Janwillem Rouweler; j.w.mrouweler@freeler.nl; Nov.

24, 2014

Multi-stage cross flow solid-liquid extraction/leaching/washing:

a) Mass of solid product L kg and of solvent V kg during each step are constant
Assume that after each extraction step, the mass of the fresh product, but also the
mass of the extracted product (= spent solids), will NOT change during the process. So
the solvent will take up the place of the mass of removed soluble component.
Assume that in every extraction step fresh solvent will be added to the (spent) solid.
This is the meaning of “cross flow”.
Assume the solvent you want to use is water.
Assume the fresh product, so before the first extraction step, consists of:
- mass fraction xC of insoluble dry matter (called “inert”); xC = mass fraction inert;
- mass fraction x0 of the soluble substance you want to remove; x0 = initial mass
fraction of the soluble substance, prior to the first extraction step.

L = The mass of the original product is L kg;

this L kg is also the mass of the extracted product (spent solids) after each
extraction step.
V = The mass of the fresh solvent (water) added per each extraction step is V kg;
this V kg is also the mass of the individual extract after each extraction step.
The equilibrium constant k or Nernst constant k per extraction step for this process:
concentration of soluble substance in extract resulting from nth extraction step
k= —―—————————————————————————————————————————
concentration of soluble substance in spent solids from nth extraction step
k = 1/(1 - xC) for solid liquid extractions.

The separation factor S per extraction stage is:

mass of soluble substance in extract resulting from nth extraction step
S= ——————————————————————————————————————————
mass of soluble substance in spent solids resulting from n th extraction step
S = k•V/L for solid-liquid extractions.

After a total number of N extraction steps, the symbols and equations are:
Mass fraction soluble substance in spent solids after N extraction steps is xN.
Degree of loss of soluble substance F = fraction of the original mass of soluble
substance which is still present in spent solids after N extraction steps;
so F = x0/xN or F = 1/(1+S)N
Required number N of cross flow extraction steps to get a degree of leaching F is:
- 10logF
N = ————————
10
log(1+S)
Mass fraction of soluble substance yM in the individual extract of the Mth
extraction:
x0 • k
yM = ——————
(1 + S)M

Mass fraction of soluble substance yTOTAL in the total extract of all N extracts
together:
x0 • k (x0 - xN) • L
yTOTAL = ———— • (1 - F) or yTOTAL = ————————
N•S N•V
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -2-

Kremser - Souders-Brown graph for multi-stage cross flow extraction

How to use the Kremser graph:

Example 1: How many cross flow extraction steps N are required to reduce the % sugar from
2% to 0.01% in 25 kg of a solid product, by using 5 kg of fresh water in each wash step as a
solvent? Product consists of 75% of insoluble dry matter, 23% of water, 2% of sugar.

Mass of fresh product: L = 25 kg. (This is also the mass of the “spent solids” after each step).
Mass of fresh solvent added at each extraction step: V = 5 kg.
Initial mass fraction of soluble substance in fresh food product: x0 = 2%/100% = 0.02.
Mass fraction of soluble substance in last spent solids, after N extraction steps:
xN = 0.01%/100% = 0.0001.
Mass fraction inert: xC = 0.75.
Equilibrium constant equation: k = 1/(1 - xC) = 1/(1 - 0.75) = 4.

Required number of cross flow extraction steps N can be read at horizontal axis at graph bottom.
To find N, you first need to know the F (at left vertical axis) and the S (at “diagonal” lines).
The degree of loss of soluble substance F: F = xN/x0 = 0.0001/0.02 = 0.005 = 5•10-3.
Separation factor: S = k • V/L = 4 • 5/25 = 0.8.

Now go to left axis, at F = 5 • 10-3. and draw horizontal line.

Go to “diagonal” line of S = 0.8; then find intersection of that S line with hor. line F = 5 • 10-3.
At the intersection, read value of N at base line of graph: N = 9 cross flow extraction steps.
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -3-

Example 1, solved by using the “Kremser” equations of page 1:

Example 1: How many cross flow extraction steps N are required to reduce the %
sugar from 2% to 0.01% in 25 kg of product, by using 5 kg of fresh water in each wash
step as a solvent?

