MEng

Research Project: Modelling and

Simulation of Micro-distillation Devices
Adri Jamil Shakir
Developments in the area of microfluidics have been vast over the last decade with many
potential applications and in which separation processes play an integral part. In this study,
one dimensional model describing this unit is developed using mass transfer coefficients
obtained from packed bed correlations. The model is then validated and compared with
experiments and model simulations by Ramirez-Gonzalez (1992) (upon which the current
work is based on) and Fanelli (2007) with moderate success. Discussions on issues, sources
of error, validity of assumptions and future recommendations is also provided.

D e p a r t m e n t o f C h e m i c a l E n g i n e e r i n g - U n i v e r s i t y C o l l e g e L o n d o n


Table of Contents
1. Introduction.................................................................................................................... 3
1.1. Process intensification ................................................................................................. 3
1.2. Microchemical systems ................................................................................................ 3
1.3. Applications ..................................................................................................................... 4
1.4. Microdistillation ............................................................................................................. 5
1.5. Fabrication and ancillaries ......................................................................................... 7
1.6. Scope of research ........................................................................................................... 7
2. Literature review....................................................................................................... 9
2.1. Zero-gravity distillation utilising the heat pipe principle................................ 9
2.2. Modelling Zero-Gravity Distillation .......................................................................10
2.3. Microdistillation of multicomponent systems ...................................................10
2.4. Micro-Scale Distillation I: Simulation.................................................................11
3. Model development ............................................................................................... 13
3.1. Assumptions ..................................................................................................................13
3.2. Control volume..............................................................................................................14
3.3. Molar balance ................................................................................................................15
3.4. Vapour and Liquid flow..............................................................................................18
3.5. Feed...................................................................................................................................19
3.6. Physical Properties ........................................................................................................19
4 Case study: Seok and Hwang (1985) ................................................................. 24
4.1 Equations .........................................................................................................................24
4.2 Results and discussion ................................................................................................26
4.3 Discussion........................................................................................................................29
4 Case studies ............................................................................................................... 31
4.1 Equations .........................................................................................................................31
4.2 Assigned Variables and Parameters ..................... Error! Bookmark not defined.
4.3 Results and discussion ................................................................................................32

1. Introduction
1.1. Process intensification
Throughout the history of chemical process engineering, since the discovery of
distillation as a method of obtaining pure water almost 2000 years ago,
engineers have been continuously improving these methods to reduce size, cost,
energy consumption; and increase safety, yield and control. However, the last
few decades have seen vast developments in this area, and this has come to be
known as process intensification, which may be defined as a strategy for making
dramatic improvements in chemical processes with regards to the criteria
mentioned above.
This area of study can be divided into two parts,
Equipment Processes are intensified by the design of novel reactors such as
monolithic reactors and microreactors; and other unit operation equipment
such as compact heat exchangers, static mixers and rotating (high gravity)
separators.
Methods Intensification is achieved by the use of new techniques such as
multifunctional reactors (integrated with separation, heat exchange or phase
transition), hybrid separation (such as membrane distillation) and the use of
alternative energy sources (solar, microwaves, ultrasound). Other methods
include new process control methods such as intentional unsteadystate
operation and the utilisation of supercritical fluids.

1.2. Microchemical systems

One aspect of process intensification is reduction in equipment size, leading to
the development of microchemical systems, which include techniques such as
injection, mixing, reaction, separation and detection being conducted in channels
ranging from 10 nm to 500 mm (Gnther, 2006). Incidentally, this vast reduction
in size also offers several other advantages, aside from the other goals of process
intensification being achieved, which are:

Safety: Highly exothermic reactions can be performed safely due to better heat
transfer, enabled by high surface-to-volume ratios. Also, if there is loss of
containment of hazardous materials, adverse impact will be minimal.
Cost: Due to the small amount of volumes involved, much lower energy demand
and lower fabrication cost. Increased opportunities for automated processes also
reduce the need for manpower.
Automation: Enabled by recent advances in digital microfluidics. Provides more
possibilities for automated processing of arrays of materials such as DNA
analysis, catalyst screening (Fair ,2007)
High throughput: More opportunities for automation enables analysis of a wider
spectrum of materials and faster.
Other key developments include methods for continuous separation of particles
based on their size using dialectropheses, electrowetting on dialectric
microfluidics and electrochemical and photochemical activation (Wiles, Kralj
2006).

1.3. Applications
Microfluid systems have many applications in different areas of technology
including biology, medical science and chemistry. Due to the advantages
explained above, there is a lot to be gained from the scale down of laboratory
techniques to the smallest size.
It can be used to cheaply and accurately measure parameters such as transport
coefficients, reaction kinetics, physical parameters and catalyst performance
(Yager, 2001). It is easier to predicting heat and mass transfer characteristics
due to mostly laminar flow, which enables better measurements. It also allows
the running reactions under more stringent conditions due to flatter
temperature and composition profiles, minimising side reactions.
It is useful in the investigation of problems with recycle streams. This is due to
the small cumulative hold-ups on these micro plants, in the order of 1 day
(Sundberg, 2009). The small volumes involved and superior heat control enables

chemists to explore different reaction conditions or catalysts which may have

been too dangerous to be conducted on a bench or production scale (wiles
2011). The thermal flatness in the radial direction enables more precise
temperature control, minimising side reactions (Wootton).
Chemical engineers often use pilot plants to optimise a process for scale up to
production. These trial and error procedures often consume a lot of time and
materials. The use of microfluidic devices would reduce the need for these costly
operations. The flexible nature of the system, units can be mixed and matched
easily, means that different configurations can be explored cheaply and quickly
(Jensen 1999).
There are also numerous applications in biomedical studies such as DNA
detection, gene sequencing and medical diagnostics. Developments in
microfluidics, particularly by the Human Genome Project, have produced
integrated chips capable of conducting polymerase chain reactions (PCR), a key
stage in DNA analysis.

