1

Materials selection, proportioning and quality control

S Mindess

1.1 Introduction
High performance concretes (HPC) are concretes with properties or attributes which satisfy the performance criteria. Generally concretes with higher strengths and attributes superior to conventional concretes are desirable in the construction industry. For the purposes of this book, HPC is defined in terms of strength and durability. The researchers of Strategic Highway Research Program SHRP-C-205 on High Performance Concrete1 defined the high performance concretes for pavement applications in terms of strength, durability attributes and water-cementitious materials ratio as follows: It shall have one of the following strength characteristics: 4-hour compressive strength ^25OO psi (17.5 MPa) termed as very early strength concrete (VES), or 24-hour compressive strength ^50OO psi (35 MPa) termed as high early strength concrete (HES), or 28-day compressive strength ^10,0OO psi (70 MPa) termed as very high strength concrete (VHS). It shall have a durability factor greater than 80% after 300 cycles of freezing and thawing. It shall have a water-cementitious materials ratio =$0.35.

High strength concrete (HSC) could be considered as high performance if other attributes are satisfactory in terms of its intended application. Generally concretes with higher strengths exhibit superiority of other attributes. In North American practice, high strength concrete is usually considered to be a concrete with a 28-day compressive strength of at least 6000 psi (42MPa). In a recent CEB-FIP State-of-the-Art Report on High

Strength Concrete2 it is defined as concrete having a minimum 28-day compressive strength of 8700 psi (6OMPa). Clearly then, the definition of 'high strength concrete' is relative; it depends upon both the period of time in question, and the location. The proportioning (or mix design) of normal strength concretes is based primarily on the w/c ratio 'law' first proposed by Abrams in 1918. At least for concretes with strengths up to 6000 psi (42MPa), it is implicitly assumed that almost any normal-weight aggregates will be stronger than the hardened cement paste. There is thus no explicit consideration of aggregate strength (or elastic modulus) in the commonly used mix design procedures, such as those proposed by the American Concrete Institute.3 Similarly, the interfacial regions (or the cement-aggregate bond) are also not explicitly addressed. Rather, it is assumed that the strength of the hardened cement paste will be the limiting factor controlling the concrete strength. For high strength concretes, however, all of the components of the concrete mixture are pushed to their critical limits. High strength concretes may be modelled as three-phase composite materials, the three phases being (i) the hardened cement paste (hep); (ii) the aggregate; and (iii) the interfacial zone between the hardened cement paste and the aggregate. These three phases must all be optimized, which means that each must be considered explicitly in the design process. In addition, as has been pointed out by Mindess and Young,4 'it is necessary to pay careful attention to all aspects of concrete production (i.e. selection of materials, mix design, handling and placing). It cannot be emphasized too strongly that quality control is an essential part of the production of high-strength concrete and requires full cooperation among the materials or ready-mixed supplier, the engineer, and the contractor'. In essence then, the proportioning of high strength concrete mixtures consists of three interrelated steps: (1) selection of suitable ingredients cement, supplementary cementing materials, aggregates, water and chemical admixtures, (2) determination of the relative quantities of these materials in order to produce, as economically as possible, a concrete that has the desired rheological properties, strength and durability, (3) careful quality control of every phase of the concrete-making process.

1.2

Selection of materials

As indicated above, it is necessary to get the maximum performance out of all of the materials involved in producing high strength concrete. For convenience, the various materials are discussed separately below. However, it must be remembered that prediction with any certainty as to how they will behave when combined in a concrete mixture is not feasible. Particu-

larly when attempting to make high strength concrete, any material incompatibilities will be highly detrimental to the finished product. Thus, the culmination of any mix design process must be the extensive testing of trial mixes. High strength concrete will normally contain not only portland cement, aggregate and water, but also superplasticizers and supplementary cementing materials. It is possible to achieve compressive strengths of up to 14,000 psi (98 MPa) using fly ash or ground granulated blast furnace slag as the supplementary cementing material. However, to achieve strengths in excess of 14,000 psi (100 MPa), the use of silica fume has been found to be essential, and it is frequently used for concretes in the strength range of 9000-14,000 psi (63-98 MPa) as well.

