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05.12.

2016

TEST REPORT Salzgitter Mannesmann Forschung GmbH


Standort Duisburg
Ehinger Straße 200
47259 Duisburg
Tel: +49 203 999-02
Fax: +49 203 999-4425

Report number E-Mail: info@du.szmf.de


Internet: www.szmf.de
SZMF-ED-PB-2016-0419

Report title

Testing of a 3-layer HDPE coating with Borealis Borcoat HE3450 top


coat and Borealis Borcoat ME0420 as adhesive layer (Borealis Poly-
olefin GmbH, WK 16_005, final report)

Date

December 5, 2016
Author

Dr. M. Betz

Distribution list print-version Distribution list PDF-version Keywords

Mr. T. Stark - Borealis ISO 21809-1, class B


Mr. D. Fedotov - Borealis DIN 30670
NF A49-710

Accreditation and certification note


Investigations presented in this report with respect to Eddy Current Testing, Flux Leakage Testing, Magnetic Particle Testing, Pene-
trant Testing, Radiographic Testing, Ultrasonic Testing were carried out by or supervised by Testing Personnel certified according to
DIN EN 473 or respectively DIN EN ISO 9712 level 3 and/or having an employer certificate according to SNT-TC-1A level III.
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Results / Summary

SZMF was assigned by Borealis Polyolefine GmbH to qualify a 3-layer polyethylene


coating with Borealis Borcoat HE3450 top coat and Borealis Borcoat ME0420 adhesive
to DIN EN ISO 21809-1:2011-10, DIN 30670:2012-04 and NF A49-710:1992-11.

All performed tests were clearly passed.

Signatures authors Head of department Head of division

Dr. M. Betz Dr. C. Bosch

This report may not be reproduced or transmitted, in whole or in part,


without the permission of the SZMF or the client.
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Contents
1  Introduction .......................................................................................................... 4 
2  Results ................................................................................................................. 4 
2.1  Elongation at break and tensile yield strength of
Borealis Borcoat ME0420 ............................................................................ 10 
2.2  Vicat softening temperature of Borealis Borcoat ME0420 ............................ 10 
2.3  Water content of Borealis Borcoat ME0420 ................................................. 11 
2.4  MFR of Borealis Borcoat Borcoat ME0420 ................................................... 11 
2.5  Density of Borealis Borcoat ME0420 ............................................................ 12 
2.6  Density of Borealis Borcoat HE3450 ............................................................ 12 
2.7  Elongation at break, tensile yield strength and tensile strength at break
of Borealis Borcoat HE3450 .......................................................................... 13 
2.8  Elongation at break of the extruded top layer of
Borealis Borcoat HE3450............................................................................. 14 
2.9  Vicat softening temperature of Borealis Borcoat HE3450 ............................ 14 
2.10  Water content of Borealis Borcoat HE3450............................................... 15 
2.11  Shore D hardness of Borealis Borcoat HE3450 ........................................ 16 
2.12  Environmental stress cracking resistance of Borealis Borcoat HE3450 .... 16 
2.13  OIT of Borealis Borcoat HE3450 ............................................................... 17 
2.14  Continuity according to ISO 21809-1 ........................................................ 19 
2.15  Degree of cure of the epoxy ...................................................................... 19 
2.16  Product stability during application of the PE top layer ............................. 19 
2.17  Impact strength & low temperature impact strength .................................. 20 
2.18  Indentation resistance of Borealis Borcoat HE3450 .................................. 20 
2.19  Peel strength ............................................................................................. 21 
2.20  Cathodic disbondment test........................................................................ 22 
2.21  Flexibility test ............................................................................................ 23 
2.22  Hot water immersion test .......................................................................... 24 
2.23  UV resistance on the basis of NF A49-710 ............................................... 25 
2.24  UV resistance according to ISO 21809-1 and DIN 30670 ......................... 27 
2.25  Thermal ageing according to NF A49-710 ................................................ 28 
2.26  Thermal ageing according to ISO 21809-1 and DIN 30670 ...................... 29 
2.27  Specific insulation resistance .................................................................... 30 
2.28  Resistance to microorganisms .................................................................. 31 

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Testing of a 3-layer HDPE coating

1 Introduction

SZMF was assigned by Borealis Polyolefine GmbH to qualify a 3-layer polyethylene


coating with Borealis Borcoat HE3450 top coat and Borealis Borcoat ME0420 adhe-
sive to DIN EN ISO 21809-1:2011-10, DIN 30670:2012-04 and NF A49-710:1992-11.
The setup of the coating is listed in Table 1. The tests for the complete coating sys-
tems were performed on specimens from a 4” pipe.