1.4. Microdistillation
Separation methods are integral to the development of microchemical systems.
These include liquid-liquid extraction, particle sorting, phase separation,
absorption and distillation. It is important to understand how these scaled down
units behave, particularly due to the increased significance of interfacial and
surface phenomena.
Distillation is one of the oldest and most understood unit operations in Chemical
Engineering. On a production scale, continuous distillation is carried out in
columns, either filled with packing or plates, with the distillate coming out of the
top of the column and the bottoms coming out the bottom. Part of the vapour is
condensed and fed back to the column as reflux while part of the liquid at the
bottom is vaporised. This creates a continuous counter-current stream of vapour
flowing up and liquid flowing down, enabling mass transfer across the column. In
this case, we rely on gravity for liquid to flow down the column while the vapour
rises to the top naturally due to the pressure in the reboiler.

The idea of a distillation method that relies on these capillary forces instead of
gravity (hence the name zero-gravity distillation) has been around since the 80s
when Seok and Hwang (1985) developed the method by utilising the heat-pipe
principle. A heat-pipe is a heat transfer device vapour is allowed to condense at
the cool end, and the condensate flows towards the hot end where it is
evaporated. Fluid flows via pressure gradients created by the heating and
cooling of opposite ends. At the heating end, analogous to the column reboiler,
vapour is generated, increasing pressure and forcing vapour down to the cooling
end, where the vapour is condensed creating the same effect in the liquid phase.
This creates the same counter current flow of vapour and liquid seen in
conventional distillation columns. By the same principle, using a binary mixture
would result in the lighter component accumulating at the cool end and the
heavier component at the hot end, as confirmed by Cotter (1965). By
continuously feeding the heat pipe with a mixture and withdrawing products
from both ends, a continuous distillation unit is created.
Aside from the utilising capillary forces instead of gravity, another major difference
with microfluidic distillation is that reflux occurs internally and is not controlled
directly. Hence the actual reflux rate is difficult to quantify which poses a
challenge to understanding the influence of geometry and flow rates on
separation performance.
In microdistillation devices, uncontrolled boiling tends to occur in the hot as the
liquid tends to superheat. This is due to the increased significance of surface
tension and low nucleation rate (Hartman and Sahoo 2009). To counter this,
some researchers have used a carrier gas such as nitrogen to be able to vaporise
the liquid below boiling point (Wootton). However, this results in a poorer
separation because there no reflux flow due to the unidirectional flow of the
carrier gas. A way of solving this problem is by providing a stable vapour liquid
interface, which can be done using membranes or using microstructures to
exploit surface tension effects (Adiche and Sundmacher (2010)).

1.5. Fabrication and ancillaries

Early microfluidic devices were made of complex silicone and glass materials
used for microchips (erickson, 2003). Currently, ceramics, metals and synthetic
polymers are becoming more common (Jensen, 1999). They are fabricated using
the same technology as microchips, photoresist and etching.
A layer of porous material can be used to direct liquid flow from the hot end to
the cold end and to prevent entrainment (Sundberg, 2009). The desired features
of this material are high porosity, good wetting characteristics, large specific
area and high permeability.
Though microdistillation devices are usually operated horizontally, there have
been experiments where it is vertical or tilted slightly towards one side.
Heating and cooling is generally conducted through the walls of the device itself
using a heating pad attached to a heating cartridge or water bath. Therefore the
heat transfer properties of the materials of construction must be considered,
keeping in mind that heat loss to the surroundings will also be a problem due to
high surface to volume ratios. Temperature, pressure and flow rates can be
measured using microsensors.
Fluid flow is created using digitally operated syringe pumps or by applying an
electric field across the channel (electrowetting). An advantage of electrowetting
is that it creates a flatter velocity profile, avoiding diffusion non-uniformities that
occur with pressure driven flow.

1.6. Scope of research

Since there the initial proof of concept in 1985 by Seok and Hwang, there have
been several experimental and modelling work on microfluidic devices. The next
major step in the development of microfluidic devices would be to increase
production, as companies such as Velocys have been trying to do for the last 5
years or so. Like cars and electronics where parts are mass-produced separately
before assembly, this would add a greater amount of flexibility and accessibility
for the applications discussed earlier. To do this, it is necessary to be able to
model these units reliably and accurately, which is the aim of this research. This

will enable use to design and predict performance of microdistillation devices

and better understand the phenomena behind the operation.
In this paper, I will present a mathematical model describing the
microdistillation process based on known mass and heat transfer theories.
Simulating conditions in previous works and comparing it with their
experimental results will verify this model. Ideally, this model should be
applicable to all variations of the microdistillation process. The motive for
developing this model is to be able to conduct simulated experiments using
different configurations, materials and operating conditions. The model will be
compared to other models found in literature to asses its validity with respect to
predicting column performance.
In the next chapter, a survey of all relevant literature is presented. First, we
review all experiments done in this area, paying particular attention to operating
conditions, results and any interesting observations. Next, we will look at the few
models that have been developed, commenting on their assumptions, theories
employed and verification of their model. Lastly, we will review works on
specific phenomena applicable to this scale of operation such as film
evaporation, flow characteristics and capillary and surface tension effects.

