Rev.

0, Date: 19th May 2016

Report – Root cause analysis

Investigations on pipe HIC-test specimens in question

Pipe producer JINDAL SAW LTD (JSAW)
Grade API 5L X65MS PSL2 for Oman Gas Project
Heat no. 412249, 17.3 mm W.T. x 36” OD
Heat no. 411987 and 411471, 19.3 mm W.T. x 36” OD

contents

1 Background _______________________________________________________________2
2 Plate production and results _________________________________________________2
3 Investigations on the pipe specimens __________________________________________4
4 Discussion ________________________________________________________________5
5 Summary _________________________________________________________________5
6 Corrective actions __________________________________________________________5
7 Preventive actions for future supplies __________________________________________6
8 General remarks ___________________________________________________________7

It shall be noted that acknowledgement of a legal obligation is outside the scope of this technical
report.

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1 Background
The HIC test results on all tested heats/pipes were provided by JSAW.
Attachments 1 to 3 are showing the certificates and Table 1 gives the results and assignment of
the HIC specimens with test results in question. The requirements for the average per specimen are
≤15% for CLR, ≤5% for CTR and ≤2% for CSR. On any section a maximum individual crack
length of 5mm is specified. Table 2 presents the chemical compositions of the heats with pipe HIC-
test results in question.

Table 1: Results and assignment of the pipe HIC specimens in question

Specimen identification 816 C4-1 and 3 824 C24-2 825 B27-3
Position 180° from long. weld 180° from long. weld 90° from long. weld
CLR 13% CLR 9%
Pipe HIC-test results CTR 1.5%
CTR 0.5% CTR 0.4%
passed CSR 0.3 %
CSR 0.2% CSR 0.1%
CLR 15.3%
Pipe HIC-test results in Maximum individual Maximum individual
Maximum individual
question crack length 7.6mm crack length 5.6mm
crack length 5.1mm
Heat no. 412249 411987 411471
Pipe no. L116B03262 L115M10143 L115M10318
Plate no. 353026-01 353063-01 346151-02
Wall thickness in mm 17.3 19.3 19.3
Plate order no. 396245 396246 396246
No. of plates received 2 (17.3 mm)
from the corresponding 28 15
heat 4 (19.3 mm)

Table 2: Chemical compositions (heat analysis) of the heats with pipe HIC-test results in
question (lab Dillinger Hütte, in wt%)
Heat C Si Mn P S Al Cr Nb Ti Ca Ca/S
412249 0.049 0.38 1.54 0.012 0.0010 0.029 0.20 0.045 0.017 0.0009 0.9
411987 0.050 0.36 1.54 0.011 0.0010 0.025 0.19 0.044 0.017 0.0014 1.4
411471 0.047 0.36 1.51 0.009 0.0010 0.029 0.19 0.043 0.015 0.0011 1.1

2 Plate production and results

Table 3a to 3c gives an overview on the plate HIC-test results for the 3 heats with pipe HIC-test
results in question. All the heats were tested on plates with several specimens and all the results
meet the requirements.
As a result of the specific HIC quality assurance system of Dillinger, heat 411471 was HIC
tested in detail since this is a first heat of a casting sequence. It is worth mentioning that the pipe
with HIC test results in question of heat 411471 (pipe L115M10318, plate 346151-02) was also
HIC tested on the corresponding plate and did not show any HIC cracking. Pipe L115M10143 out

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of heat 411987 was not tested on the corresponding plate (plate no. 353063-01).This plate did not
show any incident during steel making or casting process. Heat 412249 is the last heat of a casting
sequence and two out of the six tested plate specimens were close to (but within the limits) the
requirement with regard to the maximum individual crack length.
The plate process parameters of the plates with HIC test results on the pipes in question were
verified. All the process parameters are within the targeted range, i.e. no deviation from the
essential variables occurred.

Table 3a: HIC- test results (test lab Dillinger France) on plates produced from heat no. 412249
CLR (average) Max. indiv. crack length
Plate no. Specimen no. Position
in % in mm
1 Head 0 0
353026 2 Middle 8 4.8
(17.3mm) 3 Middle 0 0
4 Middle 0 0
357227 1 Head 0 0
(19.5mm) 2 Middle 8.3 5.0

Table 3b: HIC- test results (test lab Dillinger France) on plates produced from heat no. 411987
CLR (average) Max. indiv. crack length
Plate no. Specimen no. Position
in % in mm
1 Head 0 0
338086 2 Middle 0 0
3 Middle 0 0
4 Middle 0 0
1 Head 0 0
353073
2 Middle 0 0
338083 1 Head 0 0
2 Tail 0 0

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 Table 3c: HIC- test results (test lab Dillinger France) on plates produced from heat no. 411471
CLR (average)
Plate no. Specimen no. Position
in %
1 Head
346151 2 Middle
3 Tail
1 Head
346040 2 Middle
3 Tail
1 Head
346036
2 Middle
1 Head
350033 2 Middle
3 Tail
1 Head
346015 2 Middle
3 Tail
1 Head
346014 2 Middle
3 Tail
1 Head
346033
2 Middle
Max. indiv. crack length
in mm
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0

