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CIVE 4753 / 5753

Engineering Soil Stabilization

Fall 2022
Week 10: Lecture 5

Monday, October 17, 2022


Chemical Stabilization
Chemical Stabilization
• The state of the practice relative to selecting a stabilizer
and determining the optimum additive content based on
– Soil properties
– Chemical additives
– Chemical treatment basics
– Modification versus stabilization
– Improvements in treated soil behavior
– Relevant documents and standards.
• Basic soil-additive chemical interactions:
– Cation exchange
– Flocculation/agglomeration
– Pozzolanic reactions
– Cementation
– Carbonation.
Lime
Lime Stabilization
•QUICKLIME (Calcium Oxide) is produced by
calcining high quality limestone at elevated
temperature, volatilizing nearly half of the stone’s
weight in Carbon Dioxide.
•HYDRATED LIME (Calcium Hydroxide) is produced
by reacting the quicklime with sufficient water to
form a white powder.
Lime Stabilization

•The cemented products are


–calcium-silicate-hydrates
–calcium-aluminate-hydrates
•These are essentially the same hydrates that
form during the hydration of Portland cement
Clay – Lime Reactions
• A soil-lime-water system has a pH high enough to solubilize
silica and alumina for pozzolanic reaction.
• As long as enough residual calcium remains in the system
to combine with the clay-silica and clay-alumina and as
long as the pH remains high enough to maintain solubility,
the pozzolanic reaction will continue.

Ca++ + OH- + Soluble Clay Silica  Calcium-Silicate-


Hydrate (CSH)

Ca++ + OH- + Soluble Clay Alumina  Calcium-Aluminate-


Hydrate (CAH)
Chemical Stabilization

•Determination of the additive content of


compacted soils in the field
–Qualitative methods – pH based
–Quantitative lab methods
–X-ray fluorescence (XRF)
Chemical Stabilization

•Common chemical additives


–Cementitious
• Lime
• Cement
• Fly ash
• Cement kiln dust
Chemical Stabilization
• Chemical compositions (most components)
Item (%) Lime Class C Class F Portland CKD 1 CKD 2 CKD 3
Fly Ash Fly Ash Cement
SiO2 <1 40 55 23 12 15 16

Al2O3 <1 17 26 4 5 4 4

Fe2O3 <1 6 7 2 2 2 2

CaO 95 24 9 64 42 45 53

MgO 2 5 2 2 1 1 2

SO3 - 3 1 2 7 3 6

K2O - - - - 2 2 4

LOI - <5 <5 - 24 28 18


Chemical Stabilization
•Cation exchange
–Ca2+ released from additive in presence H2O
–Ca2+ adsorbed by soil particle diffuse double layer
• Exchanges with lower valence cations (e.g., Na+)
• Reduce soil particle electrical potential
Chemical Stabilization
• Flocculation/Agglomeration
Add
chemical

Dispersed Structure

Flocculated/Agglomerated Add water


Structure

Mix

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Chemical Stabilization
•Pozzolanic reaction products

Untreated shale Shale w/lime – 28 days


•Cementing-type materials
• Calcium-silicate-hydrates, CSHs
• Calcium-aluminate-hydrates, CAHs
Chemical Stabilization
• Electron microscopy

Untreated shale Shale w/lime – 28 days

•Cementation

Shale w/CKD – 28 days


Chemical Stabilization
•Carbonation
–Reaction of calcium-based products with carbon
dioxide in atmosphere producing calcium carbonate
–Undesirable reaction that retards development of
CSHs and CAHs

–Proper storage and handling important!