2. Literature review
2.1. Zero-gravity distillation utilising the heat pipe principle
D. R. Seok and Sun-Tak Hwang (1985)
The concept of a distillation process utilising, capillary forces was first proven by
Seok and Hwang (1985), who conducted experiments on a 54 cm long, 1.05 cm
internal diameter pipe with a fibreglass wick using methanol-water and ethanol-
water mixtures. Along with experimental results, also presented is a model,
which they developed.
Theory
Mass transfer occurs due to heat transfer and diffusion; and is controlled by the
vapour phase, with a constant mass transfer coefficient along the column,
independent of vapour and liquid flow rates. The model assumes no
concentration and temperature gradients in the radial direction and that vapour
and liquid are in constant equilibrium. The overall height of a transfer unit (HTU)
is used to evaluate column performance. Liquid flow is taken to be at its capillary
limit, which means the axial pressure gradient is only due to the surface tension
gradient, and liquid flows according to Darcys law.
Experiments were conducted for both mixtures first at total reflux and with
products, varying feed rates to study the effects of varying gas to liquid ratios.
For the model boundary conditions, it is assumed that vapour and liquid
compositions are equal at the evaporator and condenser ends, which is not true
in reality as the vapour should be richer in the lighter component. One issue with
the model was evaluating gas to liquid ratios, which was estimated by trial and
error since it could not be measured directly.
The experimental results follow the modelled column profiles quite closely,
though the actual gradients were steeper at the middle of the column.
Though this cannot be called microdistillation as it was the flow channels were in
the order of 1 cm, the transport equations is expected to be the same when
brought down to the microscale.

2.2. Modelling Zero-Gravity Distillation

E. A. Ramirez-Gonzalez et al (1992)
In this paper, experiments conducted by Seok and Hwang (1985) were modelled
with good agreement. Liquid flow is assumed to be due to capillarity, with axial
pressure gradient governed by the Young-Laplace equation and flowrates by the
Darcy equation. Perfect wetting is assumed so that the contact angle is zero.
Again, radial gradients are neglected since the ratio of the length to diameter is
large. In an attempt to justify the high mass transfer rates despite a low Reynolds
number (Re), mass transfer correlations for high and low Re for packed beds are
used and compared. It is thought that the high mass transfer rates are due to
mixing, resulting in more velocity fluctuations since interfacial area is small
compared to that of packed beds. For the liquid phase, the effective diffusivity is
used to take into account for porosity. Temperature is taken as a function of
composition by vapour liquid equilibrium, which is justified if compositions of
the bulk phase are not far from equilibrium. However, a more accurate
representation could be obtained by implementing an energy balance equation.
Liquid phase diffusivities are obtained as a function of composition by the Vignes
correlation but comparison with experimental data for methanol-water
diffusivities show that this is a poor approximation at best.
The model is limited to the adiabatic zone as to compare with Seok and Hwang s
(1985) approach. Mass transfer along in the axial direction is by convection and
diffusion though the diffusion term is expected to be relatively small compared
to the convective term. The resulting model includes a one dimensional
differential mass balance equation for each phase, which is justified since mixing
is promoted in the liquid phase due to the porous media and in the gas phase by
high diffusion rates.

2.3. Microdistillation of multicomponent systems

J. Tschernjaew et. Al (1996)
This paper presents a yet untested theoretical model for microdistillation of
multicomponent mixtures, utilising Maxwell-Stefan diffusivities. Liquid flow is
governed by the same principles as earlier papers. Unlike previous work,

10

diffusion in the axial direction is assumed to negligible and there is only

convection in this direction. As mentioned earlier this is valid since diffusion is
small compared to convection, as will be shown later in this study. Mass transfer
in the radial direction is by convection, using Maxwell-Stefan diffusivities for
multicomponent mixtures (effective diffusivity for the liquid phase) instead of
mass transfer coefficients as in Ramirez-Gonzalez (1992). These diffusivities are
taken as constant along the pipe length. This is not entirely accurate since
diffusivity is concentration dependant, especially in the liquid phase. Another
issue here is that Maxwell-Stefan diffusivity data for mixtures of more than 3
components are difficult to quantify experimentally, resulting in a lack of reliable
data. The paper suggests using correlations found in literature for to estimate
diffusivities. The paper also assumes a linearised model for vapour liquid
equilibria at the interface, which is only valid if the liquid is close to ideal. The
model results in (NC 1) 2-dimensional differential mass balance equations for
each phase, which adds considerable complexity in solving compared to previous
models. One advantage of having a 2-dimensional model is that diffusion effects
at the feed inlets and product outlets can be modelled more accurately. It will be
investigated later in this paper whether this added complexity is justified.

