymes that cause
the protein complexes to flocculate, originating larger particles that settle and make it easier to filtrate.
Clarification takes 2 hours at 50ºC or approximately 10 hours at 20ºC. Amylases are also added during
enzyme treatment to break down the starch molecules that may cause cloudiness during storage.
Finning agents like gelatine, bentonite, tannic acid or silica sol can also be added as fining agents to
help the settling of the flocs.
Apple juice production is normally a season occurrence. To preserve the juice, decrease costs
associated with transport, storage or to sell, apple juice is normally concentrated in the final processing
step. Traditionally, this concentration takes place in multi-effect evaporators. This process presents
several disadvantages like high energetic consumption due to high latent heat of water and degradation
of aromatic components. Usually, aroma compounds are removed in an evaporator, before
concentration, and are united to the concentrate afterwards.[16]

1.3. Membrane Application in Apple Juice Industry

The industrial use of membrane processes was made possible through the development of
asymmetric membranes by Loeb and Souriragin in the early 1960s. NF process was applied in several
parts of the juice industry process, such as recover aromas from fruit juices (Diban et al.), process
wastewater from juice beverage production (Hitoshi et al.) and to control sugar concentration (García-
Martín et al.). RO process was studied in the juice concentration step although could never reach the
concentration achieved through evaporation due to the high osmotic pressure limitations (Petrotos et
al.).
In apple juice clarification process, membrane fouling was studied to be caused by pectin,
tannins, proteins, starch, hemicelluloses and cellulose (Santón). Some problems that occur in filtration
processes are caused by colloids. These are either part of the fruit or are formed by microorganisms
during fruit maturing (Barros et al.). Pectin is a gel-forming agent present in fruit juices with a fibre-like
assembly that stops the clarification process by reducing permeation flux and yield (Srimanta et al.).
Therefore, juices can be depectinized to reduce viscosity and fouling (Saxena et al.).
Preservation of fruit derivates is usually made with thermal treatments (Ibarz et al.). This
treatments have as side effects non-enzymatic browning, nutrient loss and the formation of undesirable
by-products. In apple juice, the concentrated product turns brown during thermal processing due to a
nonenzymatic browning cause. (Burdulu and Karadeniz).
UF and MF processes have been used more and more in industry for clarifying fruit juice. To
succeed in this task, UF and MF processes have to maintain high fluxes and achieve desired product
qualities. Nong-xue et al. studied separation conditions of UF process for apple pectin and the
relationship between apple pectin and different relative molecular weights, concluding that 68% of apple

22
pectins had molecular weights over 300 kDa, and those with weights below 5 kDa accounted for only
3.31%. Most UF processes studies, use membranes with different pore sizes, like Onsekizoglu et al.
that used an UF membrane to filtrate 12º Brix apple juice through a 10-kDa and a 100-kDa MWCO
membranes. Colour solution was improved with the 10-kDa membrane but some minor components,
mainly phenolics and trans-2-hexenal, were retained. Apple juice composition barely changed after UF
with 100 kDa.
In juice processing the concentration should achieve at least 65 ºBrix. RO processes obliges
high operating pressures to overcome its limitations of osmotic pressure, thus, RO processes are
studied as preconcentration steps combined with other processes like osmotic evaporation. Gurak et al.
studied the concentration of grape juice with a RO process at 40, 50 and 60 bar and at 20, 30 and 40ºC.
The conditions with better results were at 60 bar and 40ºC achieving high fluxes and a 28,5º final Brix.
Sa et al. obtained high quality concentrated pineapple fruit juice with sugar contents ranging from 28 to
35º Brix.
Alvarez, Riera and Coca used the RO spiral wound aromatic polyamide membrane (MSCB 2521
R99, Separem, Italy, surface area 1.03 m 2, Na Cl 99,2%) to study the rejection coefficients concluding
it to increase with ΔP (15-35 bar) and feed flows (200-600 l/h). The major compounds responsible for
apple juice flavour the ethyl-2-methyl butanoate, ethyl butanoate and hexanol were rejected above 90%
at 35 bar and 600 l/h. It was also observed high retention of two other components that affected the
apple juice flavour negatively, ethyl acetate and isopentanol. In 2000, they purposed a new process for
apple juice: an integrated membrane reactor to clarify the raw juice; reverse osmosis to preconcentrate
the juice up to 25°Brix; pervaporation (PV) to recover and concentrate aroma compounds, and a final
evaporation step to concentrate apple juice up to 72°Brix. The process is schematized in figure 4.

Figure 4: New integrated process purposed by Alvarez et al. (2000)

Membrane performance and configurations

An optimum design of the membrane can minimize fouling and concentration polarization. This
optimization can involve transmembrane pressure, temperature and cross flow velocity. Sheu and Wiley,
studied the temperature effect between 20 and 60ºC verifying that the processing capacity suffers a rise
of 3 to 4% for each 1ºC rise.
23
 There were several studies where membrane materials and module configurations were
compared and optimized for apple juice processing. Sheu and Wiley establish that the recovery of apple
juice volatiles during concentration to 20º Brix was found to be about 80% when using a high resistance
RO (HR) membrane. Chua et al compared a commercial spiral wound cellulose acetate membrane (CA-
99) and an experimental polyamide membrane (PA-99,99/salt rejection) for concentrating apple juice
using a pilot-scale RO unit. The PA-99 membrane exhibited higher flux and concentration rates than the
CA-99 membrane. In addition, the PA-99 membrane retained 45% of the total odor-active volatiles in
the feed, while the CA-99 membrane retained 23%. Chou, Wiley and Scchlimme also tested the
permeation of apple juice with polyether-urea and polyamide thin film composite membranes during RO
process. The polyamide membrane permeated 2 to 3 times less hexanal and ethyl-2-methylbutyrate.
They concluded that polyamide membranes usually presented a stronger flavour apple juice than
polyether urea presenting also a longer useful life.
Membrane configurations can also affect aroma compounds. Chou concluded that the plate and
frame configuration had 11,5 % permeation of n-hexanal compared with 0,5% for the spiral wound.
Chou et al. achieved conclusions pertinent for this work: an increase in the processing
temperature tends to increase the permeation rate of volatiles, although there is a dependency of the
type of volatile. Increased pressure can result in higher flux, reduced process time and smaller flavour
compounds losses associated to the volatilization and adhesion at the membrane.

1.4. Concept of a Multistage Membrane Process

A traditional arrangement of a NF/RO process for sugar concentration is depicted in figure 5. A

nanofiltration membrane is used in a first stage concentration. The retentate is the feed to a reverse
osmosis stage. This traditional approach faces concentration limitations due to the high osmotic
pressure achieved in the RO stage. Higher difference between the concentration on the permeate and
on the retentate, increases the osmotic pressure forcing the use of higher applied pressure (more
expensive) or lower rejection membranes that result in product losses.

Retentate
Retentate
NF RO

Permeate Permeate

Figure 5: Traditional multistage membrane concentration diagram

A new concept of a multistage process, portrayed in figure 6, was proposed by Harasek and
Gul ( Patent US 20120238777 A1). Promising results were achieved with a sugar solution concentration
from 15 to 50º Brix[31] .In this configuration reverse osmosis occupies the first stage and the
concentration difference between retentate and perme ate is lower than in the traditional approach. This
allows for lower applied pressures and higher concentrations obtained. In the second stage, a low
24
rejection NF membrane is used. To avoid product losses the NF permeate is recovered through the
recirculation to the first stage feed.

Retentate
Retentate

RO NF

Permeate
Permeate

Figure 6: New multistage membrane concentration diagram

25
2. Scope and Research Approach
Traditionally apple juice concentration is achieved with the use of a multi-effect evaporator.
Membrane processes advantages over traditional processes have been listed before and the aim of this
work is to study the potential of the application of membrane processes in apple juice concentration.
Many studies have been made with membrane processes. There are several operational
parameters like temperature, pressure, feed velocity, module configurations and membrane materials
that influence the performance of these processes. One of the main influences on the membrane
performance, is the feed chemical and physical characterization and its interactions. In a complex
product like apple juice, the prediction of a membrane behaviour is not easy due to the complex
composition and interactions among components and with the surrounding environment. The multistage
membrane concept described before had promising results with other solutions, overcoming some of
the limitations in membrane processes. For that reason, the scope of this work was to apply this concept
to the apple juice concentration process and to compare and evaluate its results in view of the industry
requirements like conservation of apple juice aroma constituents and economic viability. For each stage
it was desired a high flux. High sugar rejection levels were preferred for the first stage.
Several combinations of membrane and membrane operations were evaluated. The potential of
each arrangement was evaluated in terms of permeate flux, sugar rejection coefficients and aroma
analysis of the feed, permeate and retentate. Membrane RO98pHt from Alfa Laval was studied at
different pressures and temperatures. MPF34, MPF36 from Koch Membrane Systems; NF270 from
Filmetec Membranes; Nadir NP010 from microdyn Nadir and DK from GE were the nanofiltration
membranes tested.
Ultrafiltration has confirmed success in apple juice clarification and the effect of Ultrafiltration pre-
treatment on permeation flux values of subsequent membrane operation was evaluated with membrane
K328 from Koch Membrane Systems. For this, UF permeate was collected and treated with RO98pHt,
DK and MPF36.
To analyse the results obtained, permeation flux and sugar rejection coefficients were portrayed
in function of the Brix of the retentate. In Ultrafiltration analysis, flux evolution was expressed through
time since this process was used as pre-treatment and not as a concentration step.
To characterize the aroma profile of the apple juice samples, headspace solid phase microextraction
(SPME) measurements were undertaken. This analysis was made by an external expert.
Membrane fluxes and sugar rejection coefficients were compared and the optimal solution of all
studied possibilities was chosen. Mass balances for a feed of 100 ton/h were effectuated allowing the
study of the energy savings of a multi-stage membrane process plus evaporation compared with the
conventional process of “only” evaporation. Total membrane area to be used and module configuration
were proposed.

26
3. Experimental Set up and Procedure

3.1. Experimental Set Up

The experimental set used works on a batch mode. It has a feed tank with a capacity of two liters
that supplies the feed to a CAT pump 231 which deliveres the desired pressure. The membrane module
is rectangular with a 0,008 m2 area. The retentate was directed to the feed tank while the permeate was
weighted at 10 minutes intervals with a RADWAG PS 8000/C/1 scale.
Conductivity, pH and Brix concentration where also measured in 30 minute intervals with a WTW
Microprocessor Conductivity Meter LF 196, Voltcraft PH-100ATC and a KRUSS DR301-95 respectively.
Pressure and feed flow were set with the valves FC. Working temperature was established with an
external heat source involved in the feed tank jacket and controlled with a RS 206-3738 thermometer
located on the inside of the feed tank.

FI
PC

TI Retentate
FC

Membrane

Feed

Permeate

Feed Tank

Balança Digital

Figure 7: Experimental set up diagram

Figure 8: Experimental set up image

27
 To characterize the flavour profile of the apple juice samples, headspace solid phase micro
extraction (SPME) measurements were undertaken which allow the characterization of the volatile
compounds emitted from the sample.
The procedure is described below:
Solid phase micro extraction:
10 ml of each sample were transferred into 15 ml screw cap vials with mininert valves and
equilibrated. Manual SPME holder with Carboxen/PDMS fibre (85 μm). Extraction for 15 min from the
sample headspace at room temperature (25°C) with stirring.
GC/MS Analysis:
Thermo Scientific GC/MS Ultra with DSQ II Quadrupole-MS and AS 2000 autosampler.
Column: Restek Rtx 5 MS, 30 m x 0.25 mm, 0.25 μm df.
Oven program: 40°C (1 min) → 10°C/min → 250°C (8 min). Total run time: 30 min.
Injection-/Desorption temperature: 250 °C. Injection mode: CT Splitless.
Column flow: 1.5 ml/min constant flow mode.
MS: Transfer Line: 250°C. Ion Source: 200°C. Data acquisition start time: 0.00 min. Scan mode:
Full
Scan. Scan range: m/z 29-300.

3.2. Experimental Procedure

Membranes were installed and experiments were performed at stable pressure and temperature.
Between each experiment a cleansing of the system was performed with the water.
Water permeability was determined before and after each experiment at working pressure and
temperature. Brix, conductivity and pH in permeate and retentate were measured in 30 minutes
intervals. Permeate weight was registered in 10 minutes intervals.
The flux, rate of mass transport through the membrane, was calculated with equation (8) where
Δm stands for the mass difference in a defined time interval (Δt). A stands for the membrane area. The
flux is often taken as a measurement of the productivity.

∆m
J= (8)
∆t.A

The rejection of the sugar compounds, R, was determined through equation 9, where C P and
CR represent the Brix of the permeate and retentate, respectively. This factor is normally associated with
the performance of the membrane.[10]
CP
R=1− (9)
CR

Osmotic pressure difference is represented by Δπ to signal the osmosis pressure difference

between the solution at membrane surface and the permeate. This is the driving force that allows the
flux through the membrane. Theoretically, osmotic pressure can be calculated through Van’t Hoff

28
relation, equation 10, in which i represents the Van’t Hoff factor, M the molecular mass, T the
temperature and RGC the ideal gas constant. However, at high concentrations, this equation differs
greatly from experimental data.[17]
π = i. M. R (GC) . T(10)

Dow and Filmtec adapted equation 10 and use equation 11 to calculate osmotic pressure where mj
stands for the sum of molality concentration of constituent j.[18]

π = 1,12 (273 + T) ∑ mj (11)

The osmotic pressure can also be calculated empirically, using equation 12.

∆P− ∆π
J= μ.Rm
(12)

By representing the permeation flux evolution with the values of applied pressure, a linear
regression can be performed. The pressure value when the flux is null corresponds to the osmotic
pressure:
𝐼𝑓 𝐽=0 → ∆𝑃 = ∆𝜋

29
4. Experiments and Results

The results obtained for all the experiments are presented below. Experiments were divided
according to the membrane type and were given an identification letter or letters. In the beginning of
each new membrane introduction, tables are presented with a summary of the membrane characteristics
given by the supplier. In Annex II full specification sheets are supplied.

4.1. UF membrane K328 from KOCH

Table 7: K328 UF membrane characterization summary

Membrane Characteristic Data

Manufacturer KOCH Membrane Systems
Model HpHT 6438-K328-VYV
Chemistry Proprietary semi-permeable polyether sulfone (PES)
Pressure range (bar) 2,1-8,3
Temperature range (ºC) 5-60
Pure water flux at 25ºC (L/m2/h/bar) 24-53
pH range 2-10
MWCO(Da) 5.000

UF process was used with the intent of removing the colloidal components, responsible for the
fast decline of flux in sequential steps. The experiment was ran until the retentate volume in the feed
tank was residual. The permeate was collected and used to feed another membrane process as
portrayed in figure 10. Figure 9 portrays an image of a retentate and permeate sample. It is visible a
very light yellow tone in the permeate which leads to the conclusion than UF filtrated more than the
colloidal components desired.

30
 Figure 9: Permeate and retentate samples of
experiences with UF membrane K328 from KOCH

Retentate
Uf- retentate

10 Brix UF-Feed PERMEATE

K328 UF-Permeate
P=5 bar
T=50ºC

Figure 10: Diagram of UF pre-treatment with K328 from KOCH membrane

Several consecutive experiments, numerated from A-G were performed in the operatory
conditions listed in table 8. It was chosen a pressure within the pressure range values presented in table
7. This decision was made to reach a compromise between desirable high flux and low energy costs.
Low energy costs were also the reason of the temperature chosen.

