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CGJ-2019-0047R1

Effect of Texturing on the Longevity of HDPE Geomembranes in Municipal

Solid Waste Landfills


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M.S. Morsy1 and R. Kerry Rowe2*


Abstract
The effect of texturing (co-extrusion using blowing agent) on the longevity of a geomembrane (GMB)

when immersed in synthetic municipal solid waste leachate is investigated over a ~ 3-year period. Based

on data at four temperatures (40, 55, 75, and 85oC), the time to antioxidant depletion of the textured

portion of a 1.5 mm core thickness high density polyethylene (HDPE) GMB is 40% (Std-OIT) and 9%

(HP-OIT) faster compared to the 1.5 mm smooth edge of the GMB. However, despite this, stress crack

resistance results show that texturing may have no significant effect on the time to nominal failure for this

GMB. It is also shown that HDPE GMBs made from nominally the same resin but from different

production lots have different rate of SCR degradation and hence time to nominal failure; this should be

considered both in landfill design and landfill construction quality assurance.

Keywords: Geosynthetics; Textured; Geomembrane; MSW landfills; Antioxidant depletion; Stress crack

resistance; Degradation; Failure; Physical ageing.

*Corresponding author
1 PhD. Student, GeoEngineering Centre at Queen’s-RMC, Queen’s University, Kingston ON, Canada,

K7L 3N6. Email: m.morsy@queensu.ca


2 Professor and Canada Research Chair in Geotechnical and Geoenvironmental Engineering,

GeoEngineering Centre at Queen’s-RMC, Queen’s University, Ellis Hall, Kingston ON, Canada K7L

3N6. E-mail: kerry.rowe@queensu.ca, Phone: (613) 533-3113. Fax: (613) 533-2128.

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1 Introduction
The long-term efficacy of the barrier system is crucial to environmental protection offered by modern

engineered municipal solid waste (MSW) landfills (Rowe et al. 2004; Rowe 2016; Touze-Foltz et al.

2016; Rowe 2018). Most modern (since ~ 1990-1999) landfill base liners are comprised of a single
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composite liner system (Rowe 2005) comprised, from top to bottom, of (Rowe et al. 2004; Rowe 2005):

waste; leachate collection system; geosynthetic or soil protection layer; geomembrane (GMB); and a

geosynthetic clay liner (GCL) and/or compacted clay liner (CCL) over a soil attenuation layer.

The stability of a landfill composite liner is affected by the interface shear strength between

different components (Jones and Dixon 2005). A higher interface friction angle between landfill’s

composite liner components is required to construct the steepest safe side slopes to maximize the

landfill’s waste capacity (Lydick and Zagorski 1991). Texturing of GMB’s surface increases the interface

shear strength between a GMB and soil/ geosynthetic liner in contact (Koerner 2005; Müller 2007;

Scheirs 2009). Texturing can be performed for one side or both sides of a GMB, and it has advantages in

both liner construction and as the landfill is filled with waste. In construction, the texturing provides more

interaction between GMB and materials in contact such as a GCL or geotextile (GTX), less risk of

workers falling, and increases veneer stability of the lining system on side slopes. In service, textured

GMBs are used on slopes to increase the factor of safety against sliding of barrier systems downslope.

Most, but not all, textured GMB’s rolls have a major textured portion and a narrow (150-200 mm) smooth

edge for welding.

There are four techniques for texturing the surface of a GMB: (i) lamination, (ii) impingement,

(iii) structuring, and (iv) co-extrusion using blowing agent (Stark et al. 1996; Hebeler et al. 2005; Müller

2007; Scheirs 2009). Now rarely used, lamination involves laminating a polyethylene (PE) layer with a

foaming agent over a base smooth sheet (Stark et al. 1996). In the impingement method, hot granulated

PE is sprayed on a base smooth polymer sheet creating a textured layer (Stark et al. 1996; Scheirs 2009).

The impingement texturing technique creates smaller and shorter asperities that result in less GMB

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surface’s friction compared to other texturing techniques (Erickson et al. 2008). In the structuring

technique, the surface of a smooth sheet made by flat die method is impressed by two counter patterned

rollers creating a structured pattern on the GMB’s surface; the GMB produced has uniform core thickness

and asperity height and hence this texturing technique is reported to have limited effect on the tensile
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strength and elongation (Scheirs 2009). The technique most widely used (Scheirs 2009) in North America

and Asia, and the one examined in this paper, involves co-extrusion using an inert gas (e.g., nitrogen)

which does not react chemically with the polyethylene. With this texturing technique polymer is fed to

three co-extrusion dies, then nitrogen is injected to one (single textured) or both (double textured) outer

polymer layers. On extrusion from the die, the nitrogen gas bubbles cool down and rupture forming the

textured surface (Erickson et al. 2008; Scheirs 2009). The disadvantages of a textured GMB produced by

this technique are: (a) variable asperity height, (b) variable core thickness, and (c) reduction in

mechanical properties (Ivy 2003; Scheirs 2009). However, a textured GMB produced by this technique is

reported to have a higher shear strength at low normal stress levels compared to a structured textured

GMB (Erickson et al. 2008).

Key factors affecting the interface shear friction between a GMB and adjacent material are: (i)

normal stress, (ii) asperity height, and (iii) characteristics of the material in contact with the GMB (e.g.,

shape of the soil particles, type of geotextile /GCL/geocomposite). For instance, increasing the asperity

height is reported to increase the interface shear strength between the GMB and material in contact, but

also decreases the uniaxial and multiaxial tensile break strength and elongation (Ivy 2003).

Oxidative degradation results in the reduction of the mechanical properties of PE GMBs used as

base liners (Hsuan et al. 2008; Scheirs 2009). The oxidative degradation, traditionally, occurs in three

successive stages (Hsuan and Koerner 1998). Stage I ends at the full depletion of antioxidants. Stage II is

an induction period at which oxidation reactions occur without noticeable reduction in the engineering

properties of the GMB. Stage III starts when there is a detectable reduction in the engineering properties

and ends when a GMB reaches nominal failure defined as when a property of interest is degraded to an

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arbitrary value assumed as 50% of the initial value (Hsuan and Koerner 1998) or 50% of the GRI-GM13

specified value (Rowe et al. 2009).

The effect of texturing on the interface shear has been investigated in different studies (Stark et
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al. 1996; Erickson et al. 2008; Hillman and Stark 2001; Thiel 2001; Fox and Stark 2015), however except

for Yoo et al. (2010), there are no published studies of the effect of texturing on the GMB longevity. Yoo

et al. (2010) immersed a 2.5 mm impingement textured and smooth HDPE GMBs in waste landfill

leachates of pH 4, 7, and 8 at temperatures of 20, 40, 60, and 80oC for four months and indicated that no

difference was observed between the degradation of the tensile properties of the textured and smooth

GMBs. While an interesting finding, four-months immersion, even at 80oC, is not long enough to evaluate

the effect of texturing on the longevity of a GMB. Thus, there is a paucity of data addressing the

longevity of a textured GMB and so the primary objective of this study is to investigate the performance

of an HDPE textured GMB and its smooth edge immersed in simulated municipal solid waste (MSW)

leachate for about 3 years to explore the effect of blown film co-extrusion texturing on its longevity. A

secondary objective is to investigate how a smooth GMB with nominally the same resin/antioxidant

package performed relative to the smooth edge of a textured GMB to assess the representativeness of

using ageing data from a smooth GMB roll as an analog for the performance to the textured roll with the

same nominal resin.

