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UNIVERSIDADE FEDERAL DE GOIÁS

ESCOLA DE ENGENHARIA CIVIL E AMBIENTAL


PROGRAMA DE PÓS GRADUAÇÃO EM GEOTECNIA,
ESTRUTURAS E CONSTRUÇÃO CIVIL

AVALIAÇÃO DA RELAÇÃO ENTRE A CURVA


GRANULOMÉTRICA E A CURVA
CARACTERÍSTICA SOLO-ÁGUA PARA UM
SOLO RESIDUAL BIMODAL SOB DIFERENTES
GRAUS DE DESAGREGAÇÃO

JAQUELINE COSTA DE SOUZA

D0230G20
GOIÂNIA - GO
2020
JAQUELINE COSTA DE SOUZA

AVALIAÇÃO DA RELAÇÃO ENTRE A CURVA


GRANULOMÉTRICA E A CURVA
CARACTERÍSTICA SOLO-ÁGUA PARA UM
SOLO RESIDUAL BIMODAL SOB DIFERENTES
GRAUS DE DESAGREGAÇÃO

Dissertação apresentada ao Programa de Pós-Graduação em


Geotecnia, Estruturas e Construção Civil da Universidade Federal
de Goiás para obtenção do título de Mestre em Engenharia Civil.
Área de Concentração: Geotecnia.
Orientador: Prof. Dr. Gilson de F. N. Gitirana Jr.
Coorientador: Prof. Dr. Sai K. Vanapalli

D0230G20
GOIÂNIA - GO
2020
Ficha de identificação da obra elaborada pelo autor, através do
Programa de Geração Automática do Sistema de Bibliotecas da UFG.

Souza, Jaqueline Costa de


Avaliação da relação entre a curva granulométrica e a
curva característica solo-água para um solo residual bimodal
sob diferentes graus de desagregação [manuscrito] / Jaqueline
Costa de Souza. - 2020.
cxx, 120 f. : il., figs, tabs.

Orientador: Prof. Dr. Gilson de F. N. Gitirana Jr.; Co-


orientador: Prof. Dr. Sai K. Vanapalli
Dissertação (Mestrado) - Universidade Federal de Goiás,
Escola de Engenharia Civil e Ambiental (EECA), Programa
de Pós-Graduação em Engenharia Civil - Geotecnia,
Estruturas e Construção Civil, Goiânia, 2020.
Bibliografia. Apêndice.
Inclui abreviaturas, símbolos, tabelas, lista de figuras,
lista de tabelas.

1. Solos não saturados. 2. Solos tropicais. 3. Estrutura. 4.


Desagregação. 5. Modelos de previsão. I. Gitirana Júnior,
Gilson de Farias Neves, orient. II. Título.
J. C. SOUZA Termo de ciência e autorização
AGRADECIMENTOS

À Deus, por ser minha inspiração, estar sempre comigo, me guiando e dando forças para seguir
adiante em busca de novas conquistas.

Aos meus pais e irmão pelo amor, carinho, apoio e compreensão nos momentos em que tanto
precisei e pelo incentivo ao aprendizado contínuo durante toda minha vida.

Ao meu namorado pelo companheirismo e apoio nessa reta final de mestrado.

A todos os meus colegas de mestrado que foram companheiros de estudo, me apoiaram e


aconselharam durante esses dois anos e meio. Ao Alexandre Britto, Carlos Amaecing, Eduardo
Ferreira, João Guabiroba, Luiz Galvani, Romulo Machado e em especial a minha grande amiga
Priscila de Oliveira que me apoiou diariamente e foi minha parceira em tantos momentos
difíceis. Aos meus amigos do NSAT: Emílio Vaz, Renan Ferreira, Roberto Alves e Vinícius
Naves por me ajudarem em vários ensaios e compartilharem conhecimentos da nossa área. E a
todos os meus outros amigos que de alguma forma me apoiaram e incentivaram durante o
mestrado, em especial aos meus amigos da graduação e da vida: Isabela Silva e Rui Vieira.

Ao meu professor e orientador Gilson Gitirana Jr., por me incentivar tanto a estudar a mecânica
dos solos não saturados. Por toda paciência e confiança depositada em mim. Pela dedicação,
prontidão e por todo conhecimento que me foi transmitido ao longo da pesquisa. Assim como
ao meu coorientador Sai Vanapalli por todas as contribuições à minha dissertação.

Ao professor Alexandre Araújo da UEG por despertar em mim durante a graduação, o amor
pela geotecnia e pela pesquisa.

À Arielly Silva, aluna de iniciação científica do curso de Engenharia Ambiental e Sanitária,


pela extensa ajuda na execução dos ensaios de laboratório.

À FURNAS Centrais Elétricas S.A., ao professor Alexandre Araújo e aos mestrandos João
Guabiroba, Luiz Galvani e Romulo Machado pelo fornecimento de amostras necessárias para
a realização dessa pesquisa.

J. C. SOUZA Agradecimentos
À Escola de Engenharia Civil e Ambiental e ao Programa de Pós-Graduação em Geotecnia,
Estruturas e Construção Civil, pelo conhecimento adquirido durante o mestrado. Agradeço
especialmente aos professores Eder Santos, João Paulo Silva, Lílian Rezende, Márcia
Mascarenha, Maurício Sales e Renato Angelin pelas aulas ministradas. Agradeço também aos
técnicos Clayton Santana e João Júnior por todo auxílio prestado em laboratório.

Ao professor Carlos Lauro, pelo apoio irrestrito no laboratório e por ser meu tutor em uma
competição internacional sobre mecânica das rochas (RockBowl) no Congresso Internacional
de Mecânica das Rochas (ISRM). Aos meus companheiros desta competição por me
convidarem para fazer parte do time da UFG e pela excelente companhia, Emílio Vaz e Marcela
Domiciano.

Por fim, à Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), pela bolsa
de pesquisa que permitiu o desenvolvimento desta dissertação.

J. C. SOUZA Agradecimentos
EPÍGRAFE

If you learn to think the way unsaturated soil behaves, then you will make wise engineering
decisions.

Prof. Dr. Delwyn G. Fredlund

J. C. SOUZA Agradecimentos
RESUMO

A curva-característica solo água (SWCC) é a propriedade mais importante para a compreensão


do comportamento de solos não saturados. A SWCC é relacionada à distribuição de tamanho
de partículas (PSD), propriedade central na caracterização de solos. A SWCC e a PSD são
influenciadas pela agregação de partículas, com significativos impactos no caso de solos
tropicais residuais. Esses solos apresentam agregações formadas por cimentações relativamente
estáveis, produzidas pela precipitação de óxidos de ferro e alumínio. O principal objetivo desta
pesquisa foi analisar o efeito das agregações na PSD e SWCC de alguns solos tropicais
brasileiros. Para isso, foram combinados métodos de desagregação química (realizada com
hexametafosfato de sódio, hidróxido de sódio, fosfato trisódico e pirofosfato tetrasódico em
diferentes concentrações) e física (realizada por copo dispersor, agitação horizontal e ultrassom
em diferentes períodos) para determinação da PSD. Já para análise da SWCC as amostras foram
desagregadas manualmente (por espatulação) e fisicamente (por copo dispersor), e então
reconstituídas a partir de um estado inicial de lama, por adensamento, até diferentes índices de
vazios. Foram analisadas também SWCCs obtidas para amostras compactadas quasi-
estaticamente. As PSDs foram determinadas por sedimentação e difração de laser, enquanto as
SWCCs pela combinação entre placa de pressão e potenciômetro de ponto de orvalho. Os
resultados revelaram que, tanto a desagregação química, quanto física, são necessárias para
obtenção de uma suspensão dispersa e estável. Porém, a dispersão física foi mais eficiente para
dispersão isolada do solo, visto que a desagregação química provocou inferior desintegração
dos agregados. O método mais eficiente para desagregação dos solos tropicais residuais
avaliados foi a combinação de o pirofosfato tetrasódico (0.10 mol/L) com copo dispersor
(utilizado durante 60 minutos). Com o intuito de medir SWCCs usando água livre de agentes
químicos que interferem no ângulo de contanto e tensão superficial do solo, e considerando a
relativamente pequena dispersão provocada pelos agentes químicos, foram analisadas amostras
desagregadas fisicamente por espatulação e copo dispersor, porém utilizando água deionizada.
Os resultados indicaram que as SWCCs apresentaram comportamento bimodal em todas as
condições de desagregação analisadas, e que a desagregação causou efeito maior sobre a
retenção de água nos macroporos do solo, enquanto que as características de retenção de água
nos microporos permaneceram praticamente inalteradas. De uma forma geral, a maior
desagregação, obtida com copo dispersor, provocou aumento da retenção de água nos
macroporos. Além disso, amostras mais porosas apresentaram alteração mais significativa nas
SWCCs devido à desagregação do solo. Esta pesquisa analisou também o efeito da
desagregação em métodos de obtenção indireta da SWCC, considerando PSDs com e sem
desagregação. Os modelos avaliados não apresentaram previsão satisfatória da SWCC para o
solo tropical analisado, subestimando o conteúdo de água para elevadas sucções. Com isso,
verificou-se que a conversão da PSD em SWCC de acordo com os modelos verificados, não é
adequada para representar a dupla porosidade e as agregações de solos tropicais bimodais.

Palavras-chave: Solos não saturados. Solos tropicais. Estrutura. Desagregação. Modelos de


previsão.

J. C. SOUZA Resumo
ABSTRACT

The soil-water characteristic curve (SWCC) is the most important property for understanding
the behavior of unsaturated soils. SWCC is related to the particle size distribution (PSD), central
property in soil characterization. SWCC and PSD are influenced by particle aggregation, with
significant impacts in the case of residual tropical soils. These soils present aggregations formed
by relatively stable cementations, produced by the precipitation of iron and aluminum oxides.
The main objective of this research was to analyze the effect of aggregations on PSD and SWCC
of some Brazilian tropical soils. For this purpose, chemical disaggregation methods (performed
with sodium hexametaphosphate, sodium hydroxide, trisodium phosphate and tetrasodium
pyrophosphate in different concentrations) and physical disaggregation methods (performed by
dispersion cup, horizontal agitation and ultrasound in different periods) were combined to
determine PSD. For SWCC analysis, the samples were disaggregated manually (by spatulation)
and physically (by dispersion cup), and then reconstituted from an initial slurry state, by
consolidation, up to different void rates. SWCCs obtained for quasi-statically compacted
samples were also analyzed. The PSDs were determined by sedimentation and laser diffraction,
while the SWCCs were determined by the combination of pressure plate and dew point
potentiometer. The results revealed that both chemical and physical disaggregation are
necessary to obtain a dispersed and stable suspension. However, physical dispersion was more
efficient for isolated dispersion of the soil, since the chemical disintegration caused inferior
disintegration of the aggregates. The most efficient method for disaggregation of the residual
tropical soils evaluated was the combination of tetrasodium pyrophosphate (0.10 mol/L) with
dispersion cup (used for 60 minutes). In order to measure SWCCs using water free of chemical
agents that interfere with the contact angle and surface tension of the soil, and considering the
relatively small dispersion caused by the chemical agents, samples physically disaggregated by
spatulation and dispersion cup were analyzed, but using deionized water. The results indicated
that SWCCs showed bimodal behavior in all analyzed disaggregation conditions, and that
disaggregation caused a greater effect on water retention in soil macropores, while water
retention characteristics in micropores remained practically unchanged. In general, the greater
disaggregation, obtained with dispersion cup, caused an increase in water retention in the
macropores. In addition, more porous samples showed more significant change in SWCCs due
to soil disaggregation. This research also analyzed the effect of disaggregation in methods of
indirect obtaining SWCC, considering PSDs with and without disaggregation. The models
evaluated did not present a satisfactory SWCC prediction for the analyzed tropical soil,
underestimating the water content for high suctions. Therefore, it was verified that the
conversion of PSD into SWCC according to the verified models is not adequate to represent
double porosity and bimodal tropical soil aggregations.

Keywords: Unsaturated soils. Tropical soils. Structure. Disaggregation. Prediction models.

J. C. SOUZA Abstract
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LISTA DE FIGURAS

Capítulo 2

Figure 1 - PSDs determined by the sampling methods studied for soil S1-1.0: a) Method 1; b)
Method 2; c) Method 3; d) Method 4; e) Method 5; and f) comparison between the average
PSDs of the analyzed methods………………………………………………………………...45

Figure 2 - Particle size frequencies of soil S1-1.0 considering various chemical dispersion
conditions: a) (NaPO3)6; b) NaOH; c) Na3PO4; d) Na4P2O7…………………………………...47

Figure 3 - Influence of undissolved dispersing agents on soil S1-1.0: a) NaOH at 10.0 mol/L;
b) Na3PO4 at 0.5 mol/L……………………………………………………………………….49

Figure 4 - Comparison between the cumulative PSDs of soil S1-1.0 using various dispersing
agents at optimum concentrations……………………………………………………………..50

Figure 5 - Particle size frequencies of soil S1-1.0 considering various conditions of physical
dispersion: a) horizontal agitation; b) dispersion cup; c) ultrasound…………………………52

Figure 6 - PSDs of soil S1-1.0 using the maximum durations of physical disaggregation……..54

Figure 7 - PSDs of soil S1-1.0 prepared on the dispersion cup and with varying drying
conditions after dispersion for 60 minutes…………………………………………………….54

Figure 8 - Particle size frequencies of soil S1-1.0 for the combined use of chemical dispersion
agents and physical disaggregation……………………………………………………………55

Figure 9 - PSDs of soil S1-1.0 for the combined use of chemical dispersion agents and physical
disaggregation………………………………………………………………………………...56

Figure 10 - Particle size frequencies of weathering profiles: a) S2; b) S3; c) S4……………….58

Figure 11 - PSDs of the weathering profiles S1, S2, S3 and S4 using: a) C 2H6O; b) Na4P2O7
(0.10 mol/L) combined with the dispersion cup……………………………………………….59

J. C. SOUZA Lista de figuras


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água...

Capítulo 3

Figure 1 - PSDs obtained by several testing procedures……………………………………….76

Figure 2 - Procedure for preparing reconstituted specimens from a slurry state: a) side view of
the consolidation cell; b) upper filter paper; c) upper porous stone; d) sample height
measurement with Vernier caliper; e) consolidation press with sample height measurement with
extensometer; f) reconstituted sample for determination of SWCC…………………………79

Figure 3 - Compression curves of the specimens prepared by static compaction and


consolidation from slurry prepared with the soil previously subjected to spatulation and
dispersion cup…………………………………………………………………………………83

Figure 4 - Measured SWCCs for the soil under various structural conditions…………………84

Figure 5 - Drying SWCCs for different void ratios: a) e0 = 0.5; b) e0 = 1.0……………………86

Figure 6 - PSD in cumulative and frequency form: a) aggregated soil; b) disaggregated soil….88

Figure 7 - Derivative of the SWCC: a) e0 = 0.5; b) e0 = 1.0…………………………………...88

Figure 8 - SWCCs predicted by the model proposed by Arya and Paris (1981), Arya and Dierolf
(1989), Aubertin et al. (2003), Wang et al. (2017) and Alves, Gitirana Jr. and Vanapalli
(2020)…………………………………………………………………………………………90

Figure 9 - Measured and predicted volumetric water content for the same suction values: a)
aggregated condition and e0 = 0.5; b) disaggregated condition and e0 = 0.5; c) aggregated
condition and e0 = 1.0; d) disaggregated and e0 = 1.0…………………………………………92

J. C. SOUZA Lista de figuras


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LISTA DE TABELAS

Capítulo 2

Table 1 - Soil samples properties...............................................................................................36

Table 2 - Chemical and physical properties of soil samples analyzed…………………………38

Table 3 - Details of the chemical dispersing agents used in aqueous solutions………………...42

Table 4 - Physical disaggregation periods……………………………………………………..43

Table 5 - Statistical analysis of the sampling methods analyzed for soil S1-1.0……………….66

Table 6 - Statistical analysis of the disaggregation methods analyzed for soil S1-1.0…………66

Table 7 - Statistical analysis of the PSD of soils S2, S3 and S4………………………………..68

Capítulo 3

Table 1 - Main characteristics and equations of some SWCC prediction models……………...74

Table 2 - R², SSE and RMSE values of predicted SWCCs using various PTFs………………..93

J. C. SOUZA Lista de tabelas


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LISTA DE ABREVIATURAS

ABNT Associação Brasileira de Normas Técnicas

AEV Valor de Entrada de Ar (“Air entry value”)

ARE Erro relativo médio (“Average Relative Error”)

Al Alumínio

BS Saturação por bases (“Base saturation”)

C Carbono total (“Total carbon”)

Ca Cálcio

CBR California Bearing Ratio

CEC Capacidade de troca catiônica (“Cation Exchange Capacity”)

CL Argila de baixa plasticidade (“Low plasticity clay”)

CV Coeficiente de variação (“Coefficient of Variation”)

DC-ND Dispersion cup without drying

DC-OD Dispersion cup with complete drying in an oven

DC-ODS Dispersion cup with drying in an oven up to the state of slurry

DRX Difração de raio-X

Fe Ferro

H+Al Acidez potencial (“Potential acidity”)

H+DC Hexametafosphate combined with dispersion cup

H+U Hexametafosphate combined with ultrasound

J. C. SOUZA Lista de abreviaturas


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água...

Ha Horizontal agitation

ISO International Organization for Standardization

K Potássio

K Kurtosis

Mg Magnésio

MK Modelo modificado de Kovács (1981)

ML Silte de baixa plasticidade (“Low plasticity silt”)

OM Matéria orgânica (“Organic Matter”)

P Fósforo disponível (“Available phosphorus”)

P+DC Hexametafosphate combined with dispersion cup

P+U Hexametafosphate combined with ultrasound

pH Potencial hidrogeniônico (“Active acidity of the soil”)

PSD Distribuição de tamanho de partículas (“Particle size distribution”)

PoSD Distribuição de tamanho de pores (“Pore Size Distribution”)

PTF Função de pedotransferência (“pedotransfer functions”)

PVC Policloreto de vinila

RMSE Root-mean-square error

R² Coeficiente de determinação (“Coefficient of determination”)

S Site

SC Areia argilosa (“Sand clay”)

SD Desvio padrão (“Standard Deviation”)

J. C. SOUZA Lista de abreviaturas


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água...

SK Skewness

SSE Soma dos erros quadrados (“Sum of Square Errors”)

SWCC Curva característica solo-água (“Soil-Water Characteristic Curve”)

U Ultrasound

USCS Unified Soil Classification System

USDA U.S. Department of Agriculture Soil Classification System

Zn Micronutriente zinco (“Zinc micronutriente”)

J. C. SOUZA Lista de abreviaturas


D0000G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água... 17

LISTA DE SÍMBOLOS

Letras romanas minúsculas:

abi Parâmetro referente ao ponto de quebra inicial da curva

ac Coeficiente de aderência

af Parâmetro correspondente à sucção do solo no ponto de inflexão da SWCC

agr Parâmetro referente ao ponto de quebra inicial da curva

d Diâmetro de um tubo capilar ou diâmetro da partícula

de Diâmetro efetivo do grão

deq Diâmetro equivalente dos poros

dm Diâmetro mínimo da partícula permitido

dr Parâmetro referente a quantidade de finos no solo

drbi Parâmetro referente a quantidade de finos no solo

d1 Maior diâmetro da fração grossa do material

d50 Média

e Índice de vazios (“Void ratio”)

e0 Índice de vazios inicial

g Aceleração da gravidade

g1 Peso do material na última fração em termos de peso total

hc Altura de água em um tubo capilar

hco Ascensão capilar equivalente do meio poroso

J. C. SOUZA Lista de Símbolos


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água..

hi Comprimento total do poro

hr Parâmetro que representa a sucção referente ao conteúdo de água residual

jbi Parâmetro referente ao segundo ponto de quebra da curva

kbi Parâmetro referente a segunda inclinação da curva

lbi Parâmetro referente à segunda forma da curva

m Parâmetro de distribuição

mbi Parâmetro referente a forma da curva

mf Parâmetro relacionado à curvatura da faixa de alta sucção do solo

mgr Parâmetro referente a forma da curva relacionado a parte de finos

n Número de frações arbitrárias ou porosidade

nbi Parâmetro referente a inclinação da curva

nc Número de coordenação

nf Parâmetro de ajuste relacionado à taxa de dessaturação do solo

ngr Parâmetro referente a inclinação da curva

ni Número de partículas esféricas

np Fator ou porosidade de empacotamento

p Parâmetros de ajuste

r Raio do poro

ri Raio médio dos poros de cada fração

w Fator de ponderação que indica a relação da amostra da fração grossa

wL Limite de liquidez

J. C. SOUZA Lista de Símbolos


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água..

wP Limite de plasticidade

ws Teor de umidade gravimétrico saturado

Letras romanas maiúsculas:

A Constante de Hamaker

AG Área dos grãos sólidos

Av Área superficial dos vazios

CC Coeficiente de curvatura

CU Coeficiente de uniformidade

Cψ Parâmetro de fator de correção em função da sucção

DH Diâmetro equivalente da partícula para uma mistura heterogênea

D10 Diâmetro correspondente a 10% do material que passa na curva granulométrica

D60 Diâmetro correspondente a 60% do material que passa na curva granulométrica

D85 Diâmetro correspondente a 85% do material que passa na curva granulométrica

GS Peso específico relativo dos sólidos (“Density of the particles”)

IP Índice de plasticidade

Me Umidade equivalente

Raev Raio da esfera circunscrita

Rcap Raio do poro

Ri Raio médio das partículas de cada fração

Sa Saturação por adesão

J. C. SOUZA Lista de Símbolos


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água..

Sc Saturação capilar

Sm Superfície específica

Sr Grau de saturação

Sres Grau de saturação residual

Ts Tensão superficial da água

V Volume total de solo da fração

Vb Volume de água correspondente ao efeito limite

Vp Volume de um anel pendular

Vv Volume dos vazios

Vsi Volume de sólidos de cada fração

Vvi Volume de vazios de cada fração

Wsi Massa das partículas de cada fração

Letras gregas:

α e α* Parâmetro empírico ou fator de forma ou ângulo de contato

ρd Densidade seca do solo

ρs Densidade das partículas ou dos grãos sólidos

ρw Densidade da água

θ Teor de umidade volumétrica ou conteúdo volumétrico de água no solo

θd Ângulo de enchimento

ψ Sucção matricial do solo

J. C. SOUZA Lista de Símbolos


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água..

ψb Sucção referente ao valor de entrada de ar

ψn Parâmetro de normalização

ψres Sucção residual

σ Ângulo de empacotamento

σw Tensão superficial da água

βw Ângulo de contato da água com a superfície do tubo

γn Peso específico natural do solo

γs Peso específico dos grãos

γw Peso específico da água

ν Ângulo de contato

υb Ângulo de contato

λ Parâmetro do material

χ Parâmetro do material

φ Ângulo de enchimento

(ua − uw )i Sucção matricial de cada fração

J. C. SOUZA Lista de Símbolos


D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água...