2.4. Micro-Scale Distillation I: Simulation

M. Fanelli et. al. (2007)
This paper presents a model neglecting heat transfer and flow instabilities,
which is then verified with experimental data with moderate agreement. The
model is contains many simplifications as it was developed to provide a rough
estimation column performance for the purpose of refining designs of
microdistillation columns. The model uses volatilities based on ChemCAD,
linearly interpolated from column extremes for concentrations at the interface.
Other parameters such as diffusivities, density and concentration are assumed to
be constant along the column, taken as the average between column ends. Unlike
previous work, this column was operated vertically, therefore liquid flow is due
to gravity, and with the porous medium functioning to keep the phases separate
through capillary pressure. The result is a 2 dimensional model for each phase.
Two cases for liquid flow were considered for comparison with literature. The

11

first assumed mesh flow, with a constant cross sectional area perpendicular to
direction of flow, equal to the mesh cross sectional area. The second case
assumed a falling film configuration, where the area of flow and velocity are
dictated by the flow rate, with fully laminar flow conditions. Simulation results
show that the first case is a more accurate representation, showing a 20%
average deviation with experimental results, though the model is only verified
based on HETP calculations as opposed to concentration profiles.

12

3. Model development

3.1. Assumptions
1. Vapour liquid interface is at the inner surface of the wick area of flow of
liquid is constant, liquid velocity controls the flow rate. Simulations by
Fanelli (2007) confirmed that this assumption leads to a more accurate
prediction of HETP compared to area of flow being dictated by flow rate.
However, Sundberg (2008) reported that while the liquid level in their
microdistillation column varied with flow rate, the surface of the wick was
constantly wet.
2. No angular concentration or temperature gradients angular velocity is
assumed to be zero and this vastly reduces the complexity of the model. Inlet,
outlet and sample ports are in the same angular position, reducing the
significance of angular gradients.
3. Vapour liquid equilibrium vapour is always in equilibrium with the liquid
phase. A common assumption in distillation problems. This may not be
entirely true at the evaporator end where the liquid is superheated as
reported by Ranjan (2011) in his studies on heat pipes.
4. Heat balance is neglected Simulations by Ramirez-Gonzalez (1992) were
conducted under this assumption with good agreement with experimental
data. Hence it is deemed unnecessary to add further complexity to the model.
5. Equimolar counter diffusion - Another common assumption for distillation
problems. This is probably not valid at the condenser and evaporator ends
where extra condensation and evaporation occur.
6. Liquid flows at its capillary limit This means liquid flows at the maximum
allowed by capillary forces.
7. Perfect wetting this is common assumption which is valid for porous
materials.
8. No velocity fluctuations The model is meant for steady state operation,
hence velocity fluctuations are assumed to be negligible.

13

9. Constant pressure (1 atm) along z Although this is not true since vapour
flow is enabled by pressure gradients along the pipe, this gradient is not very
large and its effect on physical properties is assumed to be negligible.
10. Temperature is a function of composition, constant along the radial and
angular direction This is a simplification due to the fact that heat balances
are neglected in the model. In reality composition (through relative
volatilities) are a function of temperature, which is calculated by heat
balances.

3.2. Control volume

Figure 1: Schematic of vapour and liquid phases in the microdistillation device

The device is a copper cylinder with a layer of wick to guide liquid flow on the
walls while vapour flows in the middle, in the opposite direction of liquid flow. In
the axial direction, mass transfer is mostly by convection while in the radial
direction, we have equimolar diffusion across the interface and feed entering the
liquid phase from the outer radius. A 3D diagram of our control volume used to
derive the molar and energy balances in the liquid phase is shown below

14


Figure 2: Control volume diagram

3.3. Molar balance

The molar balance across a control volume (c.v) is given by:
(net rate of molar flux from c.v) + ( rate of molar accumulation)
- (rate of molar generation) = 0

In the z direction:
Net rate of addition = n A,z

( r + r) 2 r 2
2

n A,z

z +z

( r + r) 2 r 2
2

mass flux in the z direction and is given by equation x. The

Where the nA,z is the
first term accounts for diffusion while the second term accounts for convection.

n A,z = CL DAB

x A
+ CL uz
z

In the r direction:

Net rate of addition = n A,r rz r +r n A ,r rz r

15

Due to assumption 4, we take r = r1, the inner radius, and r + r = r2, the outer
radius. At r1, we have mass transfer across the interface, which is given by:
n A,r r r = kL r1 (CA CAi )

We also have a feed coming in from r2, which is given by

n A,r r r +r = n A,F r2

Where nA,F = 0 at all axial positions except at the feed point. Calculation of this
value is explained later below. It should be noted that by this equation, it

assumes that the feed enters the bulk liquid phase with a radial velocity of 0,
hence travels along with the liquid its axial velocity. This is valid, because
simulations show that the feed flow rate is small compared to the liquid flow
rate. Furthermore, it is not possible to model exactly flow of feed as momentum
balances are not considered in this model.
In the direction:
Net rate of addition = n A, rz + n A, rz +

By assumption 3, this term is neglected.

Accumulation

Rate of generation is equal to zero since there is no chemical reaction. The rate of
accumulation within the c.v. is then given by:
2

CA ( r + r) r 2
z
t
2
Combining the above equations yield

r2 2 r12

r2 2 r12
CA r2 2 r12
dCA
dCA
z = DAB
+ v zCA

DAB
+ v zCA

2
t
2
dz
dz
z +z
z

+ kL r1 (CAi CA ) + n A,F r2 z

16

Since CA is equal to xACL, and assuming the change in CL over length z is small,
we can replace CA with xA. DAB is replaced with Deff, given by equation (x) to
account for porosity. As z approaches zero, dividing by whole equation by the
control volume results in the following differential equation

2
rn
x A
2 x A Deff x A
x
= Deff
v L A kL r1 ( x A x Ai ) + 2 A,Feed 2
=0
2 +
t
z
z z
z
CL r2 r12
(1)

