Construction and Building Materials 223 (2019) 1030–1037

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Carbonation of magnesium oxysulfate cement and its influence on

mechanical performance
Mingfang Ba, Tao Xue, Zhimin He, Hui Wang, Junzhe Liu ⇑
School of Civil and Environment Engineering, Ningbo University, 315211, China

h i g h l i g h t s

Carbonation improves the mechanical performance of MOS cement to some extent.

Compressive strength increases gradually at first, then decreases during carbonation.

Carbonation increases the toughness of MOS cement paste.

Carbonation refines the meso-pore (=38 lm) volume ratio of MOS cement by 17%.

Mg(OH)2 and basic magnesium oxysulfate phase in hardened MOS cement react with CO2.

a r t i c l e i n f o a b s t r a c t

Article history: In order to popularize magnesium oxysulfate (MOS) cement in civil engineering, it is very necessary to
Received 24 April 2019 investigate its carbonation related durability. It was found that carbonization can increase compressive
Received in revised form 27 July 2019 and flexural strength of MOS cement to some extent and compressive strength of MOS cement increases
Accepted 31 July 2019
gradually at first, then decreases during carbonation process. The displacement to ultimate compressive
Available online 7 August 2019
force of hardened MOS cement paste carbonated for 28 days is larger than that of non-carbonated one at
the same age. Evaporable water testing and X-ray computed tomography (X-CT) were adopted to
Keywords:
examine the porous structure of MOS cement paste with and without carbonation. It was found that
Magnesium oxysulfate (MOS) cement
Carbonation mechanism
carbonation refines the meso-pore (=38 mm meters) volume ratio of hardened MOS cement with 0.5
Mechanical performance water-to-cement ratio by about 17%. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy
Porous structure (FTIR) were adopted to analyze the carbonation characteristics of MOS cement. The results indicate that
magnesium hydroxide and some basic magnesium oxysulfate phase are obviously neutralized with
carbon dioxide to form magnesium carbonate phases in the hardened MOS cement, which leads to the
refined porous structures and corresponding increased toughness.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction
Magnesium oxysulfate (MOS) cement is a kind of air-dried mag-
nesia cement prepared with light-burned magnesium oxide and an
aqueous solution of magnesium sulphate [1–3]. It has the advan-
tages of light weight, low energy consumption, good cohesiveness,
excellent thermal insulation and so on. Compared with magnesium
oxychloride cement, MOS cement does not absorb moisture or
return chlorine, and thus it has little corrosion effects to steel bars
[4–6]. In recent years, many achievements have been made to
improve the mechanical properties and water resistance of MOS
cement by adding modifiers [7–14]. Durability of reinforced con-
crete (RC) structure has always been the most discussed issue since
⇑ Corresponding author.
E-mail address: liujunzhe@nbu.edu.cn (J. Liu).
the past few decades [15,16]. Typically carbonization and chloride
ions are the main causes of steel corrosion damages in Portland
cement concrete structures [17,18]. In general, both above attacks
break the protective film also known as passive film around the
steel and accelerate the corrosion process.
The steel bar will be corroded when the content of Cl reaches
1.5–6.0% for magnesium oxychloride cement [19,20]. Zhen, et al.
[21] and Chang [22] reports that the corrosion resistance of steel
bar of magnesium phosphate cementitious material is better than
that of ordinary Portland cement. The carbonation process of MOS
cement mainly depends on the category and content of hydration
products as well as the structures. Demediuk et al. [23] found that
there are four main types of basic magnesium sulfate in hardened
MOS cement and Urwongse and Sorrel [24] reported that only
3 Mg(OH)2MgSO48H2O (318 phase) is stable at a temperature
of 23 ± 3 °C. Thus it was possible that basic magnesium sulfate

https://doi.org/10.1016/j.conbuildmat.2019.07.341
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037 1031