3 Investigations on the pipe specimens

The microsections of the pipe HIC specimens with test results in question were provided to
Dillinger for investigations (Figure 1). The microsections were metallographically investigated by
light and scanning electron microscope. In addition the HIC fracture surfaces were opened for
further investigations by scanning electron microscope. The results are documented by
representative photographs in Figure 2 to 7.
In summary it can be noted:
• All the cracks are located in the mid thickness position.
• Fracture surfaces are decorated by manganese sulfides inclusions (MnS) and TiNb(CN) or
Nb(CN) precipitations. MnS are known to be potential crack initiation sites.
• Crack propagation occurs in disconnected microstructural lines with M/A and bainite
constituents arranged in small islands associated with TiNb(CN) or Nb(CN) precipitations.

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4 Discussion
According to ISO 80000-1 Appendix B (Rounding of numbers) the test result of specimen 816
C4-1 and 3 (heat 412249) should be expressed as 15% for CLR and 5mm for the maximum
individual crack length. Of course these results are very close to (but below) the specified limits, but
are in fact complying with the requirements of the maximum CLR value of 15% and the maximum
individual crack length of 5mm.
Figure 8 shows the carbon contents and Ca/S-ratios for the heats with passed and HIC pipe test
results in question. From this graph a tentative not preferable area is derived and the area with
proved HIC test results (preferable area) on pipe is added. Taking this into consideration and the
fact that the plate HIC-test results passed, the cracks on the pipe HIC specimens can be attributed to
an unfavourable combination of a higher carbon content and a lower Ca/S-ratio in combination with
cold deformation.
In Figure 9 the carbon contents and Ca/S-ratios for the heats without HIC test result on pipe are
added. Two heats are falling in the tentative not preferable area (heats 412236 and 412033) and one
heat in the transition zone between the two areas (heat 412129).

5 Summary
It shall be noted that the cause of the cracks in the pipe HIC specimens elucidated in this report
has to be clearly differentiated from the cause of the crack occurred on a pipe HIC specimen of heat
415757 (pipe no. L115L6451, size 14.2 mm W.T. x 36” OD, see separate report from 2nd March
2016). In the latter case the HIC crack was in a subsurface position and the alloying concept was
different (particularly with regard to the Mn content which was lower) due to the lower thickness.
The cause of the cracks on the pipe HIC specimens investigated in this report could be traced
back to an unfavourable combination of a higher carbon content and a lower Ca/S-ratio. A tentative
not preferable area for the combination of both values was derived. It shall be noted that the plate
HIC-test results on the heats 411987 and 411471 did not show any cracking although these heats are
falling in this area. It is known that cold deformation can impair HIC test performance and
consequently can increase the risk to fail the HIC test criteria. That means, finally an unfavourable
combination of three factors (higher carbon content, lower Ca/S ratio plus cold deformation during
pipe forming) occurred and contributed finally to the pipe HIC-test results in question.

6 Corrective actions
Heats 412249, 411987 and 411471
DH is prepared to deliver relevant plates to replace the pipes from these heats.

Additional HIC tests on heats 412236, 412033 and 412129

The carbon content and Ca/S-ratio are lying in the tentative not preferable area or in the
transition area (according Figure 9). These heats were not tested on pipe. It is proposed to test pipes
from these heats, also for verification of the tentative derived areas.

HIC tests on pipes with a thickness of 16mm, plate order 396099

The plates of this order were already delivered in 2015. It is proposed to test on pipe, in addition
to the testing frequency of 1 test/10 heats, specific heats with carbon contents and Ca/S-ratios
outside the tentative preferable area (Figure 10). These heat numbers are compiled in Table 4. As a
precaution it is further suggested that if still possible, the pipe production of the heats in the

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tentative not preferable area starts with the production of one pipe on each heat and resume once the
pipe HIC on this specific heat passed.

Table 4: Heats outside the tentative preferable area proposed for additional HIC testing on
pipes with a thickness of 16mm, plate order 396099
Heat no. C content S content Ca content Ca/S-ratio
Heats in the tentative not preferable area
410477 0,050 0,0008 0,0012 1,50
410609 0,049 0,0010 0,0012 1,20
410651 0,050 0,0007 0,0009 1,29
410701 0,047 0,0007 0,0007 1,00
410703 0,049 0,0009 0,0011 1,22
410705 0,052 0,0009 0,0013 1,44
410726 0,050 0,0008 0,0012 1,50
410760 0,049 0,0013 0,0016 1,23
410912 0,053 0,0006 0,0010 1,67
411602 0,050 0,0009 0,0013 1,44
Heats in the transition area
410475 0,049 0,0007 0,0012 1,71
410564 0,041 0,0008 0,0010 1,25
410616 0,040 0,0011 0,0014 1,27
410648 0,042 0,0007 0,0008 1,14
410698 0,042 0,0010 0,0011 1,10
410721 0,047 0,0009 0,0011 1,22
410731 0,045 0,0010 0,0011 1,10
410732 0,050 0,0007 0,0012 1,71
410738 0,048 0,0008 0,0012 1,50
410743 0,039 0,0007 0,0009 1,29
410757 0,045 0,0010 0,0012 1,20
410762 0,042 0,0011 0,0014 1,27
410861 0,041 0,0011 0,0014 1,27

