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Full notch creep test for evaluation of PE-HD materials for container and
pipes

Conference Paper · September 2009

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 Full Notch Creep Test for evaluation of PE-HD materials
for container and pipes

Ute NIEBERGALL1, Olga MERTLOVA2, Eva NEZBEDOVA3

1
Federal Institute for Materials Research and Testing, Germany, ute.niebergall@bam.de
2
Chemopetrol, a.s. Litvinov CZ, Czech Republic, olga.mertlova@chemopetrol.cz
3
Polymer Institute Ltd. Brno, Czech Republic, nezbedova@polymer.cz

Abstract:
Full Notch Creep Test (FNCT) is widely used to characterize the slow crack growth (SCG) behaviour
of particularly pipe and blow moulding PE materials, especially in Europe. However, the validity of
the FNCT data is not satisfactory, as the results show large variability so far.
Among other SCG tests, which exist and are used nowadays, the FNCT method has been selected for
standardization as a relatively simple and still sensitive SCG test method to characterize primarily PE-
HD materials (not final products), to give fully comparable data. The method should be feasible to
perform for common labs of PE material manufacturers, processors, testing institutes, etc.
The ISO 16770 has been developed by ISO TC 61/SC 9/WG 6 and published in 2004. After
publication, precision data were to be investigated for incorporation into the standard. Therefore,
several round robin tests (RRT) have been organized by ISO working group to obtain the necessary
data.

Keywords:
FNCT, container, pipes, PE-HD materials, round robin test

1
1. INTRODUCTION

The phase I of the RRT was organized by BP (i.e. before ISO publication) according to ISO
DIS 16770 [1]. The method has been applied to two PE-HD materials, a blow moulding grade
(designated as BMA) and a pipe grade (designated as PGA), with the following results: for
BMA, acceptable precision data were obtained (tf = 30.5h, stand. deviation = 1h), while for
PGA, a large, unacceptable scatter of data occurred. Due to this reason, the ISO Working
Group has decided to incorporate the data for blow moulding PE as partial precision statement
into the standard and to continue with RRT after publication of ISO 16770.
The new set of tests, RRT2, was oriented on the remaining unresolved technical items and
was aimed to lead to obtain full precision statement in the next revision of the standard.

2. EXPERIMENTAL

2.1. Materials
The method was applied to two commercial PE-HD materials, a PE80 pipe grade (designated
as PGB) and a semi-HMW blow moulding grade (designated as BMB). Basic material
properties are given Table 1.

Table 1: Basic material properties

Density MFR MFR condition
Material Grade
kg/m3 g/10 min
BMB (2005) PE-HD LITEN BS 50 950 5,0 190°C/21,6 kg
PGB (2005) PE-HD LITEN PL 10 952 0,4 190°C/5 kg

The blow moulding PE material (BMB) was included into RRT2, despite the positive RRT1
results, to confirm the conclusions (RRT1), by including the effect of specimen preparation
on results.

2.2. Test method

Scope of test: the influence of test specimen preparation on the results was investigated,
therefore the following options selected (i.e. index n for nothing + testing; index t for testing
only)
BMB/PGB = participants performed: compression moulding + machining + notching +
testing
BMBn/PGBn = participants performed: notching + testing
BMBt/PGBt = participants performed: testing.
For 1 test option, 3 test specimens were to be tested at each of the 4 stress levels, i.e. 12 test
specimens.
Any deviations to the ISO 16770 were recorded for further discussion.

2.3. Test configurations

BMB = specimen type (90 x 6 x 6) mm, notch depth 1,0 mm, reference stress 9 MPa,
temperature 50°C
PGB = specimen type (100 x 10 x 10) mm, notch depth 1, 6 mm, reference stress 4 MPa,
temperature 80°C.

2
2.4 Detergent
Different labs commonly use different types of detergents, and it was not feasible to switch
resolve this fact. Therefore 2 detergent types - Arkopal N110 and Arkopal N100 were used
during the tests. The detergent was aged for 14 days at test temperature.

2.5. Test specimen

Compression moulding conditions used for n & t test options for both materials – see Table 2.
The notch was introduced by pressing razor blade into all 4 sides of the specimens. Special
care was given to the notches being coplanar.

Table 2: Compression moulding/notching conditions

Specimen Moulding Preheating Full pressure
Full pressure Cooling rate
thickness temperature time time
mm °C min MPa min °C/min
6 180 20 5 10 15 ±2
10 180 45 10 25 *
* Heat switched off to allow cooling overnight at full pressure; cooling rate not controlled.
Note: positive mould used for both types of specimens.
Notching speed for BMBt/PGBt options: 0,330 mm/min., 6 spec per 1 razor blade.

2.6. Evaluation of data

The fracture time was recorded, fracture surface investigated by a microscope and exact
ligament area determined. The ligament stress was plotted versus failure time in double
logarithmic scale. Time to failure for nominal stress was evaluated by interpolation.

3. RESULTS AND DISCUSSION

3.1. BMB material

7 labs delivered the test data. The results are summarized in Fig. 1-3. Unfortunately not all
sets of data were relevant for proper evaluation. The main deviations from the ISO 16770
standard observed: testing at just 1 stress level (2 labs), which did not allow to interpolate the
failure time for nominal stress. Some improper bath conditions were reported, substantially
varying notching speeds (where reported), 2 types of detergent used. Therefore, interpretation
of results, especially investigating the effects of moulding the specimens was problematic due
to lack of relevant data. As “relevant” data were considered those, which did not differ from
ISO 16770 significantly.

