Construction and Building Materials 47 (2013) 1001–1009

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Construction and Building Materials

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Granitic quarry sludge waste in mortar: Effect on strength and durability

0950-0618/$ - see front matter � 2013 Elsevier Ltd. All rights reserved.http://dx.doi.org/10.1016/j.conbuildmat.2013.05.098

⇑ Corresponding author. Address: Rua do Dr. Roberto Frias, s/n, 4200-465 Porto,Portugal. Tel.: +351 225081936; fax: +351 225081441.

E-mail address: telmajr@fe.up.pt (T. Ramos).

Telma Ramos a,⇑, Ana Mafalda Matos a, Bruno Schmidt c, João Rio a, Joana Sousa-Coutinho a,b

a LABEST-FEUP – Department of Civil Engineering, Faculty of Engineering University of Porto, Portugalb FEUP – Department of Civil Engineering, Faculty of Engineering, University of Porto, Portugalc Department of Civil Construction, Federal University of Paraná, Curitiba, Brazil

h i g h l i g h t s

� An abundant waste was analyzed as cement replacement for strength and durability testing (ASR and Chlorides).� Marginal workability and strength loss are observed for up to 10% cement replacement levels.� Improvement of up to 38% reduction in ASR expansion was observed and up to 70% improvement into chloride resistance.� SEM after ASR attack showed deeper surface grooving and thicker gel layers corresponding to higher measured expansion.� SEM on mortar after chloride ingress showed that aluminates led to formation of chloroaluminates explaining good results.

a r t i c l e i n f o

Article history:Received 18 January 2013Received in revised form 13 May 2013Accepted 20 May 2013

Keywords:WasteQuarry sludgeGraniteSustainabilityConcrete

a b s t r a c t

Granitic quarry sludge is an abundant waste from granite rock processing, causing serious environmentalconcern. The use of this waste could become a valuable resource if properly engineered into a successfulsolution as a partial cement replacement in concrete.

The effect of granitic sludge from a quarry in northern Portugal was analyzed as a partial cementreplacement in mortar in terms of strength and durability, so as to envisage its use in concrete.

The experimental program included chemical analyses, laser particle size distribution and scanningelectron microscopy of granitic quarry sludge, as well as mechanical strength, expansion due to alkali sil-ica reaction and chloride penetration resistance on mortars containing different dosages of cementreplacement with granitic quarry sludge waste ground to different fineness levels.

Results showed that granitic quarry sludge waste, if ground to sufficient fineness, produces a densermatrix promoting up to 38% reduction in expansion due to ASR and almost 70% improvement in resis-tance to chlorides, without compromising workability and strength. This surprising improvement interms of chloride resistance seems to derive from captivation of chlorides by aluminates present in thewaste with formation of chloroaluminates.

Finally, a properly engineered use of granitic waste in cement-based composites, leading to enhanceddurability can turn granitic quarry sludge, an abundant waste, into a valuable resource and therefore con-tribute to sustainable construction.

� 2013 Elsevier Ltd. All rights reserved.

1. Introduction

Concrete is the world’s most widely used building material.Global production of concrete is about 12 billion tons a year [1]corresponding to almost 1 m3 per person per year. Yearly cementproduction levels are about 3 billion tons [1].

Adjustments and improvements to the present concrete makingmethods are essential in order to address environmental andeconomic issues. This has encouraged researchers in the area of

concrete engineering and technology to investigate and identifysupplementary by-product materials that can be used as substi-tutes for constituent materials in concrete production [2].

Cement industries contribute to about 7% of the total global CO2

emissions. This is due to the calcination of raw materials for theproduction of cement and burning fuels needed to maintain hightemperatures in a kiln. In recent times, one of the most importantgoals of the global environmental agenda is the reduction of emis-sions to protect the Earth’s climate pattern [1].

In fact an effective way to reduce CO2 emissions from the ce-ment manufacturing process is the use of blended cement byreducing clinker/cement ratio.

Production of cements with several main constituents like gran-ulated blast furnace slag, fly ash from coal power plants and natu-

Table 1Particle size distribution of cement, PG and PGS.

d10 (lm) d50 (lm) d90 (lm)

CEM I 42.5 R 0.69 8.09 30.81PG 1.55 13.05 55.46PGS 0.84 3.48 13.34

1002 T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009

ral pozzolans offer additional benefits in cement performance [3],especially in terms of durability properties.

