Paper No.

284

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CAUSTIC STRESS CORROSION CRACKING SUSCEPTIBILITY IN CONTINUOUS KRAFI’
DIGESTERS DUE TO PROCESS LOADINGS

Heikki Leinonen
VTT Manufacturing Technology
P. O. Box 1704
FIN-02044 VTT, Finland

ABSTRACT

Loads of the continuous kraft digester have been determined during the start-up of the digester
house. Loading was caused by the pressure of the proof test, the start-up pressures of the digester and,
finally, the normal working pressure. The apparent threshold stress level in the base metal was greater
than that achieved during the normal continuous cooking process but the level in the weld of the
impregnation zone were exceeded due to the superposition of the tensile residual stresses. This two-
axial tension is considered as the precondition for stress corrosion cracking (SCC), which was
confirmed by fractography studies. The results showed, that SCC in the impregnation zone is possible
only in the welds during the normal continuous cooking process. During the refill and blow phase of
the digester the measured loading stress changes corresponded to the stresses of the proof test and
increased the risk for SCC. Some procedures to avoid or minimize SCC are discussed.

INTRODUCTION

Continuous digesters, constructed of carbon steel, were originally believed to be relatively free of
corrosion problems. For two decades, corrosion was of relatively little concern in continuous digesters,
and visual inspection was considered sufficient to ensure the integrity of these vessels. Then in
September, 1980, the sudden failure of the digester at Pine Hill, Alabama occurred due to a form of
stress corrosion cracking (SCC) called caustic SCC1. This disaster resulted in greatly increased activity
in research of caustic SCC leading to attention of inspection, which still is very wide also in
Scandinavia. A survey revealed that nearly 75% of all continuous digesters had cracks presumed to be
SCC3.

Research is currently underway to uncover some of the factors which contribute to cracking, such
as wood species, liquor composition, and digester operation4 but the only significant correlation noted
to date for the tendency toward cracking is the stress distribution of the digesters, especially in the
welds. The total stress is composed of the additive combination of the factors such as stresses due to

Copyright
01999 by NACE International. Requests for permission to publish this manuscript in any form, in part or in whole must be made in writing to NACE
International, Conferences Oivision, P.O. Box 218340, Houston, Texas 77218-8340. The material prasented and the views expressed in this
paper are solely those of the author(s) and are not necessarily endorsed by the Association. Printad in the U.S.A.
pressure, dead weight, external loads, stress concentration due to geometric discontinuities and residual
stresses from fabrication and/or thermal treatment. It is significant to note that usual pressure vessel
stress calculations take into account only the first three factors above. In usual calculations, a safety
factor is added to take into account the other contributions to stress.

This paper will discuss the contribution of loading stresses to the caustic SCC problem in a
continuous digester, where cracks were found in the impregnation zone. The loading was caused by the

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pressure of the proof test, the start-up pressures of the digester and, finally, the normal working
pressure. The effects of the indicated residual stresses in the weld will be combined to loading stresses.
Some aspects of the loading stress changes especially during the start-up procedures affecting to the
SCC will also be discussed.

EXPERIMENTAL METHODS

The continuous digester studied was a Finnish Kamyr-digester built in 1964 with the capacity of
350 ADT/day. The material of the digester is the mild steel HIV according to the pressure vessel steel
standard DIN 17155 (1959), which corresponds to the standard ASTM A5 16M-90, Gr.60. The problem
of the continuous digester cracking burst during the annual service and inspection. The most severe
corrosion cracking occurred in the impregnation zone at a transversal weld located about three meters
below the transition cone of the digester. Weld repairs were performed during the long service life of
the vessel. The temperature in the digester was during all measurements 393 K ( 120”C), i.e. the normal
cooking process temperature.

A sample of the weld was cut from the digester in order to study the detailed reason for cracking.
The failure analysis was performed in fractography using optical and scanning electron microscope
(SEM).

The experimental stress analysis of the digester was based on the strain measurements with
resistive strain gages. The pattern of the 350 Q strain gage used was a two-element 90-degree rosette
(i.e. tee) in order to determine principal stresses, whose directions could be known in advance to be
aligned with the main axes of the digester. Two gages were glued at two locations on the outer surfaces
of the cross-section of the digester.

These places were located at the most cracked area of the cross-section, which was selected
based on the inspection indications. One of the gages was located on the middle of the transversal weld
and the other above it at a distance of 110 mm on the base material, Fig. 1.

