IEC TS 61244-1:2014

IEC TS 61244-1 ®
Edition 2.0 2014-08
TECHNICAL
SPECIFICATION
SPECIFICATION
TECHNIQUE
colour
inside
Determination of long-term radiation ageing in polymers –
Part 1: Techniques for monitoring diffusion-limited oxidation

Détermination du vieillissement à long terme sous rayonnement dans les
polymères –
Partie 1: Techniques pour contrôler l'oxydation limitée par diffusion

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IEC TS 61244-1 ®
Edition 2.0 2014-08
TECHNICAL
SPECIFICATION
SPECIFICATION
TECHNIQUE
colour
inside
Determination of long-term radiation ageing in polymers –

Part 1: Techniques for monitoring diffusion-limited oxidation

Détermination du vieillissement à long terme sous rayonnement dans les

polymères –
Partie 1: Techniques pour contrôler l'oxydation limitée par diffusion

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
X
CODE PRIX
ICS 17.240; 29.035.01 ISBN 978-2-8322-1827-3

– 2 – IEC TS 61244-1:2014 © IEC 2014
CONTENTS
FOREWORD. 4
INTRODUCTION . 6
1 Scope . 7
2 Profiling techniques to monitor diffusion-limited oxidation . 7
2.1 General . 7
2.2 Infra-red profiling techniques . 7
2.3 Modulus profiling . 10
2.4 Density profiling . 14
2.5 Miscellaneous profiling techniques . 16
3 Theoretical treatments of diffusion-limited oxidation . 18
4 Permeation measurements . 21
5 Oxygen consumption measurements . 21
6 Comparison of theory with experimental results . 22
7 Oxygen overpressure technique . 23
8 Summary . 25
Annex A (informative) Derivation of theoretical treatment of diffusion-limited oxidation . 26
A.1 General . 26
A.2 Numerical simulation . 29
A.3 Cylindrical and spherical geometries and simulation . 30
A.4 Time dependence of the simulation. 35
Bibliography . 37

Figure 1 – Relative oxidation as determined from the carbonyl absorbance versus
depth away from air-exposed surface of polyolefin material after ageing for 6 days at
100 °C (from [18]) . 8
Figure 2 – Depth distribution of carbonyl groups in irradiated (0,69 Gy/s) multilayer
samples composed of 4, 18, 27 and 44 films of 22 µm thickness . 9
Figure 3 – Micro-FTIR spectrophotometric determination of photoproduct and of
residual double-bond profiles in a SBR film photooxidized for 100 h . 10
Figure 4 – Schematic diagram of modulus profiling apparatus . 11
Figure 5 – Modulus profiles of 1,68 mm thick commercial fluoro elastomer samples
after air ageing at 5,49 kGy/h and 70 °C to the indicated radiation doses (from [15]) . 12
Figure 6 – Modulus profiles of 1,68 mm thick commercial fluoro elastomer samples
after air ageing at 0,90 kGy/h and 70 °C to the indicated radiation doses (from [15]) . 12
Figure 7 – Modulus profiles of 1,68 mm thick commercial fluoro elastomer samples
after air ageing at 0,14 kGy/h and 70 °C to the indicated radiation doses (from [15]) . 13
Figure 8 – Modulus profiles of 1,9 mm thick chloroprene rubber samples following
elevated temperature exposures in the presence of air at 150 °C, left plot, and 100 °C,
right plot (from [10]) . 13
Figure 9 – Experimental density profiles (crosses) for 0,302 cm (left) and 0,18 cm
(right) thick EPDM sheets after ageing at 6,65 kGy/h and 70 °C in airX-ray
microanalysis . 14
Figure 10 – Effect of total radiation dose on XMA profile for 2 mm thick EPDM sheet
irradiated at 1 kGy/h in air (from [24]) . 15

Figure 11 – XMA profiles of 1 mm thick EPDM sheets after thermal ageingin air (from
[24]) 16
Figure 12 – NMR self-diffusion coefficients versus distance away from sample surface
for low-density polyethylene samples after gamma-irradiation in air or vacuum at 0,6
Gy/sec for the indicated total doses (from [26]) . 17
Figure 13 – Chemiluminescence profile for a polypropylene material after gamma
irradiation in air to 0,05 MGy at 2 kGy/h (data from [30]) . 17
Figure 14 – Theoretical oxidation profiles for various values of α (indicated in the figure)
with β = 0,1 . 19
Figure 15 – Identical to Figure 14, except that β = 10 . 20
Figure 16 – Identical to Figure 14, except that β = 1 000 . 20
Figure 17 – Plot of α /(β + 1) versus β, where α denotes the value of integrated
c c
oxidation corresponding to 90 % (from [7, 23]) . 21
Figure 18 – Apparatus used for irradiation under pressurized oxygen conditions . 24
Figure 19 – Tensile elongation (left) and tensile strength (right) data for an EPR
material aged at the indicated high and low dose-rates in air and at high dose rate in
the pressurized oxygen apparatus of Figure 18. 25
Figure A.1 – Simplified kinetic scheme used to represent the oxidation of polymers
(from [44, 45]) . 26
Figure A.2 – Typical example of normalized concentration of oxygen for cylindrical
shape for β=0,01 from [46] . 31
Figure A.3 – Typical example of relative oxygen consumption for cylindrical shape for
β=0,01 from [46] . 31
Figure A.4 – Typical example of normalized concentration of oxygen for cylindrical
shape for β=100 from [46] . 32
Figure A.5 – Typical example of relative oxygen consumption for cylindrical shape for
β=100 [46] . 32
Figure A.6 – Typical example of normalized concentration of oxygen for spherical
shape for β=0,01 from [46] . 33
Figure A.7 – Typical example of relative oxygen consumption for spherical shape for
β=0,01 from [46] .
...