SUMÁRIO

INTRODUÇÃO ............................................................................................. 25

1.1 OBJETIVOS ..................................................................................................................... 26

1.2 ESTRUTURA DA DISSERTAÇÃO ............................................................................... 27

ARTIGO 1 ...................................................................................................... 29

ABSTRACT ............................................................................................................................ 29

1. INTRODUCTION .............................................................................................................. 30

2. SITES AND SOILS ............................................................................................................ 35

3. METHODS .......................................................................................................................... 38

3.1 SIEVE-SEDIMENTATION ............................................................................................ 38

3.2 LASER DIFFRACTION.................................................................................................. 39

3.2.1 Sample preparation and procedures for using chemical dispersants ....................... 40

3.2.2 Chemical disaggregation or preservation of aggregates ............................................ 41

3.2.3 Physical disaggregation ................................................................................................. 42

3.3 STATISTICAL ANALYSIS ............................................................................................ 44

4. RESULTS AND DISCUSSION ......................................................................................... 44

4.1 EVALUATION OF SAMPLE PREPARATION METHOD AND PROCEDURES


FOR USING CHEMICAL DISPERSANTS ........................................................................ 44

4.2 INFLUENCE OF THE USE OF CHEMICAL DISPERSION AGENTS ................... 46

J. C. SOUZA Sumário
D0230G20: Avaliação da relação entre a curva granulométrica e a curva característica solo-água...

4.3 INFLUENCE OF THE USE OF PHYSICAL DISAGGREGATION


PROCEDURES…................................................................................................................... 50

4.4 COMBINATION OF CHEMICAL AND PHYSICAL DISAGGREGATION .......... 54

4.5 WEATHERING PROFILES FROM SITES S2, S3, AND S4 ...................................... 57

5. CONCLUSIONS ................................................................................................................. 59

ACKNOWLEDGMENTS ...................................................................................................... 60

REFERENCES ....................................................................................................................... 61

APPENDIX ............................................................................................................................. 66

ARTIGO 2 ...................................................................................................... 69

ABSTRACT ............................................................................................................................ 69

1. INTRODUCTION .............................................................................................................. 70

2. MATERIALS AND METHODS ....................................................................................... 75

2.1 BASIC PROPERTIES OF THE STUDIED SOIL ........................................................ 75

2.2 ANALYSIS OF THE PARTICLE SIZE DISTRIBUTION.......................................... 76

2.3 DETERMINATION OF THE SOIL-WATER CHARACTERISTIC CURVE ......... 77

2.3.1 Specimen preparation ................................................................................................... 77

2.3.2 Soil-water characteristic curve tests ............................................................................ 80

2.3.3 Modeling the soil-water characteristic curve .............................................................. 81

3. RESULTS AND DISCUSSION ......................................................................................... 82

3.1 EVALUATION OF THE ROLE OF SOIL STRUCTURE IN THE SOIL


COMPRESSIBILITY AND THE SWCC ............................................................................ 82

3.2 INFLUENCE OF PSD AND PoSD IN THE SWCC ..................................................... 87

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3.3 THE INFLUENCE OF AGGREGATION ON THE PREDICTION OF THE


SWCC…. ................................................................................................................................. 89

4. CONCLUSIONS ................................................................................................................. 94

ACKNOWLEDGMENTS ...................................................................................................... 95

REFERENCES ....................................................................................................................... 95

CONSIDERAÇÕES FINAIS...................................................................... 100

4.1 CONCLUSÕES............................................................................................................... 100

4.2 RECOMENDAÇÕES PARA PESQUISAS FUTURAS ............................................. 102

REFERÊNCIAS ................................................................................................................... 103

APÊNDICE A – DESCRIÇÃO DE MODELOS DE PREVISÃO DA CURVA-


CARACTERÍSTICA SOLO ÁGUA ................................................................................... 106

A.1 ARYA E PARIS (1981) ................................................................................................. 106

A.2 ARYA E DIEROLF (1989) ........................................................................................... 108

A.3 M. FREDLUND, D. FREDLUND E WILSON (2002) ............................................... 109

A.4 AUBERTIN et al. (2003)................................................................................................ 113

A.5 ALVES, GITIRANA JR. E VANAPALLI (2020) ...................................................... 118

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INTRODUÇÃO

O comportamento hidromecânico de solos na condição não saturada é assunto de grande


interesse na Geotecnia. O entendimento de conceitos da mecânica dos solos nesta condição é
necessário para análise de uma série de problemas, como solos colapsíveis e expansivos,
estabilidade de taludes, capacidade de suporte de fundações superficiais e estruturas rodoviárias
e ferroviárias. No entanto, a implementação de tais conceitos na prática continua sendo um
desafio (NG; MENZIES, 2007; FREDLUND, D.; RAHARDJO; FREDLUND, M., 2012).

A curva característica solo água (SWCC) (i.e, a relação entre a quantidade de água e a sucção
do solo) é uma das propriedades mais relevantes para compreender e prever o comportamento
de solos não saturados. Por isso, a SWCC é considerada uma propriedade chave para a
implementação da mecânica dos solos não saturados na prática da engenharia. Outra
propriedade física do solo fundamental é a distribuição de tamanho de partículas (PSD). A PSD
é amplamente utilizada na classificação dos solos (GEE; BAUDER, 1986) e na estimativa de
várias outras propriedades, como a própria SWCC (van GENUCHTEN; LEIJ; LUND, 1992).

Todas essas propriedades são influenciadas pela estrutura, principalmente para os solos
tropicais (MITCHELL; SOGA, 2005; ROMERO; SIMMS, 2008), que são o foco dessa
pesquisa. A estrutura desse tipo de solo é frequentemente afetada pela agregação de partículas,
que proporcionam uma estrutura típica de dupla porosidade, representada pelos macroporos e
microporos (DELAGE; LEFEBVRE, 1984; MARINHO, 2005; KOLIJI; VULLIET; LALOUI,
2010). Com isso, o comportamento desses solos é associado não apenas a complexidades
relacionadas à sua estrutura, mas também devido a possíveis efeitos decorrentes da agregação
e ligação entre partículas.

Desta forma, é de grande importância avaliar as várias técnicas de desagregação de solos


tropicais e entender os graus correspondentes de dispersão de partículas. A PSD de solos
tropicais é fortemente influenciada pelo método de preparação de amostras (ZHANG et al.,
2004; HUAT; TOLL; PRASAD, 2012). A presença de agregações e fortes ligações entre
partículas, como a cimentação, tornam necessárias a dispersão química e física para

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desagregação completa e estável desses solos (GEE; BAUDER, 1986; ZHANG; GERMAINE;
WHITTLE, 2005). Assim, torna-se relevante avaliar as modificações estruturais causadas pela
desagregação química e física do solo na sua PDS, e consequentemente, na SWCC. Isso porque,
diferenças na PSD acabam proporcionando diferenças significativas na SWCC, visto que a
textura, o volume e a distribuição de poros governam o comportamento da água no solo
(MARINHO, 2005).

Além disso, é interessante avaliar também a influência da desagregação do solo no desempenho


de modelos de previsão de SWCC. Esses modelos permitem a determinação indireta da SWCC
de forma rápida para fins práticos de engenharia, baseados em propriedades mais simples do
solo com a PSD e o índice de vazios. Os trabalhos de Arya e Paris (1981), Arya e Dierolf (1989),
M. Fredlund, D. Fredlund e Wilson (2002), Aubertin et al. (2003), Wang et al. (2017) e Alves,
Gitirana Jr. e Vanapalli (2020) são alguns exemplos desses modelos. Porém, nenhum desses
modelos foi desenvolvido especificamente para solos com alto grau de intemperismo, como os
solos tropicais que apresentam SWCCs com comportamento bimodal. Isso pode acabar gerando
limitações e reduzindo a aplicabilidade desses modelos em obras geotécnicas que envolvam
este tipo de solo. Portanto, é fundamental avaliar também a aplicabilidade desses modelos para
previsão de SWCC de solos tropicais intemperizados, considerando diversos graus de
agregação de partículas. Assim, seria possível compreender melhor os mecanismos de
comportamento de solos tropicais residuais brasileiros.

1.1. OBJETIVOS

O principal objetivo desta pesquisa é analisar o efeito da desagregação na PSD e SWCC de


solos tropicais residuais do Centro-Oeste brasileiro. Como objetivos específicos destacam-se:

• Realizar uma avaliação do grau de desagregação química e física de alguns solos


tropicais residuais, por meio de uma extensa investigação experimental da PSD obtida com
amostras em várias condições de preparação.
• Estabelecer uma metodologia eficiente para desagregação de amostras de solos residuais
tropicais.
• Obter a PSD dos solos com suas agregações preservadas e destruídas, em diferentes
níveis de desagregação.

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• Analisar o papel da desagregação na capacidade de retenção de água em solo tropicais


estruturados.
• Avaliar a influência dos macroporos e microporos do solo sob diferentes graus de
desagregação, na capacidade de armazenamento de água no solo.
• Verificar o desempenho de modelos teóricos e semiempíricos de previsão de SWCC
para solos tropicais, utilizando PSDs em diversos graus de desagregação.

1.2. ESTRUTURA DA DISSERTAÇÃO

Esta dissertação está organizada em quatro capítulos. O presente capítulo introduziu a


importância da SWCC e da PSD para o entendimento do comportamento de solos estruturados
tropicais. Apresentou-se também a necessidade do estudo de técnicas para desagregação desses
solos e as consequentes modificações estruturais. Foi apresentada também a relevância de
avaliar a aplicabilidade de modelos de previsão de SWCC para solos tropicais em diferentes
níveis de desagregação. Finalmente, os objetivos principais e específicos da dissertação foram
discutidos. Uma breve descrição do conteúdo dos demais capítulos é apresentada nos parágrafos
seguintes:

O Capítulo 2 apresenta o primeiro artigo científico produzido nesta dissertação, a ser submetido
à revista Soil & Tillage Research (ISSN: 0167-1987), publicada pela ELSEVIER. O artigo
apresenta uma análise da PSD de solos tropicais com diferentes graus de agregação.
Inicialmente é apresentada uma introdução sobre a desagregação de solos estruturados. São
apresentadas as características físicas e químicas dos solos tropicais avaliados e as metodologias
utilizadas para análise do tamanho de partículas. Por fim são apresentados os resultados e
discussões sobre a influência da desagregação química e física na PSD dos perfis de solos.

O Capítulo 3 apresenta o segundo artigo elaborado nessa dissertação, a ser submetido à revista
Géotechnique Letters (ISSN: 2045-2543), publicada por ICE Virtual Library. Este artigo utiliza
algumas considerações feitas no primeiro artigo e avalia o papel da estrutura e da agregação na
SWCC do solo tropical principal analisado nesta pesquisa. Na introdução é apresentada a
importância da estrutura e distribuição de poros no comportamento hidromecânico do solo e
conceitos sobre os modelos de previsão da SWCC. Logo após são apresentadas as
características físicas, químicas e mineralógicas do solo estudado e as análises realizadas para
determinar a capacidade de retenção de água no solo em diferentes condições estruturais.

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Finalmente são apresentados os resultados e discussões sobre a influência da estrutura e


agregação na determinação direta e indireta da SWCC de um solo tropical.

O Capítulo 4 apresenta uma visão geral das conclusões obtidas de acordo com as análises dos
resultados dos dois artigos apresentados, bem como recomendações para pesquisas futuras.

Por fim, é apresentado no Apêncide A a descrição de alguns modelos teóricos e semiempíricos


de previsão de SWCC, com um detalhamento das equações e parâmetros utilizados nas
formulações propostas nesses modelos. Estes modelos foram selecionados para um estudo mais
aprofundado devido a sua maior relevância e frequente utilização na literatura.

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ARTIGO 1

Nesse capítulo será apresentado o artigo científico “Analysis of the particle size distribution of
tropical residual soils with varying degrees of aggregation using laser diffraction” produzido
como resultado da pesquisa realizada. Esse artigo será submetido a revista Soil & Tillage
Research.

Analysis of the particle size distribution of tropical residual soils


with varying degrees of aggregation using laser diffraction

J. C. Souza¹, A. F. Silva¹, G. F. N. Gitirana Jr.¹, and S. K. Vanapalli²


¹Universidade Federal de Goiás, Goiânia, Goiás, Brazil.
²University of Ottawa, Ottawa, Ontario, Canada.

ABSTRACT

The study of the degree of aggregation, often done using the particle size distribution (PSD), is
of fundamental importance for soil characterization and for the understanding of its behavior.
The study of the degree of aggregation is of particular importance for soils from tropical
regions, which often present aggregates due to cementation from Fe- and Al-oxides.
Unfortunately, there is limited information in the literature regarding the ideal techniques for
preserving and removing aggregations, considering the constraints and possibilities offered by
laser diffraction PSD analyses. The main objective of this paper is to evaluate the effect of
chemical and physical disaggregation on some Brazilian tropical residual soils, in the context
of the use of laser diffraction. Several methods of sample preparation have been evaluated,
including four chemical dispersing agents at varying concentrations and three physical
dispersion techniques with varying durations. The PSDs were highly sensitive to sample
segregation, but ideal sample preparation conditions that provide reduced variability were
statistically determined. The use of absolute ethyl alcohol provided the maximum preservation
of aggregates. Physical disaggregation using the dispersion cup and ultrasonication were

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significantly more effective than horizontal agitation. However, the often-recommended


duration of 15 minutes is insufficient and the application during up to 60 minutes produced
more disaggregation. The optimum concentration of the four chemical agents analyzed was
0.07 mol/L for sodium hexametaphosphate, 10.0 mol/L for sodium hydroxide, 0.30 mol/L for
trisodium phosphate, and 0.10 mol/L for tetrasodium pyrophosphate. However, these optimum
concentrations varied when chemical dispersion was combined with physical disaggregation,
since a significant change in the specific surface of the particles resulted from this combination.
The maximum disaggregation of the tropical soil evaluated was obtained through the
combination of tetrasodium pyrophosphate at 0.10 mol/L, with the use of the dispersion cup for
60 minutes. These results revealed that the combination of chemical and physical dispersion
provide a more dispersed and stable suspension. However, chemical dispersion had a minor
effect, when compared to the best physical dispersion techniques. Finally, these techniques
were applied to samples from varying depths from three weathering profiles, demonstrating
how the use of the studied techniques may be used in the evaluation of the degree of aggregation
along weathering profiles.

Keywords: particle aggregation. residual soils. lateritic soils.

1. INTRODUCTION

Particle size distribution (PSD) is a fundamental physical characteristic of soils, providing


information about the size of particles and corresponding percentage distribution in cumulative
of frequency form. The PSD is widely used for soil classification (GEE; BAUDER, 1986) and
for the estimation of many properties, such as the soil-water retention curve (ARYA; PARIS,
1981; FREDLUND, M.; FREDLUND, D.; WILSON, 2002; ALVES; GITIRANA JR.;
VANAPALLI, 2020), thermal conductivity (DE VRIES, 1963), hydraulic conductivity (van
GENUCHTEN; LEIJ; LUND, 1992) and filtration capacity (TERZAGHI; PECK; MESRI,
1996).

The varying degrees of particle aggregation and aggregate stability, often observed in tropical
residual soils (BARTOLI; BURTIN; HERBILLON, 1991; ROMERO; SIMMS, 2008; KOLIJI;
VULLIET; LALOUI, 2010), imposes multiple challenges to the determination of the PSDs of
these soils (ZHANG et al., 2004), interpretation of the obtained data (CONDAPPA et al., 2008),
and use of the PSDs of these materials (TOMASELLA; HODNETT; ROSSATO, 2000;
ROMERO; SIMMS, 2008; CAMAPUM DE CARVALHO et al., 2015). The determination of
the PSD when preserving or destroying aggregations meet different needs. The preservation of
particle aggregations may result in PSDs that better represent soil texture characteristics that
control its hydraulic and mechanical behavior (GEE; BAUDER, 1986; MITCHELL; SOGA,

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2005). However, obtaining the PSD after disaggregation provides valuable information
regarding the stability of the aggregates (BARTOLI; BURTIN; HERBILLON, 1991;
PINHEIRO-DICK, SCHWERTMANN, 1996; LE BISSONNAIS et al., 2018).

Condappa et al. (2008) demonstrated that pedogenesis processes in tropical regions favors the
formation of soils with aggregates and that these soils present bimodal PSDs. However, the
obtained PSDs depend on the method of sample preparation. Due to particle aggregation, the
PSD of this type of soil is strongly influenced by multiple factors, such as drying at various
temperatures (ZHANG et al., 2004), pretreatment for the removal of organic matter, iron
oxides, and hydroxides (FONTES; WEED, 1991), mechanical disaggregation (GENRICH;
BREMNER, 1972; ZHANG; GERMAINE; WHITTLE, 2005; BITTELLI et al., 2019), and
treatment with various dispersing chemical agents (WINTERMYER; KINTER, 1955;
TOWNSEND; MANKE; PARCHER, 1971; KAUR; FANOURAKIS, 2016). The aggregate
stability and corresponding mechanical energy required to disperse tropical residual soils
depends on the mineral composition, organic carbon content, and the flocculant cations content
(SUZUKI et al., 2015). It has also been demonstrated that certain interparticulate bonds may
not be easily destroyed by standard disaggregation methods (ZHANG; GERMAINE;
WHITTLE, 2005).

There is a significant amount of knowledge regarding the causes and nature of particle
aggregations in tropical and residual soils. The aggregation of these soils is mainly affected by
organic matter, Fe-oxides, and Al-oxides (MBAGWU; SCHWERTMANN, 2006; SILVA et
al., 2015). The presence of Fe- and Al-oxides is generally associated with cementing because
these oxides, once precipitated and recrystallized, act as bonding agents between particles
(FONTES; WEED, 1991; RIGHI; MEUNIER, 1995; MITCHELL; SOGA, 2005). The Fe- and
Al-oxides coat the particle surfaces and connect them, resulting in relatively stable and rigid
aggregates (ZHANG; GERMAINE; WHITTLE, 2005). Aggregates are also formed, without
crystal growth (i.e., without cementation), by the attraction between the positively charged Fe-
and Al-oxides and the often negatively charged soil particles. However, cementation bonds are
usually much stronger than those of other mechanisms of aggregation (HUAT; TOLL;
PRASAD, 2012) and are a major cause of particle aggregation in tropical residual soils
(FONTES; WEED, 1991; ZHANG et al., 2004).

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In terms of methods of particle size analysis, tropical residual soils with varying degrees of
aggregation have been commonly studied using standard procedures. Sand-sized particles (with
diameters between 0.05 to 2 mm) are generally measured by sieving, while finer particles
(smaller than 0.05 mm) are most commonly analyzed using methods based on sedimentation
(GEE; BAUDER, 1986; KROETSCH; WANG, 2008). Nevertheless, sedimentation methods
are time consuming, require relatively large samples and provide unreliable results for particles
smaller than 0.002 mm (DI STEFANO; FERRO; MIRABILE, 2010). Fortunately, several
automatic instruments for PSD analysis have been developed in the past few decades, using
alternative principles and techniques. Some of these new techniques are based on transmission
electron microscopy (PIERI; BITTELLI; PISA, 2006), image analysis (DUR et al., 2004;
BITTELLI et al., 2019), and light scattering, also known as laser diffraction analysis
(KONERT; VANDENBERGHE, 1997; ESHEL et al., 2004; BIEGANOWSKI et al., 2018).

Laser diffraction is probably the most popular amongst these alternative techniques (ISO 13320,
2009). Laser diffraction analysis allows the determination of particle sizes by means of the
intensity of diffracted light at various angles, which is proportional to an equivalent sphere size
(DE BOER et al., 1987). This method is fast, requires relatively small samples, and is
independent of particle density since it provides a distribution based on volume (PIERI;
BITTELLI; PISA, 2006; BIEGANOWSKI et al., 2018).

Regardless of the type of soil, different particle size analysis methods may provide different
PSDs, because of the inherent differences in the fundamental principles, hypotheses, and
samples preparation requirements of each technique. The differences between the PSD
determination methods have been extensively investigated (WU; BORKOVEC; STICHER,
1993; KONERT; VANDENBERGHE, 1997; BEUSELINCK et al., 1998; ESHEL et al., 2004;
PIERI; BITTELLI; PISA, 2006; VDOVIC et al., 2019). Sedimentation-based methods have
been found to overestimate the clay fraction because the sedimentation process of clay-sized
platy particles is significantly different that of ideal spheres considered in Stokes’ equation
(VDOVIC; OBHODAS; PIKELJ, 2010; BITTELLI et al., 2019). In the recent work of Bittelli
et al. (2019), the techniques of pipette, sedigraph and laser diffraction were compared with a
new automated image analysis technique, in which each individual particle is photographed, its
pixels counted, and its form analyzed. The automated image analysis technique was considered
by Bittelli et al. (2019) as a benchmark for other techniques and the main conclusion of the

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presented study indicated that laser diffraction provides results that are comparable to image
analysis and superior to the sedimentation methods.

When the measurement of the individual particles is needed, mechanical and chemical
dispersion have been traditionally combined as an attempt to mechanically destroy aggregates
and maintain a chemically stable suspension. Mechanical energy is often considered sufficient
to disintegrate aggregates caused by cementing (GENRICH; BREMNER, 1972). The main
methods of physical dispersion are mechanical and manual remolding, agitation, and
ultrasonication (GENRICH; BREMNER, 1972; ZHANG; GERMAINE; WHITTLE, 2005;
FIROOZI et al., 2015; BITTELLI et al., 2019). However, variables such as agitation speed and
duration (TEIXEIRA et al., 2017; BITTELLI et al., 2019) and ultrasound intensity and duration
(GENRICH; BREMNER, 1972; BIEGANOWSKI et al., 2018) need to be carefully evaluated,
to ensure an effective disaggregation. In addition, some authors advocate the controversial use
of dissolution techniques, using hydrogen peroxide or citrate-bicarbonate with sodium
hydrosulfite, to remove Fe- and Al-oxides that form cementation (GENRICH; BREMNER,
1972; KROETSCH; WANG, 2008).

Chemical dispersion is a process of separating (and/or maintaining separate) aggregates by


adding dispersants that eliminate electrical attractions (SRIDHARAN; JOSE; ABRAHAM,
1991). The dispersion of clay particles in water is controlled by the principles of colloidal
stability (WEAVER; POLLARD, 1973). Clay particles generally present negatively charged
faces (due to ion substitutions) and positively charged edges (due to broken ionic bonds). This
surface state promotes a general lack of positive charges, which is compensated by adsorption
of cations on the negatively charged faces, creating a double diffusive electrical layer
(WEAVER; POLLARD, 1973; ZHANG; GERMAINE; WHITTLE, 2005). Still, flocculation
may occur due to face-to-edge electrical bonding (FIROOZI et al., 2015). To stabilize a clay
suspension, face-to-edge flocculation should be eliminated by reversing face or edge charges
(CHIBOWSKI, 2011). One way to reverse edge charges is to increase hydroxide (OH-)
concentration and increase pH, by adding alkaline compounds to the clay solution. Another way
to reverse edge charges is by adding suitable dispersants containing anions to form complex
ions with cations exposed at the particle edges due to broken bonds (SRIDHARAN; JOSE;
ABRAHAM, 1991; ZHANG; GERMAINE; WHITTLE, 2005). The amount of dispersing agent
added to a suspension depends on the total amount of positive charges on the clay edges. It is
important to note that a clay suspension with an excessive amount of dispersant may become

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flocculated due to an increase in the concentration of salts in the suspension (MOORE;


REYNOLDS, 1997).

Numerous chemical dispersions have been investigated and reported (WINTERMYER;


KINTER, 1955; NORRISH; TILLER, 1976; ZHANG; GERMAINE; WHITTLE, 2005;
KAUR; FANOURAKIS, 2016). According to Gee and Bauder (1986), chemical dispersion is
usually performed by saturating the exchange complex with sodium and, for this reason, several
dispersing agents have the sodium cation in their composition. The commonly used dispersing
agents are sodium hexametaphosphate (ABNT, 2016), sodium hydroxide (TEIXEIRA et al.,
2017), trisodium phosphate, tetrasodium pyrophosphate (WINTERMYER; KINTER, 1955),
sodium dithionite, sodium citrate (ZHANG; GERMAINE; WHITTLE, 2005), sodium silicate,
sodium oxalate, disodium dihydrogen pyrophosphate (KAUR; FANOURAKIS, 2016), among
others.

Mechanical and chemical dispersion have some overlapping effects. In fact, many researchers
have found that a combination of chemical and physical processes provides the most complete
and stable dispersion of soil, especially when it presents aggregation due to cementation and
electrical bonds, such as the case of tropical residual soils (MAEDA; TAKENAKA;
WARKENTIN, 1977; GEE; BAUDER, 1986; BARTOLI; BURTIN; HERBILLON, 1991). The
use of an effective dispersant in appropriate concentration is effective in disintegrating
aggregates bonded without cementation (i.e., only by electrical charges), but is not efficient in
breaking the aggregates caused by cementation (ZHANG et al., 2004). On the other hand, even
though mechanical dispersion can destroy aggregates caused by cementation and aggregation,
without a competent chemical dispersion, the dispersed suspension is not stable, and
flocculation may occur (ZHANG; GERMAINE; WHITTLE, 2005).

In summary, it is of paramount importance to evaluate the various physical and chemical


dispersion techniques for tropical residual soils and to understand the corresponding degrees of
dispersion and of preservation of aggregates that may be obtained. Unfortunately, the number
of possible combinations of dispersion techniques is overwhelming and conflicting findings are
reported in the literature. In addition, little details are available regarding how these methods
should be applied when laser diffraction is employed and only a small fraction of the studies of
soil dispersion of tropical residual soils used laser diffraction. The objective of this study is to
analyze the effect of chemical and physical disaggregation of tropical residual soils typical of

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the Brazilian central west region, specifically in the context of the use of the laser diffraction
technique. The quantitative evaluation of the degree of dispersion is carried out through an
experimental investigation of the PSD of the dispersed samples. The results of this investigation
aim at offering guidance on the selection of appropriate techniques for sample preparation of
tropical soils.

2. SITES AND SOILS

In this study, four sites that present typical tropical residual soil profiles from the state of Goiás
and from Distrito Federal, Brazil, were analyzed. The first site (S1), located in the southwestern
region of Goiânia, Goiás, was originally studied by Leão Carvalho (2013) and Araujo (2019).
The second site (S2) is in the southern region of Goiânia and was analyzed by Galvani et al.
(2020). The third site (S3) is located in the central region of Goiânia and was studied by
Nascimento, Sales and Angelim (2019). Finally, the fourth site (S4) was studied by Guimarães
(2002) in the Asa Norte sector, in Brasília, Distrito Federal.