The temperature changes during the measurement were eliminated using of a half bridge
connection, where temperature compensation strain gages attached very close to each active strain
gage compensated the thermally induced strains. The measuring equipment consisting of a DC strain
gage amplifiers with a filter of 10 Hz or 25 Hz were installed in the digester control room, where the
signals were recorded to the tape recorder Kyowa 670A and the PC Toshiba 3200 in the analogous and
digital form, respectively. Other process parameters such as temperature and pressure were taken direct
from the control units of the digester. The estimated relative accuracy was t 2 x 10-2,* 3 x 10-2and
&5 x 10-2 for strain, temperature, and pressure, respectively.

The loading sequences used in this study were at first the proof test up to 1 MPa (10 bar) with
the unloading phases, during which the permanent deformations were recorded. The other sequences
were connected to the start-up processes of the digester: chip fill, cook and blow. Finally, the strains
due to the normal steady state process of the continuous digester were monitored.

RESULTS

The results are divided into three main categories according to the arrangement during the
experimental study. At first the results of the proof test of the digester are shown. Then the results of

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the start-up processes leading to the normal steady state process are presented. All results are shown in
strains (pm/m) of each strain gage having the zero balance when the digester was empty.

During the start of the proof test the strains in Fig. 2 showed a little tension (– sign) of all
measuring places in the filling and heating phase of cooking liquor. Under the proof pressure the axial
strains of the weld (Rl, R5) were compression (+ sign). The proof tests of the digester were repeated
and after each phase the digester was unpressurized as shown in Fig. 3, where the strains during the
start of the chip fill have been plotted.

The strain ranges remained during the start-up processes although their amplitudes increased
clearly, Fig. 4. After the chip fill the pressure disturbances in Fig. 4 caused significant changes in the
axial strains of the weld (R 1, R5), which were at the beginning of cooking practically totally relaxed.
During the refill operation the strains varied due to the service pressure, Fig. 5. At the beginning of the
continuous process the start of the blow, Fig. 5, caused strain amplitudes, which decreased later, when
the normal steady state continuous process predominated, Fig. 6. During this process more detailed
strain amplitudes could be observed, when the filtering of the data were changed from 10 Hz to 25 Hz,
Fig. 7.

DISCUSSION

Based on the standardized experimental design of pressure vessels the measured strains can be
expressed as calculated principal stresses aligned with the main axes of the digester. Thus, the
significance of the largest principal stresses due to the different loading sequences performed can be
examined.

During the proof test of the digester differences in strains were found between the base metal and
the weld. At the proof pressure of 1 MPa the measured strains in the base metal, i.e. R3, R7 and R4, R8
in Fig. 2, corresponded to the stresses aBA= -35 MPa and OBT = -70 Mpa in the axial and tangential
directions, respectively, Table 1.By using the common proof test equations and the real dimensions of
the digester, the calculated stresses are -37 MPa and -74 MPa, respectively. The difference between
these measured and calculated stresses is mainly due to the measurement uncertainty of the proof
pressure.

At the end of the proof test in the unpressurized phase IV in Fig. 3, the small residual strains of
the base metal were caused by changes of the geometry such as the ovality. The situation was different
in the weld. The tangential strains of the weld (R2, R6 in Fig. 2) corresponded on the average the stress
Crwr= -70 MPa, which equals the tangential stress of the base metal oBT above. Instead, the axial
strains of the weld R1 and R5 in Fig 2 were tension and corresponded average stress of +20 MPa,
which originated from the welding residual stresses. These residual stresses relaxed, when the
disturbances due to the pressure difference (Fig. 4) between the heater and digester elevated the
digester pressure. Based on the analysis of the transverse residual stress distribution of the weld5 in Fig.
8 the internal surface weld and HAZ may contain residual stresses in tension, whose magnitude could
be multiple to the observed in compression on the external surface, i.e. the measured compression
strains (RI and R5) correspond the transverse residual stress distribution of the weld in Fig. 8. It is
acknowledged that the stress in tension is a prevailing mechanical condition for SCC to initiate.
Additional work should be performed to determine residual stresses on the inside surface of the weld
of the digester either by the computer analysis or experimental measuring.

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During the start-up processes of the digester the loading stresses changed according to the
process phases. The effect of the net weight of the digester on the stresses was only -10 MPa
calculated from the axial strains R3 and R7 in chip fill in Figs. 3 and 4. Further the stress amplitudes
were during the start of cooking in the bottom half of the digester in Fig. 4 and in chip refill in Fig. 5
max. 22 MPa. The most significant stress amplitudes during the start-up process were indicated at the
beginning of blow in Fig. 5, where the stresses changed rapidly over 42 MPa.

At the normal working pressure when cooking was continuous and steady state the stresses were
also quite steady, Fig. 6. The small changes in the strains R1 and R3 could be caused by the axial
external support structure of the digester located closely to these strain gages. The more detailed stress
analysis of the normal continuous cooking in Fig. 7 showed two low-frequency strain amplitudes. The
pressure control and the pressure stroke of the high-pressure feeder changed at the frequencies of 0.05
Hz and 1.1 Hz causing the stress amplitudes about 3 MPa and 1 MPa, respectively.

