CRITICAL ANALYSIS OF LABORATORY TESTING PROCEDURES FOR SETTING PROPERTIES OF ROCK MATERIALS

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Rock Mechanics for Natural Resources and Infrastructure 
SBMR 2014 – ISRM Specialized Conference 09-13 September, Goiania, Brazil 
© CBMR/ABMS and ISRM, 2014 
 
SBMR 2014 
Critical Analysis of Laboratory Testing Procedures for Setting 
Properties of Rock Materials 
 
José Luiz Ernandes Dias Filho 
‘Darcy Ribeiro’ State University of Northern of Rio de Janeiro - UENF, Campos dos Goytacazes, 
Brasil, jlernandes@hotmail.com 
 
Paulo César de A. Maia 
UENF, Campos dos Goytacazes, Brasil, maia@uenf.br 
 
Gustavo de Castro Xavier 
UENF, Campos dos Goytacazes, Brasil, gxavier@uenf.br 
 
SUMMARY: The rock materials are used in construction with diversity in their applications. 
Before they are extracted from mines or quarries, it presents in a balanced alteration state with the 
environment, which was achieved in a geological interval of time. From the moment of extraction 
to the application, the environment is changed, then the rock begins to undergo changes until it 
reaches a new equilibrium. The rate of change in his new environment depends on the susceptibility 
of the rock to alteration. Thus, the alterability will depend on the qualities of material from the 
external environment and the exposure time. A rock can change in a time interval which may vary 
from thousands of years to a few months depending on the characteristics of alterability. This paper 
aims a critical analysis of laboratory testing procedures to define the properties of rock materials. 
The test procedures that exist stands out the study of the durability which is an important subject of 
research and permits to analyze the variation of the long term behavior of the physical, chemical 
and mechanical properties of the materials exposed to degradation agents. The way in which agents 
act on the materials can mobilize different degradation mechanisms. The main degradation 
mechanisms of physical and chemical in rock materials stand out to abrasion, disaggregated by 
crystal growth, the expansion due to thermal effects, fracturing for stress relief, hydrolysis and 
oxidation. The knowledge about the rock and its main characteristics will define the main 
laboratory testing procedures that better define the behavior of this material in the subject field 
degradation. The result of this paper presents the different types of Tests submitted in technical 
literature with ratings and testing procedures used to expose materials to different degradation 
mechanisms, trying to simulate the conditions of the local exposure of the material. 
 
KEYWORDS: Test methods, Laboratory tests, Rock materials, Rock alterability, Rock aging. 
 
 
1 INTRODUCTION 
 
The study of the rock materials durability is 
very important for Construction and enables a 
better understanding of changes in the behavior 
of physical, chemical and mechanical material 
properties when they are exposed to 
degradation agents. The way in which agents 
act on materials can mobilize different 
degradation mechanisms, which can be physical 
and chemical in rock materials. The Table 1 
shows the main characteristics like the abrasion, 
disaggregated by crystal growth, the expansion 
due to thermal effects, fracturing due to stress 
relief, hydrolysis and oxidation. 
 The degradation of rock materials is caused 
by intrinsic agents and extrinsic agents. The 
first are linked to their physical, chemical and 
mechanical characteristics. The second are 
related to the environment. 
 
 
 
 
 
 
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Table 1. Main characteristics of the degradation mechanisms in rocks. 
Degradation 
Mechanisms Characteristics 
Abrasion wear caused by friction or impact between particles, or even wear resulting from the movement of soil or rock 
Disaggregation 
by crystal growth 
caused by three factors that generate variation in volume in the particles: freezing water, salt 
crystallization and chemical alterations with expansion 
Expansion due to 
thermal effects the effect of temperature variation causes microcracks and possible breakdown of particles 
Fracturing for 
stress relief 
microcracks and fractures in the rock mass caused by several factors, such as underground 
excavations, cuts large embankments, erosion of surface extracts 
Hydrolysis breakage of molecular chains by the action of water molecules, causing expansion in the materials and consequently the leaching of constituents 
Oxidation formation of oxides due to the presence of oxygen in the environment 
 
 
 The main degradation agents of rock 
materials are i) the physical agents, namely 
temperature, precipitation, relative humidity, 
wind, atmospheric pressure, mechanical 
friction, solar radiation and other radiation (α, β 
and γ rays), ii) the chemical agents: the action 
of the water, acids, bases, solvents, oxygen, 
ozone and air pollutants, and finally biological 
agents due to microorganisms. 
 