2 Method and materials

2.1 The Tested Geomembrane


The textured and smooth black high density polyethylene (HDPE) GMBs investigated (Table 1) were

manufactured in 2015 using nominally the same medium density polyethylene resin (Chevron Marlex PE

K306). The double sided textured GMB (denoted generically as MxTA15) was produced by co-extrusion

with a blowing agent and had an average core thickness of 1.5 mm and an average asperity height of 0.43

mm, while the thickness of both the smooth edge of the textured GMB (denoted generically as MxTsA15)

and the smooth GMB (denoted generically as MxF15) was 1.5 mm.
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2.2 Accelerated ageing and incubation fluid


Longevity of the GMBs was investigated by accelerating ageing by immersing GMB coupons (19 × 9.5

cm) in 4-liter glass jars filled with simulated MSW Leachate. The jars were placed in forced air ovens at

temperatures of 40, 55, 75, and 85oC (with maximum variation of ±0.5oC). The MSW leachate used,
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denoted Leachate 3 (TDS~12000 mg/L; pH~7; Rowe et al. 2008) was distilled water mixed with

inorganic/organic salts, surfactants, reducing agent, and traced metal solution to simulate the Keele Valley

landfill MSW leachate (Rowe et al. 2008). The GMB coupons were separated by 5 mm glass rods to

ensure exposure of GMB to the MSW Leachate from both sides.

2.3 Index testing


Differential scanning calorimetry (DSC) was used to detect the initial oxidative induction time (OIT) and

to monitor the depletion of antioxidants in terms of Standard OIT (Std-OIT 200oC/ 35 kPa; ASTM 2007a)

and high pressure OIT (HP-OIT 150oC/ 3500 kPa; ASTM 2006). The average initial Std-OIT and HP-OIT

for the textured GMB and its smooth edge were the same (Table 1) but they were not equal to the initial

Std-OIT and HP-OIT of the smooth GMB suggesting that the smooth GMB, although supplied as

nominally equivalent, had different amount of antioxidants.

The melt flow index test (MFI 190oC/21.6 kg; ASTM 2013) was used to monitor changes in the

molecular weight distribution of the PE and to infer the type of oxidation reactions (i.e., cross linking or

chain scission). The tensile test (ASTM 2004) was performed to estimate the break tensile strength and

elongation at different incubation times. To reduce the amount of aged material tested, the tensile test was

performed according to ASTM (2004) but using the smaller Type V dog bone specimens (instead of Type

IV commonly used in quality control and assurance testing) at displacement rate of 50 mm/minute.

The notched constant tensile test (NCTL; ASTM 2007b) was used to estimate the stress crack

resistance (SCR) of both the “equivalent” smooth GMB and both portions of the textured GMB. A

dumbbell shaped specimen was notched using a sharp razor leaving a ligament thickness equal to 80% of

the average nominal thickness of the specimen (i.e., 1.2 mm for 1.5 mm GMB). Afterwards, the notched
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specimen was incubated in an environmental reagent (10% IGEPAL CO-630 surfactant and 90% distilled

water) at 50oC at an axial static tensile load that would apply a stress equal to 30% of the initial (i.e.,

unaged) yield strength of the GMB.


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Although GRI-GM13 (2016) indicated that NCTL test cannot be performed for textured GMBs, it

was performed in this study to compare the degradation trend of the textured GMB with its smooth edge,

to deduce the effect of texturing on the time to nominal failure (tNF), and to assess the physical ageing of

the GMB. The major problem of performing NCTL for textured GMBs was the non-uniform core

thickness that resulted in variations in the ligament thickness of the notched specimens. To address this

issue, the notching machine was adjusted to notch leaving a ligament thickness of 1.2 mm (80% of the

average nominal thickness). To obtain the initial SCR, a large number of specimens were prepared and

the ligament thickness was checked; only those specimens with 1.2 mm ligament thickness were tested.

This same rigorous criterion was not always possible for aged specimens due to their limited number. For

the aged textured GMB specimens, the ligament thicknesses were checked in each case and a specimen

rejected if the thickness varied from the desired value by more than 0.05 mm (4%). To address these

variations in ligament thickness for aged specimens, the applied test load was adjusted to ensure a stress

equivalent to 30% of the initial yield strength of the textured GMB was applied to all specimens based on

the minimum thickness. However, thickness was not uniform across the textured specimens and hence

neither was stress; this contributed to greater variability in textured SCR results.

3 Effect of texturing on longevity of HDPE GMB: results and discussion

3.1 Antioxidant depletion

3.1.1 Std-OIT
The Std-OIT depletion results for the textured GMB (MxTA15) and its smooth edge (MxTsA15) were

fitted using a two-parameter (first order) exponential decay function (Hsuan and Koerner 1998; Rowe et

al. 2009; Abdelaal et al. 2014), viz (Fig. 1):

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𝑂𝐼𝑇𝑡 = 𝑂𝐼𝑇𝑜 × 𝑒 ―𝑠𝑡 (1)


and taking the natural logarithm on both sides, Eq. (1) becomes

ln (𝑂𝐼𝑇𝑡) = ln (𝑂𝐼𝑇𝑜) ― 𝑠𝑡 (2)


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where, OITt (min)= OIT value after incubation time t; OITo (min)= initial OIT value; and s (month-1) =
antioxidant depletion rate.

Full depletion of Std-OIT was observed in about 12 months at 75oC and 4 months at 85oC for the

smooth edge of the textured GMB (MxTsA15). In contrast, the full depletion of antioxidants was

observed after about 8 months at 75 and 3 months at 85oC (Fig. 1) for the textured portion of the roll

(MxTA15). At lower temperatures full depletion of antioxidants was not observed for either portion of

GMB, where the Std-OIT of MxTsA15 and MxTA15, respectively, depleted to 15% and 7% of the initial

value at 55oC and 84% and 79% at 40oC.

Texturing of the GMB surface resulted in faster depletion of the Std-OIT at all incubation

temperatures (Fig. 1). For instance, the observed antioxidant depletion rates (in month-1) for the smooth

edge and textured portions (MxTsA15, MxTA15) were (0.006, 0.008) at 40oC, (0.056, 0.075) at 55oC,

(0.326, 0.526) at 75oC, and (1.074, 1.421) at 85oC (Table 2). So texturing resulted in increasing the Std-

OIT depletion rates by about 40% at temperatures of 40-85oC.

3.1.2 HP-OIT
Antioxidants depletion was also monitored using HP-OIT test to detect antioxidants/stabilizers (e.g.,

HALS) that are not detected in the Std-OIT test. The HP-OIT data depleted to high residual values, thus

the results were fitted using three-parameter (OITo, s, and OITr) exponential decay function viz:

𝑂𝐼𝑇𝑡 = {(𝑂𝐼𝑇𝑜 ― 𝑂𝐼𝑇𝑟) × 𝑒 ―𝑠𝑡} + 𝑂𝐼𝑇𝑟 (3)

where, OITt (min) is the HP-OIT value at any time (t), OITr (min) is the residual HP-OIT value, OITo

(min) is the initial HP-OIT value, and s (month-1) is the HP-OIT depletion rate.

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The HP-OIT reached residual values at all temperatures for both the textured GMB and its

smooth edge (Supplementary material; Fig. S1). The HP-OIT residual values for the textured and smooth

edge of the GMB were 1110 and 1200 at 40oC, 810 and 860 at 55oC, 480 and 510 at 75oC, and 350 and

370 minutes at 85oC with normalized values (i.e., HP-OIT residual value divided by the initial HP-OIT
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value) of 0.70,0.76 at 40oC, 0.51 and 0.54 at 55oC, 0.30 and 0.32 at 75oC, and 0.22 and 0.23 at 85oC. The

difference in residual value between textured and smooth edge is relatively small and may simply be due

to a limited number of samples. Similar to Std-OIT, the texturing resulted in slightly faster HP-OIT

depletion rate than was observed for the smooth edge at all incubation temperatures (Table 2).

3.1.3 Antioxidants depletion predictions


The Arrhenius equation (Koerner et al. 1992) was used to predict the depletion rates at different

temperatures in different solutions using the experimentally obtained rates for Std-OIT and HP-OIT

(Table 2). The Arrhenius equation can be written as:

𝑠 = 𝐴 × e ―[𝐸𝑎/(𝑅𝑇)] (4)

where, A (month-1): collision factor; Ea (J.mol-1): activation energy; R (J.mol-1): universal gas constant

equals 8.314; and T (K): temperature.

