ChE 135 - Process Engineering Laboratory Formal Report

Determination of Settling Characteristics of Kaolin Powder Using

Batch Settling Tests
Camille Margaret S. Alvarillo​ 1​, Maria Crispina B. Buensuceso​1​, Ysabel Marie C. Gonzales​1​, Jaron Nicolas T. Uy
1​
​University of the Philippines Diliman, Quezon City

Abstract. Batch settling tests were performed to determine the various settling characteristics of different
concentrations of kaolin powder, such as settling velocity and concentrations at different points in the process.
Three samples of kaolin powder slurries (4%, 5%, and 8% w/v) were subjected to batch sedimentation,
wherein interface heights of the supernatant and the fluid with solids were recorded and plotted against time.
Furthermore, the effect of adding a coagulant (0.1 %w/v alum) to the 4%w/v slurry was observed. From this
experiment, it was determined that a lower concentration of kaolin and addition of a coagulant will allow faster
initial settling rates, with the sample having a settling rate of 0.7107 mm/s. This is further supported by
obtaining critical points through the Talmadge and Fitch (1995) method, and it was determined that the 8%
w/v had the highest critical concentration of 12.0737% w/v.
Keywords:​ sedimentation; gravity settling; slurry; kaolin powder; Talmadge and Fitch

1. ​Introduction According to Rhodes (2008), the batch

settling test can supply all the information needed
Sedimentation, also known as thickening, for the design of a thickener for separation of
is a process of fluid-solid separation by increasing particles from a fluid. This test involves a
solids content of a slurry through gravity settling suspension of particles of known concentration,
(Darby, 2001). which is then allowed to settle, and the positions of
the interfaces which form are monitored over time.
There are two kinds of settling behaviors: Furthermore, McCabe states that there are different
free settling, and hindered settling. In industrial zones as sedimentation proceeds.
applications, the concentrations of suspensions can
be high enough such that there are significant
interactions between the particles. The frictional
force exerted at a particular velocity relative to the
fluid is greatly increased, which implies that all
solids settle at a common velocity, regardless of
particle size. Thus, hindered settling takes place.
On the other hand, if the sedimentation rate of a
particle is less than its terminal velocity, a free
settling behavior is observed as the rate of which
particles settle is dependent on the particle size, Figure 1. Batch Settling Zones (McCabe et. al.,
and effects mutual interference is negligible 1993)
(Coulson et. al, 1991).
Initially, the solid is uniformly distributed
in the liquid, as in Figure 1a, with a total
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling
suspension height of Z​o​. After awhile, the solid
begins to settle and forms a clear liquid zone, A, as
shown in Figure 1b. Essentially, Zone A is
composed of a supernatant fluid with no solids. In
Zone B, the concentration of the solids is uniform
and is equal to the initial concentration because the
settling rate is also constant throughout this zone.
Another zone D, which is composed of the settled
solids, is also formed, while Zone C has a varying
solid concentration. The interfaces between Zones
C and B, and C and D may not be distinct, but that
of A and B is clear. Through time, the depth of
Zone A and Zone D increase, that of Zone B
decrease, and that of Zone C remains fairly
constant, as shown in Figure 1c. Eventually, Zone
B disappears as all the solid goes to Zones C and
D.
As the sedimentation proceeds, the