1.2 Laboratory Testing Procedures 
 
The test procedures that study the durability 
permit to analyze the variation of the long term 
behavior of the physical, chemical and 
mechanical properties of the materials exposed 
to degradation agents. 
 The tests to evaluate durability are chosen in 
accordance with the research objective and the 
type of material. Experience and research 
determine the proper testing procedures. 
 
1.3 Objectives 
 
This paper aims a critical analysis of laboratory 
testing procedures to define the properties of 
rock materials. 
 To this was accomplished a vast literature on 
the subject in order to characterize the main 
procedures and tests that are used to 
characterize the durability of rock materials. 
 The paper can definer according to major 
studies an effective way to guide the use of tests 
and analyze the properties of the rocks. 
2 METHODS 
 
2.1 Tests for evaluating durability 
 
The tests for the assessment of durability in 
rock materials are chosen based on the research 
objective and on the rock type. 
 Knowing the rock and its main 
characteristics helps defining the main 
laboratory testing procedures that best define 
the behavior of this material in the subject field 
degradation. Some degradation in the laboratory 
procedures can include: condensation and 
ultraviolet radiation, chemical attack, 
breakdown by biological organisms, freeze-
thaw freezing and thawing, saturation and 
leaching and drying. 
 A critical analysis of the different types of 
tests presented in the technical literature by 
Maia and Salles (2006) for the evaluation of the 
geotechnical materials shows that there are two 
tests categories: 
 
2.1.1 Tests dedicated to the preparation of 
degraded or altered samples 
 
These tests samples of material are submitted to 
laboratory procedures where it induces or 
prioritizes any degradation mechanism. These 
procedures can be done in an expedited manner 
(field or laboratory) or in natural field 
conditions. The natural degradation of field is 
done by exposing the material directly through 
the exogenous environment. Normally on 
 
 
 
 
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accelerated life testing special procedures that 
simulate the degradation mechanisms prevalent 
in the field are used. After the accelerated 
material degradation is also conducted to 
determine their characteristic behavior. 
 
2.1.2 Tests devoted to determining the 
properties of durability 
 
These tests seek to determine characteristic 
properties of materials that demonstrate how 
variation in behavior is due to degradation or 
material degradation. Typically tests are used 
where the particular property represents the 
working condition of the material, for example, 
the parameters of strength, deformability, 
permeability and others. The determination of 
these properties can be made in material intact, 
unchanged, or materials already degraded. In 
the particular case of materialsalready 
degraded, tests can be made in both samples 
collected in the field, through the procedures of 
exhumation, as for degraded samples by 
procedures described in the previous item 
(preparation of degraded or altered samples). 
For purposes of this paper, we present the 
procedures and tests for characterization in the 
durability of rocks that are most used and are 
shown in Figure 1. 
 
2.2 Methods for evaluating durability 
 
It is important that the material is representative 
of the intact condition and the condition of 
change in laboratory and field. In academia, 
about the material under studies, there are some 
important papers which contain durability 
properties. This methodology highlights four 
stages that must be performed in the following 
order: i) obtain study material; ii) production of 
samples with accelerated alteration in the 
laboratory and natural with exposing samples 
on field alteration by external environment; iii) 
obtain the parameters characterizing the studied 
materials; iv) analysis of results and prediction 
of the durability (Figure 2). 
 