Taking the natural logarithm on both sides, Eq. 4 becomes

ln (𝑠) = ln (𝐴) ―(𝐸𝑎/𝑅) × (1/𝑇) (5)

To consider the effect of variability and its effect on depletion times, a range of Std-OIT

depletion times were predicted at each temperature (Table 3). These depletion times were based on 95%

confidence band for the depletion rates estimated from the experimental results at the four ageing

temperatures (Fig. 2a) using the (i) best fit activation energy, (ii) maximum activation energy, and (iii)

minimum activation energy. The best fit activation energy (Ea) for the textured sheet (MxTA15) was 106

kJ/mol (R2 = 0.99) with a 95% confidence band range of 75 ≤ Ea ≤ 135 kJ/mol, while that for the smooth

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edge was very similar with a best fit Ea of 104 kJ/mol (R2 = 0.99) and range 69 ≤ Ea ≤ 139 kJ/mol. The

predictions assumed an average Std-OIT residual value of 3 minutes (Table 3).

Based on the established Arrhenius plots, the Std-OIT best estimate depletion time, td, at 40oC

was 37 years (95% confidence range: 18 ≤ td ≤ 79 years) for textured MxTA15, compared to 49 years (20
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≤ td ≤ 130 years) for smooth edge MxTsA15. At 25oC, the predicted depletion time increased to 280 years

(78 ≤ td ≤ 1100 years; textured) and 370 years (75 ≤td ≤ 1800 years; smooth edge). The predicted best

estimate Std-OIT depletion times for the textured portion were shorter than the smooth edge at all

temperatures.

The experimentally obtained HP-OIT depletion rates (Table 2) were used to establish the

Arrhenius plot of HP-OIT (Fig. 2b) to predict antioxidant depletion rate at various temperatures (Table 4).

Prediction of antioxidant depletion time needs both the depletion rate and residual HP-OIT values to

substitute in Equation 3. Thus, the experimentally obtained HP-OIT residual values at the test

temperatures were used to predict the HP-OIT residual values at other temperatures (Fig. S2) and the

following equations were established for the relationship between the HP-OIT residual value and the

incubation temperature:

ln(1/OITr) = 9.5-2880/T (K) for the textured GMB (MxTA15) (6)

ln(1/OITr) = 9.65-2950/T (K) for the smooth edge (MxTsA15) (7)

The observed increase of the HP-OIT residual values at lower temperatures suggests that HALS

were more mobile and capable of diffusing outside the GMB core at higher temperatures resulting in

lower HP-OIT residual values (Rowe and Ewais 2014). This is consistent with the reported very low

solubility of the structural units of the hindered amine light stabilizers (HALS; added to the GMBs

examined in this study) at temperatures approaching room temperature (Malik et al. 1992) which make it

difficult to estimate accurate residual values at temperatures less than about 40oC even with about 3 years

of data. Thus, Equations 6 and 7 were used to estimate the HP-OIT residual value at temperatures ≥ 40oC

and not used to predict the depletion time at temperatures less than 40oC (Table 4). The predicted HP-
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OIT depletion times for the textured and smooth edge of the GMB were 2.5 and 2.7 years at 40oC and

0.79 and 0.81 years at 85oC, respectively (Table 3).

The predicted depletion times based on both Std-OIT and HP-OIT suggested a greater effect of
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texturing on accelerating the Std-OIT depletion time compared to the HP-OIT depletion time, likely due

to the lower mobility of the higher molecular weight HALS contributing to HP-OIT. More importantly,

the predicted Std-OIT depletion times were longer than the HP-OIT depletion times at temperatures less

than 75oC suggesting that the Std-OIT package played the more crucial role in protecting the GMB

compared to the antioxidants/stabilizers package detected by the HP-OIT test at most temperatures. Thus,

the time to antioxidant depletion (length of Stage I) was based on the Std-OIT depletion time (Table 3) at

temperatures less than 75oC.

3.2 Melt Flow Index


The molecular weight changes due to ageing were monitored using the high load melt flow index test

(HLMI-21.6 kg). An increase in the MFI suggests a reduction in the molecular weight of the polymer due

to oxidation induced chain scission while a reduction in MFI suggests an increase in the molecular weight

of the polymers due to oxidation induced cross linking (Hsuan and Koerner 1998).

The variations in HLMI was monitored for 34 months for both the textured GMB and its smooth

edge. At 85oC, no changes were observed in the HLMI during the first 20 months (Fig. 3). Similar

reductions of HLMI were observed for both the textured GMB and its smooth edge after 20 months of

incubation and the normalized HLMI decreased to an average of about 0.6 (Fig. 3) suggesting the

dominance of cross linking oxidation reactions. No changes in HLMI were observed at the lower

temperatures (40, 55, and 75oC) during the 34 months monitored.

There was no statistical significant difference between the HLMI of the textured and smooth edge

of the GMB over the 34 months monitored. In particular, both the textured GMB and its smooth edge

exhibited similar oxidative degradation behaviour suggesting that the co-extrusion using blowing agent

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texturing technique had no notable effect on the molecular weight distribution of the PE initially or during

degradation of the GMB.

3.3 Tensile Properties


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The results of the tensile test for the cross machine direction of the GMB indicated no degradation in the

break strength and strain of the GMB at 85oC (or lower temperatures) during the 34 months monitored

(Fig. 4), with the data scattered around the original value.

The average tensile break strength and strain for the virgin textured specimens was 38.5 kN/m

and 502% compared to 60.7 kN/m and 784% for the smooth edge (Table 1). Thus, the texturing of the

surface of the GMB resulted in about 35% reduction in the tensile break strength and strain of the unaged

GMB specimens. The texturing also resulted in notable variability in GMB’s break strength and strain.

For instance, at 85oC after 24-months incubation (Fig. S3; marked by a dotted oval) the average textured

break strength was 33.8 ± 10.5 (CoV= 27%), and the minimum and maximum textured tensile break

strength were 23.1 kN/m and 44.1 kN/m (normalized values of 0.6 and 1.15), respectively. For the same

data point (Fig. 4; marked by a dotted oval), the average textured break strain was 500 ± 127 (CoV= 25%)

and the minimum and maximum textured tensile break strain were 364% and 600% (normalized values of

0.72 and 1.2), respectively. Fig. 5a shows the tensile stress-elongation relation for the aforementioned 24

months’ data point at 85oC for: (i) the smooth edge, (ii) the textured specimen that had the maximum

break strength and strain (S1), and (iii) the textured specimen that had the minimum break strength and

strain (S2). For the smooth edge specimen, the tensile break strength was 1.73 times the yield strength,

and the break strain was 22 times the yield strain. For the textured specimen (S1), the tensile break

strength was 1.2 times the yield strength, and the tensile break strain was 14.7 times the yield strain. For

the textured specimen (S2), the tensile break strength was 0.68 times the yield strength, and the break

strain was 9.4 times the yield strain. Fig. 5b shows photo of the failed tensile specimens S1 and S2. For

S1, the failure was located slightly above the mid-length of the narrow section, while for S2, the failure

was at the top of the narrow section; likely due to a lower local textured GMB thickness at this location.
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To check the effect of surface deformation or non-homogeneous core thickness of the textured

GMB on the break tensile strength and strain, the surface of a smooth edge tensile specimen was notched

from one side only. The notch was at the top of the narrow section of the dog bone specimen with a depth

of 15% of the nominal thickness of the GMB (arbitrarily chosen notch depth to simulate the non-uniform
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cross section of the textured GMB). In addition to the three 24-months aged specimens discussed above,

Fig. 5a also shows the tensile stress-elongation relation for three unaged specimens: (iv) smooth edge, (v)

textured, and (vi) notched smooth edge specimen. For the un-notched smooth edge tensile specimen, the

tensile break strength was 2.1 times the yield strength, and the break strain was 25 times the yield strain.

