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June 17 & 20, 2019

Particle Size Analysis and Measurement

Kurt Cobain Estrella, Vince Go, Rykiel San Pedro, Nicole Kate Sequito
Department of Mining, Metallurgical and Materials Engineering
University of the Philippines Diliman
Quezon City, Philippines
ksestrella@up.edu.ph, Vince_go10@yahoo.com, rcsanpedro@up.edu.ph, nmsequito@up.edu.ph

I. OBJECTIVES AND SIGNIFICANCE OF THE STUDY


Particle size is a property of a certain powdered or granular material in which the size
measurements of a solid particle is measured. Many properties of particulate materials depend on its
particle size. Examples are flow and compaction property, suspension and emulsion stability, gloss
and tinctorial strength, reflectivity, hydration rate and strength, and other physical behaviors [1]. Other
aspects that must be considered when measuring the particle size of a material is the chemical
implications of the sizes of individual grains. Crucial properties affected by the particle size of a
material such as rate of reactions brought by the surface area of the particle, potential to dissolve due
to similar influence of the surface area of the particle must be considered in industrial fields [2]. Particle
size also affect size reduction operations as the goal is to reduce the particle size of a material into a
specific smaller size to track changes as the material undergoes crushing, homogenization,
emulsification, microfluidization, screening, filtering, and cyclones and to determine the changes
before and after the process [1].
In this experiment, two methods are employed to analyze the particle size of a fine and a
coarse sample, namely using a microscope, and by using a set of sieves. Important processes such as
the proper use and calibration of the microscope to be used, the determination of the diameter of
mineral particles by the use of the microscope, the proper particle size analysis on the two types of
samples, and the determination and the expression of the particle size distribution of ore samples must
successfully be demonstrated.

II. METHODOLOGY
A. Particle Size Analysis using Sieves

Ore samples were 200 g coarse ore sample


homogenized separately. was obtained.

Sieves were cleaned and Ore was poured on top-


stacked in correct order. most sieve.

Sieves were placed in the Retained ore on each Data were recorded and
Ro-Tap machine for 15 sieve and bottom-most process was repeated for
mins. pa were weighed. the fine ore sample.

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B. Particle size measurement using the microscope

Ore sample was sieved -100/+140 and -140/+270


manually using nos. 100, sample material were
140, and 270. collected.

Ethanol and samples


Glass slides were then
were placed in
thoroughly cleaned.
separate beakers.

Enough amounts of
Micrometer eyepiece and
balsam and sample
micrometer slide were
were placed on the
calibrated.
slides then air dried.

Pictures were taken and


Shortest and longest
diamaters of 30 particles
diameters of 10 particles
were determined using
were then measured.
ImageJ.

III. RESULTS AND DISCUSSION

Putting the stacked sieves on the working Ro-Tap Machine led to the retention of coarse ore
samples on sieves. Particles which sizes are less than the sieve’s retentiable aperture size passed
through while particles that are larger than the sieve’s hole retained. The weight of the particles on
each sieve’s size range were measured and plotted on a relative frequency table as shown below.

Table 1. Relative frequency distribution table of the


weight of the coarse ore particles based on the size Relative Frequency Histogram
(in microns) 40.00%
Relative Frequency

Particle Size 30.00%


Relative Frequency
(microns)
20.00%
less than 53 8.37%
10.00%
53 to105 6.27%
0.00%
105 to149 4.17%
less 53 105 149 177 297 840 more
149 to177 3.22% than to105 to149 to177 to to to than
177 to 297 9.59% 53 297 840 2000 2000
297 to 840 33.87% Particle Size
840 to 2000 34.39%
more than 2000 0.12% Figure 1. Relative frequency histogram of the weight of
the coarse ore particles based on the size (in microns)

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The coarse ore sample is mainly composed of particles sizing from 297-840 microns and 840-
2000 microns, which constitutes 33.87% and 34.39% the total weight, respectively, as shown on table
1 and figure 1. Results of the sieve analysis of the fine ore sample were also plotted on a relative
frequency table and histogram.
Relative Frequency Histogram
Table 2. Relative frequency distribution table
60.00%
of the weight of the fine ore particles based on

Relative Frequency
the size (in microns). 50.00%
40.00%
Particle Size Relative 30.00%
(microns) Frequency
20.00%
less than 53 25.27% 10.00%
53 to105 50.26% 0.00%
105 to149 19.40% less 53 105 149 177 to 297 to 1000 more
149 to177 3.11% than to105 to149 to177 297 1000 to than
53 2000 2000
177 to 297 1.31%
Particle Size
297 to 1000 0.42%
1000 to 2000 0.21%
Figure 2. Relative frequency histogram of the weight of
more than 2000 0.02% the fine ore particles based on the size (in microns)

Fine ore particles’ sizes that ranges from 53-105 microns and less than 53 microns mainly
constitute the weight entirety of the sample, making up 50.26% and 25.27% of the total weight,
respectively. The sieve analysis revealed that the coarse ore sample is indeed significantly coarser than
the fine sample. Particles of size more than 297 microns is only less than 1 percent of the total weight
of the fine ore sample, while it mostly constitutes the total weight of the coarser one. The histograms
also show that the coarse ore sample particle size is skewed on the right which is an indication of
relatively larger particles in comparison to the left-skewed histogram of the fine ore sample. Results
of sieve analysis of both samples were also plotted on three different graphical representations.