The climate of the central-western region of Brazil is characterized by an average annual rainfall
of 1532 mm, with 95% of total rainfall occurring during a wet season, from October to April.
The average maximum and minimum temperatures are 34ºC and 12ºC, respectively
(ALMEIDA et al., 2006). Rainfall and average temperatures, as well as the presence of two
well-defined seasons in the year, are reflected in the characteristics of the residual soils of this
region. The alternation of atmospheric conditions causes soils to undergo a process of leaching
in the wet season and desiccation in the dry season (CONCIANI; BURGOS; BEZERRA, 2015).
In addition, the horizons of these soils are poorly differentiated and characterized by the
predominance of gibbsite and kaolinite clay minerals and the presence of Fe- and Al-oxides and
hydroxides, resulting in materials in an advanced state of weathering and with a high degree of
aggregation (SANCHEZ, 2019).

Table 1 presents some of the characteristics of the soils analyzed. Specimens were taken from
varying depths predominantely along the horizon B but also including the horizon C in one
instance. Therefore, soils at varying weathering degrees could were collected. Despite the
variations in depth and site geology, all sites present weathering profiles of residual soils. The
results that will be shown later in this paper will demonstrate that textural information varies

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greatly depending on the method of sample preparation, with corresponding impacts on the
determination of the textural class of the soil. For this reason, no attempt is made here to present
preliminary textural information and classification for each soil individually. In general terms,
based on the unified soil classification system (USCS), all materials vary between low plasticity
clay (CL) or silt (ML), and sand clay (SC) when the PSD is obtained using samples dispersed
according of NBR 7181 (ABNT, 2016). In terms of the U.S. department of agriculture soil
classification system (USDA), the soils vary between clay, sandy clay, and silt under the same
conditions. However, the samples may present significantly different characteristics and may
be much coarser when not dispersed.

Table 1 - Soil samples properties.

Soil ID Location Elevation (m) Depth (m) Horizon Geology


16°43’43”S, Residual soil from micaschistes
S1-1.0 791 1.0 B
49°17’45”W and micaceous quartzite
S2-0.5 16°41’58”S, 0.5 B Residual soil from micaschistes
801
S2-6.0 49°16’14”W 6.0 B and micaceous quartzite
S3-0.5 16º40’40”S, 0.5 B Residual soil from micaschistes
795
S3-5.5 49º14’30”W 5.5 B and micaceous quartzite
S4-2.0 2.0 B
15º45’56”S, Residual soil from slate and
S4-6.0 1047 6.0 B
47º52’20”W quartzite
S4-10.0 10.0 C

The geology of the analyzed profile sites is composed of rocks from the Araxá (S1, S2 and S3)
and Paranoá (S4) groups (ALMEIDA et al., 2006). The Araxá group is considered of
Neoproterozoic age and is composed essentially of varied schists and subordinated by
micaceous quartzite, which present tonalities varying from rosy to red or even brown. The
Paranoá Group is dated to the Meso / Neoproterozoic age and S4 is located in the domain of
the Slate unit, which is composed of purple to red slate, with white stripes and occasional
interspaces on the surface of metasyltites and fine quartzite (ALMEIDA et al., 2006).

The mineralogical composition was determined by X-ray diffraction analysis. A semi-


quantitative analysis indicated, for site S1, gibbsite as the main mineral. Quartz, kaolinite,
hematite, and spinel were identified in smaller quantities and traces of diaspore, goethite and
micas were also identified. For site S2, the main observed mineral was kaolinite, with smaller
quantities of gibbisite, muscovite and goethite that reduce with the increase in the depth. Traces
of quartz and magnetite were also observed. Site S3 presented mineralogical constitutions
somewhat similar to that of site S1, with gibbsite as main mineral, followed by kaolinite,
goethite, quartz and hematite, and traces of biotite. Finally, for site S4, gibbsite predominated

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for the depths of 2.0 and 6.0 m, but for the sample S4-10.0 gibbsite was not observed, being
replaced by an increase in the kaolinite content. Site S4 also presented a high content of
hematite, particularly for samples S4-6.0 and S4-10.0, and also significant quantities of quartz
and muscovite. The observed mineralogical composition of these sites confirmed the high
weathering degree and is typical of fine lateritic soils (REZENDE et al., 2017). The presence
of gibbsite, quartz, kaolinite and hematite, especially in samples taken from shallower depths,
is generally accompanied by the presence of microaggregations with macropores (CAMAPUM
DE CARVALHO et al., 2015).

Table 2 shows the chemical properties of the soils analyzed, as well as the density of the
particles (Gs) of each sample. The laboratory analyses to determine the chemical properties of
soils were performed following the EMBRAPA standard (TEIXEIRA et al., 2017). The
exchangeable cations Ca, Mg, and Al were determined using a KCl extraction solution. The
determination of exchangeable K was performed with Mehlich solution. The extraction of the
potential acidity (H+Al) was performed with calcium acetate ((CH3COO)2Ca.H2O). The total
phosphorus (P) content in the samples was determined by spectrophotometry. The organic
matter (OM) in the soil was obtained by oxidation in the presence of a mixture of potassium
dichromate (K2Cr2O7). The total amount of carbon (C) was determined by the combustion of
the samples. Finally, the measurement of the pH of the soils was performed by means of a
combined electrode immersed in soil:water suspension, in the proportion 1:2.5. The total zinc
micronutrient (Zn), cation exchange capacity (CEC) and base saturation (BS) are also presented
in Table 2.

Due to the acidity of the soil (pH) between 4 and 6, typical of highly weathered tropical residual
soils (CONCIANI; BURGOS; BEZERRA, 2015; SANCHEZ, 2019), all analyzed samples
indicated the presence of exchangeable aluminum, even with the low amount of Al, except for
sample S4-10.0. The low values of exchangeable Ca, Mg and K bases suggest that the most of
the soils analyzed are highly weathered, except for some of the deeper samples. The only
samples with a high K content were samples S2-0.5 and S4-10.0, which indicates the presence
of primary minerals. The small quantity of exchangeable bases also implies a low saturation
per base of the soils, suggesting the presence of charges occupied by acidic components (H or
Al). The CEC presented relatively low values, below 5 cmolc/dm³, which reveals low clay
content or predominance of 1:1 clay minerals, such as illite (SANCHEZ, 2019). In addition, the

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results indicated low values of OM, below 15 g/dm³, except for the sample S3-0.5 which
presents a higher amount of organic content.

Table 2 - Chemical and physical properties of soil samples analyzed.

Soil ID Gs Ca Mg Al H+Al CEC K P Zn BS OM C pH


(cmolc/dm³) (mg/dm³) (%) g/dm³
S1-1.0 2.69 0.2 0.1 0.0 4.2 4.53 10.2 0.8 1.2 7.28 12.0 6.96 5.5
S2-0.5 2.72 0.8 0.2 0.0 2.0 3.18 71.1 0.5 1.5 37.11 11.0 6.38 5.5
S2-6.0 2.79 0.2 0.1 0.1 1.8 2.13 10.5 0.5 0.9 15.49 8.0 4.64 4.8
S3-0.5 2.74 1.2 0.2 0.0 2.7 4.13 13.6 0.8 2.5 34.62 17.0 9.86 5.1
S3-5.5 2.79 0.2 0.1 0.1 2.0 2.33 10.4 0.8 22.5 14.16 5.0 2.90 4.6
S4-2.0 2.73 0.2 0.1 0.0 1.9 2.23 10.1 1.5 2.0 14.80 8.0 4.64 5.9
S4-6.0 2.63 0.2 0.1 0.0 2.2 2.55 19.4 0.5 1.9 13.73 3.0 1.74 4.9
S4-10.0 2.82 0.2 0.1 1.5 4.1 N/A N/A N/A N/A N/A 4.0 2.32 4.2

3. METHODS

The PSD was analyzed by sedimentation and laser diffraction methods. Sedimentation was
adopted as a standard procedure, only for comparison purposes, since it is recommended by
international standards and in Brazil (ISO 11277, 2009; ABNT, 2016). However, most of the
extensive experimental program presented herein was carried out using laser diffraction.
Special procedures for sample preparation were proposed for laser diffraction testing, allowing
the use of different chemical and physical dispersion procedures.

The experimental program was divided in a preliminary phase devised to establish appropriate
methodologies and in four subsequent main phases. In the preliminary phase, the soil S1-1.0
was used in the evaluation of the ideal sample preparation method and procedure for using
chemical dispersants. In the phases 1, 2, and 3, the soil S1-1.0 was used in the evaluation of the
performance of multiple chemical and physical disaggregation procedures, individually or
combined. Finally, in phase 4, the PSD analysis methods that produced the maximum
preservation of aggregates and the maximum disaggregation, as observed for soil S1-1.0, were
used for the analysis of the soils obtained from the sites S2, S3, and S4.

3.1 SIEVE-SEDIMENTATION

Sedimentation and sieving tests followed the recommendations described by the Brazilian
standard NBR 7181 (ABNT, 2016). Sieving was done with oven-dried particles, between 0.075
and 2.0 mm. Sedimentation tests involved the following steps: collection of samples of 70 g of

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the material passing on the 2.0 mm sieve, previously dried for 24 h in an oven at 110 ºC;
immersion for 24 hours in 125 g of distilled water or in the same volume of sodium
hexametaphosphate solution ((NaPO3)6) with concentration of 45.7 g/L (0.45 mol/L), buffered
with sodium carbonate (Na2CO3) (3.5 g/L); agitation in the standard dispersion cup (electric
stirrer) during 15 minutes at 10000 rpm; sedimentation in 1 L cylinders that were initially
topped up with distilled water and agitated for 1 minute; periodic temperature and density
reading with a calibrated hydrometer.

It is important to note that the standard procedure followed herein always subjects the soil to
mechanical dispersion. However, chemical dispersion is used in the first sample but is not used
in the second one. A third sample preparation procedure where the soil would not be subjected
to neither mechanical nor chemical dispersion is not presented herein, because it leads to a
sedimentation process that is too fast to allow density readings.

3.2 LASER DIFFRACTION

The laser diffraction analysis was performed using the S3500 particle size analyzer (Microtrac
MRB Inc). The instrument has a tri-laser optical system with 3 mW of power and a wavelength
of 780 nm. The system has a range from 0.02 to 2800 μm. The Microtrac FLEX software uses
Mie's compensation theory, which is recommended by ISO 13320 (2009) for determining the
volume in each of the particle size classes. In all analyses the optical parameters of particles
and fluid of 1.58 and 1.33, respectively, were assumed regarding the soil and water refractive
indexes. The duration of each analysis was approximately 5 minutes, disregarding the
ultrasound analysis.

The experimental program involved chemical and physical disaggregation analyses, and also
the combination of these procedures, as described in the following sections. The experimental
procedures presented herein are based on a large preliminary study, where the repeatability of
PSDs was evaluated, while following good measuring practices such as the use of an ideal
obscuration index range.

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3.2.1 Sample preparation and procedures for using chemical dispersants

Several methodologies have been proposed to determine the PSD using laser diffraction (WU;
BORKOVEC; STICHER, 1993; MUGGLER; PAPE; BUURMAN, 1997; BEUSELINCK et
al., 1998; PIERI; BITTELLI; PISA, 2006; VDOVIC; OBHODAS; PIKELJ, 2010; BITTELLI
et al., 2019). However, limited attention has been given to how the chemical dispersion
procedures should be applied when using a laser diffraction instrument and how sample
preparation should be carried out. This is in part due to the fact the many authors rely on the
use of ultrasound generators available with these instruments and neglect the need for additional
disaggregation procedures (KOWALENKO; BABUIN, 2013). Because of this, a preliminary
study was carried out to define methodologies for producing adequate representative samples,
when the soil is subjected to chemical dispersion. Data repeatability with relatively low
variability was pursued.

Five methodologies for sample preparation and use of chemical dispersant were evaluated, all
using a solution of (NaPO3)6 at a concentration of 0.45 mol/L, as recommended by Brazilian
standard NBR 7181 (ABNT, 2016):

Method 1. Ten individual wet subsamples were prepared and analyzed. Each
subsample was comprised of 0.2 g of oven-dried soil that passed in the 2.0 mm sieve
and was immersed in 5 mL of (NaPO3)6 solution for 24 hours prior to testing. The
same (NaPO3)6 solution was used in the instrument reservoir;

Method 2. A single wet sample produced from 10 g of oven-dried soil that passed in
the 2.0 mm sieve was prepared and later ten subsamples of approximately 0.2 g were
collected from the 10 g sample and analyzed in the instrument. Prior to testing, the 10
g sample was immersed in 250 mL of (NaPO3)6 solution for 24 hours. The same
(NaPO3)6 solution was used in the instrument reservoir;

Method 3. Ten individual dry subsamples were prepared and analyzed. Each
subsample was comprised of 0.2 g of oven-dried soil that passed in the 2.0 mm sieve.
The (NaPO3)6 solution was used only in the instrument reservoir;

Method 4. Ten individual wet subsamples were prepared and analyzed. Each
subsample was comprised of 0.2 g of oven-dried soil that passed in the 2.0 mm sieve

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and was immersed in 5 mL of (NaPO3)6 solution for 24 hours prior to testing. However,
pure deionized water was used in the instrument reservoir;

Method 5. Identical to the previous option. However, the tested material was the
fraction passing through the 0.42 mm sieve.

All tests were carried out without any type of physical disaggregation and without ultrasound.
The subsamples’ mass of 0.2 g of dry soil was established based on the maximum amount of
soil necessary to reach the recommended obscuration index range, as suggested by Muggler,
Pape and Buurman (1997) and indicated in the instrument’s software. However, it is known and
was confirmed that the ideal sample mass depends on the soil type, with finer materials
requiring smaller subsamples (KOWALENKO; BABUIN, 2013). Because of this, samples
subjected to more efficient disaggregation procedures required masses lower than 0.2 g to reach
an adequate obscuration index.

3.2.2 Chemical disaggregation or preservation of aggregates

For the evaluation of the effect of chemical dispersing agents, sodium hexametaphosphate
((NaPO3)6), sodium hydroxide (NaOH), trisodium phosphate (Na3PO4.12H2O) and tetrasodium
pyrophosphate (Na4P2O7.10H2O) were evaluated as dispersing agents. The procedure for use
of each of these dispersants consisted of the following steps: i) ten individual wet subsamples
are prepared; each subsample being comprised of 0.2 g of oven-dried soil that passed in the
0.42 mm sieve; ii) each subsample is immersed for 24 hours in 5 mL of an aqueous dispersing
agent solution (details in Table 3), or in pure deionized water, or in absolute ethyl alcohol
(C2H6O) (99.8%); iii) the subsample solution is placed in the sample reception controller of the
laser diffraction instrument, applying constant agitation during the analyses.

One full set of 10 subsamples was used for each of the conditions tested. The concentrations
presented in Table 3 were defined by combining the recommendations of Wintermyer and
Kinter (1955), Zhang, Germaine and Whittle (2005), Kaur and Fanourakis (2016), ABNT
(2016), Teixeira et al. (2017), and Bittelli et al. (2019). The saturated salt concentration was
also considered. Deionized water was used to determine the PSD without any dispersing agent.
In addition, samples prepared with C2H6O were analyzed to observe the soil in its most
aggregate state, as proposed by Teixeira et al. (2017). C2H6O acts in the conservation of
aggregates because it attenuates their dispersion because it presents an inert behavior, with

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lower attraction between the soil particles and C2H6O, in comparison to water. Thus, the wetting
capacity of the micropore of the aggregates by the alcohol is lower than the water (DUFRANC
et al., 2004).

Table 3 - Details of the chemical dispersing agents used in aqueous solutions.

Dispersing agent Concentration (mol/L) Salt mass per liter of solution (g/L)
0.038 3.876 + 0.297 g de Na2CO3
0.07 7.140 + 0.547 g de Na2CO3
(NaPO3)6 0.13 13.260 + 1.016 g de Na2CO3
0.24 24.480 + 1.875 g de Na2CO3
0.45 45.900 + 3.515 g de Na2CO3
0.1 4.0
0.5 20.0
NaOH 1.0 40.0
5.0 200.0
10.0 400.0
0.02 7.6
0.05 19.0
Na3PO4 0.12 45.6
0.30 114.0
0.50 190.0
0.01 4.460
0.02 7.931
Na4P2O7 0.03 14.104
0.06 25.080
0.10 44.600

3.2.3 Physical disaggregation

The analysis of methods of physical soil disaggregation was performed using the dispersion
cup, horizontal agitation, and the ultrasound generator available in the laser diffraction
instrument. The samples were dispersed in the dispersing cup standardized by NBR 7181
(ABNT, 2016) at a frequency of 10000 rpm. Horizontal agitation was performed on a stirring
table at its maximum frequency, of 200 rpm. Ultrasound was applied in the laser diffraction
instrument, at a power level of 40 W recommended by ISO 13320 (2009). The disaggregation
times adopted are presented in Table 4 and are loosely based on values adopted in several
publications (GENRICH; BREMNER, 1972; ZHANG; GERMAINE; WHITTLE, 2005;
TEIXEIRA et al., 2017; BIEGANOWSKI et al., 2018; BITTELLI et al., 2019).

The experimental procedure of the tests performed with horizontal agitation and ultrasound are
as follows: i) ten individual wet subsamples are prepared; each subsample being comprised of
0.2 g of oven-dried soil that passed in the 0.42 mm sieve; ii) each subsample is immersed for
24 hours in 5 mL of pure deionized water; iii) in the case of horizontal agitation, the samples

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were shaken on the stirring table for a period of time (Table 4) prior to testing and, in the case
of ultrasound analysis, the sample is added to the equipment and the ultrasound was
continuously applied, as the PSDs were determined at all pre-established periods (Table 4) in a
continuous way.

Table 4 - Physical disaggregation periods.

Horizontal agitation Dispersion cup Ultrasound


(hours) (minutes) (minutes)
4 7.5 0.5
16 15 1
30 2
60 4
8
15

The experimental procedure of the tests performed with horizontal agitation and ultrasound are
as follows: i) ten individual wet subsamples are prepared; each subsample being comprised of
0.2 g of oven-dried soil that passed in the 0.42 mm sieve; ii) each subsample is immersed for
24 hours in 5 mL of pure deionized water; iii) in the case of horizontal agitation, the samples
were shaken on the stirring table for a period of time (Table 4) prior to testing and, in the case
of ultrasound analysis, the sample is added to the equipment and the ultrasound was
continuously applied, as the PSDs were determined at all pre-established periods (Table 4) in a
continuous way.

The methodology adopted for using the dispersion cup required larger soil samples: i) a single
samples is prepared, comprised of 70 g of oven-dried soil that passed in the 0.42 mm sieve; ii)
the sample is immersed for 24 hours in 125 mL of pure deionized water; iii) the material is
transferred to the dispersion cup, which was used for a period of time (Table 4); iv) the sample
is placed in an oven at 110 ºC and homogenized in regular intervals for 60 minutes, until
reaching a slurry state; v) 10 individual subsamples of 0.2 g as obtained and tested in the laser
diffraction instrument. This procedure was adopted to guarantee a more homogeneous sample
without great variability, since it was verified during the methodology study that the variability
of the samples is easily affected by segregation when other attempted preparation procedures
were employed.

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3.3 STATISTICAL ANALYSIS

All PSDs presented in this study are based on the average curve obtained from ten independent
subsamples and the variability of these curves is always presented. This testing replication has
the purpose of determining the standard deviation (SD) and coefficient of variation (CV) in
each of the fractions of the PSD curves and to enable the determination of a mean particle size
curve. Basic statistical analyses were performed using OriginPro 2018 (ORIGINPRO, 2018).

In order to compare the preparation methods and, therefore, sample disaggregation, the data
obtained were preferably grouped into common size classes to accommodate different numbers
of size categories in different methodologies (CENTERI et al., 2015; BITTELLI et al., 2019).
In this study, soil particles were divided into nine size classes (0.0255-0.5, 0.5-2, 2-5, 5-20, 20-
50, 50-100, 100-250, 250-420, 420-1000 μm).

The analysis of PSDs may be done by considering some statistical descriptors, such as the
median (d50), skewness (SK), and kurtosis (K). Due to their physical relevance in the evaluation
of filtration and other soils characteristics, the percentiles D10, D60, and D85 are also of interest.

4. RESULTS AND DISCUSSION

4.1 EVALUATION OF SAMPLE PREPARATION METHOD AND


PROCEDURES FOR USING CHEMICAL DISPERSANTS

The results of the study of sample preparation methods for the use of chemical dispersants in
laser diffraction equipment are presented in Figure 1. The PSD curves of ten samples for each
of the five investigated sample preparation methods are presented. As well as a comparison of
the average PSD curves for each of the analyzed methods. After the analysis of all the
methodologies, it was observed that the use of dispersing solution in the equipment reservoir
did not affect the determined PSD. In addition, this procedure was considered excessively
laborious and questionable, because it was not possible to verify the complete dissolution of
salt inside the instrument. Furthermore, it was observed the need to put the samples in previous
contact with dispersing agent for at least 24 hours for a better disaggregation.

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Figure 1 - PSDs determined by the sample preparation methods studied for soil S1-1.0: a) Method 1; b) Method
2; c) Method 3; d) Method 4; e) Method 5; and f) comparison between the average PSDs of the analyzed
methods.

100 100
Sample 1
90 Sample 2 90
Sample 3
80 Sample 4 80
70 Sample 5 70
Sample 6
Passing (%)

60 Sample 7 60
50 Sample 8 50
Sample 9
40 Sample 10 40
30 30
20 20
10 10
0 0
0.01 0.1 1 0.01 0.1 1
a) b)

100 100
90 90
80 80
70 70
Passing (%)

60 60
50 50
40 40
30 30
20 20
10 10
0 0
0.01 0.1 1 0.01 0.1 1
c) d)

100 100
Method 1
90 90 Method 2
80 80 Method 3
70 70 Method 4
Method 5
Passing (%)

60 60
50 50
40 40
30 30
20 20
10 10
0 0
0.01 0.1 1 0.01 0.1 1
Particle size (mm) Particle size (mm)
e) f)

Another finding was that using the small 0.2 g wet subsamples produced significantly lower
variability in the determined PSDs, when compared to using ten dry 0.2 g subsamples or using
the 10 g sample that was only later subdivided. A possible explanation to this finding is the
segregation of particles in the container with the 0.2 g dry subsample and in the 10 g wet sample.

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Finally, it was observed that passing the material through the 0.42 mm sieve produced PSDs
with lower variability when compared to those obtained with the material passing in the 2.0
mm sieve. This was attributed to the fact that samples of equal mass, when passing in the 0.42
mm sieve, were comprised of a much larger number of particles and, as a result, were more
homogeneous. In summary, the recommended sample preparation procedure and method of use
of chemical dispersant was Method 5.

The variability of the samples was evaluated through the SD and the CV. When analyzing the
PSD curves in cumulative terms, it was noted that the CV in the fractions of the extremes (i.e.,
less than 20 μm and greater than 420 μm) are high. This occurs because the mean particle size
frequency values are small (close to zero) at these extremes and, because of the own definition
of CV (equal to the SD divided by the mean), it starts to present very high values. Therefore,
the variability needs to be observed both in terms of the CV and SD. During the discussions of
this study, the analysis of the SD of the samples was given more relevance. The corresponding
SD varied between 0 and 2.9% for Method 1, 0 and 4.8% for Method 2, 0 and 4.2% for Method
3, 0 and 3.0% for Method 4, and 0 and 1.4% for Method 5, proving that Method 5 was the one
with the lowest variability among the sample preparation methods studied. The values of the
statistical analysis are presented in the Appendix to this paper.

4.2 INFLUENCE OF THE USE OF CHEMICAL DISPERSION AGENTS

Figure 2 shows the frequency PSDs of the soil from site S1, obtained using multiple chemical
dispersants at various concentrations. All four plots also present the results obtained with
C2H6O because they serve, in theory, as a reference to a state of minimum dispersion and
maximum preservation of aggregates (DUFRANC et al., 2004; TEIXEIRA et al., 2017). The
bars represent the mean values obtained from 10 subsamples. All bars are accompanied by an
indication of the SD. The corresponding SD varied, depending on the particle size fraction,
between 0 and 3.3% for (NaPO3)6, 0 and 7.7% for NaOH, 0 and 3.1% for Na3PO4, 0 and 3.8%
for Na4P2O7, and 0 and 2.6% for C2H6O. These values are similar to the typical SD range found
using the sample preparation methods, shown in the previous section, except for the case of
NaOH. The higher variability obtained using NaOH will be explained later. The concentration
values also did not affect the variability of test results.

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The disaggregation and dispersion of particles varied depending on the dispersion agent and its
concentration. Taking the results using C2H6O as reference, Figure 2 shows that the dispersing
agents reduced the frequency of fractions larger than 100 μm and increased the frequencies
smaller than 100 μm. This is an indication that aggregates may have sizes in the range of sands
and when subjected to these dispersing agents, produce free silt and clay particles. This finding
is consistent with observation from Camapum de Carvalho et al. (2015), for similar soils from
the region.