Table 8: Operating conditions for UF membrane K328 from KOCH and for experiments from A to G

Condition Value
Pressure 6 bar
Temperature Ambient temperature
Feed flow rate 3 L/min
Feed 100% Apfel Spar
Sugar feed concentration 10 g/L

The experiments are portrayed in graph 4 that shows a decrease in the flux through time due to
the increase in viscosity and membrane resistance. A trend line with a potential evolution was added to
help perceive the flux evolution.

31
 60
Exp.A
50
Exp B
J (kg/h.m2) 40
Exp. C
30
Exp. D
20
Exp. E
10
Exp. F
0
Exp. G
0 50 100 150 200 250 300 350 400
Time (min)

Graph 4: Permeate flux evolution through time for UF membrane K328 at ambient temperature and 6 bar

In the end of each experiment a deposit was visible in a previous white membrane. Figure 11
shows an example of that deposit.

Figure 11 : Membrane K328 after use

Exp. H started at ambient temperature however, at the point t=100 min, the temperature was
increased until 58ºC. This increase in temperature provoked a rise in the flux. Exp. I was performed at
an average 57 ºC. Operating conditions of Exp. H and Exp. I are resumed in table 9. Graph 5 shows the
fluxes of these experiments and of experiment A at ambient temperature. Although there is an
accentuated increase in the flux when the temperature increased, it does not reach the initial flux of the
first experiment A. All experiments were performed with the same membrane and there is a decrease
in flux from one experiment to the next one. Between each experiment the experimental module was
cleaned with water.

Table 9: Operating conditions for experiments A-G with membrane K328

Exp. H Exp.I
Pressure 6 bar
Area (membrane) 0,008 m2
Temperature 44 ºC 57 ºC
Feed flow rate 3 L/min
Feed Type 100% Apfel Spar
Sugar feed concentration 10 g/L

32
 60
Exp. A
50 23ºC

J (kg/(h.m2))
40 Exp. I
57ºC
30
Exp. H
20
23ºC
10 Exp. H
0 57ºC
0 50 100 150 200 250 300 350
Time (min)

Graph 5: Flux influence on time for membrane K328 at different temperatures

The increase in temperature also affects the sugar rejection. Graph 6 portrays sugar rejections
coefficients and it can be observed a decrease in rejection when the temperature was increased in
Experiment H.
Experiment I presents higher rejections values due to the lower fluxes registered with membrane
use.
60%
Exp. A
50%
23ºC
40%
Exp. H
R%

30% ~44ºC
20%
Exp. I
10% 57ºC

0%
0 50 100 150 200 250 300
Time (min)

Graph 6: Sugar rejection evolution through time for membrane K328 at different temperatures and 6 bar

Permeate flux evolution through time was represented instead of permeate flux evolution
through sugar concentration in the feed, because concentration was not the aim of these experiments.
However, permeate Brix evolution in time is shown in graph 7 to acknowledge the sugar composition of
the next stage feed. These Brix values are slightly lower than juice feed Brix that is normally between 9
and 11º Brix. According to previous studies, only 3,31% of apple pectins have molecular weight bellow
5.000 Da which means that most of this pectins should be rejected by this membrane.

33
 10

Permeate Brix (º Brix)

Exp. A
8
23ºC
6 Exp. I
57ºC
4 Exp.H
23ºC
2
Exp. H
0 57ºC
0 50 100 150 200 250 300 350
Time (min)

Graph 7: Permeate Brix evolution with time for membrane K328 at different operatory conditions

34
 4.2. RO membrane RO98pHt from ALFA LAVAL

Table 10: RO98pHt membrane from ALFA LAVAL characterization

Membrane Characteristic Data

Manufacturer ALFA LAVAL
Model RO98pHt
Chemistry Thin film composite
Pressure range (bar) 15-40
Temperature range (ºC) 5-60
pH range 2-10
NaCl rejection (%) >98

In RO, by applying a pressure in excess of the osmotic pressure, the solvent is forced, from a
region of high solute concentration, through a membrane, to a region of low solute concentration.
Several experiments were performed to test the best operational conditions of this membrane.
Table 11 resumes these conditions and presents the initial and final Brix obtained in each experiment.

Table 11: Operatory conditions for experiences J to P performed with membrane RO98pHt from ALFA LAVAL

Experiment Exp. J Exp. K Exp. L Exp. M Exp. N Exp. O Exp. P

T (ºC) 28 31 31 30 34 67 68
P (bar) 32 50 50 50 50 50 50
Feed Type Happy 100% 100% 100% 100% 100% K328
days Apfel Apfel Apfel Apfel Apfel permeate
Rauch Spar Spar Spar Spar Spar
Initial Brix 9,9 10 10 9,4 9,9 10,7 9,4
Final Brix 17,5 19,8 20 20,4 19,8 19,1 17,3

In the first attempt with this membrane, Exp. J, the juice was left in the experimental set up for
the next day. In the second day, it was noticed a turbidity in the feed, settled particles and foam at the
surface, that can be visible in Figure 12. The permeate also acquired a white turbidity. The smell of both
the permeate and the rejected had changed probably due to the degradation of organic compounds.
Although the most probable occurrence to have happened was juice fermentation, there was no
decrease in the sugar levels. There are two fermentation processes. The first in low oxygen which results
in hard cider. If the cider is left to ferment in an oxygen rich environment it will result in apple vinegar.
The experiment smell was more similar to vinegar than to alcohol but the pH of 3,46 of the concentrate
pointed to hard cider.

35
 Figure 12: Permeate and retentate image of experiment J

. Experiments K to N were performed in the same operational conditions at 30ºC and 50 bar
with the aim of collecting the retentate for a NF stage. The results obtained are displayed in graph 8
where it is observable the decrease in flux through the feed Brix increase. An exponential tendency was
the most adequate fit to the experimental results. All experiments had similar values and evolution
between themselves.

45 N
40
K
35
30
J (kg/(h.m2))

L
25
M
20
15 Exponential
(N)
10
Exponential
5 (K)

0 Exponential
(L)
9,1 11,1 13,1 15,1 17,1 19,1 21,1
Exponential
Feed Brix (º Brix) (M)

Graph 8: Feed Brix influence on permeate flux for membrane RO98pHt at 50 bar and ambient temperature

It was also tested the membrane response to an increase in temperature until 67ºC. It can be
visible in graph 9, that the initial flux obtained at elevated pressure and temperature is higher than with
lower conditions. However, it decreases faster resuming the same flux values for higher concentrations.
The faster decrease in flux is due to the faster accumulation of rejected solutes in the membrane surface.
Additionally, higher temperatures have the advantage of standing outside the temperature range of
yeast development.

120
Exp. J
100
28ºC/32
J (kg/(h.m2))

80 bar

60 Exp. N
34ºC/50
40 bar
20 Exp. O
0 67ºC/50
10 12 14 16 18 20 bar
Feed Brix (º)

Graph 9: Flux influence on feed Brix of RO98pHt under different operational conditions

36
 Characteristic of reverse osmosis membranes, the rejection coefficients are elevated, above
98% for experiments at 30ºC. With the increase in temperature, rejection suffers a minor decrease
until 96%, visible in graph 10. High sugar rejection coefficients are important since they influence the
amount of sugar “lost” in the permeate.

100% Exp. J
28ºC/32
98%
bar
96%
Exp. N
R%

94% 34ºC/50
bar
92%
Exp. O
90% 67ºC/50
9,1 11,1 13,1 15,1 17,1 19,1 21,1 bar
Feed Brix (º Brix)

Graph 10: Rejection influence on feed Brix of RO98pHt under different operational conditions

The effect of pre-treatment with Ultrafiltration was evaluated with the configuration of figure 13.
Permeate from Ultrafiltration experiments was combined until it was gathered enough volume to feed a
RO stage.

RO-Retentate
Uf- retentate

10 Brix UF-Feed RO- PERMEATE

K328 UF-Permeate RO98pHt
P=5 bar P=50 bar
T=50ºC T=65ºC

Figure 13: Diagram of reverse osmosis with Ultrafiltration pre treatment

In graph 11 it is shown the flux evolution with and without Ultrafiltration pre-treatment for two
consecutive experiments in the same operational conditions. It is obvious the benefit of Ultrafiltration on
flux values that registered an increase of 37%. Figure 14 shows permeate and retentate samples in
which is noticeable changes in the retentate sample colour.

37
 60 RO98pHt with
UF
50

40 RO98pHt
J(kg/(h.m2))

y = 3208x-1,809
30
Potencial
20 (RO98pHt
y = 1550,8x-1,621
with UF)
10
Potencial Figure 14: RO98pHt
0 (RO98pHt ) permeate and retentate with
UF pre treatment
7 12 17 22
Feed Brix (º Brix)

Graph 11: Feed Brix influence on flux evolution with membrane Ro98pHt with and without pre-treatment with UF

Osmotic pressure was determined experimentally with equation 12 through pressure and fluxes
differences as explained in chapter 3.2. The pressure values that match a null flux correspond to the
osmotic pressure values. The graphic representation of these regressions is displayed in graph 12 for
several Brix values.
40 11,1 º Brix
12,4 º Brix
30 13,3 ºBrix
J (kg/(h/m2))

15,2 º Brix
20
16,8 º Brix

10 Linear (11,1 º Brix)

Linear (12,4 º Brix)
0 Linear (13,3 ºBrix)
0 20 40 60 Linear (15,2 º Brix)
-10
ΔP (bar) Linear (16,8 º Brix)

Graph 12: Flux evolution with applied pressure for different Brix

Theoretically, osmotic pressure, was calculated through Van’t Hoff, equation 10, and Dow/Filmtec,
equation 11. Dow/Filmtec equation resulted in higher osmotic values further away from the experimental
results.
These equations required a molecular weight. Fructose and Sucrose molecular weight were used
due to being the components in higher concentrations. An average molecular weight was calculated
with the main components. Van’t Hoff factor of 1 was used since there is no ionization of sugar
components.
The results for Van’t Hoff equation are displayed in graph 13. Graph 14 shows osmotic pressure
calculated with Dow/Filmetec equation. Van’t Hoff equation presents lower osmotic pressure values than
the results obtained with the equation used by Dow/Filmtec. The experimental osmotic pressure
increases considerable more than the theoretically osmotic pressure.

38
 30
Fructose
25
Sucrose
20

Δπ (bar)
15 Average
MW
10 Exp.

0
10 12 14 16 18
Sugar Concentration (ºBrix)

Graph 13: Van’t Hoff osmotic pressure

40
35 Exp.
30
25 Fructose
Δπ (bar)

20
15 Sucrose

10
Average
5
MW
0
10 12 14 16 18
Sugar Concentration (ºBrix)

Graph 14: Dow/Filmtec osmotic pressure

39
 4.3. NF membranes

4.3.1. MPF 34 membrane from KOCH

Table 12: MPF34 membrane characterization

Membrane Characteristic Data

Manufacturer KOCH MEMBRANE SYSTEMS
Model SelRO™ MPF-34
Chemistry Proprietary composite nanofiltration membrane
Pressure range (bar) 14-35
Temperature range (ºC) 40-70
pH range 0-14
MWCO(Da) 200
Rejection NaCl (%) 35
Rejection Glucose/Sucrose (%) 95/97

MPF 34 from KOCH membrane was tested at 29ºC and 32 bar. The temperature chosen was
lower than the one recommended by the supplier since it was desired to observe the membrane
response in more economically favourable conditions with less energy expenses. The operational
conditions resume is represented in table 13.

Table 13: Experimental conditions of Exp. Q with membrane MPF34

Experiment Exp. Q
T (ºC) 29
P (bar) 32
Feed Type Happy days Rauch
Initial Brix 11
Final Brix 13,5

The permeate flux, represented in graph 15, decreases with time and it is lower than the one
obtained with other membranes. The sugar rejection coefficients vary between 94 and 98% which is a
higher value compared with other NF membranes tested.

40
 Flux (kg/h.m2) R%
30 100%
25 95%
J (kg((h.m2)) 90%
20 85%

R%
15 80%
10 75%
70%
5 65%
0 60%
8 9 10 11 12 13 14
Feed Brix (ºBrix)

Graph 15: Feed Brix influence on permeate flux and rejection in membrane MPF 34

The membrane used in this experiment, had been used in other experiments. Even with
cleansing, it could present irreversible fouling, affecting flux values. The membrane exhibited deposits
in its surface noticeable in figure 15. An image of permeate and retentate samples are presented in
figure 16. The retentate has an apple juice characteristic colour while the permeate presents a clear
tone.

Figure 15: MPF 34 membrane after use

Figure 16: MPF 34

permeate and
retentate

4.3.2. NF270 membrane from FILMTEC

Table 14: NF270 membrane from FILMTEC characterization

Membrane Characteristic Data

Manufacturer FILMTECTM Membranes
Model FILMTECTM NF270
Chemistry Polyamide Thin-Film Composite
Maximum Operating Pressure (bar) 41
Maximum Operating Temperature (ºC) 45
pH range 2-11
MWCO(Da) 400
NaCl rejection (%) 50

41
 This membrane was evaluated as a possible second stage, preceded by reverse osmosis.
Retentate from experiences with RO98pHt membrane was collected and fed to a NF270 stage, as
shown in figure 17.

20 Brix NF-RETENTATE
RO-RETENTATE

10 Brix RO-FEED
RO98pHt NF 270
P=50 bar P=32 bar

RO-PERMEATE <0,2
0,8 Brix NF-PERMEATE

Figure 17: Diagram of a reverse osmosis membrane process followed by a nanofiltration membrane

Some problems occurred when the water permeability was measured. It could be observed a
leakage of water out of the system even though all the operational parameters where within the
recommended boundaries suggested by the supplier. Several pieces of membrane were tested with the
same results obtained. The leakage stopped when it was fed concentrated juice to the system, most
likely due to the differences in viscosity between water and apple juice.
The starting Brix in Exp. S, sequential to Exp. R, is lower than the final Brix obtained in Exp R.
This happened most likely, due to residual water present in the module derived from the cleansing of
the system between membranes. In table 15, it is resumed the operational conditions of experiments
performed with membrane NF270.

Table 15: Operational conditions of experiences R and S for NF270 membrane

Experiment Exp. R Exp. S

T (ºC) 28 31
P (bar) 32 32
Feed from RO98 From Exp. R
Initial Brix 17,8 18
Final Brix 19,4 20,3

42
 Graph 16 portrays flux and rejection evolution with the increase in sugar concentration. Sugar
rejection coefficients for this membrane stand in the range of 85 to 90%, lower than with MPF34
membrane due to the highest MWCO of NF270 membrane. Permeate flux has a value of 10 Kg/(h.m2)
for a 18 ºBrix value and decreases until 4 Kg/(h.m2) for a final Brix of 20,3 ºBrix.

12 100%
Flux: Exp.
10 90% R
J (kg/(h.m2))

8 Flux: Exp.
80%

R (%)
S
6
70% Rejection
4 : Exp. R
2 60%
Rejection
0 50% : Exp. S
17,5 18 18,5 19 19,5 20 20,5
Feed Brix (º Brix)

Graph 16: Flux and rejection evolution with feed Brix for NF270 membrane

Figure 18 shows the membrane after use where it can be verified that the membrane suffered
a deposit of particles in its surface that could not be removed with manual washing. Figure 19 shows
permeate and retentate samples. The retentate presents a stronger golden colour and the permeate a
very light yellow tone indicating partial coloured components loss.

