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Accepted Manuscript

Evaluating the degree of gelation of PVC-U pipes. Comparison of currently available


methods

L.E. Pimentel Real, I.M. João, S.I. Pimenta, H.P. Diogo

PII: S0142-9418(18)30957-7
DOI: 10.1016/j.polymertesting.2018.08.001
Reference: POTE 5563

To appear in: Polymer Testing

Received Date: 18 June 2018

Accepted Date: 1 August 2018

Please cite this article as: L.E. Pimentel Real, I.M. João, S.I. Pimenta, H.P. Diogo, Evaluating the degree
of gelation of PVC-U pipes. Comparison of currently available methods, Polymer Testing (2018), doi:
10.1016/j.polymertesting.2018.08.001.

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ACCEPTED MANUSCRIPT
Test Method

Evaluating the degree of gelation of PVC-U pipes. Comparison of currently available


methods
*
L.E. Pimentel Reala ; I. M. Joãob,c; S. I. Pimentab; H. P. Diogod
a
Departamento de Materiais, Núcleo de Materiais Orgânicos, Laboratório Nacional de
Engenharia Civil, Av. do Brasil 101, 1700-066 Lisboa, Portugal

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b
Área Departamental de Engenharia Química, Instituto Superior de Engenharia de
Lisboa, IPL, Rua Conselheiro Emídio Navarro 1, 1959-007 Lisboa, Portugal

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c
CEG-IST, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais 1, 1049-
001 Lisboa

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d
Departamento de Engenharia Química , Centro de Química Estrutural, Instituto Superior
Técnico, Universidade de Lisboa, Av. Rovisco Pais 1, 1049-001 Lisboa

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1 Abstract
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Health and Safety policies have led to the recommendation of alternative tests to evaluate
the resistance to dichloromethane to estimate the degree of gelation of rigid PVC pipes
(PVC-U).
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In this work, we confirm that DSC is the best alternative method for evaluating the degree
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of gelation of rigid PVC pipes, using the relation between the enthalpy of fusion of primary
and secondary crystallites, which were measured from respective endotherms.
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The suitability of this method is established by comparison with experimental results


obtained with the test for determining the resistance to dichloromethane. Indeed, this
method has proven to be fairly reliable and is the only one that allows the quantification of
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the degree of gelation.


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Keywords: PVC-U; Degree of gelation; Dichloromethane; Differential scanning


calorimetry; Tensile properties.

*
: Corresponding author: Tel. +351 218443737; Fax 351 218 443 023; E-mail address:
lpimentel@lnec.pt
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2 Introduction

For several years, both the manufacturers of unplasticized poly(vinyl chloride) pipe
systems and the test laboratories have been facing problems with regard to the
performance of gelation tests on PVC-U pipes, due to the Safety & Health policies related
to use of dichloromethane (DCM); a solvent that has been traditionally employed for this
purpose [1]. Indeed, this substance is included in the Community Rolling Action Plan [2]

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and some uses of this substance have been restricted under REACH [3].

Moreover, this test may present some technical issues as regards DCM quality, chamfer

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preparation and the machining effect on pipes during the angular roughing. These issues
are due to the aspects as follows: the likely heat effect (as a result of friction), the

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inaccuracy in the quantification of the dichloromethane attack, as well as to the frequent
irregular geometry of the attacked zone(s) across the chamfer width. Lastly, it seems that

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the chemical attack of DCM is only observed on pipes with a degree of gelation just below
about 50%, which is confirmed in the present work.
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The latest versions of EN and EN ISO standards for PVC-U pipe systems [4-7], contain,
besides the dichloromethane resistance test (of which the results prevail in case of
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dispute), two alternative tests for determining the degree of gelation. Hence, the two tests
as follows can be adopted by the producer for carrying out factory production control, in
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compliance with the national regulations or the internal health and safety policies: the
uniaxial tensile test [8, 9] and the measurement of onset temperature (also known as
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characteristic temperature) by differential scanning calorimetry (DSC) [10].

Actually, the alternative test preferred is the tensile test, either due to it being more
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expedient or due to the test equipment being most commonly available in the laboratories
carrying out the quality control of plastic pipes. Nonetheless, despite the manufacturers’
preference, both the specification standards for pipes [4-7] and the test standard [8, 9],
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contain some requirements that are not universally satisfied by pipes for non-pressure
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applications (as will be addressed later in this article)

Moreover, the present work also shows that the method of preparation of tensile test
specimens may have a negative influence on the tensile elongation at break. This method
may introduce defects during machining, which are not intrinsic to the material, and which
may lead to premature failure.

