(PDF) ASTM C 88 Test On Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate - A Study of The Mechanisms of Damage

1/12/2018 (PDF) ASTM C 88 Test on Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate: A Study of the Mechanisms of Damage
See all › See all › See all › Join for free Login
Download citation Share Download full-text PDF
5 Citations 21 References 12 Figures
Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate: A Study of the Mechanisms of
able) in Journal of ASTM International 2(1) · January 2005 with 1,115 Reads

2517
ation
Harvey Hilbert Haynes

ean
7.51 · Haynes & Associates LLC
e mechanisms of damage to aggregate particles by sodium sulfate and magnesium sulfate solutions
ed. By using glass and aluminum containers to represent aggregate pore space and confining walls,
wed that during soaking cycles crystal growth occurred that applied some bearing pressure on the
bearing pressure, however, was secondary to more damaging pressure that occurred during the oven
During soaking cycles, mirabilite (Na 2 SO 4 10H 2O) applied bearing pressures up to about 0.6 MPa.
ying cycles, thenardite applied bearing pressures up to about 2.0 MPa. Magnesium sulfate salts
ng pressures about the same magnitude as that of the sodium sulfate salts.
orld's research
members
n publications
arch projects
ee
by Harvey Hilbert Haynes Author content
+8
https://www.researchgate.net/publication/249956516_ASTM_C_88_Test_on_Soundness_of_Aggregate_Using_Sodium_Sulfate_or_Magnesium_Sulf… 1/22
dium sulfate Physical properties of Specific gravity of sodium Summary of peak strains in
m sulfate… sodium sulfate and… sulfate and magnesium… glass and aluminum…
d by Harvey Hilbert Haynes Author content

Download full-text PDF
Journal of ASTM International, January 2005, Vol. 2, No. 1

Paper ID JAI12517
Available online at www.astm.org
arvey Haynes1
STM C 88 Test on Soundness of Aggregate Using Sodium

ulfate or Magnesium Sulfate: A Study of the Mechanisms of
amage
ABSTRACT: In this study, the mechanisms of damage to aggregate particles by sodium sulfate and
magnesium sulfate solutions were investigated. By using glass and aluminum containers to represent
aggregate pore space and confining walls, test results showed that during soaking cycles crystal growth
occurred that applied some bearing pressure on the container. This bearing pressure, however, was
secondary to more damaging pressure that occurred during the oven drying cycles. During soaking
cycles, mirabilite (Na2 SO4.10H2O) applied bearing pressures up to about 0.6 MPa. During oven drying
cycles, thenardite applied bearing pressures up to about 2.0 MPa. Magnesium sulfate salts produced
bearing pressures about the same magnitude as that of the sodium sulfate salts.
KEYWORDS: ASTM C 88, force of crystallization, physical salt attack, magnesium sulfate, salt
crystallization, salt hydration distress, salt weathering, sodium sulfate, soundness test
troduction
In 1828, Brard [3] used sodium sulfate, magnesium sulfate, and other salts to test masonry
ne for durability against weathering. The method consisted of placing pieces of stone in
iling solutions of saturated salt, and then allowing the stone to dry naturally. Salt
ystallization at or near the surface of the stone caused a scaling type of distress, much like that
freezing and thawing. Stone that showed relatively large amounts of scaling were rejected for
e in structures.
Variations of the Brard test have been used by geologists to study damage to stone by salt
athering [4,14]. Using sodium sulfate or magnesium sulfate solutions, ASTM Standard C 88
s introduced in the 1930s to test the soundness of aggregate. The mechanism of distress was
lieved to be an increase in the salt volume on conversion from a lower hydrate phase to a
gher phase.
In nature, this volume increase can occur by hydration of salts exposed to changes in ambient
mperature and relative humidity, or by formation of crystals in solution. When in solution, the
m crystallization applies to both the formation of crystals by nucleation and by growth of
isting crystals.
A description of the ASTM C 88-99a [1] test follows. The test starts by using oven-dried
gregate that has cooled to room temperature. The aggregate is sieved and weighed and then
bmerged in a saturated solution of sodium sulfate or magnesium sulfate at 21 ± 1°C for a
riod of 16–18 h, removed from the solution, allowed to drain, and placed in an oven at 110 ±
C until dry. After drying, the aggregate is cooled to room temperature, submerged again for
–18 h, and then oven dried. This process is repeated for a number of cycles that are specified
the purchaser (usually five cycles). The aggregate particles are washed to remove the salt and
en sieved and weighed to determine the amount of breakdown of aggregate particles.
nuscript received 22 December 2003; accepted for publication 23 September 2004; published January 2005.
rincipal, Haynes & Associates, Oakland, CA 94611.
yright © 2005 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.
JOURNAL OF ASTM INTERNATIONAL
Garrity and Kriege [5] presented the conventional view of damage by the C 88 test. They
marily studied sodium sulfate. Distress was considered the result of an accumulation of
dium sulfate in the pores of the aggregate particles from cycles of soaking and drying.
entually sufficient thenardite (Na2SO4) existed in aggregate pores so that during the
bsequent soaking cycle, when mirabilite (Na2SO4·10H2O) was formed, the volume of
rabilite would exceed the volume of the aggregate pore. Mirabilite would thus apply a bearing
essure to the aggregate pore walls and cause damage. Calculations showed that after the third
aking cycle, mirabilite would over-fill the pore space.2
Wuerpel [18] expressed a similar opinion regarding the mechanism of damage after
rforming C 88 tests using magnesium sulfate.
ASTM C 88-99a states that when using magnesium sulfate the test is usually more severe
an with sodium sulfate. The reason magnesium sulfate is more aggressive has not been
termined. Past studies have mainly used sodium sulfate to study the distress mechanism
17,14,15], likely because this salt is less complex than magnesium sulfate.
rpose
The purpose of this investigation was to determine the mechanism, or mechanisms, of
mage caused by sodium sulfate and magnesium sulfate. These salts are known to cause
gradation of stone in the field [6], and sodium sulfate is known to cause physical salt attack to
ncrete [8,9]. Few studies, if any, have produced convincing evidence of the actual mechanism
damage.
operties of Sodium Sulfate and Magnesium Sulfate