Figure 18: NF270 membrane after experiments

Figure 19: Permeate and retentate

samples image with NF270 membrane

43
 4.3.3. MPF36 membrane from KOCH

Table 16: MPF36 membrane characterization

Membrane Characteristic Data

Manufacturer KOCH MEMBRANE SYSTEMS
Model SelRO™ MPF-36
Chemistry Proprietary composite nanofiltration membrane
Pressure range (bar) 15-35
Temperature range (ºC) 40-70
pH range 0-14
MWCO(Da) 1000
Rejection NaCl (%) 10
Rejection Glucose/Sucrose (%) 30/50

Membrane MPF 36 was also evaluated as a secondary stage after RO98pHt membrane. After
first evaluating the behaviour at ambient temperature, Exp. T, the working temperature was increased
until 65ºC. This increase led to a rise in flux when compared with the experiments performed at lower
temperature. Experiments U,W and X were performed in sequential order by freezing the retentate and
using it in the experiment after. All operatory conditions are resumed in table 17.

Table 17: Operational conditions of experiments T,U,W,X and Y with membrane MPF 36

Experiment Exp. T Exp. U Exp. W Exp. X Exp. Y

T (ºC) 27 65 64 65 63
P (bar) 32 32 32 32 32
Feed Type Juice+ Juice+ Exp. U Exp. W K238
Sugar Sugar
Initial Brix 19 18,5 23,1 26,3 8,5
Final Brix 20,7 23,7 26,3 27,9 15,1

Graph 17 shows that the flux evolution follows a potential tendency. The experiment at higher
temperature has an initial higher flux than the one at lower temperature. However this difference
decreases for elevated Brix.

44
 25
Exp. T
27ºC/32 bar
20
Exp. U
65ºC/32 bar
J(kg/(h.m2))

15
Exp. X 65
ºC/32 bar
10
Exp. W 65
ºC/32 bar
5
Potential
(exp. T)
0
17 19 21 23 25 27 29 31 Potential
(Exp. U)
Feed Brix (º Brix)

Graph 17: Flux influence on feed Brix of membrane MPF36

Another alternative studied was the possibility of using this membrane after an UF pre-
treatment. Although the initial flux in this experiment is higher than without pre-treatment, it suffers an
accentuated decrease. Sugar rejection increases with Ultrafiltration. Even though this membrane
presents higher MWCO than NF270 the rejection values vary in the same range. An exponential
tendency was added to graph 18, to help evaluate the effect of Ultrafiltration pre-treatment.

MFF36
160 100%
140 95%
MPF36 with
90%
120 UF
85%
J (kg/(h.m2))

100 80% R% MPF36

R%

80 75%
60 70% R% MPF36
65% with UF
40
60% Exponential(
20 55% MPF36)
0 50% Exponential(
8 13 18 23 28 33 MPF36 with
Feed Brix (º Brix) UF)

Graph 18: Flux influence on concentration of membrane MPF36 with or without pre-treatment

Figure 20 shows the deposits formed in the initially white membrane after use. It is visible the
formation of patterns in its surface.

Figure 20: Membrane MPF36 after use

45
 4.3.4. Nadir membrane from Microdyn Nadir

Table 18: Nadir membrane characterization

Membrane Characteristic Data

Manufacturer MICRODYN NADIR
Model NADIR NP010 P
Chemistry PES
Temperature range (ºC) 5-95
pH range 0-14
Rejection Na2SO4(%) 35-75
Rejection NaCl (%) 10
Water flux (L//m2.h) at 40 bar, 25ºC > 200

Membrane Nadir was tested as a possibility for the first stage of juice concentration. It was
tested at 60ºC and 40 bar as presented in table 19. In graph 19 it can be noticeable that the initial flux
with nadir membrane is higher than with others NF membranes, additionally the decrease in flux is also
less accentuated. Rejection values are high and increase with the progression of the experience.

Table 19: Operational conditions of experiments Z with membrane Nadir

Experiment Exp. Z
T (ºC) 60
P (bar) 40
Feed Type 100% Apfel Spar
Initial Brix 11,4
Final Brix 18

80 100%
70
80% Flux
60 (kg/h.m2)
J (kg/(h.m2))

50 60% R%
R%

40
30 40% Potential
(Flux)
20
20% Linear (R%)
10
0 0%
10 12 14 16 18 20 22 24
Feed Brix (º Brix)

Graph 19: Flux influence on sugar concentration of experience Z with membrane Nadir

46
 4.3.5. DK membrane from GE

Table 20: DK membrane characterization

Membrane Characteristic
Manufacturer GE
Model DK Series
Chemistry Thin-film
Maximum Operating Pressure (bar) 30
Maximum Operating Temperature (ºC) 50
pH range 3-9
MWCO(Da) 150-300
Rejection MgSO4(%) 98

This membrane potential was assessed for the first and second concentration stage. The effect
of UF pre-treatment was also analysed, but due to a pump problem, the experience had to be
prematurely terminated. Table 21 summarizes the operational conditions of the experiences performed
with DK membrane.

Table 21: Operational conditions of experiments AA, AB and AC with membrane DK

Experiment Exp. AA Exp. AB Exp. AC

T (ºC) 59 60 60
P (bar) 32 32 40
Feed Type 100% Apfel Spar 100% Apfel Spar + Sugar UF permeate
Initial Brix 10,4 20,5 7,7
Final Brix 19,5 28,1 11,3

Graph 20 shows that the permeate flux follows a potential tendency with a high initial flux. To
simulate the retentate of RO process, sugar was added to supermarket juice in experience AB.

150 Exp. AB
60ºC 32
J (kg/(h.m2))

bar
100
Exp. AA
60ºC 32
50 bar

Potencial
0 (Exp. AA
60ºC 32
10 15 20 25 30
Feed Brix (º Brix) bar)

Graph 20: Sugar concentration influence on permeate flux levels for experiments AA and AB with DK membrane
47
 Sugar rejections levels, shown in graph 21, vary around 90% decreasing slightly with the
increase of sugar.

100%
Exp. AB
90% 60ºC 32
bar
80%
R%

Exp. AC
70% 60ºC 40
60% bar
Exp. AA
50%
60ºC 32
8 13 18 23 28 bar
Feed Brix (º Brix)

Graph 21: Sugar concentration influence on sugar rejection coefficients for experiments AA, AB and AC with
membrane DK

In spite of being prematurely terminated, the existing UF pre-treated results, portrayed in graph
22, shows a slight increase in in permeate flux values. The initial peak in the graph 22 as an unknown
cause.

140
Exp. AB
120
60ºC 32 bar
100
J (kg/(h.m2))

80
Exp. AC
60
60ºC 40 bar
40
20
Exp. AA
0
60ºC 32 bar
0 100 200 300 400 500
Time (min)

Graph 22: Flux evolution with time with membrane DK with and without UF pre-treatment

48
 4.4. Membrane Comparison

4.4.1. First Stage

To determine the most favourable option of all membranes tested, fluxes and rejection
coefficients evolution were compared.
In graph 23, it can be discernible the evolution of NF membranes MPF34, Nadir and DK and
reverse osmosis membrane RO98pHt. Reverse osmosis membrane was chosen due to the high flux
and high sugar rejection. High rejection levels, portrayed in graph 24, have an important role in the first
stage because all sugar compounds in the permeate are considered “lost” with no possible recovery.

300
R² = 0,9442 R² = 0,9535 MPF34 29ºC 32 bar

R² = 0,8971 R² = 0,9436 Nadir 60ºC 40 bar

J (kg/(h.m2))

200 DK 60ºC 32 bar

RO98pHt 67ºC 50bar

100 Potential(MPF34
29ºC 32bar)
Potential (Nadir 60ºC
40 bar)
Potential (DK 60ºC 32
0 bar)
8 13 18 Potential (RO98pHT
Feed Brix (º Brix) 67ºC 50bar)

Graph 23: Feed Brix influence on permeate flux for first stage membranes

100%
Nadir 60ºC
90% 40 bar

80%
R%

DK 60ºC 32
70% bar

60%
RO98pHt
50% 67ºC 50bar
10 12 14 16 18 20
Feed Brix (º Brix)

Graph 24: Feed Brix influence on sugar rejection coefficients for first stage membranes

49
 4.4.2. Second stage

In the second stage three nanofiltration membranes were evaluated. It can be observed, in
graph 25, that membrane DK presents the best possibility. The membrane MPF36 also poses a
hypothesis and NF270 presents too lower values to be considered. Rejection coefficients were also
analysed in graph 26. The values are similar between each other, with DK membrane presenting the
lowest values. This is desirable due to the lowest difference in osmotic pressure. Additionally the
permeate stream is recycled and compounds are recovered in the first stage.

20
R² = 0,982 NF270
R² = 0,9572 31ºC 32
15 bar
J (kg/(h.m2))

R² = 0,8742

10 DK 60ºC
32 bar
5
MPF36
0 65ºC 32
19 21 23 25 27 29 bar
Feed Brix (º Brix)

Graph 25: Feed Brix influence on flux for second stage membranes

100% DK 60ºC
95% 32 bar

90%
MPF36
R%

85%
65ºC 32
80% bar
75% NF270
70% 31ºC 32
19 21 23 25 27 29 bar
Feed Brix (º)

Graph 26: Feed Brix influence on sugar rejection coefficients for second stage membranes

4.4.3. Mass balance

A final diagram, portrayed in figure 21, can be advanced with the best alternative studied. With
an initial Brix of 10,7º, juice is fed to the first stage membrane, a reverse osmosis membrane at 50 bar
and 65ºC. From this stage a permeate with 0,8º Brix leaves the system while a retentate, now with 20
ºBrix is fed to the second stage, a Nanofiltration membrane DK, at 32 bar and 65ºC. The permeate is
recycled to the initial feed and the retentate leaves the system now concentrated juice with 28,1º Brix.

50
 20 Brix NF-RETENTATE
28,1 B rix
RO-RETENTATE

10 Brix RO-FEED
RO98pHt DK
P=50 bar P=32 bar

RO-PERMEATE <0,2
0,8ºBrix
Brix NF-PERMEATE

4,1 Brix

Figure 21: Final diagram for an apple juice concentration diagram with a first and second stage

Equations 13 and 14 represent the mass balance equations to each of the stages. CF, CR and
CP represent the Brix of the feed, retentate and permeate respectively.

Feed = Permeate + Retentate (13)

𝐶𝐹 . Feed = 𝐶𝑃 . Permeate + 𝐶𝑅 . Retentate (14)

A feed of 100 ton/h was arbitrated and with the Brix of each stream, the amount of water
removed was determined, results can be observed in table 22. In total, 63 736 kg/h are removed which
represents 64% of the initial water.

Table 22: Mass Balance values for the proposed diagram

Global NF Second stage RO First stage

Feed (kg/h) 100 000 54 738 118 474
Permeate (kg/h) 63 736 18 474 63 736
Retentate (kg/h) 36 264 36 264 54 738
BF 10,7 20 9,7
BP 0,80 4,10 0,8
BR 28,1 28,1 20,0

4.5. Conductivity

Even thou there is generally an increase in conductivity with the increase in sugar, adding sugar
does not increase the conductivity of the solution because sugar is a molecule that does not break apart
into ions when dissolved. The responsible for the increase in the conductivity are acids present in
juices[19] and since conductivity is directly proportional to the number of ions present in a unit of volume,
when this volume is reduced maintaining approximately the same number of ions, conductivity
increases. [20]

51
 Reverse osmosis membranes present higher percentages of ion rejection. This is noticeable by
the increase in retentate conductivity values and low conductivity values in permeate in graph 27 and
28.
Conductivity is also influenced by the temperature that affects the mobility of the ions. [21] Even
thou experiments were performed in defined operational conditions that include a design pressure and
temperature, samples analysed had to be cooled down before analyse, due to the measurement
equipment limitations, until 20-30ºC. The conductivities shown below are for experiments with RO98pHt
at 67ºC and 50 bar, DK NF membrane at 60ºC and 32 bar and K328 UF membrane at 57ºC 6 bar.

4 R-
Conductivity (mS/cm)

RO98pHt
3 R-DK(AA)

R-K328
2
Apple
1 Juice 20ºC
Apple
0 Juice 30ºC
8 10 12 14 16 18 20 Apple
Feed Brix (º Brix) Juice 40ºC

Graph 27: Conductivity evolution with feed Brix in retentate samples

3
Conductivity (mS/cm)

P-RO98pHt
2,5
2 P-DK(AA)

1,5
P-K328
1
Apple
0,5 Juice 20ºC

0
0 2 4 6 8 10
Feed Brix (ºBrix )

Graph 28: Conductivity evolution with feed Brix in permeate samples

4.6. pH

pH values are important since the pH has an influence in the taste and in the protection against
micro-organisms[22]. Apple juice is derived from apples which are rich in ascorbic acid also known as
vitamin C. Apple juice also contains acids like folic acid and Pantothenic acid[23].
Apple juice pH varies from 3.35 to 4 [24] concerning the different types of apple used. pH levels
are also affected by temperature and the processes suffered by the juice. Graphs 29 and 30 show pH
levels for retentate and permeate respectively. It is also demonstrated the lower and upper limits typical
for apple juice. Cider productions claim that between 3.2 and 3.8 microbial infection is possible and if
pH 4 is reached flavour problems can also occur. [25] Since most of experimental points are within this
interval, other steps like high temperatures are essential to avoid microbial infections.

52
 DK membrane seems to have good rejection values to acids since pH permeate values are
lower than RO98pHt while K328 shoes practically no change between permeate and retentate pH
values.
4,5
R-
4 RO98pHt
R-DK(AA)
3,5
pH

3 R-K328

2,5 Lower
limit
2
Upper
8 13 18 limit
Feed Brix (º Brix)

Graph 29: pH versus sugar concentration of the feed in the retentate

4,5
P-
RO98pHt
4
P-DK(AA)
3,5
pH

P-K328
3

2,5 Lower
Limit
2 Upper
0 2 4 6 8 10 limit
Feed Brix (º Brix)

Graph 30: pH versus sugar concentration of the feed in the permeate

4.7. Aroma Analysis

Aroma analysis was effectuated by Professor Dr. Erwin Rosenberg from TU Wien University,
according to the process described in chapter 3 of this report. Bellow follows his full conclusions which
are part of the report reproduced in annex. It is also reproduced in figure 22, the table with all the
components identified and respective area percentage. The samples analysed are permeate and
retentate from experiments with membrane RO98pHT at 67ºC/50 bar, DK NF membrane at 60ºC/32
and K328 UF membrane at 57ºC/6bar. The seventh sample analysed corresponds to the non-
concentrated apple juice. The samples were numerated and their identification is resumed in table 23.

