PETROLEUM BRANCH, AIME

Fidelity Union Building

Dallas, Texas
PAPER
NUMBER
THIS IS A PREPRINT --- SUBJECT TO CORRECTION
390-G
Strength Of Oil Well Cements And Additives
Under High Temperature Well Conditions
By
Calvin D. Saunders, Member AIME, and Wayne!. Walker,
Halliburton Oil Well Cementing Co., Duncan, Okla.
Publication Rights Reserved
This paper is to be presented at the Fall Meeting of the Petroleum Branch, American Institute of Min-
ing and Metallurgical Engineers, in San Antonio, Texas, October 17-20, 1954, and is considered the property
of the Petroleum Branch. Permission to publish is hereby restricted to an abstract of not more than 300
words, with no illustrations, unless the paper is specifically released to the press by the Branch Publica-
tions Committee Chairman or the Executive Secretary on his behalf. Such abstract should contain appropriate,
conspicuous acknowledgments. Publication elsewhere after publication in Journal of Petroleum Technology is
granted on request, providing proper credit is given that publication and the original presentation of the
paper.
Discussion of this paper is invited. Three copies of any discussion should be sent to the Petroleum
Branch office: it will be presented at the above meeting with the paper and considered for publication in
Journal of Petroleum Technology.
showed that all types of Portland and oil well ce-
ments tested had much less strength when cured at
320
0
F than when cured at 200
0
F. Also this paper con-
tained data showing some cements had a retrogression
of strength with time as the cement was cured at
320
0
F, with some cements losing more than 50 per cent
of their one-day strength after 14 days. This paper
offered no explanation as to what remedies might be
taken to alleviate or eliminate this strength retro-
gression.
TESTS MADE IN THIS INVESTIGATION
The data gathered and presented here are the
preliminary results of an investigation that has been
instigated to determine whether certain components in
cement are responsible for the low strength at high
temperatures and whether certain additives might be
used with the cement to prevent re.trogression of
strength with time. This was undertaken as an inves-
tigation of different types of cements with and with-
out additives. The additives were thought to offer
a possible remedy so that conventional cements could
more safely be' used under adverse well conditions of
temperature and pressure. The different types of ce-
ment were used in an attempt to ascertain the most
satisfactory clinker composition of cement for deep
well cementing.
ABSTRACT
No definite conclusions are drawn at this time,
but it appears that by the proper selection of addi-
tives for cement, strength loss with age at high tem-
peratures can be either eliminated or considerably
lessened.
Recent tests have shown that the strengths of
cement will decrease with increase in temperature
and age above a critical temperature. The critical
temperature appeared to be approximately 220
0
to
240
0
F.
INTRODUCTION
This paper presents results of tests which were
designed to determine, if possible, the cause and
means for overcoming this strength loss. Various
types of cements and additives were evaluated in this
investigation. These data are the results of tests
made to date in this investigation.
The strength of oil well cement is usually con-
sidered to increase with increasing temperature under
the normal conditions prevailing in an oil well.
Only recently the fact that the strength of the ce-
ment decreases rapidly with high temperature and age
was brought to the attention of the industry. The
