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Engineered Water Repellency in Frost Heave Mitigation Micheal Uduebor 1 , Emmanuel Adeyanju 1 , Mohammad Wasif Naqvi 2 , Md Fyaz Sadiq 2 1 University of North Carolina at Charlotte, Charlotte, NC, USA, 2 Michigan State University, Michigan, MI, USA Advisors: Dr. John Daniels, D.Eng., P.E., F.ASCE, Bora Cetin, Ph.D., M.ASCE Introduction/Background Cold weather and frost action have a major effect on the design, construction, performance, and maintenance of roadways. The presence of Frost Susceptible Soils (FSS) coupled with freezing temperatures and the availability of a water source provide suitable conditions for frost action (Heaving and thawing). Frost action causes changes in moisture content, stress, and strain leading to substantial damage to road pavements (Figure 1a-c). National recurrent annual maintenance costs are estimated at over 2 billion dollars annually (FHWA, 1999). This excludes other economic impacts because of related vehicle damage, road closures, and weight restrictions. Remedial techniques utilized so far (Stripping and replacement, thermo- siphoning, soil stabilization or increasing pavement thickness) are generally cost prohibitive or unfeasible. Engineered Water Repellency (EWR) is an innovative approach that improves the properties of FSS by making it hydrophobic. This involves the treatment of soil with organo-silanes(OS) to form a water repellent coating. This treatment is cost-effective and can be used in various applications to limit the transport of water through these soils, therefore, the process of frost heaving can be mitigated. Figure 1a-c: Road Damage due to Frost action (Heaving and Thawing) Objectives As part of a larger research effort (Figure 2), this study will focus on these objectives To carry out treatment of Frost Susceptible Soils (FSS) and determine the optimal dosage concentrations of selected organo-silane polymers. To determine the degree of hydrophobicity imparted to treated samples using the sessile drop method (Contact Angle Tests, Water Drop Penetration Time Test) To assess the performance of the treated samples using breakthrough and frost heave tests. Figure 2: Research Project Task Flow Study Areas/Materials The soils were collected from Asheville (NC-AS) and Boone (NC-BO) in North Carolina, Pottawattamie County (IA-PC) in Iowa, Anchorage (AK-AC) in Alaska, and Hanover (NH-HS) in New Hampshire (Figure 3a). These areas have different climatic conditions and are subjected to different magnitude of freezing index. All the index properties of soils were determined by following proper ASTM methods (ASTM D854-14, ASTM D6913-17, ASTM D7928-21e1, ASTM D4318-17, ASTM D698-12, ASTM D5918-13e1) (Figure 3b). All soils met the criteria for frost susceptibility based on the classification by the U.S. Army Corps of Engineers (1965) with large amounts of silt and clay. Figure 3a-c: US Map Showing the Soil Recovery Locations; Grain Size Distribution Curve of Selected Samples; Soil Samples Recovered Methodology Organosilane Selection & Material Treatment While a number of products abound to impart hydrophobic properties to materials, three Organosilane chemicals were selected for this study (SIL-ACT ATS-100 (Advanced Chemical Technologies), DOWSIL IE6683 (Dow Chemicals), Terrasil (Zydex Industries) Soils were treated at varying ratios (OS to soil, batched by weight) and mixed with water at a ratio of 1:1 for water soluble OS in a HDPE bottle on a laboratory tumbler for 24 hours. The resulting mixture was placed in cans and separate samples were either air dried or oven dried at 60 o C. Treated samples should possess contact angles >90 o (hydrophobic). Contact angles >150 o are considered super- hydrophobic. Contact Angle Test Water Drop Penetration Time Test Three drops of deionized water (Figure 5a) were placed on the surface of 20g treated and untreated samples in cans with a burette and the time taken for complete penetration of the droplets recorded (Figure 5b). The various time measurements where correlated into varying degree of hydrophobicity by using repellency categories. Breakthrough Pressure Test Frost Heave Test A monolayer of treated soil samples was placed on a double sided adhesive tape attached to a glass slide placed on a goniometer (Figure 4a). Drops of deionized water was placed on the surface of the specimen and contact angle measurements taken using the attached digital microscope and accompanying software (Figure 4b-c). The frost heave testing of soil specimens was conducted as per