Table 23: Sample ID

ID #1 #2 #3 #4 #5 #6 #7
Sample DK- Ret. DK-Perm RO- Ret. RO Perm K328 Ret. K328 Apple
Perm. juice

53
 Sample code Sample 1 Retentate Sample 2 Permeate Sample 3 Retentate Sample 3 Retentate Sample 4 Permeate Sample 5 Retentate Sample 5 Retentate Sample 6 Permeate Apple Juice
Retention
time (min) Compound Name R % Area P %Area P %Area R %Area P %Area R % Area R %Area P % Area J %Area
1,29 O2 X X X
1,41 CO2 X 8,47 X 3,8 X 12,71 X 3,21 X 9,5 X 7,37 X 15 X 0,7 X 22,33
1,47 Acetaldehyde X 1,5 X 0,45 X 1,2 X 0,5 X 6,9 X 1,27
1,55 Ethyl alcohol x 4,66 X 3,2 X 62,69 X 9,48 X 10,9 X 8,65 X 9,8 X 2 X 4,25
1,62 Acethydrazide X 0,6
1,67 Carbohydrazide X 0,9 X 0,72
1,96 Hexane X 1,03 X 1,49 X 1,06 X 0,9 X 0,7 X 1,87
2,04 Ethyl Acetate x 2,9 X 3,9 X 1,07 X 15,4 X 9,32 X 10 X 6,4 X 11,3
2,21 Acetix Acid x 4,16 X 9,7 X 21,32 X 2,85 X 5,2 X 5,4
2,38 1-Butanol x 3,83 X 5,3 X 2,67 X 2,03 X 8,1 X 7,41 X 6,1 X 6 X 1,26
2,61 Acetil(?) acid methyl ester x 2,16 X 2 X 1,6 X 1,3
2,86 Trimethylsilyfluoride x 1,01 X X X
3,1 2-Methyl-1-Butanol x 1,56 X 1,2 X 2,33 X 1,01 X 1,95 X 2,4 X 1,9 X 0,59
3,35 Toluene x X 0,7
3,5 Propenoic acid anhydride x X 2,37
3,81 Hexanal x X 3,3 X 3,49 X 2,8 X 1,1 X 4,62
3,86 Acethydrazide x 2,46 X 8,87 X 9,6
4 Acetic acid butyl ester x 3,35 X 2 X 2,52 X 10,55 X 9,1 X 5,7 X 18,41
4,42 Furfural x X 1,92 X 0,68
4,6 Furan, 2,5-dihydro-2,5-dimethyl x 1,96 X 2,62 X 3,87 X 3,9
4,64 Ethylbenzene X 6,4
4,81 1-Hexanol x 9,76 X 11,5 X 5,93 X 29,8 X 24,73 X 18,3 X 31,5 X 12,57
4,91 2-Methyl-1-butylacetate X X 11,46 X 12,28 X 11,2 X 13,71
5,52 1,3-Dihydroxy 2-propanone X 6,42 X 7,68
6,67 Cyclotetrasiloxane, octamethyl X
6,95 2-Hydroxy-gamma-butyrolactone X X 0,77
6,99 Acetic acid hexylester X 6,65
7,03 1,3- trans Cyclopentanediol X 2,23 X 2,064 X 1,3 X 2,4
7,23 Geranylvinylether X 2
7,69 Benzene , (2-methylpropyl) X 12,8 X 1,44 X 2,6
Cyclopropylcarbinol
8,44 (Hydroxymethylcyclopropane) X 4,49 X 5,7 X 7,79 X 1,27 X 1,6 X 5,1
4H-Pyran-4-1 2,3-dihydro 3,5-
9,14 dihydroxy-6-methyl X 1,67 X 5,39 X 1,63 X 3
9,45 Isotridecanol X 0,5
9,72 Dodecane X 2,56 X X 5,4
Butanoic acid, 3-oxo, 2-
10,16 chloroethylester(??) X 31 X 0,9 X 0,2
Propanoic acid, 3-hydroxy,
11,46 hydrazine X 0,6
Decanedioic acid 3,8-dieoxo
12,61 dimethylester X X 1,05 X 1,8
13,5 Sucrose (??) X 16,52 X 7
Phenol, 2,6-bis/1,1-
13,94 dimethylethyl X X 0,57 X 0,3
15,38 3-Deoxy-d-mannoic lactone X 18,18 X 13,7 X 10,3
1,4-Benzenediol, 2,6.bis-(1,1-
16,01 dimethylethyl) X 0,66
18,78 n-Hexadecanoic acid X 0,97 X 0,28 X 0,35

Figure 22: Aroma analysis

“ The results obtained in the (HS-SPME) measurements of the processed apple juices are
characteristic, although not easy to interpret: many of the compounds detected, in particular the esters
of acetic acid and other low-molecular weight aliphatic acids, are characteristic flavour compounds in
apple juice. They are highlighted in green in Table 1 (figure 22). Other compounds that have been
detected, however have not been highlighted in colour, have either not or only to a lesser extent been
described in literature to be characteristic for apple juice flavour. Substances highlighted in blue in Table
1 (figure 22) are measurement artefacts.
The results are difficult to interpret, as they do not show a clearly observable trend. One can
probably say that the permeate does indeed differ in its volatile compound profile from the retentate;
however, this difference is more a quantitative than a qualitative one: most of the (relevant) volatile
compounds are seen in both, the retentate and the permeate, although in different quantities.
For a better understanding of the results, it has to be pointed out that these are obtained as peak
area values, and that they have been normalized to 100% Peak Area Sum for better comparability.
In the retention time window of tr > 10 min, a number of substances elute whose identity has not
been elucidated in a satisfactory way. Although a suggestion was made in Table 1 (figure 22) for the
most likely compound in each case, some of these suggestions are questionable. Where this is the
54
case, the entries have been marked with one or two question marks (for questionable and very
questionable assignments).
A final comment pertains to the point that the measurements were done from the headspace. This
means that no conclusion can be made about the non-volatile constituents of the apple juice in the
retentate and the permeate. Not only judging from the different colour of retentate and permeate, it
seems very likely that these differ more significantly in composition (e.g. sugar content) than do the
volatile flavour compounds. In case this information is considered relevant, however, other analytical
techniques must be considered. “

Analyse of figure 22 can be difficult. Some components, like acetic acid, that do not appear in the
feed surge in all samples apart from RO98pHt permeate. This components arise most probably due to
chemical and biological reactions that samples suffer during process. This reactions are triggered by air
exposure, temperature variations and storage (samples were frozen after the end of each experience
until an analysis could be done). Formation of CO2 and ethyl alcohol are associated with juice
fermentation and graph 31 shows slightly elevated concentrations for all samples except for K328
membrane permeate and DK permeate.

25
20
% Area

15
10
Ethyl alcohol
5
CO2
0

Graph 31: Ethyl and CO2 expression on permeate and retentate samples

Ignoring the blue components that result from the experimental procedure, setting apart all
components which identification raised questions and focusing on the ones in green, known components
of apple juice, it can be observable in graph 32, that there is no evident differences between permeate
and retentate aroma constitution. UF and NF seam to present the highest similarity between permeate
and retentate, while RO process shows the biggest difference. This results indicate that none of the
membranes are able to reject the main aromatic compounds.
Other alternatives have to be studied to discover the optimal solution for the removal of aromatic
compounds that can be later added to the concentrated apple juice without changing the aromatic and
organoleptic properties.

55
 35
30
25
Area (%)

20
15
10
5
0

NF-R NF-P RO-R RO-P UF-R UF-P Apple Juice

Graph 32: Permeate and Retentate area values for known compounds

56
5. Energy consumption and Saving Estimation
5.1. Membrane Energy Consumption

To establish the quantitative advantage of a hybrid process in relation to an evaporation

process, calculations were made to quantify the energy consumption in each process.
The main source of energy consumption in membrane processes is the high pressure pumps.
The amount of energy necessary to achieve the desired water removal is determined by the volume
flow rate and by the pressure applied (ΔP). This power was calculated with equation 15, where Ep
represents the power, qv the volumetric flow rate and η the pressure piston pump efficiency. This value
varies between 0,5 and 0,8 and a value of 0,8 was chosen for calculations purposes.

qv .∆P
Ep = (15)
η

It was also determined the specific energy consumption per juice (Specific E.C. Juice) by
dividing the previously calculated energy consumption for the hourly feed flow rate, equation16.

𝐸𝑝
𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑒𝑛𝑒𝑟𝑔𝑦 𝑐𝑜𝑛𝑠𝑢𝑚𝑝𝑡𝑖𝑜𝑛 = ⁄𝑄 (16)
𝑣

The scale up for the total energy consumption for the mass balance proposed, is calculated with
equation 17 using the specific energy consumption of juice, the mass rate feed and a juice density of
1 048 kg/m3.

𝑇𝑜𝑡𝑎𝑙 𝐸𝑛𝑒𝑟𝑔𝑦 𝐶𝑜𝑛𝑠𝑢𝑚𝑝𝑡𝑖𝑜𝑛 = 𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝐸. 𝐶. 𝐽𝑢𝑖𝑐𝑒 × 𝐹⁄𝑗𝑢𝑖𝑐𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 17

The results of the membrane process energy consumption calculations are presented in table
24. Reverse osmosis presents a higher energy consumption than nanofiltration due to the higher
working pressure, however as was mentioned before, this stage removes a higher quantity of water
leading to a lower value of energy consumption per cubic meter of water removed.

57
 Table 24: Calculations of membrane energy consumption for a feed of 100 ton/h

Flow Energy Specific

Total energy
Rate ΔP Efficiency Consumption, E.C. Feed
consumption
𝐪𝐯 Ep Juice
kW.h/m3
Units m3/s Pa % W Kg/h
Juice kW
RO98pHt
5,0E-05 4900000 80% 306
50bar,60ºC 1,70 118 474 192,30
DK
5,0E-05 3100000 80% 194
32bar,60ºC 1,08 54 738 56,21
Total 500 2,78 173 212 248,50

5.2. Evaporators Energy Consumption

Traditionally, the final concentration of apple juice in industry is made in a multi-effects

evaporator. The vapour produced in the first effect serves as heating utility in the second effect and so
on as presented in figure 23. In apple juice industry, the evaporators used have between 4 to 6 effects[26].
For calculations purposes, it was selected a 4 effect evaporator with an evaporation rate of 3 kg water/kg
steam [26].

Figure 23: Multi effect evaporator diagram [27]

The minimal energy to evaporate the desired water to be removed, is represented by the thermal
power q, was calculated with the water latent heat, λ, and with the mass flow rate of steam m s, equation
18.

q = ms . λ (18)

The mass flow rate of steam was determined with the evaporation rate and the desired amount
of water to remove. This value, determined by mass balances, depends of the feed, the initial and final
Brix, equation 19.
58
 Water removed = Feed (1 − Initial Brix⁄Final Brix) (19)

The traditional concentration process calculations were made for the single use of evaporators,
with a feed previously arbitrated of 100 ton/h. The traditional process concentrates from 10 to 70º Brix.
In the hybrid process, a membrane multistage concentrates from 10 to 28,1 ºBrix, followed by multi-
effect evaporator that concentrates until 70 ºBrix. The values used and obtained are presented in table
25.

Table 25: Evaporator energy consumption for the traditional and proposed hybrid process

Traditional Process Proposed Hybrid

Process
Feed flow (kg/h) 100 000 36 264
Initial Brix (ºBrix) 10 28
Final Brix (ºBrix) 70 70
Removed water flow (kg/h) 85 714 21 706
Effects 4 4
Evaporation rate (kg water/kg steam) 3 3
Steam flow (kg/h) 25 974 6 578
Water latent heat, λ (kJ/kg) 2 200 2 200
Evaporation heat (kW) 15 873 4 020

5.3. Energy consumption: Design Comparison

To compare the two processes, the percentage of energy saving was determined. Table 26 presents
the values for the purposed process that consists in the sum of the membrane energy consumption and
evaporation consumption from 28,1 until 70º Brix. The calculated value of 73% proves that the purposed
process is more energetic favourable than the traditional one.

Table 26: Membrane and Evaporation energy consumption comparison

Membrane Energy Membrane + Evaporation Evaporation Energy Energy Saving

Consumption (kW) Energy consumption (kW) Consumption (%)
249 249+4 020= 4 268 15 873 73

Translated to the economic field, with the prices of electricity in Portugal and Austria, the energy
saving represents a monetary saving of 1 656€/hour and 1 516 €/hour respectively. Values are
presented in table 27. This calculations are done in a superficially matter only taking into account mass
balances. The values obtained are for a minimal energy consumption ignoring other sources of energy
59
spending. Also this calculations refer to operating costs and do not take into account investment costs
where normally membrane costs top traditional processes. [28]

Table 27: Hybrid Process monetary savings in Portugal and Austria

Price energy in 2014 0,1427 Economic saving in PT

(PT)[29] (€/kWh) (€/h) 1 656
Price energy in 2014 0,1306 Economic saving in AT
(AT)[29] (€/kWh) (€/h) 1 516

To further compare the two designs, the method of the substitution coefficient [30] was calculated.
This coefficient compares traditional operations, based in thermal energy, with new electricity based
operations, like membrane processes. This coefficient is defined “by the ratio between the primary
energy (thermal) saved in the new process with respect to the conventional process and the amount of
electrical energy consumed, relative to the conventional process.” [30]- Equation 20

C1 −C2
CS = (20)
E2 −E1

CS stands for the substitution coefficient while E and C stand for the consumption of electrical
and thermal primary energy respectively. The conventional process, evaporation in this case, is
represented by number 1 while the new hybrid process is assigned the number 2. Taking into
consideration that in Italy a kWh of electrical energy, requires that a power station burn 10.5 MJ of
primary energy from a combustible (oil, gas, coal, etc.), the substitution coefficient is positive for the new
process if CS is greater than 10.5 M J/kWh.

57 143 − 14 471 MJ
CS = = 171 ⁄kW. h
249 − 0
The new hybrid process substation coefficient has a value of 171 MJ/kW.h vastly superior to
10,5 MJ/kW.h contributing to the theory that the new hybrid process is more favourable than the
traditional one.

60
6. Area and Module Configuration

6.1. Membrane Area and Number of modules

Membrane area can be calculated with the average flux obtained in the experiments performed
and with the active area of each membrane. For reverse osmosis, membrane reference RO98PHT-
8038/30 with an active area of 32,9 m 2 was chosen, while for NF membrane, DK8040F1071 model with
29,7 m2 was selected. With the total active area calculated and with known area per module, the number
of modules was calculated and the results summarized in table 28.

Table 28: Membrane area calculations

RO First Stage NF Second Stage

Permeate flow (kg/h) 63 736 18 474
Permeate Flux (kg/h.m2) 43,2 9,9
Total area (m2) 1 476 1 866
2
Area per module (m ) 32,9 29,7
Number of membrane modules 45 63

6.2. First arrangement: equal number of parallel modules

There are distinct installation module configurations normally used.

The first arrangement suggested, starts with pumping the feed that is equally distributed between
the first set of parallel modules. This number of parallel modules is calculated according to the suggested
feed flow rate in the specifications sheets of each membrane. In this arrangement the number of
consecutive modules is equal in each set of parallel modules, and can be calculated dividing the total
membrane modules by the parallel modules. Since it is not a whole number, there is a surplus that will
be positioned after all consecutive modules. Figure 24 shows a small example of this type of module
arrangement. Blue represents RO membranes and orange NF membranes.

Figure 24: Diagram of the first module arrangement

61
 Concentrated juice is fed to the second NF stage which is designed in the same way although,
the total number of membranes is different due to different area requirements. The permeate is removed
in the first stage. In the second one, DK NF membrane, the permeate is recirculated to the RO feed.