While for the textured GMB, the tensile break strength was 1.05 times the yield strength, and the break

strain was 10 times the yield strain. For the 15% notched smooth edge specimen, the tensile break

strength was 0.43 the yield strength and the break strain was 8.3 times the yield strain. Thus, the

reduction in, and variability of, break properties and toughness (the area under the stress-strain curve) of

the textured GMB for the virgin and aged specimens was due to the variability of the GMB thickness that

resulted in stress concentration at the grooves between the asperities on the surface of the textured portion

(Scheirs 2009) that initiated fracturing at these zones (Brown and Lu 1987), and this fracture propagated

during the tensile test and resulted in premature break at lower break/yield strength ratio compared to an

equivalent smooth GMB. However, break strength and elongation is not critical for a GMB that forms a

part of a well-designed barrier system because the stress and strain level in the field should be

significantly less than the yield stress and strain of the GMB and hence well below the unaged break

strength and strain.

3.4 Stress- crack resistance


SCR is not normally conducted on textured GMBs due to the variability in thickness. However, an

attempt was made to find specimens with a relatively uniform (≤ 4% variation as discussed earlier)

ligament thickness for a notched specimen and while they had a larger scatter in data than the smooth

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edge they reflected a similar behaviour (Fig. 6). In particular, the trend of changing SCR with incubation

time for both the textured GMB and its smooth edge were similar.

As previously indicated, there was no change in tensile break properties at any temperature
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during the 34 months monitored. Also, the HLMI data showed no degradation during the first 20 months

of incubation at 85oC (Fig. 3) and none during the whole 34 months at the lower temperatures. Thus the

reduction in SCR observed within the first 4 months for both the textured and smooth edge of the GMB at

all test temperatures (including 40oC; Fig. 6) is attributed to physical ageing rather than surface oxidation

(Ewais and Rowe 2014; Ewais et al. 2018; Morsy 2019).

The average reduced SCR value due to physical ageing, SCRm, was calculated for both the

textured sheet and smooth edge of the GMB at all incubation temperatures after excluding the SCR

readings marked by “?” in Fig. 6. The normalized values of SCRm (λ) for the (textured, smooth edge)

portions of the GMB were (0.57±0.38, 0.56±0.09) at 40oC, (0.45±0.17, 0.30±0.06) at 55oC, (0.32±0.20,

0.24±0.11) at 75oC, and (0.42±0.28, 0.41±0.11) at 85oC (Table 5). There was no statistically significant

difference at any temperature but due to the variability of the textured specimens, the smooth edge λ is

considered more representative of the actual normalized values of SCRm where there is a difference.

Although the reduction in the SCR due to physical ageing at 55 and 75oC was greater than at 85oC for

both GMB portions, no oxidative degradation of SCR was observed at any temperature other than 85oC

during the 34 months monitored.

Thermo-oxidative degradation of SCR first became apparent for both the textured and smooth

portions of the GMB after 24-months immersion at 85oC. Both degraded similarly until nominal failure

was reached (Fig. 6). After 34-months immersion at 85oC, the SCR had degraded to normalized values of

0.05 (75 hours) for the textured GMB and 0.03 (115 hours) for the smooth edge. The tNF is often taken as

the time at which the SCR degrades to 50% of the minimum SCR value specified by GRI-GM13 (500

hours) (Rowe et al. 2009) or 50% of the unaged SCR of the tested product (Hsuan and Koerner 1998).

Since for GMBs aged physically, SCRm is the most representative long-term SCR value until the onset of
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chemical degradation of SCR (Morsy 2019), an alternative interpretation of when tNF is reached was taken

to be the time at which SCR reduced to 50% of SCRm. Thus, for the SCR data at 85oC (Table 6):

 Definition of tNF to 50% of the initial SCR value (~4000 hours) is considered unreasonable given
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that this would imply failure at ~2000 hours and hence after ~4 months at all temperatures as a

result of physical changes in SCR. Also in practice, very few SCR tests are conducted for more

than the 500 hours required by GRI-GM13 and even fewer for more than 1000 hours and so SCRo

is generally unknown for SCRo > 1000 hours.

 tNF was 29 months for the textured GMB (MxTA15) and 30 months for its smooth edge

(MxTsA15) based on degradation of SCR to 250 hours (50% of the GRI-GM13 value).

 tNF for the textured GMB and its smooth edge, was 28 and 26 months, respectively, based on the

criterion of 50% SCRm at 85oC (equivalent to a normalized SCR of 0.21 and 0.205, respectively).

 tNF for the textured GMB and its smooth edge was 29 and 28 months, respectively, based on the

criterion of 50% of the mean of SCRm at 55oC and 75oC representing the temperature range at

which minimum SCRm could be obtained (equivalent to a normalized SCR of 0.19 and 0.125,

respectively).

In summary, texturing resulted in a large variability in the SCR results for textured specimens

with the same ageing as the smooth edge but they followed the same trend. Depending on the criterion

used, there was a 0.5-2.5 month(s) difference in tNF for textured and smooth edge but with some

indicating a greater and some a smaller tNF for the textured GMB. It is concluded that there was no

significant effect of texturing on longevity at 85oC. Note, however, that the difference in the length of

Stage I was only 1 month and the uncertainty around the time to nominal failure is greater than this. Thus,

the possibility of a greater difference in tNF at lower temperatures cannot be excluded. The large

variability in textured SCR results is likely due to (a) unavoidable variability in thickness and stress

across the specimens, and (b) defects and/or discontinuities on the textured GMB surface (Müller 2007;

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Scheirs 2009) beneath the ligament under the notch. However, this also suggests that the textured GMB is

likely to be somewhat more susceptible to stress cracking due to low local SCR values and variability in

thickness (stress concentrations) as well as potential defects and/or discontinuities on the textured GMB

surface.
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4 Effect of resin lot on longevity of GMB: results and discussion


The GRI-GM13 recommends inferring the SCR of a textured GMB from the SCR of its smooth edge or

an equivalent smooth GMB due to the non-uniformity of the thickness and consequent variability in the

SCR results (as was indeed confirmed in this study). The previous section showed that the longevity of

this textured GMB can be reasonable simulated by it smooth edge based on the MFI and SCR degradation

trends for both portions. However, the area of the smooth edge is limited (150-200 mm) and hence an

“equivalent” smooth GMB is often used to infer the unaged SCR and/or the longevity of the textured

GMB. Also, some GMBs have a somewhat textured edge and hence the only option for obtaining SCR

testing an “equivalent” smooth GMB. This begs the question as to how representative is an “equivalent”

smooth GMB to its smooth edge counterpart. Therefore, this section investigates how the longevity of an

“equivalent” smooth GMB compares to that of a smooth edge by monitoring the longevity of the smooth

edge of the textured GMB (MxTsA15: manufactured 15 August 2015) and another “equivalent” smooth

GMB made the following day in the same plant from nominally the same resin (MxF15: manufactured 16

August 2015) but from a different resin lot.

4.1 Antioxidants depletion


Although the textured and “equivalent” smooth GMB were of the same nominal resin and produced only

a day apart in the same plant and both would meet typical specifications (e.g., those based on GRI-GM13)

and hence may be regarded as “equivalent”, inspection of Table 1 shows that they are not the same.

MxTA15 and MxTsA15 both had Std-OITo= 185 ± 10 minutes and HP-OITo= 1580 ± 90 minutes, the

‘equivalent” MxF15 had Std-OITo= 153 ± 6 minutes and HP-OITo= 990 ± 140 minutes. Both sets of

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values can generally be regarded as good (even high). But they are not the same and this may be expected

to affect the long term performance as discussed below.

