Waste Management, Vol. 16, No. 8, pp.

749-756, 1996
1997 Elsevier Science Ltd
All rights reserved. Printed in Great Britain
0956-053X/96 $15.00 + 0.00

Pergamon
PIh S0956-053X(97)00021-4

ORIGINAL CONTRIBUTION

THE INFLUENCE OF MIX PARAMETERS AND

BINDER CHOICE ON THE CARBONATION OF
CEMENT SOLIDIFIED WASTES

L. C. Lange 1, C. D. Hills 2. a n d A. B. P o o l e 1
IGeomaterials Unit, Engineering Department, Queen Mary and WestfieM College, Mile End Road, London, U.K., E1 4NS
2Civil Engineering Department, Imperial College of Science, Technology and Medicine, Exhibition Road, London, U.K., SW7 2BU

ABSTRACT. This paper explores the kinetics of carbonation of cement-based solidified hazardous waste. This study is part
of a wide investigation into the effects of carbonation on solidified waste forms. Two commercially produced heavy metal
wastes were solidified with three different types of Portland cement and two mineral admixtures and carbonated under
controlled conditions. Measurements of the uptake of carbon dioxide were made for the different mixes and areas showing
the degree of carbonation for each cement system were defined. The effects of water/binder ratio, waste and binder type on
both total uptake of carbon dioxide and rate of carbonation were investigated and are discussed. 1997 Elsevier Science Ltd

INTRODUCTION

ted on the role of CO2 in the hydration and

polymerisation of silicates, using cements doped
with single metal solutions. ~1,12 Work involving real
industrial waste has, however, not been carried out
to any great extent, even though carbonation could
be beneficial to certain cement-based waste systems
by, for example, incorporating waste species into a
carbonate phase by a mechanism involving solid
solution reactions with calcite. 13 This is believed to
result in improved chemical bonding of certain metal
cations within the components of the cement
matrix. 14 Also, carbonation appeared to overcome
severe retardation effects through acceleration of the
hydration reaction of C3S 9 and by generally improving mechanical and chemical properties of blended
and non-blended cement-solidified materials. 15
Based on these investigations and bearing in mind
the importance of improving the quality of solidified
materials, the application of a rapid carbonation
technique to cement-based systems has been used to
study the effects of carbonation on waste-forms.
When accelerated carbonation was used for cement
mortars, some authors observed that for different
water/cement (w/c) ratios and compaction moulding,
significant strength values could be generated within
minutes. 16,17 These result from the reaction of C3S
and fl C2S, which hydrate extensively, according to
the equation below. The overall stoichiometry of the
reaction of the silicate phases in cement indicates
that initial carbonation is accompanied by hydration

Cement-based solidification is frequently the technology of choice for immobilising soils and sludges
containing a variety of metal pollutants.~ This process is flexible, effective, accommodates complex
mixtures of contaminants and is economical enough
to be used for large volumes of waste. 2 Many workers 3-8 have tried to elucidate both individual and
synergistic effects of waste species on cement-based
binder systems in order to improve and extend the
solidification process. Nevertheless, at the present
time the mechanisms of fixation in operation during
the solidification/stabilisation are not completely
understood.
One phenomenon associated with Portland
cement-based materials that is receiving special
attention because of its potential effects on the properties of waste forms is atmospheric carbonation.
Through observations by our group and elsewhere it
has also been noticed that waste containing heavy
metals has an increased susceptibility to carbonation. 9,1 Most of the studies to date have concentra-

RECEIVED 21 NOVEMBER 1996; ACCEPTED 26 MARCH 1997.

*To whom correspondence may be addressed. Fax: 0171-594
6053; e-mail: c.hills@ic.ac.uk2
Acknowledgements--The help o f Dr A. Maries, from Trafalgar
Technology Ltd., is gratefully acknowledged. L. C. Lange wishes
also to thank the Brazilian Government, CAPES, for a
studentship.