Table 1: Setup of the coating

FBE TEKNOS EP 8054-00


Adhesive Borealis Borcoat ME0420, batch 224590
Top coat Borealis Borcoat HE3450, batch 5150707

2 Results

The following Table 2, Table 3 and Table 4 give an overview of the results. The indi-
vidual test results and the exact test conditions can be found in the corresponding
subsections.

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Table 2: Test results for the adhesive material Borealis Borcoat ME0420

Test
Test Name Standard Requirement Results
Conditions
Specimen type
1A,
ISO 21809-1 compression
Elongation at break ≥600 % 745 %
ISO 527-2 moulded,
23±2 °C,
50 mm/min
Specimen type
1A,
Tensile yield ISO 21809-1 compression
≥8 MPa 11.8 MPa
strength ISO 527-2 moulded,
23±2 °C,
50 mm/min
ISO 21809-1
Vicat softening
DIN 30670 A/50 (9.8 N) ≥85 °C 100.2 °C
temperature
ISO 306
ISO 21809-1 ISO 15512
Water content ≤0.1 % 0.020 %
ISO 15512 Procedure B2
DIN 30670 1.0
MFR 190 °C, 2.16 kg -
ISO 1133-1 g/10 min
DIN 30670
ISO 1183-1 0.9305
Density NF A49-710 -
procedure A g/cm³
ISO 1183-1

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Testing of a 3-layer HDPE coating

Table 3: Test results for the HDPE top layer Borealis Borcoat HE3450

Test Require-
Test Name Standard Results
Conditions ment
ISO 21809-1
DIN 30670 ISO 1183-1 0.9458
Density ≥ 0.93 g/cm³
NF A49-710 procedure A g/cm³
ISO 1183-1
Specimen type
ISO 21809-1 1A, ISO 21809-1:
DIN 30670 compression ≥600 %
Elongation at break 719 %
NF A49-710 moulded, NF A49-710:
ISO 527-2 23±2 °C, ≥300 %
50 mm/min
Specimen type
1A,
ISO 21809-1
Tensile yield compression
DIN 30670 ≥ 15 MPa 19.9 MPa
strength moulded,
ISO 527-2
23±2 °C,
50 mm/min
Specimen type
1A,
Tensile strength at DIN 30670 compression
- 29.2 MPa
break ISO 527-2 moulded,
23±2 °C,
50 mm/min
Specimen type
ISO 21809-1
Elongation at break 5A,
DIN 30670
(extruded extruded, ≥400 % 597 %
NF A49-710
top layer) 23±2 °C,
ISO 527-2
25 mm/min
ISO 21809-1
Vicat softening
DIN 30670 A/50 (9.8 N) ≥110 °C 113.2 °C
temperature
ISO 306
ISO 21809-1
ISO 15512
Water content NF A49-710 ≤0.05 % 0.026 %
Procedure B2
ISO 15512
ISO 21809-1
Hardness Shore D DIN 30670 ≥ 55 57.5
ISO 868

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Table 3 (continued): Test results for the HDPE top layer Borealis Borcoat HE3450

Require-
Test Name Standard Test Conditions Results
ment
ISO 21809-1 50 °C, 1000 h, ≤ 50 % 0%
ESCR
ASTM D1693 Condition A failure failure
NF A49-710 50 °C, 100 h, ≤ 20 % 0%
ESCR
ASTM D1693 Condition A failure failure
ISO 21809-1
OIT DIN 30670 210 °C ≥30 min 54 min
ISO 11357-6
DIN 30670 0.5
MFR 190 °C, 2.16 kg -
ISO 1133-1 g/10 min

Table 4: Test results for the 3-layer HDPE coating

Test
Test Name Standard Requirement Results
Conditions
Free of defects, Free of defects,
discontinuities, discontinuities,
Continuity ISO 21809-1 delaminations, delaminations,
separations and separations and
holidays holidays
ISO 21809-1:
ISO 21809-1
Degree of cure ≤ 5 °C
DIN 30670 2.38 °C
of the epoxy Manufacturer:
NF A49-710
-2 °C≤∆Tg≤3 °C
Product stabil-
ity during ISO 21809-1
application of DIN 30670 190 °C, 2.16 kg ∆MFR≤20 % ∆MFR=0.6 %
the PE ISO 1133-1
top layer
ISO 21809-1
Impact strength DIN 30670 23±2 °C ≥ 7 J/mm > 7 J/mm
NF A49-710
Low tempera-
ture impact DIN 30670 -40±2 °C ≥ 7 J/mm > 7 J/mm
strength
Indentation NF A49-710 20±2 °C, 1 h ≤0.3 mm 0.052 mm
ISO 21809-1
Indentation 23±3 °C, 24 h ≤0.2 mm 0.070 mm
DIN 30670

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Testing of a 3-layer HDPE coating

