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Weathering degradation mechanisms of chlorinated PVC

Article in International Journal of Plastics Technology · December 2013

DOI: 10.1007/s12588-013-9052-x

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Int J Plast Technol
DOI 10.1007/s12588-013-9052-x
R E S E A R C H A RT I C L E

Weathering degradation mechanisms

of chlorinated PVC

N. Merah & A. Bazoune & A. Fazal & Z. Khan

Received: 7 December 2011 / Accepted: 28 August 2013

# Central Institute of Plastics Engineering & Technology 2013

Abstract This paper reports the effects of natural and accelerated artificial weathering on
the physical, chemical and mechanical properties of Chlorinated PVC (CPVC) pipe
material. Natural outdoor exposures were carried out for periods ranging from 2 weeks
to 18 months. The accelerated artificial weathering was conducted by exposing samples to
UV radiations for periods ranging from 100 to 3000 h. The tensile test results show that
natural and accelerated weathering had limited effects on the strength and stiffness of the
material. However, the fracture strain was noticeably reduced after natural weathering for
periods as low as 15 days and artificial UV exposure of 100 h. Physical examination of
specimens revealed that both types of weathering resulted in gradual discoloration of the
specimens. ATR-FTIR spectroscopy and UV–vis analyses of exposed surfaces showed that
the photoreaction responsible for degradation of CPVC is most likely dehydrochlorination.

Keywords CPVC pipes . Natural and artificial weathering . Degradation mechanisms .

Tensile properties . Physical and chemical properties

Introduction

Chlorinated-PVC is produced by post chlorination of PVC. The basic molecular

building blocks of the CPVC molecule are chlorine, derived from salt, and ethylene,
which comes from oil or natural gas. CPVC piping systems have been installed and
operated since 1959, and initial installations are still performing faultlessly (http://
www.ppfahome.org/cpvc/faqcpvc.html). The effect of adding more chlorine to the
PVC molecule is to primarily raise the glass transition temperature (Tg) of the base
resin from 95 °C to the 115–135 °C range [1, 2]. CPVC pipes like most other

N. Merah (*) : A. Bazoune : Z. Khan

Mechanical Engineering Department, King Fahd University of Petroleum and Minerals, Dhahran,
Saudi Arabia
e-mail: nesar@kfupm.edu.sa

A. Fazal
Center of Research Excellence in Petroleum Refining and Petrochemicals, Research Institute,
King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia
 Int J Plast Technol

thermoplastic pipes (with UV screens and heat stabilizers) show good weathering
resistance against normal outdoor exposure to sunlight and other natural weathering
agents. The degree of resistance to outdoor weathering however, depends on the local
ambient temperature and humidity conditions of specific geographical location.
Jakubowicz [3] concluded that the relative durability of PVC materials in different
outdoor exposures can be very different depending on the variation in UV radiation,
temperature, duration of wet periods, pollutants and other factors specific to a given
geographical location. The high intensity of solar radiation and the long period of
sunlight exposure, coupled with temperatures in excess of 50 °C during summer months,
are ingredients that can cause serious weathering related degradation of PVC and CPVC
pipes used in Saudi Arabia [4, 5]. The service life of plastics is reported to dramatically
reduce under such harsh conditions. The extent of degradation of the PVC pipe exposed
to outdoor weathering in Dhahran (Saudi Arabia) were compared to those exposed in
Florida [4]. The tensile strength of white PVC pipes exposed for 24 months in Dhahran
decreased by 43 % while an exposure of the same duration in Florida resulted in only a
26 % decrease [4]. Merah [5] has found that among the CPVC tensile properties that are
most affected by natural weathering is the fracture strain. The author reported a decrease
in the fracture strain of more than 20 % after 1 month outdoor exposure in Dhahran,
Saudi Arabia. The degradation in fracture toughness was found to be similar to that of
fracture strain but the yield strength and the modulus of elasticity were only marginally
affected by weathering [5]. Tong and White [6] found that photo-oxidation of crystalline
polymers may lead to chemi-crystallization, which can cause significant changes in the
residual stress distribution in the material. They noticed that the major change in the
residual stress occurs near the surface, which may explain why the tensile strength is not
affected by weathering.
The presence of oxygen and humidity has also been shown to induce changes in the
mechanical properties of PVC [7]. Summers and Rabinovitch [8] found that at the air
temperature of 26 °C to 36 °C the surface temperature of plastics exposed to sunlight can
reach as high as 60 °C for common plastics, depending on color and thickness, due to heat
build-up. The high temperature is known to significantly affect the weathering process of
polymer materials [9–11]. Exposure of PVC to natural weathering conditions for short
periods has also been reported to decrease the percentage elongation [11–15]. Yield
strength and modulus of elasticity of PVC have been shown to slightly increase initially
after short exposure periods, but decreased after extended weathering [12–15]. Discolor-
ation of the PVC pipes after exposure has been examined by Ragab and Alawi [12, 15].
The above literature review shows that while PVC has had its fair share of
weathering investigations, very limited work on the weathering of CPVC has been
published. In this paper, the effect of natural and artificial weathering on the physical,
chemical and tensile properties of Chlorinated-PVC is reported. The mechanisms
responsible for the degradation of the mechanical and physical properties are ex-
plored using single reflection ATR-FTIR and UV–vis spectra.