Portland cement
There are two different requirements that any cement must meet: (i) it must develop the appropriate strength; and (ii) it must exhibit the appropriate rheological behaviour. High strength concretes have been produced successfully using cements meeting the ASTM Standard Specification C150 for Types I, II and III portland cements. Unfortunately, ASTM C150 is very imprecise in its chemical and physical requirements, and so cements which meet these rather loose specifications can vary quite widely in their fineness and chemical composition. Consequently, cements of nominally the same type will have quite different rheological and strength characteristics, particularly when used in combination with chemical admixtures and supplementary cementing materials. Therefore, when choosing portland cements for use in high strength concrete, it is necessary to look carefully at the cement fineness and chemistry. Fineness Increasing the fineness of the portland cement will, on the one hand, increase the early strength of the concrete, since the higher surface area in contact with water will lead to a more rapid hydration. On the other hand, too high a fineness may lead to rheological problems, as the greater amount of reaction at early ages, in particular the formation of ettringite, will lead to a higher rate of slump loss. Early work by Perenchio5 indicated that fine cements produced higher early age concrete strengths, though at later ages differences in fineness were not significant. Most cements now used to produce high strength concrete have Elaine finenesses that are in the range of 1467 to 1957 ft2/lb (300 to 400 m2/kg), though when Type III (high early strength) cements are used, the finenesses are in the range of 2201 ft2/lb (450 m2/kg).

Chemical composition of the cement The previously cited work of Perenchio5 indicates that cements with higher C3A contents leads to higher strengths. However, subsequent work6 has shown that high C3A contents generally leads to rapid loss of flow in the fresh concrete, and as a result high C3A contents should be avoided in cements used for high strength concrete. Aitcin7 has shown that the C3A should be primarily in its cubic, rather than its orthorhombic, form. Further, Aitcin7 suggests that attention must be paid not only to the total amount of SO3 in the cement, but also to the amount of soluble sulfates. Thus, the degree of sulfurization of the clinker is an important parameter. In addition to commercially available cements conforming to ASTM Types I, II and III, a number of cements have been formulated specifically for high strength concrete. For instance, in Norway, Norcem Cement has developed two special cements for high strength concrete, in addition to their ordinary portland cement. The characteristics of these cements are given in Table 1.1.s Note that for the two special cements (SP30-4A and SP30-4A MOD), the C3A contents were held to 5.5%.
Table 1.1 Composition of special cements for high strength concrete (developed by Norcem Cement8)

SP30*
C2S (%) C3S (%) C3A (%) C4AF (%) MgO (%) S0 3 (%) Na2O equivalent (%) Elaine fineness (m2/kg) heat of hydration (kcal/kg) setting time (min): initial final

SP30-4A
28 50 5.5 9 1.5-2.0 2-3 0.6 310 56 140 200

SP30-4A MOD
28 50 5.5 9 1.5-2.0 2-3 0.6 400 70 120 170

18 55 8 9 3 3.3 1.1 300 71 120 180

* Ordinary portland cement, for comparison Im 2 /kg = 4.89ft 2 /lb

Supplementary cementing materials

As indicated above, most modern high strength concretes contain at least one supplementary cementing material: fly ash, blast-furnace slag, or silica fume. Very often, the fly ash or slag is used in conjunction with silica fume. These materials are all specified in the Canadian CSA Standard A23.5.9 In the United States, fly ash is specified in ASTM C618,10 and blast furnace slag in ASTM C98911; there is, as yet, no U.S. standard for silica fume. These materials are described in detail in Supplementary Cementing Materials for Concrete.12 Using a somewhat different approach, a high silica modulus portland

Table 1.2 Bogue composition and other properties of HTS cement (after Aitcin et al.13) C 2 S(%) C3S (%) C3A (%) C 4 AF(%) Na2O equivalent (%) lime saturation factor silica modulus Elaine fineness, m2/kg Im 2 /kg = 4.89ft 2 /lb
22 62 3.6 6.9 0.38 92.7 4.8 320

cement (referred to as HTS, or Haute Teneur en Silica, or high silica content) was developed,13 with the composition shown in Table 1.2. Note that, compared to more conventional cements (such as the SP-30 of Table 1.1), there is a very high total silicate content (84%), and C3A content of only 3.6%. The cement is rather coarsely ground (Elaine fineness of 1565 ft2/lb (320 m2/kg)). It is made from a clinker composed of small alite and belite crystals, and minute C3A crystals. It is capable of producing concretes with excellent 28-day compressive strengths, as indicated in Table 1.3, when used in conjunction with 10% silica fume.
Table 1.3 28 day compressive strengths of concrete made with HTS cement and 10% silica fume13

vv/c 0.31 0.23 0.20 0.17

1 ksi = 6.89 MPa lMPa = 0.145ksi

fc

(MPd)