In recent years there has been an increase in the consumption ofmineral additions by the cement and concrete industries. The useof adequate industrial or agricultural by-products for partial ce-ment replacement is an environmental friendly method of disposalof large quantities of materials that would otherwise pollute land,water and air [4].

Table 2Chemical composition of cement, PG and PGS.

Composition (% mass) CEM I 45.2 R

LOI 2.61Insoluble residue 1.33SiO2 20.36Al2O3 5.1Fe2O3 3.12SiO2 + Al2O3 + Fe2O3

CaO 62.72MgO 1.81Na2OK2OSO3 3.44Free lime 1.62Pozzolanicity –

Fig. 1. SEM photos of cement

The granite cutting industry produces large amounts of wastes,solids (generated during extraction) and sludge (produced duringtransformation processes) [5].

Granite fines are often referred to as quarry or rock dust, andthis residue generally represents less than 1% of aggregate produc-tion [6] or between 1% and 2% by mass of the total aggregatecrushed in quarries, according to Abukerh and Fairfield [7].

Managing large amounts of sludge can be rather problematic forits producers, which must find appropriate places for storage anddeposition. Dumping into rivers and lagoons is obviously not anenvironmentally safe solution and landfilling has serious draw-backs. Transporting and dumping of waste in landfills involvessubstantial costs; therefore, incorporating waste into other indus-trial processes could lead to a reduction of management costs andopen up new business opportunities. Some previous studies haveshown that granite sludge has a high potential as a raw materialfor the ceramic industry and it is amenable to use as filler in dry

PG/PGS Requirements in ASTM 618 [15] (class N)

2.04 610

63.2215.664.4783.35 P703.261.822.685.020.00 64

Negative

, silica fume, PG and PGS.

Table 3Mixture proportions and workability of mortars.

Mixture proportions Control Partial cement replacement of

5% PG 10% PG 5% PGS 10% PGS SF

CEM I 42.5 R (g) 450 427.5 405 427.5 405 405PG (g) – 22.5 45 – – –PGS (g) – – – 22.5 45 –SF (g) – – – – – 45Sand (g) 1350 1350 1350 1350 1350 1350Water (ml) 225 225 225 225 225 225sp/c (%) – – – – – 0.37w/c 0.5 0.5 0.5 0.5 0.5 0.5Sp/Blinder 0.0035Workability (mm) 200 201 199 199 198 198

Fig. 2. Flexural and compressive strength results at 28 days.

T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009 1003

mortars [5]. In fact Mármol et al. [5] studied granite sludge wastefor incorporation as alternative to ordinary limestone filler into ce-ment-based mortar formulations. In this study findings revealedthat the composition of this waste, the main components of whichare SiO2, Al2O3, CaO and Fe2O3 based compounds, together with thesmall particle size, warrant its use by the mortar industry. It wasalso concluded that 10% cement can be replaced with granitesludge waste without loss of 28 d compressive strength. These re-sults support the use of granite sludge waste in mortar by virtue oftheir appropriate particle size distribution and potential pozzolanicactivity.

Fig. 3. ASR expansio

Albukersh and Fairfield referred that concrete mixes containing30% recycled red granite dust showed good fresh properties, betterthan expected mechanical properties and excellent surface finish.This concrete demonstrated better early age strength than similarfly ash – based concrete [7].

Results of Felixkala and Ilangovana et al. also clearly show thatgranite powder as a partial sand replacement has beneficial effectsof the mechanical properties of high performance concrete [8,9].

According to Ho et al. [6] in normal concrete, the introduction ofquarry dust to mixes must be limited due to its high fineness. Itsaddition to fresh concrete would increase the water demand andconsequently the cement content for given workability andstrength requirements. In fact Ho et al. demonstrated that granitefines, as supplied, could be used successfully in the production ofSCC. Compared to the use of limestone powder, both paste andconcrete studies confirmed that the incorporation of granite finesrequired a higher dosage of superplasticizer for similar yield stres-ses and other rheological properties. However, it is important topoint out that as a waste material, the properties of granite finesare expected to vary over time. Furthermore, the fineness of gran-ite fines could promote durability problems, such as alkali-silicareactions. These two issues would need to be addressed if thematerial is to be used with confidence [6].