Experimental procedure

A number of tensile specimens were obtained from 4-in. schedule 80 pipes following
the procedure reported in earlier work [16, 17]. These specimens were exposed to
Int J Plast Technol

outdoor natural weathering in Dhahran (26° 32′ N, 50° 13′ E) in accordance with the
general guidelines of ASTM D1435-99 [18]. The specimens were placed on fixed
angle racks such that the area to be tested is facing south at an angle of 45° without
backing at about 1.0 m from a usually dusty concrete ground.. The weathered samples
were collected after exposure periods of 0.5, 1, 2, 3, 6, 9, 12 and 18 months and tested
to evaluate various mechanical, physical and chemical properties. The as-received
samples were also tested to provide the baseline data.
The UV exposure tests were carried out in the Q-Sun Xe-3-HS Xenon test
chambers equipped with 6,000 W borosilicate glass-filtered xenon arc filaments.
UV exposure was carried out at irradiance=0.5 W/m2; Humidity=40 % (Minimum);
Chamber Air temperature=40±3 °C; Black panel temperature=57±3 °C. The intensity
of radiation source was frequently checked with 340 nm radiometer.
A 50-kN Instron 5569 electromechanical material testing system was used for
tensile testing. The tensile tests were performed at room temperature according to the
ASTM Standard D638-01 [19] at a strain rate of 6×10−4 s−1 (5 mm/min). A 25-mm
extensometer was used to measure the strain.
Photographs of the exposed and unexposed specimen surfaces were taken using a
digital camera for natural and accelerated exposure conditions. Visual observation of
the specimens and analysis of the photographs are used to qualitatively describe the
change of specimen surface color due to exposure.
IR spectra were collected for as received and exposed CPVC samples using smart
orbit single reflection diamond ATR accessory with 32 scans collected at 4 cm−1
resolution. ATR accessory was inserted in a Thermo Scientific Nicolet™ 6700 FT-IR
spectrometer. Furthermore, the total reflectance (%R = diffuse + specular) of exposed
samples was determined using CMSE’s UV–vis spectrophotometer (Cary 5E)
equipped with an integrating sphere at a scan rate of 600 nm/min.

Results and discussion

Effect of natural weathering on mechanical properties

Table 1 provides the results of the tensile tests of the as received and naturally
weathered CPVC specimens. The table includes the average values of the tensile
properties (modulus of elasticity, E, tensile strength, σut, stress at fracture σf, and
fracture strain, εf) of CPVC pipe material for different natural exposure periods
ranging from 0 to 18 months. It also includes the number of tests for each condition
and standard deviations in the experimental data. These results show that the effect of
natural weathering on the tensile strength, the modulus of elasticity and the fracture
strength is marginal. This marginal effect of weathering on the strength and modulus
of CPVC pipe material was expected given that the degradation due to weathering is
mainly a surface phenomenon [5, 6].
The fracture strain however, experiences an abrupt reduction after 2 weeks of
outdoor exposure (Fig. 1). Despite the scatter in the experimental results, evidenced
by the reported standard deviation, on the average, around 20 % decrease in the
fracture strain is noted after 2 weeks of natural weathering. This reduction reaches
38 % after 1 month of natural exposure. The average value of the fracture strain
 Int J Plast Technol