Chemical Stabilization
•Factors that adversely influence soil-chemical
reactions:
–Organic carbon content of soil
–Excessive quantities of exchangeable sodium
–Presence of carbonates and phosphates in soil
–Presence of sulfates in soil
Chemical Stabilization

•ODOT definitions (2009 standard specifications)


–Chapter 300 subgrade treatment, section 307.01
• A. Subgrade stabilization
– Incorporate chemical additives into the subgrade to increase the
strength of the subgrade soils and to provide structural value for
the pavement structure.
• B. Subgrade modification
– Incorporate chemical additives into the subgrade to change the PI
of the subgrade soils and improve its workability as a platform to
support construction equipment.
Chemical Stabilization
•ODOT 2009 standard specifications
–Section 307 subgrade treatment
• General construction requirements
• Material requirements found in section 700
• Application requirements
• Temperature restrictions
• Mixing requirements
• Compaction requirements
Chemical Stabilization
•ODOT OHD L-49, L-50, and L-51
–OHD L-49 Test for Determining Soluble Sulfate
Content in Soil
–OHD L-50 Soil Stabilization Mix Design Procedure
–OHD L-51 Soil Modification Mix Design Procedure
Chemical Stabilization
• ODOT OHD L-50 Soil Stabilization Mix Design Procedure
–Abbreviated procedure: uses basic soil tests and soil
stabilization table
–Complete laboratory procedure:
• ASTM D6276 Standard Test Method for Using pH to Estimate the
Soil-Lime Proportion Requirement for Soil Stabilization
– Additive content for stabilization is the lowest lime percentage that gives
pH = 12.4.
• ASTM D4609 Standard Guide for Evaluating Effectiveness of
Admixtures for Soil Stabilization
– Test treated samples with different additive contents to determine UCS
– Uses Harvard Miniature samples
– Test UCS samples immersed in water for 2 days
– Effective stabilization increases UCS by 50 psi or more
– Other indicators; PI reduction, swell reduction, etc.
• Other required tests
– Soluble sulfate (OHD L-49) for all soils – thresholds 500, 1000, 8000 ppm
– Crumb test (ASTM D6572) for dispersive soil – Divisions 2, 5, 7 or if
dispersive soils suspected
Chemical Stabilization
•ODOT OHD L-50
Chemical Stabilization
•ODOT OHD L-51
Chemical Stabilization
•Adverse reactions and unexpected outcomes
from chemical stabilization
–Sulfate bearing soil
–Post-construction wetting
–Laboratory versus field testing
Chemical Stabilization
• Sulfate rich soils
–Soils containing soluble sulfate that reacts with chemical
soil additives containing calcium (i.e., lime, fly ash, CKD)
resulting in precipitation of calcium sulfate crystals (e.g.,
ettringite, thaumasite)
Major problem is volume increase (and heave)
associated with growth of calcium sulfate
crystals.

Gypsum
crystals
Chemical Stabilization
• Sulfate heaving problem (shortly after construction)

25
Chemical Stabilization
•Forensic investigation

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Chemical Stabilization
•Forensic investigation

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Chemical Stabilization
•Forensic investigation