data presented in a paper, prepared by the API Mid- Inasmuch as the well conditions which have a
Continent Diatrict StUdy Committee on Cementing Prac- bearing on this work are those of apprOXimately
tices and Testing Oil Well Cements, given at the . 12,000 ft and deeper, there appeared to be no neces-
sity of testing those cements which could not be
References and illustrations at end of paper. handl,ed sufficiently long for in th:l,.s depth
2
STRENGTH OF OIL WELL-CEMENTS AND ADDITIVES UNDER HIGH TEMPERATURE WELL CONDITIONS 390-G
well. Therefore preliminary tests were made to de-
termine the thickening time or handling time of the
various cements with and without additives under
simulated 14,000 ft conditions according to the API
Recommended Practice for Testing Oil Well Cements
[API RP 10 B]. Nevertheless, it was necessary to
test some cements which would not normally be used
at these depths in order to evaluate the effect of
the additives. Also in order to determine the effect
of chemical composition, one series of tests was
made with a modified ASTM Type III cement.
The cements used to date have been: five
brands of slow setting cement, one of which was not
chemically retarded, one ASTM Type I, one ASTM Type
II, and one modified ASTM Type III cement.
Two types of pozzolans were used as additives
with the ASTM Type' I and II cements and a special re-
tarder was also used with these cements in order to
obtain a sufficiently long thickening time.
A number of small autoclaves were used as the
pressure curing vessels, each of which held two 2-in.
cube molds. The slurries were subjected to 3,000 psi
curing pressure [maximum pressure effect] and temper-
atures of 200
0
, 260
0
, 290
0
and 320
o
F. Results of
tests made by the API Subcommittee
l
have shown that
the maximum pressure needed for curing is 3,000 psi.
Curing pressures above this have no appreciable ef-
fect on compressive strengths. The pressure was ap-
plied immediately and the temperature was increased
at the rate of 1 1/2
0
per minute until the final
test temperature was obtained. The test temperatures
and pressure were maintained until the specimens
were ready to be broken at ages of one, three and
seven days. Only compressive strengths measurements
were made and the data presented here are the aver-
ages two or more tests at each condition.
The amount of water used in the slurries con-
taining additives was that which is customarily used
in the field, and for neat slurries the amount des-
ignated by the API RP 10 B. All slurries were con-
sidered satisfactory for normal field usage.
The pozzolans were added in equal abfolute
volume with the cement and this mixture contained 2
per cent bentonite by total weight of cement and poz-
zolan. These blends were tested because'they are
currently being used in field servicing.
PRESENTATION OF DATA
Table 1 shows the thickening time of the var-
ious cements which were evaluated and tested in this
series. As can be seen in this table, all thicken-
ing times were in excess of two hours when tested
under simulated well conditions of 14,000 ft. This
time of two hours or more is considered satisfactory
for normal casing cementing work under well condi-
tions which are comparable to the conditions of
Schedule 8 of the API RP 10 B simulating a 14,000 ft
well. The conditions of the simulated 14,000 ft cas-
ing cementing tests are: a maximum temperature of
206F, which is considered to be the average circu-
lating temperature at the bottom of this depth well,
and a pressure of 13,390 psi. These conditions are
reache4 in a period of 84 minutes which is the theo-