749

L. C. LANGE E T AL.

750

TABLE 1

and is followed, after some delay, by secondary carbonation

C3S+ yH20+ (3-x)CO2

P CxSHy+ (3-x)CaCO3

+ zCO2

:
~

C(x_z)SHy+ zCaCO3

It was also suggested that the rate of carbonation

was limited by diffusion, and the rate of hardening in
a carbon dioxide atmosphere dependent on penetration of carbon dioxide into the material. In practice,
carbonation is a complex process and very much
dependent on the nature of the type of cement and,
for example, the porosity, permeability, w/c ratio 1s-2
of the product and environmental conditions, such as
humidity and carbon dioxide pressure. 21,22
The purpose of the present work was to study the
kinetics o f the carbonation reaction under normal
environmental conditions (atmospheric pressure and
room temperature) on two industrial wastes, which
were solidified with varying proportions of three different types of Portland cement and two mineral
admixtures. Isotherms relating to the degree of carbonation were defined and used as a basis for comparing waste forms produced from different waste
cement mixes. 23 In this work, the process governing
the diffusion of CO2 into waste forms is discussed
with reference to water/binder and waste/binder
ratios for the different systems examined.
EXPERIMENTAL

The samples were prepared from OPC (ordinary

Portland cement), WOPC (white Portland cement)
and SRPC (sulphate-resistant Portland cement), all
supplied by Blue Circle (UK) Ltd. Their Bogue and
oxide analyses are given in Table 1. PFA (pulverised
fuel ash, Ready Mixed Concrete), GGBS (granulated
blast-furnace slag, Civil and Marine Ltd.) and two
industrial wastes, which were supplied as mixedmetal hydroxide filter cakes, were also used.
Waste 1 was a neutralised, commercially blended
and solidified waste, of approximately 55% (w/w)
solids, composed predominantly of heavy metals originating from sources such as electroplating, galvanising and metal finishing operations. This particular
batch of waste material had a pH of 8.0 and an aqueous soluble TOC of 2.0mg1-1. Anions such as
chloride (419mgl-l), sulphate ( l l l 2 m g 1 - 1 ) and
nitrate (648 mg 1-1) were known to be present. Waste
2 was of 30% (w/w) solids, and produced from a
primarily zinc plating process. The pH of the material was 8.4, an aqueous soluble TOC of 1.1 mg 1-I
and anions such as chloride (24.7mg1-1), sulphate
(725 mg 1-1) and nitrate (2362 mg 1-1). Both wastes
were oven-dried at 105C to constant weight and
then ground using a pestle and mortar to a particle

Analysis of Cements Used

Cements

OPC

WOPC

SRPC

Supplier

Blue circle

Blue circle

Blue circle

Phase
C3S %
C2S %
C3A %
C~,F %
CA %
Cl2A7%
C2A5%
Oxide
si02 %
A1203%
Fe203%
CaO %
Free Lime
MgO %
AlkaliEq.*
so3 %
IR*"
LOI'*

52
19
7
6

64
22
4.4
1.1

57
19
0
17

20.4
4.1
2.1
63.8
1.5
2.1
0.6
2.9

24.5
1.9
0.35
68.7
2.5
0.55
0.2
2.0

21.4
3.6
5.7
64
0.6
0.7
0.5
2.0

0.4
3.2

<0.1
1.0

0.6
1.5

*Alkali equivalent, Na20+0.658 K20; **IR, insoluble residue %;

LOI, loss on ignition %.

size of less than 500/zm. The metal contents of the

wastes were determined in triplicate using a Philip PV
8050 Inductively Coupled Plasma Emission Spectrometer, (ICP-AES) after acid digestion in HNO3 and
HC1. 24 The mean of these results are given in Table 2
for selected metals. Hg was analysed using a Cold
Vapor Atomic Absorption ( C U A A ) - - U N I C A M - SOLAR 939. The prepared wastes were dry-mixed by
hand with the different cements and mineral admixtures prior to the addition of water in sealable sample
bags prior to analysis. Mix moisture was provided by
the addition of double-distilled water and samples
were again mixed by hand. Control (waste-free)
mixes were also prepared using the same binders and
TABLE 2
Met~ Con~ntofD~ W ~ ( m g k g -I)

Metals
Sr
Cr
Cu
Mn
Ni
Pb
Sb
Zn
Cd
Ba
As
Hg*

Waste 1

Waste 2

215
6638
8650
3137
4825
3265
1201
19,475
1025
575
7464
2514

175
11,275
175
1,675
312
288
25
410,000
ND
125
200

ND

*Cold vapor atomic absorption (CUAA) used to analyseHg.