phases in hardened MOS cement easily reacts with carbon dioxide
diffused in the interior.
Wu et al.[25] found that MOS cement has strong corrosion
resistance to steel bars. Xing et al. [26] studied the effect of molar
ratio of raw materials, nitrite rust inhibitor and wet-dry cycle on
the corrosion characteristics of A3 steel bar discs in MOS cement.
Wu et al.[27] analyzed the phase composition of basic magnesium
sulfate cement paste specimens which were rapidly carbonated for
28 days and found that there was no carbonization phase in the
XRD spectrum of basic magnesium sulfate cement paste. Tomce
et al. [28] analyzed the phase composition of basic magnesium sul-
fate phase (517 phase) in natural environment and found that
there was a carbonate ion vibration peak on the surface of it.
Based on the above analysis, it was indicated that the current
preliminary study on carbonization mechanism of MOS is limited.
Therefore it is very necessary to further study the carbonation
mechanism of MOS cement and consequently its effects on
mechanical performance. In this study, accelerated carbonization
testing was adopted with reference to ‘‘Test Method for Long-
term Performance and Durability of Ordinary Concrete”
(GB50082-2009). The mechanical performance and micro-meso
structural characteristics of MOS cement before and after carbona-
tion were investigated by X-ray diffraction (XRD), Fourier trans-
form infrared spectroscopy (FTIR), X-ray computed tomography
(X-CT) technique and Evaporable water testing method.
2. Experimental
2.1. Raw materials
Industrial grade of magnesium sulfate crystals is from Tianjin in
China and the light-burned magnesium oxide is obtained by calcin-
ing magnesite at 700 °C from Yingkou in China. Their chemical
compositions are shown in Tables 1 and 2.
The particle size distribution and XRD pattern of light-burned
magnesium oxide were shown in Fig. 1.
From this figure it was seen that there was a small amount of
Al2O3 and CaO in light-burned magnesium oxide powder, and the
average particle size of magnesium oxides was about 1–5 lm.
Magnesium oxide includes over-burned MgO and active MgO,
and only active MgO reacts with water to form Mg(OH)2 for 3 h
at 105 °C [29]. Therefore the content of active MgO in this study
can be determined by Eq. (1) to be 61.0%.
 
ðm1  m2 Þ MMgO
AðMgOÞ ¼   100% ð1Þ
m1 MH 2 O
Here m1 and m2 are mass of light burnt MgO before and after
reacting with water for 3 h at 105 °C. MMgO and MH2O is the molec-
ular mass of MgO and water.
2.2. Specimen preparation and analysis
According to the mix proportions of MOS cement paste
shown in Table 3, cylindrical specimens with dimension
of U10 mm  10 mm for Evaporable water testing,
U36 mm  160 mm for carbonation, and prismatic specimens with
dimension of 40 mm  40 mm  160 mm for strength testing were
prepared. After form removal, the specimens were sealed with
fresh-keeping film and placed in room with temperature of
20 ± 5 °C and relative humidity of (70 ± 5)% for 28 days. Then parts
of above specimens were placed in a carbonization box with 20%
CO2 concentration, at 20 °C and 70% relative humidity and the cur-
ing condition of the remaining specimens remain unchanged for
comparing analysis. The changes of pH value at different depths
from the surface of carbonated specimens with dimension
U36 mm  160 mm were analyzed at age of 0 day, 7 day, 14 day
and 28 day carbonation. The mechanical properties of specimens
with and without carbonation were tested at different carbonation
age.

Table 1
Chemical compositions of MgSO47H2O.

Component MgSO4 MgCl2 NaCl Na2SO4 H2O Others

Mass fraction (wt%) 47.85 0.50 0.50 0.50 50.24 0.41

Table 2
Chemical compositions of light-burned MgO.