ASTM D5918. The soil specimens were compacted at MDD and the setup placed into a chest freezer after saturation for 24 hours. A temperature gradient was created using top and bottom plates (Maximum at -12 o C and 12 o C respectively) and temperature readings obtained throughout the specimen (Figure 11b). Heave was monitored with a laser displacement transducer. Two freeze thaw cycles were carried out for a duration of 120 hours continuously being fed from a Mariotte water supply. Treated and untreated samples compacted at maximum dry density were setup in a triaxial cell similar to the saturated hydraulic conductivity test (ASTM D5084) (Figure 6a) DI water was supplied at a rate of 2.286kPa/s using a FlowTrac II setup from Geocomp. The pressure response at the interface of the treated sample and porous stone was logged using a pressure transducer attached to the inflow valve. The breakthrough pressure is indicated by a sudden rise in slope of the pressure-time series plot due to the resistance developed at the interface Figure 4a-c: Goniometer Setup; Water Droplet on Soil Surface; Droplet Imaging for Contact Angle Measurements Figure 6a-c: Breakthrough Pressure Test Setup; Close up on FlowTrac II and Test Cell; Real-time Graph Plot on Computer Screen. Figure 5a-b: Close up of water droplets on treated soil surface; Arrangement of test setup 0 1000 2000 3000 4000 WDPT (s) Mix Ratio (OS:Soil ) g/g NC-B0 AK-AC IA-PC Results Frost Heave Tests Breakthrough Pressure Test Results Water Drop Penetration Test Results 0 1000 2000 3000 4000 WDPT (s) Mix Ratio (OS:Soil ) g/g NC-B0 AK-AC IA-PC 0 1000 2000 3000 4000 WDPT (s) Mix Ratio (OS:Soil ) g/g NC-B0 AK-AC IA-PC 0 20 40 60 80 100 120 140 160 1:1 1:6 1:12 1:24 1:50 1:100 Contact Angle (o) Mix Ratio (OS:Soil ) g/g NC-B0 AK-AC IA-PC Hydrophobic 0.00 1.00 2.00 3.00 4.00 5.00 0. 20. 40. 60. 80. 100. 120. 140. 0.00 100.00 200.00 300.00 dP/dT, kPa/s P. kPa T, sec P dP/dT Figure 8: Contact Angle of Treated Samples (a) ATS-100; (b) IE668; (c) Terrasil Figure 9: Penetration Test Times of Treated Samples (a) ATS-100; (b) IE668; (c) Terrasil Figure 10a-b: Typical Breakthrough Pressure Plot; Comparison between Breakthrough Pressure of Treated and Untreated Samples Figure 11a-d (L-R): Frost Heave Measurements for Selected Soils; Temperature Profile & Water Intake Measurements During Frost Heave Testing; Bottom: Comparison of Frost Heave Results of Untreated and Treated Samples 0 10 20 30 40 50 NC-BO IA-PC NH-HS Breakthrough Pressure (kPa) Soil Untreated Treated Figure 7a-c: Schematic Diagram showing Frost Heave Test Setup; Frost Heave Setup in Chest Freezer Contact Angle Test Results Discussion/Conclusions REFERENCES FHWA. A Quarter Century of Geotechnical Research, Chapter 4: Soil and Rock Behavior. McLean VA, USA 1999 ACKNOWLEDGEMENTS This research was sponsored by the National Science Foundation (Award #1928813) with counterpart Funding from the Iowa Highway Research Board. North Carolina Soil Sampling: Lance Byrd, P.E., Assistant District Engineer, N. Wilkesboro District Office Jeff Winkler, Project Engineer R-2915C (U.S. 221) Jim Holloway, Head Inspector RESEARCH PROJECT WEBSITE https://coefs.uncc.edu/jodaniel/engineered-water-repellency-for-frost-susceptibility/ All organo-silane products imparted hydrophobicity (contact angle > 90 o ) to the soil samples at ratio of 1:10 ( OS:Soil, batched by weight). The degree of hydrophobicity varied with decrease in concentration. Soils tested with Terrasil where hydrophobic even at small concentrations (1:1000) (Figure 8a-c). Results from WDPT correlated with those from the contact angle testing (Figure 9a-c). Treated samples with ATS-100 and Terrasil became extremely water repellent. Breakthrough Pressure required was higher in treated samples. It will take a higher pressure head/suction to transport water through the engineered barrier (Figure 10b). This is The amount of frost heaving in treated samples was reduced, indicative of a mitigation of frost action within the soils. Parametric studies still being carried out will identify the optimal concentrations for each of the soil samples. Engineered Water Repellency will be a cost-effective method for mitigation of frost heave. This innovative solution can also be usefulness in stabilizing expansive soils that experience swelling and shrinkage as well as in other applications requiring containment. Further studies on the relative Influence of matric and osmotic suction In the transport of moisture aiding frost action as well as numerical modelling is being carried out.