Answer 1:
Product consists of 75% of insoluble dry matter, 23% of water, 2% of sugar.
Mass of fresh product to be extracted: L = 25 kg.
Mass of fresh solvent added at each extraction step: V = 5 kg.
Mass fraction inert: xC = 0.75.
Initial mass fraction of soluble substance in fresh food: x0 = 2%/100 = 0.02.
Mass fraction in last spent solids, after N extraction steps: xN = 0.01%/100 = 0.0001.
Equilibrium constant k = 1/(1 - xC) = 1/(1 - 0.75) = 4.
The degree of loss of soluble substance F: F = xN/x0 = 0.0001/0.02 = 0.005 = 5•10-3.
Separation factor S: S = k•V/L = 4 • 5/25 = 0.8.
Required number of cross flow extraction steps N is:
- 10logF
N= ———————
10
log(1+S)

Substitution:
- 10log0.005 2.30
N = —————————— = ————— = 9.0
10
log(1+0.8) 0.255

So: N = 9 cross flow extraction steps.

The fraction of soluble component in the TOTAL extract (= mixture of extracts 1 to 9) :

x0 • k (x0 - xN) • L
yTOTAL = ———— • (1 - F) or yTOTAL = ————————
N•S N•V

0.02 • 4
yTOTAL = ————— • (1 - 0.005) = 0.0111
9 • 0.8

Check: Added to the product was a total amount of 9 x 5 kg solvent = 45 kg solvent.

Initially the mass of sugar present in product: 2% of 25 kg = 0.5 kg of sugar.
This 0.5 kg of sugar, dissolved in the total mass of 45 kg of solvent, makes
(0.5/45)*100 % = 1.11 % of sugar.
Thus the mass fraction of sugar in the total extract = 0.0111.
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -4-

Example 2:
1000 kg of a solid product contains 5% water, 94.9% of insoluble inert, and 0.1% of a
water soluble toxin.
By 5x cross flow washing with solvent water, the % of toxin should be reduced to
0.0001%.
Assumption: The total mass of the (spent) product (inert + water + toxin) during the
extraction will NOT change, thus stay constant at L = 1000 kg.
How much kg of fresh water (V kg) will be required for each of the 5 washing steps?

Answer 2:
Mass of fresh water (solvent) for each of the washing steps is V kg.
Use the Kremser graph of page 2 to find the value of V.

Mass of solvent V, required in each extraction step, can be calculated from equation
S = k•V/L;
in Kremser graph the S-lines are “diagonal”; so in graph find correct S line; --> S
Also: k = 1/(1 - xC),
and F = xN/x0 (F at left vertical axis of Kremser graph),
and number of extraction steps N = 5 (N at base line of Kremser graph).

Mass of fresh product, and of spent solids: L = 1000 kg.

Required number of washing steps: N = 5.
Mass fraction of inert xC in product: xC (= 94.9%/100%) =0.949.
Mass fraction of initial toxin in fresh product: x0 (= 0.1%) = 0.001 = 1•10-3.
Required mass fraction of toxin in spent solid after N = 5 washing steps:
xN = 0.0001% = 0.000001 = 1•10-6.

Substitution:
F = xN/x0 = 0.000001/0.001 = 1•10-6 / 1•10-3 = 10-3 = 0.001 = F.
k = 1/(1 - xC) = 1/(1 - 0.949) = 1/0.051 = 19.6 = k.

Find value of S in Kremser graph:

at F = 0.001 = 1•10-3 (at left vertical axis): draw horizontal line,
and at N = 5 (at Base line of graph): draw vertical line;
these lines intersect at a diagonal line of about S = 2.95.

Substitution of S = 2.95, k = 19.6, and L = 1000

in equation S = k•V/L results in:
2.95 = 19.6 • V/1000; so V = 1000 • 2.95/19.6 = 150.5 kg = V.

So N = 5x cross flow washing, each time with V = 150.5 kg of fresh water,

results in a toxin reduction from 0.1% to 0.0001%.
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -5-

b) What if initial mass of solid product L kg increases due to soaking/swelling

Often, dry foods will swell when in contact with the solvent during washing/extracting.
Examples are tea leaves, ground coffee beans, etc.
Usually the swelling takes place during the first extraction step. And the spent solid
remains swollen.
The Kremser equations about cross-flow extraction can still be used, but then the food
should be made to swell prior to the first extraction step. The Kremser equations then
will have to be based on the swollen solid product!
So in case of a swelling product:
L = mass of solid to be extracted/leached, after being swollen.
x0 = initial mass fraction of the soluble substance in the swollen fresh product, prior to
the first extraction step.
xC = mass fraction inert in the swollen product.