 
Sample 
Preparation 
Field Tests___________________________ Natural Degradation Accelerated Degradation 
 
Laboratory Degradation Tests ____
Continuous Leaching 
Wet and Dry Cycles 
Condensation and Ultraviolet Radiation 
Freeze-Thaw 
Exposure Salt Spray 
 
Durability 
Properties 
Tests for Direct 
Correlation 
Wear _____________ 
Slake Durability 
Los Angeles Abrasion 
Micro-Deval 
Amsler 
 
Impact ____________
Treton 
Impact Resistance 
 Schmidt Hammer 
 
Tests for 
Indirect 
Correlation 
Chemical_________ 
Chemical Analysis 
Sulphates Sanity 
Chemical Attack 
Petrography 
 
Physical___________ Physical Index (absorption, porosity, dry and saturated weight,) Wave Speed Propagation 
 Thermal Expansion 
 
Chemical and_____
Physical 
Scanning Electron Microscope 
X-Ray Diffraction and Energy-Dispersive X-Ray Spectroscopy 
 
Mechanical_______ Compression (Simple, Point Load and Brazilian Test) Bending Strength (3 and 4 points) 
 
Figure 1. Procedures and tests for characterization of the rocks durability. 
 
 
 
 
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Figure 2. Method to evaluate rock degradation. 
 
 
3 RESULTS AND DISCUSSIONS 
 
According with the main laboratory testing 
procedures for evaluating properties of rock 
materials, this paper shows in some Tables 
some important researches about each topic of 
the procedure and tests for characterization the 
rock materials durability. 
 The results, based on various paper analysis 
that explore the durability of rocks, were 
divided according to the procedures and tests 
for characterization of the durability of rocks 
showed in the Methods. 
 The Table 2 includes some researches that 
utilized the Method prioritizing test categories 
dedicated to Sample Preparation. The Table 3 
shows tests for characterization of the 
Durability Properties with Direct and Indirect 
Correlations. 
 The Tables 2 and 3 showed some important 
papers with characterization of rocks. The main 
topic is durability properties. Each author 
utilized tests according with his necessity. The 
variable to choose this test can be various, since 
the exogenous environment, a request from a 
company, a application of the material in a 
project, analysis from historical sites and 
monuments, until researches with another 
procedure test and new concepts. 
 Procedures and tests for characterization of 
the rocks durability in Figure 1 are in the Table 
2 and 3. The first presented was Sample 
Preparation on Field. These mechanisms intend 
to put the material on exogenous environment 
for natural alteration. Each place in the world, 
offers forms different by action of the 
Degradation Mechanisms represented by a 
Laboratory tests in the Table 1. 
 The rock materials exposed on field supply 
specimens for Direct and Indirect Test. The 
next step is analysis of the Correlations for 
Characterization of Durability Properties. 
 This exposure on field can be accelerated 
like suggest the ASTM G90-10 (2010). The 
special equipment promotes a concentration of 
solar light on the specimens. There are few 
discussions about it. The possible absence in the 
technical bibliography of studies can be related 
to the fact that the Ultraviolet Radiation is not 
as effective as other procedures of degradation 
in rocks. Salles and Maia (2004) and Azzoni et 
al. (1992) utilized Condensation and Ultraviolet 
Radiation concluded that this mechanism is one 
of the least effective as form of degradation. 
 Procedures for Sample Preparation have as 
objective to utilize the specimens to the method 
to evaluate rock degradation like showed the 
Figure 2 in highlight. The main procedures to 
Sample Preparation on the Laboratory 
Degradation Tests are the Wet and Dry Cycles 
and Continuous Leaching. The degradation 
promotes more intense alteration with these 
procedures. Frazão and Caruso (1983), Maia et 
al. (2002), Latham et al. (2006) and Maia and 
Salles (2006) conclude this test as excellent 
form to obtain specimens to correlation with 
field results for characterization of the 
durability properties. 
Freeze-Thaw and Exposure Salt Spray for 
rock were not effective forms to analyze the 
alteration (Ribeiro et al, 2008). Maybe in the 
especial places that the present weathering was 
promoted by only degradation mechanism from 
these tests. The experimental results indicate 
that the properties degradations are affected 
with the time of exposure in the procedures of 
degradation in the field or in the laboratory. 
 