retically calculated time to place 300 sacks of ce-
ment to this depth. These maximum conditions are
gradually attained by increasing the temperature and
pressure at a constant rate until the maximum condi-
tions are reached, after which these conditions are
maintained until the cement slurry reaches a viscos-
ity of 70 poises. A viscosity in excess of 70 poises
is considered too viscous to safely or satisfactorily
handle.
The average bottom hole circulating tempera-
ture of a 14,000-ft well has been found to be 206
0
F
whereas the average static formation temperature is
300
0
F. Cement attains the circulating temperature of
a well as it is placed but acquires the actual static
formation temperature as it sets and gains strength.
For this reason, thickening time tests are made at
circulating temperatures and strength test specimens
are cured at static formation temperatures for wells
of various depths.
COMPRESSIVE STRENGTHS
Tables 2, 3 and 4 give the strengths obtained
on the various cementing slurries cured for one,
three and seven days at various temperatures and un-
der 3,000 psi pressure. These same compressive
strength data are given in graphical form in Figs. 1
through 18. Each chart shows the strength change
with age at various temperatues for a particular ce-
ment or blend. According to these tables and fig-
ures the normal trend is a decrease in strength with
increase in temperature within the range covered by
thege tests. There are some exceptions where the
2900F strengths were higher than those obtained at
260 F, but in general, the strengths did decrease
with increasing temperature.
In general, the slow setting oil well cements
had theogreatest decrease in strength between 200
0
F
and 260 F, with fUrther increases in temperature hav-
ing relatively little effect.
Fig. 8 shows the strengths obtained on the modi
fied ASTM Type III cement. This particular cement
had the least decrease in strength with either age or
temperature of any of the neat cements tested.
The addition of retarder to the Type I and Type
II cements lowered the strenth, of these cements at
, temperatures of 290
0
and 320 F with very little no-
ticeable effect at 200
0
and 260
0
F. Although this ef
fect to be present in the overall strengths
obtained, Figs. 9 and 10 show the 290
0
and 320
0
-F
tests to have less retrogression with age than did
the same neat cements shown in Figs. 6 and 7.
The addition of pozzolans both X and Y tend to
converge the curves with the ASTM Type I cement so
that considerably less variation in strength was no-
ticedwith increase in temperature. Also there was
very little if any retrogression with age when pozzo-
lans were added to type cement. The same condi-
tion was when the pozzolans were added to the
ASTM Type II cement. The average strength of mixtures
390-G CALVIN D. SAUNDERS AND WAYNE A. WALKER 3
.on strength retrogression. The variations considered
were the per cent Tricalcium Aluminate [C1A], Trical-
cium Silicate [C
3
S], Diacalcium Silicate LC
2
S] and
the C
3
S/C
2
S ratio.
containing pozzolan, at ~ l l temperatures tested, was
approximately 2,500 to 3,000 psi regardless of age.
This strength is well in excess of that which is nor-
mally required for successful well casing cementing.
The addition of the special retarder to the pozzolan
cement blends caused a further convergence of the
curves so that still less. change in strength occur-
red with change in temperature. This has been char-
acteristic of all tests made to date. The general
effect of this retarder to these blends was to in-
crease the strength at the higher temperatues of 290
0
and 320F, and a slight lowering of the strength when