Using similar methods for the gas phase yields the following equation, where the
feed flux term is dropped because feed is only in the liquid phase and the partial
derivative of diffusivity is dropped because gas diffusivity is more or less
dependant of composition [6]:

y A
2 yA
y A
= DAB,G
+ 2r1kCG ( y Ai y A ) = 0
2 + vG
t
z
z

(2)

The model equations (1) and (2) are related by mass transfer through the
interface by equimolar counter diffusion.
kL CL (x A x Ai ) = kG CG (y Ai y A )

(3)

Boundary conditions

The model uses Danckwerts boundary conditions for at the evaporator and
condenser ends, given by the following equations

x A
z

(4)

(5)

(6)

(7)

=0

z =length

y
vG y A,in z =length + = vG y A ,in DAB,G A

z z =length

x
v L x A,in z =0 = v L x A,in Deff A

z z =0 +

y A
z

=0
z =0

17

3.4. Vapour and Liquid flow

The pressure difference across the vapour-liquid interface is described by the
Young-Laplace equation:

PL = PG

2L cos
,0 180
rp

(8)

Assuming constant pressure in the gas phase and a constant pressure gradient in
the liquid phase, this equation can be used to find the pressure drop in the
following equation. Liquid velocity is described by the Darcy equation for flow
through porous media (Dunn and Reay,1994).

vL =

K PL

L z

(9)

The contact angle; , can be taken as 0 under assumption 9, ie (cos 0 = 1). At the

evaporator and condenser sections, work by Ranjan (2010) to estimate the

contact angle from the heat flux. Assuming a linear change in surface tension
across the length of the device, combining the two equations above leads to:

vL =

2K (c e )

L rp Length

(10)

Where e and c are surface tension taken at the evaporator and condenser
respectively (Dunn and Reay,1994). By assumption 1, liquid molar flow rate is

given by:

L = v L ( r22 r12 )CL

(11)

Since reflux is not controlled, actual flow rates are difficult to quantify. In Seok
and Hwang (1985), they managed to estimate the gas to liquid ratio by trial and

error, which we can use to calculate the vapour flow rate. We can then calculate
the vapour phase velocity using equation (12).

18

( )

G = GL

vG =

(12)

G

r12CG

(13)

ratio

3.5. Feed

The feed enters through a hole perforated in the device. Since our model only
considers the axial dimension, we assume that it enters the liquid phase through
the outer surface of the liquid phase from all directions of , for a length dzF. In
mathematical terms, the area of flux for the feed is given by:

A feed = 2r2 dz F

(14)

Where the Afeed is equal to the area of the feed inlet in the experiment and dzF, is
the size of the element used in solving the differential equation. The feed molar
flux is then obtained from equation (14) for length dzF at the feed location, and
equals to 0 at all other points.

n A, feed =

3.6.

F
at z = z feed : z feed + dzF
A

(15)

Physical Properties

Temperature and pressure is assumed to be constant throughout the device and

physical properties are calculated using a pressure of 1 atm and a temperature
equal to the average of the boiling points of pure components.
Liquid and gas densities are assumed to be additive, given by equation (16) as
functions of pure concentration and composition

L = ( x i M i )

CL
1000 and

G = ( y i M i )

CG

1000

(16)

Liquid concentration is given by equation x while pure component

concentrations are obtained from correlations found in Perrys by the equation
after.

19

CL =

1
x
C i
L,i

CL,i =

B1

B
T 4

B21+1 B 3

(17)

(18)

Gas concentration
is obtained from the ideal gas law, which is valid at low

pressures

CG =

n
P
=
V RT

(19)

Liquid viscosities for pure components are known to vary with temperature by
equation (20). Constants for the equation are found by regression of
experimental data or data obtained from ChemCAD.

L,pure (T) = io exp(bT)

(20)

Viscosities of liquid mixtures can then be calculated using the equations

proposed by Grunberg and Nissan (1949) (Poling, 2001)

ln( L,mix ) = x A ln( L,A ) + x B ln( L,B ) + x A x B J AB

(21)

Where JAB at a reference temperature of 298 K can be found from group

contribution method found in literature. Alternatively, it can also be estimated
from regression of experimental or ChemCAD data. This constant varies with
temperature by the following equation:

J AB (T) = 1 (1 J AB,0 )

(573 T )
275

(22)

Gas viscosities for pure substances are obtained from the Chapman-Enskog
equation, where /K are found expressed by equation (24) with constant

found from literature (Poling, 2001)

20

M wT
2 ,

(23)

(24)

= 0.841Vc1/ 3

(27)

G, pure = 2.6693 10 5
/K = 0.77TC

Viscosity of the gas mixture is then obtained from equation (28), where ij is

given by equation (29) (Poling, 2001)

A,G
B,G

+
yB
yA
1+ AB 1+ BA
yA
yB

(28)

1/ 2
1/ 2
1/ 4
1 M i i M j
1+

ij =
1+

8 M j j M i

(29)

G,mix =

Liquid phase diffusivity as a function of concentration is given by the Vigness

correlation:
x

B
A
0
0

DAB,L = DAB,L
DBA,L

Where diffusivities for dilute systems are given by the following equation
proposed by Wilke and Change (1955).
1/ 2

0
AB,L

7.4 10 8 (M B ) T
=

0.6
BVA,boil

(30)

(31)

We need to adjust for porosity by the following equation.