7 Preventive actions for future supplies

In order to compensate a certain impairment of the HIC test results by the pipe forming, it is
proposed to modify for future supplies the HIC acceptance criteria on plate as follows:
• Requirements for the average per specimen: ≤10% for CLR, ≤3% for CTR and ≤1.5% for
CSR.
• On any section: 4mm for maximum individual crack length

Future supplies with higher Mn contents (Mn ≥ 1.50%)

As a matter of precaution Dillinger will take care that the carbon content and the Ca/S-ratio will
be outside the tentative not preferable area for future supplies with higher Mn contents (Mn ≥
1.50%).

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 HIC tests on pipes for current plate order 409869 (thickness 20.5mm) and 410687
(thickness 16.5mm)
It is suggested to test on pipe, in addition to the testing frequency of 1 test/10 heats, specific
heats with carbon contents and Ca/S-ratios outside the tentative preferable area (Figure 11 and 12).
These heat numbers are compiled in Table 5.
It shall be mentioned that two heats were also produced with carbon contents and Ca/S-ratios
within the tentative not preferable area. As a measure of caution the plates out of these heats will
not be delivered.

Table 5: Heats outside the tentative preferable area proposed for additional HIC testing on
pipes for current plate order 409869 (thickness 20.5mm) and 410687 (thickness 16.5mm)
Heat no. C content S content Ca content Ca/S-ratio
431267 0,045 0,0010 0,0012 1,20
431924 0,049 0,0006 0,0009 1,67
431085 0,052 0,0006 0,0011 1,83
432009 0,049 0,0008 0,0012 1,50
432015 0,049 0,0007 0,0010 1,43

8 General remarks
As alternative it is suggested to check with research institute by expert experience from full scale
tests whether slightly increased values on CLR or maximum individual crack length achieved on lab
HIC-tests, as found on the heats in question, could be acceptable.
For all the new tests we ask you to be very careful about sampling, e.g. avoid influence of
specimen cutting on edges.
It is suggested that pipe coupons from heats with additional HIC tests, as proposed in paragraph
6 and 7 of this report, are also sent to Dillinger in order to perform supplemental HIC tests also in
the Dillinger HIC lab.

Prepared by
E. Amoris, I. Lecreux, Dr. T. Staudt

Reviewed by
V. Schwinn

Approved by
Dr. M. Bott

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 a.) packed

b.) unpacked

Figure 1: HIC specimens 816 C4-1 and 3, 824 C24-2 and 825 B27-3 as provided

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 2: Microsections of HIC specimens with cracks, polished in unetched condition, light microscope,

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 3: Microsections of HIC specimens with cracks, light microscope, etched condition, magnification 50x

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 4: Microsections of HIC specimens with cracks, light microscope, etched condition, magnification 500x

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 5: Microsections of HIC specimens with cracks, etched condition, scanning electron microscope, magnification 1000x

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 6: Microsections of HIC specimens with cracks, etched condition, scanning electron microscope, magnification 5000x

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 a.) specimen 816 C4-1, heat 412249 b.) specimen 816 C4-3, heat 412249

c.) specimen 824 C24-2, heat 411987 d.) specimen 825 B27-3, heat 411471

Figure 7: Fracture surfaces of HIC specimens, scanning electron microscope

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Figure 8: Ca/S ratios and carbon contents for heats with pipe HIC test results in question and passed results, thickness 17.3mm and 19.3mm,
plate order no. 396245 and 396246

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Figure 9: Ca/S ratios and carbon contents for heats with pipe HIC test results in question, passed results and not HIC tested, thickness 17.3mm
and 19.3mm, plate order no. 396245 and 396246

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Figure 10: Ca/S ratios and carbon contents for heats with pipe HIC test results in question and passed results for thickness 17.3mm and
19.3mm (plate order no. 396245 and 396246) and for plate order no. 396099 with a thickness of 16mm (delivered in 2015)

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Figure 11: Ca/S ratios and carbon contents for heats with pipe HIC test results in question and passed results for thickness 17.3mm and
19.3mm (plate order no. 396245 and 396246) and for plate order no. 409869 with a thickness of 20.5mm (to be delivered)

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Figure 12: Ca/S ratios and carbon contents for heats with pipe HIC test results in question and passed results for thickness 17.3mm and
19.3mm (plate order no. 396245 and 396246) and for plate order no. 410687 with a thickness of 16.5mm (to be delivered)

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Attachment 1a: HIC-Test certificate heat 412249, page 1

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Attachment 1b: HIC-Test certificate heat 412249, page 2

Attachment 2a: HIC-Test certificate heat 411987, page 1

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Attachment 2b: HIC-Test certificate heat 411987, page 2

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Attachment 3a: HIC-Test certificate heat 411471, page 1

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Attachment 3b: HIC-Test certificate heat 411471, page 2

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