28
Chemical Stabilization
•Forensic investigation

29
Chemical Stabilization
•Forensic investigation

30
Chemical Stabilization
•Forensic investigation

31
Chemical Stabilization
•Sulfate rich soils (cont’d)
–Occurrence:
• Soils / formations containing soluble sulfate minerals (e.g.,
gypsum)
–Identification:
• Visual inspection and geological investigation
• Chemical analysis for soluble sulfates (e.g., ODOT OHD L-49,
National Lime Association)
–Treatment:
• Do not use lime if soil contains appreciable soluble sulfate
content (threshold is uncertain – typically 1000 to 3000
ppm)
• Conduct compatibility tests if in doubt
Chemical Stabilization
•Post-Construction Wetting
–The DCP and LWD tests showed similar trends at most
field test sites and captured the increase in strength
and stiffness of stabilized subgrade soils with
increasing curing time.
–The test results also reflected a decrease in strength
and stiffness at some sites due to significant rain
events during curing.
–Field test results also reflected the variability of
strength and stiffness at test sites. Thus, the field tests
in question show significant promise as tools for
monitoring quality and improvement of stabilized
subgrades during construction.
Chemical Stabilization
• Laboratory versus Field Testing
–The UCS and MR values obtained from the laboratory
mixed and cured samples were compared to results of
DCP and LWD field tests for ten sites (five previous, five
current).
–It was found that there was little or no correlation
between the field and laboratory strength and stiffness.
–This was attributed to the significant differences in the
curing conditions (i.e., weather) that played a significant
role in the results of field tests.
–When data from two sites, that were significantly
different, were removed from the data set, a weak
correlation was observed between MR and field test
results for the remaining eight sites.
Chemical Stabilization
•ODOT 2009 standard specifications, 307.04 I:
–After completing the final grade, use a color-sensitive
indicator solution, such as phenolphthalein or thymol
blue, to measure the thickness and uniformity of the
compacted soil and chemical mixture in accordance
with subsection 301.04.A(2), “Width and Thickness.”
–Apply the indicator solution along the side of a small
hole excavated to the required depth of chemical
treatment and note the depth and uniformity of the
color change.
Chemical Stabilization

•ASTM D3155 standard test method for lime


content of uncured soil – lime mixtures:
–Must be uncured specimens – not applicable for
forensic investigations.
–Titration process, cumbersome, lots of chemicals,
operator dependent.
–Only for lime.
Chemical Stabilization
• There is need for a versatile and reliable method for
measuring stabilizer content in the field for any
additive type and at any time after mixing!
• Construction quality control
–Can inspect stabilized subgrade and make a determination
if enough stabilizer has been used and have any issues
fixed before the pavement is laid.
• Forensic geotechnical investigations
–Inspectors can collect samples during construction and
keep them in case a roadway performs poorly in the
future
–Samples can be obtained during failure investigations –
less accurate than banking samples during construction
Mix Design
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• The use of lime to dry, modify, and stabilize soil is a well-
established construction technique.
• A variety of mixture design procedures have evolved, as
various agencies have developed criteria and procedures to
fit their specific design needs and objectives, often reflecting
local conditions and experience.
–Both for
• Short-term: drying-modifying
– Decrease in water content
Lab tests
– Reduction in PI
– Etc.
• Long-term: strength-durability
– Cyclic freezing & thawing
– Soaking Lab tests
– 28-day strength measurement
– Etc.
Mixture Design and Testing Procedures for Lime
Stabilized Soils

• Evaluate soil to gain a general understanding of its


suitability for lime stabilization.
• Determine minimum amount of lime required for
stabilization.
• Evaluate lime-stabilized soil strength for long-term
durability within its exposure environment, with
special attention to cyclic freezing and thawing and
periods of extending soaking.
• If soils to be stabilized are expansive, evaluate using
capillary soaking and expansion measurements.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
•Step 1: Initial Soil Evaluation
– Evaluate key soil characteristics as an initial step to
determine if it is suitable for lime stabilization.
– Use ASTM C136 procedures to determine the amount
of soi passing the 75 micron (75 µm) sieve size and
ASTM D4318 (wet method) to determine the soil
plasticity index (PI).
– Generally, soil with at least 25% passing a 75 µm
screen and having a PI of 10 or greater are candidates
for lime stabilization.
• Some soils with lower PI can be successfully stabilized with
lime, provided the pH and strength criteria are satisfied.
Mixture Design and Testing Procedures for Lime
Stabilized Soils