Table 29: First module arrangement

Feed flow per Parallel Modules Consecutive Plus

module (L/s) Modules
First Stage: RO 3 11 4 1
Second Stage: NF 3 5 12 3

6.3. Second Arrangement: Tapered Design

Figure 25: Diagram of second module arrangement

Tapered design is the name usually given to this arrangement, portrayed in figure 25, due to the
progressive decreasing number of parallel modules. Total membrane area, number of modules and
membranes chosen are the same as in the previous arrangement.
The total number of modules per parallel set was calculated with mass balances to each module
and supposing an average permeate flux, equal for all modules. Results are portrayed in table 30. This
rough approximations was necessary due to the lack of data to establish profiles within the membrane.
Retentate and permeate follow the same route as in the first arrangement.

62
Table 30: First and Second stage consecutive modules for each parallel module

First Stage: Second Stage: DK

RO
Parallel modules # Consecutive # Consecutive
Modules Modules
#1 11 5
#2 10 5
#3 9 5
#4 8 5
#5 7 5
#6 - 5
#7 - 5
#8 - 5
#9 - 4
#10 - 4
#11 - 4
#12 - 4
#13 - 4
#14 - 3
Total 63

63
7. Conclusions and further work

The membrane with higher flux values and higher sugar rejection levels was a reverse osmosis
membrane. The reverse osmosis membrane from Alfa Laval, RO98pHt with operatory conditions of
57ºC and 50 bar concentrated apple juice from 9,7º to 20º Brix with an average flux of 43 kg/(h.m2) and
a rejection around 98%. For the second stage, nano filtration membrane DK from GE obtained the
highest flux and lowest rejection at 60ºC and 32 bar with an average flux of 10 kg/(h.m2) and a rejection
of 80%.
Experimental values of osmotic pressure show that higher Brix values could be obtained. The low
scale of the experimental unit makes it hard to evaluate membranes response to higher concentrations.
Even thou the maximum concentration with membranes achieved was far from the 65º Brix
desired for the industry, the amount of water removed from 10 to 28 ºBrix, represents 63% of water.
This represents energy savings of 71%.
Ultrafiltration pre-treatment increases flux values in posterior stages but UF rejected some key
aromatic components. A membrane with a higher MWCO should be evaluated to remove only colloidals
components.
Exposition to air and low temperatures foments the fermentation of the juice in the system. Yeast
need an oxygen source and a substrate like sugar. If the access to an oxygen supply is limited
fermentation will be more difficult. This can be accomplished with sealed experimental set up. A
temperature increase in all process to a value above 50ºC, outside yeasts range, will also limit the
fermentation process and increase flux although, maintain the working temperature it is difficult due to
the heat exits out of the system and duo to the increase in temperature provoked by the pump and the
increasingly low level in the feed tank.
The removal of aromatic compounds using membranes has proved not to be successful. Further
studies should be effectuated to accomplish the removal of this components to avoid their loss and
degradation.
Water removed from the process can be used can be used to wash apples in the first steps of the
production process or subjected to further procedures to recover sugar and aromatic components.

64
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68
Annex

I. Flavour Profiling of Apple Juice Samples After Processing by Membrane

Separation Techniques

69
 Flavor Profiling of Apple Juice Samples
After Processing by Membrane Separation
Techniques

Commissioned by:
Mariana Sousa
Institute of Chemical Engineering
Vienna University of Technology
Getreidemarkt 9/166, 1060 Vienna, Austria
Tel: +43 1 58801/166227
Fax: +43 1 58801/16699
E-Mail: Mariana.Sousa@ist.utl.pl

E. Rosenberg
Technische Universität Wien
Institut für Chemische Technologien und Analytik
Instrumentelle Analytische Chemie
Getreidemarkt 9/164 AC
A-1060 Wien, Österreich
Tel. 01/58801-15190
Email: erosen@mail.zserv.tuwien.ac.at

Report 2015/24 ER
August 2015
1. Aim of Investigation
Six apple juice samples, obtained as the permeate and retentate, respectively, of membrane-
separation processed apple juice were to be characterized in terms of their favor profile.

2. Description of Samples
Six samples were handed over by Ms. Sousa on 03/08/2015 in frozen state, representing the
permeates and the retentates of three experiments in which apple juice was pre-concentrated by
different membrane separation procedures. All permeates were colorless, while all retentates had the
same color as the original apple juice which was also provided as a reference.
The samples were labeled as follows:
Sample #1 (Retentate):
OK → 20 brix 32 bar, 65°C 10/06/15 MS
Sample #2 (Permeate):
OK → 20 brix 32 bar, 65°C 10/06/15 MS
Sample #3 (Retentate):
RO 98, pH6 50 bar, 70°C 04/05/15 MS
Sample #4 (Permeate):
RO 98, pH6 50 bar, 70°C 04/05/15 MS
Sample #5 (Retentate):
R328 60°C, 6 bar 12/6/15 MS
Sample #6 (Permeate):
R328 60°C, 6 bar 12/6/15 MS
Apple juice (not processed):
from a local supermarket.
The samples were measured in the period 06.-13.08.2015

3. Analytical Methods
To characterize the flavor profile of the apple juice samples, headspace solid phase microextraction
(SPME) measurements were undertaken which allow the characterization of the volatile compounds
emitted from the sample.
Solid phase micro extraction:
10 ml of each sample were transferred into 15 ml screw cap vials with mininert valves and
equilibrated. Manual SPME holder with Carboxen/PDMS fibre (85 µm). Extraction for 15 min from the
sample headspace at room temperature (25°C) with stirring.

GC/MS Analysis:
Thermo Scientific GC/MS Ultra with DSQ II Quadrupole-MS and AS 2000 autosampler.
Column: Restek Rtx 5 MS, 30 m x 0.25 mm, 0.25 µm df.
Oven program: 40°C (1 min) → 10°C/min → 250°C (8 min). Total run time: 30 min.
Injection-/Desorption temperature: 250 °C. Injection mode: CT Splitless.
Column flow: 1.5 ml/min constant flow mode.
MS: Transfer Line: 250°C. Ion Source: 200°C. Data acquisition start time: 0.00 min. Scan mode: Full
Scan. Scan range: m/z 29-300.

4. Results and Discussion

In the following figures, the chromatograms of the different samples are presented, and the results of
peaks detected summarized in Table 1.

Seite 2 von 9
4.1 Apple Juice

RT: 0.00 - 30.02

1.41 NL:
100 2.34E8
TIC F: MS
95 15080606

90

85

80

75

70

65

60
Relative Abundance

55

50 3.96
2.03
45

40 4.89

35

30

25

20

15

10 3.78 6.99
2.40
5
5.22 7.48 9.45 11.46 13.66 16.95 18.85 21.22 24.08 26.80 29.20
0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Figure 1: GC/MS chromatogram of the untretaed apple juice sample.

Seite 3 von 9
4.2 Samples processed in experiment OK → 20 brix / 32 bar, 65°C / 10/06/15 MS
Retentate (#1)
RT: 0.00 - 30.03
1.41 NL:
100 5.09E7
TIC F: MS
95 15081203

90

85

80

75

70

65 1.55

60
Relative Abundance

2.21
55

50

45
2.38
40

35 4.81 4.91
4.00
9.72
30
2.61
25 13.39

20
15.38
15 5.52
5.80 8.44
15.74
12.61
10 16.25 18.78
19.08 21.73 24.15 25.31 29.99
5

0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Pemeate (#2)
RT: 0.00 - 30.02
9.72 NL:
100 4.61E7
TIC F: MS
95 15081201_
150812155
90 836

85

80

75

70 1.38

65

60 2.25
Relative Abundance

55

50

45

40
7.65
35
2.42
30

25
4.85
20 2.67
2.94
15
8.48
10 5.89 13.29
11.46 13.66 15.37
5 16.40 18.82 20.72 21.82 25.84 28.07 29.98
0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Figures 2 and 3: GC/MS chromatograms of the retentate and permeate resulting from experiment
OK → 20 brix / 32 bar, 65°C / 10/06/15 MS

Seite 4 von 9
4.3 Samples processed in experiment RO 98, pH6 / 50 bar, 70°C / 04/05/15 MS
Retentate (#3)
RT: 0.00 - 30.01
1.55 NL:
100 2.23 7.26E7
TIC F: MS
95 15081307

90

85

80

75

70

65

60
Relative Abundance

55

50

45

40

35

30 2.39
3.81
25
4.81

20 4.92 9.11
5.46
15
8.18 8.40
15.38
6.93 12.60
10 10.13 15.77
13.32
16.33 18.78
5 21.65 23.04 24.28 27.76
27.96
0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Pemeate (#4)
RT: 0.00 - 30.02
2.04 NL:
100 3.58E7
TIC F: MS
95 15081304

90

85 1.55

80

75

70

65

60
Relative Abundance

55

50

45
4.82
40
4.01
35

30
4.93
25 9.73

20

15
7.69
7.23
10 9.45 11.47 12.64 15.64 19.42 20.43 22.87 24.04 26.09 28.68
5

0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Figures 4 and 5: GC/MS chromatograms of the retentate and permeate resulting from experiment
RO 98, pH6 / 50 bar, 70°C / 04/05/15 MS

Seite 5 von 9
4.4 Samples processed in experiment R328 / 60°C, 6 bar / 12/6/15 MS
Retentate (#5)
RT: 0.00 - 30.03
1.40 NL:
100 4.88E7
TIC F: MS
95 15081308

90

85 1.55

80 2.04

75

70

65

60
Relative Abundance

4.79
55

50
2.38
45

40 4.91
3.99

35

30

25

20

15

10
5.23 8.51
9.29 13.65 13.96 14.45 16.02 17.96
5
19.13 20.13 22.74 23.66 26.09 28.76
0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Pemeate (#6)
RT: 0.00 - 30.01
1.49 NL:
100 3.42E7
TIC F: MS
95 15081306
4.77
90

85

80
2.00
75

70

65

60
Relative Abundance

4.89
2.34
55

50

45
3.99
40

35

30
2.61
25

20
12.61 15.26
7.04 8.48
15 9.18
15.63
10 12.07
16.49 18.80
21.76 23.08 23.96 25.73 28.65
5

0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Time (min)

Figures 6 and 7: GC/MS chromatograms of the retentate and permeate resulting from experiment
R328 / 60°C, 6 bar / 12/6/15 MS

Seite 6 von 9
Table 1: Overview of the individual compounds identified in the headspace-SPME measurements of the original and the processed apple juice samples.
Compounds highlighted in green are considered characteristic for apple juice flavor. Compounds highlighted in blue are artefacts occuring in the measurement
process (column bleed, introduction of air).

Sample code Sample 1 Sample 2 Sample 3 Sample 3 Sample 4 Sample 5 Sample 5 Sample 6 Apple
Retentate Permeate Retentate Retentate Permeate Retentate Retentate Permeate Juice
File name 1508120 15081201_150 15081303 15081307 15081304 15081305 15081308 15081306 1508060
3 81201155836 6
Retention Compound Name R % P % Area P % Area R % P % Area R % R % P % Area J % Area
time (min) Area Area Area Area
1,29 O2 X X X
1,41 CO2 X 8,47 X 3,8% X 12,71 X 3,21 X 9,5% X 7,37 X 15,0% X 0,7% X 22,33
1,47 Acetaldehyde ? X 1,5% X 0,45 X 1,2% X 0,5% X 6,9% X 1,27
1,55 Ethyl alcohol X 4,66 X 3,2% X 62,69 X 9,48 X 10,9% X 8,65 X 9,8% X 2,0% X 4,25
1,62 Acethydrazide ?? X 0,6%
1,67 Carbohydrazide ?? X 0,9% X 0,72
1,96 Hexane X 1,03 X 1,49 X 1,06 X 0,9% X 0,7% X 1,87
2,04 Ethyl acetate X 2,90 X 3,9% X 1,07 X 15,4% X 9,32 X 10,0% X 6,4% X 11,30
2,21 Acetic acid X 4,16 X 9,7% X 21,32 X 2,85 X 5,2% X 5,4%
2,38 1-Butanol X 3,83 X 5,3% X 2,67 X 2,03 X 8,1% X 7,41 X 6,1% X 6,0% X 1,26
2,61 Acetic (?) acid methyl ester X 2,16 X 2,0% X 1,6% X 1,3%
(more likely: Propyl acetate)
2,86 Trimethylsilylfluoride X 1,01 X X X
3,10 2-Methyl-1-butanol X 1,56 X 1,2% X 2,33 X 1,01 X 1,95 X 2,4% X 1,9% X 0,59
3,35 Toluene X X 0,7%
3,50 Propenoic acid anhydride ? X X 2,37
3,81 Hexanal X X 3,3% X 3,49 X 2,8% X 1,1% X 4,62
3,86 Acethydrazide ?? X 2,46 X 8,87 X 9,6%
4,00 Acetic acid butyl ester X 3,35 X 2,0% X 2,52 X 10,55 X 9,1% X 5,7% X 18,41
4,42 Furfural X X 1,92 X 0,68
4,6 Furan, 2,5-dihydro-2,5-dimethyl X 1,96 X 2,62 X 3,87 X 3,9%
4,64 Ethylbenzene X 6,4%
4,81 1-Hexanol (?) X 9,76 X 11,5% X 5,93 X 29,8% X 24,73 X 18,3% X 31,5% X 12,57
4,91 2-Methyl-1-butylacetate X X 11,46 X 12,28 X 11,2% X 13,71
5,52 1,3-Dihydroxy 2-propanone X 6,42 X 7,68
6,67 Cyclotetrasiloxane, octamethyl X

Seite 7 von 9
 6,95 2-Hydroxy-gamma-butyrolactone X X 0,77
6,99 Acetic acid. hexylester X 6,65
7,03 1,3- trans Cyclopentanediol X 2,23 X 2,064 X 1,3% X 2,4%
7,23 Geranylvinylether X 2,0%
7,69 Benzene, (2-methylpropyl) X 12,8% X 1,44 X 2,6%

8,44 Cyclopropylcarbinol X 4,49 X 5,7% X 7,79 X 1,27 X 1,6% X 5,1%

(Hydroxymethlycyclopropane)

9,14 4H-Pyran-4-one 2,3-dihydro, 3,5- X 1,67 X 5,39 X 1,63 X 3,0%

dihydroxy-6-methyl
9,45 Isotridecanol X 0,5%
9,72 Dodecane X 2,56 X X 5,4%
10,16 Butanoic acid, 3-oxo, 2- X 31,0% X 0,90 X 0,2%
chloroethylester (??)
11,46 Propanoic acid, 3-hydroxy, X 0,60
hydrazide
12,61 Decanedioic acid 3,8-dieoxo X X 1,05 X 1,8%
dimethylester
13,5 Sucrose (??) X 16,52 X 7,0%
13,94 Phenol, 2,6-bis/1,1-dimethylethyl) X X 0,57 X 0,3%
15,38 3-Deoxy-d-mannoic lactone X 18,18 X 13,70 X 10,3%
16,01 1,4-Benzenediol, 2,6.bis-(1,1- X 0,66
dimethylethyl
18,78 n-Hexadecanoic acid X 0,97 X 0,28 X 0,35

The identification of peaks where the compound name is followed by one (?) or two (??) question marks is questionable or very questionable.