Component SiO2 MgO CaO Al2O3 Fe2O3 LOI

Mass fraction (wt%) 0.40 96.50 0.85 0.19 0.21 1.85

10000 6
(a) (b)
MgO
8000 Al2O3
Volume ratio /%

4
Intensity(a.u.)

6000

4000
2

2000

0
0

0 20 40 60 80 100 0.25 1 4 16 64 256

Two theata Partical size / m

Fig. 1. XRD Pattern (a), and particle size distribution of Light-burned MgO (b).
1032 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037
Table 3
The mix proportion parameters of MOS cemented materials/g.
No. MgO MgSO47H2O
0.5 371 163
M0.4 371 163
M0.35 371 163
At age of 28-day carbonation, samples at 0–5 mm and 15–
18 mm from the surface of the specimens with and without car-
bonation were taken for XRD and FTIR analysis. The XRD tests of
the samples were performed on Purkinjie general instrument XD-
3 X-ray diffractometer with copper target and the adopted infrared
spectrometer is Nicolet 6700 of Thermo Company, USA.
The Evaporable water content of specimens without carbona-
tion and with 28-day carbonation at the same age were measured.
The macrospore (pore size greater than 150 nm) in the specimen
can be obtained from the fully saturated specimens in 90% relative
humidity (saturated BaCl2) environment. When the total porosity
of the fully saturated specimen is dried at 105 °C to constant
weight, then the capillary porosity (pore size greater than 30 nm
and less than 150 nm) is equal to the total porosity minus the
macro porosity [30].
X-CT was performed on the cylindered samples sawn from
U36m  160 mm specimens with 0.50 water-cement ratio under
28-day carbonation and non-carbonation condition at the same
age. A total of 1080 X-CT images were collected continuously for
each sample. And then with Avizo 9.0 software, 1080 projection
images for each sample were used to carry out the three-
dimensional reconstruction and analysis. The instrument used is
micro X-CT-400 produced by Xradia Company, USA, with a pixel
of 38 mm meter.
3. Results and discussions
3.1. Effects of carbonation on pH changes in MOS cement
Fig. 2 shows the changes of pH value at different depths of the
surface of hardened MOS cement pastes with different carboniza-
tion age. It can be seen that the pH values of the hardened MOS
cement paste before carbonization are all near 10. After carboniza-
tion for a certain age, the pH values at different locations from the
surface decreased significantly, especially at the nearest locations
to surface. It can also be seen from this figure that with the
increase of carbonization age, the pH values at various locations
also show a decreasing trend, which further indicates that the
10.2 Non-carbonization
7d-Carbonization
14d-Carbonization
28d-Carbonization
10.1
pH value
10.0
9.9
9.8
0-5 6-10 11-15 16-18
Different depths from surface /mm
Fig. 2. pH of MOS cement at different depths from surface under different
carbonation age.
hydration products in the hardened MOS cement paste react with
CO2.
H2O
142 3.2. Effects of carbonation on mechanical performance of MOS cement
96
74 The mechanical performance of MOS cement specimens with
different water-cement ratios under carbonization and non-
carbonation conditions at the same age were indicated in Fig. 3.
From Fig. 3(a), it can be seen that the compressive strength of
MOS specimens under 7-day and 14-day carbonation is signifi-
cantly higher than that of non-carbonated specimens with the
same age, especially when the water-cement ratio is 0.5. However,
the compressive strength of MOS specimens with different water-
cement ratios under 28-day carbonization is obviously lower or
close to that of un-carbonated specimens with the same age. This
indicates that with the development of carbonization process, the
compressive strength of MOS cement increases gradually at first,
then decreases. From Fig. 3(b), it can be seen that the flexural
strength of MOS cement specimens with 0.5 water-cement ratio
under carbonation process is lower than that un-carbonated ones
with the same age, while the flexural strength of MOS cement
specimens with water-cement ratio of 0.35 and 0.4 under 14 day
and 28-day carbonization condition is higher than that of non-
carbonated specimens with the same age. This indicates that the
lower the water cement ratio of MOS cement, the greater the
increase of the flexural strength after carbonization compared with
un-carbonated specimens of the same age.
The effect of carbonization on compressive force-displacement
curves of MOS cement with different water-cement ratios was
illustrated in Fig. 4. It can be seen from this figure that the displace-
ment corresponding to the ultimate compressive force of MOS
cement specimens carbonated for 7 days with different water-
cement ratio is much lower than that of the non-carbonated spec-
imens with the same age. As for the displacement corresponding to
the ultimate compressive strength of specimens under 14-day and
28-day carbonation with different water-cement ratio is obviously
larger than that of non-carbonated specimens with the same age.
It can also be seen from Fig. 4 that only when the water cement
ratio is 0.50, the ultimate force of MOS cement under 28-day car-
bonization is higher than that of the noncarbonated specimens
with the same age, and those of the other specimen with different
water-cement ratio decreases accordingly. This indicates that with
the development of carbonation process, the toughness of MOS
cement with different water-cement ratio increases to some
extent.
3.3. Effects of carbonation on microscopic compositions of MOS cement
3.3.1. Microscopic composition of MOS cement with and without
carbonation
Fig. 5 shows the FTIR and XRD spectrum of the hardened MOS
cement paste with 0.5 water-cement ratio at the same age under
28-day carbonation and non-carbonation. The wave range of
anti-symmetric stretching vibration peak of CO2 3 , SO4
2
and
MgO-H are all shown in this figure. It is easy to understand that
the amount of CO2 3 produced by carbonization of MOS cement
can be determined according to the peak strength of CO2 3 anti-
symmetric stretching vibration, i.e. the stronger the peak after car-
bonization, the higher the degree of carbonization. It can be seen
from Fig. 5(a) that the strong CO2 3 anti-symmetric stretching
vibration peak appears at 1400 cm1 position of MOS paste carbon-
ated for 28 day compared with the non-carbonated sample with
the same age, which indicates that the new carbonate phase is
formed due to carbonization of MOS cement.
From Fig. 5(b) it was observed that the main peak strength of
Mg(OH)2 after carbonization is significantly lower than that of
 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037 1033