Resistance to SCC is generally measured by the apparent threshold stress at and below which
SCC does not occur. The principal stresses due to the loading sequences in the digester structure
should be summarized with the residual stresses in order to get the total stresses, which can be
compared to the apparent threshold stress. The yield strength of the mild steel used in the digester was
RP0.2= 260 MPa at 393 K (120°C). Unfortunately, no exact threshold stress value of the mild steel in
the environment of the digester has been reported. Anyway it can be estimated, that the apparent
threshold stress could be in comparable environments as low as a half of the yield strengtl$.

Thus, this study suggests that the threshold level in the base metal is greater than that achieved
during the normal continuous cooking process. Instead, the threshold level in the weld of the
impregnation zone could easily be exceeded due to the superposition of the residual stresses, which
was detected in the axial direction as observed SCC.

There is much evidence which confirms that fully post weld heat treated digesters resist SCC7.
However, in this study the exceptional pressure peak relaxed residual stresses in the heat treated weld.
Better control of post weld heat treatment is required to ensure true stress relief.

The most significant stress changes were measured at the beginning of blow, where the changes
were of the order of the axial proof stress. Other minor changes were during the start of cooking in the
bottom half of the digester and in chip refill. This kind of periodic loading and/or unloading such as the
measured small vibration due to the high-pressure feeder can be examined as a special case of SCC,
Fig. 9. Although the constant load test has been technically preferred for detecting the SCC
susceptibility of the alloys, the principal advantage of the slow strain rate test (SSRT) or constant
extension rate test (CERT) in Fig. 9 is the rapidity with which the SCC susceptibility of the particular
alloy and environment can be assessed. It is difficult to separate in these cases SCC and corrosion
fatigue from each other. Both the vibration and loading/unloading has been observed in the laboratory
tests to increase SCC notably8. Thus, the continuous digester process should be run with a minimal
number of shutdowns and start-ups.
 The effects of different loading sequences on SCC in the kraft digesters should finally be
connected with fundamental models of SCC phenomena. One such model describes corrosion-
deformation interaction in the initiation and propagation of cracks. It is shown that selective dissolution
interacts with the dislocations leading to cleavage-like SCC in austenitic stainless steels in caustic9 and
chloride10 solutions. If the model could be applied for the digester process, the strain rates would be
more critical as stresses to measure, inspect and control, because according to the model vacancies

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generated by corrosion are first consumed by dislocations which enhances creep. Also, on-line
monitoring of the corrosive environment in the digester will be the next step for the fundamental
understanding of SCC in the digesters.

CONCLUSIONS

The following main conclusions can be drawn from the results obtained:

. The apparent threshold stress level in the base metal was greater than that achieved during the
normal continuous cooking process. There is no risk for SCC in the base metal.

. On the other hand, the apparent threshold stress level in the weld of the impregnation zone was
exceeded due to the superposition of the tensile residual stress. The direction of the observed SCC
confirmed this fact. Better control of post weld heat treatment is required to ensure true stress relief.

● The most significant loading stress changes were measured at the beginning of blow. Other minor
changes were during the start of cooking in the bottom half of the digester and in chip refill. All the
stress changes detected increased the risk of SCC. The continuous digester process should be run
with a minimal number of shutdowns and start-ups.

ACKNOWLEDGEMENTS

This study was funded through a research contract with the UPM-Kymmene Corporation Kymi.
The successful completion was heavily dependent on the assistance provided by Mr. Timo Suominen
and Mr. Pentti Tiihonen. Their cooperation is gratefully acknowledged.

REFERENCES

1. D. C. Bennett, Cracking in Continuous Digesters-History of the Problem and the Search for
Predictive Measures, Tappi Journal 65, 12 (1982): p. 43-45.

2. S. Strom, “Crack Development and Corrosion in Continuous Kraft Digesters”, Proc. Conf.
Engineering Solution to Industrial Corrosion Problems, Sandefjord, Norway, 7–9 June 1993,
Paper No. 37. (NACE International, 1993).

3. A. Wensley, Cracking of Continuous Digesters: an Updated Survey, Tappi Journal 72,

8(1989): p. 211-215.

4. L. Kiessling, “A. Study of the Influence of Modified Continuous Cooking Processes on the
Corrosion of Continuous Digester Shells”, Proc. Int. Symposium on Corrosion in the Pulp &
 Paper Industry, Stockholm, Sweden, May 16-19, 1995. Pulp & Paper Industry Corrosion
Problems, Vol. 8, p. 12–19.