Table 1 summarizes various properties of sodium sulfate and magnesium sulfate.
nversion of anhydrous or lower hydrate phases of salt to higher hydrate phases results in an
crease in crystal volume. For example, the conversion of thenardite (Na2SO4) to mirabilite
a2SO4·10H2O) yields an increase in crystal volume of 315 %. However, it should be
entioned that the change in total volume of water and thenardite combining to form mirabilite
a decrease of 5.6 %. Similarly with magnesium sulfate, the conversion of kieserite
MgSO ·H O) to epsomite (MgSO ·7 H O) yields an increase in crystal volume of 159 %;

MgSO4·H2O) to epsomite (MgSO4·7 H2O) yields an increase in crystal volume of 159 %;
wever, the change in total volume of water and kieserite combining to form epsomite is a
crease of 10.9 %.
The solubility curves of sodium sulfate and magnesium sulfate are shown in Fig. 1, and
ecific gravity curves are shown in Fig. 2. For sodium sulfate at 20°C, a saturated solution
curs at 19.06 g anhydrous salt per 100 g H2O, and for magnesium sulfate, 33.70 g anhydrous
t per 100 g H2O. After oven drying, thenardite remains for sodium sulfate, while kieserite
mains for magnesium sulfate, and on a volume basis, 127 % more kieserite is deposited than
enardite. Thus, aggregate pore volume that is flooded with saturated solutions and then oven-
ed will more rapidly accumulate kieserite than thenardite.
Table 1 gives heat of crystallization data for sodium sulfate and magnesium sulfate at 18°C
d infinite dilution. Crystallization of mirabilite is exothermic at –78.5 kJ/mol, while
he present author found errors in Garrity and Kriege’s calculation methodology. Revised calculations were made,
ich are not given in this paper, that showed aggregate void space did not become filled or over-filled with
drated salt regardless of the number of cycles.
HAYNES ON ASTM C 88 TEST 3
ystallization of thenardite is endothermic at 1.9 kJ/mol. For epsomite, crystallization is

othermic at –13.3 kJ/mol, while kieserite is endothermic at 58.6 kJ/mol [13]. The C 88 test is
nducted at saturated solution concentrations, which has the effect of reducing the heat of
ystallization. Myerson [12] provided a value of heat of crystallization of –73 kJ/mol for
rabilite at near saturated conditions.
TABLE 1—Physical properties of sodium sulfate and magnesium sulfate.

Salt, Stable Temp. Stable Molecular Molecular Density of Heat of Coefficient of
Phases Phase, ºC Mass, g/mol Volume Crystal, Crystallization* Thermal**
[12] cm3/mol g/cm3 kJ/mol [13] Expansion,
µm/m/ºC
dium Sulfate
Thenardite, 32.4 to 220 142.04 53.0 2.680 + 1.9 28.8
Na2SO4
Mirabilite, 0 to 32.4 322.19 220.1 1.464 -78.5 …
.
2SO4 10H2O
Magnesium
Sulfate
Anhydrous, >180 120.36 45.3 2.657 +88.3 …
MgSO4
Kieserite, 68 to 180 138.40 56.6 2.445 -58.6 23.1
MgSO4.H2O
exahydrite, 48.6 to 68 228.48 129.8 1.760 +2.3 …
gSO4.6H2O
Epsomite, 1.8 to 48.3 246.49 146.7 1.680 -13.3 …
gSO4 .7H2O
decahydrate, –3.9 to 1.8 336.57 … … … …
gSO4 .12H2O
ndothermic and – exothermic.
xperimental values determined herein, see Appendix A.
FIG. 1—Solubility of sodium sulfate and magnesium sulfate [10].
FIG. 2—Specific gravity of sodium sulfate and magnesium sulfate [10].
perimental Scope-of-Work
C 88 tests were conducted using glass and aluminum containers, which represented aggregate
re space and the confining wall. The volume used for simulated pores was 150 cm3. Tests
ng sodium sulfate and magnesium sulfate were conducted. Two to four duplicate tests were
ade for each test condition. Thirteen total tests were conducted, where each test consisted of
7 cycles of soaking and oven drying.
st Set-up
Glass and aluminum containers were instrumented with three strain gages and three
ermocouples. The strain gages were mounted on the exterior wall of the container for
ngential strain measurement and were located at distances of 7, 13, and 19 mm from the inside
ttom of the container. The thermocouples were mounted on the inside of the container wall
ectly opposite a strain gage. Figure 3 shows the test set-up for the glass containers.
Strain and temperature readings were taken at 20 s intervals during the soaking cycles and
s during the oven drying cycles. The thermocouples provided temperature measurements that
peared to vary randomly by about ± 1.5°C. These data were smoothed by a running average of
readings before temperature corrections were made to the strain readings.
Temperature corrections to strain readings were made by the following procedure. Glass and
uminum containers were subjected to temperature cycles of 22–120°C while empty, filled with
0 cm3 of water, and filled with 150 cm3 of saturate salt solution. The raw strain versus
mperature relationships were linear and essentially equal for the empty and filled containers.
uations representing the average curve for glass and for aluminum were determined, and these
uations were used to correct individual raw strain measurements for temperature effects during
e C 88 cycles. All strain data presented herein have been temperature corrected.
Ad
FIG. 3—Test set-up using glass containers. Strain gages and thermocouples were located at
13, and 19 mm from the inside bottom of the container. A similar arrangement was used for
e aluminum containers.
st Results and Discussion

