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Construction and Building Materials 36 (2012) 205–215
h i g h l i g h t s
" Glass powder is thoroughly analysed as a partial cement replacement material in mortar.
" Testing is carried out far beyond the usual mechanical testing and ASR by most authors.
" Chloride ingress, carbonation, sulphate attack and sorptivity are also considered for durability assessment.
" SEM demonstrated effect of fine glass particles well encapsulated into a dense matrix.
" This holistic study confirms that glass powder contributes to sustainability in construction.
a r t i c l e i n f o a b s t r a c t
Article history: It is well known that Portland cement production is an energy-intensive industry, being responsible for
Received 21 August 2011 about 5% of the global anthropogenic carbon dioxide emissions worldwide. An important contribution to
Received in revised form 28 March 2012 sustainability of concrete and cement industries consists of using pozzolanic additions, especially if
Accepted 25 April 2012
obtained from waste such as waste glass.
Crushed waste glass was ground (WGP) and used in mortar as a partial cement replacement (0%, 10%
and 20%) material to ascertain applicability in concrete.
Keywords:
An extensive experimental program was carried out including pozzolanic activity, setting time, sound-
Waste
Glass powder
ness, specific gravity, chemical analyses, laser particle size distribution, X-ray diffraction and scanning
Mortar electron microscopy (SEM) on WGP and resistance to alkali silica reaction (ASR), chloride ion penetration
Addition resistance, absorption by capillarity, accelerated carbonation and external sulphate resistance on mortar
Durability containing WGP.
Pozzolanic activity Glass particles well encapsulated into dense and mature gel observed by SEM, may help explaining
enhanced durability results and thus confirming that waste glass powder can further contribute to sus-
tainability in construction.
Ó 2012 Elsevier Ltd. All rights reserved.
0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.04.027
206 A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215
Despite the existence of large amounts of industrial waste such The environmental and economic benefits from the reuse of
as blast furnace slag, fly ash, silica fume, slag and agricultural res- recycled waste glass in cement and concrete production can also
idues such as rice husk ash, which have been used for many years be very significant depending on the end uses and production scale
in large amount as raw materials and components in the cement [9].
industry, there are still many other industrial wastes not used Therefore the present work besides the usual strength and ASR
yet [7], such as waste glass. In fact a few studies have successfully testing encompasses a wider range of analysis of effect of waste
investigated the potential use of finely ground waste glass as a poz- glass powder, including pozzolanic activity, setting time, sound-
zolanic material focusing on strength development and alkali-silica ness, specific gravity, chemical analyses, laser particle size distri-
reactivity [9–18,20–23]. bution, X ray diffraction and scanning electron microscopy (SEM),
Glass is the result of the merger of several inorganic mineral chloride ion penetration resistance, absorption by capillarity,
raw materials, which after undergoing a process of controlled cool- accelerated carbonation and external sulphate attack. This holistic
ing becomes a hard, homogeneous, stable, inert, amorphous and study corroborates that glass powder as a partial replacement
isotropic material [8]. Based on the major composition, glass can material is a waste material that contributes to sustainability in
be classified into several categories but soda-lime glass is the most construction.
widely used to manufacture containers, float and sheet glass and
therefore composing over 80% by weight of waste glass [9].
2. Experimental program
With the exception of Al2O3 and CaO, the percentages of the
main constituents of different types of glass are similar [4,6]. For 2.1. Materials
soda lime glass the typical glass composition is approximately
70% of silica, 13–17% Na2O and 10% CaO [9]. Typical commercial Type I 42.5R Portland cement was used and commercial sil-
In fact, glass can be considered a pozzolanic-cementitious mate- ica fume (SF) was employed as a reference pozzolanic material. Waste glass was ob-
tained from a recycling glass industry in Portugal where waste glass such as car
rial according to the chemical requirements in ASTM C 618 [33] if windscreens is crushed and sold to the bottle industry. Fine waste glass from this
the alkali content is disregarded. industry was ground during 48 h in a ball mill in the laboratory (WGP). Fig. 1 shows
Alkalis can cause alkali-aggregate reaction and expansion if particle size distribution of cement and WGP. X-ray diffraction on WGP showed that
aggregates are alkali-reactive. Therefore high alkali content of glass no substantial crystalline phases were detected. Soundness and setting time tests
(NP EN 196-3 [36]) were carried out on pastes with 100% CEM I 42.5R (CTL) and
is a typical concern for its use in concrete but studies have shown
on paste with 10% (WGP10) and with 20% (WGP20) cement replacement with
that finely ground glass does not contribute to ASR [15,20,21]. The WGP. Pozzolanicity test was carried out following NP EN 196-5 [37] on a sample
pozzolanic properties of glass are first notable at particle sizes be- with 90% of cement and 10% of WGP. Chemical composition and physical character-
low approximately 300 lm. Below 100 lm, glass can have a pozzo- istics of WGP and cement are given in Table 1. Scanning Electron Microscopy (SEM)
lanic reactivity which is greater than that of fly ash at low percent was carried out on CEM I 42.5R, silica fume and WGP samples shown in Fig 2.