Introduction/Background Objectives Study Areas/Materials

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Engineered Water Repellency in Frost Heave MitigationMicheal Uduebor1, Emmanuel Adeyanju1, Mohammad Wasif Naqvi2, Md Fyaz Sadiq2

1 University of North Carolina at Charlotte, Charlotte, NC, USA, 2 Michigan State University, Michigan, MI, USA

Advisors: Dr. John Daniels, D.Eng., P.E., F.ASCE, Bora Cetin, Ph.D., M.ASCE

Introduction/Background

• Cold weather and frost action have a major effect on the design,construction, performance, and maintenance of roadways.

• The presence of Frost Susceptible Soils (FSS) coupled with freezingtemperatures and the availability of a water source provide suitableconditions for frost action (Heaving and thawing).

• Frost action causes changes in moisture content, stress, and strain leadingto substantial damage to road pavements (Figure 1a-c).

• National recurrent annual maintenance costs are estimated at over 2 billiondollars annually (FHWA, 1999). This excludes other economic impactsbecause of related vehicle damage, road closures, and weight restrictions.

• Remedial techniques utilized so far (Stripping and replacement, thermo-siphoning, soil stabilization or increasing pavement thickness) are generallycost prohibitive or unfeasible.

• Engineered Water Repellency (EWR) is an innovative approach thatimproves the properties of FSS by making it hydrophobic. This involves thetreatment of soil with organo-silanes(OS) to form a water repellent coating.

• This treatment is cost-effective and can be used in various applications tolimit the transport of water through these soils, therefore, the process offrost heaving can be mitigated.

Figure 1a-c: Road Damage due to Frost action (Heaving and Thawing)

Objectives

• As part of a larger research effort (Figure 2), thisstudy will focus on these objectives• To carry out treatment of Frost Susceptible

Soils (FSS) and determine the optimal dosageconcentrations of selected organo-silanepolymers.

• To determine the degree of hydrophobicityimparted to treated samples using the sessiledrop method (Contact Angle Tests, WaterDrop Penetration Time Test)

• To assess the performance of the treatedsamples using breakthrough and frost heavetests.

Figure 2: Research Project Task Flow

Study Areas/Materials• The soils were collected from Asheville (NC-AS) and

Boone (NC-BO) in North Carolina, PottawattamieCounty (IA-PC) in Iowa, Anchorage (AK-AC) in Alaska,and Hanover (NH-HS) in New Hampshire (Figure 3a).

• These areas have different climatic conditions and aresubjected to different magnitude of freezing index.

• All the index properties of soils were determined byfollowing proper ASTM methods (ASTM D854-14,ASTM D6913-17, ASTM D7928-21e1, ASTM D4318-17,ASTM D698-12, ASTM D5918-13e1) (Figure 3b).

• All soils met the criteria for frost susceptibility basedon the classification by the U.S. Army Corps ofEngineers (1965) with large amounts of silt and clay.

Figure 3a-c: US Map Showing the Soil Recovery Locations; Grain SizeDistribution Curve of Selected Samples; Soil Samples Recovered

Methodology

Organosilane Selection & Material Treatment

• While a number of products abound to impart hydrophobicproperties to materials, three Organosilane chemicals wereselected for this study (SIL-ACT ATS-100 (Advanced ChemicalTechnologies), DOWSIL IE6683 (Dow Chemicals), Terrasil(Zydex Industries)

• Soils were treated at varying ratios (OS to soil, batched byweight) and mixed with water at a ratio of 1:1 for watersoluble OS in a HDPE bottle on a laboratory tumbler for 24hours.

• The resulting mixture was placed in cans and separatesamples were either air dried or oven dried at 60oC.

• Treated samples should possess contact angles >90o

(hydrophobic). Contact angles >150o are considered super-hydrophobic.

Contact Angle Test Water Drop Penetration Time Test

• Three drops of deionized water (Figure 5a) were placedon the surface of 20g treated and untreated samples incans with a burette and the time taken for completepenetration of the droplets recorded (Figure 5b).

• The various time measurements where correlated intovarying degree of hydrophobicity by using repellencycategories.

Breakthrough Pressure Test Frost Heave Test

• A monolayer of treated soil sampleswas placed on a double sidedadhesive tape attached to a glass slideplaced on a goniometer (Figure 4a).

• Drops of deionized water was placedon the surface of the specimen andcontact angle measurements takenusing the attached digital microscopeand accompanying software (Figure4b-c).

• The frost heave testing of soil specimens was conducted as perASTM D5918. The soil specimens were compacted at MDD andthe setup placed into a chest freezer after saturation for 24 hours.

• A temperature gradient was created using top and bottom plates(Maximum at -12oC and 12oC respectively) and temperaturereadings obtained throughout the specimen (Figure 11b).

• Heave was monitored with a laser displacement transducer.• Two freeze thaw cycles were carried out for a duration of 120

hours continuously being fed from a Mariotte water supply.