Figure 2 - Particle size frequencies of soil S1-1.0 considering various chemical dispersion conditions: a)
(NaPO3)6; b) NaOH; c) Na3PO4; d) Na4P2O7.

60 60
0.038 mol/L 0.1 mol/L
0.070 mol/L 0.5 mol/L
50 50
0.130 mol/L 1.0 mol/L
0.240 mol/L 5.0 mol/L
40 40
Frequency (%)

0.450 mol/L 10.0 mol/L


C2H6O C2H6O
30 30

20 20

10 10

0 0
a) b)

60 60
0.02 mol/L 0.01 mol/L
0.05 mol/L 0.02 mol/L
50 50
0.12 mol/L 0.03 mol/L
0.30 mol/L 0.06 mol/L
40 40
Frequency (%)

0.50 mol/L 0.10 mol/L


C2H6O C2H6O
30 30

20 20

10 10

0 0
0.5 2 5 20 50 100 250 420 0.5 2 5 20 50 100 250 420
2 5 20 50 100 250 420 1000 2 5 20 50 100 250 420 1000
μm μm
c) d)

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The concentration of dispersing agent had varying effects, depending on the compound. It is
also important to note that the maximum concentration does not necessarily corresponds to
maximum dispersion, because after a certain concentration, saturation adsorption of the
dispersants might occur on the clay particles, and therefore cause aggregation of particles
(BINDU; RAMABHADRAN, 2010; KAUR; FANOURAKIS, 2016). In the case of (NaPO3)6,
the optimum concentration that produces maximum disaggregation was 0.07 mol/L, with > 100
μm fractions reducing from 80.5% using C2H6O, to 70.1% using the dispersing agent. An
equivalent increase is observed in the frequency of the fractions < 100 mm, increasing from
19.5% to 29.9%. In the case of NaOH, the optimum concentration of 10.0 mol/L produced
significantly higher degrees of disaggregation, with > 100 μm fractions reducing from 80.5%
using C2H6O, to 30.1% using the dispersing agent. For Na3PO4, the optimum concentration was
0.30 mol/L, with > 100 μm fractions reducing from 80.5% to 60.2%. Finally, for Na4P2O7, the
optimum concentration was 0.10 mol/L, with > 100 μm fractions reducing from 80.5% to
64.9%. In summary, the optimum concentrations are close but not equal to the saturation
concentration in the case of NaOH and Na4P2O7, and significantly lower than the saturation
concentration in the case of (NaPO3)6 and Na3PO4. These results indicated that (NaPO3)6,
Na3PO4, and Na4P2O7 presented similar results when compared to each other, considering the
optimum concentrations, and the NaOH had a significantly superior dispersion effect. It is
important to note the data presented in Figure 2 do not indicate whether aggregates were fully
destroyed.

Disaggregation with NaOH proved to be significantly higher. However, due to the high
variability of the results obtained from the ten subsamples, evidenced mainly for the highest
concentration (10 mol/L) (with SDs within textural classes varying from 0% to 7.7%), a more
in-depth study was performed to evaluate the hypothesis that undissolved NaOH was present
in the analyzed samples. This was evidenced by performing tests with the pure NaOH solution
(i.e., no soil added) in the concentrations used in this study and comparing the obtained results
with determinations made with the soil dispersed in the same NaOH solution concentration.
Tests were executed in two condition, by executing the using as reference measurement medium
(denoted by the instrument software as “setzero”) pure deionized water and then by using the
NaOH solution at the same concentration as the reference medium. Based on the results shown
in Figure 3, it was found that the equipment would detect salt particles, and therefore they were
not completely dissolved. Similar behavior was also observed for Na3PO4, but with

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significantly lower effect to the test results. This indicates that great care must be exercised
when using dispersing agents that may not come into solution easily, despite being below the
saturation concentration. In the specific case of NaOH at 10 mol/L, this option was considered
inadequate, unless an identical solution is used to set the reference measurement medium, which
is not practicable for the equipment. In this way, it was found that the equipment was reading
finer particles of salt and that this influenced the PSD, mainly in the fine fraction, masking the
results for these dispersing agents.

Figure 3 - Influence of undissolved dispersing agents on soil S1-1.0: a) NaOH at 10.0 mol/L; b) Na3PO4 at 0.5
mol/L.

100 100
NaOH Na3PO4
solution solution
Soil (setzero Soil (setzero
80 with solution) 80 with solution)
Soil (setzero Soil (setzero
with water) with water)
Passing (%)

Passing (%)

60 60

40 40

20 20

0 0
0.0001 0.001 0.01 0.1 1 0.0001 0.001 0.01 0.1 1
Particle size (mm) Particle size (mm)
a) b)

A comparison between the PDS for the optimum analyzed concentrations of each dispersing
agent (with the exception of NaOH at 10 mol/L, which was disregarded), are shown in Figure
4. The PSDs obtained for the soil treated with C2H6O and deionized water (H2O) are also shown,
to serve as references. It is noted that NaOH was the best dispersing agent and Na3PO4 was the
second best dispersant. However, the chemical agents selected for a study concomitant with
physical dispersion were (NaPO3)6 and Na4P2O7 because they did not present problems of
undissolved salts of the dispersing agents. Wintermyer and Kinter (1955) also observed that
Na4P2O7 and (NaPO3)6 were capable of dispersing a lateritic tropical soil, but their findings
indicated that best dispersing agent was Na3PO4. However, no detailed study of salt
concentration was performed by these authors. Zhang, Germaine and Whittle (2005) also
confirmed that the deflocculants (NaPO3)6 and Na4P2O7 presented superior dispersion
capabilities. However, the best results were found by treating the sample with NaHCO3 prior
to using (NaPO3)6 for dispersion. The use of NaHCO3 removes cementing formed by cristalized

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Fe- and Al-oxides and, as a result, removes cementing aggregation. Their findinds indicate that
the treated sample is completely dispersed and produces a much larger fraction of clay.
However, it is argued by Zhang, Germaine and Whittle (2005) that the dissolution and removal
of Fe- and Al-oxides produces a new soil that cannot be the compared with the original material,
as solids originally present in the sample are removed. The same findings where presented by
Kaur and Fanourakis (2016), who concluded that the method using (NaPO3)6 combined with
pretreatment with NaHCO3 and Na4P2O7 were the first and second most efficient options.

In general terms, sodium phosphates increase the negativity of the surface charge of clay
mineral particles and replace cations in their double layers by Na+ ions (ANDREOLA et al.,
2004), resulting in repulsion between particles and hindering sedimentation of the fine fraction.
With this, there is an increase in the dispersion of soil particles, keeping them in more stable
suspensions.

Figure 4 - Comparison between the cumulative PSDs of soil S1-1.0 using various dispersing agents at optimum
concentrations.

100
(NaPO3)6 (0.07 mol/L)
90 NaOH (5.0 mol/L)
Na3PO4 (0.30 mol/L)
80
Na4P2O7 (0.10 mol/L)
70 C2H6O
H2O
Passing (%)

60
50
40
30
20
10
0
0.001 0.01 0.1 1
Particle size (mm)

4.3 INFLUENCE OF THE USE OF PHYSICAL DISAGGREGATION


PROCEDURES

Figures 5 and 6 present PSDs obtained using different methodologies of physical dispersion,
applied to soil S1-1.0. The results obtained with C2H6O are also presented, serving as a

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reference to a state of maximum preservation of aggregates. The results for each testing
condition are based on the average values of ten subsamples. The SD shown in Figure 5 for
each particle size interval are represented as ranges of values at the top of each bar. The obtained
SD varied between 0 and 4.5% for horizontal agitation, 0 and 3.1% when using the dispersion
cup, and between 0 and 3.5% when using ultrasonication. These values are similar to the SD
ranges observed for the sample preparation methods, as presented previously.

To evaluate the efficiency of the different physical dispersion procedures shown in Figure 5,
the obtained fractions of particles with sizes > 100 μm may be compared to the result using
C2H6O. Horizontal agitation produced a change from 80.5% using C2H6O, to 80.1% after
applying agitation for 4 hours and no variation after applying agitation for 16 hours. The use of
the dispersion cup resulted in changes from 80.5%, to values that gradually ranged from 69.3%
for 7.5 minutes to 48.8% for 60 minutes of dispersion. Finally, ultrasonication resulted in
changes from 80.5%, to values that also decreased gradually with time, ranging from 74.7% for
0.5 minutes to 57.3% for 15 minutes of ultrasonication.

The results shown in Figures 5 and 6 indicate that the use of horizontal agitation, even for longer
periods of time, proved to be relatively less effective in soil disaggregation. Although the
horizontal agitation method was recommended by Gee and Bauder (1986) and Teixeira et al.
(2017), it was not efficient for disaggregation of soil S1-1.0. An alternative procedure would
be to introduce coarse sand as abrasive material during agitation, as performed by Oliveira et
al. (2002) for gibbsitic latosols, similar to the soil of this study. However, this procedure was
not evaluated because it was not widely adopted. Disaggregation with the dispersion cup was
significantly more effective, with increasing disaggregation in relation to the application time.
However, significant changes were observed between 15, 30, and 60 minutes, with fractions of
particles > 100 μm decreasing from 60.9% to 54.6% and to 48.8%, respectively. This finding
indicates that the application time of 15 minutes, recommended by TMH1 (1986), D422–63
(ASTM, 1999) and NBR 7181 (ABNT, 2016), did not produce complete disaggregation. It is
also important to note that even the maximum duration of 60 minutes adopted herein may not
produce maximum disaggregation. A similar behavior was verified with the use of ultrasound,
with steadily increasing degrees of disaggregation over time. Higher durations of use of the
dispersion cup and ultrasound were not evaluated herein because they were considered
unfeasible in practice. In summary, using the dispersion cup offered the best method for

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physical disaggregation, but for longer periods than recommended in the literature and testing
standards.

Figure 5 - Particle size frequencies of soil S1-1.0 considering various conditions of physical dispersion: a)
horizontal agitation; b) dispersion cup; c) ultrasound.

60 60
7.5 minutes
4 hours
50 50 15 minutes
16 hours 30 minutes
40 40 60 minutes
Frequency (%)

C2H6O
C2H6O
30 30

20 20

10 10

0 0
0.025 0.5 2 5 20 50 100 250 420 0.025 0.5 2 5 20 50 100 250 420
0.5 2 5 20 50 100 250 420 1000 0.5 2 5 20 50 100 250 420 1000
μm μm
a) b)

60
0.5 minute
1 minute
50 2 minutes
4 minutes
40 8 minutes
15 minutes
Frequency (%)

C2H6O
30

20

10

0
0.025 0.5 2 5 20 50 100 250 420
0.5 2 5 20 50 100 250 420 1000
μm
c)

The relative effectiveness of the disaggregation methods observed herein is in agreement with
the results from Zhang, Germaine and Whittle (2005) on an old alluvium soil aggregated by Fe-
oxides. The authors noted that the clay fraction increased with the stirring time, accompanied
by a reduction in the silt and sand fractions. The degree of dispersion increases with increased

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remolding time basically because both agitation and stirring apply shearing and collision forces
to mechanically break down aggregates. However, there is some controversial information in
the literature regarding the required time for disaggregation. Gee and Bauder (1986), Kroetsch
and Wang (2008) and the international standard itself ISO 11277 (2009) recommend dispersion
for only 5 minutes. Zhang, Germaine and Whittle (2005) reported that the disaggregation in
dispersion cup for 15 minutes was sufficient to disintegrate all aggregates. However, Ogunwole
et al. (2001) observed increased disaggregation as a function of time, from 5 minutes to 24
hours and stabilized results between 24 and 48 hours.

The results selected for presentation in Figure 6 offer some interesting comparisons,
considering specific disaggregation times and the PSD obtained from a sedimentation and
sieving test on a sample prepared for 15 minutes in the dispersion cup, but without chemical
dispersing agent. The three PSDs obtained after disaggregation for 15 minutes are somewhat
similar, with the fraction > 100 μm equal to 60.9%, 57.3%, and 58.0% using laser diffraction
on samples prepared on the dispersion cup, laser diffraction on samples subjected to ultrasound,
and sedimentation on samples prepared on the dispersion cup, respectively. The differences
between the laser diffraction results and sedimentation are difficult to interpret, because the two
determination methods are based on completely different principles and because the interfering
factors differ greatly. Bittelli et al. (2019) observed that methods based on Stokes' law, as
sedimentation and others, provide an overestimation of the clay fraction in relation to the laser
diffraction method. This occurs due to the assumption that the sphericity of particles is not
correctly applied to particles in the clay range (VDOVIC; OBHODAS; PIKELJ, 2010;
BITTELLI et al., 2019).

The methodology developed for the preparation of soil samples agited using the dispersion cup
required drying and stirring the soil. This procedure was devised to avoid the effects of
hydrodynamic segregation that produced high variability when samples were collected before
drying, even during active stirring using a pipette. Figure 7 is presented to show why the soil
should not be completely dried prior to obtaining subsamples for the laser diffraction analyses,
but rather dried to a slurry state. It was found that oven-drying to zero water content causes an
increase in the aggregation of soil particles, with the soil returning to its original texture.

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Figure 6 - PSDs of soil S1-1.0 using the maximum durations of physical disaggregation.

100
Horizontal agitation (16 hours)
90 Dispersion cup (15 minutes)
Dispersion cup (60 minutes)
80 Ultrasound (15 minutes)
C2H6O
70 Sieve-sedimentation (without chemical dispersant)
Passing (%)

60
50
40
30
20
10
0
0.0001 0.001 0.01 0.1 1
Particle size (mm)

Figure 7 - PSDs of soil S1-1.0 prepared on the dispersion cup and with varying drying conditions after dispersion
for 60 minutes.

100
No drying
90
Oven-drying to slurry
80
Complete oven-drying
70
C2H6O
60
Passing (%)

50
40
30
20
10
0
0.0001 0.001 0.01 0.1 1
Particle size (mm)

4.4 COMBINATION OF CHEMICAL AND PHYSICAL


DISAGGREGATION

The combined effects of the use of chemical dispersion agents and physical disaggregation was
evaluated because their distinct effects may contribute in different ways to particle

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disaggregation and its size measurement. The selected chemical dispersants were (NaPO3)6, at
0.038 and 0.450 mol/L and Na4P2O7, at 0.010 and 0.10 mol/L. The optimum concentration of
(NaPO3)6 of 0.070 mol/L was not used, in favor of the 0.038 mol/L and 0.450 mol/L
concentrations recommended by Teixeira et al. (2017) and NBR 7181 (ABNT, 2016). The
method of physical disaggregation adopted was the use of the dispersing cup for 60 minutes,
with subsampling from the soil oven-dried to a slurry state. An additional analysis was
performed using sieving and sedimentation for a sample subjected, in conjunction, to 15
minutes of disaggregation in the dispersion cup and using (NaPO3)6 (0.450 mol/L), as
recommended by NBR 7181 (ABNT, 2016). Figures 8 and 9 present the obtained results. The
corresponding SD (shown in Figure 8) varied between 0.1 and 3.6% for (NaPO3)6 at 0.038
mol/L, 0.3 and 3.3% for (NaPO3)6 at 0.450 mol/L, 0 and 1.8% for Na4P2O7 at 0.010 mol/L, and
0.2 and 2.3% for Na4P2O7 at 0.10 mol/L. These values are similar to the SD ranges observed
for the sample preparation methods, as presented previously.

Figure 8 - Particle size frequencies of soil S1-1.0 for the combined use of chemical dispersion agents and
physical disaggregation.

60
(NaPO3)6 (0.038 mol/L)
(NaPO3)6 (0.450 mol/L)
50 Na4P2O7 (0.01 mol/L)
Na4P2O7 (0.10 mol/L)
40 Dispersion cup (60 minutes)
(NaPO3)6 (0.038 mol/L) + Dispersion cup
Frequency (%)

(NaPO3)6 (0.450 mol/L) + Dispersion cup


30
Na4P2O7 (0.01 mol/L) + Dispersion cup
Na4P2O7 (0.10 mol/L) + Dispersion cup
20 C2H6O

10

0
0.025 0.5 2 5 20 50 100 250 420
0.5 2 5 20 50 100 250 420 1000
μm

The disaggregation level has been evaluated by examining the fractions of particles with sizes
larger than 100 μm and comparing to those obtained using C2H6O, which was 80.5%. The use
of chemical dispersing agents and of the dispersion cup without combining these procedures
was shown in the previous sections, indicating that the best dispersing agent among those
presented in this section was Na4P2O7 at 0.10 mol/L, which produced a fraction of particles
with sizes > 100 μm of 64.9%. However, the effect of the dispersion cup was significantly

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superior, with a reduction to 48.8%. The combination of dispersing agents and physical
disaggregation was effective in further reducing the fraction of material > 100 μm, to 41.4%
and 39.2% for combination of dispersion cup and (NaPO3)6 at 0.038 and 0.450 mol/L,
respectively, and to 47.2% and 43.3% for combination of dispersion cup and Na4P2O7 at 0.010
and 0.10 mol/L, respectively. The results were not as intuitive. While the lower concentration
of (NaPO3)6 was more effective in reducing the fraction > 100 μm, once the soil is physically
disaggregated using the dispersion cup, a higher concentration of (NaPO3)6 becomes more
effective. Silva et al. (2015) noted that the increase in concentration of chemical dispersion
agent had different effect on the disintegration of several soils with variable mineralogical
composition. Kaur and Fanourakis (2016) also noted that higher concentrations do not always
produce better soil disaggregation. However, they observed this behavior by combining both
(NaPO3)6 and Na4P2O7 with physical dispersion with a standard paddle.

Figure 9 - PSDs of soil S1-1.0 for the combined use of chemical dispersion agents and physical disaggregation.

100
(NaPO3)6 (0.450 mol/L)
90 Na4P2O7 (0.10 mol/L)
80 Dispersion cup (60 minutes)
Dispersion cup + (NaPO3)6 (0.450 mol/L)
70 Dispersion cup + Na4P2O7 (0.10 mol/L)
Passing (%)

60 Sieve-sedimentation (with chemical dispersant)


C2H6O
50
40
30
20
10
0
0.0001 0.001 0.01 0.1 1
Particle size (mm)

It was observed that the isolated use of (NaPO3)6 and Na4P2O7 considering different
concentrations presented similar results, and that these results are also similar to those obtained
using C2H6O, which is supposed to preserve aggregations. Therefore, the combination of
chemical and physical disaggregation is necessary to obtain a stable and more disaggregated
suspension as possible. This finding is in accordance with that of other authors. Bartoli, Burtin
and Herbillon (1991) observed that latosols rich in gibbsite, such as the S1 sample, have
extremely stable aggregates, requiring a combination of physical and chemical treatments.

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Zhang, Germaine and Whittle (2005) also concluded, for a highly weathered soil formed in
tropical region, that chemical dispersion alone is not effective in disintegrating the aggregates
caused by cementation, and also requires physical disaggregation.

However, the addition of chemical dispersion to the physical disaggregation had relatively
limited effect on the PSD. It was noted that only a higher concentration of Na4P2O7 caused a
significant change in the soil dispersion, when used along with physical disaggregation.
Moreover, an only slightly higher dispersion using (NaPO3)6 at 0.45 mol/L is observed, when
comparing to Na4P2O7 at 0.10 mol/L. However, the results using (NaPO3)6 presented greater
variability than those using Na4P2O7. It is also interesting to note that the result using the
dispersion cup and Na4P2O7 was closer to the PSD determined by sedimentation and sieving,
considered the standard method from NBR 7181 (ABNT, 2016). In summary, the
disaggregation obtained by using Na4P2O7 at 0.10 mol/L, combined with agitation in a
dispersion cup for 60 minutes, was considered the superior methodology for disaggregation of
the tropical residual soil analyzed. This proved that latosols are generally difficult to disperse
due to the high content of Al- and Fe-oxides, which form relatively stable microaggregates
(PINHEIRO-DICK; SCHWERTMANN, 1996).

4.5 WEATHERING PROFILES FROM SITES S2, S3, AND S4

Chemical dispersion method with Na4P2O7 at 0.10 mol/L combined with the use of dispersion
cup for 60 minutes was the method that presented the best disaggregation of soil S1-1.0. For
this reason, this method was used in the analyzes of three tropical soil profiles (S2, S3 and S4).
Once again, C2H6O was used as a reference method, for a state of maximum aggregation.

Figures 10 and 11 present the obtained results. Statistical analysis of the SD of PSDs of soil
profiles S2, S3 and S4 indicated a more significant variability when compared to soil profile
S1, mainly for smaller depths and disaggregated samples. The SD obtained for chemically and
physically disaggregated samples varied between 0.6 and 5.2% for S2-0.5, 0.4 and 4.2% for
S2-6.0, 0.3 and 7.5% for S3-0.5, 0.1 and 4.7% for S3-5.5, 0.5 and 7.3 for S4-2.0, 0.4 and 8.7%
for S4-6.0, 0 and 0.8% for S4-10.0.

Analyzing the PSDs using only C2H6O, it is observed that the soils S1-1.0 and S2-0.5 have very
similar degree of aggregation. Soils S2-6.0 and S3-0.5 are also quite similar, as are the soils S3-

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5.5, S4-2.0 and S4-6.0, with small variations. In general, the soils when in the aggregate state
always show similar PSDs, indicating that the profiles of natural tropical soils have similar and
homogeneous characteristics for significant depths, that have similar degrees of weathering
(ZHANG; GERMAINE; WHITTLE, 2005; CAMAPUM DE CARVALHO et al., 2015). One
exception was sample S4-10.0, which is significantly finer.

Figure 10 - Particle size frequencies of weathering profiles: a) S2; b) S3; c) S4.

60 60
S2-0.5 | C2H6O S3-0.5 | C2H6O

50 S2-0.5 | Na4P2O7 50 S3-0.5 | Na4P2O7


+ Dispersion cup + Dispersion cup

40 S2-6.0 | C2H6O S3-5.5 | C2H6O


40
Frequency (%)

S2-6.0 | Na4P2O7 S3-5.5 | Na4P2O7


30 + Dispersion cup 30 + Dispersion cup

20 20

10 10

0 0
0.025 0.5 2 5 20 50 100 250 420 0.025 0.5 2 5 20 50 100 250 420
0.5 2 5 20 50 100 250 420 1000 0.5 2 5 20 50 100 250 420 1000
μm μm
a) b)

60
S4-2.0 | C2H6O
S4-2.0 | Na4P2O7 + Dispersion cup
S4-6.0 | C2H6O
50 S4-6.0 | Na4P2O7 + Dispersion cup
S4-10.0 | C2H6O
S4-10.0 | Na4P2O7 + Dispersion cup
40
Frequency (%)

30

20

10

0
0.025 0.5 2 5 20 50 100 250 420
0.5 2 5 20 50 100 250 420 1000
μm
c)

While the aggregated soils are relatively similar, when the same soils are subjected to chemical
dispersing agents and physical disaggregation, significant variations in the PSDs are observed.

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The degree of highest disaggregation was observed for soils S2-0.5 and S3-0.5, with the
fractions > 100 μm decreasing from 79.2% to 29.5% and from 72.6% to 21.8%, respectively.
On the other hand, the lowest degree of disaggregation was observed for soil S4-10.0, with the
fraction > 100 μm decreasing from 10.6% to only 4.5%. Therefore, the proposed method for
the disaggregation of tropical soils proved to be very efficient for surface soil samples. The
small disaggregation observed for soil S4-10.0 indicated that this soil does not present stable
aggregates and, was therefore already quite disaggregated before the use of chemical dispersant
combined with physical disaggregation. Le Bissonnais et al. (2018) confirmed for two soils
from tropical regions with high Fe- and Al-oxides, that soil aggregates are more stable near the
ground surface than in deeper soil layers with lower degrees of weathering. The authors also
observed a large quantity of organic matter in the topsoil, as in the surface samples of the
analyzed profiles, which positively affects the aggregate stability. This can justify the increased
disaggregation of the most superficial samples.

Figure 11 - PSDs of the weathering profiles S1, S2, S3 and S4 using: a) C 2H6O; b) Na4P2O7 (0.10 mol/L)
combined with the dispersion cup.

100 100
S1-1.0 S1-1.0
90 S2-0.5 90 S2-0.5
80 S2-6.0 80 S2-6.0
S3-0.5 S3-0.5
70 70 S3-5.5
S3-5.5
60 S4-2.0 60 S4-2.0
Passing (%)

Passing (%)

S4-6.0 S4-6.0
50 50
S4-10.0 S4-10.0
40 40
30 30
20 20
10 10
0 0
0.0001 0.001 0.01 0.1 1 0.0001 0.001 0.01 0.1 1
Particle size (mm) Particle size (mm)
a) b)

5. CONCLUSIONS

A variety of sample preparation methods, including various types and concentrations of


chemical dispersants and physical disaggregation, were analyzed to disperse tropical residual
soils from central-western Brazil. The physical and chemical dispersion methods were
evaluated for determination of PSD in a laser diffraction equipment and compared with the

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standard sieving and sedimentation procedures of the Brazilian standard NBR 7181 (ABNT,
2016). The resulting degree of dispersion was evaluated through granulometric soil analysis.