Table 1 calculation of the chloride diffusion coefficient (Dns) from an accelerated test. An
Chemical and physical characteristics of cement and glass. external electrical potential is applied axially across the specimen and forces the
chloride ions outside to migrate into the specimen. After a certain test duration,
CEM I 45.2R WGP Silica fume the specimen is axially split and a silver nitrate solution is sprayed on to one of
Chemical composition (% mass) the freshly split sections. The chloride penetration depth can then be measured
LOI 2.61 0.92 from the visible white silver chloride precipitation, after which the chloride migra-
Insoluble residue 1.33 tion coefficient can be calculated from this penetration depth as follows:
SiO2 20.36 70 >99 pffiffiffiffiffi
RTL xd a xd
Al2O3 5.1 1.2 Dns ¼ : ð3Þ
ZFU t
Fe2O3 3.12 0.65
CaO 62.72 8.7 rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
MgO 1.81 3.7 RTL
a¼2 e ð4Þ
Na2O 16 ZFU
K2O 0.35
Na2O eq 17 2C d
e ¼ erf 1 1 ð5Þ
SO3 3.44 <0.05 C0
Cl 0012 <0005
where Dns is the apparent diffusion coefficient obtained in a non-steady state migra-
Free lime 1.62
tion test (cm2/s), R the gas constant R = 8.314 J/(mol K), T the absolute temperature
Pozzolanic activity Positive Positive
(K), L the thickness of specimen (cm), Z the ion valence, F the Faraday constant,
Physical properties F = 9.648 104 J (V mol.), U the effective voltage applied (V), xd the depth of chloride
Specific gravity (g/cm3) 3.16 2.68 2.20 penetration measured by using a colorimetric method (cm), t the time of test dura-
Soundness (mm) 0 0 0 tion (s), a the laboratory constant, e = 0.764 if external chloride concentration of
Initial setting time 0.5 M. Cd the concentration of free chloride at which the colour changes when using
WGP10/WGP20 2 h, 20 m/2 h, 15 m the colorimetric method to measure the chloride penetration depth (kg Cl/m3 solu-
CTL 2 h, 30 m tion) and C0 is the concentration of free chloride in the external solution.
Final setting time Results can be seen in Fig. 7.
WGP10/WGP20 3 h, 25 m/3 h, 25 m
CTL 3 h, 25 m 2.6. Absorption by capillarity
Absorption by capillarity testing was undertaken on two months old cast test
Several test specimens were produced. After demoulding the following day, test
specimens, approximately 50 mm diameter by 100 mm length generally following
specimens were cured in water at 20 °C in a fog room until testing.
standard procedure RILEM TC 116-PCD [45]. The samples were put to dry in a ven-
tilated heater at 40 °C until constant mass. For the test itself, test specimens were
2.3. Strength placed moulded face downwards, in a shallow water bath. Water level was adjusted
automatically so that the formwork face was dipped to a depth of approximately
Flexural and compressive strength testing was undertaken at 7, 28, 90 and 3 mm. During the test, water was drawn into the core by capillary forces and
180 days (and 562 days for CTL and WGP10) following the standard procedure in weighed at time intervals up to 4.5 h from the start of the test [45].