These features contribute negatively to the adoption of the tensile method as a


preferential alternative method.
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The second alternative method proposed by ISO pipe standards is based on the
specification for ‘Onset temperature’, which establishes the limits Tonset ≥ 185°C for
PVC-U pressure pipes (EN ISO 1452-2) and Tonset ≥ 180°C for sewage PVC-U pipes
(EN ISO 1401-1, last revision).

The request for a value of onset temperature by DSC not less than 185 °C for PVC-U
pressure pipes also limits the adoption of ISO 18372-1 [10] as a valid method. Indeed, this
value may be higher for the new lead free formulations, which require a lower mass

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temperature to achieve a good gelation level [11], and thus it may not be adequate for all
PVC formulations.

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However, it is known that the degree of gelation of rigid PVC pipes can be assessed by
the relation between the enthalpy of fusion of primary and secondary crystallites, which

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are measured from respective endotherms by DSC, when the general principles
established in ISO 18372-2 [12] are adopted.

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In this work, the degree of gelation of rigid PVC pipes was evaluated using these different
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methods. This has made it possible to confirm that the method based on the relation
between the enthalpy of fusion of primary and secondary crystallites is the best alternative
method to DCM for this assessment.
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3 Experimental
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3.1 Materials
9 different PVC samples were prepared from rigid PVC pipes, both for water supply and
for buried and above-ground drainage and sewerage, with and without pressure [4-7]. All
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these samples were characterized by dichloromethane resistance tests and tensile


properties. However, only 5 of these samples were characterized by DSC.
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Some pipes, with a diameter less than 110 cm, which were used for tensile tests, were
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softly heated above glass transition temperature, near 95ºC, and then subjected to
pressure, so as to be flattened for specimen preparation.

The samples for DSC testing were extracted from the walls of the pipes by a hollow
punch, and afterwards were cut into layers (core, inner and outer surfaces) and cleaned
prior to testing.

All samples and test specimens were kept for at least 24h at a temperature of (23 ± 2) ºC
and a relative humidity of (50 ± 5) %.
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3.2 Performance under dichloromethane action
The dichloromethane resistance test is a qualitative evaluation performed in compliance
with standard ISO 9852 [1]. The specimens were previously chamfered and immersed in a
specific stainless-steel container equipped with a cooling system and an exhaust hood.

The collected samples (both DCM attacked and not attacked) were stored and,
subsequently, used for comparison with the results obtained from other alternative

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methods (traction and DSC).

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3.3 Tensile proprieties
Tensile specimens of type 1 of ISO 6952-2 [9] were prepared from 7 different samples,

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using 3 different machining conditions:

 A: manual machining with spindle, dye and milling cutter, without cooling;

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 B: computer numerical control (CNC), rotary milling machining;
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 C: automatic machining with spindle, dye and milling cutter, with cooling.

The tensile tests were carried out using a calibrated Universal Mechanical Testing
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Machine Instron, Model 4467, with a Class 0.5 30 kN load cell capacity. The tests were
performed using a test speed of 5 ± 1 mm/min in a conditioned room at a temperature of
(23 ± 2) ºC and a relative humidity of (50 ± 5) %.
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3.4 DSC characterization


DSC specimens were prepared from 5 different samples, which were selected from the
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ones used in the tensile and dichloromethane resistance tests.

The DSC specimens tested were previously weighed in a calibrated balance METTLER
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AE240 (R = ± 0,01 mg) and the DSC measurements were carried out using a temperature
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and enthalpy calibrated DSC 2920 MTDSC from TA Instruments. The calibration
procedure was as described elsewhere [13].

The scans were carried out in the range from 20ºC to 260ºC, at a heating rate of 25 ± 1
ºC/min1 and using 20 ± 5 ml/min of N2 as purging gas.

1
: A fast scan rate is used to prevent degradation of the PVC during the DSC test.
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DSC tests were performed on two specimens from each sample, which were extracted
from random points of the outer surface of the samples. A temperature of 230ºC was
selected as the upper limit for the integration of endotherm B.

4 Results and discussion

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4.1 Dichloromethane tests
The DCM attack of PVC-U pipes tested by this conventional method may occur on the

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whole zone of the chamfer that has been immersed in the dichloromethane or only in
certain disperse spots. In certain situations, when the degree of gelation is very low, a
generalized attack and consequent dissolution of PVC occurs, which leads to the

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formation of a paste (Figure 1).