As a result of their composition with the presence of Fe- and Al-oxides and the high weathering
process during their formation, tropical soils are not easily dispersible in water, because the
high weathering causes the formation of aggregates through cementation and aggregation in
these soils. The results revealed that both physical and chemical dispersions are necessary to
obtain a stable and completely dispersed suspension. Therefore, the most efficient method with
less variability for disaggregation of the tropical soils analyzed was the combination of Na4P2O7
at 0.10 mol/L and the dispersion cup for 60 minutes. The isolated chemical disaggregation
showed to have a varied effect depending on the composition and concentration of the
dispersing agent used, since the increase in concentration did not always correspond to an
increase in soil dispersion. In turn, the physical disaggregation showed to have a more
significant isolated effect on the disintegration of aggregations, with increasing disaggregation
as a function of the increased time of soil dispersion.

In addition, it was found that tropical soils are strongly influenced by the segregation of samples
and that the complete drying of the dispersed solution at high temperatures causes the almost
complete reaggregation of soil particles. The drying is usually accompanied by some physical-
chemical reaction, which can cause the opposite effect of dispersion in the soil. In addition, it
was noted that the proposed methodology for chemical and physical disaggregation of tropical
soils presents excellent results for more superficial samples and that soil aggregates are more
stable near the surface than in deeper soil layers with lower degrees of weathering.

ACKNOWLEDGMENTS

This research project was funded by the Coordenação de Aperfeiçoamento de Pessoal de Nível
Superior - Brasil (CAPES) - Finance Code 001.

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APPENDIX

The variability study was performed for all methods evaluated in the sample preparation
methods and for chemical and physical analyses, individually or combined. The results of
standard deviation (SD) and coefficient of variation (CV), for interpretation of the data
variability in relation to the mean of the PSD for each fraction analyzed, are presented in Table
5, 6 and 7.

Table 5 - Statistical analysis of the sample preparation methods analyzed for soil S1-1.0.

Method 1 Method 2 Method 3 Method 4 Method 5


Fractions (μm) SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
0.5 - 2 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
2-5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
5 - 20 0.2 18.5 0.4 29.5 0.6 49.7 0.3 16.8 0.1 12.4
20 - 50 0.5 7.4 0.8 12.2 1.1 24.3 0.4 5.3 0.3 4.4
50 - 100 1.5 7.8 2.6 16.6 1.9 17.4 2.5 12.2 1.1 4.9
100 - 250 2.7 6.1 2.4 5.9 3.6 9.8 2.4 5.4 1.1 2.1
250 - 420 2.9 11.8 1.8 7.8 2.6 10.3 3.0 13.6 1.4 8.1
420 - 1000 1.5 31.2 4.8 41.1 4.2 24.1 1.5 42.9 1.3 74.8

Table 6 - Statistical analysis of the disaggregation methods analyzed for soil S1-1.0.

C2H6O (NaPO3)6 (mol/L) NaOH (mol/L)


0.038 0.070 0.130 0.240 0.450 0.10 0.50 1.00
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
0.5 - 2 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 210.8 0.2 40.9 0.9 69.5
2-5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.3 36.2 0.5 26.4 2.4 48.4
5 - 20 0.0 0.0 0.5 160.5 0.1 64.6 0.1 68.8 0.1 73.2 0.1 57.6 0.5 9.2 0.9 11.7 5.5 40.7
20 - 50 0.3 9.8 1.8 29.2 0.7 10.7 1.0 15.7 1.1 19.0 0.4 6.3 0.4 2.9 0.6 3.8 1.1 5.4
50 - 100 1.3 8.0 2.3 11.4 2.3 10.2 2.5 11.6 2.7 13.5 1.6 8.6 0.8 3.4 1.4 5.2 4.9 20.8
100 - 250 1.8 3.4 2.8 5.5 2.3 4.3 1.3 2.4 2.1 4.1 2.3 4.6 1.4 3.3 1.8 5.0 3.3 12.2
250 - 420 2.6 10.1 2.9 14.9 2.5 17.2 2.9 16.0 2.5 11.5 3.3 14.3 1.1 9.6 0.6 7.6 0.6 8.9
420 - 1000 0.7 23.9 1.0 52.3 0.6 67.4 0.6 46.0 0.8 35.4 0.7 27.0 0.5 35.2 0.4 19.3 0.3 16.4

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NaOH (mol/L) Na3PO4 (mol/L) Na4P2O7 (mol/L)


5.00 10.00 0.02 0.05 0.12 0.30 0.50 0.01 0.02
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0
0.5 - 2 0.1 32.4 0.5 47.9 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.1 316.2 0.0 0.0 0.0 0.0
2-5 0.1 1.7 2.6 30.4 0.0 0.0 0.0 0.0 0.1 47.2 0.2 31.4 0.2 26.7 0.0 0.0 0.0 0.0
5 - 20 0.4 2.0 5.8 17.5 0.2 21.9 0.3 12.4 0.2 5.1 0.4 9.3 0.5 11.2 0.1 18.8 0.1 10.9
20 - 50 0.8 3.0 7.7 47.3 0.5 6.4 0.6 5.5 0.4 3.9 0.7 5.6 0.5 3.7 0.6 8.2 0.5 6.1
50 - 100 0.7 4.3 1.0 9.2 1.5 6.9 2.3 11.0 1.8 8.7 2.2 9.8 1.3 5.9 2.4 11.7 1.9 9.6
100 - 250 0.5 2.2 2.4 11.2 1.5 2.9 1.5 3.3 0.9 2.0 1.1 2.4 0.8 1.8 1.9 3.9 2.2 4.6
250 - 420 0.7 9.6 2.2 32.0 2.5 13.1 3.1 18.2 1.8 11.6 2.6 18.5 1.4 9.4 3.8 17.6 3.3 15.7
420 - 1000 0.7 20.1 1.2 56.8 0.7 39.5 0.6 37.4 0.3 24.1 0.4 28.1 0.4 27.2 0.9 41.2 0.9 37.4
Na4P2O7 (mol/L) HA DC-ND
0.03 0.06 0.10 4 hours 16 hours 7.5 min 15 min 30 min 60 min
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 315.9 0.4 78.4 0.5 29.2
0.5 - 2 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.3 263.4 1.0 32.3 1.3 20.1 1.7 15.8
2-5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.7 211.7 0.6 18.0 0.8 16.1 1.0 14.6
5 - 20 0.0 1.6 0.2 10.2 0.3 15.6 0.0 0.0 0.0 0.0 1.2 62.5 0.8 15.8 0.8 13.6 1.1 14.7
20 - 50 0.3 3.0 0.8 9.5 0.8 9.0 0.8 26.3 0.6 21.4 1.3 18.7 1.0 11.8 1.1 11.5 1.1 11.0
50 - 100 1.1 5.2 2.3 12.1 3.0 14.5 3.0 17.8 2.5 15.8 1.6 7.8 0.9 4.4 1.2 6.7 0.5 2.6
100 - 250 1.4 2.9 1.5 3.2 2.0 4.5 1.9 3.6 3.8 7.4 2.3 4.2 2.4 5.1 2.8 6.4 4.1 10.8
250 - 420 1.8 9.3 3.3 15.1 2.9 17.2 4.5 17.7 4.5 16.8 3.1 23.4 2.1 16.4 2.7 25.7 1.8 23.0
420 - 1000 0.7 35.5 0.7 26.0 3.1 122.1 1.7 56.8 1.2 39.5 0.4 44.5 0.3 24.2 0.3 36.2 0.4 58.3
DC-OD DC-ODS U
15 min 60 min 60 min 0.5 min 1 min 2 min 4min 8 min 15 min
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.2 18.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 139.2
0.5 - 2 0.0 0.0 0.0 0.0 0.4 3.8 0.0 0.0 0.0 0.0 0.0 0.0 0.8 158.1 1.1 47.2 1.3 31.6
2-5 0.0 0.0 0.0 0.0 0.2 3.7 0.0 0.0 0.0 0.0 0.0 0.0 0.6 163.6 0.8 45.7 0.6 21.7
5 - 20 0.0 2.8 0.1 8.4 0.3 3.7 0.1 233.7 0.2 55.2 0.3 27.9 0.5 29.5 0.9 29.4 0.7 17.0
20 - 50 0.2 3.2 0.5 6.0 0.4 3.8 1.0 20.4 1.0 14.3 1.1 13.8 1.3 14.4 1.4 15.3 1.7 16.5
50 - 100 0.7 3.4 1.4 8.0 0.7 4.0 2.2 11.1 2.1 9.6 2.1 9.6 2.0 8.8 1.9 8.7 1.8 8.5
100 - 250 0.9 2.1 1.4 3.9 1.7 4.7 1.6 3.0 1.2 2.2 1.1 2.1 1.7 3.2 2.7 5.5 3.2 6.8
250 - 420 1.3 5.6 1.2 4.6 1.7 15.2 3.5 18.0 2.7 16.4 2.5 17.0 2.5 18.9 2.5 21.4 2.5 25.6
420 - 1000 0.4 10.8 3.3 33.6 1.4 80.1 0.8 51.4 0.5 38.4 0.4 37.5 0.3 28.8 0.5 54.6 0.6 77.9
H+U (mol/L) P+U (mol/L) H+DC (mol/L) P+DC (mol/L)
0.038 0.45 0.01 0.10 0.038 0.45 0.01 0.1
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.1 16.1 0.3 22.5 0.0 3.3 0.2 15.9
0.5 - 2 0.1 153.8 0.2 47.4 0.3 30.5 0.3 13.5 0.6 6.5 1.3 11.4 0.2 2.4 0.6 6.1
2-5 0.8 74.9 0.1 5.5 0.2 9.3 0.3 7.7 0.5 5.8 1.0 11.1 0.2 2.7 0.5 5.5
5 - 20 0.5 14.5 0.2 3.4 0.4 7.5 0.4 5.5 0.6 5.3 1.2 12.6 0.2 2.6 0.5 5.2
20 - 50 0.6 6.4 0.4 3.6 0.5 4.9 1.1 8.7 1.1 9.7 1.4 12.2 0.3 3.3 0.5 5.3
50 - 100 2.1 10.0 0.8 3.9 1.7 8.5 1.8 9.3 1.3 7.6 1.3 7.0 0.5 2.6 0.6 3.7
100 - 250 0.9 1.9 1.4 3.0 0.4 0.8 1.9 4.3 1.9 5.8 3.0 9.1 1.0 2.8 0.6 1.7
250 - 420 1.7 12.0 1.7 14.6 1.7 13.1 2.8 28.4 3.7 44.6 3.3 56.2 1.9 19.4 2.3 28.8
420 - 1000 0.1 6.8 0.3 36.6 0.1 8.8 0.6 67.9 0.9 89.6 0.6 120.9 0.4 41.8 0.5 53.1
HA:horizontal agitation; DC-ND: dispersion cup without drying; DC-OD: dispersion cup with complete drying in
an oven; DC-ODS: dispersion cup with drying in an oven up to the state of slurry; U: ultrasound; H+U: (NaPO 3)6
combined with ultrasound; P+U: Na4P2O7 with ultrasound; H+DC: (NaPO3)6 with dispersion cup; P+DC: Na4P2O7
with dispersion cup.

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Table 7 - Statistical analysis of the PSD of soils S2, S3 and S4.

S2-0.5 S2-6.0 S3-0.5 S3-5.5


C2H6O P+DC C2H6O P+DC C2H6O P+DC C2H6O
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.0 0.0 0.6 16.8 0.0 0.0 0.4 10.7 0.0 0.0 0.9 16.4 0.0 0.0
0.5 - 2 0.0 0.0 2.8 15.3 0.0 0.0 1.3 9.5 0.0 0.0 2.9 15.3 0.0 0.0
2-5 0.0 0.0 2.6 14.9 0.0 0.0 1.4 9.6 0.0 0.0 2.6 15.0 0.1 62.1
5 - 20 0.1 102.7 2.4 15.2 0.7 48.6 2.0 9.7 0.5 69.3 2.9 15.8 0.6 11.2
20 - 50 0.7 16.7 0.7 11.5 1.4 18.1 0.8 7.0 1.9 25.0 0.9 10.3 1.1 10.2
50 - 100 1.9 11.8 0.9 10.2 2.3 11.3 0.8 7.2 2.7 13.9 1.3 13.7 1.3 6.9
100 - 250 4.0 8.2 5.2 23.6 1.8 3.7 4.2 22.0 4.9 11.8 7.5 41.5 1.6 4.2
250 - 420 4.1 15.4 3.9 60.8 4.6 24.5 2.0 47.2 5.1 19.8 1.7 52.1 2.7 12.3
420 - 1000 1.9 52.5 0.8 71.2 1.0 52.7 0.5 60.7 2.5 47.6 0.3 55.1 0.6 17.7
S3-5.5 S4-2.0 S4-6.0 S4-10.0
P+DC C2H6O P+DC C2H6O P+DC C2H6O P+DC
Fractions (μm) SD CV SD CV SD CV SD CV SD CV SD CV SD CV
0.0255 - 0.5 0.1 162.8 0.0 0.0 0.6 18.9 0.0 0.0 0.7 18.9 0.1 137.0 0.0 4.4
0.5 - 2 0.7 23.8 0.0 210.7 2.2 14.4 0.0 0.0 2.4 19.1 0.5 8.6 0.2 1.9
2-5 0.6 10.6 0.5 133.5 2.3 14.9 0.3 106.1 3.5 19.6 1.7 6.7 0.5 1.6
5 - 20 1.9 9.8 1.8 40.3 2.1 14.9 1.3 31.8 4.2 18.7 3.3 7.8 0.8 1.8
20 - 50 1.7 8.1 2.1 19.5 1.2 14.2 1.8 16.2 1.6 13.7 0.4 4.9 0.2 2.4
50 - 100 0.8 4.5 3.5 14.8 2.2 16.7 3.9 15.2 2.9 25.9 2.4 34.1 0.1 4.4
100 - 250 4.7 19.0 8.1 20.4 7.3 29.7 2.7 5.7 8.7 51.7 2.9 37.9 0.7 21.0
250 - 420 1.7 28.1 3.8 21.2 3.4 68.4 5.1 47.9 2.5 85.3 0.4 16.4 0.5 43.0
420 - 1000 0.5 51.2 1.6 55.3 0.5 94.2 0.7 90.9 0.4 96.6 0.3 31.1 0.2 145.4
P+DC: Na4P2O7 with dispersion cup.

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ARTIGO 2

Nesse capítulo será apresentado o produto final dessa pesquisa, o artigo científico “The role of
the structure and aggregation of a tropical residual soil in its soil-water characteristic curve”.
Esse artigo será submetido a revista Géotechnique Letters.

The role of the structure and aggregation of a tropical residual


soil in its soil-water characteristic curve

J. C. Souza¹, G. F. N. Gitirana Jr.¹, and S. K. Vanapalli²


¹Universidade Federal de Goiás, Goiânia, Goiás, Brazil.
²University of Ottawa, Ottawa, Ontario, Canada.

ABSTRACT

The pore size distribution (PoSD) and the soil-water characteristic curve (SWCC) are important
properties for the study of unsaturated soil behavior. These properties are strongly related to the
particle size distribution (PSD) but depend also on the aggregation and soil structure. The
behavior of an aggregate tropical soil under various structural conditions was evaluated through
its SWCCs and considering the relationship between the SWCC and the PSD. The analyzed
soil was compacted statically, disaggregated by spatulation, or using a dispersion cup, and then
reconstituted from an initial slurry state to different void ratios. SWCCs were determined using
pressure plate and dew point potentiometer devices. The results showed that the SWCCs
presented bimodal behavior. It was also observed that the structural changes imposed by the
different soil preparation techniques has a greater effect on soil macropores, with micropores
remaining unaffected. In addition, higher void ratios resulted in a greater change in the retention
properties due to the disaggregation of the soil macrostructure. The modeling of the SWCC
using pedotransfer functions and PSDs under different aggregation conditions underestimated
the water content when the suction is relatively high. This proves that the conversion of PSD
into PoSD and SWCC of the prediction models analyzed cannott adequately to represent the
double porosity of bimodal tropical soils.

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Keywords: unsaturated soils. disaggregation. tropical soils. bimodal behavior. prediction


model.

1. INTRODUCTION

Studies regarding soil-water retention characteristics have gained momentum in recent years.
This has occurred because the soil-water characteristic curve (SWCC) is a useful tool for
interpreting unsaturated soil behavior and predicting unsaturated soil properties such as
permeability, shear strength, and volume change (NG; MENZIES, 2007; FREDLUND, D.;
RAHARDJO; FREDLUND, M., 2012).

The mechanical and hydraulic behavior of soils is influenced by their fabric and structure
(MITCHELL; SOGA, 2005; ROMERO; SIMMS, 2008), but is of particular importance for
structured soils such as tropical residual soils (MARINHO, 2005; KOLIJI; VULLIET;
LALOUI, 2010). Soil fabric refers to the arrangement and grouping of particles and the
formation of the corresponding porous volumes, while structure refers to the arrangement of
particles that is produced by the combined effects of fabric, soil composition and stress state
(MITCHELL; SOGA, 2005). The soil fabric and structure may be evaluated by techniques such
as mercury intrusion porosimetry (DELAGE et al., 1996; KOLIJI et al., 2006), SWCC
(MASCARENHA, 2008; MIGUEL; BONDER, 2012; SUN et al., 2016), scanning electron
microscopy (DELAGE; LEFEBVRE, 1984; DJÉRAN-MAIGRE et al., 1998; ROMERO;
SIMMS, 2008), neutron radiography and computed tomography (KOLIJI; VULLIET;
LALOUI, 2010; ARAUJO et al., 2020).

According to Lambe and Whitman (1969), the soil pores forming the soil structure can be
subdivided into inter- and intra-aggregate pores. The inter-aggregate pores are found between
multi-particle aggregates, while intra-aggregate pores occur between the particles forming the
aggregates (LAMBE; WHITMAN, 1969). According to Romero, Gens and Lloret (1999) and
Tuller, Or and Dudley (1999), water present in the macro-structure (inter-aggregate) occurs
predominantly in the form of funicular and pendular water, having a dominant capillary storage
mechanism, whereas inside the micro-structure (intra-aggregate), the retention mechanism may
be greatly associated with the adsorbed water or film water and, therefore, governed by
physical-chemical bonds. However, significant amounts of pendular water and funicular water

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may also be found in intra-aggregate pores, depending on their dimensions (LIKOS; JAAFAR,
2013; WANG et al., 2017).

Capillary storage is mainly related to the void ratio and pore size distribution (GVIRTZMAN;
ROBERTS, 1991; ALVES; GITIRANA JR.; VANAPALLI, 2020). Pore size distribution
(PoSD) corresponds to the geometric arrangement of soil particles (KOLIJI et al., 2006). This
property is sensitive to mechanical actions, which mainly produce a change in macro-structure,
affecting menisci and free water contained in the interconnected and inter-aggregated pores
(DJÉRAN-MAIGRE et al., 1998; ROMERO; GENS; LLORET, 1999). On the other hand, in
low water contents corresponding to intra-aggregate water, the influence of PoSD changes is
considered insignificant, indicating that the relationship between suction and water is mainly
dependent on the specific surface and the chemical composition of the soil (MCQUEEN;
MILLER, 1974; ROMERO; VAUNAT, 2000). As a result, the SWCC is directly influenced by
volume changes, PoSD and adsorption (MARINHO, 2005). However, the retention mechanism
related to adsorbed water is more relevant in soils with active clay minerals (AUBERTIN et al.,
2003).

The PoSD is related but not necessarily completely defined by the particle size distribution
(PSD). Arya and Paris (1981) proposed a linear relationship for converting the PSD into the
PoSD, considering that the relative fraction of pores and the relative fraction of particle mass
were equal. Several researchers focused on improving the estimation of pore size from particle
size. PoSD can be estimated using a proportionality factor between pore size and associated
particle diameter (HAVERKAMP; PARLANGE, 1986), be determined using the concept of
bulk density and non-similar media (ZHUANG; JIN; MIYAZAKI, 2001), or based on particle
packing patterns (MOHAMMADI; VANCLOOSTER, 2011). Some researchers have also
considered a non-linear relationship between the PSD and the PoSD, indicating that when the
particle size is smaller than a certain critical value, the effective radius of the pores decreases
at faster rate as particles get smaller (HWANG; POWERS, 2003; CHANG; CHENG; QIAO,
2019).

The PoSD is not exclusively determined by PSD, because physical, chemical, and mineralogical
aspects related to the soil structure also have an important role (MITCHELL; SOGA, 2005).
The relationship between soil structure and its PoSD is particularly significant for tropical
residual soils (ROMERO; SIMMS, 2008; KOLIJI; VULLIET; LALOUI, 2010). The fabric of

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this type of soil is often influence by the aggregation of particles (MARINHO, 2005; KOLIJI;
VULLIET; LALOUI, 2010). Aggregate soils are characterized by a double porosity structure,
corresponding to the micropores and macropores (DELAGE et al., 1996; MARINHO, 2005;
KOLIJI et al., 2006; KOLIJI; VULLIET; LALOUI, 2010). Delage and Lefebvre (1984), relate
macropores as inter-aggregate pores and micropores as intra-aggregate pores. Thus, the
behavior of these soils is generally considered complex, not only because of their structure, but
also because of possible effects resulting from aggregation and particle cementing (FONTES;
WEED, 1991; ZHANG et al., 2004). Some studies have illustrated the importance of the size,
shape, and arrangement of aggregations, as well as the distribution and connectivity of pores in
soil behavior (DJÉRAN-MAIGRE et al., 1998; ROMERO; SIMMS, 2008).

Camapum de Carvalho, Gitirana Jr. and Carvalho (2012) explain that to understand the behavior
of tropical residual soils, attention should be given to the characteristics of the macropores. In
general, the macro-structure of tropical residual soils depends on the processes of laterization
and weathering, while the micro-structure depends on the nature of the original rock, the
genesis, and the degree of cementation (GIDIGASU, 2012). In this regard, microstructural
studies are important to improve the understanding of the macroscopic behavior and physical
properties of these soils, especially when under unsaturated conditions (ROMERO; SIMMS,
2008).

A limited number of studies on the SWCC of tropical residual soils may be found in the
literature, such as Feuerharmel, Gehling and Bica (2006), Miguel and Bonder (2012), Sun et al.
(2016) and Pecapedra et al. (2017). The SWCC is strongly influenced by the history of stress
and, consequently, by the void ratio (MARINHO, 2005). Moreover, tropical residual soils often
present SWCCs that are influenced by their irregular PSDs, sometimes poorly graded, and with
bimodal characteristics (CAMAPUM DE CARVALHO; GITIRANA JR.; CARVALHO,
2012). The characteristics of the soils’ PSD, along with structural characteristics, influence the
PoSD. The soils that present bimodal SWCCs usually have their PoSD divided in two groups
of pore-size ranges (macropores and micropores) and, therefore, present two suction ranges
producing desaturation. Thus, SWCCs with bimodal behavior have two air entry values, the
first corresponding to the desaturation of the macropores, and the second of the micropores
(FEUERHARMEL; GEHLING; BICA, 2006).

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The PoSD and the SWCC are important properties for the understanding of water storage and
water movement in soil (WU, 1988; FREDLUND, D.; RAHARDJO; FREDLUND, M., 2012).
The laboratory determination of these properties involves relatively complex and time-
consuming testing. Therefore, several researchers have proposed models for the prediction of
the PoSD and of the SWCC, based on relatively simple soil properties, such as the PSD, void
ratio, and Atterberg limits. These models are often referred to as pedotransfer functions (PTFs).
The development of PTFs allow a better understanding of soil behavior and may even replace
experimental determinations in preliminary studies and design. The works of Gupta and Larson
(1979), Arya and Paris (1981), Haverkamp and Parlange (1986), Arya and Dierolf (1989), M.
Fredlund, D. Fredlund and Wilson (2002), Aubertin et al. (2003), Likos and Jaafar (2013),
Wang et al. (2017) and Alves, Gitirana Jr. and Vanapalli (2020) are some examples of PTFs
for the prediction of the SWCC. Table 1 summarizes some characteristics of these models.