•Step 1: Initial Soil Evaluation


– Soil with organics content above 1-2% by weight as
determined by ASTM D2974 may be incapable of
achieving the desired unconfined compressive
strength for lime stabilized soil.
– Soils containing soluble sulfates greater than 0.3%
(3,000 ppm) can be successfully stabilized with lime,
but may require special precautions.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
•Step 2: Determine the Approximate Lime Demand.
–Determine the minimum amount of lime required for
stabilization.
–Use ASTM D6276 procedures (known as the “Eades-
Grim” test).
–The lowest percentage of lime in soil that produces a
laboratory pH of 12.4 (flat section of the pH vs. lime
percentage curve produced by the test) is the minimum
lime percentage for stabilizing the soil.
–Note that lime can react with moisture and carbon
dioxide.
• Careful storage is required to maintain lime’s integrity and
produce reliable results.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• Step 3: Determine Optimum Moisture Content and
Maximum Dry Density of the Lime-Treated Soil.
–Determine optimum moisture content (OMC) and maximum
dry density (MDD) of the soil after lime has been added.
• This is necessary because adding lime will change the soil’s OMC
and MDD.
–Make a mixture of soil, lime, and water at the minimum
percentage of lime as determined from Step 2 (Eades-Grim
test), using a water content of OMC + 2-3%.
–Seal the mixture in an airtight, moisture proof bag stored at
room temperature for 1-24 hours.
–Determine the OMC and MDD of the mixture using ASTM
D698 procedures (standard compaction effort).
–Note: when using quicklime, the mixture should be stored
for 20-24 hours to ensure hydration.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• Step 4: Prepare Unconfined Compressive Strength
(UCS) Specimens
– Using ASTM D5102 procedure B, prepare a minimum of
two test specimens of lime, soil and water using the
amount (percentage) of lime determined from Step 2 at
the OMC (±1%) as determined from Step 3.
– The soil-lime-water mixture should be stored in an
airtight, water-proof bag for 1-24 hours prior to preparing
the test specimens.
– When using quicklime, the mixture should be stored for
20-24 hours to ensure hydration.
– Additional specimens may be prepared if additional
testing is desired.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• Step 5: Cure and Condition the Unconfined
Compressive Strength (UCS) Specimens
– Approximate, in an accelerated manner, field curing and
moisture conditions.
– Immediately following the preparation of the test
specimens, wrap the specimens in plastic wrap and seal
in an airtight, moisture-proof bag.
– Cure the specimens for 7 days at 40oC.
– Subject the specimens to a 24-hour capillary soak prior to
testing.
– The capillary soaking process should be done by removing
the specimens from the airtight bag, then removing the
plastic wrapping.
Mixture Design and Testing Procedures for Lime
Stabilized Soils

•Step 5: Cure and Condition the Unconfined


Compressive Strength (UCS) Specimens
– The specimens are wrapped with wet adsorptive
fabric and placed on a porous stone.
– The water level should reach the top of the stone
and be in contact with the fabric wrap throughout
the capillary soak process, but the specimens should
not come directly in contact with the water.
– A minimum of two cured and moisture conditioned
specimens for UCS testing.
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• Step 6: Determine the Unconfined Compressive Strength
(UCS) of the Cured and Moisture Conditioned Specimens
– To determine the UCS of the lime-stabilized soil to ensure
adequate field performance in a cyclic freezing and thawing
and extended soaking environment
– Use ASTM D5102 procedure B to determine the UCS of the
cured and moisture conditioned specimens
– The UCS is the average of the test results for at least two
specimens
– The minimum desired UCS depends on the intended use of the
soil, the amount of cover material over the stabilized soil,
exposure to soaking conditions, and the expected number of
freezing and thawing cycles during the first winter of exposure
– Suggested minimum UCS are shown in the following table:
• Unconfined Compressive Strength (UCS) Values:
Mixture Design and Testing Procedures for Lime
Stabilized Soils
• Step 7: Determine the Change in Expansion Characteristics
[only for expansive soils]
– To evaluate the expansiveness of lime stabilized soils.
– Note the vertical and circumferential dimensions of the
samples prepared in Step 5 prior to performing the capillary
soak.
– After soaking, perform new measurements using a caliper for
the vertical dimension and a tape for the circumference.
– Calculate the volume change between the initial and the
soaked condition.
– Three-dimensional expansion of between 1 and 2% is
commonly regarded as acceptable.
– If the expansion exceeds the design parameter, prepare
additional samples increasing the lime content by 1 and 2%
and repeat the test.
Sulfate Effect
Effect of Sulfates on Lime – Soil Interactions
•Sulfate rich soils.
Effect of Sulfates on Lime – Soil Interactions