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Figure 1
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The qualitative results of PVC-U resistance to dichloromethane are presented in Table 1.
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Table 1: Results of dichloromethane tests


Sample DCM result Sample DCM result Sample DCM result
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TL1 SA2 SC2


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TC5 Not attacked SA3 Attacked SL2 Not attacked

SA1 SC3 SL4


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4.1.1 Tensile tests


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Table 2 presents the results obtained in the tensile tests, including a reference to the
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method of preparation of test specimens, as well as the respective evaluation, by taking


into account both the elongation at break (≥ 80%) and the maximum stress (≥ 45MPa)
requirements established in the test standard [8-9] and in the specifications for PVC-U
pipes, fittings and system [4-7]. Table 2 also includes a reference to DCM results for
comparison purposes.

As can be seen in this table, some tensile results are inconclusive because, although the
yield stress are below the threshold value of acceptance criteria established in the
standards, they are very close and can be considered satisfactory by rounding since the
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expanded uncertainty of the test method is in the range of 0.4 MPa. There is also
evidence of contradictory results between tensile and dichloromethane resistance
acceptance criteria on some samples. Moreover, in some samples, inconsistency in the
strain at break between specimens belonging to the same sample is also evident, which
shows the influence of the machining conditions of the tensile test specimens on the
elongation at break.

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Table 2: Tensile proprieties of samples tested
Preparation Yield stress Strain at break

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Sample n Evaluation DCM result
method ± SD (MPa) ± SD (%)

TL1-1 6 A 49,1 ± 3,1 125 ± 17 Satisfactory

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Not attacked
TL1-2 4 A 44,5 ± 2,0 100 ± 14 Inconclusive

TC5-1 4 A 36,1 ± 3,2 32 ± 4 Not Satisfactory

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Not attacked
TC5-2 4 A 36,6 ± 3,5 32 ± 4 Not Satisfactory
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SA1 5 B 49,9 ± 1,1 186 ± 48 Satisfactory Not attacked
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SA2-1 5 A 52,1 ± 0,4 8±4 Not Satisfactory

SA2-2 5 B 48,2 ± 0,8 197 ± 17 Satisfactory Attacked


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SA2-3 3 B 49,7 ± 2,0 197 ± 46 Satisfactory


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SA3-1 5 A 50,1 ± 0,5 66 ± 10 Not Satisfactory

SA3-2 5 B 49,5 ± 0,3 119 ± 26 Satisfactory Attacked


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SA3-3 3 B 51,7 ± 0,9 138 ± 52 Satisfactory

SC3 5 B 37,9 ± 0,5 68 ± 15 Not Satisfactory Attacked


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SC2-1 5 A 40,7 ± 0,8 50 ± 12 Not Satisfactory


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SC2-2 5 B 39,1 ± 0,2 110 ± 20 Not Satisfactory Not attacked

SC2-3 4 B 44,3 ± 2,4 112 ± 53 Not Satisfactory

SL2-1 5 C 51,5 ± 2,3 112 ± 46 Satisfactory


Not attacked
SL2-2 3 C 52,9 ± 1,8 147 ± 31 Satisfactory

SL4-1 5 C 44,6 ± 0,4 161 ± 18 Inconclusive


Not attacked
SL4-2 5 C 44,7 ± 0,4 170 ± 19 Inconclusive
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4.2 DSC tests
Standard ISO 18373 [10], [12] includes figures illustrating typical DSC thermograms,
which show two endothermic peaks in DSC patterns of processed rigid PVC; a feature
that was identified for the first time by Gilbert and Vyvoda.[14].

Part 1 of the ISO standard, that is at the basis of the DSC method proposed for evaluating
the degree of gelation of PVC as an alternative to the DCM method, focuses on the onset

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temperature (or PVC “processing temperature”) located between the first endotherm (“A”),
attributed to the melting of secondary crystallites formed as a result of processing, and the
second endotherm (“B”), attributed to primary crystallites.

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Table 3 presents the results of the onset temperature obtained in the DSC method as well

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as the DCM results for comparison purposes.