The complexity of existing PTFs varies. Typically, these models are based on simplified
interpretations of soil pore size and pore geometry. In most cases, the PTFs are based on the
hypothesis that the PSD allows the indirect determination of the PoSD of the soil, through an
idealized particle arrangement (ARYA; PARIS, 1981; ARYA; DIEROLF, 1989; AUBERTIN
et al., 2003; LIKOS; JAAFAR, 2013). The models can be considered theoretical, empirical, or
semi-empirical (WU, 1988). In general, theoretical models such as M. Fredlund, D. Fredlund
and Wilson (2002), Likos and Jaafar (2013), and Alves, Gitirana Jr. and Vanapalli (2020) are
fundamentally based on formulations that follow physical concepts. Empirical models, such as
Gupta and Larson (1979), Saxton et al. (1986) and Tomasella, Hodnett e Rossato (2000)
consider statistically determined parameters specific to each type of soil. A considerable
number of models combine empirical parameters with physical representation of other
parameters. These models, such as Arya and Paris (1981), Arya and Dierolf (1989), Aubertin
et al. (2003) and Wang et al. (2017), are considered semi-empirical. Despite providing a simple
and practical way to estimate the SWCC, most PTFs have important limitations. The most
common limitations are related to not considering the effects of hysteresis, stress level, soil
structure, and volume change (AUBERTIN et al., 2003). However, the PTFs recently proposed
by Likos and Jaafar (2013) and Alves, Gitirana Jr. and Vanapalli (2020) consider hysteresis and
pore scale analysis, as an attempt to better represent soil structure, although only for relatively
simple coarse-grained materials.

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Table 1 - Main characteristics and equations of some SWCC prediction models.

Authors Type Principle Equation


Arya and Semi- Capillary 2Ts 4eni (1− )
 = ri = Ri
Paris (1981) empirical retention ri 6
Arya and
Semi- Capillary 2Ts 4 Ri 3e
Dierolf  = ri =
(1989)
empirical retention ri 3 *
 
   
M.     
 ln 1 +  
Fredlund,  hr    
w = ws 1 − 
Regression 1
 
6 
D. Fredlund Theoretical
analysis 
 ln 1 + 10     nf 
mf

and Wilson
  
  hr    ln exp (1) +   


(2002)     af   
 
     
Capillary hco 2 h
and S = Sc + S a* (1 − Sc ) Sc = 1 − [( ) + 1]m exp[−m( co ) 2 ]
Aubertin et Semi- adhesion  
al. (2003) empirical forces and (hco / n ) 2/3
regression S a* = 1 − (1 − Sa ) Sa = ac C 1/3
e ( /  n )1/6
analysis
R fill Rmáx
Likos and
Jaafar
(2013)
Theoretical
Pore scale
analysis
S= 
Rmín
f ( R )dR + 
R fill
S a / w f ( R )dR

Capillary
and 1
−1
Wang et al. Semi- adhesion    n  n
S = 1 +   
(2017) empirical forces and    
regression  
analysis
Alves,
Gitirana Jr. 
Pore scale 2     sin  1 − cos       
and Theoretical Vp = 2 R3 (1 − cos  ) 1 + cot  sin  + cot  1 − cos  −  +    
analysis  
 
   cos  sin   cos     

Vanapalli
(2020)
Notes: ψ: suction; Ts: surface tension of water; ri: radius of the cylindrical capillary tube of fraction i; R i: particle
radius of fraction i; e: void ratio; n i: number of particles of fraction i; α: empirical parameter related to particle
shape dependent of ni; α*: empirical parameter related to particle shape independent of ni; w: gravimetric water
content; ws: gravimetric water content at saturation; hr: constant parameter used to adjust the lower portion of the
curve; af: fitting parameter related to the air-entry value; nf: fitting parameter related to the maximum slope of the
curve; mf: fitting parameter related to the curvature of the slope; S: total degree of saturation; S c: degree of
saturation caused by capillary forces; Sa*: truncated adhesion component of the degree of saturation; S a: degree of
saturation caused by adhesive forces; hco: equivalent capillary rise in the porous media; m: distribution parameter
of the influence of PoSD; ac: adhesion coefficient; Cψ: correction factor; ψn: normalization parameter; Rfill: pore
radius corresponding to snap off for cylindrical capillary; Rmin: minimum bundled radius; Rmax: maximum bundled
radius; f(R): probability distribution function; Sa/w: degree of saturation of a partially saturated unit pore; α and n:
fitting parameters; Vp: volume of water corresponding to the pendular ring; R: spherical particles radius; φ: filling
angle; Vbe: volume of water corresponding to the boundary effect; R cap_1 and 2: radius of the each caps; h: pore
height.

The SWCC prediction models found in the literature do not consider, in a specific manner, the
characteristics of tropical residual soils with bimodal structures. As a result, the existing PTFs
may not be suitable for soil with aggregates and double porosity (KOLIJI et al., 2006). In these

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materials, although a significant portion of the pore-water is stored in micropores, the


permeability of macropores is much higher than that of micropores (TUNCAY;
CORAPCIOGLU, 1995). Therefore, the limitation of these models reduces their applicability
in engineering design involving this type of soil. Research on the SWCC prediction of tropical
soils also allows a better understanding of their overall behavior mechanisms, including volume
change and shear strength characteristics. Thus, it becomes relevant to analyze the various PTFs
available in the literature and evaluate the use in tropical residual soils.

Therefore, the objective of this work was to evaluate how the structure and aggregation of a
laterialized tropical residual soil influences its soil-water retention properties. For this purpose,
SWCCs were determined with their preserved and destroyed aggregations, given the
importance of the aggregations in the behavior of these tropical soils. In the same way,
information regarding of degree of aggregation was obtained under the same preserved and
removed aggregation conditions, in terms of the PSD. Finally, the performance of some
prediction models for the SWCC, based on theoretical approaches and incorporating capillarity
and adsorption retention, were evaluated. The models were evaluated using the PSDs at various
degrees of aggregation.

2. MATERIALS AND METHODS

2.1 BASIC PROPERTIES OF THE STUDIED SOIL

The soil studied is a residual micaschiste soil, highly weathered, typical of the city of Goiânia,
Goiás, Brazil (16°43'S, 49°17'W). The soil was classified as red oxisols, according to the USDA
soil taxonomy, with homogeneous and deep profile. The soil was removed by trenching at 1 m
of depth (horizon B). Physical characterization tests were performed by Araujo (2019) and
indicated a specific weight of solids (γs) of 26.39 kN/m3, a liquid limit (wL) of 33%, a plastic
limit (wP) of 22%, and a plasticity index (IP) of 11%. The soil under study is classified as a low
plasticity clay (CL) by the unified soil classification system (USCS).

The chemical characterization of the soil indicated predominance of potassium in its


composition, low organic matter content (12.0 g/dm³), a cation exchange capacity of 4.53
cmolc/dm³ and a pH of 5.5. The mineralogical characterization of the soil, based on the X-ray

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diffraction technique, identified the presence of gibbsite as the main mineral. In addition, the
minerals quartz, kaolinite, hematite, and traces of diaspore, goethite and mica minerals were
also observed. The presence of gibbsite as the main mineral and the chemical properties
reported indicate significant weathering, which leads to soils that present high degrees of
aggregation (CONCIANI; BURGOS; BEZERRA, 2015; SANCHEZ, 2019).

2.2 ANALYSIS OF THE PARTICLE SIZE DISTRIBUTION

Figure 1 presents the obtained PSDs that were considered in this study. PSD analyses were
performed by the laser diffraction method, according to ISO 13320 (2009), and presented in
detail by Souza et al. (2020). Some methodological changes were made to the procedures
recommended by ISO 13320 (2009). These modifications were designed to identify the
maximum possible preservation of aggregates and the maximum possible degree of
disaggregation. These varying degrees of aggregation identified from the various PSDs are used
herein as basic information on the soil structure that can be used in its evaluation and for the
prediction of the SWCC.

Figure 1 - PSDs obtained by several testing procedures.

100
Preparation only in C2H6O
90
Preparation only in H2O
80 Dispersion cup + H2O
70 Dispersion cup + Na4P2O7
Passing (%)

60
50
40
30
20
10
0
0.0001 0.001 0.01 0.1 1
Particle size (mm)

The study presented by Souza et al. (2020) involved four chemical dispersion agents at various
concentrations and three physical disaggregation procedures at various application times. The
obtained results demonstrated a wide range of possible degrees of disaggregation, depending

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on the testing procedures. The two extreme conditions presented in Figure 1 involve chemical
agents that interfere with the properties of the soil particles’ surfaces (WEAVER; POLLARD,
1973; SRIDHARAN; JOSE; ABRAHAM, 1991) and modify the contact angle and water
surface tension (SOBOLEV et al., 2000; YUAN; LEE, 2013). These conditions were obtained
using ethyl alcohol (C2H6O), considered the state of highest aggregation (DUFRANC et al.,
2004), and tetrasodium pyrophosphate (Na4P2O7) at 0.10 mol/L combined with dispersion cup
for 60 minutes, considered the best method for disaggregation of the analyzed tropical soil.
However, Figure 1 shows that the PSDs obtained using the dispersion cup for 60 minutes
(without dispersing agent) and obtained for the soil prepared with pure deionized water are
relatively close to the extreme PSDs. Considering the intention to determine the SWCC using
water free of chemical agents, only the PSDs obtained using pure deionized water were
considered in this study, being assumed as representative of the soil structure at two
significantly distinct conditions of preservation of aggregates.

2.3 DETERMINATION OF THE SOIL-WATER CHARACTERISTIC


CURVE

The SWCCs were determined using the pressure plate method and a dew point potentiometer
instrument. Specimens were prepared at various conditions, representing different soil
structures, with special focus on the use of specimens that preserve the soil aggregates and on
the testing of specimens prepared under conditions of maximum possible disaggregation. The
specimen preparation conditions were specified to correspond to the sample preparation
methods adopted for the determination of the PSD.

2.3.1 Specimen preparation

Three specimen preparation procedures were used. The first method consisted in the static
compaction of the soil that was previously air-dried and wetted below optimum moisture
content. The second method was based on the one-dimensional consolidation of a slurry
prepared with the soil previously subjected to spatulation. The third method was the one-
dimensional consolidation of a slurry prepared with the soil previously subjected to
disaggregation in the dispersion cup. The first condition was expected to produce a soil structure
condition that predominantly preserves particle aggregates. The third condition was designed

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to be an extreme disaggregation procedure, was shown by Souza et al. (2020). The second
procedure was expected to offer an intermediate particle disaggregation state. Two void ratios,
of 0.5 and 1.0, were studied for each of the three specimen preparation methods.

Specimens reconstituted by static compaction are obtained in highly controlled procedures


using the Emic DL2000 automated loading frame. The specimens were compacted in the
dimensions required for the tests in a single soil layer and compressed at a constant rate of 1
mm/min. Specimens were reconstituted with a gravimetric water content (w) of 18%,
corresponding to a value less than the optimum soil moisture determined under standard Proctor
optimum conditions.

The procedure of hand mixing by spatulation consisted in the vigorous disintegration of the soil
prepared with a water content slightly above the liquid limit, as described in the following steps:
i) the soil sample was initially dried in an oven at 110 ºC and passed through a 2 mm sieve; ii)
the material with slurry consistency was obtained by mixing soil and deionized water; iii) the
slurry was dispersed through continuous spatulation for 30 minutes; iv) the slurry was
transferred to a consolidation ring; v) one-dimensional saturated consolidation was carried out
up to the desired void ratio, according to D2435 (ASTM, 2011).

The procedure using the dispersion cup was similar to that described using spatulation, with a
few changes in the first steps: i) soil preparation by drying and sieving was done according to
the previous method; ii) deionized water was added to the soil until it was completely
submerged and left for approximately 24 hours; iii) the sample was placed in the standard
dispersion cup, which was activated for 60 minutes in a rotation of 10000 rpm; iv) the mixture
was dried in an oven at 110 ºC and stirred every 10 minutes, until it reached a homogeneous
slurry state; v) the slurry was transferred to the consolidation ring and its one-dimensional
consolidation was performed. The samples were kept saturated throughout the consolidation
process by flooding the consolidation cell with deionized water up to the height of the
specimens. The range of effective consolidation stresses applied to reach e0=0.5 was from 1.8
to 3584.3 kPa for statically compacted samples, from 0.3 to 1998.8 kPa for disaggregated
samples by spatulation, and from 0.7 to 202.0 kPa for the soil diaggregated using the dispersion
cup.

In order to contain the slurryand minimize solids loss, the consolidation ring bottom was sealed
with filter paper and two filter papers were used on the sample surface. This allowed water to

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escape from the specimen during consolidation, while containing solids. For monitoring the
consolidation process, the height of the specimen was initially measured using a Vernier caliper,
and later using the regular extensometer setup. To improve the quality of measurements, the
specimen weight was also recorded several times during consolidation, with specimen height
calculated based on the known mass of solids. Figure 2 illustrates the consolidation steps.

Figure 2 - Procedure for preparing reconstituted specimens from a slurry state: a) side view of the consolidation
cell; b) upper filter paper; c) upper porous stone; d) sample height measurement with Vernier caliper; e)
consolidation press with sample height measurement with extensometer; f) reconstituted sample for
determination of SWCC.

After consolidation, the specimens were taken from the consolidation cell and prepared for
SWCC testing. For the pressure plate test, the samples were taken directly to the equipment,
since the dimensions of the consolidation ring are compatible with the SWCC determination
equipment. For the dew point potentiometer test, subsamples were extracted from the
reconstituted specimen, by using PVC rings with beveled ends. The procedure of extraction of
subsamples was carried out carefully, using steel wire, to avoid disturbing the soil. The
specimens were then packed in plastic film and stored in closed containers to avoid moisture
variation before the SWCC tests.

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2.3.2 Soil-water characteristic curve tests

SWCCs were determined by combining pressure plate and dew point potentiometer methods,
allowing the measurement of the complete suction range. Not all methods used for the
determination of the SWCC are able to cover all suction ranges (MARINHO, 2005). Thus, the
pressure plate test was performed to impose matric suctions from 0 to 300 kPa, and the dew
point potentiometer for determination of total suctions from 300 to 100000 kPa. This range of
potentials is necessary for the complete structural characterization of this soil, as will be shown
later. It is important to note that these two tests produce data in terms of matric and total suction.
The combination of matric and total suction to form the same SWCC may be justified by the
need to combine complementary water retention mechanisms (FREDLUND, M.; FREDLUND,
D.; WILSON, 2002; SCHELLE et al., 2013) and by the fact that osmotic suction (due to the
presence of solutes in the soil-water) is relatively small for the high suction range determined
using the dew point potentiometer (FREDLUND, D.; RAHARDJO; FREDLUND, M., 2012).

The pressure plate test is based on the concept of axis translation (FREDLUND, D.;
RAHARDJO; FREDLUND, M., 2012). This test was performed on SWC-150 device,
developed by GCTS Testing Systems (Tempe, AZ, USA). The reconstituted saturated
specimens were compacted or consolidated in the same consolidation ring used during pressure
plate tests. Specimens were inserted on the pressure plate, put in contact with a saturated high
air-entry value ceramic disk (3 Bar). A token load of 3.7 kPa was applied to the specimen, to
ensure full contact with the ceramic disk. With the chamber closed, air pressure values and the
corresponding matric suctions were applied in stages, doubling the increments until reaching a
maximum matric suction of 300 kPa. The estimated accuracy of suction readings was ±0.05
kPa from 0 to 10 kPa and ±0.5 kPa from 10 to 300 kPa. SWCCs were obtained for three paths,
first drying, wetting and second drying. This was made possible with the use of accumulation
burettes. During the entire process of SWCC determination, the specimen height was measured
using an extensometer installed outside the equipment chamber and connected to the loading
ram. The observed equilibrium time for each applied matric suction step varied between 2 and
8 hours. Finally, after completion of the last matric suction step, the final water content of the
sample was determined, to back-calculate the water content corresponding to each matric
suction step.

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The determinations using the dew point potentiometer were performed in the WP4C Dew Point
PotentiaMeter equipment, developed by Decagon Devices (Pullman, WA, USA). The
measurement technique of this equipment is based on the dew point, which is calculated from
the partial pressure of air vapor in equilibrium with the sample in a closed measuring chamber.
The instrument has with specifications a range of 0 to 300 MPa and an accuracy of ±0.05 MPa
from 0 to 5 MPa and 1% from 5 to 300 MPa. Before performing the tests, the equipment was
calibrated using a standard KCl solution (0.5 mol/Kg). Each subsample was air-dried to a
different total mass, corresponding to various moisture contents. The specimens were carefully
sealed with plastic film and stored, during an equilibration period of 24 hours. Finally, the
samples were placed in the potentiometer and the suction reading of each sample was performed
in two or three steps, until two subsequent readings differed by less than 5%. The equilibrium
time for each determination step was approximately 15 minutes and was minimized by assuring
the soil temperature was lower than the block temperature by no more than 0.3 oC. Additional
determinations were carried out on a wetting path, adding distilled water to the same specimens,
and following a similar procedure.

2.3.3 Modeling the soil-water characteristic curve

The PSDs of the soil corresponding the two reference aggregation states were used for the
prediction of the SWCC of the soil using several PTFs found in the literature. These obtained
results were compared to the SWCCs determined for the soil, also prepared in structural
conditions corresponding to the maximum possible preservation of aggregates and maximum
obtainable disaggregation. These comparisons were designed to allow the evaluation of the role
of soil structure on the modeling of the SWCC.

The prediction models used herein are based on the PSD and other basic physical characteristics
of the soil. The models used in the prediction exercises were presented by Arya and Paris
(1981), Arya and Dierolf (1989), Aubertin et al. (2003), Wang et al. (2017), and Alves, Gitirana
Jr. and Vanapalli (2020). Table 1 presents brief descriptions of each PTF. The models were
implemented in spreadsheets and carefully verified, using predictions available in the original
publications of each model.

To measure the modeling errors, the paired of measured and modeled water contents along the
SWCCs were used for the computation of the coefficient of determination (R²), the sum of

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square errors (SSE), the root-mean-square error (RMSE), and the average relative error (ARE)
for each set of predictions.

3. RESULTS AND DISCUSSION

3.1 EVALUATION OF THE ROLE OF SOIL STRUCTURE IN THE SOIL


COMPRESSIBILITY AND THE SWCC

The consolidation and SWCC data presented herein, corresponding to the behavior of
specimens consolidated from a slurry, was produced during the second stage of a larger
experimental program, devised to study the effects of soil structure on the SWCC. The
complementary data presented for the case of statically compacted specimens was obtained
from Araujo et al. (2020), who reported results from the first stage of this experimental
program.

Figure 3 shows the compression curves of the specimens consolidated from slurry and statically
compacted. There is a clear effect of soil structure and remolding method on the compressibility
of the soil. The soil prepared in the dispersion cup resulting a the destruction of the cemented
bonds and a more disaggregated state, becoming relatively more compressible with a virgin
compressibility index of 0.368. This specimen preparation procedure leads to a normaliy
consolidated condition along the entire compression curve. The compressibility of the
spatulated soil is intermediate, with a virgin compression index of 0.242, but still presenting a
normally consolidated behavior. The statically compacted soil, which should have a maximum
degree of preservation of aggregations and particle bonds, presents a significantly pre-
consolidation stress (about 8 kPa), resulting in a less compressible condition represented by a
recompression index of 0.019 and a virgim compression index of 0.467.

The SWCCs of the specimens prepared under the various structural conditions are presented in
Figure 4. The maximum volume change for the spatulated soil consolidated from a slurry was
equal to 0.9% and 1.0%, for e0 = 0.5 and e0 = 1.0, respectively. In the case of the soil
disaggregated in the dispersion cup and soil consolidated from a slurry state, the maximum
volume change was equal to 3.4% and 2.9%, for e0 = 0.5 and e0 = 1.0, respectively. The volume
change of the statically compacted soil during SWCC determination was negligible. The

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relatively low volume changes, even for the soil prepared under the most disaggregated state,
lead to a maximum change in void ratio of 0.06, therefore presenting relatively low effect on
the degree of saturation.

Figure 3 - Compression curves of the specimens prepared by static compaction and consolidation from slurry
prepared with the soil previously subjected to spatulation and dispersion cup.

2.0
Static compaction
1.8
Spatulation + consolidation from
1.6 slurry
Dispersion cup + consolidation
1.4 from slurry
Void ratio, e

1.2

1.0

0.8

0.6

0.4
0.1 1 10 100 1000 10000 100000
Effective consolidation stress, σ' (kPa)

The SWCC data obtained from the pressure plate and dew point potentiometer are adequately
complementary. The main suction gaps, around 1000 kPa, correspond to flat portions of the
SWCC, before the air-entry value of the micropores. It is also noted that the curves determined
by the dew point potentiometer in drying and wetting paths did not differ significantly,
indicating that hysteresis only occurred for matric suction values below the residual condition
of the macropores, as was also observed by Sun et al. (2016) for another tropical soil. The
wetting curves sometimes did not reach full saturation, and for specimens spatulated and
consolidated from slurry and e0 = 1.0 the maximum degree of saturation reached was 91.6%.
This could indicate the occurrence of occluded air bubbles (MATYAS, 1967). However, the
lower maximum values of degree of saturation for e0 = 1.0 indicate that the pore-size
heterogeneity and the bottle neck effect (FREDLUND, D.; RAHARDJO; FREDLUND, M.,
2012) may be the main factors responsible for the observed hysteresis. Macropores of larger
size may interfere with the maximum degree of saturation after a wetting path.

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Figure 4 - Determined SWCCs for the soil under various structural conditions.

40 40
Static Static
35 35 compaction
compaction
Gravimetric water content (%)

30
e0 = 0.5 30
e0 = 1.0

25 25

20 20

15 15

10 Pressure plate (1ª drying) 10


Pressure plate (wetting)
5 Pressure plate (2ª drying) 5
WP4C
0 0
0.1 1 10 100 1000 10000 100000 0.1 1 10 100 1000 10000 100000
Suction (kPa) Suction (kPa)

40 40
Spatulation and Spatulation and
35 consolidation 35
consolidation
Gravimetric water content (%)

30
from slurry 30 from slurry
e0 = 0.5 e0 = 1.0
25 25

20 20

15 15

10 10

5 5

0 0
0.1 1 10 100 1000 10000 100000 0.1 1 10 100 1000 10000 100000

Suction (kPa) Suction (kPa)

40 40
Dispersion cup Dispersion cup
35 and consolidation 35 and consolidation
Gravimetric water content (%)

from slurry from slurry


30 30
e0 = 0.5 e0 = 1.0
25 25

20 20

15 15
Pressure plate (1ª drying)
10 10 Pressure plate (wetting)
Pressure plate (2ª drying)
5 5 WP4C (drying)
WP4C (wetting)
0 0
0.1 1 10 100 1000 10000 100000 0.1 1 10 100 1000 10000 100000
Suction (kPa) Suction (kPa)

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Figure 5 presents a comparison between the drying SWCCs of the soil under the various
structural conditions, for each analyzed void ratio, in terms of degree of saturation. Degree of
saturation was selected to incorporate the minor effect of volume change. The best fit curves
obtained using the equation proposed by Gitirana Jr. and Fredlund (2004) are also presented.
The air-entry values (ψb1 and ψb2), the residual suctions (ψres1 and ψres2) and the residual
saturation degrees (Sres1 and Sres2) corresponding to the micropores and macropores, and the
degree of saturation for the second air-entry value (Sb) are also presented. The behavior
observed in SWCCs suggests that both macropores and micropores govern the water input and
output of the soil mass (FEUERHARMEL; GEHLING; BICA, 2006; PECAPEDRA et al.,
2017).

In general, the increased disaggregation of the soil obtained with dispersion cup, which was
demonstrated from the comparison of the PSDs, has caused significant modifications in the
retention properties of the soil macro-structure. This can be observed by the increased matric
suctions of the disaggregated soil, when compared to the other specimen preparation conditions.
Significant change was observed in the macropore air-entry value (ψb1) for e0 = 0.5 and in the
residual suction of the macropores (ψres1), for specimens with e0 = 1.0. Negligible change was
observed in the suction required to drain the micropores. Therefore, the variation in the void
ratio during consolidation from slurry and during static compaction, caused significant
variations only in the condition of the macropores. The reduction of the voids ratio caused an
increase in the first air-entry value (ψb1). However, the variation in the voids ratio did not affect
the air-entry value of the micropores (ψb2). This behavior was also observed by Sun et al.
(2016). Note that while the air-entry value of the macropores seem to be closely related to e0,
the slope of the SWCC corresponding to the drainage of the macropores is closely related to
the degree of disaggregation and destruction of bonds. The disaggregated soil presents a more
disperse structure, resulting in a wider PoSD at the macropore level.

When comparing the curves obtained for e0 = 0.5, slight difference was observed between the
SWCCs of the soil physically destructured in the dispersion cup and statically compacted. But
for e0 = 1.0, spatulation produced a soil with a SWCC similar to the statically compacted soil.
This is probably due to the fact that aggregates still remain present in the reconstituted
specimens, as suggested by Delage and Lefebvre (1984). However, physical disaggregation
using the dispersion cup proved to be more efficient for disaggregating the soil and affecting
its macrostructure, as shown by the displacement to the right of the SWCC. These observations

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indicate that the disaggregation using the dispersion cup was more efficient than by spatulation,
as was demonstrated by the analysis of the PSDs (SOUZA et al., 2020).

Figure 5 - Drying SWCCs for different void ratios: a) e0 = 0.5; b) e0 = 1.0.

