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Simina Alungulesa (260CHEE

639 135)
351
COUNTER-CURRENT
WASHING
McGill Processes
University
Separation
CASCADE

Assignment #1

The following experiment is an attempt at simulating the process of a


counter-current washing cascade by decreasing the salt fraction in salt water
present in a sand slurry.
EXPERIMENTAL PROCEDURE
The experimental procedure implemented involved a starter pack of 5 stage
cups, 15 cups containing 100 ml of demineralized water and 15 containing salty
slurry. The slurry was prepared by making a NaCl (table salt) solution with a
conductivity of about 14 mS/cm and filling the cups with about 90 ml of this
solution. The conductivity of the salt solution was lower than the one prescribed
because the addition of sand actually increased its conductivity. Therefore, an
appropriate amount of sand was added to obtain a volume of approximately 100 ml
and an average conductivity of 15.5 mS/cm per slurry cup. A cup of fresh water and
slurry was placed beside each stage and the process was started by mixing these
cups into their stage cup and separating them back into their respective cups. The
mixing process was done by rapidly stirring the slurry cup and transferring it into
the stage cup followed by the addition of the water. The stage cup was then stirred
to ensure uniform concentration and left to decant. The separation step was done
by using a syringe to transfer 100 ml of the new salt solution (waste water) back
into its initial water cup and the remaining salt solution with the sand (cleaner
slurry) was transferred back into the slurry cup. The fresh water cups followed the
same order as the stage cups (i.e. fresh water cup 1 started out next to stage cup 1)
whereas the slurry cups were placed the opposite way (i.e. slurry cup 1 was next to
stage cup 5). The same mixing and separation procedure was then repeated as the
slurry cups moved right and the water cups moved left. For the first ten cups, the
conductivity of every exiting cup from the washing cascade was measured and this
allowed to visualize the stabilization of the outlet concentration.
TRANSIENT TO STEADY STATE TRANSITION
The graph presented below illustrates the evolution of the washing cascade
towards steady state where the conductivity data in the transient zone represents
the first five cups of slurry and waste water that exited the counter-current washing
cascade. The time axis is in the fact the number of the cup of slurry or waste water
exiting which means that the fifth cup exiting the cascade is supposed to have the
1

equilibrium concentration and thus, the following cups should have the exact same
concentration as the system has reached steady-state.

Transient State
State

Fresh water

Steady

Slurry

Figure 1: Conductivity of slurry and waste water exiting counter-current washing cascade

It can be noted in Figure 1 that the conductivities of both the slurry and the
waste water have in fact reached constant values around the fifth cup and thus,
since conductivity is proportional to salt concentration, it can be concluded that the
amount of salt in the slurry is decreasing as that of the waste water is increasing. It
makes sense that steady-state is reached at slurry/water cup 5 because from this
cup on, every cup of slurry will have seen five cups of water and there are actually
five stages of washing occurring.

CONVERSION BETWEEN CONDUCTIVITY AND CONCENTRATION


The conversion between conductivity and concentration was done by using
the TDS factor (total dissolved solids) for NaCl which was assumed to be constant at
0.49 (Fisher , 2011). Therefore, the following equation was used:

[ ]
[ ]

mg
L
=TDS factor
S
Conductivity
cm

Concentration

Equation 1: Conductivity to concentration conversion

The following sample calculation illustrates the equivalent salt concentration

salt ,
C

corresponding to the conductivity of the incoming sand slurry

C
( ) into

the washing cascade:

C =15.5

mS
S
15 500
cm
cm

salt ,=15500

S
mg
g
0.49=7 595
7.595
cm
L
L
C

This concentration was then used to calculate the mass fraction of salt in the
underflow liquid ( X

by assuming the density of water is

g
c m3

g
g
7.595 =7.595
L
kg
X =

7.595 g
=0.007595
1000 g

Measuring the conductivity for exiting cups only, allows for information about
the salt concentration of the general system (i.e. control volume includes all five
stages of washing) but a concentration profile can be constructed by measuring the
conductivity at each stage. This was done using the last five cups remaining. The
results obtained experimentally were compared with the calculated salt mass
fractions at each stage.
3

CONCENTRATION PROFILE Stage-by-stage calculation


The stage-by-stage calculation procedure was done by following the same
model as the one proposed in Separation Process Engineering (Wankat & Hall,
2011):

y N +1

y j +1
xj

xN

Figure 2: Stage-by-stage calculation procedure


model

Note that:

y=mass fractionof salt overflow liquid


x=mass fraction of salt underflow liquid

O=100 ml 0.0001kg (underflow liquid )


U=90 ml 0.00009 kg (overflow liquid )

From this model, the following equation was used to solve for the salt fraction
in the slurry at each stage where O and U are assumed to be constant throughout
the process:

x j=

O
U
y j +1 y N+1 + x N
U
O

Equation 2: Salt mass fraction in underflow liquid, taken from (Wankat & Hall, 2011)

In order to visualize how this model was applied to this experiment, the
following flowchart illustrates the moment at which the last cup has just entered the
washing cascade and mixing and separation has occurred (i.e. the upper cup
15 and lower cup 11 have the same salt concentration):
4