Table 4 (continued): Test results for the 3-layer HDPE coating

Test
Test Name Standard Requirement Results
Conditions
Indentation NF A49-710 70±2 °C, 1 h ≤1.0 mm 0.173 mm
70±2 °C,
Indentation DIN 30670 ≤0.4 mm 0.222 mm
24 h
ISO 21809-1 80±2 °C,
Indentation ≤0.4 mm 0.238 mm
DIN 30670 24 h
Average
Peel strength ISO 21809-1 23±2 °C ≥442 N/cm
≥150 N/cm
Minimum
Peel strength DIN 30670 23±2 °C ≥ 400 N/cm
≥150 N/cm
Minimum
Peel strength NF A49-710 23±2 °C ≥ 400 N/cm
≥80 N/cm
Minimum
Peel strength DIN 30670 70±2 °C ≥ 149 N/cm
≥30 N/cm
DIN 30670 Minimum
Peel strength 70±2 °C ≥ 149 N/cm
NF A49-710 ≥20 N/cm
Average
Peel strength ISO 21809-1 80±2 °C ≥ 151 N/cm
≥30 N/cm
28 d,
Cathodic disbond- ISO 21809-1
20±2 °C, ≤7 mm 2.5 mm
ment DIN 30670
USCE=-1.5 V
24 h,
Cathodic disbond-
ISO 21809-1 65±3 °C, ≤7 mm 0.5 mm
ment
USCE=-3.5 V
28 d,
Cathodic disbond-
ISO 21809-1 80±3 °C, ≤15 mm 9.5 mm
ment
USCE=-1.5 V
7 d,
Cathodic disbond-
NF A49-710 40±2 °C, ≤10 mm 2.1 mm
ment
USCE=-1.5 V
2 d,
Cathodic disbond-
DIN 30670 60±2 °C, ≤7 mm 2.2 mm
ment
USCE=-1.5 V
No cracking/
Flexibility ISO 21809-1 0 °C, α=2.0° No cracking
holidays
20±2 °C, No cracking/ No cracking/
Flexibility NF A49-710
=2.5% holidays holidays

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Table 4 (continued): Test results for the 3-layer HDPE coating

Test
Test Name Standard Requirement Results
Conditions
Delamination:
Hot water immersion 80±3 °C, Average ≤2 No loss of
ISO 21809-1
test 48 h mm adhesion
Max. ≤3 mm
NF A49-710
UV resistance 800 h ∆MFR≤25 % ∆MFR=3.7 %
ISO 4892-2
NF A49-710
UV resistance 800 h ∆B < 50 % ∆B < 1 %
ISO 4892-2
ISO 21809-1
UV resistance DIN 30670 7 GJ/m² ∆MFR≤35 % ∆MFR=6.1 %
ISO 4892-2
ISO 21809-1 4800 h,
Thermal ageing ∆MFR≤35 % ∆MFR=9.1 %
DIN 30670 100±2 °C
1000 h,
Thermal ageing NF A49-710 ∆MFR≤25 % ∆MFR=3.6 %
100±2 °C
Specific insulation DIN 30670 100 d, 8 ≥ 1.69*1013
≥ 10 m²
resistance NF A49-710 23±2 °C m²
Peel strength
Resistance against 6 months ≥ 84 %
NF A49-710 ≥ 80 % of ini-
microorganisms burying (≥ 376 N/cm)
tial value

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Testing of a 3-layer HDPE coating

2.1 Elongation at break and tensile yield strength of


Borealis Borcoat ME0420

10 compression moulded specimens of type 1A were tested according to ISO 527-2


at 23±2 °C and 50 % relative humidity (Table 5). The speed of testing was 50
mm/min and the thickness of the specimens was 3.34–3.57 mm.

Table 5: Tensile test results for Borealis Borcoat ME0420

Specimen no. Elongation at break / % Tensile yield strength / MPa


1 830 11.9
2 680 11.7
3 710 11.8
4 830 11.8
5 810 11.7
6 570 11.8
7 830 11.7
8 720 11.8
9 670 12.0
10 800 11.7
Average 745 11.8
Standard deviation 84 0.1

2.2 Vicat softening temperature of Borealis Borcoat ME0420

Vicat softening temperature was determined to ISO 306 procedure A on specimens


according to paragraph 5.1 of ISO 306. The start temperature was 29 °C, holding
time 5 min, temperature gradient 50 K/h and the applied load was 1019 g. The re-
sults are summarized in Table 6.

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Table 6: Vicat softening temperature for Borealis Borcoat ME0420

Specimen no. Thickness Target Achieved Vicat softening


/mm penetration penetration temperature /°C
/mm /mm
1 3.60 1.00 1.00 100.3
2 3.62 1.00 1.00 100.6
3 3.57 1.00 1.00 99.7
Average 3.60 100.2
Standard 0.03
0.4
deviation

2.3 Water content of Borealis Borcoat ME0420

Water content was determined to DIN EN ISO 15512 procedure B2 and the results
are listed in Table 7.