dium Sulfate
Soaking Cycles—Soaking cycles started when saturated solution at 20°C was added to the
ntainers,
riod such that
of about 24 the total allotted
h was volume offorsolution
soakingand
tooven-dried salt (thenardite)
observe mirabilite was 150
formation. cm3. A
Figure 4
presents the fourth soaking cycle using a glass container, and it shows typical behavior of
ain in the container and temperature in the salt as a function of time.
Temperature Behavior—At the start of the cycle, just after the saturated solution was added
the container, there was an immediate temperature increase. This temperature increase was
e to exothermic behavior from dissolution of thenardite and crystallization of mirabilite.
Without an increase in temperature, a thermodynamic imbalance would not have existed to
solve thenardite, because the added solution was already saturated at 20°C. With an increase
temperature, the salt solution was able to hold a higher concentration of ions. Once the
mperature of the solution began to decrease, supersaturation of the solution permitted further
ystallization of mirabilite.
An important observation was that only a limited amount of oven-dried thenardite dissolved
ring the soaking cycle. The conventional view of the C 88 test was that thenardite dissolved
tirely [5]. Experimentally, two methods showed the limited dissolution of thenardite. The first
ethod measured the height of the oven-dried salt in the container before saturated solution was
ded and then again at the end of the soaking cycle. These measurements were approximate,
cause the surface of the salt was rough. A small increase in height of the crystals at the end of
e soaking cycles was observed (Fig. 5). A greater height change was anticipated if all
enardite converted to mirabilite because the size of mirabilite crystals was about four times the
e of thenardite crystals3.
FIG. 4—Strain in glass container and temperature of sodium sulfate during the fourth
aking cycle of a simulated C 88 test.
FIG. 5—Height of sodium sulfate salt in glass container at the beginning and end of soaking
cles.
lso, at the end of the soaking cycles, a thin layer of translucent salt was observed on the surface of white salt.
enardite is opaque and white, while mirabilite is translucent. Hence, this observation indicated that a shell of
abilite deposited on the surfaces of thenardite.
The second method measured relative temperature behavior of two forms of thenardite
ring a soaking cycle. Experience working with sodium sulfate showed that when mirabilite
ed at room conditions (about 20ºC and 50 % RH), the resulting thenardite was light and fluffy
texture. This air-dried thenardite contrasted with thenardite formed at oven drying conditions,
hich resulted in a hard, dense mass of salt. (This hard mass of thenardite was strain gage
trumented for determination of coefficient of thermal expansion. See Appendix A.) The bulk
ecific gravity of air-dried thenardite was about 1.0, and oven-dried thenardite was about 2.1.
he specific gravity of thenardite is 2.68.) Hence, the surface area of air-dried thenardite was
nsiderably greater than that of oven-dried thenardite.
A separate soaking-cycle test was conducted where an equal mass of air-dried thenardite
placed oven-dried thenardite at the start of the third soaking cycle. Figure 6 shows the
mperature behavior during the initial 8 h for both the air-dried and oven-dried thenardite test.
relatively larger amount of heat was generated by the air-dried thenardite compared to that of
e oven-dried thenardite. The additional heat showed that more air-dried thenardite dissolved
d more mirabilite crystallized. Or, in other words, only a limited portion of the oven-dried
enardite dissolved. The reason oven-dried thenardite remained undissolved was because a shell
mirabilite encapsulated the thenardite and prevented rapid dissolution. It was not determined
hether all air-dried thenardite dissolved; however, white salt was observable within translucent
t, so it was assumed that some air-dried thenardite also remained at the end of the cycle.
FIG. 6—Temperature of oven-dried and air-dried sodium sulfate during a third soaking
cle.
Interestingly, the maximum temperature in the air-dried thenardite test was about 32.4°C,
hich corresponds to the phase change from mirabilite and thenardite (Fig. 1). During the test,
hen the temperature exceeded 32.4°C, thenardite would form, and mirabilite would dissolve.
th of these activities are endothermic. If the temperature decreased below 32.4°C, mirabilite
ould crystallize, and thenardite would dissolve; both of these activities are exothermic. Thus,
e temperature was self-regulated at about 32.4°C for approximately 30 min before the
mperature steadily decreased to ambient room temperature.
Strain Behavior—Strain behavior of the container showed that the salt applied a bearing
essure to the container wall (Fig. 4). The maximum strain in the wall, called the peak strain,
s about 120 µm/m.
During this fourth soaking cycle, the salt in the container ranged in height from about 15–20
m (Fig. 5), yet the strain gage at 19 mm did not measure appreciable strain. Strain was
easured by gages at 7 and 13 mm from the bottom of the container. This indicated that the salt,
ar the top of the salt mass, did not push on the container wall.
The increase in bearing pressure with time could be attributed to crystal growth at the
erface of salt mass and container wall. Becker and Day [2] demonstrated that crystal growth
n apply bearing pressure, and Taber [16] and Hansen [7] discussed the mechanism. A
cessary condition is that supersaturated solution exists at the site of crystal growth.
The solubility of sodium sulfate increases as pressure increases. For this test set-up, the top
the salt mass had a bearing pressure of essentially zero. Hence, the top surface of the salt mass
ould have grown preferentially to the wall and bottom. This would probably occur with
fficient time; however, the test measurements were taken during significant thermodynamic
balance.
Table 2 summarizes the peak strains. For soaking cycles in glass containers, sodium sulfate
owed an average peak strain of 70 ± 40 µm/m, when the peak strains were averaged for cycles
and higher. The maximum peak strain of all the cycles was 150 µm/m. For aluminum
ntainers, the average and maximum peak strains were higher because these containers had a
ger diameter and thinner wall thickness than that of the glass containers. Hence, for the same
agnitude of bearing pressure, the strain would be greater in the aluminum containers. Later in
s paper, the maximum peak strains will be used to predict bearing pressures applied by the
ts.
TABLE 2—Summary of peak strains in glass and aluminum containers during soaking and
ying cycles.
Sodium Sulfate Magnesium Sulfate