C/W=0.35 uncarbonation
15
60 C/W=0.35 Carbonation C/W=0.35uncarbonation
C/W=0.40 uncarbonation C/W=0.4 uncarbonation
C/W=0.4 Carbonation
C/W=0.50 uncarbonation
C/W=0.5 Carbonation 12 C/W=0.5 uncarbonation
Compressive strength /Mpa

Flexural strength(Mpa)
50
9 C/W=0.35 carbonation
C/W=0.4 carbonation
40 C/W=0.5 carbonation
6

30
3

20 0
28+0 28+7 28+14 28+28 28+0 28+7 28+14 28+28
Age /day Age(d)
(a) Compressive strength (b) Flexural strength
Fig. 3. Effects of carbonation on mechanical property of MOS cemented materials.

50
+bc28d 50 Bc+ bc28 d
Compressive force /KN

40 +Tc28d Bc+Tc28

Compressive force /KN

40
+bc14 d Bc +bc14 d
30 Bc +Tc14 d
+Tc 14 d 30
Bc+ bc7 d
+ bc 7 d Bc+Tc7 d
20 20
+Tc 7 d Bc
10 10
(b) W/C=0.40
0 (a) W/C=0.35) 0

0.00 0.01 0.02 0.03 0.04 0.05 0.00 0.01 0.02 0.03 0.04 0.05
Displacement /mm Displacement /mm

Bc +bc 28 d Bc +Tc28 d
Bc +bc14 d Bc +Tc14d
50
Bc+bc7 d Bc +Tc7 d
Compressive force /KN

40 Bc

30

20

10

0 (c)W/C=0.50

0.00 0.01 0.02 0.03 0.04 0.05

Displacement /mm
Fig. 4. Effect of carbonization on compressive force-displacement Curve of MOS Cement, 28-day indoor curing + continued indoor curing (Bc + bc), 28-day indoor curing
+ continued carbonation condition (Bc + Tc).

non-carbonated sample with the same age. This indicates that Mg ðn þ 1ÞMgðOHÞ2  MgSO4  ðm þ 1ÞH2 O þ CO2
(OH)2 in MOS cement paste reacts with CO2. It can also be seen ! MgCO3 þ nMgðOHÞ2  MgSO4  mH2 O ð3Þ
from Fig. 5(b) that the content of basic magnesium oxysulfate
phase in MOS cement samples with carbonation is lower than that
of non-carbonation ones with the same age. This further indicates 3.3.2. Microscopic composition of MOS cement from different depth
that Mg(OH)2 and basic magnesium oxysulfate in the MOS cement carbonated 28 day
paste has obviously been carbonated, which is consistent with Fig. 6 shows the FTIR and XRD spectrums of MOS cement sam-
above results of FTIR analysis. The possible carbonation reactions ples with 0.5 water-cement ratio from different depths with 28-
is shown in following Eqs. (2) and (3). day carbonation. It can be seen from Fig. 6(a) that the anti-
MgðOHÞ2 þ CO2 ! MgCO3 ð2Þ symmetrical stretching vibration peak intensity of CO2 3 in the
samples closer to the surface is much stronger, which indicates
1034 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037