Table 7: Water content of Borealis Borcoat ME0420

Measurement Water content / %


1 0.019
2 0.020
Average 0.020

2.4 MFR of Borealis Borcoat Borcoat ME0420

MFR was determined to ISO 1133-1 procedure A at 190 °C with a load of 2.16 kg
and a cut-off interval of 180 s. The results are listed in Table 8.

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Testing of a 3-layer HDPE coating

Table 8: MFR190/2.16 of Borealis Borcoat ME0420

Measurement Weight / g MFR /g/10min


1 0.3034 1.011
2 0.2965 0.988
3 0.2946 0.982
Average 0.2982 0.994
Standard deviation 0.0038 0.012

2.5 Density of Borealis Borcoat ME0420

Density was determined to DIN EN ISO 1183-1 procedure A with deionised water at
23.0 °C on 3 specimens. The results are listed in Table 9.

Table 9: Density of Borealis Borcoat ME0420

Specimen no. Density /g/cm³


1 0.9296
2 0.9296
3 0.9324
Average 0.9305
Standard deviation 0.0013

2.6 Density of Borealis Borcoat HE3450

Density was determined to DIN EN ISO 1183-1 procedure A with deionised water at
23.0 °C on 4 specimens. The results are listed in Table 10.

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Table 10: Density of Borealis Borcoat HE3450

Specimen no. Density /g/cm³


1 0.9422
2 0.9478
3 0.9491
4 0.9440
Average 0.9458
Standard deviation 0.0028

2.7 Elongation at break, tensile yield strength and tensile


strength at break of Borealis Borcoat HE3450

10 compression moulded specimens of type 1A were tested according to ISO 527-2


at 23±2 °C and 50 % relative humidity (Table 11). The speed of testing was 50
mm/min and the thickness of the specimens was 3.44–3.59 mm.

Table 11: Tensile test results for Borealis Borcoat HE3450

Specimen Elongation at Tensile yield Tensile strength at


no. break / % strength / MPa break / MPa
1 740 20.1 30.7
2 690 19.9 28.0
3 730 20.0 30.5
4 760 19.9 30.6
5 740 19.8 31.3
6 620 19.9 22.3
7 750 19.9 31.3
8 700 19.9 29.6
9 860 20.0 33.8
10 600 20.0 23.6
Average 719 19.9 29.2
Standard
70 0.1 3.4
deviation

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Testing of a 3-layer HDPE coating

2.8 Elongation at break of the extruded top layer of


Borealis Borcoat HE3450

7 specimens of type 5A with a thickness of 2 mm were prepared from the extruded


top layer and were tested according to ISO 527-2 at 23±2 °C and 50 % relative hu-
midity (Table 12). The speed of testing was 25 mm/min, as requested in DIN 30670
Annex F.

Table 12: Tensile test results for Borealis Borcoat HE3450

Specimen no. Elongation at break / %


1 560
2 640
3 530
4 650
5 610
6 600
7 590
Average 597
Standard
39
deviation

2.9 Vicat softening temperature of Borealis Borcoat HE3450

Vicat softening temperature was determined to ISO 306 procedure A. The start tem-
perature was 29 °C, holding time 5 min, temperature gradient 50 K/h and the applied
load was 1019 g. The results are summarized in Table 13.

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Table 13: Vicat softening temperature for Borealis Borcoat HE3450

Specimen no. Thickness Target Achieved Vicat softening


/mm penetration penetration temperature /°C
/mm /mm
1 3.48 1.00 1.00 112.7
2 3.45 1.00 1.00 113.3
3 3.52 1.00 1.00 113.7
Average 113.2
Standard
0.4
deviation

2.10 Water content of Borealis Borcoat HE3450

Water content was determined to DIN EN ISO 15512 procedure B2 and the results
are listed in Table 14.

Table 14: Water content of Borealis Borcoat HE3450

Measurement Water content / %


1 0.025
2 0.027
Average 0.026

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Testing of a 3-layer HDPE coating

2.11 Shore D hardness of Borealis Borcoat HE3450

Shore D hardness was measured to DIN EN ISO 868 at 23 °C with a meter reading
time of 15 s. The results are listed in Table 15.

Table 15: Shore D hardness of Borealis Borcoat HE3450

Measurement Shore D hardness


1 56.4
2 56.5
3 58.0
4 57.8
5 57.1
6 56.2
7 58.2
8 58.2
9 58.1
10 58.1
Average 57.5
Standard deviation 0.8

2.12 Environmental stress cracking resistance of


Borealis Borcoat HE3450

A test sheet of Borealis Borcoat HE3450 was moulded in accordance with procedure
C of Annex A1 of practice ASTM D 4703 and conditioned in accordance with the pro-
cedure A of ASTM D 618.

