IBP1126_19

LABORATORY CHARACTERIZATION OF
MINERARIS SLURRIES FOR DUTY
TRANSPORTATION
Maycon S. Maycon , Rafael Araujo. Rafael 2
1

Copyright 2019, Brazilian Petroleum, Gas and Biofuels Institute - IBP

This Technical Paper was prepared for presentation at the Rio Pipeline Conference and Exhibition 2019, held
between 03 and 05 of September, in Rio de Janeiro. This Technical Paper was selected for presentation by the
Technical Committee of the event according to the information contained in the final paper submitted by the
author(s). The organizers are not supposed to translate or correct the submitted papers. The material as it is
presented, does not necessarily represent Brazilian Petroleum, Gas and Biofuels Institute’ opinion, or that of its
Members or Representatives. Authors consent to the publication of this Technical Paper in the Rio Pipeline
Conference and Exhibition 2019.

Abstract

It is common to carry mineral slurrys through pipelines of long distances, however, for the
correct design and design of these systems, a deep knowledge of the characteristics of the
particles and of the solid-liquid mixture to be transported is necessary. The present work
presents a minimum battery of specific laboratory tests for the characterization of the slurry and
the mineral particles with focus on the qualitative and quantitative knowledge of the basic
premises for use in the models of dimensioning of long distance pipelines.

Keywords: Laboratory test, ducts, slurry.

1. Introduction

The transport of coarse particles via duct is a trend of the mineral operations in force due
to the quality decrease of the deposits and the distance between the exploration fronts and the
ports of embarkation. Despite being a modal with a relatively high implantation cost, the
economy, flexibility and reliability put the pipeline in a prominent position regarding the
transport of minerals over long distances.
The development of an appropriate pipeline project involves, in addition to knowledge of
hydraulics, mechanics and piping, etc., an in-depth knowledge of the chemical, physical and
mineralogical characteristics of the ore and the liquid solid mixture (slurry) intended to be
transported. Regarding mineral slurrys, it is also necessary to know the rheological conditions,
whose data are used in several models of calculations.
In addition to the usual tests used in the characterization of mineral slurrys such as optical
microscopy, X-ray diffraction, among others, there is a battery of specific tests that aims to
qualitatively predict the behavior of the slurry inside the pipe as well as the conditions of
abrasive wear and sedimentation of the particles in the duct.
Investigatory tests were carried out on a sample from drilling holes in sediment dam, with
a 100% pass - through in the 0.3 mm mesh. The objective was to determine the minimum duct
construction angle, abrasive and corrosive wear rate, solids granulometry, penetration tests and
rheological tests

______________________________
1
Senior, Mechanical Engineer - PROGEN ENGENHARIA
2
Senior, Process Engineer – VALE
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2. Materials and methods

The iron ore samples tested in the present work were obtained from systematic drilling
holes in a sediment dam located in the Carajás region of the State of Pará, Brazil. The material
was dried and had the solids concentration and pH adjusted with the addition of filtered water
to achieve the usual concentration conditions in known slurries, ranging from 56.5 to 72.4%
solids. Subsequently, each sample was characterized in terms of particle size distribution, solids
specific weight, rheology, penetration, angle of rest and slippage, corrosive and abrasive
potential. The tests are described below.

2.1. Granulometric Distribution Test

The granulometric distribution tests were carried out by the SENAI-MG Center of
Innovation and Technology, using the technique of wet sieving and for the fractions of solids
below 0.045 mm, the technique of granulometric analysis was used by means of the
granulometer laser Cilas 920 liquid. The sample was filtered, and oven dried at no more than
100øC for a period of 12.0 hours.

2.2. Test of Real Density of Solids

The tests were carried out by the Innovation and Technology Center of SENAI-MG.
The samples were sent as slurry which was filtered, dried in an electric oven, quartered and
sifted. The density measurements were performed in the fractions above and below 0.045 mm.
For this, a real density analyzer was used in which the pressure exerted by the volume of helium
injected in a specific volume of sample was measured using a Stereopicnometer to Helium of
the manufacturer QuantaChrome.