- basic magnesium sulphate

0.82 - Mg(OH)2
1.75 carbonation 0.80
MgO

Transmittance(%)
0.78
1.50 - MgCO3

w-0.5
0.76

0.74
1.25
Transmittance(%)

carbonation
0.72 uncarbonation

1.00 0.70
1380 1390

Wave Number(/cm-1)
0.75 2- Carbonization
SO4
0.50 2-
CO3
0.25 MgO-H
uncarbonation
0.00 Non-carbonated
1000 1500 2000 2500 3000 3500 4000
10 20 30 40 50 60 70 80
Wave Number /cm-1 Two theata /
(a) FTIR (b) XRD
Fig. 5. FTIR and XRD spectrum of samples with 0.5 water-cement ratio at the same age under non-carbonation and carbonation.

1.8 0.9
transmittance(%)

1.6 - basic magnesium sulphate

0.8
- Mg(OH)2
1.4
MgO
1.2
Transmittance(%)

0.7
1380
-1
1390 - MgCO3
wave number(/cm )
1.0
0.8
2-
SO4 CO3
2-
0.6
(0-5)mm depths from surface
0.4 0-5 mm depths
0.2 15-18 mm depths MgO-H
0.0 (15-18)mm depths from surface
1000 1500 2000 2500 3000 3500 4000
wave number/cm-1 10 20 30 40 50 60 70 80
Two theata /
(a) FTIR (b) XRD
Fig. 6. FTIR (a) and XRD (b) spectrums of MOS cement with 0.5 water-cement ratio with 28-day carbonation at different depths.

that the sample at the surface obtains much higher carbonation porosity is in the structure of MOS cement paste, and thus the fas-
degree. It is also found that the peak strength of SO2 4 at ter the diffusion of CO2 in it, which leads to the higher degree of
1104 cm1 and MgO-H at 3718 cm1 is significantly lower than carbonization. Therefore the compressive strength of MOS cement
that of samples at deeper position. It can be seen from Fig. 6(b) that samples with high water-cement ratio increases greatly after 7-day
the closer the sample is to the surface of MOS cement specimen and 14-day carbonization.
after 28-day carbonization, the higher the peak strength of MgCO3
is, and thus the higher the content of MgCO3 is. It can also be seen
from Fig. 6(b) that the main peak strength of basic magnesium oxy- 3.4. Effects of carbonation on porous structures of MOS cement
sufate phase in MOS cement at the surface is lower than that at the
position of 15–18 mm depth from the surface. As for X-CT images have a resolution of 38 mm meters, so the
pores tested here by X-CT is defined as mespores. Fig. 8 shows
3.3.3. Microscopic composition of MOS cement with different water- the reconstructed three-dimensional X-CT images of MOS cement
cement ratio paste with 0.5 water to cement ratio under carbonization and
Fig. 7 shows FTIR and XRD spectrums of MOS cement samples at non-carbonation condition at the same age, in which the dark areas
0–5 mm depth with different water-cement ratios under 28-day are the pores. From this figure, it can be seen that the meso-porous
carbonization. From Fig. 7(a), it can be seen that the CO2
3 antisym- volume ratio in hardened paste with carbonation decreases obvi-
metrical stretching vibration peak strength of MOS cement sample ously, especially in the area nearer to the carbonization surface.
with 0.35 water-cement ratio is the lowest, while the CO2 3 It is also found that there is no obvious change in the pore structure
antisymmetrical stretching vibration peak strength of samples at the center of the specimen. Avizo 9.0 software was adopted to
with 0.4 and 0.50 water-cement ratio increases in turn. From the calculate and compare the average porosity of reconstructed
XRD spectrum shown in Fig. 7(b), it was also observed that the images. The results show that the average pore volume ratio of
main peak strength of MgCO3 in sample with 0.40 and 0.50 the specimens without carbonization is 12.74% while that of car-
water-cement ratio is much stronger than that in sample with bonated specimens at the same age decreases to 10.6%. Therefore,
0.35 water-cement ratio. This indicates that the higher the it can be determined that carbonization can refine the mesoporous
water-cement ratio is, the higher carbonation degree is. It is mainly structure of hardened MOS cement paste with 0.5 water to cement
attributed that the larger the water cement ratio is, the larger ratio about by 17%.
 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037 1035