Seite 8 von 9
The results obtained in the (HS-SPME) measurements of the processed apple juices are
characteristic, although not easy to interpret: Many of the compounds detected, in particular the esters
of acetic acid and other low-molecular weight aliphatic acids, are characteristic flavor compounds in
apple juice. They are highlighted in green in Table 1. Other compounds that have been detected,
however have not been highlighted in colour, have either not or only to a lesser extent been described
in literature to be characteristic for apple juice flavor. Substances highlighted in blue in Table 1 are
measurement artefacts.
The results are difficult to interpret, as they do not show a clearly observable trend:
One can probably say that the permeate does indeed differ in its volatile compound profile from the
retentate; however, this difference is more a quantitative than a qualitative one: Most of the (relevant)
volatile compounds are seen in both, the retentate and the permeate, although in different quantities.
For a better understandig of the results, it has to be pointed out that these are obtained as peak area
values, and that they have been normalized to 100% Peak Area Sum for better comparability.
In the retention time window oft tr > 10 min, a number of substances elute whose identity has not been
elucidated in a satisfactory way. Although a suggestion was made in Table 1 for the most likely
compound in each case, some of these suggestions are questionable. Where this is the case, the
entries have been marked with one or two question marks (for questionable and very questionable
assignments).
A final comment pertains to the point that the measurements were done form the headspace. This
means that no conclusion can be made about the non-volatile constituents of the apple juice in the
retentate and the permeate. Not only judging from the different color of retentate and permeate, it
seems very likely that these differ more significantly in composition (e.g. sugar content) than do the
volatile flavor compounds. In case this information is considered relevant, however, other analytical
techniques must be considered.

Wien, 30.08.2015 Prof. Dr. Erwin Rosenberg

Seite 9 von 9
II. Membrane Specification Sheets
 Fact Sheet

DK Series
Industrial High Rejection Nanofiltration Elements
The D-Series family of proprietary thin-film nanofil- Spacer Active area Part
Model Outer wrap
tration membrane elements is characterized by an mil ft2 (m2) number
(mm)
approximate molecular weight cut-off of 150-300 DK2540C1076 30 (0.76) 28 (2.6) Cage 1206918

Dalton for uncharged organic molecules. Divalent DK2540C1077 50 (1.27) 18 (1.6) Cage 1206919
and multivalent anions are preferentially rejected DK2540F1072 30 (0.76) 28 (2.6) Fiberglass 1206925
by the membrane while monovalent ion rejection is DK2540F1073 50 (1.27) 18 (1.6) Fiberglass 1206926
dependent upon feed concentration and composi- DK4040C1024 30 (0.76) 98 (9.1) Cage 1206945

DK4040C1025 50 (1.27) 65 (6.0) Cage 1206946

DK4040F1020, Stinger 30 (0.76) 98 (9.1) Fiberglass 3050075

DK4040F1021, Stinger 50 (1.27) 65 (6.0) Fiberglass 3050073

membrane systems to operate at feed pressures
DK8040C-30D 30 (0.76) 347 (32.1) Cage 1206978
below those of RO systems.
DK8040C-50P 50 (1.27) 270 (25.1) Cage 1206979

DK8040F1001 30 (0.76) 390 (36.2) Fiberglass 1206993

DK8040F1002 50 (1.27) 272 (25.3) Fiberglass 1206994

sodium chloride diafiltration and metals recovery.
DK8040F1071 30 (0.76) 320 (29.7) Fiberglass 1206997
Table 1: Element Specification

Membrane D-Series, Thin-film membrane (TFM*)

Average
Minimum MgSO4
Model permeate flow rejection 1,2
gpd (m3/day)1,2

DK2540C1076 560 (2.1) 98%

DK2540C1077 350 (2.3) 98%

Figure 1: Element Dimensions Diagram – Female
DK2540F1072 540 (2.0) 98%

DK2540F1073 340 (1.3) 98%

DK4040C1024 2,000 (7.6) 98%

DK4040C1025 1,300 (4.9) 98%

DK4040F1020, Stinger 2,000 (7.6) 98%

DK4040F1021, Stinger 1,300 (4.9) 98%

DK8040C-30D 6,900 (21.1) 98%

Figure 2: Element Dimensions Diagram – Male, Stinger
DK8040C-50P 5,400 (20.4) 98%

DK8040F1001 7,800 (30.0) 98%

DK8040F1002 5,400 (20.4) 98%

DK8040F1071 6,400 (24.2) 98%

1 Average salt rejection after 24 hours operation.
Individual flow rate may vary ±25%
2 Testing conditions: 2,000ppm MgSO solution at 110psi (760kPa) operating
4
pressure, 77 °F (25°C), 15 % recovery.

Contact us for GE membranes, Purtrex, Hytrex, Aquatrex, RO Save Zplex filters.

www.gemembranes.com
Find a contact near you by visiting www.ge.com/water and clicking on “Contact Us” .
www.bigmembrane.com
©2010, General Electric Company. All rights reserved.
www.codelinehousings.com
www.easternro.com
910-612-6700
AM-FSpwDKSeires_EN.doc Apr-10
Table 2: Dimensions and Weight Table 3: Operating and CIP parameters

Dimensions, inches (cm) Boxed Typical Operating Flux 5 - 20 GFD (8 – 34 LMH)

Model1 Maximum Operating Pressure 600psi (4,137kPa) if T<95°F (35°C)
Weight
A B2 C3 435psi (3,000kPa) if T>95°F (35°C)
lbs (kg)
Maximum Temperature Continuous operation: 122°F (50°C)
40.0 0.75 2.4 4 Clean-In-Place (CIP): 104°F (50°C)
DK2540C1076 (1.90) OD (6.1) (1.8)
(101.6)
pH Range Continuous operation: 3-9
0.75 2.4 4 Clean-In-Place (CIP): 2-10.5
40.0
DK2540C1077 (1.90) OD (6.1) (1.8)
(101.6) Maximum Pressure Drop Over an element: 15psi (103kPa)
0.75 2.4 4 Per housing: 60psi (414kPa)
40.0 (1.90) OD (6.1) (1.8)
DK2540F1072 Chlorine Tolerance 500 ppm hours,
(101.6)
0.75 2.4 4 dechlorination recommended
40.0 (1.90) OD (6.1) (1.8)
DK2540F1073
(101.6) 0.625 3.9 9
(1.59) (9.9) (4.1)
40.0
DK4040C1024
(101.6) 0.625 3.9 9
(1.59) (9.9) (4.1)
40.0
DK4040C1025
(101.6) 0.75 3.9 9
(1.9) (9.9) (4.1)
40.0
DK4040F1020, Stinger 0.75 3.9 9
(101.6)
(1.9) (9.9) (4.1)
40.0 1.125 7.9 29
DK4040F1021, Stinger
(101.6) (2.86) (20.1) (13.2)

40.0 1.125 7.9 29

DK8040C-30D
(101.6) (2.86) (20.1) (13.2)

40.0 1.125 7.9 29

DK8040C-50P (2.86) (20.1) (13.2)
(101.6)
1.125 7.9 29
40.0 (2.86) (20.1) (13.2)
DK8040F1001
(101.6)
1.125 7.9 29 (13.2)
40.0 (2.86) (20.1)
DK8040F1002
(101.6)

40.0
DK8040F1071
(101.6)
1 Theseelements are dried then bagged before shipping.
2Internaldiameter unless specified OD (outside diameter).
3The element diameter (dimension C) is designed for optimum performance in GE

pressure vessels. Other pressure vessel dimension and tolerance may result in
excessive bypass and loss of capacity.
Page 2 Fact Sheet
HpHT HFK-328 FOOD & DAIRY UF ELEMENTS
High pH and Temperature Cleanable Ultrafiltration Spiral Element Series
PRODUCT Membrane Chemistry: Proprietary semi-permeable polyethersulfone (PES)
Membrane Type: HpHT HFK-328 with observed separation range of 5,000 Daltons
DESCRIPTION Construction: Sanitary spiral wound with net outer wrap
Regulatory Status: Compliant with US FDA CFR Title 21, EC Reg. No. 1935/2004, and EU
Reg. No. 10/2011
Options: Element Diameter: 6.4 or 8.0
Feed Spacer: N (31 mil), V (46 mil) or H (62 mil)
Outer wrap: Controlled (e.g. NYV) or trimmable (e.g. NYT)

Koch Model Feed Spacer Active Membrane Area

SPECIFICATIONS Part Number ft2 (m2)
0757611 HpHT 6438-K328-VYV 46 mil 171 (15.9)

OPERATING & Typical Operating Pressure: 30 - 120 psi (2.1 - 8.3 bar)
Operating Temperature Range: 41 - 140°F (5 - 60°C)
DESIGN Cleaning Temperature Range: 105 - 185°F (40 - 85°C)
INFORMATION* Allowable pH - Continuous Operation: 2.0 - 10.0
Allowable pH - Clean-In-Place (CIP): 1.8 – 12.5
Design Pressure Drop below 140°F (60°C):
Pressure Drop Per Element: N spacer: 12-15 psi (0.8-1.0 bar)
V spacer: 15-20 psi (1.0-1.4 bar)
H or F spacer: 15-25 psi (1.0-1.7 bar)
Pressure Drop Per Vessel (3 in series): N spacer: 36-45 psi (2.5-3.1 bar)
V spacer: 45-60 psi (3.1-4.1 bar)
H or F spacer: 45-75 psi (3.1-5.2 bar)
Pressure Drop Per Vessel (4 in series): N spacer: 48-60 psi (3.3-4.1 bar)
V spacer: 60-68 psi (4.1-4.7 bar)
Maximum Pressure Drop above 140°F (60°C): 10 psi (0.7 bar) per element for N and V spacers
15 psi (1.0 bar) per element for H spacer
* Consult KMS Process Technology Group for specific applications.

NOMINAL
DIMENSIONS

Model A B C
inches (mm) inches (mm) inches (mm)
HpHT 6438-K328 38.0 (965) 6.4 (162) 1.138 (28.9)
 HpHT FOOD & DAIRY UF ELEMENTS

Membrane Characteristics:  Sanitizing should be done only after a complete cleaning

 The membrane used in these modules consists of a
semipermeable polyethersulfone (PES) layer on a
polyolefin backing material.
 Pure water flux of these HpHT HFK328 membranes is 1.0-
2.2 gfd/psi (24-53 l/m2/h/bar) at 77°F (25°C).
Operating Limits:
 Operating Pressure: Maximum operating pressure is 140
psi (9.7 bar).
 Permeate Pressure: Permeate pressure should not
exceed baseline (concentrate) pressure at any time
(including online, off-line and during transition). Reverse
pressure will damage the membrane.
 Differential Pressure: The maximum differential pressure
per element is listed in the front of this document, including
design values for multi-element housings. Maximum
differential pressure per element at temperature higher than
140°F (60°C) is 10 psi (0.7 bar) for all feed spacers.
 Temperature: Maximum operating temperature is 140°F
(60°C); maximum cleaning temperature is 185°F (85°C).
 pH: Allowable range for continuous operation is 2.0 to 10.0.
Allowable pH range for cleaning is 1.8 to 12.5.
Water Quality for Cleaning & Diafiltration:
 Turbidity and SDI: Maximum feed turbidity is 1 NTU.
Maximum feed SDI is 5.0 (15-minute test).
 Guidelines: Please refer to the KMS “Water Quality
Guidelines for CIP and Diafiltration” for more detailed
information.
Chemical Exposure:
 Chlorine: Exposure of HpHT membrane to free chlorine or
other oxidizing agents such as permanganate, ozone,
bromine and iodine is not recommended.
 Cleaning and sanitizing limits for chemical concentrations,
pH, temperature and exposure time must be observed in
order to achieve maximum useful module life and to
maintain the warranty.
 Iron or other catalyzing metals in the presence of free
chlorine or hydrogen peroxide will accelerate membrane
degradation.
cycle and with water of acceptable quality - refer to
cleaning instructions and feedwater quality technical
bulletins.
Cationic Polymers and Surfactants:
PES membranes may be irreversibly fouled if exposed to
cationic (positively charged) polymers or surfactants. Exposure
to these chemicals during operation or cleaning is not
recommended and will void the warranty.
Lubricants:
For module installation, use only water or glycerin to lubricate
seals. The use of petroleum or vegetable-based oils or
solvents may damage the module and will void the warranty
Supplemental Technical Bulletins:
 Water Quality Guidelines for CIP and Diafiltration
 HpHT Element Cleaning Procedures
Service and Ongoing Technical Support:
Koch Membrane Systems (KMS) has an experienced staff of
professionals available to assist end-users and OEM’s for
optimization of existing systems and support with the
development of new applications. Along with the availability of
supplemental technical bulletins, KMS also offers a complete
line of KOCHKLEEN® membrane pretreatment, cleaning and
maintenance chemicals.
KMS Capability
KMS is the leader in crossflow membrane technology,
manufacturing reverse osmosis, nanofiltration, microfiltration,
and ultrafiltration membranes and membrane systems. The
industries we serve include food, dairy and beverage,
semiconductors, automotive, water and wastewater, chemical
and general manufacturing. KMS adds value by providing top
quality membrane products and by sharing our experience in
the design and supply of thousands of crossflow membrane
systems worldwide.

The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any warranty or guarantee of performance. We
assume no responsibility, obligation or liability for results obtained or damages incurred through the application of the information contained herein. Refer to Standard Terms
and Conditions of Sale and Performance Warranty documentation for additional information.