The present study aims at analyzing the effect of using graniticquarry sludge as partial cement replacement on strength and dura-bility of mortar in terms of not only alkali silica reaction but alsochloride ion ingress.

n versus time.

Fig. 4. ASR final expansion after 14 days.

1004 T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009

In fact, the rate of chloride ion ingress into concrete is of greatimportance for the performance of reinforced concrete structuresexposed to chloride-contaminated environments. It is widelyknown that diffusion of chloride ions in concrete is an importantaspect related to corrosion of reinforcement [10]. Corrosion of steelin concrete occurs only if certain species are efficiently transportedto the vicinity of the reinforcement. The presence of aggressiveagents such as chlorides can cause depassivation of the reinforcingsteel. This can happen in concrete even when the surrounding pHis as high as 12.5 [11]. The property of diffusion of chloride ions inconcrete appears to be the dominant factor in this type of corro-sion. Again, this property depends to a large extent on the pore sizedistribution in the concrete matrix and whether the pore system iscontinuous [12,13].

The experimental program carried out consisted of characteriz-ing granite powder obtained from the dried and ground graniticsludge waste taken from a quarry in northern Portugal. These testsincluded chemical analyses, scanning electron microscopy (SEM)and laser particle size distribution. Then mechanical and durabilityproperties were determined on mortar produced with different ce-ment replacement dosages as well as for different fineness levels ofthe granite powder. Alkali–silica reaction (ASR) of mortar contain-ing this waste was thoroughly analyzed and observations underscanning electron microscopy (SEM) were carried out after ASRtesting for full understanding of the effect of granitic sludge.Chloride ion penetration testing was also undergone on mortarspecimens with cement replacement by granitic powder and SEMobservations detailed and completed this study.

Results of this program show that granitic sludge waste, ifground to sufficient fineness and used up to 10% cement replace-ment in mortar does not compromise workability or strength andgreatly enhances durability in terms of resistance to ASR andchloride ion penetration. These results may lead to the successfuluse of this abundant waste in concrete.

2. Research programme and results

2.1. Materials and methods

Type I 42.5 R Portland cement (specific gravity 3.16 g/cm3) was used. Commer-cially available silica fume (SF) (specific gravity 2.20 g/cm3) was used as a referencecement replacement material.

Granitic quarry sludge was dried at 105 ± 5 �C for 24 h and ground to two dif-ferent levels of fineness. The dried sludge was ground in a ball mill for 30 minand is henceforward referred to as PG (Powder from quarry Granitic sludge). A finer

material, referred to as PGS (superfine powder from granitic sludge) was obtainedfrom PG submitted to further grinding in a planetary mill RETCSH PM 100 using zir-conia balls of 1 mm diameter, for 10 min at constant 450 rpm.

Particle size distribution and chemical composition for PG and PGS are shown inTables 1 and 2 respectively.

Chemical composition, which can be seen in Table 2, was carried out on granitepowder following NP EN 196:2 [14].

Pozzolanic activity was assessed by comparing the concentration of calcium ion,expressed as calcium oxide, present in the aqueous solution containing the binder,in this case 90% cement and 10% PG, after 15 days, with the quantity of calcium ioncapable of saturating a solution of the same alkalinity, as described in NP EN 196-5[15]. The binder tests positive for pozzolanicity if the concentration of calcium ionin the solution is lower than the saturation concentration. Results obtained were aCaO concentration of about 13.6 mmol/l and a OH-concentration of 48 mmol/l,leading to a negative result, as expected.

Fig. 1 shows scanning electron microscopy (SEM) carried out on cement, silicafume and PG/PGS samples. Commercially available silica fume with over 99% SiO2

was used for comparison. As can be observed PG particles are coarser than cementparticles and PGS particles are finer in accordance with the particle size distributioncurves. PG and PGS particles seem more angular and more prismatically shapedcompared to cement particles which look rounder. Silica fume spherical particlesare far smaller than the PG and PGS and cement, as expected.