cured at 200
0
to 260
0
F.
Table 5 gives a summary or the per cent; change
in compressive strengths between 200
0
and 320
0
F only.
This percentage change is tabulated for one, three
and seven day strengths. The lowest percentage dif-
ference between these two temperature limits was ob-
tained with slurries of Type I and Type II cements to
which retarder and pozzolan had been added. All poz-
zolan cement mixtures had a lower percentage change
at seven days' than did any other cement tested, ex-
cept the modified ASTM Type III. The most retrogres-
sion occurred with cements containing chemical re-
tarders without the addition of pozzolanic additives.
Fig. 21 shows a comgarison of the effect of cur-
ing for seven days at 320 F on the following four
cements:
1. ASTM Type I
2. ASTM Type I with pozzolan and retarder
3. Slow setting oil well cement A
4. Slow setting oil well cement B
Cement A had the most retrogression and cement B had
the least of the slow setting cements tested. These
curves show it is possible to use additives to pre-
vent retrogression in a cement that, otherwise, retro
gresses rather badly [ASTM Type I]. With the addi-
tives, this cement was comparable to the best of the
deep well cements and much better than the poorest
deep well cement.
The cements used had a wide variation in chemi-
cal composition [Fig. 19] and probable clinker compo-
sition [Fig. 20]. These were picked in an attempt to
determine what effect the different compositions had
There appears to be no correlation between the
chemical composition of the cements and the effect
of temperature and time on the strengths. Cements
high in tricalcium silicate were both good and poor
in their ability to withstand high temperatures with-
out drastic change. The same is found when correlat-
ing the other individual cement compounds with cement
performance, or when considering ratios of compounds.
Different types of chemical retarders may af-
fect the ability of cements to safely withstand high
temperatures but this has not been determined in
this initial investigation.
SUMMARY
These data tend to show that it is possible to
lessen the amount of strength retrogression with age
and temperature by the s.election of proper additives
for the cement. Considerably more work is needed
along these lines before any definite conclusions can
be reached as to the most satisfactory remedy for
this purpose. This work is being continued and other
cements and additives will be investigated in an at-
tempt to answer some of the remaining questions and
to find the best materials for use in high tempera-
ture wells.
ACKNOWLEDGMENT
The authors wish to express their appreciation
to the Halliburton Oil Well Cementing Co. for per-
mission to prepare and publish this paper. Apprec-
iation is also extended to those of this organization
who helped obtain data and offered. suggestions for
the preparation of this paper.
REFERENCES
1. The Mid-Continent District Study Committee on
Cementing Practices and Testing of Oil Well
Cements: "Effects of High Temperatures And Pres-
sures on Strengths Of Oil Well Cements," Spring
Meeting API, [1954].
Slow setting cement A
Slow setting cement B
Slow setting cement C
Slow setting cement D
Slow setting cement E
Retarded ASTM Type I
Retarded ASTM Type II
Retarded ~ Type III
Retarded ASTM'I'ype I with Pozzolan X
Retarded ASTM Type I with Pozzolan Y
Retarded ASTM Type II with Pozzolan X
Retarded ASTM Type II with Pozzolan Y
TABLE 1
THICKENING TIME
AT
14,000 FOOT SIMULATED WELL DEPTH
Thickening times
Cement or Blend Hours:M1nutes
3148
2:07
3:46
3:05
2:24
2:54
2;53
2:33
3:18
3:00 +