Type of No. of Tests/ Avg. of Peak Max. Peak No. of Avg. of Peak Max. Peak
Cycle and Cycles* Strains from Strain µm/m Tests/ Strains from Strain µm/m
Container Cycles µm/m Cycles* Cycles, µm/m
Soaking
Glass 4 / 18 70a ± 40 150 a 2/8 110 a ± 60 200 a
Aluminum 4 / 16 130 a ± 60 300 a 3 / 12 290 a ± 130 480 a
Drying
Glass 4 / 13 240 b ± 110 430 b 2/8 270 c ± 140 430 c
2/8 260 d ± 80 380 d
Aluminum 4 / 11 110 b ± 40 200 b 3 / 12 840 d ± 220 1200 d
*Total number of cycles used in averaging peak strains. For each test, strain data from the 1st and 2nd cycles were
not used in the averages.
a
Crystal growth of mirabilite or epsomite.
b
Coefficient of thermal expansion of thenardite.
c
Coefficient of thermal expansion of salt mass composed of kieserite, epsomite, and hexahydrite during first 2 h
of oven drying as the temperature increased to about 75ºC.
d
Crystal growth of magnesium sulfate dihydrate at temperatures above 85°C.
Oven Drying Cycles—Behavior of the solution–salt mass system was more complex during
en drying than during soaking. When glass containers were used, the containers broke during
e oven drying cycles. Four tests were conducted with glass containers, and the containers broke
cycles #3, 4, 7, and 7.4
The glass containers broke in a similar manner. Although vertical cracks were found in the
ntainers, it appeared that the significant crack was circumferential around the bottom of the
ntainers near the wall to bottom transition. This circumferential crack gave the appearance of
e wall being pushed out too far or the bottom being pushed off, or both.
Figure 7 shows strains and temperatures in a glass container during the sixth drying cycle.
e temperature of the salt showed three plateaus. The first plateau, at about 80°C, was due to
aporative cooling. (At 9 h the abrupt increase in temperature was due to tightly closing the
en door, which was inadvertently ajar.) The second plateau was at a temperature of about
5°C, which was caused by the formation of a salt crust that spanned the container and
creased the effects of evaporative cooling. The third plateau, at about 110°C, was after all
O evaporated.
Drying cycles typically required two days to complete because evaporation was significantly
ndered by the formation of the salt crust. When a salt crust was intentionally broken, the
mperature of the salt solution decreased to about 80°C. Garrity and Kierge [5] also observed
https://www.researchgate.net/publication/249956516_ASTM_C_88_Test_on_Soundness_of_Aggregate_Using_Sodium_Sulfate_or_Magnesium_Su… 10/22
e formation of salt crusts.
FIG. 7—Strain in glass container and temperature of sodium sulfate during the sixth oven
ying cycle.
rior to this experimental program, exploratory tests were conducted on glass containers without instrumentation.
otal of 16 containers broke during oven drying cycles using sodium sulfate, magnesium sulfate, and sodium
bonate. Containers did not break using sodium chloride.
Strain behavior basically followed temperature. During increases in temperature, the strains
the container increased. A large portion of the salt mass at the start of oven drying cycles was
enardite, which was surrounded by a shell of mirabilite. As the oven temperature increased
m room temperature to 32ºC, thermal expansion of this salt mass caused the salt to push
ainst the glass container. As the temperature rose above 32.4°C, mirabilite melted, and the
ain in the container decreased. Only thenardite remained, and with further increases in
mperature, thermal expansion caused thenardite to push against the container. The coefficient
thermal expansion of thenardite was determined as approximately 28.8 µm/m/°C (Appendix
. The coefficient of thermal expansion of Pyrex glass is 3.4 µm/m/ºC. Hence, expansion of
enardite was considerably greater than the increase in the diameter of the glass container for a
ven change in temperature5.
This mechanism of applying load to the container wall was verified by the tests using
uminum containers. Thenardite applied a bearing pressure to the aluminum container that was
s than that applied to the glass container. This was shown by the peak strain data (Table 2).
e coefficient of thermal expansion of aluminum was 23.9 µm/m/°C, so the aluminum
ntainers expanded more than the glass containers, and the thenardite was not as highly
nfined.
Table 2 shows the average peak strain for the glass container was 240 ± 110µm/m, and the
aximum peak strain was 430 µm/m. For the aluminum container, the average peak strain was
0 ± 40 µm/m, and maximum peak strain was 200 µm/m. For mineral aggregates, such as
anite, the coefficient of thermal expansion ranges from 2–12 µm/m/°C and for sandstone from
14 µm/m/°C. The glass container at 3.4 µm/m/°C was closer to representing aggregate than
at of the aluminum container at 23.9 µm/m/°C. Hence, damage would occur to aggregate by
ermal behavior of thenardite during oven drying.
During the first and second temperature plateaus, the strains slowly decreased. This was
ely due to creep relaxation of the mass of thenardite. During the third temperature plateau,
er all H2O had evaporated, the oven-dried mass of thenardite did not show creep relaxation.
Two glass containers broke during the temperature increase from the first to second plateau
0–105°C), and two containers broke during the temperature increase from the second to third
ateau (105–110°C).
agnesium Sulfate
Soaking Cycles—Figure 8 represents the third soaking cycle using a glass container, and it
ows typical behavior of strain in the container and temperature of the salt as a function of time.
the start of the cycle, just after saturated solution was added to the container, which held
en-dried kieserite, there was an increase in temperature of the solution. This activity was
milar to that of the sodium sulfate test, but the rate of temperature gain was slower with
agnesium sulfate. The temperature increased for the first ½ h, which was related to kieserite
solving and epsomite crystallizing. Both activities were exothermic. The maximum
mperature at about 31ºC was within the stable range of temperatures for epsomite (1.8–
.3ºC).
the coefficient of thermal expansion of the salt and the container material were equal, then an increase in
meter of the salt mass would equal the increase in diameter of the container for a given change in temperature.
FIG. 8—Strain in glass container and temperature of magnesium sulfate during the third
aking cycle.
The initial strains, which occurred during the temperature increase, were likely related to
ermal expansion of the mass of kieserite, which was surrounded by a shell of epsomite. As the
mperature decreased to room temperature there was a slight decrease in strain in the container,
hich was related to thermal behavior. When the strains started to increase again at about 2 to 3
this was from slow crystal growth of epsomite from the supersaturated solution. The strains
creased to a peak strain of about 200 µm/m at 23 h., when the cycle was stopped.
Table 2 summarizes the peak strains. For the glass containers, the average peak strain was
0 ± 60 µm/m, and the maximum peak strain was 200 µm/m. For the aluminum containers, the
ak strains were greater because of the thinner wall thickness and larger diameter.
Oven-Drying Cycles—Figure 9 shows the strains and temperatures in a glass container