As table 3 shows, the ‘Onset’ temperatures do not match the DCM results in all cases.
Actually, they give contradictory results for the two specimens tested from one sample

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(SA2), and lead to opposite acceptance criteria on both specimens tested from two other
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samples (SA1 and SC3).
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Table 3: Comparison of results of the ‘onset’ temperature determined by DSC and DCM tests
Sample Onset temperature (ºC) Acceptance criteria [10] DCM result
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SC2-1 187,4 Satisfactory


Not attacked
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SC2-2 189.4 Satisfactory

SA1-1 170,8 Not Satisfactory


Not attacked
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SA1-2 189,8 Satisfactory

SA2-1 186,3 Satisfactory


Attacked
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SA2-2 185,2 Satisfactory


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SA3-1 181,6 Not Satisfactory


Attacked
SA3-2 183,1 Not Satisfactory

SC3-1 186,0 Satisfactory


Attacked
SC3-2 180,7 Not Satisfactory

Part 2 of the same ISO standard allows for a measurement of the enthalpy for the smaller
of the two endotherms that are observed on a typical PVC DSC plot (“A”), but it does not
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establish a measurement procedure for obtaining the enthalpy for the second endotherm
(“B”).

Although some researchers [15, 16] propose a percent gelation calculation, which is
exclusively based on endotherm A, by comparing it with endotherm A for a 100 percent
∆ 2
gelled sample ( = 100) , and hence avoiding the uncertainty of the endpoint

determination of endotherm B, this method has not yet been well established.

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Nevertheless, several studies [15-20] have been published which describe a different
procedure for calculating the “percent gelation” of the PVC pipe material. This procedure

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consists of measurements of the enthalpy of both the lower and upper endotherms (“A”

and “B”) of the DSC thermogram ( = 100) and, therefore, it only requires one
∆ ∆

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scanning of PVC pipes, because the second endotherm is already present in processed
PVC pipes.

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Figure 2 shows a typical curve obtained by DSC, from which it is possible to calculate the
degree of gelation based on the enthalpy ratio of the lower and upper temperature
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endotherms ("A" and "B").Table 4 presents the degree of gelation calculated with this
method on all samples tested.
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Figure 2
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: When an endotherm for an 100 percent gelled sample is not available, a second scan of the
sample that has been heated to above the end of endotherm B temperature can be performed,
which yields a greater endotherm A, without endotherm B.
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Table 4: Comparison of the degree of gelation calculated by the enthalpy ratio and results of the DCM
test
Sample Δ (J/g) Δ (J/g) Degree of gelation (%) DCM result

SC2-1 3,820 1,2900 74,8


Not attacked
SC2-2 4,215 1,7910 70,2

SA1-1 2,390 0,3090 88,6


Not attacked

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SA1-2 3.448 0,2574 93,0

SA2-1 2,700 2,5880 51,1

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Attacked
SA2-2 2,285 3,0300 43,0

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SA3-1 2,412 4,0560 37,3
Attacked
SA3-2 3,218 3,177 50,3

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SC3-1 1,591 2,1990 42,0
Attacked
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SC3-2 2,266 2,9040 43,8
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As Table 4 shows, the degree of gelation calculated by the enthalpies of both the lower
and upper endotherms (“A” and “B”), are in agreement with the DCM results, hence
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confirming that the PVC withstands a dichloromethane attack below about 50% of the
degree of gelation.
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5 Conclusions
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It has been shown that the tensile method is not good enough for evaluating the degree of
gelation and cannot be considered as a preferential alternative method for replacing the
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dichloromethane resistance test, due to the following reasons:

 it does not always lead to results consistent with those obtained by the DCM
method;
 it can give contradictory results on different specimens of the same sample, which
shows that the method of preparation of tensile test specimens may have a
negative influence on the tensile elongation at break, probably due to the
introduction of defects by machining, which are not visible to the naked eye;
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 certain “good” PVC-U pipes are not able to present a yield stress in compliance
with the requirements established in the European standard EN ISO 3259-2 [9].

The specification standards [4-6] establish a different PVC content limit, and a reduction in
the maximum stress in the tensile test below 45 MPa is expected to occur, as the PVC
content is reduced and the CaCO3 content is increased. This has been demonstrated by a
study performed by Portuguese manufacturers, in which it was confirmed that the PVC-U

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pipes show an elongation at break above 110%, but presented reduced values of stress at
break, which are in compliance with the PVC content limit 3 . Although it is generally
accepted that calcium carbonate has a negative influence on the tensile strength, it is also

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known that this filler has little or negligible influence on both the gelation and the
performance of PVC-U pipes for non-pressure applications.

