Original citation: Lee, G., Ling, T.-C., Wong, Y.-L., Poon, C.-S.

(2011) Effects of crushed glass cullet sizes, casting methods and pozzolanic materials on ASR of concrete blocks. Construction and Building Materials; 25 (5): 2611-2618. http://www.sciencedirect.com/science/article/pii/S0950061810006859

Effects of crushed glass cullet sizes, casting methods and pozzolanic materials on ASR of concrete blocks
Gerry Lee, Tung-Chai Ling, Yuk-Lung Wong and Chi-Sun Poon* Department of Civil and Structural Engineering The Hong Kong Polytechnic University Abstract The aim of this study is to investigate the influence of using different particle sizes of recycled glass, casting methods and pozzolanic materials in reducing the expansion due to alkali-silica reaction (ASR) of concrete blocks prepared with the use of crushed glass as fine aggregate. In this work, 2525285mm mortar bar specimens were prepared using conventional wet-mixed and dry-mixed methods. Except for the control mortar bar, all the specimens were prepared by completely replacing river sand with different particle sizes of recycled glass. In addition, the influence of fly ash (PFA) and metakaolin (MK) content on the reduction of ASR expansion was also investigated. The flexural strength of the mortar bar specimens before and after they had been exposed to 1 N NaOH solution was determined to complement the results of ASR expansion test. SEM was performed to examine the microstructure as well as nature of the cement binder-glass interfacial zone. The results reveal that ASR expansion reduced with reducing particle size of glass used. For the same given mix proportion, the dry-mixed method resulted in 44% less expansion when compared with the wet-mixed method. Both PFA and MK were demonstrated to be able to reduce ASR expansion of the concrete glass blocks significantly. Keywords: Recycled glass, particle size distribution, ASR, dry-mixed method, pozzolanic materials 1. Introduction Recently, the use of recycled glass as aggregate in concrete has attracted much research interest. It is known that concrete containing glass aggregate has lower water absorption and drying shrinkage [1-3]. However, the use of glass in concrete may result in expansion due to alkali-silica reaction (ASR) [4-6]. A number of studies have been done by several researchers to study the influence of different particle sizes, colours and percentages of glass used in concrete on ASR expansion. In general, the ASR expansion decreased with decreasing particle size of glass aggregate. Meyer et al. [10] found that there was no deleterious expansion when the particle size of glass was less than 100m.This phenomenon is related to the large surface area of glass which allows the pozzolanic reaction to occur [2]. Byars et al. [7] examined the effect of glass colour on ASR reactivity and found that blue glass aggregate appeared to be most reactive, followed by *Second author: t.ling.1@bham.ac.uk; tcling611@yahoo.com Page 1

amber and then flint glass. Green glass showed the least ASR reactivity. Tapcu et al. [8] also reported that the higher content of silica in clear glass caused the concrete to suffer more in ASR expansion. Some of the researchers have reported that different glass colours have different pessimum size. Pessimum size refers to the size of the reactive glass aggregate where the largest ASR expansion may occur. For regular soda lime clear glass, Pyrez glass and fused silica, the pessimum size is found to be at 1.18mm, 150m and 75m, respectively [9]. For the effect of percentage of glass, most of the reported data concluded that ASR expansion decreased with decreasing percentage of recycled glass used in concrete [4]. Modifying the cementitious system may also reduce the ASR reaction. Several papers have been published [7, 11] on the use of suitable pozzolanic materials such as silica fume (SF), fly ash (FA), ground granulated blast furnace slag (GBFS) and metakaolin (MK) in the concrete mix at appropriate proportions to react with calcium hydroxide to reduce the alkalinity of the cementitious system. Among the mineral additives, SF was found to be the most effective in reducing the expansion [7]. Recently, studies have found that a combination of mineral additives was more effective than using a single type of mineral additive alone in reducing ASR expansion [12, 13]. Byars et al. [7] have assessed the effect of cement alkali levels on glass ASR reactivity. In their work, white cement which had a lower alkali content (Na2O equivalent: 0.17%) appeared to cause less expansion than ordinary Portland cement (Na2O equivalent: 0.62%). However, not much attention has been paid to assess the effect of different concrete casting methods on the expansion caused by ASR. It is expected that lower moisture level (water amount) in dry-mixed concrete could be an effective alternative solution to reduce ASR expansion. The objective of this study was to determine the ASR expansion of mortar bars prepared with different casting methods (dry-mixed and wet-mixed). The effects of different particle sizes of recycled glass were also evaluated. Ways to further reduce the ASR expansion by using different pozzolanic materials were compared.