Six mortar types were prepared following the procedure described in NP EN196-1 [17]: a control mix with 100% cement (CTL), two mixes with 5% (PG 5%and PGS 5%) cement replacement with granitic powder (PG) and superfine graniticpowder (PGS), respectively, two mixes with 10% (PG 10% and PGS 10%) cementreplacement with PG and PGS, respectively and a last mix with 10% (SF) cementreplacement with silica-fume.

Mortar workability was maintained at the same level and measured accordingto ASTM C 109 [18] and ASTM C 230 [19], and the results are given in Table 3.Superplasticizer (Sikament) was only needed for silica fume mortar.

2.2. Strength

Flexural and compressive strength testing was undertaken at 28 days, on40 � 40 mm � 160 mm mortar specimens, following standard procedure in NP EN196-1 [17]. Results of flexural and compressive strength are presented in Fig. 2.

2.3. Alkali silica reaction (ASR)

In order to measure the ASR expansion for a given mix proportion, anaccelerated mortar bar test was carried out on three prism specimens of25 � 25 � 250 mm in accordance with ASTM C 1567 [20].

After 24 h of production, mortar bar specimens were demoulded and stored indistilled water at 80 �C for another 24 h after which a zero reading was taken. Thebars were then transferred and immersed in 1 N NaOH (1 Normal Sodium Hydrox-ide solution) at 80 �C.

Expansion of each mortar bar was measured within 15 ± 5 s after being re-moved from the 80 �C distilled water or alkali storage condition by using a lengthgauge. Measurements were taken for 14 days.

Expansion with time and final expansion of mortar type are shown in Figs. 3and 4, respectively.

(a)

(b)

(c)Fig. 5. SEM on PGS (a) and CTL specimens submitted to ASR (b) and reactive sand before attack (c).

T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009 1005

Combinations of cement, pozzolanic materials and aggregate that expand morethan 0.1% (14 days in solution) are indicative of potentially deleterious expansion.However, the occurrence of deleterious reaction should be confirmed by testingthe same combination of materials in concrete.

After testing for ASR, SEM with EDS spectrums were undertaken on PGS (Fig. 5a)and CTL (Fig. 5b) mortar specimens (Figs. 5–7). SEM photos were also taken on reac-tive sand used, prior to ASR, and show in Fig. 5.

2.4. Chloride ion diffusion

The rapid chloride migration test (CTH) is a non-steady-state migration methodbased on a theoretical relationship between diffusion and migration which enablesthe calculation of the chloride diffusion coefficient from an accelerated test [21].

It is based on measuring the depth of color change of a silver nitrate solutionsprayed on specimens previously submitted to a migration test and application ofthe following equation [22,23]:

Dns ¼RTLZFU

xd � affiffiffiffiffixdp

tð1Þ

a ¼ 2

ffiffiffiffiffiffiffiffiffiRTLZFU

re; e ¼ erf�1 1� 2Cd

C0

� �ð2Þ

where Dns is the apparent diffusion coefficient obtained in a non-steady-state migra-tion test (cm2/s); R the gas constant R = 8.314 J/(mol K); T the absolute temperature(K); L the thickness of specimen (cm); Z the ion valence; F is Faraday constant; con-stant F = 9.648 � 104J (V mol); U the effective voltage applied (V); xd the depth ofchloride penetration measured by using a colorimetric method (cm); t the time of

Fig. 6. SEM and EDS on CTL mortar after ASR.

Fig. 7. SEM and EDS on PGS 10% mortar after ASR.

1006 T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009

the test duration (s); a the laboratory constant; e = 0.0764 if external chloride con-centration of 0.5 M; C = 0.0764 if external chloride concentration of 0.5 M; Cd theconcentration of free chloride at which the color changes when using the colorimet-ric method to measure the chloride penetration depth (kg/m3

solition); and C0 is theconcentration of free chloride in the external solution.

The procedure for determining the apparent diffusion coefficient (Dns) consistedof: after switching off the electrical field the specimens were split in two halves andthe penetration of chlorides was measured by using the colorimetric method. Thismethod consists of spraying silver nitrate solution over the split faces, storing themin a dark place for 1 h and then exposing them under a fluorescent light for a few

Fig. 8. Apparent diffusion coefficient Dns (cm2/s).