2.3. Rheology Testing

The rheology tests were performed by Brass do Brasil LTDA, through the rheometer
Anton Paar Rheolab QC, with concentric cylinder system, in six different concentrations of
solids. In this test the shear rate is varied by recording the value of the corresponding shear
stress.
The tests were carried out at 6.0 different solids concentrations and due to the difference
in solids density, it was necessary to adjust the slurry solids percentage using the following
rheological relations.

y = A  B / =10 Vr B′ (1)

At where:

  l
 (2)
 s  l

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l
  (3)
l
1  cw (  1)
s


Vr  (4)
1

Cw = concentration of solid by weight;

 = volumetric fraction of solids;
Vr = volumetric ratio of solids;
y = stress to flow in dina/cm2;
 slurry viscosity in centiPoise;
= water viscosity at measured temperature;
= Reduced viscosity;
s = Specific mass of solids;
A = yield stress coefficient;
B = yield stress exponent;
B´ = viscosity exponent.

The results obtained in the cited rheometer were interpreted using the Binghan plastic
fluid model as shown below:

= +y, (5)

Onde:

 = shear stress (Pa);

 = slurry viscosity (mPa.s);
 = shear rate (1/s);
y = stress to flow (Pa).

2.4. Penetration tests

The purpose of this test is to qualitatively determine the degree of compaction of the
mineral particles. To perform this test, a calibrated mass system with a penetrometer type and
standardized weights was used, and the mass required for the test was measured through the
layer of sedimented solid in a 600 ml beaker after 24 hours of the slurry at rest to reach the
compression point close to the maximum.
After this period of rest, the tip is positioned at the solid / liquid interface. Then the
dough is added gradually until the dough touches the bottom of the beaker. This step of the
penetration test is repeated three times for each sample, so that the value of the incremental test
is considered as the arithmetic mean of the three values obtained.
The values obtained in the step of the test with gradual increase of mass serve as
reference for the test of direct penetration, that is, with a single mass. In another beaker,
containing the same sample quartet, the tip is again positioned at the solid / liquid interface, but
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this time a single calibrated mass is placed, based on the graded test, and it is observed if the
penetrometer can reach the bottom of the beaker with a single movement. If not, the test is
repeated with a weight greater than that previously tested, until the penetrometer touches the
bottom of the beaker. The figure 1 below shows the device used.

Figure 1. Penetration test

2.5. Slip tests

The objective of this test is to indicate the boundary angle at which sliding of sedimented
solids within the acrylic tube begins to occur, in addition, the value obtained in this test is used
as reference for performing the angle of repose test. First, the slurry is homogenized by shaking
and transferred to an acrylic tube, which is sealed. The slurry inside the acrylic tube is agitated
for some time, to achieve homogenization inside the tube. It is then held at 0% slope for 24
hours to achieve maximum compaction. After the sedimentation period, the slope of the tube is
increased and measured gradually until the sliding of the solids layer is visually observed. See
the following figure.

Figure 2. Slip angle test - Positioning of acrylic tubing

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2.6. Rest tests

For this test, the slurry is agitated for some time inside an acrylic tube to homogenize it.
Thereafter, the acrylic tube is positioned on the slope determined by the slip angle so that the
slurry is kept at rest. After the settling time of 24 hours is observed if there is formation of plugs
inside the tube. If so, the test should be repeated with a smaller slope until there is no clogging.
See the following figure.

Figure 3. Repose angle test - Positioning of acrylic tubing

2.7. Corrosion tests

The tests were carried out by CeelBi Tecnologia em Cerâmica LTDA and the objective
was to determine the corrosion rate of the working material in contact with the mineral slurry
(electrolyte). An electrochemical measurement system using a cell of three electrodes.
The working electrode consisted of API X70 steel. The contraletro was constituted of
platina and the reference electrode used was the one of saturated Ag. The solutions were shaken
with a mechanical stirrer and the oxygen content of the solution was also monitored. The
temperature control was performed with a thermostated bath. The measured temperature used
was 25 ° C.
Linear polarization measurements were performed over approximately 20 hours at
regular intervals of 60 minutes. These measurements were performed with a potentiostat
AUTOLAB that mathed the control of the potential differential according to the electrochemical
stability of the slurry. The current density or corrosion rate was linearized from the polarization
curve obtained in the test and transformed into corrosion rate by applying the following
equation:

(6)
Onde:

i0 = corrosion current;
MM = mean molar mass
n = number of electrons;
F = constant;
A = electrode area;
ρ = material density;
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2.8. Abrasion tests