Figure 3: Counter-Current Washing Cascade Mechanism

The calculation was done from right to left which means that the first mass
balance is done at stage 5 (the other way would have been possible as well). This
implies that
and

y N +1

and

xN

are known and, in this case, they are equal to

x out . It is also important to note that

xN

and

y j +1 are always equal

because these fractions are those after mixing and separation have occurred which
is why the upper cup 15 and the lower cup 11 have the same salt fraction.
Assuming that the cascade is infinite, it can now be reasoned that in order for the
cups 15 and 11 to have a certain salt concentration, it is because the cups after
them mix and result into these equal concentrations at steady-state. From this, we
can back-calculate the salt mass fraction that the slurry has before entering stage 5
and mixing with the water which results in the known concentration of cup 11. It is
also important to note that cup 11 has the salt concentration of the exiting clean
sand.
A sample calculation around stages 4 and 5 illustrates the stage-by-stage
calculation procedure in order to obtain a concentration profile. By referring to

Figure 3 and doing a mass balance around stage 5 allows to solve for the salt mass
fraction in cup 12 using Equation 2 as follows:

x 12=

0.0001 kg
0.00009 kg
0.0013230+
0.001323 =0.002793
0.00009 kg
0.0001 kg

*The salt mass fraction of 0.00132 is the salt fraction of the exiting slurry cups.
Since the cup of slurry 12 will have the same concentration as the waste
water cup 14, the mass balance around stage 4 can be done again by following the
model in and calculate the salt mass fraction of the slurry cup 13:

x 14 =

0.0001kg
0.00009 kg
0.0027930.001323+
0.002793 =0.004426
0.00009 kg
0.0001 kg

*To obtain the concentration from the mass fraction, it is sufficient to multiply by 1000.

y N +1

It is important to note that the incoming waste water denoted by

has

the same salt mass fraction as the waste water cup 15 and the outlet salt mass
fraction denoted by

xN

and

y j +1 will be equal since they denote the cup of

slurry 12 and the waste water cup 14, respectively. In other words, mixing slurry cup
13 and water cup 15 leads to the new and equal salt concentrations of slurry cup 12
and water cup 14. Thus, the same calculation procedure was applied to every stage
in order to obtain a calculated concentration profile. The results obtained
following the sample calculations can be viewed in Table 1 including the additional
values (highlighted) used as the starting point for the stage-by-stage calculation
which are

y N +1

for the water stream and

Stage

xN

for the slurry stream.

Water cup (W)

11W

12W

13W

14W

15W

Experimental Concentration
(g/L)
Calculated Concentration
(g/L)
Slurry (S)
Experimental Concentration

6.37

4.90

3.82

2.21

1.27

8.26

6.24

4.43

2.79

15S
5.98

14S
4.95

13S
3.72

12S
2.50

1.32
11S
1.27

10S
1.32
6

(g/L)
Calculated Concentration
(g/L)

8.26

6.24

4.43

2.79

1.32

Table 1: Experimental and Calculated Concentrations of Slurry and Water Cups at Each Stage

Fresh water - experimental

Slurry - experimental

Slurry/Fresh water - calculated


Figure 4: Concentration Profile (Experimental vs calculated data)

The graph shown above illustrates the comparison between values obtained
by measuring conductivity at each stage and calculating them. These salt
concentrations are those obtained after mixing and separating. The results of this
graph can be easily analyzed by referring to Figure 3 as it can be noted that the salt
concentration at stage 1 is the highest because that is the starting point for the salt
slurry and the endpoint for the fresh water which has the accumulated salt of five
stage of washing. Looking at the experimental data only, it can be concluded that
proper washing has occurred as the salt concentration after mixing and separation
of the slurry is more or less equal to that of the waste water. These slight
fluctuations can be due to the fact that the salt concentration of each initial cup of
slurry was approximated to an average of 15.5 mS/cm. As well, this implies that as
the salt concentration of the slurry decreases, that of the water increases by the
same amount. However, when comparing these results with the calculated ones, it
can be seen that the salt concentration of the exiting waste water and entering
slurry cup are supposed to be higher than the ones measured. In other words, with

the experimental outlet salt concentration of the slurry, calculations indicate that
the initial salt concentration in the slurry should have been higher. Furthermore, it
can be noted that if the stage-by-stage calculation was done the other way
around (left to right), this would imply that the inlet salt concentration in the slurry
would be set (to the measured value) and the outlet one would be calculated. In
that case, the calculations would conclude that a cleaner slurry should be obtained.
Overall, the results obtained are concordant with the theory but different sources of
error altered their efficiency.
Possible sources of error can be attributed to the procedure and the
instrumentation used as cross-contamination could have occurred between slurry
and water cups at different stages in the washing cascade. For instance, when
pouring the water and the slurry into the stage cup, small quantities of salt solution
or sand could remain in the cups and slightly increase the salt concentration as the
cleaner slurry and the waste water are poured back into their original cups. Another
source of error can be due to the fact that the stirring in the stage cup was not done
properly and some of the salt was not completely dissolved in the water and could
have been stuck in the sand leading to a less clean slurry exiting the cascade.
Lastly, the estimation of the porosity of the sand slurry was not necessary in
this experiment as it was mentioned in the experimental procedure that the amount
of salt solution was controlled before actually adding the sand. However, a way to
determine this value would be to set certain known volume of sand and add water
to it until it reaches the surface of the sand. The amount of water that fills the voids
between the sand particles can then be reported as the sand porosity.

REFERENCES
Fisher . (2011). Conductivity and Total Dissolved Solids. Retrieved from Thermo
Scientific:
https://static.fishersci.com/cmsassets/downloads/segment/Scientific/pdf/Wate
rAnalysis/Log93TipConductivityTDS.pdf
Wankat, P., & Hall, P. (2011). Separation Process Engineering.

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