T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009 1007

hours, after which the average front of the white zone in the central part of eachspecimen is measured with a precision of 0.5 mm. Apparent diffusion coefficientDns results are shown in Fig. 8.

SEM was carried out on PGS 5% and PGS 10% mortar specimens after the accel-erated chloride ion penetration test. Photos are show in Figs. 9 and 10.

3. Discussion

As can be seen in Table 2, quarry granite sludge is mainlycomposed of silica and alumina, chemically similar to granite

Fig. 9. SEM and EDS specimens on PGS5% sp

Fig. 10. SEM and EDS specimens on PGS 10%

sludge wastes studied by Mármol et al. [5] and Abukersh and Fair-field [7]. Chemical properties are in accordance with requirementsstated in ASTM C 618 [16] regarding pozzolanic materials.

SEM observations, Fig. 1, indicate that quarry granite sludgeparticles seem more angular, more elongated and more prismati-cally shaped compared to cement. This confirms findings by Hoet al. [6] who observed that the shape of granite fines is flakierand more elongated compared to limestone particles.

SEM and laser particle size distributions, Table 1, show that PGparticles are slightly coarser than cement. However PGS is finerthan cement and naturally, both are much larger than spherical sil-ica fume particles.

According to Ho et al. [6] and as stated before, the introductionof quarry dust to mixes is limited due to its high fineness. Its addi-tion to fresh concrete would increase the water demand and con-sequently the cement content for given workability and strengthrequirements. However, as can be seen in Table 3, no superplasti-cizer was needed for mortar containing PG and PGS where similarworkability was obtained, comparing with control mortar. Therewas no need of extra superplasticizer when using quarry powdercould, therefore, be an economic advantage for future use in con-crete mix design.

Strength results for PG and PGS mortars at 28 days were lowerthan control, where flexural and compressive strength decreasedwith increase of replacement dosage. Nevertheless strength lossis marginal when using PGS. This confirms findings by otherauthors such as Abukersh and Fairfield [7] for coarser granite dust

ecimens submitted to chloride testing.

specimens submitted to chloride testing.

Fig. 11. Performance of mortars compared to CTL mortar.

1008 T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009

(d50 < 38 lm), by Ho et al. [6] for granite sludge waste, also coarser(d50 = 23.8 lm) and by Mármol et al. [5] where granite sludgewaste was also coarser with 80% of particles with a diameter of2–60 lm [5].

Coarser granite sludge, this is PG must have led to more voids inthe mix hardened structure compared to cement only structure.This may explain lower mechanical strength of PG containing mor-tar as well as higher ASR expansion and higher apparent diffusioncoefficients (Dns).

Analyzing ASR results, for PG there was generally no improve-ment of resistance to ASR compared to CTL but for PGS, expansionreduced with increase in replacement (19% reduction for PGS 5%and 38% for PGS 10%). Nevertheless PGS was not as effective asSF (reduction of 81%, compared to CTL).

Considering ASR SEM observations, a reactive sand particle isshown in Fig. 5c at different magnifications where the morphologyof the surface can be observed and compared to the grooved sur-faces of a sand particle in mortar after attack by alkalis whereASR gel can also be detected in Fig. 5a and b. Differences in PGand CTL mortar can be observed in terms of the intensity of thegrooves resulting from the alkalis attack and also the thickness ofthe gel resulting from the ASR attack on the surface of the reactivesand particles. In Fig. 5a and b for 5000 times magnification,grooves on the surface of a reactive particle in CTL mortar seemravenous canyons compared to the smoother and less marked sur-face of a reactive particle in PGS mortar. Comparing for example,Fig. 5a and b for 1000 times magnification it can be seen that thelayer of ASR gel formed on the surface of the reactive aggregatein CTL mortar is thicker than the layer formed in PGS mortar.

EDS was carried out and gel was found in the grooves of the sur-face of the aggregate or in the layers covering the aggregate. Thisgel has considerable amount of sodium as can be seen in the spec-trum, showing that this is ASR gel. Although PGS containing mor-tar, compared to CTL mortar, presented lower overall expansionin the ASR test, ASR gel was still found in grooves and as layerson the aggregate surface.