The Std-OIT results were fitted using Equations 1 and 2. Full depletion of Std-OIT of the smooth GMB
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(MxF15) and smooth edge (MxTAs15) were, respectively, observed to be about 3 and 4 months at 85oC,

and 8 and 12 months at 75oC (Fig. 7). The full depletion of antioxidants was not observed for either GMB

at lower temperatures during the 34 months monitored. The normalized Std-OIT (Std-OITt /Std-OITo)

after 34 months at 55oC was 0.06 (MxF15) and 0.07 (MxTsA15), while at 40oC it was 0.79 (MxF15) and

0.84 (MxTsA15) (Fig. 7).

Best fit, maximum and minimum activation energies (95% confidence band) obtained from an

Arrhenius plot based on the observed depletion rates (Fig. S4) were used to predict a range of depletion

times for an average Std-OIT residual value of 3 minutes (Table 3). The Std-OIT depletion time at 40oC

was 28 years (17 to 49 years range based on 95% confidence limit) for MxF15 compared to 49 years (20

to 130 years range based on 95% confidence limit) for MxTsA15. At 25oC, the predicted depletion time

of MxF15 increased to 200 years (80 to 500 years) compared to 370 years (75 to 1800 years) for

MxTsA15. Thus the time to depletion, in this case, of the equivalent smooth GMB was 50-60% of that of

the textured GMB smooth edge.

The HP-OIT results were fitted using Equation 3 and reached residual values at all incubation

temperatures for both MxTsA15 and MxF15. The observed normalized residual values of MxF15 were

0.86, 0.65, 0.48, and 0.36 at temperatures of 40, 55, 75, and 85oC, respectively, compared to 0.76, 0.54,

0.32, and 0.23, respectively, for MxTsA15 (Fig. S5). The depletion rates for both GMBs were almost the

same at all temperatures except at 85oC where the depletion rate of MxF15 was 1.4 times faster than

MxTsA15.

The experimentally obtained HP-OIT depletion rates (Table 2) were used to establish the

Arrhenius plot of HP-OIT (Fig. S6) to predict antioxidant depletion rate at various temperatures (Table 4).

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Prediction of antioxidant depletion time needs both the depletion rate and residual HP-OIT values to

substitute in Equation 5. Thus, the experimentally obtained HP-OIT residual values at the test

temperatures were used to predict the HP-OIT residual values at other temperatures (Fig. S7). Equation 7

was established for the relationship between the HP-OIT residual value and the temperature for
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MxTsA15, and the following equation was obtained for MxF15:

ln(1/OITr) = 6.76-2076/T (K) (8)

Equations 7 and 8 were only used to estimate the HP-OIT residual value at temperatures ≥ 40oC

for the reasons discussed in Section 3. The predicted HP-OIT depletion times for MxF15 at temperatures

of 40 and 85oC were 2.9 to 0.67 years, respectively (Table 4). While, for MxTsA15 the predicted HP-OIT

depletion time at 40 and 85oC were 2.7 to 0.81 years, respectively (Table 4).

Similar to the textured GMB and its smooth edge, the Std-OIT package for the smooth GMB was

more effective in protecting the GMB at temperatures (≤65oC) as evidenced by the longer depletion time

for the Std-OIT compared to the HP-OIT.

4.2 Melt flow index and tensile properties


Although produced from nominally the same resin one day later by the same manufacturer, MxTsA15 had

slightly broader molecular weight distribution (higher Melt flow ratio; Table 1) (Scheirs 2009) and higher

molecular mass (lower MFI; Table 1) (Haward and Owen 1977) compared to MxF15. As indicated above

for OIT this suggest that rolls from nominally the same resin (but different resin lots) are not necessarily

the same and highlights the limitations of typical quality control practices.

During the 34-months monitoring period no changes in HLMI were observed for either MxF15

and MxTsA15 at 40, 55, and 75oC. At 85oC, no changes were observed in HLMI for either GMBs during

the first 20 months (Fig. 8). Reduction of HLMI was observed for MxTsA15 and MxF15 after 20 months

of ageing and the normalized MFI at 34 months had decreased to 0.5 and 0.6, respectively, implying the

dominance of cross-linking oxidation reactions. However, the results of tensile test (break strength and

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strain) in the cross machine direction showed no degradation at any temperatures (Fig. S8 and 9) for

either GMB.

4.3 Stress-crack resistance


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The early reduction of SCR due to physical ageing observed for MxTsA15 was also observed for the

smooth “equivalent” MxF15 at all incubation temperatures (Fig. 10). The average value of SCRm was

calculated for both GMBs at all incubation temperatures excluding the SCR readings for the data points

marked by a question mark “?”. The values of λ for (MxTsA15, MxF15) were (0.56±0.09, 0.36±0.15) at

40oC, (0.30±0.06, 0.19±0.07) at 55oC, (0.24±0.11, 0.15±0.03) at 75oC, and (0.41±0.11, 0.40±0.12) at

85oC (Table 5). For MxF15, the difference between the values of λ at 55 and 75oC was not statistically

significant (at the 95% confidence level) and hence the minimum value of λ (i.e.; the maximum effect of

physical ageing on SCR) (based on 55 to 75oC data) was 0.17±0.06 (SCRm ~640 hours) which is notably

less than 0.24±0.08 (SCRm ~1000 hours) for MxTsA15. The minimum estimated value of λ was at 75oC

followed by 55oC indicating that the minimum values of λ was in the temperature range of 55 to 75oC for

both MxTsA15 and MxF15. This is likely because full relaxation of manufacture residual stresses is

achieved at an incubation temperature equal to approximately 50% of the melting point of the GMB

(Vöhringer 1987) estimated as 126.15 to 127oC for both GMBs (i.e., at about 63oC). The observed

difference in the value of λ and SCRm between the smooth edge and its equivalent smooth counterpart

suggested variations in the magnitude of manufacture induced residual stresses in both GMBs. Although

the value of λ at 85oC was higher than observed at 55 and 75oC, thermo-oxidative degradation of SCR

was observed only at 85oC for both GMBs. At 85oC, Stage III started after 20 months (MxF15) and 24

months (MxTsA15) and SCR degraded to a normalized value of 0.016 (61 hours) and 0.03 (115 hours),

respectively (Fig. 10). The tNF was estimated based on the three criteria mentioned in Section 3 (Table 6)

and was: (i) 27 and 30 months for the smooth roll (MxF15) and the smooth edge (MxTsA15), based on

degradation of SCR to 250 hours (50% of the GRI-GM13 value), (ii) 23 and 26 months for MxF15 and

MxTsA15, based on the criterion of 50% SCRm at 85oC (equivalent to a normalized SCR of 0.20 and

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0.205, respectively), and (iii) 26 and 28 months for MxF15 and MxTsA15, based on the criterion of 50%

of the minimum SCRm (based on 55oC and 75oC data); with a difference of 6-14% depending on the

criterion used.
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Although the difference between the initial values of SCRo of “equivalent smooth” GMB

(MxF15) and the textured smooth edge (MxTsA15; Table 1) was not statistically significant (at 95%

confidence level), there was a difference in terms of both physical ageing (λ) and oxidative degradation

and time to nominal failure (tNF). Given the similar performance of the textured and smooth portions of

the same roll, the difference between the smooth edge and smooth “equivalent” rolls may be regarded as

reflecting the difference between two GMBs from different resin lots of nominally the same resin; a factor

to keep in mind in construction quality control for projects where a GMB with a with a long service-life is

required.

5 Conclusions
The effect of co-extrusion blown-film texturing on the longevity of a HDPE GMB with a core thickness

of 1.5 mm was investigated. The performance of the textured and smooth edge portions of a GMB (all

meeting the requirements of typical specifications based on GRI-GM13), and an “equivalent” smooth

GMB manufactured one day later in the same plant from nominally the same polymer resin but a different

lot, were monitored for 34 months. Arrhenius modeling was used to predict antioxidant depletion time for

the antioxidants/stabilizers detected by the ASTM Std-OIT and HP-OIT tests. For the GMBs examined,

immersed in simulated MSW leachate at four temperatures (40-85oC), it is concluded that:

1. OIT depletion for the textured portion was 40% (Std-OIT) and 9% (HP-OIT) faster than for the

smooth edge portion of the GMB. This is attributed to the texturing using a blowing agent which

results in larger surface area exposed to the incubation fluid due to the presence of the corrugations

giving a faster evaporation and/ or dissolution of antioxidants from the GMB surface.