3
 50 50
34,3 40,1
Time to failure, hr.

Time to failure, hr.

40 39,1
40
24,8 25,6 26,5 26,4 24,9 25,1 24,2 32,4
30 27,4 24,9 18,4
30
18,4
20 20

10 10

0 0
1 3 5 7 8 9 10 10r 1 3 5 7 8 10 10r

Number of lab Number of lab

Figure 1: BMBn – Influence of notching Figure 2: BMBn – Influence of compression

Moulding

45,3
50
Time to failure, hr.

40
26,4
30
23 21,4 19,4 19,1
20

10

0
3 5 7 8 9 10
Number of lab

Figure 3: BMBt – Influence of test method

However, the influence of any of the observed factors did not seem to be too significant. The
standard deviations (in %) were comparable with that obtained in RRT1 (where the influence
of moulding conditions was not considered). As a conclusion, the RRT1 results, implemented
in ISO 16770 as partial precision statement, were taken as confirmed.

3.2. PGB material

10 labs delivered the test data. The results are summarized in Fig. 4-6.
Again for PGB, and in much greater extend than for BMB material, not all sets of data were
relevant for proper evaluation. The main observed deviations from the ISO 16770 standard: 3
labs tested at just 1 stress level, which did not allow interpolating the failure time for nominal
stress. Some data had to be obtained by extrapolation. Similar to BMB material, some cases
of improper bath conditions (variation of temperature, adding of un-aged solution during the
test) were reported, rather broad range of notching speeds (where reported) and 2 types of
detergent used.

4
 141,5
160 160
125,7 135,8
140 140

Time of failure, hr
105,7 100,1
Time of failure, hr

117 101,9
120 120
97,4 87
93,2 100
100
73,2 80
80
48,8 53,3 60
60 31,1
38,6 31,1 40
40
20
20 0
0 1 2 7 8a 8b 10 11
1 2 6 7 7r 8a 9 10 11
Number of lab
Number of lab

Figure 4: PGBn – Influence of notching Figure 5: PGB – Influence of compression

moulding

250
220,2
Time of failure, hr

200

150
110,6
73,7 77,3
100
52,4 49,2 53,3 32,7 51,2
50

0
1 6 7 7r 8a 9 10 11 12
Number of lab

Figure 6: PGBt – Influence of test method

The most critical however, were differences in compression moulding procedure, namely in
cooling rate method. The compression moulding condition defined in ISO 16770, e.g. cooling
rate of (2 ± 0,5) °C/min proved not to be feasible to implement on most commercial presses in
a controllable manner.

4. CONCLUSION

The RRTs did not succeed in obtaining the precision statement for ISO 16770 fully, probably
from the following reasons:

4.1. Insufficient number of testing points

Some labs did not test at the 4 stress levels and used just one stress level (misunderstanding,
lack of testing capacity, etc.). Minimally 3 specimens shall be used per each of 4 stress levels
to compensate for possible ligament variation.

4.2. Detergent
Previous experience showed that a detergents with the number of (-CH2-CH2-O-) groups,
n=10 give slightly longer times to failure than detergents with n=11, the observed difference
being approximately 10%. It is therefore reasonable to compare only data obtained on one
type of detergent. This was not possible to fulfil during the tests. Furthermore, there was a

5
 case when an un-aged solution was added during longer tests to prevent evaporation. This
may invalidate the test results. Suggestion for using balls or oil in the bath if necessary to
compensate for possible evaporation can be included into ISO 16770.

4.3. Notching
Notching speed is sure a factor influencing the crack initiation process [2]. The labs used
broad range of notching speeds, when reported (minority of them). The ISO 16770
recommends “to avoid excessive speed/force”, which may be misinterpreted without
specifying any limiting value. The possibility how to avoid this problem is to utilize the
recommendation given for PENT test [3]. PENT test defines notching speed of not more than
0.25 mm/min.

4.4. Compression moulding

Critical factor is probably the quality of test specimen with bigger cross section of 10x10 mm;
e.g. problems are in the compression moulding conditions. Examination of the plaques
showed inhomogeneity e.g. not ideally melted areas, which most probably decrease the times
to failure and contribute to the large scatter of the results. The most discussed factor is the
cooling rate. Cooling conditions have crucial effect on material crystallinity, which influences
the rate of crack growth. It was confirmed during the test that faster cooling (15°C/min) gave
longer failure times in comparison to “slow cooling” (2°C/min) defined in ISO 16770.
Nevertheless this type of cooling can be implemented only by switching-off the heat and thus
no control is possible. The temperature gradient is probably non-linear, as it depends on room
temperature variations and may vary for different presses (different masses). This condition
was however chosen in the standard, to enable slower cooling of thicker plaques.

4.5. Consequences of the large scatter of results

The FNCT has been accepted lately in Europe as a decisive criterion for material approval
(qualification) for different applications (IBC containers, pipes, etc.), due to its good
sensitivity to distinguish among materials, together with relative simplicity (material testing
instead of product). Of course, product testing has to follow, however material data represent
the input information. It has been found that different testing bodies may achieve different
results on the same material. Such situation is to be solved urgently.

5. REFERENCES

1. ISO 16770: Plastics – Determination of environmental cracking (ESC) of Polyethylene

(PE) – Full Notch Creep Test.
2. N. Brown and X. Lu, Polymer Trstiny, 11 (1992) 309.
3. ISO/DIS 16241: Notch tensile test for measure the resistence to slow crack growth of
Polyethylene materials for pipe and fitting products (PENT-test).

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