In terms of chloride ion ingress, for coarser waste material suchas PG, a resulting more permeable matrix reduced chloride resis-tance around 20% compared to CTL (22% increase of Dns for PG5% and 15% for PG 10%). Surprisingly positive results were obtained

for PGS mortar where the finer material seems to induce a densermatrix leading to a better resistance to chloride compared to SFmortar. In fact improvement of this resistance to chlorides was al-most 70% compared to CTL and improved with dosage replacement(67% reduction for PGS 5%, 70% for PGS 10% and 66% for SF).

Figs. 9 and 10 show SEM and EDS results on mortar specimensafter chloride ingress. As can be observed for PGS (5% and 10% ce-ment replacement) chloroaluminates (Friedel’s salt) according to[24,25] were frequently found, some of which shaped as hexagonalplates in accordance with St. John et al. [26]. The presence of chlo-roaluminates suggests that alumna present in granite sludge mayreact with chlorides and thus retard chloride ingress. This may helpexplain lower apparent chloride diffusion coefficients for PGS,however fineness of granite sludge as a partial cement replacementmaterial plays an important role as this effect is only revealed forsufficient fineness.

Performance of mortar with granite powder is compared to CTLin Fig. 11. SF mortar results are also presented for reference. PGmortar showed worst performance but PGS mortar presented bet-ter results than CTL, close to SF results and even better in relationto chlorides for PGS 10 mortar.

4. Conclusion

Quarry granitic sludge waste studied is mainly composed of sil-ica and alumna and therefore in accordance with chemical require-ments in ASTM 618 [16] regarding pozzolanic materials.

Particles observed in SEM showed to be more angular and elon-gated compared to cement but this did not seem to affect work-ability of mortar.

Mortars Strength at 28 days for coarser (PG) and finer (PGS) gra-nitic sludge waste used at 10% cement replacement was lower thancontrol mortar but strength loss was marginal for PGS.

In terms of ASR there was generally no improvement of resis-tance to alkali reaction for PG mortar but for PGS, expansion re-duced with increase in replacement dosage although notattaining effectiveness of SF mortar.

SEM observations and EDS analysis on reactive aggregate parti-cles prior to ASR attack and also after ASR testing led to the follow-ing conclusions:

� ASR testing leads to varying groove depth on the surface of theattacked aggregate surface.� ASR testing leads to the formation of a varying layer thickness of

the gel formed on the surface of the attacked aggregate surface.� More deeply grooved surfaces of the attacked aggregate corre-

spond to thicker gel layer formed.� It seems that deeper grooved surfaces resembling ravinous can-

yons and thicker ASR gel layers were observed on CTL mortar,corresponding to higher measured expansion results.

In terms of chloride ingress, the coarser waste material, PG re-duced chloride resistance but for PGS, finer than cement, animprovement of almost 70% was observed in the resistance to chlo-rides. SEM and EDS analysis on PGS specimens after chloride in-gress revealed the presence of chloroaluminates, suggesting thatalumna present in granite sludge ground to sufficient fineness, re-acts with chlorides, thus retarding chloride penetration.

Therefore this work showed that granitic quarry sludge waste, ifground to sufficient fineness, produces a denser matrix promotingup to 38% reduction in expansion due to ASR and almost 70%improvement in resistance to chlorides (higher than SF mortar).This surprising improvement for fine waste seems to derive fromcaptivation of chlorides by aluminates present in the waste withformation of chloroaluminates.

T. Ramos et al. / Construction and Building Materials 47 (2013) 1001–1009 1009

Finally, a properly engineered use of granitic waste in cement-based composites, leading to enhanced durability without compro-mising workability and strength as shown in this study, can turngranitic quarry sludge, an abundant waste, into a valuable resourceand therefore contribute to sustainable construction.

Acknowledgments

The authors would like to thank DST-DOMINGOS DA SILVATEIXEIRA, S.A., the R&D unit LABEST, Laboratory for Concrete Tech-nology and Structural Behaviour and to LEMC, Laboratory for Test-ing Construction Materials. This work was financed by FEDERfunds under the Operational Program Factors of Competiveness –COMPETE and by National Funds under FCT – Foundation for Sci-ence and Technology through Project PTDC/ECM/098117/2008:Additions from waste materials for sustainable structural concrete.

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