The abrasion tests were carried out by Spectrum Engenheiros Consultores Reunidos
LTDA. The experiments were carried out in order to determine the relative abrasiveness of the
slurry in contact with the API X70 working material after the cyclic contact between both. The
results are plotted by determining the Miller Number and the SAR number, and the laboratory
procedure for preparation, execution and mathematical treatment is defined by the International
Standard for Material Standardization and Testing, ASTM G75.
Basically, the Miller number quantitatively describes the abrasive potential of the slurry
when placed in dynamic contact with a standard chrome steel material, while the SAR number
shows the abrasive performance of a given material upon being put in contact with the slurry
object of analysis. Both analyzes are based on the survey of the accumulated lost mass curve of
the studied metal or the standard metal during contact with the slurry.
After obtaining the cumulative mass loss curve with the respective ordered wear rate
pairs by the test time, the points are adjusted according to the exponential equation given below:

(7)
At where:

M = Loss of accumulated mass;

A = coefficient 01 obtained from the accumulated mass loss curve
B = coefficient 02 obtained in the accumulated mass loss curve;
t = time;

The Miller number is then calculated from the first derivative of equation 07 considering
the time of 2 hours multiplied by the scaling factor of 18.18 h / mg. The SAR number in turn is
calculated by multiplying the Miller number by the ratio of the densities of the working material
and the reference material.

2.9. Criteria for classifying the sample

Most of the tests described above are carried out by companies and professionals
specializing in long-distance slurry transport systems, so they are not in fact based on national
or international standards, except the abrasive and granulometry tests, as mentioned. Thus, the
interpretation and use of the results obtained in the tests described oversees the pipeline
designer.
However, after several experiments in pipeline projects, it was possible to create
classification criteria to determine which bands are conducive to transport by pipeline and
which are not. Table 01 below presents the classification criteria for mineral slurrys for the
evaluation of flow and selection of design elements.

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Table 01 – Slurry classification criterion - Focus on transport by pipeline

Classification Criteria
Low (B) Average (M) High (A)
cP]
≤5 5 < < 12 ≥12
Rheology y
[din/cm2] y ≤ 5 5 < y < 50 y ≥ 50
Penetration P < 20g 20g ≤ P < 50g P ≥ 50g
Presence of a film at the Total plug. No supernatant at the
Plug Potential No plug
top of the tube top of the tube.
Corrosion 0mpy ≤ C < 4mpy 4mpy ≤ C ≤8mpy C > 8mpy
(1) Low Penetration and Medium
(1) Low Plug
Dificult Resetting (1) Low Penetration and
Penetration and (2) Medium Penetration and
Pumping Medium Plug
Low Plug High Plug
(3) High Penetration

3. Results and discussions

3.1. Granulometric Distribution

The particle size of the sample is too thin and therefore the best pumping condition.
Several mathematical models that aim to determine the minimum speed of transportation use
the granulometric parameters for this. The lower the particle size of the material, the lower the
transport velocity of the slurry.
The mean particle size, that is, the d50 is the main granulometric reference for slurry
pumping, being used to determine the drag parameter (FL) of the Durand equation in addition
to the pressure loss models.
In the studied sample, the d50 presented an approximate value of 5.0 microns being,
therefore, too fine in granulometric terms for transport through pipeline. The following figure
shows the granulometric distribution of the study sample.

Figure 4. Particle Size Distribution

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3.2. Real Density of Solids

As well as the particle size distribution, the density of solids is also used to determine
several important parameters in the pipeline solids transport technology. The values found are
usual for the material that has been tested (iron ore concentrate). The test was performed 3 times
and the mean value was adopted as the density of solids to be used in the pumping analysis.
The following table shows the values obtained in the 3 tests and the arithmetic mean of
the results.

Table 02 – Solids density of the sample

Measurement Density (t/m3)

1º 4,73
2º 4,71
3º 4,71
Average 4,72

3.3. Rheology

Rheological tests were performed at concentrations of solids by weight of 56.0 / 59.0 /

62.0 / 65.0 / 69.0 and 73%. As expected, there was an exponential increase in yield stress and
dynamic viscosity at the highest concentrations. At 65.0-68.0% solids, yield stress and viscosity
increase becomes critical, so the existing long-distance ore pipelines for iron ore transport
usually operate within this range. From 73.0% solids the shear stress and the viscosity increase
too much, which may be indicative of changes in the rheological behavior of slurry-sized slurry.
The following table presents the results obtained in the rheological analysis of the sample.