accumulation of solids at the bottom causes flocs
to compress, and liquid is expelled to the upper
zones. When the weight of the solid is equal to the
compressive strength of the flocs, the settling
process ends. Figure 2 shows a typical batch
settling curve of a slurry.
Figure 2. Batch Settling Curve (McCabe et. al.,
1993
From the curve, it can be seen that during
the early phases of settling, the velocity (slope of
the height vs. time plot) is fairly constant. When
Zone B disappears, the rate of settling starts to
decrease until the final height is reached. Settling
rates greatly depend on feed concentration, and in
the latter stages, on the initial height, Z​o​. In
general, the higher the initial concentration, the
smaller the rate of settling. This is because the
upward velocity of the displaced fluid is great, and
there would be steeper velocity gradients in the
fluid.
In this experiment, the slurries are made
up of water and Kaolin powder, with the solid
powder being a type of clay that is often used in
medicine. In the analysis of sedimentation data, it
is useful to create settling curves. With these plots,
the effects of slurry concentration on the settling
behavior of the powder can be determined, as well
as the effects of chemical coagulant-addition to the
sedimentation process.
2. ​Materials and Methodology
Tubes of the slurry solutions composed of
Kaolin powder and water were prepared as
follows.
Table 1. Slurry Solution Preparation
Water Kaolin Slurry
(mL) Powder Concentration
(g) (%w/v)
A 2000 80 4
B 2000 100 5
C 2000 160 8
In addition, Groups 1, 2, and 7 prepared
another slurry solution with the specifications of
Tube A, and added 0.1% w/v alum to the solution,
in lieu of Tube C.
Each slurry was transferred to its own
respective sedimentation tube, which was filled
until it was 90% full. The tubes were shaken, and
were then allowed to stand and were observed for
ten increments of 10 seconds, 30 seconds, 1
minute, and 5 minutes; five increments of 10
minutes and 30 minutes; and lastly, overnight.
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling
3.​ ​Results and Discussion
Three out of four of the settling zones
were evident in the observed batch sedimentation
processes. That is, Zones A, B, and D were all
distinct, as were their interfaces. Zone C was not
observed because the distinction between it and
Zone D was not clear. The following figure shows
the tubes at the point of final reading; that is, when
the solids have ultimately settled.
Figure 1. Settling Zones at Final Reading
Figure 3. Batch Settling Curve of Tube A (4% w/v Slurry)
Only Zone A (clear fluid) and Zone C
(sludge zone of heavier particles) are identified at
this point because the settling velocity of the
heavier particles are faster such that they coalesce
together. The lighter particles which have a slower
settling velocity are scattered in between Zone A
and Zone C, thus producing a blurred distinction
between the layers. This is why at early part of the
settling experiment, it is only Zone C’s height,
composed of the heavier particles, that is
measured. However, at the final reading, the
suspension of Zone C had reached its ultimate
height as all the solids, both light and heavy, had
been compressed.
The height of the interface, being the most
evident one of Zone A or B, of the observed
sedimentation tubes were then plotted against time,
thus obtaining the following plots. For Figure 3,
the sedimentation curves of the slurries containing
alum are superimposed against the slurries (of the
same concentration) that did not.
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

Figure 4. Batch Settling Curve of Tube B (5% w/v Slurry)

Figure 5. Batch Settling Curve (8% w/v Slurry)

ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling
Generally, the plots for all cases for all
participating groups depict the expected behavior
of batch settling curves, such that the plot is first
linear, then the rate of change begins to decrease
until the observed interface height is constant
towards the end of the sedimentation process.
Furthermore, Figures 3 to 5 (Tubes A, B, C,
respectively) indicate that the different groups had
gathered precise data following similar trends,
since the points of inflection occur at roughly an
average time of 1300 s for Tube A and 1400 s for
Tube B. For Tube C, the average time at the
inflection point was 1200 s.
In addition, from Figure 3, the solutions
containing alum appear to have steeper linear
portions, with the exception of that of Group 2.
Steeper linear portions may mean that the added
alum increased the initial settling speed of kaolin.
However, inconsistent results may have been
brought about by errors in measurement of both
the height of the settled kaolin and the time when
it was measured. Because the kaolin powder
settled faster, the different settling zone may have
been less distinct, thus making it more difficult to
measure the needed height.
Data from each group were subjected to
sedimentation calculations, such that their
respective initial settling rates were determined by
taking the slope of the linear portions. This is in
line with Kynch’s Theory of Sedimentation, which
states that the initial slope of the curve gives the
sedimentation velocity for the initial concentration
(v​o​). Sample calculations, as well as the
summarized data for each group are presented in
the appendix. Meanwhile, the means of the
determined initial settling rates for all participating
groups are listed in the following table.
Table 1. Initial Settling Velocities
Initial Mean
Concentration Settling Rate
(%w/v) (mm/s)
Tube A 4 0.6772
Tube A 4
0.7107
with Alum
Tube B 5 0.3431
Tube C 8 0.3415
From Table 1, it can be observed that Tube
A with alum resulted to the greatest average
settling velocity of 0.7101 mm/s, followed by the
slurry in Tube A without alum, with a mean
settling velocity of 0.6772 mm/s. Generally, it was
observed also that less initial amounts of Kaolin
powder corresponded to a faster settling rate. This
is expected because lower concentrations of
Kaolin powder would indicate less interference in
the motion between surrounding particles. Thus, it
can be said that the relationship between initial
concentration and settling rate is inversely
proportional. Furthermore, the added coagulant,
alum, allowed the particles to clump together, thus
increasing particle size, leading to an increased
initial rate of settling.
From the batch settling data, the final
concentrations of the slurry could also be derived
from the following equation, as stated by Kynch’s
Theory:
cf z f = co z o (1)
where ​c​o and ​z​o are
​ the initial concentration of
slurry and height of the interface, respectively,
while c​f ​and z​f are the final concentration of slurry
and height of interface, respectively.
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

Table 2. Final Slurry Concentrations coagulants increase the rate of sedimentation, as

this would yield more settled solids in the most
Initial Mean Final
Concentration Concentration concentrated zone of the tube.
(%w/v) (%w/v)
In addition, the overall relationship
Tube A 4 103.9229 between the initial concentration and the final
concentration is exactly the same as with what is
Tube A 4
110.1330 observed from settling velocities. That is, the
with Alum
greater the initial concentration, the slower the
Tube B 5 49.8820 settling velocity, and thus, there are less settled
solids in the zone in consideration.
Tube C 8 34.8962
To provide additional information to the
Table 2 shows that Tube A with alum has obtained data from the seven groups, the following
the largest average final concentration of statistical parameters were calculated for, as
110.1330% w/v, which agrees with hypothesis that summarized in Table 3.

Table 3. Statistical Analysis for Initial Settling Rates and Final Concentrations
Tube A Tube A with Alum Tube B Tube C

v​o C​f v​o C​f v​o C​f v​o C​f

Mean 0.6772 103.9229 0.7232 110.1330 0.3431 49.8820 0.0645 34.8962

Std. Dev. 0.1720 45.8064 0.1969 24.3885 0.1567 11.5525 0.0096 9.0565

Variance 0.0296 2098.2258 0.0388 594.7995 0.0245 133.4599 0.0001 82.0210

Skewness 1.624 1.1298 1.5765 0.0928 0.8578 0.6196 -0.1228 -0.0738

Min. 0.5447 62.4000 0.5827 86.0000 0.1194 35.7143 0.0532 23.7091

Max. 1.0170 188.2105 0.9483 134.7692 0.6379 66.9173 0.0752 45.8592

Based on Table 3, the data on the initial
settling rates and final concentrations of Tube C
had the least variance and standard deviation,
which only means that the data gathered was more
precise with only a difference of about 0.001 from
each other, although it must be noted that the
sample size is only four trials, as compared to
Tubes A and B, which had seven. Moreover, it can
be seen that data gathered from Tube C is highly
skewed to the left while data gathered from Tube
A, with and without alum, are highly skewed to the
right. This may be an indication that Tube A
achieved faster initial settling velocities given that
it had the smallest initial kaolin concentration.
Tube C, on the other hand, had slower initial
settling velocities which explains the skewness of
their data to the left side since its initial kaolin
concentration is higher. Overall, the data gathered
did not have any outlier, hence the mean presented
in Table 3 of the initial settling rates and final
concentration displays similar values to the data
gathered in the experiment. In addition, it was
observed that the standard deviation, variance, and
skewness of final concentration from Tubes A, B,
and C are relatively high. This is perhaps due to
subjective measurement of the final height of
kaolin which caused error in the data gathered.
The critical settling point can also be
determined using the settling curves. This is the
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