 
 
 
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Table 2. Paper with method prioritizing test categories dedicated to Sample Preparation. 
Reference Material 
Sample Preparation Durability Properties 
Note 
Field Laboratory Direct Indirect 
Varilova et al. 
(2011) 
Sedimentary 
Rock 
15 
years - - 
All Chemical-Physical 
Tests and Chemical Attack 
Monitoring of a tourist area that suffers severe weathering. 
Observed physical and chemical alterations. 
Nunoo et al. (2009) Granite 25 to 40 years - Slake Durability 
Petrography and Point 
Load 
The rock material among 25 to 40 years still presents high 
resistance 
Frazão and Caruso 
(1983) Basalt 
4 and 11 
months Wet and 
Dry Cycles 
 
Los Angeles Abrasion 
and Treton Wave Speed Propagation 
Loss of the resistance with the degradation increase. The 
immersion in sulfate of sodium represents the most severe 
Latham et al. (2006) Armourstone - 
All Tests less Slake 
Durability and Impact 
Tests 
All Tests less X-Ray 
Analysis and Scanning 
Electron Microscope 
Durability guide with different researches in the field and 
in the laboratory 
Maia et al. (2003) 
Basalts 25 years 
Wet and Dry 
Cycles and 
Continuous 
Leaching 
- 
Compression (Simple, 
Point Load and Brazilian 
Test) 
The materials were analyzed and the methodology of study 
of the durability was validated. The tests were shown 
appropriate for the forecast long term behavior of the 
materials, which were influenced by the rehearsal procedure. Maia et al. (2002) Slake Durability and Micro-Deval 
Petrography, Physical 
Index and Chemical 
Analysis 
Dias Filho et al. 
(2013b) Gneiss 9 months 
Continuous 
Leaching 
Slake Durability Bending Strength 
The research was appropriate to predict durability of 
ornamental rocks. Significantly influences in the results with 
the specimens thickness 
Maia and Salles 
(2006) Gneiss 3 years - Bending Strength 
The tests generated equations that allow service life the 
durability of the material. 
Dias Filho et al. 
(2012) and Dias 
Filho et al. (2013a) 
Gneiss - Slake Durability - 
Durability study using special laboratoryequipment. The 
wear follows an approximately linear relationship with the 
increasing rotation. 
Salles and Maia 
(2004) Gneiss 1 year 
Salt Spray 
Exposure and 
Condensation 
and Ultraviolet 
Radiation 
- Physical Index and Bending Strength 
Physical alterations of materials, color and changes in 
mechanical strength. The authors found that Freeze-Thaw 
produced less variation of the rocks properties in relation to 
Condensation and Ultraviolet Radiation followed by Salt 
Spray Exposure. 
Azzoni et al. (1992) Diorite and Marble - 
Ribeiro et al. (2008) Granites - 
Salt Spray 
Exposure and 
Freeze-Thaw 
Amsler Compression Simple and Chemical Attack 
 
 
 