ring the fifth drying cycle. The temperature behavior showed the same general features as that
sodium sulfate, but not as pronounced. The first temperature plateau was at about 95°C, the
cond about 108°C, and the third about 115°C.
As a reminder, at the end of the soaking cycles, the salt mass was mostly kieserite with a
ell of epsomite (and perhaps some metastable hexahydrite). During the beginning of the oven
ying cycle, the initial strains in the container were due to thermal expansion of the salt mass as
e temperature increased from room temperature to about 68°C. The coefficient of thermal
pansion of epsomite is not known; however, the coefficient for kieserite was determined to be
out 23.1 µm/m/°C (Appendix A).
FIG. 9—Strain in glass container and temperature of magnesium sulfate during the fifth oven
ying cycle.
Figure 9 shows that at a temperature of about 68°C, the strains started to decrease to zero.
bove 48°C epsomite is unstable, and above 68°C hexahydrite is unstable, so these crystals
idently melted, and the remaining mass of kieserite was not in contact with the glass wall.
ter the temperature increased above about 85°C and during the following 3.5 h (from 1.5–5.0
the strains increased steadily to a maximum of 320 µm/m. This increase in strain indicated
at a hydration phase of magnesium sulfate was crystallizing and applying a bearing pressure on
e container. This increase in strain was not related to thermal behavior. It appeared that the
etastable dihydrate phase was crystallizing. Evidence of magnesium sulfate dihydrate was
own at 18 h, when the strain started decreasing to zero. The dihydrate phase lost H2O, and a
lume decrease occurred. The dihydrate phase reportedly melts at a temperature of 112°C [18],
hich was the approximate temperature of the salt at the time of strain decrease. Once all
aporable water was lost, the temperature increased slightly to 115°C (at about 26 h). At this
ndition, kieserite was the remaining phase. Kieserite is stable to 180°C.
Table 2 summarizes the average and maximum peak strains that occurred during the initial
ermal expansion stage and during the crystallization stage. Strains from both stages were
milar in magnitude.
The aluminum containers showed different behavior than that of the glass containers during
e crystallization stage; here the bearing pressure of the salt caused yielding of the aluminum.
gure 10 shows the second drying cycle in an aluminum container. The strain in the aluminum
adily increased over a period of 55 h and reached 1100 µm/m. Again, this increase in strain
s not related to thermal behavior. Upon removal of load, much of the strain was permanent.
uring subsequent oven drying cycles, the peak strain increased substantially.
FIG. 10—Strain in aluminum container and temperature of magnesium sulfate during the
cond oven drying cycle.
Two glass containers were tested, and one container broke at the end of cycle #4 and the
her at cycle #6. Both containers broke when the temperature just started to increase from the
cond to the third plateau. During exploratory tests, some glass containers with magnesium
fate broke earlier in the oven drying cycle, during the time of crystallization of magnesium
fate dihydrate.
alculations of Salt Bearing Pressures

Empirical data are scarce on bearing pressures of salt, also called forces of crystallization.
is study calculated the bearing pressures by using the strain data from the glass and aluminum
ntainers. A structural model of the containers was analyzed using the general purpose finite
ment program SAP 90.
The models represented one-quarter of a glass or aluminum container, where the base was
e to move horizontally, but not vertically. A salt mass in the glass container had a height of
.1 mm, and in the aluminum container 17.8 mm. It was assumed that the salt applied a
iform bearing pressure on the container wall. This assumption did not model actual
nditions, as the strain data showed a non-uniform distribution of bearing pressures. The effect
the results was to underestimate the bearing pressures actually applied to the containers.
The glass containers had an interior diameter of 64.0 mm, height of 88.9 mm, and wall
ckness of 2.30 mm. The aluminum containers had an interior diameter of 71.4 mm, height of
.1 mm, and wall thickness of 0.76 mm. The modulus of elasticity and Poisson’s ratio for glass
s 64.0 GPa and 0.20, respectively, and for aluminum 69.0 GPa and 0.33.
The calculations were made using an assumed bearing pressure of 0.7 MPa. For this loading
ndition, the maximum tangential strain in the glass container was calculated as 150µm/m, and
the aluminum container as 500 µm/m. Using the maximum peak strain in the containers, the
perimental bearing pressures of the salts were calculated by proportion.
Table 3 shows the bearing pressures of the salts, as calculated from maximum peak strains.
summary, during soaking cycles mirabilite developed a bearing pressure of about 0.6 MPa,
d epsomite 0.8 MPa. During oven drying, thenardite and kieserite showed a bearing pressure
about 2.0 MPa caused by thermal expansion. The bearing pressure from crystallization of
agnesium sulfate dihydrate was about 1.8 MPa in the glass containers. However, it was during
s portion of the test that the bearing pressure caused yielding of the aluminum container wall.
nce, the greatest bearing pressure occurred, which means it was greater than 2.0 MPa, but no
imated bearing pressure is given. Bearing pressures that developed during oven drying were
o to three times those during soaking cycles.
During soaking cycles the ambient temperature was representative of field conditions, so the
aring pressures of 0.6 and 0.8 MPa for mirabilite and epsomite can likely occur in the field to
use salt weathering of rocks, concrete, and other materials. However, oven drying is an
ificial condition, so the bearing pressures of 1.8 MPa or greater would not likely be
perienced in the field.
scussion on Improvement of ASTM C 88 Test