Deff =

DAB
2 DAB , where 1/

Gas phase diffusivity is obtained from equation (32) proposed by Wilke and

Lee (1955) where AB and AB are given by equations (33) and (34)

21

DAB,G

[3.03 (0.98 M )] 10 T
=
1/ 2
AB

3/2

2
TM 1/AB2AB
D

(32)

AB = 0.5(A + B )

(33)

AB = A B

(34)

Parameters can be found from litereature

Mass transfer coefficients are obtained from the following correlations for
mass transfer in fixed beds (Treybal, 1981)
vG

kG =

v L

Re Sc 2 / 3

kL =

Sc 2 / 3

(35)

(36)

For laminar flow, = 1.09 and = 2/3, while for turbulent flow, = 20.4 and =

0.815. The Reynolds number for flow through porous media and the Schmidt
number are shown below.

Re =

L v L d p

L

Sc =

DAB

for liquid and gas phase

(37)

(38)

Surface tensions at evaporator and condenser ends are found from literature or

ChemCAD. Since our model is meant for steady state simulations, surface
tensions at these ends can be input as single parameters
Vapour Liquid Equilibrium
Compositions at the interface follow the relationship

yi =

i yi
at r = r1
i yi

22

(39)

Relative volatility for component i is given by the following equation where the
least volatile component should be chosen as nc, although this is just a matter of
convention.

Pivap i
i = vap
Pnc nc

(40)

Vapour pressures for pure components are obtained from correlations found in

Perrys by the equation.

E
Pivap = exp E1 + 2 + E 3 ln(T ) + E 3T E 4

(41)

By the modified Raoults law and the assumption of bubble point at all positions,

the
f
ollowing
e
quation
m
ust
b
e
o
beyed.

(P

vap

i xi ) = P

(42)

The activity coefficients are a function of composition, which can be found from

Wilsons equation or for a binary system, it is much simpler to regress data

obtained from ChemCAD.

i = f ( x1, x 2 ...x nc )

23

(43)

4 Case study: Seok and Hwang (1985)

The mathematical model equations used in gProms are shown below, along with
the variables and parameters assigned. Actual values for variables and constants
used in the equations are included in the raw data file attached. The results of
our model are then compared to experimental data as well as the model
developed by Ramirez-Gonzalez (1992).

4.1 Equations
Mass Balances

2
rn
x A
2 x A Deff x A
x
= Deff
uG A kL r1 ( x A x Ai ) + 2 A,Feed 2
= 0
2 +
t
z
z z
z
CL r2 r12

y A
2 yA
y A
= DAB,G
+ 2r1kG ( y Ai y A ) = 0
2 + uG
t
z
z

Equimolar counter diffusion

kCL CL (x A x Ai ) = kCG CG (y Ai y A )

Vapour liquid equilibrium

yi =

i yi
at r = r1
i yi

i =

Pivap i
Pncvap nc

E
Pivap = exp E1 + 2 + E 3 ln(T ) + E 3T E 4

(P

vap

i x i ) = P i = f (x A )

i = H i,1 x12 + H i,2 x1 + H i,3

Fluid flow
8rp 3 cos (Tc ) (Te )

uL =
150(1 ) 2 L
Leff

u (r 2 r 2 )C
uG = G L L 2 2 1 L
rC

( )

n A, feed =

F
at z = z feed : z feed + dzF
2r2 dz F

24

Mass transfer coefficients

kG =

uG

ScG 2 / 3

kL =

uL
Re Sc 2 / 3 - alpha = 20.4, beta = 0.815

Re =

L uL d p

L

Sc L =

L

L DAB,L

ScG =

G

G DAB,G

Physical properties

L,pure (T) = io exp(bT)

ln( L,mix ) = x A ln( L,A ) + x B ln( L,B ) + x A x B GAB

GAB (T) = 1 (1 GAB,0 )

Deff = f (x A )

(573 T )
275

NC

= x i i

i=1

CL = L,A M w,A x A + L,B M w,B x B

CG =

n
P
=
V RT

Ancillary relationships

x A + x B = 1

y A + y B = 1

x Ai + x Bi = 1

y Ai + y Bi = 1

25

Assigned Variables
DAB0
DBA0
C

From eq 30 at average T
From eq 30 at average T
ChemCAD at condenser T
and x
ChemCAD at condenser T
and x
From eq 32 at average T
From eq 19 at average T
and x

E
DAB,G
CG,ave

F
xin
yin

From experimental data

From experimental data
From experimental data

ChemCAD at average T and y

L,ave
CL,ave

From experimental data

From eq 17 at average T and x

Device Parameters
r1, r2

Lt

0.093, 0.0105 m from P

literature
0.355 from literature
(G/L)
0.55 m
dp

Feed
location

101325 bar
From literature
0.0007 m, adjusted parameter,
starting point estimated from
Dunn and Reay (1994)
At z = 0.12 m

4.2 Results and discussion

x methanol (mol)

Methanol-Water Total Re]lux

1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Length (m)
Current Model

Experimental Results

Total reflux experiments for methanol water were used as a base case for
estimating pore size, dP,, which is why the model shows an almost perfect fit.