INFLUENCE OF MIX PARAMETERS AND BINDER CHOICE ON CARBONATION

a fine inert sand (< 500/zm) to replace the waste. A

wide range of mixes were used to prepare samples in
triplicate and the addition ranges for the different
compounds are represented in Table 3. Figure 1
shows the mix designs chosen.
After mixing samples were submitted to a standard
compaction pressure of I MPa. However, for samples
with w/b (water/binder) ratio higher than 0.4 this
standard compaction was not applied, to avoid the
evolution of bleed water.
Immediately after preparation the samples were
placed in a Eudiometer designed to measure gas uptake,
and consisting of a gas syringe coupled to a chamber
which holds a small cylindrical sample of cement
paste (20 10 mm in size). The syringe, which is filled
with CO2 gas, is interfaced to a computer which displays in real-time graphics the progressive consumption of carbon dioxide.25 The work was conducted at
normal atmospheric conditions in a laboratory, i.e.
normal atmospheric pressure and room temperature
(21C+2) and a relative humidity Rh of 55% +5.
Samples with very high w/b ratio were constantly
agitated by hand during carbonation to avoid the
sedimentation of any material at the bottom of the
sample holder. Every tenth sample consisted of a
control sample to ensure the reproducibility of the
method. The samples were analysed in triplicate and
a 95% confidence interval was applied to estimate the
range within which the true mean may be found.

Waates or Smld

10

OPC
WOPC
SRPC
PFA
GGBS
Waste 1
Waste 2
Water/binder (w/b) ratio

70

40

60
50

6O

~)

70

~)

80

B~ndecs

2O

10

20

30

~4)

50

60

70

80

90

Water

Note Binders = Cement : Cement + Admixtures

F I G U R E 1. Ternary diagram showing the mix designs investigated

in this work.

From an examination of different mixes (Fig. 1), it

was possible to define three distinct fields related to
the degree of carbonation of the samples and they are
illustrated in Fig. 3(a-g). They are nominated as:
H = highly carbonated; M = moderately carbonated

C 02 Uptake: OPC and Waste 1

10

w/c ratio

0~0

w/c ratio = 1,0

40

2O

60

80

100

Time (rain.)
CO2 Uptake: WOPC and Waste 1
12
-- 10
8
w/c ratio = 0 . 2 0

L'-

2
0

20

40

60

0 = 1.0

80

100

Time (min.)
CO2 Uptake: SRPC and Waste 1

Composition r a n g e - - % (w/w)
5-80
5-80
5-80
15
40
10-80
10-80
0.07-3.0

50

TABLE 3
Range of Material Compositions in the Cement Solidified Wastes
Tested
Materials

8o

30

Figure 2 shows eudiometer traces for three mixes

consisting of OPC, WOPC and SRPC and waste 1, at
two different w/c (water/cement) ratios. It can be
seen that during the first 15min, the carbonation
reaction was extremely rapid, and that the induction
time (the interval between mixing and the start of the
reaction) was extended at higher w/c ratios. OPC and
SRPC appear to react more quickly with CO2 at the
lower w/c ratio than WOPC.

9o

20

8 2

RESULTS

751

12
10
8
~ 6
~ 4

o!
0

/
20

40

60

80

100

Time (rain.)
Binders are defined as cement only or cement + P F A or cement +
GGBS, P F A and GGBS were used at a fixed proportion of 15%
and 40%, respectively.

F I G U R E 2. Rate of CO2 consumption for mixes at w/c of 0.2

and 1.0.

L . C . LANGE E T AL.