 
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Table 3. Paper with method of the direct and indirect test correlations for characterization of Durability Properties. 
Reference Material 
Durability Properties 
Note 
Direct Indirect 
Dhakal et al. (2002) Sedimentary Rock 
Schmidt Hammer, 
Slake Durability 
and Micro-Deval 
Physical Index Appropriate research for determination of the materials behavior 
Agustawijaya 
(2003) Weak rocks Slake Durability - 
Significant changes in the results according 
to the specimen’s geometry. 
Barroso et al. (2005) Gneiss Schmidt Hammer 
Speed of 
Wave 
Propagation 
The exposed rock material with 100 years 
continued still little altered 
Renner and 
Pulz (2005) 
Granite Impact Resistance Test and Amsler 
Petrography, 
Physical Index 
Excellent application on structures, floors 
and tiles 
Fuenkajorn and 
Scri-in (2007) 
Various rocks Slake Durability - Physical alterations in the materials and change in strength. satisfactory durability 
Yagis (2010) Carbonate Rocks Slake Durability - 
Correlation between of the slake cycles 
quantity in the results analysis. 
Lane et al. (2011) Various rocks Micro-Deval - Modifying the duration time of the test 
Erichsen et al. 
(2011) Various rocks 
Micro-Deval and 
Los Angeles 
- Comparison of the test methods for different test fraction 
Miscevic and 
Vlastelica (2011) 
Weak Rocks Slake Durability 
Point Load 
and Physical 
Index 
It was confirmed low durability of the 
material according to the carbonate 
content. 
Keaton and Mishra 
(2010) 
Sedimentary 
Rock Slake Durability - The wear follows the linear relationship so 
much with the increase of the time as with 
the increase of the rotation Dias Filho et al. 
(2013a) 
Gneiss Slake Durability and Micro-Deval - 
Allam and 
Ebrahimpour (2013) 
Sedimentary 
rock Micro-Deval - Repeatability of the tests 
 
For the quantitative analysis, the changes in 
the parameters studied are evaluated with the 
type or rate of alteration using the alteration 
indexes (Farjallat, 1972). The alteration indexes 
compare a particular characteristic from 
Durability Properties of the material in the 
initial state, intact, and the same characteristic 
in the degraded state. Thus, the index I can be 
defined by the Equation 1: 
 
%100


o
o
P
PP
I (1) 
 
where P0 is an intact rock parameter and P is an 
altered rock parameter. The index value I vary 
from zero, for the material intact, to a maximum 
value, always less than 100%, for the most 
altered material. 
 The index I can be used in anyone test for 
Durability Properties, where P is a parameter 
chosen to analyze the rock specimen according 
the degradation time. 
When the project wants fast results the 
researcher utilized Tests to Direct Correlation 
of the Durability Properties by i) Wear with 
Slake Durability, Los Angeles Abrasion, Micro-
Deval and Amsler, and ii) Impact with Treton, 
Impact Resistance and Schmidt Hammer. 
In the Table 3, highlight for Fuenkajorn and 
Scri-in (2007) that studied procedures with and 
without water during the Slake Durability Test, 
Keaton and Mishra (2010) with a modification 
in the variable time and Dias Filho et al. 
(2013a) the rotation increase in the equipment. 
All the Tests for Direct Correlation shows 
strip with classification of your quality and long 
term behavior. Thus it is possible to 
 
 
 
 
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characterize the material classifying by its 
quality. According to the results of standard 
tests ranging from very high, high, medium, 
low and very low durability. 
 
 
4 CONCLUSIONS 
 
The result of this paper cites the different types 
of tests submitted in technical literature with 
ratings and testing procedures used to expose 
materials to different degradation mechanisms. 
The critical analysis of laboratory testing 
procedures for setting properties of rock 
materials was an experience to identify the main 
test methods for study of the durability. 
 This paper shows various forms to analyze 
the variation of the long term behavior with 
physical, chemical, chemical-physical and 
mechanical properties of the materials exposed 
to degradation agents through the correlation 
between the sample preparation on the field and 
in the laboratory. 
Tests Methods for Direct Correlation for 
evaluates the rock degradation possibility to 
found an estimative of the durability with a 
result in a few time in the laboratory and it is 
show an easy process to use in project and 
researches, becomes an attractive alternative for 
characterization of rock. 
 
 
ACKNOWLEDGEMENTS 
 
The authors thank CAPES, CNPq (Process: 
305708/2012-0), UENF, FAPERJ (Process: E-
26/102.203/3013) and ‘Serraria Olho do 
Pombo’ for supporting this research. 
 
 
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