Ten specimens were cut from the sheet to the dimensions given in ASTM D 1693
Fig. 2 and Table 1, condition A. Each one got a controlled notch on one surface. The
specimens were bent into a holder and the holder was inserted in the test tube with
the reagent.

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The test conditions were as follows:

Reagent: 10 weight-% IGEPAL® CO-630 (SIGMA-ALDRICH)


Synonym: Polyoxyethylene(9)nonylphenylether, branched
Average molecular weight: 617 g/mol
Test temperature: 50 °C  0.5 °C
Duration of the test: 1000 h

For Borealis Borcoat HE3450 0 % of the specimens failed while testing for 1000 h.
Borealis Borcoat HE3450 clearly passed the test for 1000 h.

2.13 OIT of Borealis Borcoat HE3450

The oxygen induction time (OIT) of Borealis Borcoat HE3450 was performed accord-
ing to ISO 11357-6. The flow of nitrogen respectively oxygen was 20 ml/min and the
temperature was kept constant at 210 °C during the measurement. For evaluation
the tangent method according to ISO 11357-6 was used. The results are listed in
Table 16 and can be seen in Figure 1.

Table 16: OIT of Borealis Borcoat HE3450

Measurement weight of sample /mg OIT / min


1 5.46 54.1
2 5.80 53.9
Average 54.0

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Testing of a 3-layer HDPE coating

Figure 1: OIT of Borealis Borcoat HE3450

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2.14 Continuity according to ISO 21809-1

A visual inspection of the coating came to the result that the coating is free of de-
fects, discontinuities, delaminations and separations. A holiday test was performed to
ISO 21809-1 Annex B (average total layer thickness: 4.9 mm) at 25 kV. No holidays
were detected.

2.15 Degree of cure of the epoxy

The degree of cure of the epoxy was determined according to ISO 21809-1
Annex D / DIN 30670 Annex B and the results are presented in Table 17.

Table 17: Degree of cure to ISO 21809-1 Annex D

Tg3 Tg4 ∆Tg


99.95 °C 102.33 °C 2.38 °C

2.16 Product stability during application of the PE top layer

The melt flow index MFR190/2.16 was measured before and after extrusion of Borealis
Borcoat HE3450 (Table 18) according to ISO 1133-1 procedure A.

Table 18: MFR190/2.16 before and after extrusion of Borealis Borcoat HE3450,
cut-off interval: 180 s

MFR190/2.16 /g/10min
Measurement MFR/%
before extrusion after extrusion
1 0.502 0.502
2 0.499 0.496
3 0.502 0.495
Average 0.501 0.498 0.6
Standard
0.001 0.003
deviation

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Testing of a 3-layer HDPE coating

2.17 Impact strength & low temperature impact strength

Testing was carried out on cut plates, which were supported with a wooden base as
described in CSA Z245.20. The impacts were performed with a hard steel punch with
a hemispherical head (diameter 25 mm) and a distance of about 50 mm between the
impacts. In Table 19 the results of the impact tests are summarized.

Table 19: Impact testing

Coating
Tem- Drop Drop Impact Holi-
Speci- Im- thick-
perature height weight strength days
men pacts ness
/ °C /m / kg / J/mm (25 kV)
/ mm
Pl. 1 23±2 °C 3 1.0 4.029 8.1 4.9 0
Pl. 2 23±2 °C 3 1.0 4.029 8.1 4.9 0
Pl. 3 23±2 °C 3 1.0 4.029 8.2 4.8 0
Pl. 4 23±2 °C 3 1.0 4.029 8.1 4.9 0
Pl. 5 -40±2 °C 2 1.0 4.029 7.8 5.1 0
Pl. 6 -40±2 °C 2 1.0 4.029 7.9 5.0 0
Pl. 7 -40±2 °C 3 1.0 4.029 7.9 5.0 0
Pl. 8 -40±2 °C 3 1.0 4.029 8.1 4.9 0

2.18 Indentation resistance of Borealis Borcoat HE3450

For the test temperatures 23±3 °C, 70±2 °C and 80±2 °C tempering of the specimens
was performed with water. The thickness of the specimens was about 2 mm and the
diameter of the used indenter was 1.8±0.05 mm with a cross-sectional area of
2.5 mm². The applied force was 25±0.5 N. Indentation was determined with a dial
gauge with an accuracy of ±0.003 mm. The individual results are given in Table 20
and the average indentations of 3 specimens are listed in Table 21.