2. Experimental details 2.1. Materials Ordinary Portland cement (OPC) complying with BS 12 [14] and ASTM Type I was used as the principal cementitious material. Fly ash (PFA) and metakaolin (MK) were used as pozzolanic materials. The chemical compositions and physical properties of all the cementitious materials are presented in Table 1. River sand was used as the fine aggregate for the control mortar bar mixture and its density and fineness modulus were 2,630 kg/m3 and 2.46, respectively. Post-consumer glass bottles with a green color obtained from a local glass recycling plant were used. The recycled glass bottles were crushed into smaller particle sizes and used to replace sand in the mortar bar mixtures. 2.2. Preparation of mortar bar specimens 2.2.1. Prepared with different particles size of recycled glass In this study, four different particles size of recycled fine glass was used as a full replacement (100%) of river sand by mass in all mixes and their gradation curves are shown in Fig. 1. The four different particles size of crushed glass used were:

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a) FG-A was un-sieved glass having maximum size of 5 mm with a fineness modulus of 3.29. b) FG-B was sieved glass (2.36mm) with a fineness modulus of 3.03. c) FG-C was sieved glass (1.18 mm) with a fineness modulus of 2.33. d) FG-D was sieved glass (600 m) with a fineness modulus of 0.43. Table 1. Chemical composition and physical properties of cementitious materials Cement PFA MK SiO2 (%) 19.61 56.79 53.20 Fe2O3 (%) 3.32 5.31 0.38 7.33 28.21 43.90 Al2O3 (%) CaO (%) 63.15 <3 0.02 MgO (%) 2.54 5.21 0.05 SO3 (%) 2.13 0.68 Na2O (%) 0.17 K2O (%) 0.10 TiO2 (%) 1.68 Loss on Ignition (%) 2.97 3.9 0.50 Density (kg/m3) 3,160 2,310 2,620 Specific Surface Area (cm2/g) 3,520 3,960 12,680

100 90 80

P ercen ta g e p a ssin g (% )

70 60 50 40 30 20 10 0 0 .0 0 0 .1 5 0 .3 0 0 .6 0 1 .1 8 2 .3 6 5 .0 0 1 0 .0 0

Max Limit o f BS 822 Min Limit o f BS 822 S and A-F G (un-sieved ) B-F G (< 2.36mm) C -F G (< 1.18mm) D-F G (< 0.6mm)

B S sie v e size (m m )

Fig. 1. Grading curves of fine aggregates

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2.2.2. Prepared by wet-mixed and dry-mixed (casting) method For each mortar bar mix, a fixed cement to fine aggregate ratio of 1:2.25 was used and the prepared mortars were cast into rectangular prisms of dimensions 2525285 mm. Different water contents were used for the production of the wet-mixed and dry-mixed mortar bars. The mix proportions are presented in Table 2. For the wet-mixed method, the water to cement ratio was kept constant at 0.45 and a superplasticizer- Sulfonated naphthalene formaldehyde condensate was used to adjust the workability. Table 2. Mix proportions of wet-mixed and dry-mixed mortar bars (kg/m3) Mix Notation Cement Sand FG-A FG-B FG-C FG-D W/C (SP, %) 440 WM-Control 990 0 0 0 0 0.45 0 440 0 WM-A 990 0 0 0 0.45 1.0 440 0 WM-B 0 990 0 0 0.45 1.3 440 0 WM-C 0 0 990 0 0.45 1.5 440 0 990 2.1 WM-D 0 0 0 0.45 440 DM-Control 990 0 0 0 0 0.27 0 440 0 DM-A 990 0 0 0 0.27 0 440 0 DM-B 0 990 0 0 0.28 0 440 0 DM-C 0 0 990 0 0.29 0 440 0 0.34 DM-D 0 0 0 990 0 Cement and fine aggregate materials were first placed in a pan mixer and mixed for about 1 minute before water was added. The superplasticizer thoroughly mixed with water was added to the mixer, and the mixing was continued for another 2 minutes. The freshly wet-mixed materials were placed into the mortar bar mould in two layers of approximately equal depth. After each layer was filled, a uniform vibration was applied by using a vibrating table. For the dry-mixed method, the materials were prepared with only sufficient amount of water to produce a cohesive mix but with zero slump. After mixing the materials in the pan mixer, the materials were placed into the mortar bar moulds in four layers of about equal thickness. A compression force was applied manually by hammering a wood stem on the surface layer to provide an evenly distributed compaction for the first three layers. At fourth layer, the overfilled materials were subjected to a static compaction load by using a compression machine. The load increased at the rate of 600 kN/min for 50 seconds for the first static compaction. The excess material was then removed to provide a good surface texture and second compaction was applied at the same rate until it reached 500 kN. After casting, all the wet-mixed and dry-mixed mortar bar specimens were covered with a plastic sheet in the laboratory at 233C and 75% relative humidity. After one day, all the specimens were demoulded and stored in a water tank at an average temperature of 253 C until the day of testing. 2.2.3. PFA and MK replacement of OPC Some dry-mixed mortar bar specimens with the inclusion of PFA and MK were also prepared in order to further investigate the effect of admixture content on the ASR expansion. The