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Thus, the specification standards for pipes [4-7], as well the test standard ISO 6259 [8, 9]
contain some requirements that are not universally satisfied by pipes for non-pressure

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applications and, consequently, it is not possible to meet the mentioned requirements.
Therefore, the complementary test is no longer appropriate for such cases.
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It is also concluded that the same tensile specimens, prepared by methods A and B,
produce opposite results. This leads to the conclusion that method A may use deficient
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machining conditions, probably due to the lack of cooling fluid, which produces excessive
spot heating during machining of test specimens. This feature may lead to unsatisfactory
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results with erroneous evaluation of the material and final product . Therefore, when the
test results are unsatisfactory, further evaluation must be done so as to confirm whether
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the poor results are due to the preparation method.

On the other hand, the alternative methods to DCM, based on the determination of ‘Onset’
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temperatures by DSC, are also inadequate because the results do not always match the
DCM results. Nonetheless, the degree of gelation based on the enthalpy ratio of the lower
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and upper temperature endotherms ("A" and "B) is in agreement with the DCM results,
when the PVC shows a dichloromethane attack about 50% below the degree of gelation.
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At the outset, the DSC method could be considered to be less representative than the
tensile method, because it only gives the possibility of characterising small amounts of
samples collected on several parts of the pipe, which could lead to inconsistent
conclusions between the two methods under study, if different zones of the pipe were to
be analyzed. Nonetheless, despite this limitation, we were able to confirm that DSC is the

3
: According to these unpublished data from Portuguese manufacturers, it is possible to confirm a
reduction in the stress level, from a medium result of maximum stress, of 49MPa to 41MPa,
when the PVC content is reduced from 95% to 80%, by increasing filler (calcium carbonate).
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method with the greatest potential to estimate the percent gelation of the processed PVC
materials, due to its sensitivity and ability to describe crystallite melting in a quantitative
way (instead of only qualitative), hence displaying good agreement with the DCM test.
Additionally, since the thermal protocol is in a ramp (non-isothermal), the time to complete
a test is relatively short and it makes possible evaluation of either specific or localized
zones of the PVC-U pipe. The non-use of aggressive chemical agents is also an
advantage in terms of health and safety . Therefore, the inconsistent conclusions are

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mainly a consequence of the heterogeneous micro structure of the PVC-U pipe.

However, to consolidate these conclusions and to ensure the preferential adoption of the

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DSC method for gelation assessment of U-PVC pipes, some improvements must be
performed to increase the reproducibility and repeatability of the DSC method [16],

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particularly as regards some aspects that could be a significant source of errors. These
aspects refer to sampling procedures, sample inhomogeneity (due to poor mixing of
additives and/or poor processing, causing interference with the DSC curve due to

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spurious peaks), the possible degradation of PVC during DSC testing above 210ºC, and
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uncertainty in the determination of the endotherm endpoint.
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Acknowledgments
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The authors would like to thank the pipe manufacturers FERSIL and POLITEJO for their
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valuable support. The authors would also like to acknowledge the financial support of
LNEC in the scope of P2I research project "Behavior and performance of plastic products,
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polymer materials with recycled and bio-composites with application in construction


(ECOPOL)".
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References
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[1] EN ISO 9852:2017 - Unplasticized poly(vinyl chloride) (PVC-U) pipes -


Dichloromethane resistance at specified temperature (DCMT) - Test method (ISO
9852:2007)

[2] CORAP, Justification Document for the Selection of a CoRAP Substance, 2016,
available in https://echa.europa.eu/information-on-chemicals/evaluation/community-
rolling-action-plan/corap-table/-/dislist/details/0b0236e180b89717
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[3] Regulation (EC) No 1907/2006 of the European Parliament and of the Council on
the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH),
Official Journal of the European L 396, Volume 49, 30 December 2006 (with last
update of 10 January 2018), pp. 1-509, Brussels, 2006

[4] EN 1329-1:2014 - Plastics piping systems for soil and waste discharge (low and
high temperature) within the building structure - Unplasticized poly(vinyl chloride)
(PVC-U) - Part 1: Specifications for pipes, fittings and the system

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[5] EN 1401-1:2009 - Plastics piping systems for non-pressure underground drainage
and sewerage - Unplasticized poly(vinyl chloride) (PVC-U) - Part 1: Specifications

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for pipes, fittings and the system

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[6] EN ISO 1452-2:2009 - Plastics piping systems for water supply and for buried and
above-ground drainage and sewerage under pressure - Unplasticized poly(vinyl
chloride) (PVC-U) –Part 2: Pipes (ISO 1452-2:2009)

