3. EXPERIMENTAL PROCEDURE
3.3 Materials
3.3.1 Fly Ash
The carried out experimental work utilized low calcium Class F fly ash obtained from Collie Power Station located south of Perth, Western Australia. Throughout the research, the fly ash used was from the same delivered batch. The fly ash was obtained in bulk bags and measured from here into the respective amounts required.
3.3.2 Sodium Hydroxide
A sodium hydroxide solution was utilized in all mixes as a constituent in the alkaline reactor. The product was obtained from a local supplier in the form of pellets with a purity of 98%. The solution was prepared by dissolving the pellets into distilled water at specified concentration in molars, M, for the concrete. In the laboratory research carried out, the solution was prepared with a concentration of approximately 10 M by dissolving the sodium hydroxide solids into distilled water.
To produce 1 kg of sodium hydroxide solution, 416.8 grams of pellets was dissolved into 583.2 grams of distilled water. The solid was added to the water gradually and stirred for approximately 20 minutes until all solid had dissolved. It was noticed that upon addition of the solid to water, the solution became hot as the exothermic reaction of dissolution carried out.
Upon preparation of the first mix produced, the sodium hydroxide solution was prepared 4 days prior to its addition to sodium silicate, and then production of concrete. It was discovered that after 4 days of standing, some sodium hydroxide solids had appeared in the solution after being dissolved completely when initially combined, this required stirring of approximately half an hour to reduce the solid content. Subsequent sodium hydroxide solutions made throughout the year were not prepared to a schedule prior to mixing the concrete. Generally though, dilution of
sodium hydroxide occurred a few days before concrete production in order to limit the time spent preparing the chemicals on the concrete mixing day.
3.3.3 Sodium Silicate
The sodium silicate was obtained in 30.5 kilogram pallets from a local chemical supplier, PQ Australia. The grade of material used is known as PQ‐D with a SiO2/Na2O ratio of 2.0. The pH of this liquid was 11.9 and was in the form of a heavy syrup.
The weight analysis of this material was as given by the supplier:
Na2O : 14.7%
SiO2 : 29.4%
Water : 55.9%
No dilution was required, after being weighed out it was used in the concrete as delivered.
3.3.4 Calcium Hydroxide
The calcium hydroxide used in Mix Three is known as HYLIME by Cockburn Cement. It was an industrial grade powder obtainable from the local hardware store, typically used in masonry mortars or plastering applications. This product was used in anticipation of developing a faster curing concrete with a higher early strength.
XRF analysis carried out on the product shows the majority of the composition of HYLIME to consist of 84% by mass of calcium oxide, 7.2% silicon dioxide and 5.3%
magnesium oxide.
3.3.5 Silica Fume
Silica fume was used in Mix Two as a fly ash replacement in hope that it would aid the ambient curing properties of the concrete.
The silica fume used was obtained from local supplier Simcoa, Western Australia. The product was delivered in bags of 10 kilograms, and was known just as Microsilica or densified silica fume. This same product is also used in concrete batching plants in Western Australia, in particular for marine applications. The silica fume is in the form of extremely fine particles and therefore makes the concrete less impermeable upon addition.
3.3.7 Alkaline Liquid
The alkaline solutions for all mixes produced during the research were prepared by combining the sodium hydroxide solution to sodium silicate gradually. This mixture was then stirred moderately for a few minutes and then sealed in the buckets with lids until addition to the concrete mix. This process took place immediately prior to beginning production of the concrete, the ratio of sodium silicate to sodium hydroxide was kept consistent at 2.5 upon recommendation from Hardjito and Rangan (2005).
3.3.8 Aggregate
The aggregate used was supplied by Cemex to Curtin University, stored outside uncovered in storage divisions. The aggregate supplied consisted of two components;
coarse aggregate obtained from the Cemex Gosnells Quarry and a fine aggregate that originated from Baldivis Sand. For the purpose of this research, coarse aggregates were used with nominal sizes of 7mm, 10mm and 20mm, and fine aggregates in the form of sand.
The aggregate was measured approximately a week prior to pouring and sealed in bins. The moisture content of the aggregate was measured at the time of being used in the concrete, and subsequently used to determine the free water content of the concrete mix.
The aggregate proportions were found in accordance with utilizing British Standards BS 882.92 (Neville 2000, 172) grading requirement limits for all‐in aggregate. The grading curve was constructed in order to satisfy the grading limits with an application sourced from the University of Patras.
As can be seen the sieve analysis of the utilized aggregate displayed a grading‐gap, which is displayed on the grading curve below (Figure 3.1). This made proportioning the aggregate components a more stringent process. Neville (2000) suggests that a grading curve closer to the bottom limit is comparatively workable, and can therefore be used in mixes with a low liquid/binder ratio. The results of sieve analysis and grading combinations of the utilized aggregates can be seen below in Table 3.1.
Particle size (mm) BS Sieve
ISO Sieve
Figure 3.1: Grading Curve of Combined Aggregates
(Grading Curve 2009)
Table 3.1: Grading of Combined Aggregates
20 mm 10 mm 7 mm Fine
19.00 mm 98.10 100.00 100.00 100.00 99.43 95‐100
9.50 mm 0.19 90.68 100.00 100.00 68.66
4.75 mm 0.14 1.16 44.67 99.94 41.37 35‐55
2.36 mm 0.14 0.71 1.49 99.78 30.46
1.18 mm 0.14 0.69 0.52 99.47 30.12
600 μm 0.14 0.69 0.37 70.98 21.53 10‐35
300 μm 0.13 0.68 0.25 17.81 5.55
150 μm 0.11 0.66 0.11 1.96 0.75 0‐8
Ratio 30 15 25 30
3.4 Preliminary Laboratory Work
The aim of this research was to gain a knowledge and understanding of the effect of altering mix designs in a geopolymer concrete mix. Due to the lack of experience in any geopolymer concrete production by the author, it was suggested that to begin with, a standard geopolymer concrete mix using the established sodium hydroxide and sodium silicate alkaline solution would be made first to familiarize with the process and use a reference to other mixes.
The first two mixes were undertaken at the beginning of June, 2009, with the use of the 70 litre capacity pan mixer (Figure 3.2) to produce approximately 65 litres (156 kilograms) of geopolymer concrete. Samples were placed in test specimens, 100mm x 200mm compression cylinders and 150mm x 300mm tensile cylinders, and cured under the ambient conditions after pouring.
The preliminary laboratory works focused on the following main objectives:
- To familiarize with the making of fly ash based geopolymer concrete.
- To develop an understanding of an appropriate mix procedure in the production of fly ash based geopolymer concrete.