2. The antioxidant depletion rates for the textured GMB (both the smooth edge and textured portion)

were notably different to those of a smooth GMB with nominally the same resin suggesting that
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despite being the “same product” they had differences in the proportions/concentration/type of Std-

OIT and HP-OIT antioxidants/stabilizers in nominally the same GMBs. For instance, the Std-OIT

depletion rate for the smooth GMB was 1.5 times faster than the smooth edge, while both had

almost the same HP-OIT depletion rate.


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3. Based on MFI, detectable cross-linking was inferred to have started after 20 months at 85oC for

both the textured and smooth edge portions of the GMB and the smooth GMB made from

nominally the same resin; this apparent cross-linking and the decrease in MFI continued for the

remainder of the period monitored (34 months).

4. Physical ageing in terms of SCR was observed in all examined GMBs at all test temperatures, and

the minimum value of SCRm was observed for the temperature range of 55 to 75oC.

5. At 85oC there was no clear difference in the time at which the oxidative degradation in SCR started

(20 months) for the textured or smooth edge portions of the GMB. There was about a 1-2 month(s)

difference in time to nominal failure, tNF, for textured and smooth edge. This difference is

relatively small in absolute value (~5% of tNF), however this uncertainty in the time to nominal

failure is greater than the 1-month difference in the length of Stage I. Thus, the possibility of a

greater difference in tNF at lower temperatures, where there was a greater difference in the length of

Stage I, cannot be excluded.

6. The difference between the best estimate time to antioxidant depletion (28 years at 40oC) for the

smooth “equivalent” roll and (49 years at 40oC) for the smooth edge of the textured roll may be

regarded as reflecting the difference between two GMBs from different resin lots of nominally the

same resin; a factor to keep in mind in construction quality control for projects where a GMB with

a long service-life is required. The warning of a likely difference was evident from the initial Std-

OIT and HP-OIT values.

The results of this study suggested that, at least for the product tested, texturing results in an

acceleration of the depletion rate of antioxidant detected by both Std-OIT and HP-OIT but, at 85oC, the

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results suggest that texturing did not significantly affect the observed longevity of this GMB. More

incubation time is needed to observe the relative performance of the textured GMB and its smooth edge at

lower temperatures. The current study investigated one double-side textured GMB. More textured GMBs

products with different thickness and/or texturing techniques need to be examined in order to verify the
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effect of texturing on the longevity of GMBs.

While the results of this study are generally positive with respect to the use of a textured GMB

relative to an otherwise identical smooth product, the much higher variability and the 40% faster rate of

Std-OIT depletion (i.e., shorter Stage I of its service-life) suggests that, in the absence of evidence to the

contrary, textured GMB should only be used where essential for slope stability and not on the base of

landfills if not required for stability.

Acknowledgements
The research reported in this paper was supported by a Natural Sciences and Engineering Research

Council of Canada (NSERC) grant (A1007) to Dr. R.K. Rowe. The equipment used was funded by

Canada Foundation for Innovation (CFI) and the Government of Ontario’s Ministry of Research and

Innovation.

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Rowe, R.K., Rimal, S., and Sangam, H. 2009. Ageing of HDPE geomembrane exposed to air, water and

leachate at different temperatures. Geotextiles and Geomembranes, 27(2): 137-151.

Scheirs, J. 2009. A guide to polymeric geomembranes: a practical approach. John Wiley and Sons.

Stark, T.D., Williamson, T.A., and Eid, H.T. 1996. HDPE geomembrane/geotextile interface shear

strength. Journal of Geotechnical Engineering, 122(3): 197-203.

Thiel, R.S. 2001. Peak vs. Residual Shear Strength for Landfill Bottom Liner Stability Analysis, 15th

Annual GRI Conference. Geosynthetic Institute, Folsom, PA, USA.

Touze-Foltz, N., Bannour, H., Barral, C., and Stoltz, G. 2016. A review of the performance of

geosynthetics for environmental protection. Geotextiles and Geomembranes, 44(5): 656-672.

25
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Vohringer, O. 1987. Relaxation of residual stresses by annealing or mechanical treatment. Pergamon

Press, Advances in Surface Treatments. Technology--Applications--Effects. Edited by A Niku-

Lari. Pergamon. pp. 367-396.

Yoo, H., Jeon, H.Y., Lee, K., Yoo, C., and Herath, C.N. 2010. Evaluation of the chemical resistance of
Can. Geotech. J. Downloaded from www.nrcresearchpress.com by KUNGLIGA TEKNISKA HOGSKOLAN on 04/01/19

high‐density polyethylene geomembranes. Journal of applied polymer science, 117(5): 2575-

2582.

26
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List of Figures:

Figure 1. Variation of the normalized Std-OIT (OITt/OITo) with incubation time for the textured GMB

and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3: (a) 40 and 75oC;
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(b) 55 and 85oC.

Figure 2. Arrhenius plot of OIT depletion for the textured GMB and its smooth edge (MxTA15 and

MxTsA15): (a) Std-OIT; (b) HP-OIT. Maximum and Minimum Ea for Std-OIT predictions were

calculated at 95% confidence interval.

Figure 3. Variation of normalized high load melt flow index (MIt/MIo) with incubation time for the

textured GMB and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3 at

85oC. The solid line (smooth edge) coincides with the dashed line (textured). Error bars represent

range of results.

Figure 4. Variation of the normalized tensile break strain in cross machine direction with incubation time

for the textured GMB and its smooth edge (MxTA15 and MxTsA15) immersed in MSW

Leachate 3 at 85oC. The solid line (smooth edge) coincides with the dashed line (textured). Error

bars represent range of results.

Figure 5. The effect of texturing on the break strength and elongation-cross machine direction in tensile

uniaxial test: (a) Stress-elongation; (b) Plane of failure.

Figure 6. Variation of the normalized SCR-cross machine direction (SCRt/SCRo) with incubation time for

the textured GMB and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3:

(a) 40oC; (b) 55oC; (c) 75oC; (d) 85oC.

Figure 7. Variation of the normalized Std-OIT (OITt/OITo) with incubation time for the smooth edge of

the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed in MSW Leachate 3:

(a) 40 and 75oC; (b) 55 and 85oC.

27
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Figure 8. Variation of the normalized high load MFI (MIt/MIo) with incubation time for the smooth edge

of the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed in MSW Leachate 3

at 85oC. The solid line (smooth edge) coincides with the dashed line (textured) in the incubation
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time interval 0 to 20 months. Error bars represent range of results.

Figure 9. Variation of the normalized tensile break strain - cross machine direction with incubation time

for the smooth edge of the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed

in MSW Leachate 3 at 85oC. The solid line (smooth edge) coincides with the dashed line (smooth

roll). Error bars represent range of results.

Figure 10. Variation of the normalized SCR-cross machine direction (SCRt/SCRo) with incubation time

for the smooth edge of the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed

in MSW Leachate 3: (a) 40oC; (b) 55oC; (c) 75oC; (d) 85oC.

28
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List of Tables:

Table 1. Initial properties of GMBs.


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Table 2. Observed OIT depletion rates and residual values (Std-OIT and HP-OIT).

Table 3. Predicted Std-OIT depletion time (years).

Table 4. Predicted HP-OIT depletion time (years).

Table 5. Values of SCRm at different temperatures.

Table 6. Predicted durations of the three Stages of degradation at 85oC.

29
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Table 1. Initial properties of GMBs.