Cumulative % Passing vs. Cumulative % Passing vs.


Nominal Aperture Size Nominal Aperture Size
100.00% 100.0000%
Cumulative % passing

Cumulative % passing

80.00% 80.0000%

60.00% 60.0000%

40.00% y = 0.0005x + 0.1339 40.0000% y = 0.0002x + 0.7606


R² = 0.9546 R² = 0.174
20.00% 20.0000%

0.00% 0.0000%
0 500 1000 1500 2000 0 500 1000 1500 2000
Nominal Aperture Size (microns) Nominal Aperture Size (microns)

Figure 3. Cumulative % Passing vs. Nominal Figure 4. Cumulative % Passing vs. Nominal
Aperture Size line graph of coarse ore sample. Aperture Size line graph of fine ore sample.

Cumulative % passing of the coarse ore particles against the nominal aperture size were plotted
on figure 3 while the graph of the fine ore sample is shown on figure 4. The two different generated
line graph shows that 95.46% of coarse ore sample’s particle sizes can be approximated given the
equation of the line, y = 0.0005x + 0.1339. However, only 17.4% of fine ore sample’s particle sizes
can be approximated given the equation of the line, y = 0.0002x + 0.7606.

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Product sizes are usually extracted from one point on the cumulative passing vs. aperture size
curve, whereas 80% passing size is often used [4]. Based on the graph, coarse ore sample’s 80%
passing size is about 1350 microns while fine ore sample’s 80% passing size is about 100 microns. A
passing size of 80% does not accurately exhibit the overall size distribution of the material but it is an
adequate conveyor of a coarseness or fineness of a particle [4]. The gathered 80% passing sizes of both
samples, prove that the coarse ore sample is about ten times coarser than the fine ore sample.
Gates/Gaudin/Schumann plot, a graph of cumulative % passing versus nominal sieve size with the x-
axis being a logarithmic plot [5], is done to further analyze the particles’ data. Data from sieve analysis
of both coarse and fine ore samples were plotted into a Gates/Gaudin/Schumann graph, as shown on
figures 5 and 6 respectively.

Gates/Gaudin/Schumann Plot Gates/Gaudin/Schumann Plot


100.00% 100.0000%
Cumulative % passing

Cumulative % passing
1 10 100 1000 1 10 100 1000

10.00%

y = 0.0005x + 0.1339
R² = 0.9546 y = 0.0002x + 0.7606
R² = 0.174
1.00% 10.0000%
Logarithmic Scale of Nominal Aperture Size Logarithmic Scale of Nominal Aperture Size
(microns) (microns)
Figure 5. Gates/Gaudin/Schumann plot of coarse Figure 6. Gates/Gaudin/Schumann plot of fine ore
ore sample. sample.

The equations of the line generated from the Gates/Gaudin/Schumann Plot of both fine and
coarse ore samples are also the same from figures 3 and 4. Thus, these equations can be used to
linearize the particle size analysis results of coarse and fine ore samples, at 95.46% and 17.4% of the
total samples, respectively. The equations of the line generated from the Gates/Gaudin/Schumann can
be used to fit the experimental particle size distribution data [3].
On the other hand, Rosin-Rammler distribution is used to assess the particle size distribution
data [3]. Logarithmic scale of nominal aperture sizes of sieves used in the analysis of both coarse and
fine ore samples were plotted against the calculated fitted cumulative % retained. Cumulative %
retained of each sieves were fitted to ensure the accuracy and linearity of the plot generated. Rosin-
Rammler (RR) plot of both samples were plotted and are shown on figure 7 and figure 8.

Rosin-Rammler Plot Rosin-Rammler Plot


100.00% 60.00%
y = -0.0001x + 0.2255
Fitted Cumulative % Retained
Fitted Cumulative % Retained

R² = 0.4264
40.00%
50.00%
y = -0.0005x + 0.8411
20.00%
R² = 0.8678
0.00%
0.00%
1 10 100 1000 10000
1 10 100 1000 10000
-50.00% -20.00%
Logarithmic Scale of Nominal Aperture Size Logarithmic Scale of Nominal Aperture Size
(microns) (microns)

Figure 7. Rosin-Rammler plot of coarse ore sample. Figure 8. Rosin-Rammler plot of fine ore sample.