point that signals a slower settling rates. A less than that of the slurry without. This is another
graphical method proposed by Talmadge and Fitch indication that the addition of alum coagulated the
(1995) can be applied to approximate critical solid particles, allowing it them reach compression
points. This is done by taking the bisection of the settling faster.
angle formed by the tangents to the hindered
settling zone (initial slope) to the compression Statistical analysis was also conducted,
settling zone (final slope) of the batch settling and is summarized in the table below.
curve. The intersection of the bisector with the
curve gives the critical height, z​C​. Table 5. Statistical Analysis for Critical
Concentrations (%w/v)
Tube
Tube Tube Tube
A with
A B C
Alum

Mean 8.8182 6.7727 9.9316 12.0737

Std. Dev. 0.8998 1.0699 1.6629 0.6772

Variance 0.8097 1.1447 2.7654 0.4586

Skewness 0.5337 1.6301 1.2441 0.0908

Figure 6. Talmadge and Fitch Method
(Subosa, B.N, 2016) Min. 7.8892 6.0364 8.1818 11.2572

Max. 10.0541 8.0000 13.1818 12.9109

Meanwhile, the critical concentration, C​C​, can be
obtained from the following mass balance
equation: Since the standard deviation of the values
are relatively close to zero, the values therefore are
cc z c = co z o (2)
closer to the mean. In addition, since the variance
calculations are also relatively small, this indicates
Table 4. Critical Conditions of Batch Settling that the values are not only close to the mean, but
also to each other. Furthermore, the skewness
Mean Critical Mean Critical
Height (cm) Concentration values indicate symmetry with the data, and since
(%w/v) the skewness values are small, this indicates that
the values are not too far from each other.
Tube A 377.4286 8.8182
This method tends to be very inaccurate
Tube A 498.3322
6.7727 because it is highly subjective, but it can be used to
with Alum
determine the required area for clarification and
Tube B 423.5714 9.9316 thickening tanks, given that appropriate scale
factors are used.
Tube C 540.7500 12.0737

4. Conclusions and
Evidently, the slurry with the highest
Recommendations
initial concentration (Tube C at 8% w/v) has the
greatest mean critical concentration, and likewise,
The objective of this experiment was to
took the longest amount of time to achieve
generate batch settling curves and analyze the
compression settling. It is also observed that the settling characteristics of kaolin powder in water.
critical concentration of the slurry with alum is It aimed to determine the effect of different slurry
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

concentration and the addition of a coagulant to [5] Rhodes, M. J. (2008). ​Introduction to particle
the settling characteristics of kaolin powder. It also technology​. John Wiley & Sons.
aimed to perform a statistical analysis on the data
provided by the numerous experiments conducted
over the semester. It was found that the trials were
able to exhibit the expected batch settling curve
trends. In addition, it was also found that the tube
with the highest average settling velocity was the
tube that used alum, at 0.7101 mm/s, followed by
Tube A without alum. This was also because the
added coagulant made settling faster for the tube.
Furthermore, it was found that the slurry with the
highest concentration (Tube C) also took the
longest time to settle. For the statistical data, it was
found that generally, all trials from different
groups observed similar trends and close values, as
observed by the low standard deviation, variance,
and skewness values.

For future studies and trials of this

experiment, it is highly recommended to have an
equal number of trials per slurry. This experiment
had 7 trials each for Tube A and Tube B, but only
4 for Tube C, and 3 for Tube A with alum.
Statistically speaking, having different sample
sizes would not lead to accurate results;
nonetheless, for the sake of this study, it was still
done.
To further understand the effects of the
coagulant, it is also recommended to test various
concentrations of alum in the slurry.