2:30
3 :_00 +
TABLE 2
24-HOUR COMPRESSIVE STRENGTH - IN PSI
CURl!."'D AT 3,000 PSI AND VARIOUS
TABLE 4
7-DAY COO'RESSIVE STRENG'mS - IN PSI
CURED AT 3,,000 PST AND VARIOUS TEMPERATURES Cpo
200
0
F 260
0
F 290
0
F 320oj!'
7,200 6,930 4,300 2,600
6,500 5,780 2,850 1,540
3,010 2,550 3,320
3,400 2,680 2,260
2,500 1,990 2,850
3,380 2,420 2,940
4,84 4,800
7,020' 4,220
4,650 4,370
320
0
F
1,9.50
3,460
2,300
1,960
2,090
1,910
1,720
2,290
3,040
2,730
2,210
3,240
3,.570
7,900
4,480
2,710
2,100
2,600
2,.530 2,310
1,970 2,000
2,870 2,220
3,1.50 2,810
4,100
2,550
3,.500
2,050
6,250
4,100
3,300
3,100
4,530
2,960
3,770
3,170
3,850
3,.560 3,320
3,8.50 2,290
2,650 3,300
3,5.50 2,960
6,250 4,790 4,480 2,080
7,100 5,310 3,970 1,270
4,680 4,1.50 4,200 3,490
7,350 5,160 3,200 1,310
7,100 4,480 1,410 1,120
200
0
F 260
0
F 290
0
F
11,600
9,600
9,480
8,500
10,120
Cement or Blend
ASTM Type I
ASTM Type II
ASTM Type III
Retarded ASTM I
Retarded ASTM Type II
ASTM Type I with Pozzolan X
ASTM Type I with Pozzolan Y
Retarded ASTM Type I with Pozzolan X
Retarded ASTM Type I with Pozzolan Y
ASTM Type II with Pozzolan X
ASTM Type II with Pozzolan Y
Retarded ASTM Type II with Pozzolan X
Retarded ASTM Type II with Pozzolan Y
Slow setting cement A
Slow setting cement B
Slow setting cement C
Slow setting cement D
Slow setting cement E
2,40
2,030
3,180
3,000
2,550
2,480
3,100
3,450
4,220
3,120
2,140
1,940
2,820
4,400
2,300
3,030
2,580
7,850
5,720
2,750
2,650
5,060
2,680
2,750
2,450
2,240
4,640
4,250
4,120
3,100
6,430
5,350
6,570
4,080
6,900
2,960
3,250
3,620
7,020
4,890
3,390
2,880
3,440
5,750
7,980
4,910
Cement or Blend
ASTM Type I
ASTM Type II
ASTM Type III
Retarded ASTM Type I
Retarded ASTM Type II
ASTM Type I with Pozzolan X
ASTM Type I with Pozzolan Y
Retarded ASTM Type I with Pozzolan X
Retarded ASTM Type I with Pozzolan Y
ASTM Type II with Pozzolan X
ASTM Type II with Pozzolan Y
Retarded ASTM II with Pozzolan X
Retarded ASTM Type II with Pozzolan Y
Slow setting cement A
Slow setting cement B
Slow setting cement C
Slow setting cement D
Slow setting cement E
TABLE 3
72-HOUR COMPRESSIVE STRENGTHS - IN PSI
CURED AT 3,000 PSI AND VARIOUS
TABLE 5
PER CENT CHANGE IN STRENG'mS BETWEEN TEMPERATURES
OF 200
0
AND AT VARIOUS AGES
200
0
F 260
0
F 290
0
F Cement or Blend
Slow setting cement A
Slow setting cement B
Slow Setting cement C
Slow setting cement D
Slow setting cement E
ASTM Type I
ASTM Type II
ASTM Type III
Retarded ASTM Type I
Retarded ASTM Type II
ASTM Type I with Pozzolan X
ASTM Type I with Pozzolan Y
Retarded ASTM Type I with Pozzolan X
Retarded ASTM Type I with Pozzolan Y
ASTM II with Pozzolan X
ASTM II with Pozzolan Y
Retarded ASTM Type II with PozEolan X
Retarded ASTM Type II with Pozzolan Y
10,780
8,070
9,010
8,950
8,420
6,630
7,600
4,950
7,480
6,800
3,680
3,590
2,690
3,310
3,400
3,430
2,600
3,400
6,030
4,160
3,220
3,100
5,800
.5,100
5.240
3,.580
6,280
4,760
3,460
2,680
3,240
2,630
3,150
2,620
2,530
2,840
6,340
4,050
2,730
2,430
2,810
5,530
5,920
4,360
3,750
2,000
3,290
2,440
3,200
3,680
2,940
2,660
3,1.50
3,6.50
320
0
F
3,260
3,620
2,470
1,770
'2,060
3,400
2,.540
4,020
1,610
1,3.50
2,220
1,940
3,000
3,100
2,470
2,1.50
2,810
3,210
Cement or Blend
Slow setting cement A
Slow setting cement B
Slow setting cement C
Slow setting cement D
Slow setting cement E
ASTM Type I
ASTM Type II
ASTM Type III
Retarded ASTM Type I
Retarded ASTM Type II
ASTM Type I with Pozzolan X
ASTM Type I with Pozzolan Y
Retarded ASTM Type I withPozzolan X
Retarded ASTM Type I with Pozzolan Y
ASTM Type II with Pozzolan X
ASTM Type II with Pozzolan Y
Retarded ASTM Type II with Pozzolan X
Retarded ASTM Type II with Pozzolan Y