Table 1 Tensile properties of CPVC for different outdoor exposure periods

Exposure No Tests E (MPa) STDV σut (MPa) STDV σf (MPa) STDV εf (%) STDV
Time (Months)

0 8 2871.0 260.9 47.0 1.0 41.2 1.4 21.3 4.3

0.5 4 2863.6 276.2 46.3 1.1 40.8 1.6 17.2 2.4
1 3 3302.1 26.3 48.1 0.8 47.9 0.7 13.2 1.4
2 4 2702.6 123.2 46.4 1.1 42.6 1.7 17.1 2.4
3 4 2989.6 251.3 47.9 0.7 44.1 1.2 16.4 1.5
6 4 2979.5 166.8 48.0 0.7 42.9 1.9 16.3 1.6
9 4 2817.6 145.4 46.8 0.6 46.4 0.9 12.8 2.0
12 4 2703.4 158.4 46.4 0.6 46.4 0.5 13.1 2.6
18 5 2879.7 184.4 47.1 0.8 44.1 1.3 14.1 1.7

remains almost constant afterwards. This initial decrease in the fracture strain is
consistent with that reported by several researchers for PVC and CPVC [5, 15, 20,
21]. As will be explained in the following section, the degradation in fracture strain is
believed to be caused by the predominant process of chain scission (breakdown of
polymer chain) at the specimen surface. This breakdown in the bonds of polymer
chain is caused mainly by UV [22]. Oxidation combined with physical ageing of the
polymer may have also contributed to this initial drop in the fracture strain due to
longer day light periods of radiant exposure and high temperature conditions of
Dhahran. As fracture strain is generally considered as a measure of material toughness,
its reduction also implies a degradation in toughness of CPVC pipe material. Merah [5]
showed that fracture toughness of the material decreased in a manner similar to that of
the fracture strain.

30

25
Strain at Fracture, %

20

15

10

0
0 2 4 6 8 10 12 14 16 18
Time, Months
Fig. 1 Variation of CPVC fracture strain with outdoor exposure time
Int J Plast Technol

Effect of natural weathering on physical and chemical properties

The photograph of the exposed and unexposed samples are provided in Fig. 2. As can be
seen from this figure the weathering effect on the color of the CPVC pipe material surface
starts at the period of 2 months of natural outdoor exposure. No noticeable color change
was observed below 2-months of natural exposure. Apparent loss of gloss and discolor-
ation of the specimen surface may have been induced by chain scissions originating from
radiation and temperature induced oxidation. The photographs in Fig. 2 show also that the
as-received specimen deformed plastically before failure while weathered specimens
experienced a rather brittle fracture. This is consistent with the reduction in fracture strain
indicated by the tensile testing results. A more quantitative analysis of the effects of natural
weathering on the material was performed using single reflection ATR-FTIR as well as
UV–vis Spectrophotoscopy for exposure periods of 3, 6 and 12 months.
The ATR-FTIR and UV–vis focused on changes in the absorption pattern in three main
regions: stretching vibration of the CH group between 2,800 and 3,100 cm−1, stretching
vibration of the C = C group between 1,560 and 1,650 cm−1and the C = O stretching
vibration between 1,690 and 1,750 cm−1. The IR absorption pattern characteristic of
alkene structures was observed for all the exposed samples at around 1,620 cm−1. The
spectral range 1,690 to 1,750 cm−1 shows characteristic carbonyl absorption bands for all
specimens. The IR spectra of selected regions for unexposed and natural outdoor exposed
CPVC samples over a period of 12 months are shown in Figs. 3 and 4.
It is observed that with outdoor exposure polyene and carbonyl formation increase. A
quantitative estimation of the two groups can be made by employing the following
relationships:
.
Polyene IndexðPI Þ ¼ A1620 −Abaseline A2920 −Abaseline
.
Carbonyl IndexðCI Þ ¼ A1724 −Abaseline A2920 −Abaseline

The results of the two indices are given in Table 2.