Past studies to improve the repeatability and reproducibility of the C 88 test [5,18,14,15]
vestigated parameters deemed important by the conventional view of distress, which
mphasized factors related to the soaking cycles. Much effort was misdirected because the
esent study has shown that the oven drying cycles were more damaging. Improvements in
ecision are possible by evaluating parameters related to oven drying.
The current C 88 method of drying to constant mass, which is defined as achieving a mass
s of less than 0.1 % of sample mass in a 4 h drying period, does not assure complete removal
all evaporable water. Complete drying is a significant parameter when using sodium sulfate
cause the most damaging stage of the test occurred at the temperature increase related to
aporation of all water. Without complete drying, this stage is missed. The formation of salt
usts slows the evaporation of water, such that longer than expected time periods may be
quired for oven drying.
Temperature control during oven drying is also important. Temperatures above the permitted
aximum of 115°C may cause extra damage from thermal expansion because the change in
mperature from the second to the third plateau will be larger than typical. Temperatures less
an the permitted minimum of 105°C may cause less damage. It may also be found that the
rmitted temperature range of 105–15°C is too great, that is, damage caused at 115°C may be
nificantly greater than that caused at 105°C.
It appears that a C 88 test using magnesium sulfate should be less sensitive to oven drying
nditions than that of sodium sulfate because the test was relatively independent of the
aximum oven temperature and the range of oven temperatures of 110 ± 5°C. Damage by
agnesium sulfate was related to thermal expansion of kieserite at low temperatures (20–75ºC)
d to crystal growth of magnesium sulfate dihydrate at temperatures above about 85°C. In fact,
STM C 88-99a shows better precision for magnesium sulfate than for sodium sulfate, which
pports the above reasoning.
Another parameter for investigation is the removal of oven-dried salt from the pores of
gregate by washing with water at the end of the test. The oven-dried salts do not dissolve
ickly.
TABLE 3—Calculated bearing pressures by sodium sulfate and magnesium sulfate.