752
a) Control

b) OPC/admixtures/Waste1

Sand

Waste I

Generalarea
foundfor all
binders

37

7% 7X0

47

4\

70

P=<0.1%

[ ] OPC/WI HI=I0-15%
N~0
[ ] OPC/PFA/WIH2=8-11~
X 0 [ ] OPC/GGBS/W1H3=9-13eh

1V
20////

5y

AHI~

60"

~'-Y

Binders 10

20

I
30

40

c) OPC/admixtures/Waste2

50

70

80

90

Water Binders 10

Waste2
1

20////

20

30

40

d) WOPC/admixtures/WasteI
[ ] OPC/W2 HI =6-9%
[ ] OPC/PFA/W2H2 = 5-6%

x~0

50

60

10

20

30

40

50

90

Water

Waste I

3y

20
M__0A_4%

f~0

80

Xo

'

Binders

70

[ ] WOPC/WI HI =6-8%
[ ] WOPC/PFA/Wl H2 = 5 - 6%
~1 WOPC/GGBS/WI H3 = 6 - 8%

/ XO [] OPCIGGBSIw2H3~8-12%

4~30

N 10
60

X0

30
20

90/

X 0

707

.......X

60

70

80

90

Water

Binders

10

20

X
X,0

30

40

50

60

70

80

90

Water

FIGURE 3 (a--d). Ternary diagrams for the different waste/binder systems showing the effect of mix proportions on the degree of
carbonation.

and P = poorly carbonated. To further illustrate these

results, Fig. 4 shows the maximum CO2 uptake in %
by weight of solids after 100min for selected
mixes. 16-20
The waste-free control specimens exhibited a relatively uniform behaviour for all types of binders
examined. The uptake of CO2 increased for lower w/
b ratios and higher content of cement.
The addition of waste 1 to OPC (blended and
non-blended) caused a marked change in the uptake
of CO2. For OPC and OPC/GGBS, the addition of
up to 60% of the metal waste considerably increased
the total CO2 consumed. For example, in Fig. 1, the
highest values of 14.7 1.8% CO2 / w/w solids (rate
of carbonation = A = 0.41% min -1) and 13.3 + 0.52%
C O / / w / w solids (A= 0.30% min -1) were found for
mixes 13 (OPC/WI) and 19 (OPC/GGBS/Wl) at w/b
ratios 0.66 and 0.50, respectively. OPC/PFA mixes
were similar to the control, as the maximum value of
11.2+1.4% CO2 / w/w solids (A=0.08%min -l)
(mix 17), and w/b ratio at 0.09 was recorded. For
OPC/W2 systems, the main differences were registered
when slag was added. The higher values for carbon
dioxide uptake of 10.2i0.33% (A=0.10%min -~)

and 12.0 + 0.78% CO 2 / w/w solids (A = 0.08% min -1)

were found at relatively higher w/b ratios of 0.5 and
1.0 for mixes 19 and 20, respectively.
WOPC/W1 samples showed a consistent carbon
dioxide consumption for all specimens (blended and
non-blended), with values for carbon dioxide uptake
around 7.0% CO2 / w/w solids for the highly carbonated specimens. The highest values were registered
for WOPC/GGBS/Wl at w/b ratios 0.5. When W2
was added no significant change was noted.
The results from SRPC/Wl mixes were very similar to those of OPC/Wl, however, a general decrease
of up to 3-4% of the maximum total uptake of CO2
was registered.
For W2, the addition of the pozzolans increased
the uptake of the gas by up to 6% at higher w/b
ratios (0.5 and 1.0) compared to SRPC alone.
For almost all waste-containing mixes the carbon
dioxide uptake was 3-6% higher than for the control
mixes. When PFA was used, the rate of carbonation
was decreased significantly.
The maximum rate of carbonation observed was
not necessarily proportional to the maximum CO2
consumed (see Fig. 2).