•Soluble sulfates present a concern when


stabilizing the soil with any calcium-based
stabilizer.
– Soluble sulfates in high enough concentrations can
interfere with pozzolanic reactions.
– Can produce a reaction product that consists of
calcium, alumina, water, and sulfate.
•The reason that the calcium-sulfate-aluminate-
hydrates are harmful is because of the expansion
that results from their formation.
Effect of Sulfates on Lime – Soil Interactions

•This expansion can occur with a high potential


pressure (approximately 240 MPa (35,000 psi)
within the crystal).
•This is different from the traditional pozzolanic
reaction products such as calcium-silicate-
hydrates (CSH) and calcium-aluminate-hydrates
(CAH).
•Calcium-sulfate-alumina-hydrate is not a problem
if it forms prior to compaction of the soil.
Effect of Sulfates on Lime – Soil Interactions

•When it forms after compaction or even after the


roadway has been placed in service, the resulting
heave can be very destructive.
•If the soils are rich in soluble sulfates, the calcium
in the lime can react with the sulfates to produce
– Ettringite, and/or
– Thaumasite
•These minerals (ettringite and/or thaumasite) can
undergo significant expansion, causing severe
damage to structures and pavements.
Effect of Sulfates on Lime – Soil Interactions
Effect of Sulfates on Lime – Soil Interactions

•Sulfate-resisting cements like ASTM Type II, Type


V, or other special class cements have been
successfully used in concrete to reduce the effects
of sulfate attack.
•The resistance of these cements to sulfate attack
is attributed to their low C3A content.
•In clay stabilization, however, “sulfate-resisting”
cements are useless in reducing sulfate attack
since most of the aluminates necessary for the
formation of ettringite are provided by the clay in
a high pH environment.
Effect of Sulfates on Lime – Soil Interactions

•The factors that affect the chemical reactions that


result in the formation of the ettringite are
known to be the amount of soluble sulfates in the
soil, the amount of calcium hydroxide, aluminates
and water, and the soil pH.
•In order to control the lime-induced heave, at
least one of these factors would have to be
controlled.
Effect of Sulfates on Lime – Soil Interactions

•Soluble sulfates may be found in very high


concentrations in soils and groundwater
– Including magnesium, sodium, potassium, and
calcium sulfate (gypsum)
•The distribution of soluble sulfates in the ground
is not necessarily uniform. Rainfall or
groundwater can dissolve the sulfates and
transport them to lower-lying areas.
Effect of Sulfates on Lime – Soil Interactions

•Sulfate rich soils can usually be distinguished


visually due to their translucent colorless/white
crystals visible in the walls of fresh excavations.
•Sulfate concentrations in the soil are typically
expressed as parts per million (ppm), which is
equivalent to milligram per liter of solution.
Effect of Sulfates on Lime – Soil Interactions

•Ettringite is a highly expansive mineral that forms


when soluble sulfates react with calcium
hydroxide, aluminum, and water.

𝐶𝐶𝐶𝐶6 𝐴𝐴𝐴𝐴 𝑂𝑂𝑂𝑂 6 2 𝑆𝑆𝑆𝑆4 3 26𝐻𝐻2 𝑂𝑂

•This mineral can expand to a volume equal to


227% of the volume of reactant solids.
Effect of Sulfates on Lime – Soil Interactions

•The supply of sufficient sulfate and carbonate


ions at high humidity and temperatures between
4.5 and 15oC lead to the transformation of
ettringite to thaumasite.
•Thaumasite:

𝐶𝐶𝐶𝐶6 𝑆𝑆𝑆𝑆 𝑂𝑂𝑂𝑂 6 2 𝑆𝑆𝑆𝑆4 𝐶𝐶𝐶𝐶3 2 26𝐻𝐻2 𝑂𝑂


Effect of Sulfates on Lime – Soil Interactions

•The long term pozzolanic reactions are also


affected by the formation of ettringite since the
amount of hydroxyls in the system declines
resulting in the loss of the high pH environment
optimal for the production of calcium-silicate-
hydrates (CSH)
Effect of Sulfates on Lime – Soil Interactions

•The current methodology to identify risk of


sulfate-induced damage is based on the
concentration of available (usually water soluble)
sulfates in the soil.
•Many cases are documented in the literature
where soils with varying levels of sulfate, from
above 1,000 ppm to 10,000 ppm, form ettringite
when treated with calcium-based stabilizers.
Effect of Sulfates on Lime – Soil Interactions

•Perhaps the most practical construction-based


approach in controlling or limiting deleterious
reaction effects when treating high sulfate
content soils with calcium-based stabilizers is to
create conditions in the soil system that favor the
dissolution of available sulfates and force the
formation of these expansive minerals before
compaction.
Effect of Sulfates on Lime – Soil Interactions

•The effectiveness of this method depends


primarily on the possible extent of dissolution of
naturally available sulfates in the soil system.
•Typically, an additional 3 to 5% above optimum
moisture content is added to soils during the
mellowing period.
•Mellowing periods have been specified, which
range from as little as 24 hours to as long as 7
days, primarily depending on soluble sulfate
content in the soils.
Soils Containing Sulfates
•For lime stabilization of clay soils containing
soluble sulfates
– It is critical to perform a thorough investigation of the
site where sulfates have been identified so that a
program can be developed to produce a strong,
stabilized structural layer that will perform as
expected for its entire design life.
Soils Containing Sulfates

•Any additional testing and analysis that is


required can easily be justified considering the
enormous expense of alternatives to lime
stabilization which commonly include removal
and replacement of the expansive clays or full-
depth paving with an unnecessary thick asphalt
or concrete pavement section.
Soils Containing Sulfates

• Four components responsible for sulfate-induced


distress in stabilized soils:
– Calcium, aluminum, water, and sulfates
• Together in the right combination these
components will produce:
– Calcium-aluminate-sulfate-hydrate minerals with very
large expansion potential, high swelling pressures
• The formation of ettringite and/or thaumasite
minerals can be prevented by interrupting the
supply of any of the four components: calcium,
aluminum, water, or sulfate.
Soils Containing Sulfates

•There is no easy answer to the problem:


– Calcium is present when either lime or Portland
cement is used for soil stabilization.
– Soils containing clay are rich with aluminum, a
basic structural unit of clay.
– Water is necessary for compaction and for
stabilization reactions and is present within
pavement structures during their service life.
– Unfortunately, the sulfates usually cannot be
efficiently or economically removed from the soil.
Soils Containing Sulfates

• Presently, the best approach when dealing with


lime stabilization of clay with a significant soluble
sulfate content is to force the formation of the
deleterious minerals prior to compaction.
– If these minerals form during the mellowing period
before placement and compaction, no damage will be
done to the pavement.
– Fortunately, the expansive minerals do form relatively
rapidly as long as the sulfates are soluble, the
aluminum is released from the clay and adequate
water is available for the formation of the minerals.
Soils Containing Sulfates

•Adequate mellowing time may (practically) be


as little as 24 hours or as much as 7 days,
depending on the level of soluble sulfates in
the soil.
•Adequate amount of water is typically 3 to 5
percentage points above the optimum needed
to achieve maximum density during
compaction.
•Water is the most important component of the
equation.
Soils Containing Sulfates

•The worst scenario would be to compact a


lime-treated and sulfate-bearing clay with too
little water.
– This is especially a problem if quicklime is used.
– Use of lime slurry is always recommended in
stabilization of sulfate-bearing clays.
• Lime slurry provides the abundance of water and
uniformity of hydration required to lower the risk.

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