Property Method Unit Mean ± SD1

GMB -- -- Textured Smooth edge Smooth roll


Designator -- -- MxTA15 MxTsA15 MxF15
Type -- -- HDPE HDPE HDPE

Thickness2 -- mm 1.5 1.5 1.5


ASTM D59944 ASTM D51995 ASTM D51995
Asperity height2 ASTM D74666 mm 0.43 -- --
GMB density 2 ASTM D15057 g/cm3 0.947 0.947 0.947
Std-OIT ASTM D38958 min 185±10 185±10 153±6
HP-OIT ASTM D58859 min 1580±90 1580±90 990±140
HLMI (21.6kg) g/10min 13.3±0.5 13.3±0.5 15.3±0.3
LLMI (2.16 kg) ASTM D123810 g/10min 0.11±0.002 0.11±0.002 0.135±0.002
Melt flow ratio unitless 121 121 113

SCR ASTM D539711 hours 1600±1640 3970±1020 3860±700


(150-5700)3 (2700-5700)3 (3100-4800)3
Tensile properties ASTM D669312 -- -- -- --
Break stress-cross machine direction kN/m 30.5± 1 28.6± 1 28.3± 1
Type IV
Break strain-cross machine direction % 35.3± 2 59.0± 4.50 55.2± 2.34
Break stress-cross machine direction kN/m 38.5±4 61.0±2 58.5±2
Type V
Break strain-cross machine direction % 502±41 784±44 796±13
1standard deviation; Provided by the manufacturer; (minimum-maximum) SCR
2 3 readings. 4
ASTM (2010a). 5 ASTM (2012). 6 ASTM (2010b). 7
ASTM. (2010c). 8 ASTM (2007a). 9 ASTM (2006). 10 ASTM (2013). 11 ASTM (2007b). 12 ASTM (2004) .
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Table 2. Observed OIT depletion rates and residual values (Std-OIT and HP-OIT).

Temperature (oC) GMB MxTA15 MxTsA15 MxF15


sStd-OIT (month-1) 0.008 0.006 0.011
Std-OITr (min) N/A1 N/A1 N/A1
40
sHP-OIT (month-1) 0.09 0.07 0.05
HP-OITr (min) 1110 1200 850
sStd-OIT (month-1) 0.08 0.06 0.08
Std-OITr (min) N/A1 N/A1 N/A1
55
sHP-OIT (month-1) 0.14 0.13 0.11
HP-OITr (min) 810 860 640
sStd-OIT (month-1) 0.53 0.33 0.48
Std-OITr (min) 3.0 4.0 3.0
75
sHP-OIT (month-1) 0.28 0.26 0.28
HP-OITr (min) 480 510 480
sStd-OIT (month-1) 1.42 1.07 1.51
Std-OITr (min) 3.0 3.0 2.0
85
sHP-OIT (month-1) 0.40 0.38 0.43
HP-OITr (min) 350 364 310
1 The Std-OIT has not depleted yet.

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Table 3. Predicted Std-OIT depletion time (years); rounded to 2 significant digits.


MxTA15 MxTsA15 MxF15
Minimum Maximum Minimum Maximum Minimum Maximum
Temperature
Ea at 95% Ea at 95% Ea at 95% Ea at 95% Ea at 95% Best fit Ea at 95%
(oC) Best fit Ea Best fit Ea
confidence confidence confidence confidence confidence Ea confidence
level level level level level level
10 390 > 2000 > 2000 330 > 2000 > 2000 450 1600 > 2000
15 230 1300 > 2000 200 1600 > 2000 250 780 > 2000
20 130 590 > 2000 120 760 > 2000 140 390 1200
25 78 280 1100 75 370 1800 80 200 500
30 47 140 440 47 190 730 47 100 230
35 29 72 180 30 95 300 28 53 100
40 18 37 79 20 49 130 17 28 49
45 11 20 35 13 26 54 10 16 24
50 7.5 11 16 8.8 14 24 6.6 9 12
55 4.9 6.0 7.5 5.9 8.0 11 4.2 5 5.9
60 3.2 3.3 3.6 4.1 4.5 5.0 2.7 2.8 3.0
65 2.2 2.0 1.7 2.8 2.6 2.4 1.7 2.0 1.6
70 1.5 1.1 0.86 2.0 1.5 1.20 1.2 1.0 0.85
75 0.99 0.6 0.44 1.4 0.9 0.58 0.77 0.6 0.46
85 0.48 0.2 0.12 0.72 0.3 0.15 0.35 0.2 0.15
Std-OIT depletion times assessed based on a residual value of 3 minutes for all GMBs at different temperatures.

3
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85
75
70
65
60
55
50
45
40
(oC)
Temperature

1.0
1.2
1.4
1.6
1.8
2.1
2.3
2.5

0.79
MxTA15

4
1.1
1.3
1.5
1.7
2.0
2.3
2.6
2.7

0.81
HP-OIT
MxTsA15

1.2
1.5
1.8
2.1
2.5
2.8
2.9

0.67
0.99
MxF15
Table 4. Predicted HP-OIT depletion time (years); rounded to 2 significant digits.
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Table 5. Values of SCRm at different temperatures; rounded to two significant digits.

Mean ± Range
GMB Unit
MxTsA15 MxF15
SCRo (mean±SD) hours 3970±1020 3860 ± 700
Range in SCRo (min, max) hours 2700-5700 3100-4800
SCRm (mean±SD) at 85oC hours 1650 ±440 1540±470
SCRm/SCRo(mean±SD) at 85oC - 0.41±0.11 0.40±0.12
SCRm (mean±SD) at 75oC hours 880 ± 310 570±110
SCRm/SCRo(mean±SD) at 75oC - 0.24±0.11 0.15±0.03
SCRm (mean±SD) at 55oC hours 1200 ±250 720±290
SCRm/SCRo(mean±SD) at 55oC - 0.30±0.06 0.19±0.07
SCRm (mean±SD) at 40oC hours 2200 ±340 1410±590
SCRm/SCRo(mean±SD) at 40oC - 0.56±0.09 0.36±0.15
Minimum SCRm (mean±SD) based on 55 and 75oC hours 990 ±330 640 ±220
Minimum SCRm/SCRo(mean±SD) based on 55 and 75oC - 0.24 ±0.08 0.17 ±0.06

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Table 6. Predicted durations of the three Stages of degradation at 85oC (rounded to two significant digits; some numbers may not add due to
rounding).

tNF based on tNF based on tNF of SCR based on


td-Std-OIT 1 td – HP-OIT 2 Stage (I)3 Stage (II)4 Stage (III)6
GMB 50% of SCRm 50% SCRm-min5 50% of SCRGRI-GM13
(months) (months) (months) (months) (months)
(months) (months) (months)

Textured
2.7 9.5 9.5 15 28 29 29 5.0
MxTA15
Smooth edge
4.0 9.7 9.7 14 26 28 30 6.0
MxTsA15
Smooth roll
2.8 8.1 8.1 12 23 26 27 10
MxF15
1 Predicted Std-OIT depletion time based on Std-OIT residual value of 3.0 minutes; 2 Predicted HP-OIT depletion time based on a variable HP-OIT

residual value; 3 Predicted length of Stage (I) based on the longer depletion time predicted from Std-OIT and HP-OIT; 4 Observed length of Stage
(II) based on the degradation of SCR with incubation time; 5 SCRm-min was estimated as the mean for the SCRm observations at both 55oC and 75oC;
6 Length of Stage (III) and is the difference between the maximum estimated t , based on SCR, and the summation of the lengths of Stages I and
NF
II.