• Treated and untreated samples compacted at maximum dry densitywere setup in a triaxial cell similar to the saturated hydraulicconductivity test (ASTM D5084) (Figure 6a)

• DI water was supplied at a rate of 2.286kPa/s using a FlowTrac II setupfrom Geocomp. The pressure response at the interface of the treatedsample and porous stone was logged using a pressure transducerattached to the inflow valve.

• The breakthrough pressure is indicated by a sudden rise in slope of thepressure-time series plot due to the resistance developed at theinterface

Figure 4a-c: Goniometer Setup; Water Droplet on Soil Surface; Droplet Imaging for Contact Angle

Measurements

Figure 6a-c: Breakthrough Pressure Test Setup; Close up on FlowTrac II and Test Cell; Real-time Graph Plot on Computer Screen.

Figure 5a-b: Close up of water droplets on treated soil surface; Arrangement of test setup

0

1000

2000

3000

4000

WD

PT

(s)

Mix Ratio (OS:Soil ) g/g

NC-B0

AK-AC

IA-PC

Results

• Frost Heave Tests• Breakthrough Pressure Test Results

• Water Drop Penetration Test Results

0

1000

2000

3000

4000

WD

PT

(s)

Mix Ratio (OS:Soil ) g/g

NC-B0

AK-AC

IA-PC

0

1000

2000

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WD

PT

(s)

Mix Ratio (OS:Soil ) g/g

NC-B0

AK-AC

IA-PC

0

20

40

60

80

100

120

140

160

1:11:61:121:241:501:100

Co

nta

ct A

ng

le (

o)

Mix Ratio (OS:Soil ) g/g

NC-B0

AK-AC

IA-PC

Hydrophobic

0.00

1.00

2.00

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4.00

5.00

0.

20.

40.

60.

80.

100.

120.

140.

0.00 100.00 200.00 300.00

dP

/dT, kP

a/s

P. kP

a

T, sec

P

dP/dT

Figure 8: Contact Angle of Treated Samples (a) ATS-100; (b) IE668; (c) Terrasil

Figure 9: Penetration Test Times of Treated Samples (a) ATS-100; (b) IE668; (c) Terrasil

Figure 10a-b: Typical Breakthrough Pressure Plot; Comparison between Breakthrough Pressure of Treated

and Untreated Samples

Figure 11a-d (L-R): Frost Heave Measurements for Selected Soils; Temperature Profile & Water Intake Measurements During Frost Heave Testing;

Bottom: Comparison of Frost Heave Results of Untreated and Treated Samples

0

10

20

30

40

50

NC-BO IA-PC NH-HS

Bre

akth

rough

Pre

ssure

(kP

a)

Soil

Untreated Treated

Figure 7a-c: Schematic Diagram showing Frost Heave Test Setup; Frost Heave Setup in Chest Freezer

• Contact Angle Test Results

Discussion/Conclusions

REFERENCESFHWA. A Quarter Century of Geotechnical Research, Chapter 4: Soil and Rock Behavior. McLean VA, USA 1999ACKNOWLEDGEMENTSThis research was sponsored by the National Science Foundation (Award #1928813) with counterpart Funding from the Iowa Highway Research Board.North Carolina Soil Sampling:Lance Byrd, P.E., Assistant District Engineer, N. Wilkesboro District OfficeJeff Winkler, Project Engineer R-2915C (U.S. 221)Jim Holloway, Head InspectorRESEARCH PROJECT WEBSITEhttps://coefs.uncc.edu/jodaniel/engineered-water-repellency-for-frost-susceptibility/

• All organo-silane products imparted hydrophobicity (contact angle > 90o) to the soil samples atratio of 1:10 ( OS:Soil, batched by weight). The degree of hydrophobicity varied with decreasein concentration. Soils tested with Terrasil where hydrophobic even at small concentrations(1:1000) (Figure 8a-c).

• Results from WDPT correlated with those from the contact angle testing (Figure 9a-c). Treatedsamples with ATS-100 and Terrasil became extremely water repellent.

• Breakthrough Pressure required was higher in treated samples. It will take a higher pressurehead/suction to transport water through the engineered barrier (Figure 10b). This is

• The amount of frost heaving in treated samples was reduced, indicative of a mitigation of frostaction within the soils. Parametric studies still being carried out will identify the optimalconcentrations for each of the soil samples.

• Engineered Water Repellency will be a cost-effective method for mitigation of frost heave. Thisinnovative solution can also be usefulness in stabilizing expansive soils that experienceswelling and shrinkage as well as in other applications requiring containment.

• Further studies on the relative Influence of matric and osmotic suction In the transport ofmoisture aiding frost action as well as numerical modelling is being carried out.