5. References
[1] Subosa, B.S. (2016). ​Thickener Design.
Retrieved from https://uvle.upd.edu.ph/ on
May 21, 2018.

[2] Coulson, J. M., Richardson, J. F., Backhurst, J.

R., & Harker, J. H. (1991). ​Particle
technology and separation processes​(Vol. 2).
Pergamon Press.

[3] Darby, R., Chhabra, R. P., & Darby, R. (2001).

Chemical engineering fluid mechanics,
revised and expanded​. CRC Press.

[4] McCabe, W. L., Smith, J. C., & Harriott, P.

(1993). ​Unit operations of chemical
engineering (Vol. 5, p. 154). New York:
McGraw-Hill.
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

Appendix: Class Data

Group 1 - Kabiting, et. al. Group 2- Hipe et. al.

Tube A with Tube A with
Time (s)
Tube A (mm) Tube B (mm) Alum (mm) Tube A (mm) Tube B (mm) Alum (mm)

30 894 870 740 783 796 903

60 815 810 730 760 784 880

90 800 790 700 750 772 860

120 795 780 690 725 758 840

150 780 745 680 715 748 820

180 775 725 630 683 733 800

210 750 705 610 652 726 780

240 720 685 570 639 716 739

270 700 665 540 620 701 730

300 675 640 510 590 692 720

360 610 590 480 555 669 660

420 560 550 400 520 648 627

480 500 510 330 485 628 585

540 440 470 220 440 609 555

600 390 435 150 390 589 525

660 360 400 80 355 570 485

720 320 360 50 308 551 455

780 280 330 45 260 525 410

840 240 285 45 220 508 383

900 205 255 43 196 493 355

1200 45 155 40 88 414 245

1500 40 133 36 73 360 198

1800 37 112 34 69 318 176

2100 30 107 33 65 281 156

2400 28 104 32 63 250 138

2700 32 100 31 61 222 121

3000 30 97 30 59 196 105

3300 29 94 29 57.5 174 97

3600 28 92 29 56 162 94

3900 27 90 29 55 158 91

4500 26 87 29 52 151 86
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5100 21 84 28 50 146 82

5700 20 82.5 28 48.5 142 79

6300 20 81 28 47 138 77

6900 20 79 28 46 135 74

8700 19.5 75.5 27 43 127 68

10500 19.5 73 27 41 120 62.5

12300 19.5 70 27 40 114 58

14100 19 69 27 40 109 54

15900 19 68 27 39 104 52

Group 3 - Alindayu, et. al. Group 4 - Calma et. al.

Tube C
Time (s)
Tube A (mm) Tube B (mm) Tube C (mm) Tube A (mm) Tube B (mm) (mm)
30 780 850 801 930 740 815
60 765 845 800 860 725 813
90 750 836 800 790 710 812
120 730 831 799.5 756 695 810
150 709 824 799 723 685 807
180 690 817 798.5 690 665 805
210 665 810 798 657 655 803
240 655 804 797 624 640 801
270 640 798 796 623 625 799
300 620 792 795 623 620 799
360 584 781 791 621 614 796
420 545 770 788 562 588 792
480 510 760 784 428 567 786
540 470 750 781 318 546 782
600 440 740 777 263 523 777.5
660 400 731 773 174 500 773
720 370 723 769 102 477 768
780 340 714 766 76 457 764
840 305 705 762 73 437 760
900 273 697 758 70 416 755
1200 156 654 738 58 362 735
1500 124 617 720 51 293 764
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1800 100 581 700 50 276 693

2100 93 547 682 48 220 672
2400 90 513 663 45 195 650
2700 86 481 645 43.5 171 631
3000 84 450 627 42 152 609
3300 82 421 610 40 145 590
3600 80 391 592 39 141 570
3900 78 363 575 38 137 549
4500 75 309 540 36 132 507
5100 72 264 505 34 128 467
5700 70 251 465 33.5 124 429
6300 68 244 430 32 121 381
6900 65 233 390 32 118 345
8700 61 224 350 30 110 319
10500 57.5 214 335 30 103 304
12300 56 205 323 30 98 294
14100 53.5 198 313 30 93 284
15900 52 191.5 305 29 88 275

Group 5 -Fabros, et. al. Group 6 - Alvarillo et. al.