[7]

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EN 1453-1:2017/AC:2017 - Plastics piping systems with structured-wall pipes for
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soil and waste discharge (low and high temperature) inside buildings Unplasticized
poly(vinyl chloride) (PVC-U) Part 1: Specifications for pipes and the system
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[8] EN ISO 6259-1:2015 - Thermoplastics pipes - Determination of tensile properties -


Part 1: General test method (ISO 6259-1:2015)
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[9] ISO 6259-2:1997 - Thermoplastics pipes -- Determination of tensile properties --


Part 2: Pipes made of unplasticized poly(vinyl chloride) (PVC-U), chlorinated poly
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(vinyl chloride) (PVC-C) and high-impact poly (vinyl chloride) (PVC-HI)

[10] ISO 18373-1:2007 - Rigid PVC pipes -- Differential scanning calorimetry (DSC)
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method -- Part 1: Measurement of the processing temperature

[11] CASTILLO, J. L. - Longitudinal crack in large PVC-U pressure pipes. Pipe gelation
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influence. Case study discussion (I), Proceedings of the 18th Plastic Pipes
Conference PPXVIII, September 12-14, 2016, Berlin, Germany
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[12] ISO 18373-2:2008 - Rigid PVC pipes -- Differential scanning calorimetry (DSC)
method

[13] See for instance, the ref. MOURA RAMOS, J.J., TAVEIRA-MARQUES, R., DIOGO,
H.P. -- Estimation of the fragility index of indomethacin by DSC using the heating
and cooling rate dependency of the glass transition, Journal of Pharmaceutical
Sciences, 93 (6), 2004, pp. 1503-1507.)
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[14] GILBERT, M, VYVODA, J. C. -- Thermal analysis technique for investigating
gelation of rigid PVC compounds. Polymer, Vol. 22 (8), 1981, pp. 1134-1136

[15] TEH, J. H., COOPER, A. A., RUDIN, A., BATISTE, J. L. H – Interpretation of DSC
Measurements of the Degree of Fusion of Rigid PVC, Journal of Vinyl Technology,
Vol. 11 (1), 1989, pp. 33-41

[16] FILLOT, L.A., HAJJI, P., GAUTHIER, C. - U-PVC Gelation Level Assessment, Part

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2: Optimization of the Differential Scanning Calorimetry Technique, Journal of Vinyl
& Additive Technology, Vol, 12 (3)2006, pp. 108-114, DOI 10.1002/vnl.20078

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[17] VANSPEYBROECK, P., DEWILDE, A. Determination of the degree of gelation of
PVC-U using a DSC. Proceedings of the 12th Plastics Pipes Conference PPXII,

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2004, Baveno, Italy.

[18] FILLOT, L.A., GAUTHIER, C., HAJJI, P. - DSC technique: A powerful tool to
characterise PVC gelation. Proceedings of the 9th Int. PVC Conference., Brighton,
2005, pp. 425-437

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[19] FILLOT, L.A., HAJJI, P., GAUTHIER, C., VARLOT, K. M. - U-PVC Gelation Level
Assessment, Part 1: Comparison of Different Techniques, Journal of Vinyl &
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Additive Technology, Vol. 12 (3), 2006, pp. 98-107, DOI 10.1002/vnl.20077

[20] FUMIRE, J. - DSC-Gelation measurement: influence of Pipe-formulation on result,


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PVC Proceedings of the 13th Plastic Pipes Conference PPXIII, 2006, pp.
Washington, USA
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Figure 1: PVC-U pipes showing dichloromethane attack: a) attack on chamfer, around the whole perimeter
of the pipe; b) generalized attack and consequent dissolution of PVC, with the formation of a paste

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Figure 2: DSC thermogram for specimen 2 of sample SC2

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Evaluating the gelation degree of PVC-U pipes. Comparison between currently available methods

HIGHLIGHTS

The paper shows that both two alternative tests proposed in the last versions of EN and EN ISO
standards for evaluating gelation degree of PVC-U pipe systems are not the most appropriate to
replace the DCM test, due to several issues.

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The paper confirms that the chemical attack of DCM (which is the conventional adopted method in
the standards) is only observed on pipes with a gelation degree just below about 50%,

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The paper confirms that DSC is the best alternative method for evaluating the gelation degree of rigid
PVC pipes, using the relation between the enthalpy of fusion of primary and secondary crystallites,

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which were measured from respective endotherms.

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