100
ψb1 = 45.0 kPa a)
90 ψres1 = 170.0 kPa
Sres1 = 69.0 %
80 ψb2 = 5,750 kPa
ψb1 = 19.1 kPa Sb = 66.0 %
Degree of saturation (%)

70 ψres1 = 133.8 kPa ψres2 = 27,888 kPa


Sres1 = 54.9 % Sres2 = 6.6 %
60 ψb2 = 7,611 kPa
Sb = 53.9 %
50 ψres2 = 26,521 kPa
Sres2 = 7.8 %
40
30
20 Static compaction
Spatulation + consolidation from slurry
10 Dispersion cup + consolidation from slurry
Best-fit
0
0.01 0.1 1 10 100 1000 10000 100000 1000000
Suction (kPa)

100
b)
90
ψb1 = 4.43 kPa
80 ψres1 = 1400.00 kPa
Sres1 = 30.00 %
Degree of saturation (%)

70 ψb2 = 3808.47 kPa


ψb1 = 4.06 kPa Sb = 37.18 %
60 ψres1 = 29.50 kPa ψres2 = 23835.44 kPa
Sres1 = 38.77 % Sres2 = 2.99 %
50 ψb2 = 8903.92 kPa
Sb = 31.64 %
40 ψres2 = 16947.02 kPa
Sres2 = 4.56 %
30
20 Static compaction
Spatulation + consolidation from slurry
10 Dispersion cup + consolidation from slurry
Best-fit
0
0.01 0.1 1 10 100 1000 10000 100000 1000000
Suction (kPa)

The influence of tropical soil structure on SWCC was also evaluated in studies by Sun et al.
(2016), who analyzed the microporosity of intact and compacted laterite clays. The authors also
observed that the initial voids ratio only influences the change in the volume of inter-aggregate
pores, while the intra-aggregate pore volume remains almost constant. Therefore, similar to the
behavior found in this study, SWCCs present significant differences only for low suction

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values, when macropore drainage occurs. For high suction values, the SWCCs remain almost
unchanged in relation to the variation of the void ratio and the analyzed disaggregation
condition. Koliji, Vulliet and Laloui (2010) also observed this same behavior for a structured
soil with double porosity.

3.2 INFLUENCE OF PSD AND PoSD IN THE SWCC

The PSD provides information of the dominant sizes of particles present in the soil. While the
cumulative form of the PSD is more commonly used, its frequency form may offer another way
to represent the PSD that can be used for a clearer visualization of the particle size. In order to
facilitate the visualization of cumulative and frequency PSDs, the curves were fitted using the
bimodal equation proposed by M. Fredlund, D. Fredlund and Wilson (2000) and the first
derivative of the equation was obtained for the presentation of the frequency curve. The
obtained results for the various sample preparation conditions are presented in Figure 6. The
bimodal equation was chosen because two distinct groups of soil particles (i.e., similar to a gap-
graded soil) were observed. It is important to note that the derivatives were taken with respect
to the logarithm value of the particle size, corresponding to a logarithmic probability density
function.

It can be observed that the soil samples with a higher degree of aggregation present a PSD that
tends to a unimodal shape, with the range of particle sizes around 0.2 mm. For the soil
disaggregated using the dispersion cup, the PSD has a wider range, with bimodal behavior
characterized by two main particle size classes. The particle size peaks were close to 0.002 and
0.15 mm. The derivative of the PSD is also be useful for the analysis of the corresponding water
storage properties of the families of particle sizes.

Similarly, the first derivation of the SWCC with respect to suction allows the evaluation of the
water storage in the soil. The derivative of the experimental SWCCs, presented in Figure 5, was
accomplished by using the bimodal equation proposed by Gitirana Jr. and Fredlund (2004).
Figure 7 shows that, in all structural conditions analyzed, a bimodal soil-water retention
behavior can be observed. For the soil with e0 = 0.5, it is observed that the different degrees of
aggregation affected only the macropores, represented by the first peak of the curves. The
micropores, represented by the second peaks, remained stable. For the soil at e0 = 1.0, the

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varying degrees of aggregation caused a greater change in soil behavior, significantly changing
both macropores and micropores.

Figure 6 - PSD in cumulative and frequency form: a) aggregated soil; b) disaggregated soil.

2.0 2.0
Cumulative PSD: data a) Cumulative PSD: data b)
1.8 1.8
Cumulative PSD: best fit Cumulative PSD: best fit
1.6 1.6
Frequency PSD Frequency PSD
Relative percentage

1.4 1.4
1.2 1.2
1.0 1.0
0.8 0.8
0.6 0.6
0.4 0.4
0.2 0.2
0.0 0.0
0.0001 0.001 0.01 0.1 1 0.0001 0.001 0.01 0.1 1
Particle size (mm) Particle size (mm)

Figure 7 - Derivative of the SWCC: a) e0 = 0.5; b) e0 = 1.0.

100 100
Static compaction a) Static compaction b)
90 90
Spatulation + Spatulation +
80 consolidation from slurry 80 consolidation from slurry
Water storage (%) - dS/dΨ

70 Dispersion cup + 70 Dispersion cup +


consolidation from slurry consolidation from slurry
60 60

50 50

40 40

30 30

20 20

10 10

0 0
0.1 1 10 100 1000 10000 100000 0.1 1 10 100 1000 10000 100000
Suction (kPa) Suction (kPa)

Thus, it appears evident that the SWCC of the tropical residual soil studies herein is not only
related to the PSD, but also to its structure. Similar findings are presented by Romero, Gens
and Lloret (1999), Marinho (2005), Koliji et al. (2006), and Satyanaga et al. (2013), for other
soil types. It is important to note that the different methodologies used for soil disaggregation
caused structural changes at different levels and revealed the structural effects in the water
retention capacity of the soil studied. In addition, it was also confirmed the presence of two

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families of pores in bimodal soils: microstructure (related to elementary particle associations


within soil aggregates) and macrostructure (related to soil aggregates arrangement).

3.3 THE INFLUENCE OF AGGREGATION ON THE PREDICTION OF


THE SWCC

The SWCCs predicted by the models proposed by Arya and Paris (1981), Arya and Dierolf
(1989), Aubertin et al. (2003), Wang et al. (2017) and Alves, Gitirana Jr. and Vanapalli (2020)
are presented in Figure 8. The PTFs were applied using the PSDs corresponding to the selected
aggregation conditions described previously. These results were compared to the SWCCs
obtained for the soil at varying structural conditions. For the application of the Aubertin et al.
(2003) model, the equations for non-cohesive soils were considered, trying to predict with
greater precision the first part of the SWCC, corresponding to the macropores. The non-
cohesive model considers the coefficient of uniformity, as in the model of Wang et al. (2017).

The values for the empirical parameters α and α* adopted for the models of Arya and Paris
(1981) and Arya and Dierolf (1989) are 1.459 and 1.0 cm, respectively, as suggested by the
original authors. The SWCCs were highly sensitive to these parameters and provided relatively
poor predictions of the experimental curves. This can be justified by the fact that the α and α*
parameters of the models were not empirically developed for tropical residual soils with
bimodal behavior. Since the uncertainty associated with these empirical parameters can be
considered high, further studies should be conducted to improve the performance of these
prediction models, considering the bimodal structure often observed in tropical soils. It is also
important to note that the Wang et al. (2017) model was insensitive to porosity.

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Figure 8 - SWCCs predicted by the model proposed by Arya and Paris (1981), Arya and Dierolf (1989),
Aubertin et al. (2003), Wang et al. (2017) and Alves, Gitirana Jr. and Vanapalli (2020).

100 100
90 Arya and Paris 90 Arya and Paris
(1981) e0 = 0.5 (1981) e0 = 1.0
80 80
70 70
Degree of saturation (%)

60 60
50 50
40 40
30 30
20 20
10 10
0 0
1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6 1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6

100 100
Arya and Arya and
90 90
Dierolf (1989) Dierolf (1989)
80 e0 = 0.5 80 e0 = 1.0
Degree of saturation (%)

70 70
60 60
50 50
40 40
30 30
20 20
10 10
0 0
1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6 1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6

100 100
Aubertin et al. Aubertin et al.
90 90
(2003) e0 = 0.5 (2003) e0 = 1.0
80 80
Degree of saturation (%)

70 70
60 60
50 50
40 40
30 30
20 20
10 10
0 0
1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6 1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6

100 100
Wang et al. Wang et al.
90 90
(2017) e0 = 0.5 (2017) e0 = 1.0
80 80
Degree of saturation (%)

70 70
60 60
50 50
40 40
30 30
20 20
10 10
0 0
1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6 1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6

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100 100
90 Alves, Gitirana 90 Alves, Gitirana
Jr. and Vanapalli Jr. and Vanapalli
80 (2020) e0 = 0.5 80 (2020) e0 = 1.0
Degree of saturation (%)

70 70
60 60
50 50
40 40
30 30
20 20
10 10
0 0
1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6 1E-1 1E+0 1E+1 1E+2 1E+3 1E+4 1E+5 1E+6
Suction (kPa) Suction (kPa)

The performance of the models was also evaluated by comparing the measured and predicted
volumetric water contents for the various structural conditions analyzed. The comparison of
methods is presented in Figure 9. A combination of sample preparation conditions for the
determination of PSDs and SWCCs was proposed for this analysis. The SWCCs predicted by
PTFs for the PSDs determined with samples aggregated were compared with the SWCCs
determined for specimens statically compacted, and the SWCCs predicted for the PSDs
determined with samples disaggregated were compared with the SWCCs determined for
specimens disaggregated in a dispersion cup and consolidated from slurry. When comparing
the predicted and determination SWCCs, it was observed that all models underestimated the
water content, in almost all structural conditions. This was more noticeable for low water
contents and high suctions, similarly to what was observed by Hwang and Powers (2003) and
Chang, Cheng and Qiao (2019). The only exception was for samples aggregated and e0 = 1.0,
in which the models proposed by Arya and Paris (1981) and Arya and Dierolf (1989)
overestimated the volumetric content for low suctions.

In general, prediction methods had superior performance for low suctions, for both aggregated
and disaggregated conditions. In addition, the analyzed PTFs were considerably more accurate
for the higher void ratio, showing that the PSD of the aggregated soil offers a relatively good
representation of the macropore structure. This demonstrates that, while all the prediction
models analyzed were developed for soils with unimodal behavior, the selection of the
representative PSD may allow an improved prediction.

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Figure 9 - Measured and predicted volumetric water content for the same suction values: a) aggregated condition
and e0 = 0.5; b) disaggregated condition and e0 = 0.5; c) aggregated condition and e0 = 1.0; d) disaggregated
and e0 = 1.0.

35 35
Arya and Paris (1981) a) b)
30 30
Predicted water content (%)

Arya and Dierolf (1989)

25 Aubertin et al. (2003) 25

20 Wang et al. (2017) 20


Alves, Gitirana Jr. and
15 15
Vanapalli (2020)
1:1 line
10 10

5 5

0 0
0 5 10 15 20 25 30 35 0 5 10 15 20 25 30 35

50 50
45 c) 45 d)
Predicted water content (%)

40 40
35 35
30 30
25 25
20 20
15 15
10 10
5 5
0 0
0 5 10 15 20 25 30 35 40 45 50 0 5 10 15 20 25 30 35 40 45 50
Measured water content (%) Measured water content (%)

Statistical parameters such as R², SSE, RMSE and ARE were also determined to compare the
performance of the analyzed SWCC prediction models. Table 2 shows the parameters
determined for various combinations of soil preparation for the PSD and SWCC determination.
The R² values were quite scattered, and in many conditions significantly low, indicating that
most PTFs performed poorly. In three cases, R² showed negative values, suggesting that the
regression was worse than the mean of the measured values. The corresponding SSE and RMSE
values were high in most cases, confirming the poor performance of the PTFs. The RMSE
values range from 0.049 to 0.124 for the Arya and Paris (1981) method (mean 0.090), from
0.061 to 0.136 for the Arya and Dierolf (1989) model (mean 0.100), from 0.047 to 0.171 for
the Aubertin et al. method. (2003) (mean 0.114), from 0.116 to 0.203 for the model of Wang et

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al. (2017) (mean 0.148) and from 0.090 to 0.191 for the method of Alves, Gitirana Jr. and
Vanapalli (2020) (mean 0.128). In general, the model proposed by Arya and Paris (1981)
presented the best performance, despite being relatively poor. Furthermore, it is also confirmed
that the analyzed models were not efficient in predicting the bimodal behavior, with high ARE
values well above 20%, as recommended for a good modeling by Guan, Rahardjo and Choon
(2010) and Satyanaga et al. (2013). The lowest values found for this parameter were for
disaggregated samples, mainly with the predictions of PTFs proposed by Arya and Paris (1981),
Arya and Dierolf (1989), Aubertin et al. (2003).

Table 2 - R², SSE and RMSE values of predicted SWCCs using various PTFs.

Alves, Gitirana
Structural Void Arya and Arya and Aubertin et Wang et
Jr. and Vanapalli
condition ratio Paris (1981) Dierolf (1989) al. (2003) al. (2017)
(2020)

Aggregated 0.5 0.312 0.808 - - -
Aggregated 1.0 0.147 0.198 0.601 0.158 0.074
Disaggregated 0.5 0.586 0.445 0.824 0.326 0.153
Disaggregated 1.0 0.912 0.864 0.839 0.511 0.708
SSE
Aggregated 0.5 0.520 0.717 1.143 1.611 1.428
Aggregated 1.0 0.797 0.750 1.497 1.082 0.865
Disaggregated 0.5 0.113 0.151 0.048 0.362 0.231
Disaggregated 1.0 0.061 0.093 0.111 0.337 0.201
RMSE
Aggregated 0.5 0.115 0.136 0.171 0.203 0.191
Aggregated 1.0 0.124 0.120 0.170 0.144 0.129
Disaggregated 0.5 0.072 0.083 0.047 0.128 0.103
Disaggregated 1.0 0.049 0.061 0.067 0.116 0.090
ARE
Aggregated 0.5 0.450 0.501 0.572 0.724 0.678
Aggregated 1.0 0.519 0.530 0.659 0.620 0.566
Disaggregated 0.5 0.343 0.397 0.234 0.691 0.468
Disaggregated 1.0 0.309 0.247 0.289 0.591 0.407

The poor performance of the PTFs may result from the effect of blocked pores and the
simplified representation of the pore system, which may be significantly more complex in
bimodal soils with a double porosity structure (MOHAMMADI; MESKINI-VISHKAEE, 2012;
CHANG; CHENG; QIAO, 2019). Tropical soils often have a hybrid character, as described by
Sharma and Uehara (1968), Tomasella, Hodnett and Rossato (2000) and Sanchez (2019). These
authors have indicated that highly weathered tropical soils exhibit water retention properties

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typical of sands at low suctions and resemble clay at high suctions. Therefore, it became evident
that the semi-empiric and theoretical models available are not able to describe the behavior of
a highly structured soil with the presence of aggregations. Wu (1988) also verified this
limitation in his studies and explained that a single parameter or correction factor would not be
enough to adjust the relationship between particle size and pore size. Therefore, it seems more
reasonable to combine physical and empirical parameters to describe the relationship between
PSD, PoSD and SWCC.

4. CONCLUSIONS

The paper presents an evaluation of the relationship between particle size, pore size and the
influence of aggregations on water retention characteristics in a Brazilian tropical residual soil.
The SWCC of the analyzed tropical soil showed a bimodal shape in several particle aggregation
and corresponding structural conditions. The behavior observed in the SWCCs suggests that
both macropores and micropores govern the water movement of the soil mass. In addition, the
aggregations also presented a significant effect on PoSD and SWCC, suggesting the existence
of a well-developed microstructure in the soil.

However, changes in the structure of the soil caused significant changes only in the macropores,
while the micropores remained practically unchanged. Physical disintegration by dispersion
cup was more efficient than manual disaggregation by spatulation, as evidenced in the
determined PSDs and SWCCs. The disaggregated soil presented a higher retention capacity.
The soil structure obtained by spatulation and static compaction was relatively similar, as
observed by the similar SWCCs. This is an indication of the stability of particle aggregates, that
are not easily destroyed. It was also observed that the higher the void ratio, the greater change
in retention properties caused by the disaggregation of soil macrostructure.

Finally, it was noted that the selected PTFs found in the literature, often employed for SWCC
prediction, underestimated the water content within a relatively high suction range. The errors
may be due to poor conversion of PSD to PoSD and simplifications adopted for the
representation of pore size distribution. The performance of the predictions indicated that the
linear relationship between PSD and PoSD (or between particle volume or pore volume) may

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not be appropriate for an irregular bimodal PSD system, such as that found in a highly
weathered tropical residual soil.

ACKNOWLEDGMENTS

This research project was funded by the Coordenação de Aperfeiçoamento de Pessoal de Nível
Superior - Brasil (CAPES) - Finance Code 001.

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University. Corvallis, Oregon, USA, 1988.
YUAN, Y.; LEE, T. R. Contact angle and wetting properties. Surface science techniques.
Springer, Berlin, Heidelberg, 2013. p. 3-34.
ZHANG, G.; GERMAINE, J. T.; WHITTLE, A. J.; LADD, C. C. Index properties of a highly
weathered old alluvium. Geotechnique, v. 54, n. 7, p. 441-451, 2004. DOI:
10.1680/geot.2004.54.7.441
ZHUANG, J.; JIN, Y.; MIYAZAKI, T. Estimating water retention characteristic from soil
particle-size distribution using a non-similar media concept. Soil Science, v. 166, n. 5, p. 308-
32, 2011. DOI: 10.1097/00010694-200105000-00002

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CONSIDERAÇÕES FINAIS

4.1. CONCLUSÕES

Essa pesquisa apresentou uma extensa investigação experimental sobre a influência da


desagregação na distribuição granulométrica (PSD) e na curva característica solo-água (SWCC)
de alguns solos tropicais residuais. Vários métodos de desagregação química e física foram
avaliados, incluindo diversos agentes dispersantes e desagregação manual, com copo dispersor,
agitador horizontal e ultrassom. Verificou-se que os dispersantes químicos isoladamente não
provocaram desagregação considerável dos solos tropicais analisados, mesmo variando sua
concentração. Assim como o agitador mecânico horizontal por longos períodos.

A maior desintegração de agregações e cimentações desses solos se deu pela combinação de


desagregação química e física. A desagregação realizada com pirofosfato tetrasódico (Na4P2O7)
com concentração de 0.10 mol/L, combinada com rotação em copo dispersor por 60 minutos,
foi considerada a melhor metodologia para desagregação dos solos tropicais analisados. A
dificuldade de desagregar esses solos pode ser associada ao elevado teor de óxidos de ferro e
alumínio nos solos tropicais, que formam microagregados bastante estáveis.

O método proposto para desagregação de solos tropicais foi bastante eficiente e expressivo para
amostras superficiais, e consequentemente, mais intemperizadas. Além disso, uma elevada
variabilidade das PSDs foi observada para as demais amostras retiradas em várias
profundidades de perfis de solos do centro-oeste brasileiro. Além da difícil desagregação, os
solos tropicais se mostraram altamente influenciados pela segregação de partículas, exigindo a
avaliação de métodos ideias de manipulação de amostras. Foi também observado que a secagem
total em estufa à 110 ºC provocou a reagregação quase completa das partículas de solo,
retornando praticamente a sua textura original.

Desta forma, demonstrou-se que a modificação da estrutura do solo devido a desagregação de


partículas tem grande influência no comportamento de solos estruturados. Por isso, avaliou-se
também o efeito da desagregação sobre a capacidade de retenção de água no solo. Amostras

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reconstituídas a partir de estado inicial de lama foram avaliadas após desagregação por
espatulação e por copo dispersor, método semelhante ao que provocou maior desagregação na
PSD. Mesmo com amostras inicialmente próximas ao limite de liquidez, não foram observadas
variações volumétricas significativas durante os ensaios para determinação de SWCC.

As SWCCs determinadas para amostras do solo tropical analisado indicaram que o


comportamento de retenção da água nesses solos é governado pelos macroporos e microporos
e que a desagregação causa aumento na capacidade de retenção de água. A maior desagregação,
obtida com copo dispersor, provocou aumento da retenção de água nos macroporos,
principalmente para amostras mais porosas. No entanto, pouca modificação foi observada nos
microporos do solo. Além disso, a redução do índice de vazios causou aumento no primeiro
valor de entrada de ar das SWCCs, correspondente aos macroporos. Porém, novamente não se
observou modificação no segundo valor de entrada de ar, referente a dessaturação dos
microporos.

Assim, observou-se que a SWCC de solos tropicais não é relacionada apenas à PSD, mas
também à sua estrutura, pois a desagregação desses solos alterou bastante sua capacidade de
retenção. A distribuição de tamanho de poros de solos tropicais influencia diretamente no seu
comportamento hidromecânico. Para avaliar a relação entre tamanho de partículas e tamanho
de poros, foram analisados diversos modelos de previsão de SWCC, considerando PSDs com e
sem desagregação. De forma geral, os modelos avaliados não apresentaram previsão satisfatória
da SWCC para o solo tropical em estudo. Os modelos subestimaram o conteúdo de água em
quase todas as condições estruturais analisadas, principalmente para elevadas sucções. Assim,
os métodos de previsão foram melhores para baixas sucções tanto para amostras agregadas,
quanto desagregadas.

Os modelos de Arya e Paris (1981) e Arya e Dierolf (1989) apresentaram alta sensibilidade aos
seus parâmetros empíricos e não se ajustaram de forma adequada as curvas experimentais, visto
que esses parâmetros foram determinados pelos autores para solos unimodais. Já os modelos de
Aubertin et al. (2003), Wang et al. (2017) e Alves, Gitirana Jr. e Vanapalli (2020) não foram
satisfatórios para previsão da SWCC possivelmente por terem sido desenvolvidos para
materiais granulares e dependerem do coeficiente de uniformidade. Para solos com PSDs
bimodais, esse parâmetro pode não ser adequado para representação completa desses solos,
devido a presença de dois trechos de dessaturação. Por isso, esses modelos foram efetivos

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apenas para previsão do trecho referente aos macroporos da SWCC. A análise estatística dos
modelos de previsão indicou elevada dispersão em relação às SWCCs experimentais e que o
modelo de Arya e Paris (1981) foi o que apresentou melhor concordância entre os resultados.

Portanto, os modelos de previsão da SWCC avaliados não apresentaram bom desempenho na


previsão completa da SWCC do solo bimodal. Isso ocorreu provavelmente devido a
simplificação do arranjo de partículas e distribuição de poros desses modelos, bem como a
presença de dupla porosidade e agregações nos solos tropicais. A complexidade estrutural
desses solos, por causa principalmente da presença de agregações, mostrou ter efeito
significativo na PSD e SWCC de solos tropicais brasileiros.

4.2. RECOMENDAÇÕES PARA PESQUISAS FUTURAS

A partir dos resultados obtidos nesta dissertação, assim como o conhecimento adquirido no
desenvolvimento desta pesquisa, são apresentadas algumas sugestões para pesquisas futuras:

• Avaliar todos os métodos propostos para desagregação química e física para outros solos
tropicais bimodais provenientes de outras regiões brasileiras.
• Estudar mais profundamente a alta variabilidade das PSD determinadas no granulomêtro a
laser.
• Estender a avaliação da influência da desagregação na SWCC para outros solos tropicais.
• Realizar um estudo experimental específico para avaliação da estrutura de amostras
desestruturadas já preparadas nas mesmas condições estudadas, como os ensaios de
microscopia eletrônica de varredura (MEV), difratometria de raios-x (DRX) e porosimetria
por intrusão de mercúrio.
• Avaliar outros modelos para previsão de SWCC para os solos tropicais residuais analisados.

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APÊNDICE A – DESCRIÇÃO DE MODELOS DE PREVISÃO


DA CURVA-CARACTERÍSTICA SOLO ÁGUA

A.1. ARYA E PARIS (1981)

O modelo proposto por Arya e Paris (1981) considera que a PSD pode ser dividida em n frações
arbitrárias. Cada fração apresenta um determinado diâmetro médio de poro e uma respectiva
SWCC idealizada, a qual é definida pelo seu valor de entrada de ar e por uma drenagem total e
abrupta.

Algumas hipóteses são adotadas para simplificação do método, tais como:

• A massa específica do solo é considerada a mesma para todas as n frações. Em outras


palavras, o volume da vazios relativo na fração fina é igual ao da fração grossa.
• As partículas de cada fração são consideradas esféricas e com diâmetro igual ao
diâmetro médio de cada fração.
• O volume e a geometria dos poros de cada fração podem ser idealizados como sendo
um tubo capilar cilíndrico, onde o raio é associado ao raio médio das partículas da fração.
• A equação de capilaridade pode ser aplicada a cada fração.
• E não são considerados o efeito da histerese e seus mecanismos geradores.