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The equations of the line generated from the Rosin-Rammler plot of both coarse and fine ore
samples are displayed on figures 7 and 8, respectively. The slope, -0.0005, is the slope of the fitting
line for 86.78% of the total data of coarse ore sample. On the other hand, -0.0001 is the slope of the
line of best fit for 42.64% of the total data of fine ore sample.
Based on the equations generated, Rosin-Rammler plot is more reliable to fit the data set of
fine ore sample. The RR plot linearizes 42.64% of the fine ore data as compared to the 17.4% of the
GGS plot. On contrary, Gates/Gaudin/Schumann plot fits the data set of coarse ore sample better than
the RR plot. The GGS plot linearizes 95.46% of the coarse ore data as compared to the 86.78% of the
RR plot.
However, certain factors can increase the accuracy and precision of the particle size distribution
of the sample. Sieving is an old but commonly used method in particle size analysis. This can be done
manually and/or the through machine sieving. The latter is usually used since the other requires tedious
work. The longer the machine sieving time and the shaking could increase its accuracy and precision
[4]. Discrepancies can also affect the size distribution’s accuracy, such as the uncleanliness of the sieve
that can lead to erroneous data results and the presence of unwanted dust and particles that may
constitute to the resulting weight which is technically not a part of the original sample.
Aside from the particle size determination through sieve analysis, method of microscopy was
also used. The determination of the particle diameter using a microscope generated imaged results,
which samples are shown on figure 9 and figure 10.

Figure 7. Microscopic image of coarse ore sample. Figure 8. Microscopic image of fine ore sample.
In the determination of the particle diameter, the use of an application was employed alongside
the optical determination. The application known as ImageJ was used on the image of the sample to
determine the feret’s diameter of the particles obtained. The results obtained (See Appendix) via the
optical microscopy averaged at 170.5 microns and 80 microns for the maximum and minimum feret’s
diameter respectively for the coarse sample and 97.5 microns and 60 microns for the maximum and
minimum feret’s diamter respectively for the fine sample. The use of the ImageJ application however
shows that the coarse sample yielded an average maximum feret’s diameter of 183.54 microns and an
average minimum feret’s diameter of 125.7 microns for the coarse sample. An average of 93.89
microns was obtained for the maximum feret’s diameter for the fine sample, and an average of 66.29
microns for the minimum feret’s diameter for the fine sample. Assuming that the ImageJ application
shows a more accurate value for the maximum and minimum feret’s diamater for the particle, the
obtained data shows a percent error as shown:

Percent Error
Coarse Fine
Maximum 7.106% 3.848%
Minimum 36.36% 9.486%

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ImageJ helps measure the diameter by drawing lines between the edges then it will analyze by ImageJ
after being calibrated with the given scale. The data will then be used to calculate for the average
diameter. Determining the particle size with the help of ImageJ is important as the optical acquisition
by the optical microscopy may be subjected to human errors. ImageJ is more accurate because it has
less error due to having less procedure involving human judgement as certain bias and adjustments
such as estimations are easily committed in optical microscopy. The range of particles analyzed is 125
to 220 micrometers for the coarse sample and 65 to 130 micrometers for the fine sample which falls
within the expected size range of the aperture size used for the experiment. Presence of particles that
is too large or is too small may be attributed to errors in the process such as spills during sieving or
particles left on the sieves that were not extracted properly.
Other methods of determination of particle size are sedimentation, electrical sensing zone
method, laser diffraction, and permeametry method [6]. The sedimentation method uses the velocity
of a particle in fluid to determine the size of the particle [6]. This is inexpensive but may not be
applicable to all particles such as soluble particles and particles that undergo re-agglomeration. The
electrical sensing zone method uses changes in impedance generated as particles pass through an
opening in a solution with electrolytes [6]. The method is now used for counting and sizing cells,
bacteria, and viruses [6]. The laser diffraction method uses the fact that particles diffract light when in
a solution. The method is fast and accurate but is expensive. The permeametry method uses the fact
that a particle permeates a substance and the pressure drop and flow rate of the substance correlates to
the particle size of the solid.