6
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2
(a)
1

ln [normalized Std-OIT (-)]


-0

-1 T (oC) GMB Regression line equation


Textured ln (OITt)=ln (185)-0.008×t
40
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Smooth edge ln (OITt)=ln (185)-0.006×t


-2
Textured ln (OITt)=ln (185)-0.53×t
75
Smooth edge ln (OITt)=ln (185)-0.33×t
-3
Smooth edge-40oC
-4 Textured-40oC
Smooth edge-75oC
-5 Textured-75oC
-6
2
T (oC) GMB Regression line equation
(b) Textured ln (OITt)=ln (185)-0.08×t
1 55
Smooth edge ln (OITt)=ln (185)-0.06×t
Textured ln (OITt)=ln (185)-1.42×t
ln [normalized Std-OIT (-)]

85
-0 Smooth edge ln (OITt)=ln (185)-1.07×t

-1

-2

-3
o
Smooth edge-55 C
-4 Textured-55oC
Smooth edge-85oC
-5
Textured-85oC
-6
0 10 20 30 40

Incubation time (months)

Figure 1. Variation of the normalized Std-OIT (OITt/OITo) with incubation time for the textured GMB
and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3: (a) 40 and 75oC; (b) 55
and 85oC. Error bars represent range of results; The data are presented in two figures for clearer
presentation of data points.

1
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4
Textured- Best fit
Textured-95% confidence band
2 Smooth edge- Best fit
Smooth edge-95% confidence band
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ln [S (months-1)] 0

-2

-4
Ea
Arrhenius equation; R2
(kJ/mol)
-6 Best fit:106 ln(s)= 35.9-(12695/T);0.99
Textured Max.: 135 ln(s)= 46.2-(16180/T);0.92
Min.:75 ln(s)= 25-(9036/T);0.91
-8 Best fit:104 ln(s)= 34.97-(12508/T);0.99
Smooth
Max.: 139 ln(s)= 47.6-(16740/T);0.88
edge
Min.:69 ln(s)= 22.3-(8268/T);0.88 (a) Std-OIT
-10
2
Textured- Best fit
Textured-95% confidence band
0
Smooth edge- Best fit
Smooth edge-95% confidence band
ln[S (month-1)]

-2

-4
Ea Temp.
GMB Arrhenius equation R2
(kJ/mol) range
Textured 31.78 ln(s)= 9.32-(3680/T) ≥40oC 0.99
-6 Smooth edge 32.24 ln(s)= 10.53-(4120/T) ≥40oC 0.99

(b) HP-OIT
-8
2.7 2.8 2.9 3.0 3.1 3.2 3.3

[1/Temperature] x 103 (K-1)

Figure 2. Arrhenius plot of OIT depletion for the textured GMB and its smooth edge (MxTA15 and
MxTsA15): (a) Std-OIT; (b) HP-OIT. Maximum and Minimum Ea for Std-OIT predictions were
calculated at 95% confidence interval.

2
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1.4

1.2 Smooth edge


Textured

Normalized HLMI (-)


1.0
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0.8

0.6

0.4

0.2

0.0
0 10 20 30 40

Incubation time (months)

Figure 3. Variation of normalized high load melt flow index (MIt/MIo) with incubation time for the

textured GMB and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3 at 85oC. The

solid line (smooth edge) coincides with the dashed line (textured). Error bars represent range of results.

3
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1.4

Normalized break strain- xMD (-)


1.2
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1.0

0.8

0.6

0.4
Smooth edge
0.2
Textured

0.0
0 10 20 30 40

Incubation time (months)


Figure 4. Variation of the normalized tensile break strain in cross machine direction with incubation time
for the textured GMB and its smooth edge (MxTA15 and MxTsA15) immersed in MSW Leachate 3 at
85oC. The solid line (smooth edge) coincides with the dashed line (textured). Error bars represent range of
results.

4
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70
(a)
60

Tensile stress (kN/m)


50

40
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30
Smooth edge-unnotched-virgin
o
Smooth edge-85 C-24months
20 o
Textured-S1-85 C-24months
o
Textured-S2-85 C-24months
10 Textured-virgin
Smooth edge-notched-virgin
0
0 50 100 150 200 250 300

Elongation (mm)

(b)

S1 S2

Figure 5. The effect of texturing on the break strength and elongation-cross machine direction in
tensile uniaxial test: (a) Stress-elongation; (b) Plane of failure.

5
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1.8
(a) 40oC Textured (b) 55oC Textured
1.6 Smooth edge Smooth edge
Normalized SCR (-) 1.4

1.2

1.0 ?
?
0.8

0.6

0.4

0.2

0.0
1.8
(c) 75oC Textured (d) 85oC Textured
1.6 Smooth edge Smooth edge
1.4
Normalized SCR (-)

1.2 ?
1.0

0.8
?
0.6

0.4 ?
0.2

0.0
0 10 20 30 40 0 10 20 30 40

Incubation time (months) Incubation time (months)

Figure 6. Variation of the normalized SCR-cross machine direction (SCRt/SCRo) with incubation time for the textured GMB and its smooth edge
(MxTA15 and MxTsA15) immersed in MSW Leachate 3: (a) 40oC; (b) 55oC; (c) 75oC; (d) 85oC.
Error bars represent range of results; Data points marked by (“?”) were excluded from interpretation.

6
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2
(a)
1

ln [normalized Std-OIT (-)]


-0

-1 T (oC) GMB Regression line equation


Smooth edge ln (OITt)=ln (185)-0.006×t
40
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Smooth roll ln (OITt)=ln (185)-0.01×t


-2 Smooth edge ln (OITt)=ln (185)-0.33×t
75
Smooth roll ln (OITt)=ln (185)-0.48×t
-3
o
Smooth edge-40 C
-4 o
Smooth roll-40 C
Smooth edge-75oC
-5
Smooth roll-75oC
-6
2
(b) T (oC) GMB Regression line equation
1 Smooth edge ln (OITt)=ln (185)-0.06×t
55
Smooth roll ln (OITt)=ln (185)-0.08×t
ln [normalized Std-OIT (-)]

Smooth edge ln (OITt)=ln (185)-1.07×t


-0 85
Smooth roll ln (OITt)=ln (185)-1.51×t

-1

-2

-3
o
Smooth edge-55 C
-4 Smooth roll-55oC
Smooth edge-85oC
-5
Smooth roll-85oC
-6
0 10 20 30 40

Incubation time (months)


Figure 7. Variation of the normalized Std-OIT (OITt/OITo) with incubation time for the smooth edge of
the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed in MSW Leachate 3: (a) 40 and
75oC; (b) 55 and 85oC.

7
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1.4

Smooth roll
1.2
Smooth edge
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Normalized HLMI (-)


1.0

0.8

0.6

0.4

0.2

0.0
0 10 20 30 40

Incubation time (months)

Figure 8. Variation of the normalized high load MFI (MIt/MIo) with incubation time for the smooth edge
of the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed in MSW Leachate 3 at 85oC.
The solid line (smooth edge) coincides with the dashed line (textured) in the incubation time interval 0 to
20 months. Error bars represent range of results.

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1.4

Normalized break strain- xMD (-)


1.2

1.0
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0.8

0.6

0.4
Smooth roll
0.2 Smooth edge

0.0
0 10 20 30 40

Incubation time (months)


Figure 9. Variation of the normalized tensile break strain - cross machine direction with incubation time
for the smooth edge of the textured GMB and the smooth roll (MxTsA15 and MxF15) immersed in MSW
Leachate 3 at 85oC. The solid line (smooth edge) coincides with the dashed line (smooth roll). Error bars
represent range of results.

9
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1.6
(a) 40oC Smooth edge (b) 55oC Smooth edge
1.4 Smooth roll Smooth roll

1.2
Normalized SCR (-)

?
1.0
?
0.8

0.6

0.4

0.2

0.0
1.6
(c) 75oC Smooth edge (d) 85oC Smooth edge
1.4 Smooth roll Smooth roll

1.2
Normalized SCR (-)

1.0 ?
0.8
?
0.6

0.4

0.2

0.0
0 10 20 30 40 0 10 20 30 40

Incubation time (months) Incubation time (months)

Figure10. Variation of the normalized SCR-cross machine direction (SCRt/SCRo) with incubation time for the smooth edge of the textured GMB
and the smooth roll (MxTsA15 and MxF15) immersed in MSW Leachate 3: (a) 40oC; (b) 55oC; (c) 75oC; (d) 85oC.
Error bars represent range of results; Data points marked by (?) were excluded from interpretation.
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