NT-12 Months

NT-06 Months

NT-03 Months

NT-02 Months

As Received

Fig. 2 Discoloring of specimen surface due to natural weathering

 Int J Plast Technol

Fig. 3 ATR-FTIRIR spectra of unexposed and outdoor exposed CPVC showing the CH stretching bands at
2,920 cm−1

The increase in polyne and carbonyl indices, PI and CI with the increase in the
outdoor exposure period are consistent with dehydrochlorination leading to polyenes
and photo-oxidation, respectively. Polyenes are formed with different conjugation
lengths, with some of them being oxidized [23]. The overall discoloration observed is
likely the result of both phenomena.

Degradation mechanisms

The first of the two mechanisms responsible for the overall discoloration of chlorinated
poly(vinyl)chloride, like poly(vinyl)chloride, is photo-discoloration, which is formation
of polyenes from a non-oxidative photochemical reaction. This reaction is accelerated
by UV and is mainly limited to surface. Second mechanism is photobleaching; photo-
oxidation of the polyenes formed by photo-discoloration [23]. Polyenes are formed in a
multistep photochemical reaction that is initiated by photolysis of C-Cl bond next to the

Fig. 4 ATR-FTIR spectra of unexposed and outdoor exposed CPVC showing the polyene and carbonyl
regions
Int J Plast Technol

Table 2 Polyene and carbonyl indices for outdoor exposed CPVC samples

Index type Exposure time in months

3 6 12

Polyene Index (PI) 0.16 0.35 1.2

Carbonyl Index (CI) 0.41 0.85 0.93

double bond shown in Eq. 1.

Photolysis of C-Cl bond
CH2 CH CH CH2 CH CH CH2 + Cl

Cl

(1)
Chlorine radical can abstract a hydrogen atom from the neighboring carbon as
expressed in Eq. 2:
Chain extension and formation of Hydrochloric acid

CH CH CH CH2 CH CH CH CH + HCl

(2)

With hydrogen abstraction by chlorine radical, extension of the length of conjugation is

obtained and hydrochloric acid is formed. The distribution of the polyenes conjugation
length is dependent on the spectral distribution of light source. With short wavelength
source (300–380 nm) short polyenes are formed. The sources with a spectrum closer to
the solar spectrum permit formation of the whole range of polyenes. These polyenic
sequences highly absorb in the UV-visible and are responsible for marked discoloration.
The extent of discoloration, among various factors, depends on the rate of photo-
oxidation of the polyenes. With very low permeability to oxygen, oxygen starvation
effects are expected to occur and the photo-oxidation of the polyenes is controlled by
oxygen diffusion [23]. In the presence of oxygen these polyenes are readily photo-
oxidized as shown in the mechanism by Hasegawa [24]. These oxidation photoproducts
such as aldehydes, carboxylic acids, absorb at short wavelength due to de-conjugation of
the system. The polyenyl radical shown in Scheme 1 may also recombine to form
crosslinking of the polymer chain (Scheme 2) [24].
UV-visible spectroscopy (UV–vis) is one of the most prominent methods used for
analyzing thermal degradation in polymers. In particular for PVC, UV–vis spectros-
copy is very useful because polyenes formed in the process of degradation selectively
absorb in the visible range and their wavelength of absorption depends on the length
of conjugated double bond sequence [25]. The reflectance spectra obtained using
UV–vis spectrophotometer of the CPVC samples where the total reflectance
(diffuse + specular) is expressed in %R, are given as a function of wavelength in Fig. 5.
 Int J Plast Technol

Scheme 1 Oxidation reaction resulting in the formation of carbonyl groups

Wavelengths ranging from 350 to 800 nm were considered and the total reflectance
(%R) was obtained for specimens exposed to outdoor weathering for 3, 6 and 12 months.
Lodi et al. [26] reported that 300–800 nm band includes high energy UV light and is
considered important in photo degradation. The visible light may also have an indepen-
dent or synergistic effect on materials photo degradation. The exposed surfaces of the
specimens were analyzed and the results of Fig. 5 show that the effect of exposure time
on the total reflectance of the specimen surface occurs in the visible range. The
maximum reflectance occurs around the 450 nm wavelength. The difference in %R
between the exposure periods of 3 months and longer exposure time is observed to
increase in the 500–800 nm bands. This reduced reflectance in the visible range is
believed to directly affect the color of the material chemicals and lead to the observed
color change seen in Fig. 2. Reflection usually occurs on the polymer surface and
degradation due to weathering can make a polymer lose its gloss [27].