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Table 20: Individual results of indentation resistance tests

sample no. temperature / °C time / h indentation / mm


1 23±3 1 0.058
2 23±3 1 0.049
3 23±3 1 0.048
1 23±3 24 0.078
2 23±3 24 0.069
3 23±3 24 0.064
1 70±2 1 0.167
2 70±2 1 0.210
3 70±2 1 0.141
1 70±2 24 0.214
2 70±2 24 0.254
3 70±2 24 0.199
1 80±2 24 0.231
2 80±2 24 0.239
3 80±2 24 0.244

Table 21: Average results for indentation resistance

temperature / °C time / h indentation / mm Standard deviation / mm


23±3 1 0.052 0.004
23±3 24 0.070 0.006
70±2 1 0.173 0.028
70±2 24 0.222 0.023
80±2 24 0.238 0.005

2.19 Peel strength

Peel strength was measured with a tensile testing machine at a constant rate of pull
of 10 mm/min. The width of the coating strips, which were peeled off, was about
20 mm. For determination of the peel strength the exact width was considered. The
results are summarized in Table 22. As required in ISO 21809-1, no single recorded
peeling value is 30 % below the requirement.

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Testing of a 3-layer HDPE coating

Table 22: Peel strength at different temperatures

Measurement T/°C Min. peel Average peel Separation


strength /N/cm strength /N/cm
1 23±2 400 442 Adhesive:Adhesive
2 23±2 412 445 Adhesive:Adhesive
3 23±2 434 451 Adhesive:Adhesive
1 70±2 149 151 Adhesive:Adhesive
2 70±2 212 214 Adhesive:Adhesive
3 70±2 168 171 Adhesive:Adhesive
1 80±2 144 155 Adhesive:Adhesive
2 80±2 148 159 Adhesive:Adhesive
3 80±2 146 151 Adhesive:Adhesive

2.20 Cathodic disbondment test

The test conditions are listed in Table 23 and the results can be found in
Table 24 to Table 28.

Table 23: Test conditions

Electrolyte: 3 % NaCl
Drill: 6 mm
Reference electrode: Ag/AgCl, saturated KCl electrolyte
Heating for tests above room temp.: Oven

Table 24: Test results for 28 d CD test at 23±3 °C, USCE = -1.50 V

Specimen Max. disbondment radius / mm Av. disbondment radius / mm


1 4.4 2.7
2 3.3 2.5
3 2.5 2.2
Average 3.4 2.5

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Table 25: Test results for 24 h CD test at 65±3 °C, USCE = -3.50 V

Specimen Max. disbondment radius / mm Av. disbondment radius / mm


1 0.5 0.3
2 0.8 0.5
3 0.9 0.7
Average 0.7 0.5

Table 26: Test results for 7 d CD test at 40±2 °C, USCE = -1.50 V

Specimen Max. disbondment radius / mm Av. disbondment radius / mm


1 2.1 1.9
2 2.4 2.2
3 2.6 2.3
Average 2.4 2.1

Table 27: Test results for 2 d CD test at 60±2 °C, USCE = -1.50 V

Specimen Max. disbondment radius / mm Av. disbondment radius / mm


1 3.3 2.8
2 3.1 2.0
3 2.1 1.8
Average 2.8 2.2

Table 28: Test results for 28 d CD test at 80±3 °C, USCE = -1.50 V

Specimen Max. disbondment radius / mm Av. disbondment radius / mm


1 11.6 9.7
2 10.0 9.2
3 11.3 9.6
Average 11.0 9.5

2.21 Flexibility test

Based on the sample dimensions the mandrel radius was calculated to give the re-
quired bend. Additionally the bend of the specimens was measured and bending was

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Testing of a 3-layer HDPE coating

stopped when the required bend was reached. Details of the flexibility test to
ISO 21809-1 can be found in Table 29 and of the flexibility test to NF A49-710 in Ta-
ble 30.

Table 29: Flexibility test to ISO 21809-1, 0 °C, mandrel radius 214 mm,  = 2.0 °

Cracks Holiday test


Specimen Coating thickness / mm
yes/no (25 kV)
1 4.7–5.2 no no
2 4.8–5.5 no no
3 4.8–5.3 no no

Table 30: Flexibility test to NF A49-710, 23±3 °C, mandrel radius 153 mm,  = 2.5 %

Cracks Holiday test


Specimen Coating thickness / mm
yes/no (25 kV)
1 4.7–5.3 no no
2 4.9–5.5 no no
3 4.9–5.5 no no

2.22 Hot water immersion test

3 specimens were completely immersed in 80±3 °C hot deionised water for 48 h. Af-
ter hot water immersion the specimens were cooled down to room temperature and
were inspected for loss of adhesion at borders and edges. No loss of adhesion was
detected (Figure 2 and Figure 3) hence the test is passed.