INFLUENCE OF MIX PARAMETERS AND BINDER CHOICE ON CARBONATION

c) V~'OFC/admixturcs/Wastc2

Waste2

f) SRPC/admixtuccs/WastI

Waste 1

OFC/W2 HI = 3 5~:~

[]

70

[ ~ WOPC/PFAN2H2= 5 t)=/;

,X,~0

[ ] WOPC/GGBS/W2H~= ~ 7%

3O

753
SRPC/WI HI=6

1117~

~ ] SRPC/PFA/Wl H2=6 8c,;

20

~0

~0

30~M=0,=, 1 - .5 c/~

[]

SRPC/GGBS/WI H3=6-7rz ,

~ / ~

40

5(1

50

60/

,,,u~/

5~4 o

70 6 6 0 ~ ~
P=<0.1 ~

30

P=<0. 1%

30
2O

~/

"J

/ '/

\
20
30
40
50
60
70
Note: The area of WOPC/GGBS is overlapped by WOPC only
Binders

10

80

90

Water

g) SRPC/admixtures/Waste 2

Binders 10
20
30
40
50
60
70
Note: The SRPC only area is partially overlapped by SRPC/GGBS

80

90

Water

Waste 2

gtPCandSRPC/PFA/W2 HI/H2=4 7c~

~PC/GGBS/W2 H3= 5 8cg

5O

Binders

10

20

30

40

50

60

70

80

90

Water

FIGURE 3 (e--g). Ternary diagrams for the different waste/binder systems showing the effect of mix proportions on the degree of
carbonation.

DISCUSSION
The influence of binder choice on the carbonation of
cement-solidified wastes has been investigated and
detailed in this work. It has been established that if
samples are highly carbonated (see optimised mix
designs in Fig. 3), they will have enhanced physical
and chemical properties when compared to nonoptimised samples, z3 Carbonation was strongly influenced by the complexity of industrial wastes, type of
cement/admixture and w/b ratio, supporting the premise that these factors determine the effective diffusivity of carbon dioxide within a waste/binder system.

Waste Composition and Cement Type

The addition of metal waste to cement paste resulted
in an increased susceptibility to carbonation in the
following order: OPC > SRPC > WOPC, particularly when higher amounts of metal waste (e.g. up to
60% for waste 1) were used.
These results suggest, first, that the presence of
certain cement phases, for example ferrite, in the
cement may be important (ferrite content is much
lower in WOPC) to the formation of ettringite, which

in the presence of C O 2 normally decomposes to form

gypsum, calcium carbonate and alumina gel. z6 Second, the presence of metal waste can influence the
gas-permeability of a cement productfl 7 consequently
causing both a degree of decalcification of the anhydrous calcium silicate phases and an acceleration of
hydration leading to the widespread formation of
CaCO3. Third, waste forms containing the two metal
wastes behaved quite differently on exposure to CO2;
in general, waste 2 consumed less CO2 than waste 1.
Therefore, the concentration of specific metals or
other waste species within a waste might be important in governing the rate of the carbonation reaction. The presence of other elements, such as organics
and anions, could also have a influence in this respect
by reacting with the cement paste and influencing the
CO2 effective diffusion coefficient.

Addition of Mineral Admixtures

The addition of PFA had little effect, except when
used with WOPC/W2 resulting in a reduced rate of
CO2 consumption. GGBS resulted in the highest CO2
uptake above a w/b ratio of 0.5 for all cement/waste
systems examined and might be caused by some

L . C . L A N G E ET AL

754

_oo

Sand/OPC
14

'~

Systems

4a

10

I w/b=o.o9

w/b = 0.33
w/b=0.5

Waste I /OPC
14" 4b

0 !

OPC

'

OPC/PFA

[I

"~
~ 10"

4c

OPC

I~

OPC/PFA

OPC/GGBS

Systems

4d
J

12-

w/b = 0.33

i~I

,.~ = o.5

~.~

6-

~5~~,~

4-

] woo = 0.09
w/b = 0.20
] w/b = 0.33
w/b = 0.5
w/b = 1.0

10.
-~

8-

14.