NP EN 196-1 [35]. Results are presented in Fig. 3. The pozzolanic effect of glass pow- The absorption of water into concrete under capillary action is dependent on
der may be assessed with the Activity Index (AI) (Fig. 4) which is the ratio between the square-root of time and may be modelled [24] by the following equation:
strength of WGP containing mortar and strength of equivalent control mortar at the
same age. A ¼ A0 þ St 0;5 ð6Þ
2
where A (mg/mm ) is the water absorption by unit area of concrete surface since the
2.4. Alkali silica reaction (ASR) moment the core was dipped in water, S is the sorptivity of the material, t is the
elapsed time and A0 (mg/mm2) is the water absorbed initially by pores in contact
The potential risk of alkali-silica reaction in concrete was monitored in accor- with water. The above equation was found to provide a very good fit to the data with
dance with the accelerated mortar bar test following ASTM 1567 [34], where two correlation coefficients of over 0.96 (Fig. 8). The average sorptivity value of each
mortar prisms with 25 25 250 mm were used for each mortar type. mortar type is shown in Fig. 9.
In this test method, higher temperature (80 °C) and increased alkalinity (1 N
NaOH) accelerates the reaction. ASTM C 1567 method is not intended to capture
2.7. Carbonation
the effect of increased alkalis from glass powder; rather it is used in this study to
understand the expansion characteristics of plain and modified mortar. In fact this
Resistance to carbonation was assessed in accordance with the procedure de-
test method can be used to evaluate the effectiveness of supplementary cementing
scribed RILEM CPC-18 [44] where test specimens were exposed to 5 ± 0.1% carbon
materials in reducing the expansion due to ASR [17].
dioxide, relative humidity (RH) of 60 ± 5% and temperature of 23 ± 3 °C, in an accel-
Two slight modifications were performed when following the procedure in
erated carbonation chamber.
ASTM. Instead of 1:2.25:0.47 cement:aggregate:water ratio required in ASTM, the
Carbonation depth was evaluated on three test specimens for each mortar type,
ratio used was 1:3:0.5 which is considered in NP EN 196-1 [35]. ASTM C 1567 also
water cured at 20 °C followed by 2 and 4 months in the chamber. After splitting the
requires particle size distribution of (reactive) aggregates shown in Table 3, but the
specimens, the surface was cleaned and sprayed with a phenolphthalein pH indica-
particle size distribution used was the one considered in NP EN 196-1 CEN sand,
tor. In the noncarbonated part of the specimen, where the mortar was still highly
which was found to be reactive. ASTM C 1567 was followed for the remaining pro-
alkaline, a purple-red colour was obtained. In the carbonated part of the specimen
cedure, so immediately after casting, the moulds were covered and demoulded 24 h
where the alkalinity of mortar is reduced, no coloration occurred. Each value corre-
later. Then they were preconditioned for a further 24 h in water maintained at
sponds to the mean of twelve measurements taken around the four sides of the
80 °C. The lengths of these mortar bars after immersion in hot water, measured
freshly split and sprayed surface of each test specimen. Results can be seen in Fig. 10.
along the 4 faces of each specimen, were then taken as the initial readings (L0).
The mortar bars were subsequently transferred to 1 N NaOH solution maintained
at 80 °C and periodically measured for 14 days. 2.8. External sulphate attack
Therefore the actual length (Lx) of each specimen, on day x is taken as
P4 Resistance to external sulphate attack was evaluated according to the Portu-
i¼1 Li guese standard E-462 [42], on six (1, 2, 3, 4, 5 and 6) mortar prisms of
Lx ¼ ð1Þ
4 16 16 160 mm. Test specimens were immersed in calcium hydroxide solution
The expansion of each specimen at day x is given by during 28 days, measured along the 4 side faces of each specimen and taken as ini-
Lx L0 tial readings (L0). Test specimens 2, 4 and 6 were transferred to a sodium sulphate
e¼ 100% ð2Þ solution and the others were maintained in calcium hydroxide saturated solution.
250
Readings were taken throughout 26 weeks and sulphate solution was renewed
Expansion with time is shown in Fig. 5 as well as final expansion in Fig. 6.
every 2 weeks. The actual length increase of each specimen on day x is taken as:
Lx L0
2.5. Chloride ion diffusion ExpCaðOHÞ2 ðxÞ ¼ ð7Þ
1600
The resistance to chloride permeability was evaluated by the CTH Rapid Method
according NT Build 492 [44] which is a non-steady state migration method based on Lx L0
ExpSO4 Na2 ðxÞ ¼ ð8Þ
a theoretical relationship between diffusion and migration which enables the 1600
208 A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215
CEM I 42.5 R 200 times enlarged CEM I 42.5 R 1000 times enlarged CEM I 42.5 R 5000 times enlarged
attaining CTL although under SF levels. WGP20 gained significant SF and WGP were effective in reducing ASR expansion. Increasing
strength between 28 and 90 days showing pozzolanic reaction tak- glass powder content led to lower expansion despite the high alkali
ing place in this period. Idir et al [26] for fine glass with particle size content. Frederico and Chidiac [4] reported results on ASR expan-
range under 41 lm and mean particle size of 7.8 lm obtained sim- sion relating to particle size of glass and cement replacement dos-
ilar results concluding that the general trend is for replacement of age including work by Jin et al [25] and Shao et al [12] with which
cement by glass to lead to a decrease in compressive strength [26]. present results are in accordance.