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5. W. Dahl & H. Krebs, “Determination and Assessment of Residual Stresses in a Multilayer
Submerged Arc Welded Joint”, Proc. Int. Conf. on Residual Stresses Nancy, France,
November 23–25, 1988. In: Beck, G., Dennis, S. & Simon, A. (eds.) Elsevier Applied
Science, 1989. P. 683-689.

6. M. J. Humpfries & R. N. Parkins, Stress-Corrosion Cracking of Mild Steels in Sodium

Hydroxide Solutions Containing Various Additional Substances, Corrosion Science 7(1967):
p. 747-761.

7. D. Singbeil & A. Garner, Caustic Stress Corrosion Cracking of Pressure Vessel Steels in
Dilute Alkaline-Sulfide Solutions, Materials Performance 34, 10(1985):p. 9-15.

8. M. O. Speidel, “Design Against Environment Sensitive Fracture”. In: Miller, K.L. & Smith
R.F. (eds.). Third Int. Conf. on Mechanical Behaviour of Materials. Cambridge, England, 20-
24 August, 1979. P. 109-137.

9. J. H. Zheng & F. Bogaerts, “Transpassive Chromium Dissolution - Interaction with Stress

Corrosion Cracking of Austenitic Stainless Steel in Caustic Solutions”. In: Magnin, T. (cd.).
Second Int. Conf. on Corrosion-Deformation Interactions. Nice, France, 24–26 September,
1996. European Federation of Corrosion Publications Number 21. The Institute of Metals,
1997. P. 104-116.

10. H. Leinonen & H. H&minen, “Prediction of Stress Corrosion Cracking Susceptibility of

Austenitic Stainless Steels in 50% CaC12Solution”. In: Magnin, T. (cd.). Second Int. Conf. on
Corrosion-Deformation Interactions. Nice, France, 24-26 September, 1996. European
Federation of Corrosion Publications Number 21. The Institute of Metals, 1997. P. 131-139.

TABLE 1
THE RESULTS AS STRESSES (MPa) IN THE PROOF TEST AT 1 MPa

Base metal Weld Theory

kid stressCA -35 +20 -37

Tang. stress @ -70 -70 -74

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1,-14 = Intake pipe Joints
+
WD = Verlicel weld down WU = Vertical weld up WI m

FIGURE 1- The cross-section of the digester in the impregnation zone where the strain gages
R1.. .R8 were glued
Tam @eae

‘“”P
ZBM “

100

o 0
z F
-z
~ -1oo E
& -1oo
~
~ -200 F---’- ~ -200
03

&
(JI r
-300

L-
-300

1 i
-400 40
t 1 1 1! I I 1 1 ) 1 1
0 0.2 0.4 .6 0.8 1.0 1.2 1.4 1.6 1.8 0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.6 2.0 2.2
TIME (h) TIME (h)

FIGURE 2- The strains as a function of time FIGURE 4- The strains as a function of time
during the start of the proof test during the end of chip fill and at the beginning
of cooking
CddngchipmK# COddng
mow
I I

4
I I I

o
E
%
~ -1oo g.,:

j -200
~ -200
W
0
-300
-200

-400 -400

TIME (h) TIME (h)

FIGURE 3- The strains as a function of time at FIGURE 5- The strains as a function of time
the beginning of chip fill during refill and in the early stage of blow
 24 -
A Weld metal

F 0 ● Base mebl
~ 16 -
g.-loo
-
R3 co
~

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(n

g -200
g ,2 _
W
Y
-300 +’ k

R4 R8 R2
-400 - 6 - <~ *
I 1 I I I I I I 1 I 1 1 1 1 I I I I I 1 1 I
*
02 4 6 810121416182022242828 30 -4W -3@3 -200 -loo 0 100 200 300 403
TIME (rein)
TRANSVERSE RESIDUAL STRESSES (lN/mm’)

FIGURE 6- The strains as a function of time FIGURE 8- The transverse residual stresses of
during the normal continuous cooking process the welded mild steel across the thickness of
the plate (+ tension, - compression).
-280 ) I I I I I I 1 [ I f
-282 Scc ! Scc?
q

DD
0, (7,
-284
&, E, E,
@ -286 K K K
~ -286
~ .290
~ -292 Time Time lime
0 -294 Q o Q
-268 G, o, 0,
-298 e, &, E,
I I
I K E,k K K
-300 I
O
1
6
1
12
I
16
1
24
1
30
#
36
1
42
t
465460
1

TIME (s)
IQ
Time Time Time
FIGURE 7- The detailed strain amplitudes SCC ! (SSRT; CERT) CF 1 CF!
during the normal continuous cooking process
FIGURE 9- The principle differences between
stress corrosion cracking (SCC) and corrosion
fatigue (CF).