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specimens were prepared with four different particle sizes of 100% recycled glass. For each particular size of glass, PFA and MK at dosages of 5, 10 and 20% by weight of cement were added in the mortar mixtures. The mix proportions of dry-mixed mortar bar prepared with PFA and MK are shown in Tables 3 and 4, respectively. 2.3. Test program To measure the ASR expansion for a given mix proportion, an accelerated mortar bar test was carried out on three prism specimens of 2525285 mm in accordance with ASTM C1260 [15]. After 28 days of water curing, the mortar bar specimens were removed from the water tank and stored in distilled water at 80 oC for another 24 hours at which a zero reading was taken. The bars were then transferred and immersed in 1 N NaOH ( solution were prepared by diluting 40 g of sodium hydroxide crystals into 900 mL of distilled water) at 80 C until the testing time at 1st, 4th, 7th, 14th and 28th day. The expansion of the mortar bars was measured within 155 seconds after the mortar bars were removed from the 80 C distilled water or alkali storage condition by using a length comparator. Before and after the ASR test, the flexural strength test was carried out under a central line load simply supported over a span of 120 mm with a displacement rate of 0.05 mm/min. After the mechanical testing, selected samples were used to examine the microstructure by Scanning Electron Microscopy (SEM), in particular the nature of the binder-glass interfacial zone. The fractured samples with size smaller than 101010 mm were immersed in acetone for 4 hours and dried in a vacuum oven in order to eliminate any free water for cement hydration. The samples were then gold coated and analyzed by SEM operated at an accelerating voltage of 20 kV with a probe current of 70 to 78 A.

3. Results and discussion 3.1. Effect of particle size of recycled glass on ASR expansion The average ASR expansion results of the mortar bars prepared with different particle sizes of glass are shown in Fig. 2. The results show that in all cases, the ASR expansions of the wet-mixed samples were higher than that of the dry-mixed sample. Regardless of the particle size of glass, all the ASR expansion of the dry-mixed mortar bars were found to be within the permissible limit of 0.1% at 14 days. However, the expansion of the wet-mixed mortar bars prepared with FG-A and FG-B were found to be higher than the limit set by ASTM C 1260. It can also be noticed that there was an increase of approximately 8% and 28% respectively in average of the expansion when the wet-mixed and dry mixed mortar bars were continued to be placed in the aggressive ( 1N NaOH alkali solution) for an additional 14 days. From the figure, it can be clearly observed that the ASR expansion decreased with decreasing particle size of glass. This might be due to some fine glass containing high content of active silica can be classified as a reactive aggregate or a pozzolanic material [16]. This is consistent with the results of Shi et al. [11]. They reported that glass particle with size less than 0.7 mm had a pozzolanic strength activity index of 74% at 7 days which is nearly achieved the minimum of 75% as specified in ASTM C618 for pozzolanic materials. Also, the figure shows the influence of particle size of glass on the wet-mixed mortar bars was more pronounced than that on the dry-mixed mortar bars.

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0 .16
dry -m ix ed (14 day s )

0 .14 A S R exp an sio n (% ) 0 .12 0 .10 0 .08 0 .06 0 .04 0 .02 0 .00 contro l un-sieve d <2.36m m

dry -m ix ed (28 day s ) w et-m ix ed (14 day s ) w et-m ix ed (28 day s )

<1.1 8m m

<0.60m m

S iz e c las ses o f g la ss ag g re g ate (m m )