Table 03 – Rheological data of the sample

s Temp. y
Cw pH  Vr  (cP) /
(g/cm3) (°C) (din/cm2)
56,0 % 0,22 26,99 0,28 8,00 9,40 22,70
59,0 % 0,23 25,18 0,31 9,30 10,49 37,46
62,0 % 0,26 21,28 0,35 13,00 13,38 60,70
6,42 4,72
65,0 % 0,28 22,21 0,39 15,40 16,21 99,10
69,0 % 0,32 23,85 0,46 23,30 25,48 212,74
73,0 % 0,36 22,18 0,56 61,40 64,58 530,30

The following figures show the graphs demonstrating the exponential growth of shear
stress and viscosity to higher percent solids as discussed above.

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Figure 5. Results of slurry dynamic viscosity

Figure 6. Slurry yield stress results

3.4. Penetration test

The sample presented low resistance to the penetration of the pontalete, therefore,
qualitatively it is possible to conclude that it is a soft slurry, in other words, if there is a stoppage
of the pumping system, the slurry may sediment in the inferior generatrix of the tube, however,
due to to the aforesaid feature, the mineral particles present in the slurry readily enter in
movement by unclogging the tubing after resuming pumping. The following table shows the
values of the masses required to cross the bed of sedimented particles until reaching the bottom
of the beaker for the concentration of solids of interest.

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Table 04 – Penetration test results

Massa (g)
Temp.
Sample pH Graded Test with single Concentration of
(°C)
incremental test movement solids (%)
Slurry sample
iron ore
25,1 6,4 30 20 60,0

3.5. Slip angle and rest test

The sample had slip angle of 27% and rest of 15%. Therefore, it can be said that if the
pipeline is built at a maximum slope of 27%, there will be a sliding of the solids and the closing
of the section of the pipe, the same will not happen if the pipeline is installed with a maximum
slope of 15%. The following table presents the values found for the concentration of solids of
interest.

Table 06 – Results of slip and rest angle tests

Sample pH Slip angle Angle of Rest

Slurry sample
iron ore
6,42 27% 15%

3.6. Corrosion tests

The corrosion test was performed at Ceelbio Tecnologia em Cerâmicas Ltda. The
methodology adopted for the accomplishment of the electrochemical measurements is included
in the ASTM standards G5, G102, G59 G61. The tests were performed under open regime and
closed regime and the values of corrosion rate and corrosive potential are shown in the table
below:

Table 06 – Results of slip and rest angle tests

Corrosion rate (mm/ano) Potential of
Sample
Open Regime Closed Regime corrosion (V)
Slurry sample
iron ore
0,0260 0,0180 -0,660

The concentration of oxygen in the sample showed a significant reduction in the first
two hours of the test in the period that the test was performed openly, however, there were
oscillations during the test period in a closed regime until the stabilization in the presented rate.
The following figure shows the evolution of the test.

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Figure 7. Slurry yield stress results

3.7. Abrasiveness test

The abrasiveness as well as the response of the material to the dynamic contact with the
slurry under test was low, evidenced by low values of Miller and SAR numbers. The following
table shows the values found in the test performed.

Table 07 – Results of Slurry abrasiveness

Miller's
Sample SAR number Abrasiveness
number (MN)
Slurry sample
iron ore
55 54 Low

4. Conclusions

The test battery in which the slurry was submitted allowed the knowledge of some
properties essential for the design of slurry transport systems. It was verified that, for the
concentrations of solids studied, it was possible to identify the bands in which the viscosities
and the shear stress undergo an exponential increase making the transport by pumping complex.
The knowledge of the abrasive and corrosivity conditions of the slurry besides the
sedimentation properties helped to evaluate the coating material of the ducts and the equipment
that composes the system besides questions about the best angle of duct assembly.

5. References

ALVES, M.S. O uso dos hidrociclones em usinas de beneficiamento de minérios - UFMG, p.57,
2013
TRATAMENTO DE MINÉRIOS: Práticas Laboratoriais/Ed. João Alves Sampaio, Silvia
Cristina Alves França, Paulo Fernando Almeida Braga. – Rio de Janeiro: CETEM/MCT,
2007.

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