Effect of artificial weathering on mechanical properties

Table 3 shows the average values of the tensile properties of CPVC pipe material for
different accelerated artificial exposure to UV radiation. The table also includes the
number of tests for each condition and standard deviations in the experimental data.
The results indicate that, similar to natural weathering, the effect of artificial accel-
erated weathering on the tensile strength, fracture strength and the modulus of
elasticity is marginal. The material however, looses 1/3 of its toughness (Fig. 6) after
only 100 h of exposure to UV. The fracture strain continues to decrease by about
40 % at the UV exposure of 300 h. Exposures at periods longer than 300 h appear to
cause less degradation and even recovery of the material toughness. The reason for

Scheme 2 Polyenyl radical recombination resulting in crosslinking

Int J Plast Technol

Fig. 5 Variation of the total reflectance of CPVC material after exposure to outdoor weather for a 3 months,
b 6 months and c 9 months

this recovery may be explained by heat induced material softening that could be
expected to occur with prolonged exposure to hot and humid weather. In general, the
reduction in fracture strain (embrittlement) is caused by oxidation brought about
by exposure to combined UV, heat (temperature 57 °C), oxygen and moisture
(RH=40 %) conditions. As explained above, dehydrochlorination is believed to
be the photoreaction responsible for degradation of CPVC toughness observed under
these conditions.
As can be seen from the comparison of photographs of exposed and unexposed
specimens (Fig. 7), discoloring of the CPVC samples surface after 100 h of UV
exposure is very light. A significant color change starts at the exposure period of
300 h by the gradual increase in the tanning of the specimen surface with the color
becoming brown (deep tan) at 3000 h. The observed loss of surface gloss and deep
tan may have been caused by oxidation produced mainly by the combination of UV
radiation, temperature and humidity. It should be noted that the loss of surface gloss
due to accelerated artificial weathering is more pronounced than that of natural
weathering causing more severe degradation translated by 33 % of reduction in
toughness for 100 h of exposure as compared to 20 % for ½ month natural exposure.

Table 3 UV effect on tensile properties of CPVC

Exposure time No tests E (MPa) STDV σut (MPa) STDV σf (MPa) STDV εf (%) STDV
(hours)

0 8 2871.0 260.9 47.0 1.0 41.2 1.4 21.3 4.3

100 6 2618.3 234.5 48.2 0.9 44.6 2.3 14.2 5.3
300 7 2626.2 181.6 48.0 1.3 42.3 0.7 12.5 2.9
1000 4 3035.0 345.4 47.2 1.3 44.4 2.4 15.1 4.2
3000 4 2742.3 396.8 48.3 1.1 15.3 5.7
 Int J Plast Technol

Fig. 6 Variation of CPVC ultimate elongation with UV exposure time

Conclusions

From the results reported in this paper the following conclusions can be drawn on the
effect of natural and artificial UV weathering on the CPVC pipe material:
& Both the natural outdoor and artificial accelerated UV exposures do not cause any
noticeable degradation in the tensile properties of the material except a lowering in
its fracture strain.
& A clear color change from bright grey to tan was observed after 3 months of
exposure. photo-oxidation with formation of polyenes and carbonyl groups, and
hydrochloronation are believed to be the two mechanisms responsible for the
degradation of CPVC material.
& Visual analysis of exposed specimens revealed that both types of exposures
resulted in the discoloration and loss of surface gloss of the CPVC pipe material

Fig. 7 Discoloring of CPVC specimen surface caused by UV

Int J Plast Technol

with artificial weathering producing a much pronounced deterioration evidenced

by the color change to a deep tan of the exposed surface.

Acknowledgments The authors thankfully acknowledge the support of King Fahd University of Petroleum
& Minerals (KFUPM) through funding of the project IN 080407. The authors would like to thank Dr. Avni A.
Argun from Chemical Engineering Department at MIT for performing the UV–vis photospectroscopy tests.

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