Fig. 2. Effect of different particles size of glass on ASR expansion at 14 and 28 days 3.2. Effect of wet-mixed and dry-mixed (casting) methods on ASR expansion The effect of the dry-mixed (casting) method on the reduction (compared with the wet-mixed method) of ASR expansion of the mortar bars incorporating different particle sizes of glass is shown in Fig. 3. The results show that using dry-mixed method was very effective in reducing the ASR expansion especially for larger particle size (higher reactivity) glass aggregates. This may be due to the mortar bars prepared with the dry-mixed method contained higher porosity and larger capillary pores (see Fig. 4a), thus, able to accommodate larger amount of ASR gel (see Fig. 4b), resulting in lower expansion and less cracks when compared with the mortar bars made with the wet-mixed method. Another possible reason is that the dry-mixed method had limited the availability of excessive moisture in the cement matrix that would be effective in preventing ASR deterioration. It is known that the ASR expansion is closely related to the durability of concrete. Fig. 5 shows the effect of the wet-mixed and the dry-mixed (casting) methods on the reduction of flexural strength after the mortar bars were exposed to the aggressive environment (1 N NaOH at 80C) for 14 days. It can be clearly observed that the ASR caused a large reduction in the flexural strength especially for the mortar bars prepared with the wet-mixed method. This phenomenon could be explained by the ASR gel led to expansion and cracks in the mortar bars. As seen in Fig. 6, the mortar bars prepared with the wet-mixed method experienced severe ASR cracking. From the SEM images, it can be seen that the width of these ASR cracking increased consistently with increasing particle size of the glass used. On the other hand, no cracks were observed in all the mortar bars made by the dry-mixed method, with an average reduction of 50% in flexural strength reduction as compared to wet-mixed method. *Second author: t.ling.1@bham.ac.uk; tcling611@yahoo.com

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60 Reduction of ASR expansion (%) 50 40 30 20 10 0 control -10 -20 -30 Size classes of glass aggregate (mm) un-sieved <2.36mm <1.18mm <0.60mm
14 days 28 days

Fig. 3. Effect of dry-mixed method on the reduction (compared with wet-mixed method) of ASR expansion

(a)

(b)

Fig. 4. SEM image of DM-A (a) before and (b) after exposed to 1 N NaOH at 80C

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70 Reduction of flexural strength (%)

wet-mixed

60 50 40 30 20 10 0 control un-sieved <2.36mm <1.18mm

dry-mixed

<0.60mm

Size classes of glass aggregate (mm)

Fig. 5. Effect of wet-mixed and dry-mixed on the reduction of flexural strength after exposed to rapid environment (1 N NaOH at 80C) for 14 days

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(ai) WMControl No crack observed

(bi) DMControl No crack observed

(aii) WM-A Cracks observed

(~8-12m)

(bii) DM-A No crack observed

(aiii) WM-B Cracks observed

(~8-10m)

(biii) DM-B No crack observed

(aiii) WM-C Cracks observed

(~4-6m)

(biii) DM-C No crack observed

(aiv) WM-A Cracks observed

(<4m)

(biv) DM-D No crack observed

Fig. 6. SEM image of mortar bars after exposed to rapid environment for 14 days (a) wetmixed (b) dry-mixed 3.3. Influence of PFA and MK on ASR expansion Figs. 7 and 8 show the influence of PFA and MK content on the ASR expansion at 14 and 28 days, respectively. It can be seen that the ASR expansion noticeably decreased with an increase in PFA and MK content regardless of the particle sizes of recycled glass used. This

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could be due to the pozzolanic reaction led to the formation of C-S-H gel that is able to take up alkalis and subsequently led to the reduction of ASR expansion [8]. A comparison of efficiency of PFA and MK on ASR expansion of mortar bars prepared with different particles sizes of glass is also included in Figs. 7 and 8. It is found that when the amount of PFA is at 5%, the ASR expansion at 14 days was reduced to the range of 0.028% to 0.035% regardless of the particle size of glass used. However, as the amount of PFA was increased to 10% and 20%, there was no significant change in ASR expansion. On the other hand, as the amount of MK increased from 0% to 5%, 10% and 20%, there was a gradual reduction in ASR expansion by approximately 14.2%, 29.3% and 47.2%, respectively, regardless of the particle sizes of glass used. Fig. 9 compares the effectiveness of PFA and MK in reducing the ASR expansion at 14 days. It is worth to note that the expansion reduction of mortar bars containing 5% PFA was clearly higher than that of the mortar bars containing the same percentage of MK. This indicated that at a low content of pozzolanic materials used, PFA is found to be more effective than MK in reducing the expansion due to ASR. However, as the PFA and MK contents increased to 20%, for any given mix proportion, the effectiveness on the reduction of ASR expansion were quite similar.
0.09 0.08 0.07 ASR Expansion (%) 0.06 0.05 0.04 0.03 0.02 0.01 0
Control Control Control
14 days 28 days