Koch Membrane Systems, Inc., www.kochmembrane.com

Corporate Headquarters: 850 Main Street, Wilmington, Massachusetts 01887-3388, US, Tel. Toll Free: 1-888-677-5624, Telephone: 1-978-694-7000, Fax: 1-978-657-5208
European Headquarters: Koch Chemical Technology Group Ltd., Units 3-6, Frank Foley Way, Stafford ST16 2ST, GB, Telephone: +44-178-527-2500, Fax: +44-178-522-3149
• Aachen DE • Lyon FR • Madrid ES • Milan IT • Wijnegem BE • Beijing & Shanghai CN • Mumbai & New Delhi IN • Melbourne & Sydney AU • Singapore • Sao Paulo BR • Dubai UAE •
For related patent and trademark information, visit www.kochmembrane.com/legal
Koch Membrane Systems, Inc. is a Koch Chemical Technology Group, LLC company.
© 2015 Koch Membrane Systems, Inc. All rights reserved worldwide. 01/15 Rev 15
 NADIR® NP010 P
- Nanofiltrationsmembran / Membrane for Nanofiltration -
Datenblatt / Data Sheet

Membrandaten / Membrane data

Membranmaterial / Membrane material PES
Trägermaterial / Backing material PE/PP
1)
Wasserfluss / Water flux [l/(m²h)] > 200
1)
Rückhalt / Rejection Na2SO4 [%] 35 - 75
Dicke / Thickness [µm] 210 - 250
1)
Testbedingungen: 40 bar, 20 °C, Rührzelle (700 U/min)
Test conditions: 40 bar, 20 °C, stirred cell (700 rpm)

Zulässige Betriebsbedingungen / Allowable operating conditions

pH-Bereich / pH range 0 - 14
Temperaturbereich / Processing temperature [°C] 5 - 95

Hauptanwendungsbereich / Main application

Säure/Lauge-Aufbereitung / Acid/Caustic Preparation

Wichtigste Märkte / Main markets

Metall, Chemie / Metal, Chemical Industry

MICRODYN-NADIR behält sich das Recht vor,

Angaben ohne vorherige Ankündigung
anzupassen.
Lenntech
We reserve the right to change specifications info@lenntech.com Tel. +31-152-610-900
without prior notification.
www.lenntech.com Fax. +31-152-616-289
D_NP010P_V1_01
 KMS FLAT SHEET MEMBRANE SAMPLES
Flat Sheet Membrane Samples for Feasibility Tests

MEMBRANE HRX™: High Rejection RO membrane

SR3D™: NF membrane, 200 Dalton MWCO
TYPE
SelRO™ MPF-34: Acid/Base Stable NF membrane, 200 Dalton MWCO
SelRO™ MPF-36: Acid/Base Stable NF membrane, 1,000 Dalton MWCO
HFK-328: Polyethersulfone UF membrane, 5K Dalton MWCO
HFK-131: Polyethersulfone UF membrane, 10K Dalton MWCO
HFM-180: PVDF UF membrane, 100K Dalton MWCO
HFM-183: PVDF Positive charge UF membrane, 100K Dalton MWCO
MFK-618: Polyethersulfone MF membrane, 0.1 micron pore size
MFK-603: Polyethersulfone MF membrane, 0.1 micron pore size, high temperature operation

PART Part Number Model Membrane Dimensions

NUMBERS 8150001 HRX™ 40” x 12”
8150002 SR3D™ 40” x 12”
AND
0770002 SelRO™ MPF-34 18” x 18”
DIMENSIONS 0770007 SelRO™ MPF-36 18” x 18”
0030896 HFK-328 18” x 18”
0030880 HFK-131 18” x 18”
0030887 HFM-180 18” x 18”
0030889 HFM-183 18” x 18”
0030898 MFK-618 18” x 18”
0030893 MFK-603 18” x 18”

OPERATING AND Typical Operating NF/RO (SR3D™ / HRX™): 100 - 650 psi (7 - 45 bar)
Pressure: UF/MF: 30 - 120 psi (2 - 8 bar)
DESIGN SelRO™ NF: 200 - 510 psi (14 - 35 bar)
INFORMATION*
Typical Operating NF/RO (except SelRO™): 40 - 113°F (5 - 45°C)
Temperature: SelRO™ NF: 104 -158°F (40 - 70°C)
UF/MF (except MFK-603): 40 - 130°F (5 - 55°C)
MFK-603: 40 - 176°F (5 - 80°C)
* Consult KMS Process Engineering for specific applications and other operating parameters.

The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any warranty or guarantee of performance. We assume no responsibility,
obligation or liability for results obtained or damages incurred through the application of the information contained herein. Refer to Standard Terms and Conditions of Sale and Performance Warranty
documentation for additional information.

Koch Membrane Systems, Inc., www.kochmembrane.com

Corporate Headquarters: 850 Main Street, Wilmington, Massachusetts 01887-3388, US, Tel. Toll Free: 1-888-677-5624, Telephone: 1-978-694-7000, Fax: 1-978-657-5208
European Headquarters: Koch Chemical Technology Group Ltd., Units 3-6, Frank Foley Way, Stafford ST16 2ST, GB, Telephone: +44-178-527-2500, Fax: +44-178-522-3149
• San Diego US • Aachen DE • Lyon FR • Madrid ES • Milan IT • Wijnegem BE • Beijing & Shanghai CN • Mumbai & Chennai IN • Melbourne & Sydney AU • Singapore • Sao Paulo BR • Manama BH •
The FLOW LINES DESIGN, SelRO, HRX and SR3D are trademarks of Koch Membrane Systems, Inc.
The STYLIZED K is a registered trademark of Koch Industries, Inc.
Koch Membrane Systems, Inc. is a Koch Chemical Technology Group, LLC company.
© 2014 Koch Membrane Systems, Inc. All rights reserved worldwide. 06/14 Rev.14-2
 Product Information

FILMTEC™ Membranes
FILMTEC NF270 Nanofiltration Elements for Commercial Systems

Features The FILMTEC™ NF270 membrane elements are ideal for removing a high percentage of
TOC and THM precursors with medium to high salt passage and medium hardness passage.
The FILMTEC NF270 membrane is an ideal choice for surface water and ground water
where good organic removal is desired with partial softening.

Product Specifications
Active Area Applied Pressure Permeate Flow Rate Stabilized Salt
Product Part Number ft2 (m2) psig (bar) gpd (m3/d) Rejection (%)
NF270-2540 149986 28 (2.6) 70 (4.8) 850 (3.2) >97.0
NF270-4040 149987 82 (7.6) 70 (4.8) 2,500 (9.5) >97.0
1. Permeate flow and salt rejection based on the following test conditions: 2,000 ppm MgSO4, 77°F (25°C) and 15% recovery at the pressure specified above.
2. Permeate flows for individual NF270-2540 elements may vary by -20% / +30%. NF270-4040 individual elements may vary -15% / +50%.
3. Developmental products available for sale.

A
Figure 1 B B

C DIA D DIA
FilmTec sells coupler part number
89055 for use in multiple element
housings. Each coupler includes
Outer Wrap two 2-210 EPR o-rings, FilmTec
part number 89255.
Feed End Cap Brine Product

Dimensions – Inches (mm)

Product A B C D
NF270-2540 40.0 (1,016) 1.19 (30) 0.75 (19) 2.4 (61)
NF270-4040 40.0 (1,016) 1.05 (27) 0.75 (19) 3.9 (99)
1. Refer to FilmTec Design Guidelines for multiple-element systems. 1 inch = 25.4 mm
2. NF270-2540 has a tape outer wrap. NF270-4040 has a fiberglass outer wrap.

Operating Limits • Membrane Type Polyamide Thin-Film Composite

• Maximum Operating Temperature 113°F (45°C)
• Maximum Operating Pressure 600 psi (41 bar)
• Maximum Feed Flow Rate - 4040 elements 16 gpm (3.6 m3/hr)
- 2540 elements 6 gpm (1.4 m3/hr)
• Maximum Pressure Drop - tape wrapped 13 psig (0.9 bar)
- fiberglassed 15 psig (1.0 bar)
• pH Range, Continuous Operationa 2 - 11
• pH Range, Short-Term Cleaning (30 min.)b 1 - 12
• Maximum Feed Silt Density Index SDI 5
• Free Chlorine Tolerancec < 0.1 ppm

a Maximum temperature for continuous operation above pH 10 is 95°F (35°C).

b Refer to Cleaning Guidelines in specification sheet 609-23010 for NF90.
c Under certain conditions, the presence of free chlorine and other oxidizing agents will cause premature membrane failure.
Since oxidation damage is not covered under warranty, FilmTec recommends removing residual free chlorine by
pretreatment prior to membrane exposure. Please refer to technical bulletin 609-22010 for more information.

Page 1 of 2 ™® Trademark of The Dow Chemical Company (“Dow”) or an affiliated company of Dow Form No. 609-00519-1206
Important Proper start-up of reverse osmosis water treatment systems is essential to prepare the
Information membranes for operating service and to prevent membrane damage due to overfeeding or
hydraulic shock. Following the proper start-up sequence also helps ensure that system
operating parameters conform to design specifications so that system water quality and
productivity goals can be achieved.

Before initiating system start-up procedures, membrane pretreatment, loading of the

membrane elements, instrument calibration and other system checks should be completed.

Please refer to the application information literature entitled “Start-Up Sequence” (Form No.
609-02077) for more information.

Operation Avoid any abrupt pressure or cross-flow variations on the spiral elements during start-up,
Guidelines shutdown, cleaning or other sequences to prevent possible membrane damage. During
start-up, a gradual change from a standstill to operating state is recommended as follows:
• Feed pressure should be increased gradually over a 30-60 second time frame.
• Cross-flow velocity at set operating point should be achieved gradually over 15-20 seconds.
• Permeate obtained from first hour of operation should be discarded.

General • Keep elements moist at all times after initial wetting.

Information • If operating limits and guidelines given in this bulletin are not strictly followed, the limited
warranty will be null and void.
• To prevent biological growth during prolonged system shutdowns, it is recommended that
membrane elements be immersed in a preservative solution.
• The customer is fully responsible for the effects of incompatible chemicals and lubricants
on elements.
• Maximum pressure drop across an entire pressure vessel (housing) is 30 psi (2.1 bar).
• Avoid static permeate-side backpressure at all times.

FILMTEC™ Membranes Notice: The use of this product in and of itself does not necessarily guarantee the removal of cysts and pathogens from water.
For more information about FILMTEC Effective cyst and pathogen reduction is dependent on the complete system design and on the operation and maintenance of
membranes, call the Dow Liquid the system.
Separations business:
North America: 1-800-447-4369 Notice: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws
Latin America: (+55) 11-5188-9222 may differ from one location to another and may change with time, Customer is responsible for determining whether products
Europe: (+32) 3-450-2240 and the information in this document are appropriate for Customer’s use and for ensuring that Customer’s workplace and
Pacific: +60 3 7958 3392
disposal practices are in compliance with applicable laws and other governmental enactments. Seller assumes no obligation or
Japan: +813 5460 2100
liability for the information in this document. NO WARRANTIES ARE GIVEN; ALL IMPLIED WARRANTIES OF
China: +86 21 2301 9000
MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED.
http://www.filmtec.com

Page 2 of 2 ™® Trademark of The Dow Chemical Company ("Dow") or an affiliated company of Dow Form No. 609-00519-1206
.

ky Hygienic Spiral Membranes for Reverse Osmosis

Alfa Laval RO98pHt for Dairy, Beverage and Food Applications

The Alfa Laval RO98pHt spiral elements are tailor made for processes
requiring high temperatures and a wide pH range in dairy, food and
beverage applications.
The elements are based on a thin film composite polyamide type
membrane with polypropylene (PP) backing material
The hygienic full fit design offers optimum cleaning conditions and
minimizes stagnant spaces.
All the materials used for the production of the membranes and
membrane elements comply with EU and FDA regulations (CFR) Title
21 , pending USDA approval.
All elements are shipped dry.

Designation Characteristics NaCl rejection

RO98pHt Thin film composite ≥98%*
*measured on 2000 ppm NaCl, pH 8, 16 bar, 25 ºC, 15% recovery

Spiral membrane designation

Alfa Laval RO98pHt-8038/30

Alfa LavalRO98pHt = Membrane type
.80 = Outer diameter of element (8.0")
38 = Element length (38")
30 = Feed spacer thickness

Dimensions
L1 OD = outer diameter of element
L2 L1 = total length of element without ATD
ID = diameter of ATD socket
L2 = depth of ATD socket
For specific measurements of AL housings, please consult the product
OD
ID

specification

TD 710-001

.
Standard Element Dimensions (without ATD system)

OD L1 ID L2 Area
Part No. Element type
mm ( “ ) mm ( “ ) mm ( “ ) mm ( “ ) m2 ( sqft )
517037 RO98PHT-2517/30 64.0 - 65.0 (2.52 - 2.56) 432 (17.0) 21.1 (0.83) 26.0 (1.023) 0.9 (11.5)
517592 RO98PHT-2517/48 64.0 - 65.0 (2.52 - 2.56) 432 (17.0) 21.1 (0.83) 26.0 (1.023) 0.6 (7.5)
516645 RO98PHT-3838/30 95.0 - 96.5 (3.74 - 3.80) 965 (38.0) 21.1 (0.83) 50.0 (1.97) 6.3 (77.5)
516646 RO98PHT-3838/48 95.0 - 96.5 (3.74 - 3.80) 965 (38.0) 21.1 (0.83) 50.0 (1.97) 4.7 (57)
522333 RO98PHT-3838/65 95.0 - 96.5 (3.74 - 3.80) 965 (38.0) 21.1 (0.83) 50.0 (1.97) 3.8 (47)
517314 RO98PHT-8038/30 198.5 - 201.5 (7.81 - 7.93) 965 (38.0) 28.9* (1.138) 79.0 (3.110) 32.9 (409)
518424 RO98PHT-8038/48 198.5 - 201.5 (7.81 - 7.93) 965 (38.0) 28.9* (1.138) 79.0 (3.110) 24.7 (302)
522332 RO98PHT-8038/65 198.5 - 201.5 (7.81 - 7.93) 965 (38.0) 28.9* (1.138) 79.0 (3.110) 20.0 (240)
For sizes not mentioned in this table please contact Alfa Laval.
* Elements with permeate tube internal diameter of 28.58 mm (1.125”) are also available.
Recommended operation limits

Production
pH range 2 - 10
Typical operating pressure 15 - 40 bar (220 - 600 psig)
Maximum operating pressure at 30 °C (85 °F) 55 bar (800 psig)
Maximum operating pressure at 60 °C (140 °F) 27 bar (400 psig)
Temperature 5 - 60 °C (40 - 120 °F)
Free chlorine concentration < 0.1 ppm
Hydrogen peroxide
Continuous operation at 25 °C (75 °F) 25 °C (75 °F) < 20 ppm

Cleaning (2 hours per day)

pH range 1 - 12.5
Typical cleaning pressure 1 - 5 bar (15 - 75 psig)
Temperature 25 - 60 °C (75 - 140 °F)
Free chlorine concentration < 0.1 ppm

Sanitation (1 hour per week)

Hydrogen peroxide short time sanitation 2 x ½ hour per week 25 °C (75 °F) < 1.000 ppm
Note: The use of oxidative cleaning agents and similar chemicals influence the actual membrane performance over time. Any contamination with
chlorine has to be avoided. Please consult the Alfa Laval “Water Quality” PD leaflet 1603.

.
Maximum pressure drop and typical cross flow rate at cP1

Element diameter 2.5" 3.8" and 3.9" 8.0"

Feed spacer m3/h (ft3/min) bar (psig) m3/h (ft3/min) bar (psig) m3/h (ft3/min) bar (psig)
30 mil 1.0 (4.5) 0.5 (7.5) 7 (30) 1.1 (17) 19 (83) 0.9 (17)
48 mil 1.5 (6.5) 0.6 (7.5) 9 (35) 1.1 (17) 23 (102) 0.9 (17)
65 mil - - - - 11 (48) 1.1 (17) 27 (118) 0.9 (17)
Note: Flow rates and pressure drops for tight fit spiral elements and use of standard ATD systems. Transmembrane pressure drop per housing not to
exceed 4.1 bar (60 psig) during production operation and 2.7 bar (40 psig) during cleaning operations.

Important Information Operation guidelines

New spiral elements must be cleaned prior to first use. The cleaning
procedure should be in accordance with the instructions provided in
AlfaLaval’s cleaning description for the spiral element type concerned.
The customer is fully responsible for the effects that any incompatible
chemicals may have on the spiral elements.
• After initial wetting, the spiral elements must be kept moist at all
times.
• If the operating specifications given in this product description are
not strictly followed, the limited warranty will be null and void.
• To prevent biological growth during system shutdowns, Alfa
Laval recommends that spiral elements should be immersed in a
protective solution.
• Avoid permeate-side back pressure at all times.
• Alfa Laval recommends using a rigid stainless steel ATD end device
at the housing outlet end.
• Alfa Laval recommends that the inner diameter of the housing
should be approx. 2 mm bigger than the outer diameter of the
spiral element in question.
Avoid any abrupt pressure or cross - flow changes on the spiral
elements during start - up, shutdown, cleaning or other sequences,
in order to prevent possible damage. Alfa Laval recommends the
following start - up procedure from stand still to operating condition:
• The unpressurized plant should be refilled with water.
• Feed pressure should be gradually increased over a 30 - 60 second
time scale.
• Before initiating cross - flow at high permeate flux conditions (e.g.
start - up with high temperature water), the set feed pressure
should be maintained for 5 - 10 minutes.
• Cross-flow velocity at the set operating point should be gradually
achieved over a period of 15 - 20 seconds
• Temperature changes should be implemented gradually over a
period of 3 - 5 minutes.
.