26

Ramirez-Gonzalez (1992) did not present a case study for this experiment so we
are unable to compare our model with theirs. For the boundary conditions, xin
was taken as 0.999 and yin, was 0.001. The velocity of the liquid is 0.16 m/s,
which is quite large but since the data was taken directly from Ramirez-Gonzalez
experiment, this was assumed to be true, though a possible error may have been
made in assuming that the area of flow was constant and equal to the cross
sectional area of the wick.

x methanol (mol)

Methanol-Water G/L = 1.09

1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Length (m)
Experimental Results

Ramirez-Gonzalez

Current Model

x methanol (mol)

Methanol-Water G/L = 1.21

0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Length (m)
Experimental Results

Ramirez-Gonzalez

27

Current Model

Using the dp, found from total reflux simulations, the cases of G/L > 1 were
simulated. The feed term is not thought to make a large difference in the
composition profiles as the liquid flow rate is much larger than feed flow rates,
which may be why Ramirez-Gonzalez neglected this term. The current model
shows a better fit for G/L = 1.09 but worse for G/L = 1.21 compared to Ramirez-
Gonzalez (1992). It should be noted that the current model shows a smoother
curve because Ramirez-Gonzalez only used 8 elements in the discretisation of
length while the current model uses 50. The boundary conditions for the vapour
phase inlet, yin, were significantly larger than the liquid composition at the
evaporator. This will be discussed at the end of the chapter. Model results for
ethanol-water experiments are also shown below.

Ethanol-Water G/L = 1.1

0.8
x ethanol (mol)

0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Length (m)
Experimental

Ramirez-Gonzalez

28

Current Model

Ethanol -Water Total Re]lux

x ethanol (mol)

1
0.8
0.6
0.4
0.2
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Length (m)
Experimental

Current model

The results for ethanol-water experiments do not show as good a fit as that of
methanol-water. One reason may be that dp was estimated using the methanol
water experiments as a lower dP would result in a sharper curve at the
evaporator end. It may have been better to estimate dP using both ethanol and
methanol experiments to find a compromise between fitting the two cases at
total reflux. More significantly, ethanol-water forms an azeotropic mixture and is
highly non-ideal at higher concentrations of ethanol. The estimation of activity
coefficients by regressing data found in ChemCAD did not show as good a fit for
ethanol compared to that of methanol.

4.3 Discussion

1. The vapour inlet compositions were not reported in either of the papers
used in this case study and hence had to be estimated. Ramirez-Gonzalez
assumed x = y at the condenser and evaporator ends but this does not
make much sense since the vapour should be richer in the lighter
component (ethanol/methanol) although it was found that this
assumption holds for total reflux methanol water experiments. It was
first though that the vapour composition would correspond to the liquid
composition by equilibrium relations. However, it was found that a larger
value of yin had to be used for cases with G/L >1 to fit the experimental
data, and this value was larger with higher G/L. This is likely to be due to
the fact that the column is modeled as a rectification section, neglecting

29

evaporation and condensation at the ends. Instead, liquid and vapour

flows in and out of the device at either ends, with ratios as reported by
experiments. In reality however, a higher G/L ratio results in a higher
heat input at the evaporator resulting in a) a higher relative volatility and
2) different mass transfer characteristics, which are not properly
described in this model.
2. Liquid and vapour velocites are surprisingly large, around 0.16 m/s and
10 m/s respectively. The assumption of constant flow area equal to that of
wick and vapour core cross sectional area for the liquid and vapour phase
respectively also results in a high flow rates, around 100 times larger the
feed. This could be why the feed term is neglected in Ramirez-Gonzalezs
(1992) model. What is actually happening is slightly ambiguous. Fanelli
reported that this assumption led to a better prediction of HETP
compared to variable flow area dictated by flow rates and velocity.
However, Sundberg (2007) reported that while liquid flow area varied
with flow rates, the surface of the wick was constantly wet. This should be
investigated in future work to improve the model.
3. It should also be noted that not all the equations developed in the
previous section are included in the model case study, the main reason
being to simplify the model for stability purposes. However, these
simplifications are not thought to be the main sources of error as these
values are calculated at average temperature and compositions and are
not expected to vary much along the column.
4. Heat balance is not included in this model and instead, T is a function of
liquid composition at the interface and is constant in the radial and
angular direction. In reality it should be the other way round with
compositions as a function of temperature through relative volatilities.
This could be included in future work to further improve the model.
5. Although the model seems to fit experimental data fairly well, it is by no
means good enough to be used to simulate column performance in the
absence of experimental data as a fair amount of estimating, particularly
in yin, to fit the data.

30

5 Case study : Fanelli (2007)

This section is a case study on experiments and model developed by Fanelli
(2007). The microdistillation device was in vertical orientation with liquid
flowing due to gravity with mesh to guide flow. There was no feed and
experiments were conducted using hexane and cyclohexane. They developed a
of a 2 dimensional model, which will be compared to our current model.

