INTERNATIONAL ISO

STANDARD 10147

Second edition
2004-11-15

Pipes and fittings made of crosslinked

polyethylene (PE-X) — Estimation of the
degree of crosslinking by determination
of the gel content
Tubes et raccords en polyéthylène réticulé (PE-X) — Estimation du
degré de réticulation par le mesurage du taux de gel

Reference number
ISO 10147:2004(E)

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 ISO 10147:2004(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.

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Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 10147 was prepared by Technical Committee ISO/TC 138, Plastics pipes, fittings and valves for the
transport of fluids, Subcommittee SC 5, General properties of pipes, fittings and valves of plastic materials and
their accessories — Test methods and basic specifications.

This second edition cancels and replaces the first edition (ISO 10147:1994), which has been technically
revised.

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 INTERNATIONAL STANDARD ISO 10147:2004(E)

Pipes and fittings made of crosslinked polyethylene (PE-X) —

Estimation of the degree of crosslinking by determination of the
gel content

1 Scope
This International Standard specifies a method for the assessment of the degree of crosslinking in
polyethylene (PE-X) pipes and fittings by determination of the gel content by solvent extraction.

2 Principle
The mass of a test piece taken from a pipe or a fitting is measured before and after immersion of the test
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piece in a solvent for a specified period of time. The degree of crosslinking is expressed as the percentage by
mass of the insoluble material.

3 Solvent
3.1 Xylene, analytically pure, to which 1 % of antioxidant has been added [either 2,2-methylene-
bis(4-methyl-6-t-butylphenol) or 3-(3,5-di-t-butyl-4-hydroxyphenyl) propionate, or a combination of both].

WARNING — Xylene is a harmful and inflammable solvent that can be absorbed through the skin and,
as such, should be handled carefully. Attention is drawn to any relevant regulations and associated
exposure limits. Use only in a ventilated hood. Check the effectiveness of the hood before starting the
test. Do not inhale the vapour. Excessive inhalation of the vapour may cause dizziness, headache or
both. In the event of excessive vapour inhalation, seek fresh, clean air.

4 Apparatus
4.1 Reflux condenser, of the general type shown in Figure 1.

4.2 Round-bottomed flask, of at least 500 ml capacity.

NOTE A 2 000 ml flask is suitable for up to six determinations at one time.

4.3 Heating mantle, to fit the flask (4.2), and with sufficient heating capacity to boil xylene (boiling range:
138 °C to 144 °C).

4.4 Cage, with lid, large enough to contain a test piece (see Clause 5).

The cage shall be made of wire cloth or mesh, of aluminium or stainless steel, with a pore size of
(125 ± 25) µm. The wire cloth or mesh shall be free of grease, oil or other contaminants soluble in xylene. If
not, it shall be washed with acetone and dried before use.

4.5 Lathe with automatic feed, for machining out test pieces, or microtome or other suitable cutting
tool.

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Key
A identification tag and fine wire attached to cage G variable transformer
B reflux condenser H water outlet
C ring clamp I stand
D water inlet J xylene
E ground-glass joint or cork K heating mantle
F wide-necked round-bottomed flask L wire cage enclosing test piece

Figure 1 — Extraction apparatus

4.6 Vacuum oven or forced-ventilation oven, capable of maintaining the specified conditions (see 6.6).

4.7 Balance, capable of weighing the cage, with or without a test piece, to an accuracy of 1 mg.

5 Preparation of test pieces

Any protective layer on the pipe or test sample shall be removed prior to preparation of test pieces.

Each test piece shall comprise a slice or shaving having a thickness of (0,2 ± 0,02) mm, taken from a cross-
section of the pipe or fitting to include the full wall thickness round at least one circumference unless specified
otherwise by the referring standard. The mass of the test piece shall be W 0,2 g.

The degree of crosslinking can vary through the wall thickness of a pipe or fitting and therefore, for surface or
midwall measurements, test pieces shall be machined accordingly.

NOTE It is recommended that a lathe be used to machine test pieces from pipe. Alternatively, a microtome or other
suitable cutting tool may be used, and may be necessary for obtaining test pieces from fittings.

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6 Procedure
6.1 Weigh a clean, dry cage, including its lid (see 4.4), to an accuracy of 1 mg (mass m1).

6.2 Place a test piece in the cage and weigh the cage and test piece together to an accuracy of 1 mg
(mass m2).

6.3 Place the cage and test piece in the flask (4.2) and ensure that there is sufficient xylene solvent to
maintain total immersion and to provide a ratio by mass of solvent to test piece of at least 200:1.

6.4 Boil the solvent vigorously to ensure good agitation for 8 h ± 30 min.

6.5 Carefully remove the cage and the residue of the test piece from the solvent after the time specified in
6.4. If the residue can be easily separated from the cage, place the residue only in pure boiling xylene for
5 min. If the residue cannot be separated from the cage and lid, place the complete assembly in pure boiling
xylene for 5 min.

NOTE Take care when removing the cage from the boiling solution (see warning in 3.1).

6.6 Complete the drying of the residue, or cage, lid and residue, by placing them for at least 3 h in:

a) either a vacuum oven (see 4.6), kept at (90 ± 2) °C under a vacuum (negative pressure) of at least
0,85 bar (85 kPa) (i.e. approximately 0,15 bar absolute pressure or less);

b) or a forced-ventilation oven (see 4.6), with an adequate extraction facility, kept at (140 ± 2) °C.

6.7 After drying, allow to cool to ambient temperature and weigh the residue (mass m4), or cage, lid and
residue (mass m3), to an accuracy of 1 mg.

7 Calculation and expression of results

Calculate the degree of crosslinking, G, of the material in the test piece as the percentage by mass of the
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insoluble material, using one of the following equations, as appropriate:

when the residue only was weighed:

m4
G= × 100
m 2 − m1

when the cage, lid and residue were weighed:

m 3 − m1
G= × 100
m 2 − m1

where

m1 is the mass of the cage and lid, in milligrams;

m2 is the mass of the original test piece, the cage and the lid, in milligrams;

m3 is the mass of the residue, cage and lid, in milligrams;

m4 is the mass of the residue, in milligrams.

Express the result to the nearest whole number.

The mass of any filler present in the material shall be taken into account.

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8 Test report
The test report shall include the following information:

a) a reference to this International Standard;

b) all details necessary for identification of the test piece;

c) the degree of crosslinking, G, of the material in the test piece;

d) details of any variation in the specified procedure and of any abnormal behaviour observed during the
test;

e) the date of the test.

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 ISO 10147:2004(E)

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ICS 23.040.20; 23.040.45

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