O volume dos vazios de cada fração, Vvi , com as frações variando de 1 até n , pode ser

determinado da seguinte forma:

Wsi
Vvi = e (A.1)
s

onde: Wsi é a massa das partículas de cada fração, considerando uma quantidade total de massa

de solo unitária. O valor desta variável é igual à porcentagem gravimétrica de partículas


pertencentes à fração i, obtida através da PSD (Wsi = Pi +1 − Pi ). Além disso, e é o índice de

vazios e  s é a densidade das partículas sólidas.

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Admite-se a hipótese de que os poros são preenchidos de água de forma progressiva em função
do seu tamanho e que a umidade volumétrica do solo, acumulada até a fração n , pode ser obtida
pela Equação A.2:

i Vvj i
vi =  = Vvj d (A.2)
j =1 V j =1

onde: Vvj é o valor obtido pela Equação A.1, V é o volume total de solo da fração

(V = Wsi / d = 1/ d ) e  d é a densidade seca do solo.

Assim, a umidade volumétrica referente ao ponto central de cada fração de solo é dada pela
equação A.3:

( vi +  ( vi +1) )
 *vi = (A.3)
2

Além disso, é necessário determinar a sucção matricial correspondente à cada fração. Para isso,
Arya e Paris (1981) consideram que cada fração de solo é formada por ni partículas esféricas,

resultando em um volume de sólidos, Vsi , e volume de vazios, Vvi , expressos pelas seguintes

equações.

4ni Ri 3 Wsi
Vsi = = (A.4)
3 s

Wsi
Vvi =  ri 2 hi = e (A.5)
s

onde: Ri é o raio médio das partículas de cada fração, ri é o raio médio dos poros de cada fração

e hi é o comprimento total do poro.

Os autores sugerem que se iguale o comprimento total do poro ao número de partículas


alinhadas ao longo do poro, multiplicado pelo comprimento contribuído por cada partícula.
Admitindo-se uma configuração cúbica de esferas idênticas, o comprimento do poro seria
2ni Ri . Os autores sugerem a inclusão de um parâmetro empírico  , para considerar a não

esfericidade das partículas, resultando em 2ni Ri . Os valores de ni podem ser obtidos

J. C. SOUZA Apêndice
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utilizando-se a Equação A.4. Com isso, equiparando as Equações A.4 e A.5, considerando a
parcela 2ni Ri , tem-se:

4eni (1− )
ri = Ri (A.6)
6

Arya e Paris (1981) citam que o valor de  que melhor se ajustou experimentalmente aos solos
analisados por estes autores está entre o intervalo de 1.35 a 1.39. Já Arya et al. (1999) sugere
valores médios estimados para  na ordem de 1.285, 1.459, 1.375, 1.150 e 1.160 para solos do
tipo areia, areia argilosa, solo argiloso, silte argiloso e argila, respectivamente.

Desta forma, o valor de sucção correspondente a cada fração determinada inicialmente é


calculado aplicando-se a equação de capilaridade descrita a seguir:

2Ts
(ua − uw )i = (A.7)
ri

onde: Ts é a tensão superficial da água, correspondente à 7,2×10-5 kN/m.

A.2. ARYA E DIEROLF (1989)

O modelo de previsão desenvolvido por Arya e Dierolf (1989) apresenta uma formulação
alternativa para os raios dos poros proposta por Arya e Paris (1981), acrescentando o parâmetro
 * , representando o comprimento de poro efetivo de cada fração, conforme Equação A.8:

hi = ni * (A.8)

Por meio da combinação das Equações A.4, A.5 e A.8, pode-se obter a seguinte equação:

4 Ri 3e
ri = (A.9)
3 *

Esta equação não tem relação com o número de partículas ni e, por isso, os autores sugerem

que a sensibilidade do modelo que aplica o valor de  * é reduzida quando comparada à


sensibilidade do modelo que aplica a variável  , formulado por Arya e Paris (1981).

J. C. SOUZA Apêndice
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Os valores encontrados pelos autores para o parâmetro  * variam entre 0,3 e 1,5 cm,
representando a faixa molhada e seca das SWCCs de três solos texturalmente diferentes. Os
autores desse método observaram que um valor médio de 0,911 para  * produziu excelente
concordância entre SWCC medidas e previstas para dois solos diferentes. No entanto, a
sensibilidade da SWCC prevista para variações no parâmetro  * , apresentou-se bastante baixa
(ARYA; DIEROLF, 1989).

A.3. M. FREDLUND, D. FREDLUND E WILSON (2002)

M. Fredlund, D. Fredlund e Wilson (2002) apresentaram um modelo para estimar a SWCC a


partir de dados como a PSD e as propriedades massa-volume do solo. O modelo proposto
fornece um método aproximado para estimar a SWCC correspondente a um solo inicialmente
saturado, próximo ao limite de liquidez. No entanto, os efeitos da estrutura do solo, histórico
de tensões, tensão de confinamento e histerese não são abordados pelo modelo.

O método proposto pelos autores apresenta uma nova abordagem para o modelo de previsão
desenvolvido por Arya e Paris (1981). O modelo representa a porosidade do solo através do uso
de um fator de agrupamento para os vários tamanhos de partículas e admite a hipótese de que
para cada grupo uniforme de partícula corresponde a uma SWCC única.

Para representar a curva de PSD são utilizadas as equações de ajuste de distribuição


granulométrica propostas por M. Fredlund, D. Fredlund e Wilson (2000). As equações
unimodal e bimodal, apresentadas nas Equações A.10 e A.11, respectivamente, permitem um
ajuste contínuo da PSD, incluindo as partículas grossas e finas. O ajuste matemático da PSD
fornece a base para estimar a SWCC.

   
7

  ln 1 + d  

r
1    d  
Pp ( d ) = 1 −   (A.10)
 
 
ngr mgr 
   dr   
 a   ln 1 + 
ln exp (1) +        d m   
gr

   d     
  

onde: agr é um parâmetro referente ao ponto de quebra inicial da curva, ngr é um parâmetro

relativo a inclinação da curva, mgr é um parâmetro referente a forma da curva relacionado a

J. C. SOUZA Apêndice
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parte de finos, d r é um parâmetro relacionado a quantidade de finos no solo, d é o diâmetro da

partícula e d m é o diâmetro mínimo da partícula que é permitido.

   
   
   1 
 
w 
nbi mbi
 + (1 − w ) 
    abi      7

  ln  exp (1) +        ln 1 + d rbi  
 d       
    
 d  
Pp ( d ) =   1 −   (A.11)
     ln 1 + d rbi  
       
 
dm  
 1   
  kbi lbi
 
   jbi    
  ln  exp (1) +  d    
     

onde: abi é um parâmetro referente ao ponto de quebra inicial da curva, nbi é um parâmetro

relacionado a inclinação da curva, mbi é um parâmetro relativo a forma da curva, jbi é um

parâmetro referente ao segundo ponto de quebra da curva, kbi é um parâmetro relativo a

segunda inclinação da curva, lbi é um parâmetro relacionado à segunda forma da curva, d rbi é

um parâmetro correspondente a quantidade de finos no solo, d é o diâmetro da partícula, d m é

o diâmetro mínimo da partícula que é permitido e w é um fator de ponderação que indica a


relação do conjunto de amostra que constitui a fração grossa.

O modelo desenvolvido por M. Fredlund, D. Fredlund e Wilson (2002) divide em frações


uniformes a curva de PSD e considera que em cada fração, ao invés de ter uma drenagem
abrupta como era adotado pelo modelo de Arya e Paris (1981), a drenagem ocorre de forma
gradual. Assim, para representar a SWCC de cada fração do solo, o modelo propõe a utilização
da equação de Fredlund e Xing (1994). A Equação A.12 representa o modelo de ajuste proposto
pelos autores.

 
     
 ln 1 +    
hr    
ww = ws 1 − 
 1
(A.12)
 6  
 10    nf

mf

 ln 1 +    ln exp 1 +   


  hr     ( )    
  af   
   

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onde: ws é o teor de umidade gravimétrico saturado, a f é um parâmetro correspondente à

sucção do solo no ponto de inflexão, que está de certa forma relacionado com o valor de entrada
de ar do solo, n f é um parâmetro de ajuste referente à taxa de dessaturação do solo, m f é um

parâmetro relativo à curvatura da faixa de alta sucção do solo, hr é um parâmetro constante

usado para representar a sucção do solo referente ao conteúdo de água residual, proposto pelos
autores como 3000 kPa, e  é a sucção do solo (kPa).

Para determinar o valor de entrada de ar referente à um específico raio de poro médio de uma
fração, os autores consideram como base o modelo capilar, conforme apresentado na Equação
A.13. Por esta equação, a sucção do solo correspondente ao valor de entrada de ar equivalente
para um solo com partículas de tamanho uniforme pode ser definida. Esta sucção pode ser
considerada pelo modelo como equivalente ao parâmetro a f da equação de Fredlund e Xing

(1994).

cos 
 = a f = 2Ts (A.13)
 w gr

onde: Ts é a tensão superficial na água,  é o ângulo de contato,  w é a densidade da água, g

é a aceleração da gravidade, r é o raio do poro e  é a sucção do solo.

O modelo assume que para cada tamanho de partículas, uma SWCC pode ser calculada. Com
isso, é necessário determinar o diâmetro efetivo da partícula para cada curva, conforme
apresentado na Equação A.14:

1 3 g1 i = n g i
= + (A.14)
d e 2 d1 i =2 di

onde: d e é o diâmetro efetivo do grão, d1 é o maior diâmetro da fração grossa do material e

g1 é o peso do material na última fração em termos de peso total.

Para estimar os valores dos parâmetros n f e m f , uma equação com uma forma semelhante à de

van Genuchten (1980) foi ajustada através de dados experimentais, com base no diâmetro
efetivo do tamanho de grão, resultando na Equação A.15.

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p4
 
 
 1 
P ( ) = p1   + p5 (A.15)
   − log ( d e ) −1

p3


 ln 
10
exp (1) +   
   p2   
  

onde: p1 , p2 , p3 , p4 e p5 são parâmetros de ajuste, d e é o diâmetro efetivo e p ( ) é o valor

para n f ou m f . De acordo com os autores, os parâmetros da equação para representar n f são

p1 = 19, p2 = 50, p3 = 30, p4 = 1 e p5 = 1 . Já os parâmetros para representar mf são

p1 = 1.5, p2 = 100, p3 = 10, p4 = 1 e p5 = 0.5 .

O fato de realizar a divisão da PSD em frações, permite maior precisão na estimativa da SWCC
para a distribuição do tamanho dos grãos agrupados. Considera-se que cada porção tem uma
porosidade ou fator de empacotamento ( n p ) e a soma da porosidade de cada fração deve ser

maior que a porosidade natural do solo. O modelo propõe que a soma das SWCC comece pelas
porções do solo com as menores partículas até que a porosidade natural seja alcançada,
negligenciando a influência de partículas maiores. O fator de empacotamento pode ser estimado
por um método estatístico ou utilizando uma rede neural.

A estimativa da SWCC a partir da PSD proposta por M. Fredlund, D. Fredlund e Wilson (2002),
foi implementada pelos autores para vários tipos de solo. O modelo mostrou-se razoavelmente
confiável para areias e siltes, porém apresentou maior dificuldade em estimar a SWCC para
solos argilosos, embora a precisão do modelo ainda fosse razoável para este tipo de solo. Os
resultados apresentados pelos autores se mostraram sensíveis ao fator de empacotamento
assumido para cada tipo de solo.

Contudo, o modelo proposto por M. Fredlund, D. Fredlund e Wilson (2002) apresentou melhor
capacidade de previsão quando comparado com outros modelos, como de Arya e Paris (1981),
Rawls e Brakensiek (1985), Vereecken et al. (1989), Tyler e Wheatcraft (1990) e Scheinost,
Sinowsky e Auerswald (1997).

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A.4. AUBERTIN et al. (2003)

O modelo proposto por Aubertin et al. (2003) é baseado no modelo de Kovács (1981), que foi
modificado e denominado MK (modified Kovács,1981). Este modelo considera que a retenção
de água pelo solo é resultado do efeito combinado de forças capilares e de adesão.

O modelo MK é baseado na ascensão capilar equivalente do meio poroso, hco . Este parâmetro

é fundamental para definir a relação entre o grau de saturação, S r , ou teor de umidade

volumétrica,  , e a sucção matricial,  . O parâmetro hco é derivado da altura hc de água em

um tubo capilar com diâmetro d , sendo seu valor dado por:

4 w cos  w
hc = (A.16)
 wd

onde:  w é a tensão superficial da água,  w é o ângulo de contato da água com a superfície do

tubo (  w = 0 para quartzo e vidro) e  w é o peso específico da água.

A Equação A.16 indica que a ascensão capilar é inversamente proporcional ao diâmetro do


tubo. No entanto, o diâmetro dos poros de solos costuma não ser uniforme, de modo que hc

não seja facilmente definida. Desta forma, o sistema de poros pode ser substituído por um
sistema de canais regulares como um diâmetro equivalente dos poros, deq , definido pela

seguinte Equação:

Vv
d eq = 4 (A.17)
Av

onde: Vv e Av são, respectivamente, o volume e a área superficial dos vazios. Na prática, Av

pode ser aproximada da área dos grãos sólidos, AG , que pode ser correlacionada com a

superfície específica, S m . Assim, a Equação A.17 pode ser transformada em:

e
d eq = 4 (A.18)
 s Sm

onde: e é o índice de vazios e  s é a densidade dos grãos sólidos.

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Com isso, a ascensão capilar equivalente do meio poroso, hco , em um solo pode ser obtida por

meio da substituição da Equação A.18 na A.16 e expressa como:

 w cos  w  s Sm
hco = (A.19)
 we

Para solos de granulação grossa, a superfície específica, S m , pode ser estimada a partir da
distribuição granulométrica, utilizando a seguinte expressão definida por Kovács (1981):


Sm = (A.20)
 s DH

onde:  é um fator de forma definido pelos autores como sendo igual à 10 e DH é o diâmetro
equivalente da partícula para uma mistura heterogênea, que representa teoricamente o diâmetro
de uma mistura homogênea que tem a mesma superfície específica que uma mistura
heterogênea. Assim, a Equação A.19 pode ser reescrita para calcular a ascensão capilar
equivalente em um solo acima do nível freático:

 w cos  w
hco,G = (A.21)
 weDH

O índice G significa ser referente à um material granular. Em solos desse tipo, Sm e DH podem
ser avaliados através da subdivisão da PSD. Para aplicações práticas na geotecnia, o valor de

DH também pode ser aproximado, através da seguinte equação:

DH = [1 + 1,17log(CU )]D10 (A.22)

onde: D10 é o diâmetro correspondente a 10% do material passante na curva de PSD e CU é o

coeficiente de uniformidade (CU = D60 / D10 ).

Portanto, para a ascensão capilar equivalente em solos granulares, a Equação A.21 é expressa
da seguinte forma:

b
hco,G = (A.23)
eD10

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Sendo:

 w cos  w
b= (A.24)
[1 + 1,17 log(CU )] w

No entanto, as equações para solos granulares mencionadas acima não fornecem estimativas

confiáveis para Sm e hco , particularmente quando o limite de liquidez, wL , está entre 30% e 40%

(AUBERTIN et al., 2003). Para solos finos, o valor de Sm pode ser estimado através da relação

entre a superfície específica e wL . Uma relação empírica entre essas variáveis foi proposta por
Mbonimpa et al. (2002), conforme apresentada na equação a seguir:

Sm =  wL  (A.25)

onde:  e  são parâmetros do material. Baseado nos resultados de várias pesquisas, foi

estabelecido que  = 0, 2 m2/g e  = 1, 45 para materiais com 22 m2/g ≤ Sm ≤ 433 m²/g e 18%

≤ wL ≤ 127% (MBONIMPA et al., 2002). Com estes valores, obtém-se:


hco , P = wL1,45 (A.26)
e

O índice P significa tratar-se de um material coesivo. Sendo o parâmetro  definido como:

 w cos  ws
=
w (A.27)

O modelo MK assume que a água é retida no solo por forças capilares, responsáveis pela

saturação capilar, S c , e por forças adesivas, causando a saturação por adesão, S a . A

componente S c é mais importante para valores de sucção relativamente baixos, enquanto o

componente S a se torna dominante para maiores sucções quando a maior parte da água capilar
é retirada. Este modelo propõe que o grau de saturação é definido da seguinte maneira:


Sr = = Sc + S a* (1 − Sc ) (A.28)
n

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onde:  é a umidade volumétrica de água e


*
n é a porosidade. Nesta equação, o valor de Sa é

introduzido no lugar da componente S a utilizada no modelo original desenvolvido por Kovács


*
(1981), para se certificar de que a componente de adesão não exceda a 100%. Assim, Sa é

expresso pela seguinte equação:

Sa* = 1 − 1 − Sa  (A.29)

Sendo Sa = 1 para Sa  1 , e Sa = Sa para Sa  1 .


* *

As contribuições das componentes capilares e de adesão para o grau de saturação são definidas

como funções de hco e  , usando as Equações A.30 e A.31.

hco 2 m h
Sc = 1 − [( ) + 1] exp[− m( co ) 2 ] (A.30)
 

(hco /  n ) 2/3
Sa = acC (A.31)
e1/3 ( /  n )1/6

A Equação A.30 avalia S c no intervalo de 0 ≤ S c ≤ 1, que é um limite proposto por Kovács


(1981), em que a função estatística exponencial foi expandida para refletir melhor a influência
do tamanho do diâmetro dos poros através do parâmetro de distribuição m . O parâmetro m
influência no valor de entrada de ar, ou seja, o valor que teoricamente corresponde à sucção
quando no maior diâmetro do poro começa acontecer a drenagem.

A Equação A.31 também é baseada em Kovács (1981). Nesta equação ac é o coeficiente de

aderência e  n é um parâmetro de normalização, considerado igual à 1 cm quando  também

é dado em cm. O parâmetro C é um fator de correção em função da sucção, quando ocorre


teor de umidade residual. O teor de umidade tende a zero quando  atinge um limite imposto

pelo equilíbrio termodinâmico (  = 0 para  =  o = 107 cm de água, correspondendo


aproximadamente a secagem total). O parâmetro C é definido pela seguinte equação:

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ln(1 + /  r )
C = 1 − (A.32)
ln(1 + o /  r )

Na Equação A.32,  r representa a sucção residual referente ao teor de umidade residual. O


valor de  r pode ser calculado para solos granulares e coesivos de acordo com a formulação a

seguir:

0, 42
r = (A.33)
(eDH )1,26

Baseado na Equação A.23, os autores desenvolveram uma relação entre  r e a ascensão capilar

equivalente hco,G para materiais granulares, como definido na Equação A.34:

 r = 0,86hco ,G1,2 (A.34)

Infelizmente a Equação A.34 não é aplicável para materiais finos, pois muitas vezes os

parâmetros D10 e CU são desconhecidos. A determinação direta de  r , assim, torna-se difícil

para esse tipo de solo. As aplicações do modelo MK presumem que os valores  r para o solos

com granulação fina pode estar relacionado a hco, P , utilizando a mesma correlação para os solos

granulares. Assim, a expressão usada para solos coesivos torna-se:


 r = 0,86( )1,2 wL1,74 (A.35)
e

Uma vez determinado  r para cada tipo de material, Aubertin et al. (2003) avaliaram os valores

dos parâmetros m e ac para efetuar procedimentos de ajustes com os dados experimentais.


Para solos granulares, o valor do parâmetro m encontrado pelos autores foi bem aproximado

do inverso do coeficiente de uniformidade (m = 1/ CU ) e o valor de ac pode ser considerado


constante, sendo igual à 0,01. Enquanto que para solos coesivos, os autores afirmam que ambos

os valores de m e ac podem ser tomados como constantes na previsão das aplicações, sendo
−4
m = 3 10−5 e ac = 7 10 .

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A.5. ALVES, GITIRANA JR. E VANAPALLI (2020)

Alves, Gitirana Jr. e Vanapalli (2020) apresentaram um modelo de previsão teórico da SWCC
com uma nova abordagem, substituindo parâmetros empíricos frequentemente introduzidos por
outros modelos, por uma análise tridimensional aproximada da geometria dos poros usando o
conceito de células unitárias. A célula unitária idealizada pelos autores é considerada formada
pela conexão dos centros de oito partículas esféricas parciais.

O modelo apresenta uma análise de escala de poros, isto é, uma escala microscópica relevante
na qual as partículas e poros podem ser observados e medidos. A modelagem em escala de
poros é uma forma de melhorar a representação física dos poros e da água no poro. Com isso,
o modelo desenvolvido pelos autores apresenta alguns avanços na incorporação da modelagem
de escala de poros em modelos de previsão de SWCC, assim como também abordado por Likos
e Jaafar (2013).

O modelo desenvolvido por Alves, Gitirana Jr. e Vanapalli (2020) é avaliado considerando
materiais ideais compostos de partículas quase esféricas de vidro uniformes, graduados e
considerando solos naturais de textura grossa, como areias. A célula unitária considerada na
modelagem foi aumentada para solos não uniformes usando a PSD. Assim, uma análise de
sensibilidade do modelo de célula unitária proposto é apresentada pelos autores, oferecendo
uma visão sobre os mecanismos de retenção considerados. O modelo avalia o efeito de dois
mecanismos de retenção capilar de água, a água pendular e funicular.

Semelhante a metodologia proposta por M. Fredlund, D. Fredlund e Wilson (2002), os autores


partem da divisão da PSD em frações pequenas e a determinação do ajuste da granulometria
pela equação proposta por M. Fredlund, D. Fredlund e Wilson (2000). A porosidade ( n. ) de
cada fração de célula unitária é determinada pela Equação A.36, desenvolvida por Mayer e
Stowe (1965), em função do ângulo de empacotamento (  ).


n = 1− (1 − 3cos 2  + 2 cos3  ) −1/ 2 (A.36)
6

O volume de vazios ( Vv ) de uma célula unitária pode ser calculado pela Equação A.37.

Vv = 8nR3 (1 − cos  ) 1 + 2cos  (A.37)

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Outra característica importante da célula unitária considerada pelos autores é o número de


esferas vizinhas que cada esfera individual toca, denominado como número de coordenação

(nc ) . O modelo propõe a utilização da Equação A.38, determinada de forma empírica por
Haughey e Beveridge (1969) em função da porosidade.

10.73
nc = 26.49 − (A.38)
1− n

O modelo considera que é formado um anel pendular de água entre duas partículas esféricas de
mesmo raio e o ângulo de enchimento (  ), que é definido como uma medida da quantidade de

água pendular armazenada na célula unitária. Assim, o volume de um anel pendular ( V p ) pode

ser determinado pela Equação A.39.

 2    sin  1 − cos      
Vp = 2 R3 (1 − cos  ) 1 + cot  sin  + cot  1 − cos  −  +     (A.39)
     cos  sin   cos    

onde:  =  / 2 –  − 

Já para considerar a água funicular, o modelo supõe que esta é completamente drenada quando
a sucção matricial atinge um valor crítico que corresponde à curvatura da maior esfera

circunscrita dentro do poro da célula unitária. O raio da esfera circunscrita ( Raev ) pode ser
calculado pela Equação A.40.

Raev = R  4sin 2 ( 2) + 1 − 1 (A.40)


 

Desta forma, a sucção matricial correspondente ao valor de entrada de ar (AEV) pode ser obtida
usando a equação de Young-Laplace.

2Ts
(ua − uw ) aev = cos  (A.41)
Raev

Com isso, a SWCC completa de uma célula unitária é então obtida pela combinação dos efeitos
pendular e funicular, calculando para cada fração, o volume cumulativo de água para cada
incremento de sucção matricial. As SWCCs de cada fração são então somadas, conforme
proposto inicialmente por M. Fredlund, D. Fredlund e Wilson (2002).

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Para verificar o modelo desenvolvido por Alves, Gitirana Jr. e Vanapalli (2020), SWCC
experimentais altamente controladas foram determinadas em esferas de vidro. O modelo
apresentou resultados razoáveis para curvas de secagem. No entanto, a modelagem de curvas
de molhagem utilizando ângulos de contato específicos indicou a necessidade de considerar
mecanismos de histerese adicionais, pois frequentemente o modelo produziu sucções matriciais
levemente subestimadas, assim como para a maioria das areias testadas. Com isso, os autores
propõem um fator de correção com base no coeficiente de uniformidade.

No entanto, ao comparar a abordagem proposta com outros modelos de previsão, como de Arya
e Paris (1981), Arya e Dierolf (1989), M. Fredlund, D. Fredlund e Wilson (2002) e Aubertin et
al. (2003), o método proposto exibiu desempenho superior. Mas todos os modelos testados, de
uma forma geral, apresentaram baixo desempenho na previsão da zona residual para os
materiais testados.

Além disso, o modelo proposto por Alves, Gitirana Jr. e Vanapalli (2020) foi capaz de prever
razoavelmente bem a forma da SWCC e suas principais características, como a valor de entrada
de ar e a inclinação da zona de transição. Com isso, a modelagem da SWCC baseada na escala
dos poros provou ser uma abordagem válida e viável.

J. C. SOUZA Apêndice

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