Alfa Laval reserves the right to change specifications without prior

notification. ALFA LAVAL is a trademark registered and owned by Alfa Laval
ESE00624EN 1410 Corporate AB. © Alfa Laval

How to contact Alfa Laval

Contact details for all countries
are continually updated on our website.
Please visit www.alfalaval.com to
access the information direct.
SelRO™ MPS-34 pH STABLE ELEMENTS
Nanofiltration Spiral Element Series - 8040

PRODUCT Membrane Chemistry: Proprietary composite nanofiltration membrane

Membrane Type: pH stable nanofiltration membrane
DESCRIPTION
Molecular Weight Cut-Off (MWCO) 200 Daltons
Construction: Spiral wound element with hard overwrap and polysulfone
permeate tube
Major Applications: Acid and caustic recovery, product concentration
Options: Feed channel spacers: 31 mil (N) and 57 mil (Z)

SPECIFICATIONS* Model Part Number Rejection [%] Permeate Flow Membrane Area Feed Spacer
Glucose NaCl gpd (m3/day) ft2 (m2) mil (mm)
/ Sucrose
8040 MPS-34-NYHN 0770255 95 / 97 35 10,900 (41.2) 308 (28.6) 31 (0.8)
8040 MPS-34-ZYHN 0770256 95 / 97 35 7,450 (28.1) 210 (19.5) 57 (1.4)

*Test Conditions: RO water at 440 psi (30 bar), 86°F (30°C). Feed solution for rejection tests is 3% glucose / 3% sucrose or 5% NaCl.

OPERATING AND Typical Operating Pressure: 220-510 psi (15-35 bar)

Maximum Temperature: 158°F (70°C)**
DESIGN Allowable pH - Continuous Operation: 0-14
INFORMATION* Allowable pH - Clean-In-Place (CIP): 0-14
Maximum Pressure Drop Per Element: 10 psi (0.7 bar)
Maximum Pressure Drop Per Vessel: 50 psi (3.5 bar)
* Consult Process Technology group for specific applications.
** Refer to the Operating Envelope of the SelRO Elements when temperature is higher than 122°F (50°C).

NOMINAL
DIMENSIONS

Model A B C Interconnector O-Rings

inches (mm) inches (mm) inches (mm)
8040 MPS-34-NYHN 40.0 (1016) 7.93 (202) 1.125 (28.6) 0030585 0035464
8040 MPS-34-ZYHN 40.0 (1016) 7.93 (202) 1.125 (28.6) 0030585 0035464

TYPICAL 5% HCl 15% Acetic acid 3% NaOH

PROCESS 37% HCL 5% HNO3 20% NaOH
STREAMS 15% H2SO4 20% H3PO4 10% KOH
 SelRO™ MPS-34 pH STABLE ELEMENTS
Membrane Characteristics and Performance:  Operating Envelope For SelRO Elements:
SelRO™ composite nanofiltration membrane in a spiral wound It is important to follow the pressure - temperature relationship
configuration, with superior pH and temperature stability. guidelines, in order to prevent irreversible compaction and
Performance specifications shown on the front side of this performance deterioration. The following diagram should be
document are nominal values. used as a guideline to operating the MPS-34 spiral element:
Operating Limits: 180
220 psi, 158°F
 Operating Pressure: Maximum operating pressure for (15 bar, 70°C)
160
SelRO MPS-34 is 510 psi (35 bar). Actual operating pressure 360 psi, 140°F
is dependent upon system flux rate, as well as feed, recovery (25 bar, 60°C)

Temperature (°F)
140
and temperature conditions. 510 psi, 122°F
(35 bar, 50°C)
120
 Permeate Pressure: Maximum allowed permeate pressure is
3 psi (0.2 bar). 100

 Differential Pressure: Maximum differential pressure limit is

80
10 psi (0.7 bar) per element. Maximum differential pressure
for any length vessel is 50 psi (3.5 bar). 60

 Temperature: Maximum operating temperature is 158°F

(70°C). For guidelines of recommended temperature and
pressure please refer to the "Operating Envelope for SelRO
Elements" in this document.
 pH: Allowable range for continuous operation is 0-14.
 Water Quality for Cleaning and Diafiltration:
Turbidity: For best performance maximum feed turbidity is 1
NTU.
 Chlorine and Chemical Exposure:
- It is not recommended to expose the MPS-34 membrane
to chlorine or other oxidants, as it may affect the
membrane performance.
- Sodium metabisulfite (without catalysts such as cobalt) is
the preferred chemical to eliminate free chlorine or other
oxidizers in the feed.
- It is not recommended to expose the MPS-34 membrane
to organic solvents, such as alcohol, acetone, etc.
 Feed Flow Rate: Maximum and minimum flow rate for the
MPS-34 spiral element are as follows:
Min. 25 gpm (95 liter/min)
Max. 75 gpm (285 liter/min)
Actual feed flow rate is dependent upon system flux rate, feed
characteristics, fouling tendency and system design.
0 150 300 450 600
Pressure (psi)
Element Handling:
 Recommended Cleaning Materials: Depending on the nature of
the feed, the following cleaning agents can be chosen:
- 0.1-5% w/w sodium hydroxide at 122°F (50°C)
- 0.2-1% w/w nitric or phosphoric acid at 122°F (50°C)
- 0.1-0.5% w/w detergent mix KOCHKLEEN™ KLD-III at 122°F
(50°C)
- 0.5% anionic surfactant (such as SDS) at 122°F (50°C)
Consult KMS regarding the use of other cleaning materials.
 Lubricants: For element installation, use only water or glycerin
to lubricate seals. The use of petroleum or vegetable-based oils
or solvents may damage the element and will void any warranty.
 Storage Solution: Should be made with:
- Short Term (up to two weeks): 0.25 w/w sodium metabisulfite.
- Long Term: 0.7% w/w benzalkonium chloride.
- Glycerin should not be used for storage of SelRO membranes.
- The membrane element should not get dry. It should be
stored in a sealed bag, at a temperature ranging from 36°F -
86°F (2°C - 30°C).
Service and Ongoing Technical Support:
Koch Membrane Systems (KMS) has an experienced staff of
professionals available to assist end-users and OEM’s for
optimization of existing systems and support with the development
of new applications. KMS also offers a complete line of
KOCHKLEEN™ membrane pretreatment, cleaning, and
maintenance chemicals.

The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any warranty or guarantee of performance. We assume no
responsibility, obligation or liability for results obtained or damages incurred through the application of the information contained herein. Refer to Standard Terms and Conditions of Sale and
Performance Warranty documentation for additional information.

Koch Membrane Systems, Inc., www.kochmembrane.com

Corporate Headquarters: 850 Main Street, Wilmington, Massachusetts 01887-3388, US, Tel. Toll Free: 1-888-677-5624, Telephone: 1-978-694-7000, Fax: 1-978-657-5208
European Headquarters: Koch Chemical Technology Group Ltd., Units 3-6, Frank Foley Way, Stafford ST16 2ST, GB, Telephone: +44-178-527-2500, Fax: +44-178-522-3149
• Aachen DE • Lyon FR • Madrid ES • Milan IT • Wijnegem BE • Beijing & Shanghai CN • Mumbai & Chennai IN • Melbourne & Sydney AU • SG • Sao Paulo BR • Manama BH •
The FLOW LINES DESIGN and KochKLEEN are trademarks of Koch Membrane Systems, Inc.
The STYLIZED K is a trademark of Koch Industries, Inc.
SelRO is a trademark of Membrane Products Kiryat Weizmann, Ltd.
Koch Membrane Systems, Inc. is a Koch Chemical Technology Group, LLC company.
© 2013 Koch Membrane Systems, Inc. All rights reserved worldwide. 04/13 Rev 13-2
SelRO™ MPS-36 pH STABLE ELEMENTS
Nanofiltration Spiral Element Series - 8040

PRODUCT Membrane Chemistry: Proprietary composite nanofiltration membrane

Membrane Type: pH stable nanofiltration membrane
DESCRIPTION
Molecular Weight Cut-Off (MWCO) 1000 Daltons
Construction: Spiral wound element with hard overwrap and polysulfone
permeate tube
Major Applications: Acid and caustic recovery, product concentration
Options: Feed channel spacers: 31 mil (N) and 57 mil (Z)

SPECIFICATIONS* Model Part Number Rejection [%] Permeate Flow Membrane Area Feed Spacer
Glucose NaCl gpd (m3/day) ft2 (m2) mil (mm)
/ Sucrose
8040 MPS-36-NYHN 0770257 30 / 50 10 36,250 (137) 308 (28.6) 31 (0.8)
8040 MPS-36-ZYHN 0770258 30 / 50 10 25,100 (95) 210 (19.5) 57 (1.4)

*Test Conditions: RO water at 440 psi (30 bar), 86°F (30°C). Feed solution for rejection tests is 3% glucose / 3% sucrose or 5% NaCl.

OPERATING AND Typical Operating Pressure: 220-510 psi (15-35 bar)

Maximum Temperature: 158°F (70°C)**
DESIGN Allowable pH - Continuous Operation: 1-13
INFORMATION* Allowable pH - Clean-In-Place (CIP): 1-13
Maximum Pressure Drop Per Element: 10 psi (0.7 bar)
Maximum Pressure Drop Per Vessel: 50 psi (3.5 bar)
* Consult Process Technology group for specific applications.
** Refer to the Operating Envelope of the SelRO Elements when temperature is higher than 122°F (50°C).

NOMINAL
DIMENSIONS

Model A B C Interconnector O-Rings

inches (mm) inches (mm) inches (mm)
8040 MPS-30-NYHN 40.0 (1016) 7.93 (202) 1.125 (28.6) 0030585 0035464
8040 MPS-30-ZYHN 40.0 (1016) 7.93 (202) 1.125 (28.6) 0030585 0035464
 SelRO™ MPS-36 pH STABLE ELEMENT
Membrane Characteristics and Performance:  Operating Envelope For SelRO Elements:
SelRO™ composite nanofiltration membrane in a spiral wound It is important to follow the pressure - temperature relationship
configuration, with superior pH and temperature stability. guidelines, in order to prevent irreversible compaction and
Performance specifications shown on the front side of this performance deterioration. The following diagram should be
document are nominal values. used as a guideline to operating the MPS-36 spiral element:
Operating Limits: 180
220 psi, 158°F
 Operating Pressure: Maximum operating pressure for (15 bar, 70°C)
160
SelRO MPS-36 is 510 psi (35 bar). Actual operating pressure 360 psi, 140°F
is dependent upon system flux rate, as well as feed, recovery (25 bar, 60°C)

Temperature (°F)
140
and temperature conditions. 510 psi, 122°F
(35 bar, 50°C)
120
 Permeate Pressure: Maximum allowed permeate pressure is
3 psi (0.2 bar). 100

 Differential Pressure: Maximum differential pressure limit is

80
10 psi (0.7 bar) per element. Maximum differential pressure
for any length vessel is 50 psi (3.5 bar). 60

 Temperature: Maximum operating temperature is 158°F

(70°C). For guidelines of recommended temperature and
pressure please refer to the "Operating Envelope SelRO
Elements" in this document.
 pH: Allowable range for continuous operation is 1-13.
 Water Quality for Cleaning and Diafiltration:
Turbidity: For best performance maximum feed turbidity is 1
NTU.
 Chlorine and Chemical Exposure:
- It is not recommended to expose the MPS-36 membrane
to chlorine or other oxidants, as it may affect the
membrane performance.
- Sodium metabisulfite (without catalysts such as cobalt) is
the preferred chemical to eliminate free chlorine or other
oxidizers in the feed.
- It is not recommended to expose the MPS-36 membrane
to organic solvents, such as alcohol, acetone, etc.
 Feed Flow Rate: Maximum and minimum flow rate for the
MPS-36 spiral element are as follows:
Min. 25 gpm (95 liter/min)
Max. 75 gpm (285 liter/min)
Actual feed flow rate is dependent upon system flux rate, feed
characteristics, fouling tendency and system design.
0 150 300 450 600
Pressure (psi)
Element Handling:
 Recommended Cleaning Materials: Depending on the nature of
the feed, the following cleaning agents can be chosen:
- 0.1-5% w/w sodium hydroxide at 122°F (50°C)
- 0.2-1% w/w nitric or phosphoric acid at 122°F (50°C)
- 0.1-0.5% w/w detergent mix KOCHKLEEN™ KLD-III
- 0.5% anionic surfactant (such as SDS) at 122°F (50°C)
Consult KMS regarding the use of other cleaning materials.
 Lubricants: For element installation, use only water or glycerin
to lubricate seals. The use of petroleum or vegetable-based oils
or solvents may damage the element and will void any warranty.
 Storage Solution: Should be made with:
- Short Term (up to two weeks): 0.25 w/w sodium metabisulfite.
- Long Term: 0.7% w/w benzalkonium chloride.
- Glycerin should not be used for storage of SelRO elements.
- The membrane element should not get dry. It should be
stored in a sealed bag, in a temperature ranging from 36°F -
86°F (2°C - 30°C).
Service and Ongoing Technical Support:
Koch Membrane Systems (KMS) has an experienced staff of
professionals available to assist end-users and OEM’s for
optimization of existing systems and support with the development
of new applications. KMS also offers a complete line of
KOCHKLEEN™ membrane pretreatment, cleaning, and
maintenance chemicals.

The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any warranty or guarantee of performance. We assume no
responsibility, obligation or liability for results obtained or damages incurred through the application of the information contained herein. Refer to Standard Terms and Conditions of Sale and
Performance Warranty documentation for additional information.

Koch Membrane Systems, Inc., www.kochmembrane.com

Corporate Headquarters: 850 Main Street, Wilmington, Massachusetts 01887-3388, US, Tel. Toll Free: 1-888-677-5624, Telephone: 1-978-694-7000, Fax: 1-978-657-5208
European Headquarters: Koch Chemical Technology Group Ltd., Units 3-6, Frank Foley Way, Stafford ST16 2ST, GB, Telephone: +44-178-527-2500, Fax: +44-178-522-3149
• Aachen DE • Lyon FR • Madrid ES • Milan IT • Wijnegem BE • Beijing & Shanghai CN • Mumbai & Chennai IN • Melbourne & Sydney AU • SG • Sao Paulo BR • Manama BH •
The FLOW LINES DESIGN and KochKLEEN are trademarks of Koch Membrane Systems, Inc.
The STYLIZED K is a trademark of Koch Industries, Inc.
SelRO is a trademark of Membrane Products Kiryat Weizmann, Ltd.
Koch Membrane Systems, Inc. is a Koch Chemical Technology Group, LLC company.
© 2013 Koch Membrane Systems, Inc. All rights reserved worldwide. 02/13 Rev 13-2