Control

Fig. 7. Influence of PFA content on the ASR expansion at 14 and 28 days

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D M M A -A D M P5 -A D -P1 M -A 0 -P 20 D M D M B -B D M -P5 -B D -P1 M -B 0 -P 20 D D M-C M D C -P M -C 5 D -P 1 M -C 0 -P 20 D M D M -D -D D M P5 -D D -P 1 M -D 0 -P 20 D

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0.09 0.08 0.07 ASR Expansion (%) 0.06

Control Control Control Control
14 days 28 days

0.05 0.04 0.03 0.02 0.01 0

D M M -A -A D M M5 -A D -M 1 M -A 0 -M 20 D M D M -B -B D M M5 -B D -M 1 M -B 0 -M 20 D M D M -C D C-M M -C 5 D -M M 1 -C 0 -M 20 D D M-D M D D-M M -D 5 D -M M 1 -D 0 -M 20

Fig. 8. Influence of MK content on the ASR expansion at 14 and 28 days

5%PFA 10%PFA 20%PFA 5%MK 10%MK 20%MK

Reduction of ASR expansion (%)

70 60 50 40 30 20 10 0 un-sieved <2.36mm <1.18mm <0.60mm

Size classes of glass aggregate (mm)

Fig. 9. Comparison of PFA and MK on the reduction of ASR expansion at 14 days 3.4. SEM observation SEM was performed to examine the microstructures of the cement binder-glass interfacial zone matrix. Fig. 10 presents SEM images obtained on (a) DM-A, (b) DM-D and (c) DM-AP20 after they were exposed to 1 N NaOH solution. Compared to DM-A, there were greats deals of crystals of calcium silicate hydrate (C-H-S) as well as crystals of calcium aluminate that can be seen in DM-D. A similar manner to that of DM-D was also observed in DM-AP20, where the microstructure of the hydrated paste is presented by the formation of an *Second author: t.ling.1@bham.ac.uk; tcling611@yahoo.com Page 11

additional C-S-H, possibly due to hydration of PFA hydration products. This revealed that the particle sizes of glass less than 600m and the use of PFA significantly enhanced the pozzolanic reaction in cement mortar and thus less of the alkali content was available for activity of ASR. (a) DM-A

Glass

(b) DM-D

Glass

(a) DM-A-P20

Glass

Fig. 10. SEM images of sample (a) DM-A, (b) DM-D and (c) DM-A-P20

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4. Conclusions Based on the experimental test results, the following conclusions can be drawn: 1. ASR expansion reduced with reducing particle sizes of glass, in particular for glass size less than 600 m. 2. The dry-mixed method was very efficient in reducing the ASR expansion especially for larger particle size (highly reactive) glass aggregate. For a given mix proportion, the reduction of expansion is up to about 44% as compared with the wet-mixed method. It was understood by the mortar bars made by dry-mixed method had higher porosity which was able to accommodate more gel produced due to ASR resulting in lower expansion and cracks. 3. Both PFA and MK can effectively mitigate ASR expansion regardless of the particle sizes of glass used. At low replacement level, PFA was more effective than MK in controlling ASR. However, at higher replacement percentage, both PFA and MK showed similar effectiveness in suppressing ASR expansion. 4. Observation of SEM images confirmed that the use of very fine glass (< 600m) and pozzolanic material had significantly enhanced the pozzolanic reaction and leads to a lower content of alkali level in preventing activity of ASR.

Acknowledgement The authors would like to thank the Hong Kong Polytechnic University for funding support.

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[11] Shi C, Wu Y, Riefler C, Wang H. Characteristics and pozzolanic reactivity of glass powders. Cem Concr Res 2005;35(5):987-93. [12] Schwarz N, Cam H, Neithalath N. Influence of a fine glass powder on the durability characteristics of concrete and its comparison to fly ash. Cem Concr Compos 2008;30(6):486-96. [13] zkan O, Yksel I. Studies on mortars containing waste bottle glass and industrial byproducts. Constr Build Mater 2008;22(6):1288-98. [14] BS 12. Specification for Portland cement. British Standards Institution; 2001. [15] ASTM C 1260. Standard test method for potential alkali reactivity of aggregates (mortar-bar method). American Society of Testing Materials; 2007. [16] Zhu HY, Chen W, Zhou W, Byars EA. Expansion behaviour of glass aggregates in different testing for alkali-silica reactivity. Mater Structur 2009;42(4):485-94.

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