Tube C
Time (s)
Tube A (mm) Tube B (mm) Tube C (mm) Tube A (mm) Tube B (mm) (mm)
30 786 816 814 805 810 826
60 756 802 810 785 795 825
90 731 790 807 763 783 824
120 705 776 804 745 772 823
150 688 765 802 720 761 822
180 658 756 799 703 750 821
210 640 748 796 685 740 820
240 620 739 794 668 730 819
270 596 730 792 644 718 817
300 582 719 788 628 705 815
360 542 701 784 598 686 813
420 501 682 779 554 662 809
480 470 666 774 517 641 806
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540 429 647 770 484 619 800

600 385 630 765 443 596 796
660 349 612 760 412 577 793
720 313 596 755 368 556 790
780 273 580 750 338 534 787
840 240 562 745 303 514 783
900 204 545 740 266 495 767
1200 96 472 717 129 424 751
1500 76 414 694 98 379 735
1800 70 369 672 86 345 719
2100 68 331 648 82 315 703
2400 65 300 626 79 288 703
2700 63 268 604 76 262 687
3000 61 242 582 74 238 672
3300 60 218 560 72 215 656
3600 58 195 537 70 191 640
3900 57 178 516 69 188 624
4500 55 168 470 66 181 592
5100 52 162 428 64 175 558
5700 51 157 382 62 171 525
6300 49 152 336 60 167 491
6900 48 149 302 58 164 455
8700 46 140 279 54 155 368
10500 43 133 266 51 149 349
12300 42 127 255 49 142 337
14100 42 121 247 48 137 327
15900 42 117 240 48 132 318

Group 7 - Margate, et. al.

Tube A with
Time (s)
Tube A (mm) Tube B (mm) Alum (mm)
30 830 890 876
60 828 885 868
90 815 880 859
120 805 870 850
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150 800 865 842

180 790 860 833
210 780 850 825
240 775 840 816
270 760 830 808
300 750 821 800
360 710 796 760
420 670 768 720
480 630 744 680
540 590 716 640
600 550 690 600
660 510 665 560
720 470 638 520
780 430 614 480
840 400 587 430
900 370 560 410
1200 160 437 220
1500 50 333 53
1800 46.5 273 46
2100 44 237 43
2400 41 206 40.5
2700 39 180 39
3000 38.5 157 38
3300 36.5 141 36
3600 35 135 34.5
3900 34 131 33
4500 32 126 32
5100 31 122 20
5700 29 118 29
6300 29 115 29
6900 28.5 112 28
8700 27 104 27
10500 26.5 98 26.5
12300 26.5 92 26.5
14100 26.5 88 26.5
ChE 135 - (Alvarillo, C.M.S.; Buensuceso, M.C.B.; Gonzales, Y.M.C.; Uy, J.N.T.) - Batch Settling

15900 26.5 84 26.5

Appendix: Sample Calculations

Final Concentration
Taking Group 6’s data for Tube A as an example.

co z o = cf z f
(4%) (805 mm) = cf (48mm)
⇒ cf = 67.0833%

Appendix: Talmadge and Fitch Method

C​i​Z​i​ = C​c​Z​c
C​i =
​ 5% w/v ; Z​i​ = 870 mm
From the graph above (encircled green), Z​c​ = 330 mm
C iZ i
C​c​ = Zc = 13.18181818 %w/v