0.82 - basic magnesium sulphate

W/C=0.35

transmittance(%)
0.80
1.4 0.78 W/C=0.5
- Mg(OH)2 ;
0.76 W/C=0.35 MgO
1.2 0.74
W/C=0.4 - MgCO3
Transmittance(%)
0.72 C-O
1.0 1380 1390
-1
wave number(/cm )

0.8
W/C=0.5
0.6 2-
SO4
2- W/C=0.4
0.4 CO3 W/C=0.4
W/C=0.5
0.2

0.0 W/C=0.35
1000 1500 2000 2500 3000 3500 4000 10 20 30 40 50 60 70 80
-1
Wave number /cm Two theata/
(a) (b)
Fig. 7. FTIR (a) and XRD (b) spectrum of MOS carbonated for 28 days with different water-cement ratio.

(a) transverse and longitudinal sections images of sample without carbonation

(b) transverse and longitudinal sections images of sample with carbonation

Fig. 8. Meso porous structures of MOS cement specimen without and with carbonization at the same age.

Fig. 9 shows the pore structure of MOS cement sample with this is consistent with the effect of carbonization on meso-
and without carbonation at the same age by measuring the porosity measured by X-CT techniques. It is well known that
evaporable water content. It can be seen that after carboniza- the coarse porosity was in better accord with the compressive
tion, the proportion of capillary pores in total pore of MOS strength [31]. This may help explain why carbonization can
cement sample with different water-cement ratio increases improve the compressive strength of MOS cement to some
obviously, while the coarse pore porosity decreases. Obviously, extent.
1036 M. Ba et al. / Construction and Building Materials 223 (2019) 1030–1037

0.20 0.25 Total Pore Fine Pore Large Pore

Total Pore Fine Pore large Pore

0.20 (b)
0.15 (a)
Volume Porosity /%

Volume Porosity
0.15
0.10
0.10

0.05
0.05

0.00 0.00
Non-carbonated Carbonization Non-carbonated Carbonization
W/C=0.35% W/C=0.4%
Total Pore Fine Pore Large Pore
0.3
(C)
Volume Porosity

0.2

0.1

0.0
Non-carbonated Carbonization
W/C=0.5
Fig. 9. Effect of carbonization on porosity of MOS cement with different water-cement ratio.

4. Conclusions Declaration of Competing Interest

Carbonization can increase the compressive and flexural The authors declare that they have no known competing finan-
strength of MOS cement to some extent. The higher the water- cial interests or personal relationships that could have appeared
cement ratio of MOS cement is, the more the compressive to influence the work reported in this paper.
strength of carbonated specimens increases at age of 7-day and
14-day carbonation. The compressive strength increases gradu- Acknowledgements
ally at first, then decreases when carbonation progresses. Con-
versely the lower the water cement ratio of MOS cement, the The authors are grateful to Wenjiang Huang, Ph.D candidate from
greater the increase of the flexural strength during carbonation Virginia Tech for his language check. Also, we would like to thank
process. the anonymous reviewers for their thoughtful and valuable
The displacement corresponding to ultimate compressive feedbacks.
force of MOS cement carbonated for 28 days is larger than that
of non-carbonated MOS cement with the same age. It illustrates
that the toughness of hardened MOS cement paste increases by Funding
carbonation. This should be related to the formation of new
phases in hardened MOS cement paste during carbonization, or This work was supported by the Natural Science Foundations of
the corresponding structure changes of some hydration products Zhejiang Province, China (Grants No. LY17E080009, LY17E08007);
after carbonization which needs further study and analysis. Dur- The National Natural Science Foundation of China (Grants No.
ing carbonation process, magnesium hydroxide phase and basic 51778302) and the project supported by K.C. Wong Magna Fund
magnesium oxysulfate phase in MOS cement are neutralized in Ningbo.
with carbon dioxide to form a magnesium carbonate phase,
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