Example 3: 400 kg of dry tea leaves consist of about 100 kg of soluble substances,
280 kg of inert material, and 20 kg of water. After swelling with water and draining, the
400 kg of dry tea leaves has increased to 1000 kg of swollen leaves.
3a) How many cross flow extraction steps, each with 500 kg of fresh water on the
swollen tea leaves, are required to extract 99.9% of the initial amount of soluble
substances?
3b) Calculate the concentration of soluble substances in the total extract.

Worked answer:
Given: The mass of dry tea leaves swells from initially 400 kg to 1000 kg after
swelling; so the mass of product (and thus the mass of spent solids) is L = 1000 kg.
The initial mass fraction of soluble substances x0 = mass solubles/mass swollen leaves
x0 = 100 kg/1000 kg = 0.1 = x0.
The mass fraction inert xC = mass of inert/mass of swollen leaves = 280 kg/1000 kg; so
xC = 0.28.
The mass of fresh solvent (water) in each extraction step V = 500 kg.

Answer 3a) Required number of cross flow extraction steps N =

- 10logF
N= ———————
10
log(1+S)
in which
F = degree of loss of soluble substance F = fraction of the original mass of soluble
substance which is still present in spent solids after N extraction steps;
or F = x0/xN or F = 1/(1+S)N
x0 = mass faction of solubles in 1000 kg swollen “fresh” food = 100 kg/1000 kg,
= 0.1 = x0;
Solubles should be 99.9% removed, so after N extraction steps only 0.1% of the
original mass of 100 kg of solubles should be present; 0.1% of 100 kg = 0.1 kg
solubles in the last 1000 kg spent solids. So xN = mass fraction solubles in last
1000 kg spent solid = 0.1 kg/1000 kg = 0.0001 = xN.
Thus F = x0/xN = 0.1/0.0001 = 0.001 = F.
(Simpler: The process should extract 99.9% of the initial amount of soluble
substances; so 0.1% of the initial amount will remain in spent solids; so degree
of loss of soluble solids F = 0.1% = 0.001).
S = k•V/L = separation factor for solid-liquid extractions.
k = 1/(1 - xC),
in which xC = mass fraction inert in swollen food = 280 kg/1000 kg
xC = 0.28
thus k = 1/(1 - 0.28) = 1.389 = k
V = 500 kg
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -6-

L = mass of swollen food = 1000 kg = L

So S = k•V/L = 1.389 • 500/1000 = 0.699 = S

Substitution of F = 0.001 and S = 0.278 in equation

- 10logF
N= ——————
10
log(1+S)
results in:
N = -[10log0.001/10log(1+0.699)] = 3/0.230 = 13
So 13x 500 kg fresh water will reduce the amount of soluble substances to 1/1000 of
the original amount.

Solve the required number of extraction stages N by use of Kremser graph:

To find the number of extraction steps N (horizontal line at bottom of Kremser graph),
we have to find:
F (vertical line at left of graph);
S (“diagonal” lines in graph).
As has been calculated above: F = 0.001 = 1•10-3 (left vertical axis);
S = 0.699 (“diagonal” lines).
The intersection of a horizontal line through F = 10-3 and the diagonal line S = 0.699,
shows that (at bottom line of graph) N = 13 stages.

Answer 3b) Calculate the concentration of soluble substances in the total extract.
According to the equations at page 1, the fraction of soluble component in the TOTAL
extract (= mixture of extracts 1 to N = 13) is:
x0 • k (x0 - xN) • L
yTOTAL = ———— • (1 - F) or yTOTAL = ————————
N•S N•V
All symbols to be based on the swollen feed and swollen spent solids.
x0 = 100 kg solubles per 1050 kg fresh solids = 100/1050 = 0.0952 = x0.
k = 1/(1 - xC), in which xC = mass fraction inert in swollen food = 280 kg/1000 kg;
so xC = 0.28; thus k = 1/(1 - 0.28) = 1.389 = k.
N = 13 extraction steps; calculated at answer 3a).
S = k•V/L = 1.389 • 500/1000 = 0.6945 = S.
F = 0.1 % = 1/1000 = 0.001 = F.
Substitution in equation of the mass fraction of solubles yTOTAL in the total extract
x0 • k
yTOTAL = ———— • (1 - F) results in:
N•S
0.0952 • 1.389
yTOTAL = ———————————— • (1 - 0.001) = 0.0146
13 • 0.6945
So 0.0146 = mass fraction solubles in total extract yTOTAL = 0.0146