5.1 Equations

Differential mass balance

kL r1 ( x A x Ai )
x A
2 x A Deff x A
x A
= Deff
+

G
t
z 2
z z
z
r2 r1

y A
2 yA
y A kG ( y Ai y A )
= DAB,G
+

2 + uG
t
z
z
r1

Equimolar counter diffusion

kCL CL (x A x Ai ) = kCG CG (y Ai y A )

Vapour liquid equilibrium

yi =

i yi
at r = r1
i yi

i =

Pivap i
Pncvap nc

E
Pivap = exp E1 + 2 + E 3 ln(T ) + E 3T E 4

i = f (x A )
Fluid flow
u (r 2 r 2 )C
uG = G L L 2 2 1 L
rC

( )

Mass transfer coefficients

Re =

L uL d p

L

Sc L =

L

L DAB,L

31

ScG =

kG =

uG

ScG 2 / 3

kL =

uL
Re Sc 2 / 3

G

G DAB,G

Physical properties

L,pure (T) = io exp(bT)

ln( L,mix ) = x A ln( L,A ) + x B ln( L,B ) + x A x B GAB

GAB (T) = 1 (1 GAB,0 )

Deff = f (x A )

(573 T )
275

NC

= x i i

i=1

CL = L,A M w,A x A + L,B M w,B x B

CG =

n
P
=
V RT

Ancillary relationships

x A + x B = 1

y A + y B = 1

x Ai + x Bi = 1

y Ai + y Bi = 1

5.2 Results and discussion

32

Liquid composition pro]ile for

case 1
0.9
x Hexane (mol)

0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

Length (m)
Current Model

Fanelli

A porosity of 0.7 was assumed for this case, which is typical of steel mesh used in
heat pipes. Parameter dP, was then adjusted to fit the model results as reported
by Fanelli and a value of 0.045 m was found to be the best value. This is much
higher than the usual >0.001 m found in literature. The model uses the low mass
transfer coefficient correlation for the liquid side, consistent with the
recommendation that it be used for low Re, which is around 10 along the column.

33

Driving force between bulk phase and

interface
Concentration difference

0.14
0.12
0.1
0.08
0.06
0.04
0.02
0
-0.02 0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

Length (m)
Liquid Side - Current Model

Vapour Side - Current Model

Liquid Side - Fanelli

Vapour Side - Fanelli

The driving force for mass transfer, ie bulk composition interfacial

composition, is shown above and compared with that of reported by Fanelli
(2007). The current model is in agreement with Fanellis (2007) model in that
the vapour bulk phase is much closer to equilibrium than the vapour phase
though this is not surprising as diffusion is much better in vapour. The difference
in liquid driving force is most likely due the assumption of linear change in
volatility along the column by Fanelli while the current model uses activity
coefficients and vapour pressures for volatility. In general however, the shape of
the graph is similar.
The driving force is used to calculate the height of a theoretical plate (HETP)
using the equations below and with the results compared to that of Fanellis
(2007) and experimental:
x Aout, j

nj =

x Ain, j

dx A , j
Length

and HETP j =
x A,ij x A, j
nj

HETPtotal = HETPvap +

mG
HETPliq
L

34


Case 1

Case 2

HETP
(cm)
Liquid
Vapour
Total
Liquid
Vapour
Total

Fanelli

Current
Model
1.27
0.03
1.3
1.95
0.03
1.98

1.2
0.5
1.7
1.7
0.9
2.4

Experimental
-
1.3
-
2.1

It is observed that the current model overpredicts the proportion of HETP in the
liquid phase to the vapour phase compared to Fanellis (2007) model. Fanellis
(2007) also concluded that since the flow rates had more of an effect on the
vapour HETP, mass transfer was controlled by the vapour phase. However, the
current model shows that flow rates had no effect on the vapour HETP and mass
transfer was controlled by the liquid phase. We may conclude then that the
current model overpredicts the mass transfer capability of the vapour phase,
though this cannot be confirmed since the current model actually better predicts
the total HETP.

35

6 Conclusion
The model was verified against case experiments as well as their simulations
with moderate success and this was after degree of parameter estimation. Hence,
the model is not suitable for simulations without experimental work.one of the
main issues is with the area of liquid flow, which is likely to be the source of
errors. The question of whether mass transfer coefficients for packed beds are
valid for predicting microdistillation devices remain unsolved. A more accurate
study could be made given more experimental data, particularly porosity and
particle diameter. For future work there are several recommendations:
1) Implementation of heat balances to enable a more accurate modelling of
the evaporator and condenser ends.
2) A proper comparison between this one dimensional model with mass
transfer coefficients and the two dimensional model such as the ones
used by Fanelli (2007) and Tscherjaew (1997)
3) Extension of the model to multicomponent systems since binary systems
are quite rare in real life applications. Work by Tscherjaew would be a
good starting point for this work.

36

7 Notation
Letters

Area (m2)

Concentration
(mol/m3)
Cp
Heat capacity
(J/mol.K)
D
Mass diffusivity
(m2/s)
dp
Pore diameter (m)
e
Molar energy
(J/mol)
F
Feed flow rate
(mol/s)
G
Vapour flow rate
(mol/s)
hL,hG Specific enthalpy
(J/mol)
Hvap Heat of
vaporisation
hT
Heat transfer
coefficient
(W/m2.K)
kc
Mass transfer
coefficient (m/s)
kT
Heat conductivity
(W/m.K)
K
Permeability (m2)
L
Liquid flow rate
(mol/s)
Mw
Molecular weight

Density (kg/m3)

Molar flux
(mol/m2.s)
Pressure (Pa)

Heat flux (W/m2)

Surface tension
(N/m)
Constant

rP

Pore radius (m)

Re

Reynolds number

Relative
volatility
Subscripts

Sc
T

Schmidt number
Temperature (K)

A, B
G,L

Species A or B
Gas or liquid

Internal energy
(J/mol)
Velocity (m/s)

Feed

Species i

Liquid mole
fraction
Vapour mole
fraction
Axial position (m)

z, r,

eff

Directions

v
x
y
z

Symbols

effective

Porosity (-)

Viscosity (Pa.s)
Angle ( )

Constant

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