Strength activity indexes obtained were higher than 90% at 90 ASR results in the present study also confirm findings by Sch-
days of curing for 10% and 20% replacement by fine glass powder, warz et al [20] where expansion for 10% and 20% replacement with
confirming results obtained by Jin et al [25]. Shao et al [12], used glass powder was slightly higher, presumably due to use of coarser
higher replacement (30%) by fine glass powder (<38 lm) in con- glass particles. Sacanni and Bizigoni [21], where fine aggregate was
crete and obtained concrete strength activity indexes higher than also replaced by glass particles, obtained ASR expansion similar to
90% at 90 days. Shi et al, for 25% replacement and coarser material values in the present study.
(<100 lm) obtained strength activity values around 74% at 28 days, Therefore ASR testing confirmed that glass powder assisted in
with which the results of the present study for 20% replacement hindering expansion compared to control specimens, confirming
seem to be in accordance. conclusions by other authors [20–22].
The possible explanations for this phenomenon according to
3.3. Alkali silica reaction Taha and Nounu [22] is that available reactive silica in glass pow-
der as an amorphous material will dissolve very quickly during the
Results obtained for ASR expansion respecting control mortar pozzolanic reaction and react with other chemicals to form the
indicated potential deleterious expansion according to ASTM mineral phases of concrete. Therefore, the dissolved reactive silica
1567 (higher than 0.10% after 14 days in NaOH). Results for both of glass powder will be accommodated in the crystals of concrete
A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215 211
Fig. 8. Linear regression for absorption by capillarity during 4 h 30 min on test cores.
minerals and not available for the ASR which occurs in later stages. Additions with low CaO content act as ASR inhibitors, whereas
With the presence of other chemicals the dissolved reactive silica those with more than 10% CaO content act as ASR promoters [27]
of glass powder will not be able to form ASR gel during the pozzo- and therefore WGP proved once again to inhibit ASR.
lanic reaction, or even a gel having a swelling property likewise the
ASR gel. Otherwise, if there was any chance to form ASR gel during
the pozzolanic reaction from the reactive silica of glass powder one 3.4. Chloride diffusion, absorption by capillarity, carbonation and
can envisage that any existing ASR expansion would be noticeable. sulphate attack
If any ASR could occur during the pozzolanic reaction stage, the
produced expansion would vanish and accommodate within the CTH rapid method results show that using WGP as a partial ce-
plasticity of fresh concrete. On the other hand, in the first 4 weeks ment replacement drastically enhances resistance to chloride pen-
of the pozzolanic reaction and hydration process, most of the alka- etration compared to control mortar specially for 20% replacement
lis would have been consumed in order to catalyse the pozzolanic dosage (on average, CTL Dns is about double compared to WGP20)
reaction and act as chemical activators to compensate for the lower and even compared to 10% SF mortar. Samples of silica fume and
calcium content in the glass powder. Therefore, in later age, there WGP10 have very similar diffusion coefficients. Results obtained
would not be enough free alkali to interact with the reactive silica in the present study, confirm values by other authors [16,19,20],
in the pore solution of the concrete to induce ASR, as illustrated in where performance of glass powder mortar is better than control
Fig. 13. mortar regarding chloride penetration. Only Jain and Neithalath
212 A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215
Fig. 10. Carbonation depth results after 2 months curing followed by 4 months in the chamber.