~=o.2o

~0 ~

"

Sand / WOPC

I w/b = 0.09

12 ~

w/b = 0.33
w/b=0.5

6'

Waste 2 / OPC Systems

14-

'-I w/b=0.09

O-

OPC/GGBS

oo.

Systems

8.

6.
4.

20

OPC

OPC/PFA
Waste I /WOPC

14

4e

OPC/GGBS
Systems

10

8
O
r..)

WOPC

WOPC/PFA
Waste 2/WOPC

41

[ w/b : 0.09
w/b = 0.20
w/b = 0.33
w/b = 0.5
w/b : 1.0

12

0.

4f

12
10

WOPC/GGBS
Systems

] w/b = 0.09
w/b = 0.20
w/b = 0.33
w/b = 0.5

6
4

2o

WOPC

WOPC/PFA

WOPC/GGBS

0~

WOPC

WOPC/PFA
Waste I /SRPC

Sand / SRPC Systems

WOPC/GGBS

Systems
1

14- 4g

[
[-'--7

"~ 1o;

w / b = 0.20

141

w / b = 0.33
w / b = 0.5

10

I w / b = 0.09

12-'

w / b = 1.0

O
~s

6-

4h

] w,'b=0.09 I

12

w/b = 0.33 I

w.:_o: /

8-t
67

4-

:1

2SRPC

SRPC/PFA

SRPC/GGBS

SRPC

SRPC/PFA

Waste 2 / SRPC Systems

14- 4i

,,, 12
o

10

~.

I w/b = 0.09
w/b = 0.20
w/b = 0.33
w/b = 0.5
w/b = 1.0

2
SRPC
FIGURE

SRPC/PFA

SRPC/GGBS

4. T o t a l c a r b o n d i o x i d e u p t a k e a f t e r 100 m i n f o r s e l e c t e d m i x e s o f d i f f e r e n t w / b r a t i o .

SRPC/GGBS

INFLUENCE OF MIX PARAMETERS AND BINDER CHOICE ON CARBONATION

microstructural changes in the silica gel phase (topochemical precipitation of gel). Some authors have
shown that the microporosity (gel pores) inside the
reaction product (silica-gel) is enhanced by the presence of CO2 ,28 GGBS/cement pastes contain less
calcium hydroxide than Portland cement and consequently a reaction between CSH and CO2 may
become more pronounced. As more CSH becomes
involved in the carbonation process, precipitation of
calcium carbonate results, accompanied by a sharper
decrease.
Moisture Content
The amount of water in the waste/binder system is
crucial for carbonation to proceed at an optimum
rate. Water is necessary for a reaction with CO2, but
too much water severely limits the rate of the reaction. In other words, as the pores are filled with
water, the penetration of carbon dioxide is hindered
as the rate of diffusion of COz is reduced; if on the
other hand pores are completely dry, the reaction of
CO2 is absent. Therefore, this implies that solvation
of carbon dioxide is critical for effective carbonation
to proceed. It is also shown that different water contents are required for different cement types and
might in return be related to the specific surface area
of individual cements. Figure 2 illustrates these
effects by showing the increased delay in induction
time in the carbonation reaction as water content
increases.

3.

4.

5.
6.
7.
8.

9.
10.
11.
12.

13.

14.

SUMMARY AND CONCLUSIONS

15.

This work examines the effect of variations in the mix

parameters, namely w/c ratio, cement type, waste
concentration and type of mineral admixtures, on the
rate and total amount of carbonation of waste forms.
Cement pastes blended with the two industrial
wastes react with carbon dioxide in higher proportions than cement paste alone. Pastes containing
waste and pozzolans were found to be vulnerable to
carbonation and this phenomenon can aid the
immobilisation of certain metals in waste form. 9,15
The complexity of industrial wastes (presence of
different anions, organics and a wide range of metals)
has a strong influence on the rate and total amount
of carbonation. In addition, GGBS affects the carbonation reaction, which increases with water content greater than w/c = 0.5. Carbon dioxide uptake
generally decreases with an increase in w/c ratio.
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17.
18.
19.
20.

21.
22.
23.
24.
25.

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