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Figure 2: Side 1 of the specimens after hot water immersion

Figure 3: Side 2 of the specimens after hot water immersion

2.23 UV resistance on the basis of NF A49-710

Specimens of extruded Borealis Borcoat HE3450 with a thickness of about 2 mm


were exposed to UV light in a Q-SUN Xe-3-HSC from Q-Lab under the conditions
summarized in Table 31 for 800 h. The chosen test conditions correspond to
ISO 4892-2 and are harsher than the conditions requested by NF A49-710.
MFR190/2.16 of the 3 specimens was determined after UV ageing to ISO 1133-1 pro-
cedure A and was compared to the initial value (Table 32). From 6 specimens tensile

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test specimens of type 5A to ISO 527-2 were cut and the results of the tensile tests
are listed in Table 33.

Table 31: Detailed test conditions for UV ageing (corresponding to ISO 4892-2)

Black standard temperature 65 ± 3 °C


Relative humidity 65 ± 5 %
Chamber temperature 38 ± 3 °C
Irradiance @340 nm 0.51±0.02 W/m²*nm
18 min ± 0.5 min spray
Cycle
102 min ± 0.5 min dry

Table 32: MFR190/2.16 after UV ageing and comparison to


initial value (MFR190/2.16= 0.498 g/10min), cut-off interval: 180 s

MFR190/2.16 /g/10 min


Specimen Measurement Measurement Measurement MFI/%
Average
1 2 3
1 0.487 0.488 0.488 0.487 2.0
2 0.472 0.476 0.469 0.472 5.1
3 0.479 0.476 0.478 0.477 4.0
Average 3.7

Table 33: Tensile testing at 23±2 °C and 50 % relative humidity after UV ageing and
comparison to initial elongation at break (B = 597 %)

Specimen no. Elongation at break / % ∆B / %


1 590
2 640
3 650
4 630
5 520
6 550
Average 597 <1
Standard
48
deviation

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2.24 UV resistance according to ISO 21809-1 and DIN 30670

3 specimens of extruded Borealis Borcoat HE3450 with a thickness of about 2 mm


were exposed to UV light in a Q-SUN Xe-3-HSC from Q-Lab under the conditions
summarized in Table 31. The irradiation of 7 GJ/m² was achieved after test duration
of 2210 h. MFR190/2.16 of the 3 specimens was determined to ISO 1133-1 procedure A
after UV ageing and was compared to the initial value (Table 34). 6 tensile test
specimens of type 5A to ISO 527-2 were cut and the results of the tensile tests are
listed in Table 35.

Table 34: MFR190/2.16 after UV ageing and comparison to


initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 /g/10 min


Specimen Measurement Measurement Measurement MFI/%
Average
1 2 3
1 0.477 0.471 0.471 0.473 5.0
2 0.469 0.467 0.465 0.467 6.2
3 0.465 0.464 0.461 0.463 7.0
Average 6.1

Table 35: Tensile testing at 23±2 °C and 50 % relative humidity after UV ageing and
comparison to initial elongation at break (B = 597 %)

Specimen no. Elongation at break / % ∆B / %


1 590
2 600
3 600
4 590
5 590
6 590
Average 593 0.7
Standard
5
deviation

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Testing of a 3-layer HDPE coating

2.25 Thermal ageing according to NF A49-710

3 specimens of extruded Borealis Borcoat HE3450 with a thickness of about 2 mm


were exposed for 1000 h at 100±2 °C in a circulating air oven. MFR190/2.16 of the 3
specimens was determined to ISO 1133-1 procedure A after thermal ageing and was
compared to the initial value (Table 36). From 5 specimens tensile test specimens of
type 5A to ISO 527-2 were cut and the results of the tensile tests are listed in
Table 37.

Table 36: MFR190/2.16 after 1000 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 /g/10 min


Specimen Measurement Measurement Measurement MFI/%
Average
1 2 3
1 0.479 0.479 0.479 0.479 3.7
2 0.473 0.484 0.471 0.476 4.4
3 0.485 0.485 0.484 0.484 2.6
Average 3.6

Table 37: Tensile testing at 23±2 °C and 50 % relative humidity after thermal ageing
and comparison to initial elongation at break (B = 597 %)

Specimen no. Elongation at break / % ∆B / %


1 620
2 630
3 610
4 620
5 500
Average 596 <1
Standard
48
deviation

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2.26 Thermal ageing according to ISO 21809-1 and DIN 30670

Extruded Borealis Borcoat HE3450 with a thickness of about 2 mm was exposed at


100±2 °C in a circulating air oven. MFR190/2.16 was determined after 800 h, 1600 h,
2400 h, 3200 h, 4000 h and 4800 h thermal ageing to ISO 1133-1 procedure A and
was compared to the initial value (Table 38 to Table 43). 6 tensile test specimens of
type 5A to ISO 527-2 were cut and the results of the tensile tests are listed in
Table 44.