Cycle and Salt Container Max. Peak Strain Calculated Bearing Pressure
in Container, µm/m of Salt, MPa
Soaking
Mirabilite Glass 150 0.7
Aluminum 300 0.4
Average = 0.6a
Epsomite Glass 200 0.9
Aluminum 480 0.7
Average = 0.8b
Drying
Thenardite Glass 430 2.0c
Aluminum 200 …d
Magnesium Sulfate Glass 430 2.0c
Dihydrate Glass 380 1.8e
Aluminum 1200 …f
a
Bearing pressure due to crystal growth of mirabilite.
b
Bearing pressure due to crystal growth of epsomite.
c
Bearing pressure due to thermal expansion of salt.
d
Bearing pressure not given because aluminum container expanded only slightly more than thenardite, so
calculated bearing pressure was low.
e
Bearing pressure due to crystal growth of magnesium sulfate dihydrate.
f
Bearing pressure not calculated because aluminum container showed considerable yielding.
mmary
Experimental tests were conducted using glass and aluminum containers to represent
gregate pore space and wall. All tests on glass containers resulted in the glass breaking during
e oven drying cycles.
This investigation found that the mechanisms of damage by the ASTM C 88 test were
fferent than those of the conventional view. It was shown by experiment that oven-dried salt
owed limited dissolution during soaking cycles in saturated solution, that a shell of hydrated
t formed on the oven-dried salt during soaking cycles, and that crystal growth of hydrated salt
wly applied a bearing pressure to the container, yet this pressure was not the primary damage
echanism. Maximum damage occurred during the oven drying cycles. Here, sodium sulfate as
enardite caused damage due to thermal expansion. The coefficient of thermal expansion of
enardite was larger than that of glass and aluminum, and, for that matter, mineral aggregate.
uring oven drying, when the oven temperature was constant, two stages occurred that resulted
increases in temperature of the salt system. The first stage was formation of a salt crust that
duced evaporative cooling effects, and the second stage was complete evaporation of water.
e resultant temperature increases caused thenardite to bear more strongly against the container
ll. For magnesium sulfate, the damaging processes were due to thermal expansion at the
ginning of the oven drying cycle when temperatures were less than 68°C, and then due to
ystallization of magnesium sulfate dihydrate at temperatures above about 85°C.
Strain measurements from the containers were used to calculate the experimental bearing
essure of the salts. During soaking cycles, the hydrated salts showed bearing pressures that
wly increased to about 0.6 MPa for mirabilite and 0.8 MPa for epsomite. During the oven
ying cycles, sodium sulfate and magnesium sulfate salts showed a bearing pressure of about
0 MPa.
Previous observations that magnesium sulfate is more damaging than sodium sulfate during
88 tests can be explained by these findings. First, magnesium sulfate solutions deposited a
eater volume of salt after each soaking and drying cycle than that of sodium sulfate. Hence,
e bearing pressure applied by magnesium sulfate, which was essentially similar in magnitude
that of sodium sulfate, created more damage because the pressure acted on a larger area of the
gregate pore walls. Second, magnesium sulfate solutions caused damage at lower temperatures
an sodium sulfate solutions. The magnesium sulfate test was less dependent on controlling
aximum oven temperature and obtaining completely dry test samples, so more repeatable test
ults could be expected than from the sodium sulfate test.
knowledgments
Appreciation is extended to Dr. Julio Miranda of New Dynamics, Fremont, CA, for his
uctural analysis of the containers, and to Mr. Perry Joiner, technician, for his assistance with
trumentation and data reduction.
ferences
ASTM Standard C 88-99a, Test Method for Soundness of Aggregates by Use of Sodium
Sulfate or Magnesium Sulfate, Annual Book of ASTM Standards, Vol. 4, No. 2, 2003, pp.
42–46.
Becker, G. F. and Day, A. L., “The Linear Force of Growing Crystals,” Proceedings of the
Washington Academy of Sciences, Vol. VII, 1905, pp. 283–288.
Brard, “On the Method Proposed for Immediate Detection of Stones Unable to Resist the
Action of Frost,” Annales de Chimie et de Physique, 38, 1828, pp. 160–192.
Evans, I. S., “Salt Crystallization and Rock Weathering: A Review,” Revue de
Geomorphologue Dynamique, 19, 1970, pp. 155–177.
Garrity, L. V. and Kriege, H. K., “Studies of the Accelerated Soundness Tests,” Highway
Research Board, Vol. 15, 1935, pp. 237–258.
Goudie, A. and Viles, H., Salt Weathering Hazards, John Wiley & Sons, Chichester, 1997.
Hansen, W. C., “Crystal Growth as a Source of Expansion in Portland Cement Concrete,”
ASTM Proceeding, Vol. 63, 1963, pp. 932–945.
Haynes, H., O’Neill, R., and Mehta, P. K., “Concrete Deterioration from Physical Attack by
Salts,” Concrete International, Vol. 18, No. 1, January 1996, pp. 63–68.
Hime, W., Martinek, R. A., Backus, L. A., and Marusin, S. L., “Salt Hydration Distress,”
Concrete International, Vol. 23, No. 10, October 2001, pp. 43–50.
0] Linke, W. F., Solubilities: Inorganic and Metal-Organic Compounds, American Chemical
Society, 4th ed., 1964.
1] Montillon, G. H. and Badger, W. L., “Rate of Growth of Crystals in Aqueous Solution,”
Industrial and Engineering Chemistry, TP 1.I6, Vol. 19, July 1927, pp. 809–816.
2] Myerson, A. S., Handbook of Industrial Crystallization, Butterworth-Heineman, 1993, p. 4.
3] Perry, R. H. and Green, D. W., Chemical Engineering Handbook, 6th ed., McGraw-Hill
Book Co., New York, 1984.
4] Price, C. A., “The Use of Sodium Sulfate Crystallization Test for Determining the
Weathering Resistance of Untreated Stone,” UNESCO/Rilem International Symposium
Determination and Protection of Stone Monuments, Reilure, Paris, 3.6, 1978, 23 pp.
5] Sheftick, W., “Na2SO4 Soundness Test Evaluation,” Cement, Concrete, and Aggregates,
Vol. 11, No. 1, ASTM International, West Conshohocken, PA, 1989, pp.73–79.
6] Taber, S., “The Growth of Crystals Under External Pressure,” American Journal of Science,
Vol. XLI, 1916, pp. 532–557.
7] Walker, S. and Proudley, C. E., “Studies of Sodium and Magnesium Sulfate Soundness
Tests,” Appendix II, Report of Committee C-9, ASTM Proceeding, Vol. 36, Part 1, 1936, pp.
327–338.
8] Wuerpel, C. E., “Factors Affecting the Testing of Concrete Aggregate Durability,”
Appendix II, Report of Committee C-9, ASTM Proceeding, Vol. 38, 1938, pp. 327–351.
ppendix A
efficient of Thermal Expansion of Thenardite and Kieserite
The coefficient of thermal expansion of thenardite and kieserite was experimentally
termined by using oven-dried samples of the salts. These samples were instrumented with
ain gages and cycled though the temperature range of 22–110°C. In addition, samples of
rbon steel and glass and aluminum from the containers were instrumented and cycled along
th the salt samples. Raw strains versus temperature measurements were plotted for each
aterial, and linear relationships were found. A slope to each curve was obtained that
presented raw strain per °C.
The experimental coefficients of thermal expansion for the salts were determined by using a
ethod of differences. Steel was used as the known condition, where the coefficient of thermal
pansion for carbon steel was 11.7 µm/m/ºC. Table A shows the data and method of
fferences. The experimental coefficients for glass and aluminum were near those of handbook
lues. The coefficient of thermal expansion for thenardite was determined as 28.8 µm/m/°C,
d for kieserite 23.1 µm/m/˚C.
TABLE A—Determination of coefficient of thermal expansion of thenardite and kieserite.

Material Slope to Curve of Raw Strain Experimental Coefficient of Handbook Value of
Versus Temperature, µm/m/ºC Thermal Expansion, µm/m/ºC Coefficient of Thermal
Expansion, µm/m/ºC
Steel, Carbon –1.3 13.0* – 1.3 = 11.7 11.7a
Glass, Sodium –10.7 13.0 – 10.7 = 2.3 3.4b
Borosilicate
Aluminum, +10.9 13.0 + 10.9 = 23.9 19.5 – 24.2b
3003-0
Oven-Dried
Thenardite,
Sample #1 +17.4 13.0 + 17.4 = 30.4
Sample #2 +14.2 13.0 + 14.2 = 27.2
Average = 28.8
Oven-Dried +10.1 13.0 + 10.1 = 23.1
Kieserite
his coefficient of thermal expansion represents that of the strain gage itself, and its value was selected because it
ve the proper coefficient of thermal expansion for carbon steel.
anual of Steel Construction, American Institute of Steel Construction, New York, 6th ed., 1964, p. 6.11.
allister, W. D., Jr, Materials Science and Engineering: An Introduction, John Wiley & Sons, 4th ed., 1997, pp.
8–789.
References (21)
ete treatment of sodium sulfate phase transitions with corresponding crystallization pressure
function of temperature and of the anhydrous sodium sulfate phase (III or V) is given elsewhere [35].
alts, such as magnesium sulfate, can behave analogously [36][37][38][39][40] [41] . ...
mage in practice: A theoretical insight into laboratory tests

available
Francesco Caruso · Robert J. Flatt · Michael Steiger
act
e invariably effective in destroying any type of rock?
c Spec Publ
ki Oguchi
act
e salt-free stone is 12.0 ± 0.4 lm/m°C. The CTE of the salt-bearing stone is expected to be larger, since
erally have a larger CTE than carbonate stones (e.g., CTE of kieserite is 22 lm/m°C according to
The composite model according to Hashin (1983) predicts the CTE of the saltbearing stone as a
olume fraction of stone Environ Earth Sci (2011) 63:1463–1473 1467 and salt. ...
-wetting of magnesium sulfate salts lead to damage of stone?