Different way of calculation of the fraction of solubles in total extract:

Total mass of solubles in original feed = 100 kg.
Total mass of water added by 23 extraction steps = 13 • 500 kg = 6500 kg.
If all 100 kg of solubles would be present in the 6500 kg total extract,
the mass fraction solubles in the total extract would be 100/6500 = 0.0154 = yTOTAL.
This roughly calculated fraction of solubles in the total extract is only a fraction larger
than the yTOTAL = 0.0146 of the equation on yTOTAL.
The fraction solubles in the total extract should be a bit smaller because in reality some
soluble solids still are present in the 50 kg of solution clinging to the 1000 kg of dry
leaves.
Multi-stage cross flow solid-liquid extraction solved by Kremser equations and graph -7-

Example 4: To remove contaminations such as soil, dirt, and chemicals, 1000 kg of

leafy vegetables are submerged in a tank with 1000 kg of agitated fresh water.
After removing from the washing tank, draining, and shaking on a vibrating perforated
belt, the washed vegetables have a mass of 1050 kg.
4a) Why did the mass of the vegetables increase during washing?
4b) Which fraction of the original contamination is still attached to the 1050 kg washed
wet vegetables?
4c) To safe water, the 1000 kg of fresh dry vegetables first were sprayed with 50 kg of
fresh water, to soak and “dissolve” the contaminants. Next the soaked 1050 kg of wet
vegetables are submerged in a tank with 100 kg of fresh washing water, drained,
shaked and submerged again in 100 kg of fresh water, etc.
How many times will this 1050 kg of soaked vegetables have to be submerged in a tank
with 100 kg of fresh water to remove the same amount of contaminants similar to 1x
submerging of 1000 kg dry vegetables in 1000 kg of fresh water?

Worked answer 4:
Answer 4a) The mass of the 1000 kg of leafy vegetables increased to 1050 kg because
some 50 kg of “dirty” wash water clings to the leafs.
Answer 4b) If all contaminants are dissolved in the 1000 kg of washing water, and
some 50 kg of that used washing water clings to the vegetables, about 50/1000 parts
of the original contamination will still be attached to the wet leafy vegetables, so a
fraction of 0.05 (or 5%) of the original dirt is still present at the 1050 kg vegetables.
Using Kremser equations for cross flow extraction of swollen product:
F = fraction of the original mass of soluble substance which is still present in spent
solids after N extraction steps (see page 1); F = 1/(1+S)N
We know that N = 1.
S = k•V/L, with L = 1050 kg swollen product = 1000 kg vegetables + 50 kg clinging
water.
Thus the mass of solvent added to the swollen vegetables V = 1000 - 50 = 950 kg = V
= water added to the “swollen” leafy vegetables!
k = 1/(1 - xC),
with xC = mass fraction inert in 1050 kg = fraction of leafy vegetables;
so xC = 1000/1050, thus
k = 1/[1 - (1000/1050)] = 21 = k.
So S = k•V/L = 21•950/1050 = 19 = S.
So F = 1/(1 + 19)1 = 1/20 = 0.05; so a fraction of F = 0.05 of the original dirt is still
present at the washed wet leafy vegetables, or 5% of the original dirt is still present.
Using Kremser Graph for cross flow extraction of swollen productto find F. N =
1 (at bottom line graph), and separation factor S = 19 (diagonal lines). Unfortunately in
the graph the line S = 15 is the maximum. So this Kremser Graph can not be used.

4c) Find the number of times the 1050 kg soaked leafy vegetables have to be washed
with 100 kg fresh water.
Use Kremser graph to find N. Thus calculate F and S first, and next read the graph.
We know that F should be F = 0.05 (see answer 4b) after Nx of washings.
S = k•V/L
in which k = 1/(1 - xC); xC is 1000 kg leaves in 1050 kg wet vegetables
so k = 1/(1 - 1000/1050) = 21
V = 100 kg of fresh water; L = 1050 kg of soaked vegetables
so S = 21 • 100/1050 = 2 = S
The intersection of “diagonal” line S = 2 and horizontal line F = 0.05 = 5•10-2 in the
Kremser graph gives a value of N = 2.7. So 3x washing in 100 kg of fresh water.
Using Kremser equations for soaked solids:
- 10logF - 10log0.05 1.30
N = ———————— = ——————— = ——— = 2.72: 3x washing in 100 kg fresh water.
10 10
log(1+S) log(1+2) 0.477