[13] carried out the NT Build 492 [43] test as in the present study silica fume. This may be explained by higher SF reactivity and thus
and obtained similar improvement to WGP 20 at 56 days. further CH reduction, compared to WGP. When WGP replacement
Absorption by capillarity and sorptivity proved to be similar for is doubled, carbonation depth is similar to SF. Although a less reac-
WGP and CTL mortar and a little lower for SF mortar. This situation tive material, higher WGP replacement and less cement in the mix-
may be explained by similar fineness of both WGP and cement (see ture, both contribute to CH reduction levelling out intense CH
Fig. 9). Much finer SF particles physically fill capillary pores reduc- reduction in SF mortar.
ing capillary absorption. Other authors, such as Taha and Nounu Sulphate expansion at 26 weeks should be under 0.10% accord-
[23] also showed similar results for concrete with cement replace- ing to the Portuguese standard E-462 and therefore Portland ce-
ment materials, but following BS 1881. ment used is not sulphate resistant. Blended Portland cement
Carbonation depth for all blended cement mixtures was greater with 10% replacement with WGP showed an impressive resistance
than for the Portland cement mixture. It was found that carbon- to sulphate attack, far higher than SF marginally within the limit of
ation increased along with the increase in WGP content, which is 0.10%. The pozzolanic activity of WGP and SF binds portlandite
consistent with the trend observed in concrete for various pozzola- (CH) released in the hydration of calcium silicates (C3S and C2S),
nic materials and probably due to CH reduction. WGP10 carbon- so CH is no longer available for reaction with sulphates, in
ated almost half of SF10 mortar, albeit pore refinement due to accordance with [28,29]. This prevents the formation of gypsum.
A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215 213
CTL 562 days 2500 times enlarged CTL 562 days 5000 times enlarged CTL 562 days 10000 times enlarged CT L 562 days 20000 times enlarged
WGP10 562 days 2500 times enlarged WGP10 562 days 5000 times enlarged WGP10 562 days 10000 times enlarged WGP 562 days 20000 times enlarged
Pozzolanic reaction produces a secondary C–S–H that also de- in WGP10 was found to contain more calcium as well as more alka-
creases the capillary porosity of mortar and enhances significantly lis compared to CTL mortar. These findings are in accordance with
the paste–aggregate interface [28]. Sobolev et al [30] who suggested that the main difference between
glass containing mortar and reference Portland cement is related to
3.5. Scanning electron microscopy the decrease in size and the amount of CH, caused by consumption
of CH as a result of the pozzolanic reaction involving glass grains.
Regarding SEM observations, glass particles seem to be thor- More alkalis found in the gel of WGP10 compared to CTL also con-
oughly encapsulated and dispersed into to the hydrated products firm findings by Shayan and Xu [17] who proposed that the pozzo-
of a dense and mature gel with needle shaped ettringite crystals lanic reaction of glass powder with cement causes the binding of
(see WGP10 10,000 and 20,000 times enlarged, Fig. 12). CH layered alkalis in the paste, making it unavailable for ASR [17] and therefore
crystals were observed in the CTL mortar (see CTL 5000 times en- in accordance with the mechanism proposed by Taha and Nounu
larged, Fig. 12) and CSH gel filling the hydrated structure. CSH gel [22] explaining lower expansion due ASR when glass is used.
214 A.M. Matos, J. Sousa-Coutinho / Construction and Building Materials 36 (2012) 205–215
Table 4
Requirements in standards.
European Standards
Fly ash (NP EN 450-1) Silica fume Slag (NP EN 15167-1) GP Remarks
(NP EN
13263-1)
Chemical requirements Cl 60.10% 60.3% 60.10% <0005 OK
SO4 63.0% 62.0% 62.5% – OK
SO3 – – 62.0% <0.05
Free CaO 62.5% 61.0% 8.70% Only the total content of CaO
is known but soundness is OK
Reactive CaO 610% –
SiO2 P25% P85% 70% OK
SiO2 + Al2O3 + Fe2O3 P70% 71.82% OK
CaO + MgO + SiO2 P67.0% OK
NaO2eq 65.0% 17% KO, but OK in ASR testing
LOI Class A 6 5% 64.0% 63.0% 0.92%
Class B 2–7% OK
Class C 4–9%
Pozzolanicity – – Positive OK
Physical requirements Activity index P75% at 28 days P100% at P45% at 7 days and P75% KO Almost OK for 28 days, and ok
28 days old at days for 90 days
P85% at 90 days
Start setting time 6120 min plus start time of 62 times the start time of OK
the paste-setting reference the paste-setting reference
Soundness 610 mm 610 mm OK
This study aimed to evaluate use of glass powder in cement Future research comprising use of glass powder is underway,
based materials. An experimental study on the mechanical and including use in self-compacting concrete, taking advantage of in-
durability properties of mortar containing waste glass powder as creased workability provided by this waste material.
cement replacement provided the following results:
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