Table 38: MFR190/2.16 after 800 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 /g/10 min


MFI/%
Measurement 1 Measurement 2 Measurement 3 Average
0.482 0.481 0.485 0.483 3.0

Table 39: MFR190/2.16 after 1600 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 / g/10 min


MFI/%
Measurement 1 Measurement 2 Measurement 3 Average
0.468 0.472 0.467 0.469 5.8

Table 40: MFR190/2.16 after 2400 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 / g/10 min


MFI/%
Measurement 1 Measurement 2 Measurement 3 Average
0.479 0.476 0.469 0.475 4.6

Table 41: MFR190/2.16 after 3200 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 / g/10 min


MFI/%
Measurement 1 Measurement 2 Measurement 3 Average
0.470 0.470 0.476 0.472 5.2

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Table 42: MFR190/2.16 after 4000 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 / g/10 min


MFI/%
Measurement 1 Measurement 2 Measurement 3 Average
0.464 0.465 0.464 0.464 6.8

Table 43: MFR190/2.16 after 4800 h thermal ageing at 100±2 °C and comparison to
initial value (MFR190/2.16=0.498 g/10 min), cut-off interval: 180 s

MFR190/2.16 /g/10 min


Specimen Measurement Measurement Measurement MFI/%
Average
1 2 3
1 0.459 0.458 0.460 0.459 7.8
2 0.451 0.452 0.453 0.452 9.2
3 0.445 0.448 0.449 0.447 10.2
Average 9.1

Table 44: Tensile testing at 23±2 °C and 50 % relative humidity after thermal ageing
and comparison to initial elongation at break (B = 597 %)

Specimen no. Elongation at break / % ∆B / %


1 600
2 620
3 610
4 600
5 610
6 580
Average 603 <1
Standard
12.5
deviation

2.27 Specific insulation resistance

Specific electrical insulation resistance was determined according to DIN 30670 and
NF A49-710 on 3 pipe segments (P.1 to P.3) after a holiday test. An area of 0.049 m²

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of the coating was exposed for each specimen to 0.1 N NaCl solution for a duration
of 100 d at 23±2 °C. The electrical resistance was measured with a teraohmmeter at
500 V after the current was applied for 10 min as average over a duration of 1 min.

In the following Table 45 the values of the specific electrical insulation resistance af-
ter a test period of 40 d, 70 d and 100 d are presented.

Table 45: Specific electrical insulation resistance at 23±2 °C

Specific electrical insulation resistance rU / Ω m2


Time/d P. 1 P. 2 P. 3
13 13
40 2.10*10 2.87*10 2.02*1013
70 1.82*1013 2.76*1013 1.84*1013
100 1.69*1013 2.33*1013 1.71*1013

After the time of 100 days the specific electrical insulation resistance of the speci-
mens shows values between 1.69*1013 and 2.33*1013 Ω m2 at 23±2 °C. All values are
much above the specified minimum value of DIN 30670 and NF A49-710.

Also the additional requirements of NF A49-710 are fulfilled (Table 46).

Table 46: Additional requirements of NF A49-710

Requirement Achieved values


NF A49-710 P.1 P.2 P.3
ru(100d)/ru(70d) > 0.8 0.93 0.84 0.93
α < (0.2/30) Rgr(55 d) yes yes yes
α= α= α=
with -6.83*1010 Ωm2d-1 -9.00*1010 Ωm2d-1 -5.17*1010 Ωm2d-1
α = (ru(100d)-ru(40d))/60 Rgr(55 d) = Rgr(55 d) = Rgr(55 d) =
2.00*1013 Ωm2 2.74*1013 Ωm2 1.94*1013 Ωm2

2.28 Resistance to microorganisms

Resistance to microorganisms was tested according to NF A 49-710. The test was


performed on pipe segments with 150 mm length. Altogether 3 straps with a width of
50 mm were cut into the coating to the steel. Then the specimens were buried in soil

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Testing of a 3-layer HDPE coating

and were exposed for 6 months at 29±1 °C and 97±2 % relative humidity (ISO 846
method D). After exposure no damage on the specimens was detected visually. The
peel strength was determined to NF A 49-710 at room temperature with a peeling
rate of 10 mm/min (Table 47). The requirement of at least 80 % of the initial peel
strength was clearly met.

Table 47: Peel strength at room temperature after exposure for 6 month at 29±1 °C
and 97±2 % rel. humidity in soil (initial peel strength: 446 N/cm)

Measurement Average peel strength / N/cm Peel strength in relation to


initial value /%
1 376 84
2 418 94
3 414 93

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