-38.8
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T
STRENGTH VS. AGE
SLOW- SETTING CEMENT A
10
P

e
I
x
/

...-
I
-
....
---
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6
-- -- --
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2 -
0
0
I
AGE IN DAYS
FIRURI" 3
COMPRESSIVE STRENGTH VS. AGE
SLOW-SETTING CEMENT C
10
-
/'
/'
x
e
J
I
V

6
z
/
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a:

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I
AGE IN DAYS
FIAlIRI" 5
COMPRESSIVE STRENGTH vs. AGE
SLOW-SETTlNG CEMENT E
10
---

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I
AGE IN DAYS
FIGURE 2
COMPRESSNE STRENGTH VS.AGE
SLOW- SETTING CEMENT B
10
..-.

---
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II
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x
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e /
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AGE IN DAYS
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COMPRESSIVE STRENGTH VS. AGE
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AGE IN DAYS
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COMPRESSIVE STRENGTH VS.AGE
ASTM -T't.PE 1:
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AGE IN DAYS
FIGURI;: .,
COMPRESSIVE STRENGTH VS. AGE
ASTM-TYPE :II:
10

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if
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AGE IN DA'tS
101 r.IIRIO 8
COMPRESSIVE STRENGTH VS. AGE
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AGE IN DA'tS
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COMPRESSIVE STRENGTH VS. AGE
RETARDEO ASTM-TYPE J:
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._.
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AGE IN DA'tS
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COMPRESSIVE STRENGTH VS.AGE
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IS
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AGE IN DA'tS
FIGURE II
COMPRESSIVE STRENGTH VS.AGE
ASTM-TYPE X WITH POZZOLAN X
10

8
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if
I

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...... 280"1
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AGE IN DA'tS
I=I(,IURE 12
COMPRESSIVE STRENGTH VS.AGE
ASTM - TYPE "I: WITH POZZOLAN Y
10

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if
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AGE IN DA'tS
FI(.;URF 13
COMPRESSIVE. STRENGTH VS. AGE
RETARDED ASTM-TYPE 1: WITH POZZOLAN X
10

8
x

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AGE IN DAYS
FI(.;URF 14
COMPRESSIVE STRENGTH VS. AGE
RETARDED ASTM-TYPE I WITH FOZZOLAN Y
10

8
x

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AGE IN DAYS
FIGURE 15
COMPRESSIVE STRENGTH VS. AGE
ASTM-TYPE I[ WITH POZZOLANX
10

8
x

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AGE IN DAYS
FI(.;[]RE 16
COMPRESSIVE STRENGTH VS. AGE
ASTM-TYPE It WITH POZZOLAN Y
10

8
x

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AGE IN DAYS
FIGURE 17
COMPRESSIVE STRENGTH VS. AGE
RETARDED ASTM-TYPE It WITH POZZOLAN X
10

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x

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AGE IN DAYS
FIGURE 18
COMPRESSIVE STRENGTH VS. AGE
RETARDED ASTM-TYPE I[ WITH FOZZOLAN Y
10

8
x

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AGE IN DAYS
FIc:lLJRF 19
I
CHEMICAL ANALYSIS
I
I
OF CEMENTS
I .",
en
193'1
I-
ffi60
;::
I. SLQ-SET CEMENT A
w 2. "
" "
B_
0
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u."",
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5. II
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z
6. ASTM TYPE I
- 0
F
7.
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~ 40
8.
u
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m
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0
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30
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W
0
0::
20 w
a-
10
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rT n
nrrTHlllHnlln
12345678 12345678 12345678
0
SILICON IRON ALUMINUM CALCIUM MAGNESIUM SULFUR LOSS ON
DIOXIDE OXIDES OXIDE OXIDE OXIDE TRIOXIDE IGNITION
FIc:lLJRF :>0
CLINKER COMPOSITION OF CEMENTS
~
LOSS FREE BASIS
0::
EllIJII
w
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AB CO
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U
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0 A BGD E IlIm
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iii
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ABCOE IlIlII
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10
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I r nil rfh ABCOEllIm ABCOEllIm
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0
I I HHI I n n1TIl n I n,...,----n,....
1
TRICALCIUM D1CALCIUM TETRAau..GIUM TRICALCIUM CALCIUM MAGNESIUM
SILICATE SILICATE ALUMINUM ALUMINATE SlJLFATE OXIDE
FERRITE
FIGURE 21
COMPARISON OF STRENGTH VS. AGE
OF FOlJl CEMENTS CURED AT ~ < f F
10
~
x B
iii
a.
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B
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w T WITH POZZOLAN Y.
IX:
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til
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.AGE IN DAYS