available
ON EARTH SCI
George W. Scherer · Rosa M. Espinosa-Marzal · Eric Doehne
act
e salt-free stone is 12.0 ± 0.4 lm/m°C. The CTE of the salt-bearing stone is expected to be larger, since
erally have a larger CTE than carbonate stones (e.g., CTE of kieserite is 22 lm/m°C according to
The composite model according to Hashin (1983) predicts the CTE of the saltbearing stone as a
olume fraction of stone Environ Earth Sci and salt. ...
-wetting of magnesium sulfate salts lead to damage of stone?

available
Geol
George W. Scherer · Rosa M. Espinosa-Marzal · Eric Doehne
ulus and the thermal expansion coefficient of thenardite are 43.4 GPa [13] and 28.8 ppm/˚C [14] ,
persaturation, solution density and water activity were computed through the Pitzer model [15]. ...
essure Exerted by in-Pore Confined Crystals

available
erer · Rosa M. Espinosa-Marzal
act
Recommended publications
Discover more publications, questions and projects in Magnesium Sulfate
Article Full-text available

Sulfate attack on concrete: Laboratory versus field experience
January 2002
Harvey Hilbert Haynes
View full-text
Physical salt attack on concrete

January 2011
Harvey Hilbert Haynes · M. T. Bassuoni
View full-text
Article
Research evaluation of physical corrosion of soluble salt substance to concrete
September 2008 · Corrosion and Protection
Y.-H. Liu · M.-X. Shi · K.-L. Ma · Y.-J. Xie
The physical deterioration mechanism, characteristics salt, experimental methods, appraisable index and main
influencing factors of soluble salt crystallization corrosion to concrete reviewed. The transmission process of
deleterious ions in concrete, crystallization dynamics of salt solution in concrete and updating experimental methods
are necessary to be further studied. The experimental ... [Show full abstract]
Read more
Forces of hydration that can cause havoc in concrete

January 2003 · Concrete International
Dipayan Jana · B. Erlin
View full-text
Discover more
Ad
About Support Business solutions
News Help center Recruiting

Company FAQ Advertising
Careers
© ResearchGate 2018. All rights reserved. Imprint · Terms · Privacy

(PDF) ASTM C 88 Test On Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate - A Study of The Mechanisms of Damage

Încărcat de

Informații document

Titlu original

Drepturi de autor

Formate disponibile

Partajați acest document

Partajați sau inserați document

Opțiuni de partajare

Vi se pare util acest document?

Este necorespunzător acest conținut?

Drepturi de autor:

Formate disponibile

(PDF) ASTM C 88 Test On Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate - A Study of The Mechanisms of Damage

Încărcat de

Drepturi de autor:

Formate disponibile

1/12/2018 (PDF) ASTM C 88 Test on Soundness of Aggregate Using Sodium Sulfate or Magnesium Sulfate: A Study of the Mechanisms of Damage

able) in Journal of ASTM International 2(1) · January 2005 with 1,115 Reads

Harvey Hilbert Haynes

by Harvey Hilbert Haynes Author content

d by Harvey Hilbert Haynes Author content

Journal of ASTM International, January 2005, Vol. 2, No. 1

STM C 88 Test on Soundness of Aggregate Using Sodium

JOURNAL OF ASTM INTERNATIONAL

operties of Sodium Sulfate and Magnesium Sulfate

MgSO ·H O) to epsomite (MgSO ·7 H O) yields an increase in crystal volume of 159 %;

HAYNES ON ASTM C 88 TEST 3

ystallization of thenardite is endothermic at 1.9 kJ/mol. For epsomite, crystallization is

TABLE 1—Physical properties of sodium sulfate and magnesium sulfate.

FIG. 1—Solubility of sodium sulfate and magnesium sulfate [10].

JOURNAL OF ASTM INTERNATIONAL

FIG. 2—Specific gravity of sodium sulfate and magnesium sulfate [10].

HAYNES ON ASTM C 88 TEST 5

st Results and Discussion

JOURNAL OF ASTM INTERNATIONAL

HAYNES ON ASTM C 88 TEST 7

JOURNAL OF ASTM INTERNATIONAL

Sodium Sulfate Magnesium Sulfate

HAYNES ON ASTM C 88 TEST 9

e formation of salt crusts.

JOURNAL OF ASTM INTERNATIONAL

HAYNES ON ASTM C 88 TEST 11

Oven-Drying Cycles—Figure 9 shows the strains and temperatures in a glass container

JOURNAL OF ASTM INTERNATIONAL

HAYNES ON ASTM C 88 TEST 13

alculations of Salt Bearing Pressures

JOURNAL OF ASTM INTERNATIONAL

scussion on Improvement of ASTM C 88 Test

HAYNES ON ASTM C 88 TEST 15

TABLE 3—Calculated bearing pressures by sodium sulfate and magnesium sulfate.

JOURNAL OF ASTM INTERNATIONAL

HAYNES ON ASTM C 88 TEST 17

TABLE A—Determination of coefficient of thermal expansion of thenardite and kieserite.

mage in practice: A theoretical insight into laboratory tests

Francesco Caruso · Robert J. Flatt · Michael Steiger

e invariably effective in destroying any type of rock?

-wetting of magnesium sulfate salts lead to damage of stone?

-wetting of magnesium sulfate salts lead to damage of stone?

essure Exerted by in-Pore Confined Crystals

erer · Rosa M. Espinosa-Marzal

Article Full-text available

Article Full-text available

Physical salt attack on concrete

Article Full-text available

Forces of hydration that can cause havoc in concrete

About Support Business solutions

News Help center Recruiting

© ResearchGate 2018. All rights reserved. Imprint · Terms · Privacy

S-ar putea să vă placă și