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V. APPENDIX
TABLE 1. PARTICLE SIZE ANALYSIS FOR COARSE ORE SAMPLE
Size fraction Nominal Mass Cumulative Cumulative % Cumulative %
(mesh) Aperture Size Retained Mass Retained Retained Passing

+10 2000 0.2300 g 0.2300 g 0.12 99.88


+20 1000 68.16 g 68.39 g 34 65.49
+50 297 67.12 g 135.51 g 68 31.62
+80 177 19.00 g 154.51 g 78 22.03
+100 149 6.380 g 160.89 g 81 18.81
+140 105 8.270 g 169.16 g 85 14.64
+270 53 12.42 g 181.58 g 92 8.37
-270 0 16.59 g 198.17 g 100 0

TABLE 2. PARTICLE SIZE ANALYSIS FOR FINE ORE SAMPLE


Size fraction Nominal Mass Cumulative Cumulative % Cumulative %
(mesh) Aperture Size Retained Mass Retained Retained Passing

+10 2000 0.0407 g 0.0407 g 0.02057 99.98


+20 1000 0.4100 g 0.4507 g 0.2277 99.77
+50 297 0.8400 g 1.2907 g 0.6522 99.35
+80 177 2.600 g 3.8907 g 1.966 98.03
+100 149 6.150 g 10.0407 g 5.074 94.93
+140 105 38.39 g 48.4307 g 24.47 75.53
+270 53 99.46 g 147.8907 g 74.73 25.27
-270 0 50.01 g 197.9007 g 100 0

TABLE 3. FERET’S DIAMETERS OF COARSE AND FINE SAMPLE


Coarse Sample Fine Sample
Minimum Maximum Minimum Maximum
1 50 150 75 110
2 50 125 50 100
3 25 175 50 65
4 50 200 105 130
5 50 150 65 115
6 125 160 50 65
7 100 165 45 75
8 90 220 40 110
9 110 200 75 100
10 150 160 45 105
Average 170.5 80 97.5 60

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TABLE 4. FERET’S DIAMETERS OF COARSE AND FINE SAMPLE USING IMAGEJ


Coarse Fine
Maximum Feret Minimum Feret Maximum Feret Minimum Feret
(micrometers) (micrometers) (micrometers) (micrometers)
1 224.446 154.039 106.008 91.793
2 146.73 114.957 73.212 57.886
3 210.396 139.696 88.833 66.195
4 224.843 70.996 134.727 59.81
5 168.98 122.57 69.253 55.228
6 167.196 126.932 88.422 62.388
7 197.438 144.656 102.003 63.501
8 144.855 112.352 116.304 69.134
9 223.992 120.222 115.274 85.016
10 151.657 113.873 172.688 113.883
11 188.978 152.258 94.39 61.798
12 212.443 145.712 88.944 62.086
13 147.97 116.629 68.357 50.526
14 185.84 109.135 85.449 65.474
15 152.629 122.003 91.023 61.242
16 178.537 119.467 71.881 53.32
17 226.632 130.515 100.734 77.751
18 198.886 145.972 104.981 70.842
19 162.452 120.81 92.949 53.648
20 166.38 133.724 93.921 61.777
21 163.4 114.813 66.725 54.032
22 165.292 101.223 87.423 63.976
23 169.084 132.563 91.478 71.276
24 203.629 121.632 92.118 76.781
25 159.395 127.226 79.603 60.376
26 178.883 135.413 77.366 59.496
27 165.702 98.144 67.719 57.112
28 160.916 118.326 102.448 65.222
29 261.614 163.016 104.033 70.88
30 197.056 142.135 88.356 66.188
Average 183.5417 125.7003 93.8874 66.2879

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REFERENCES

[1] Horiba Instruments Inc. “A guidebook to particle size analysis”. Horiba Scientific. Accessed June
23, 2019.
https://www.horiba.com/fileadmin/uploads/Scientific/eMag/PSA/Guidebook/pdf/PSA_Guidebook.p
df
[2] ATA Scientific. “7 reasons particle size analysis is essential”. Last modified June 18, 2018.
Accessed June 23, 2019. https://www.atascientific.com.au/7-reasons-particle-size-analysis-essential/
[3] M.M. Ahmed & S.S. Ahmed. “A comparison study to determine the mean particle size distribution
for truthful characterization of environmental data (part 1),” Assiut University: Egypt. Accessed June
24, 2019. http://www.aun.edu.eg/journal_files/15_J_5973.pdf
[4] B.A. Wills, J.A. Finch FRSC, FCIM, P. Eng, “Chapter 4 – particle size analysis,” An Introduction
to the Practical Aspects of Ore Treatment and Mineral Recovery, 2016, pp. 91-107.
[5] Unknown. “Calculating and plotting size distributions,” Accessed June 23, 2019.
http://www.chem.mtu.edu/chem_eng/faculty/kawatra/CM2200_2009_HW_3_sizedist.pdf
[6] Quadro Engineering Corp. "Methods Of Particle Size Measurement" Last Modified August 21,
2018. Accessed June 25, 2019. https://www.quadro.com/blog/methods-of-particle-size-measurement/

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