74 106 115 124

Silica fume It is possible to make high strength concrete without silica fume, at compressive strengths of up to about 14,000psi (98MPa). Beyond that strength level, however, silica fume becomes essential, and even at lower strengths 9000-14,000 psi (63-98 MPa), it is easier to make HSC with silica fume than without it. Thus, when it is available at a reasonable price, it should generally be a component of the HSC mix. Silica fume14 is a waste by-product of the production of silicon and silicon alloys, and is thus not a very well-defined material. Consequently, it is important to characterize any new source of silica fume, by determining the specific surface area by nitrogen adsorption, and the silica, alkali and carbon contents. In addition, it is desirable to minimize the content of

the mixes shown in Table 1.9, Burg and Ost19 found that, when specimens that had been moist cured for 28 days were then subjected to air curing, their strengths at 91 days exceeded those of continuously moist-cured specimens; however, by 426 days, the continuously moist-cured specimens were from about 3% to 10% higher in strength than the air-cured ones. On the other hand, several investigators have reported that, as long as a week or so of moist curing is provided, subsequent curing under ambient conditions is not particularly detrimental to strength development. Peterman and Carrasquillo16 have stated that 'the 28-day compressive strength of high strength concrete which has been cured under ideal conditions for 7 days after casting is not seriously affected by curing in hot or dry conditions from 7 to 28 days after casting.' Finally, contrary results were reported by Moreno30 who indicated that air-cured specimens were about 10% stronger than moist-cured specimens at all ages up to 91 days.

Type of mold for casting cylindrical specimens

ASTM C470: Molds for Forming Concrete Test Cylinders Vertically, describes the requirements for both reusable and single-use molds, and ASTM C31: Making and Curing Concrete Test Specimens on the Field permits both types of mold to be used. However, it has long been known that different molds conforming to ASTM C470 will result in specimens with different measured strengths. This is true for both normal strength and high strength concretes. In general, more flexible molds will yield lower strengths than very rigid molds, because the deformation of the flexible molds during rodding or vibration leads to less efficient compaction than when using rigid molds. The experimental data largely bear this out. It should be noted that, whatever the mold materials, the molds must be properly sealed to prevent leakage of the mix water. If any significant leakage does occurs, the apparent strength will generally increase, because of the lower effective w/c ratio, and increased densification of the specimens. For the standard 6x12 in. (150x300 mm) molds, Carrasquillo and Carrasquillo29 found that steel molds gave strengths about 5% higher than plastic molds, while Hester31 found about a 10% difference. Similar results were reported by Howard and Leatham.32 Peterman and Carrasquillo16 reported that steel molds gave strengths about 10% higher than those obtained with cardboard molds, and Hester31 showed that steel molds gave strengths about 6% higher than tin molds. On the other hand, Cook15 reported that 'good success was experienced on the use of single-use rigid plastic molds', while Aitcin33 reports increasing use of rigid, reusable plastic molds. In addition, Carrasquillo and Carrasquillo29 have reported that for the smaller 4 x 8 i n . (100 x 200 mm) molds, there were no strength differences between steel, plastic or cardboard molds.

In view of the above results, it would be prudent to use rigid steel molds whenever practicable, particularly for concrete strengths in excess of about 14,000 psi (98 MPa), at least until more test data become available for the smaller molds.

Specimen size
For most materials, including concrete, it has generally been observed that the smaller the test specimen, the higher the strength. For high strength concrete, however, though this effect is often observed, there are contradictory results reported in the literature. The results of a number of studies are compared in Table 1.11. It may be seen that the observed strength ratios of 4 x 8 i n . (100x200 mm) cylinders to 6x12 in. (15Ox 300 mm)cylinders range from about 1.1 to 0.93. These contradictory results may be due to differences in testing procedures amongst the various investigators. It must be noted that while for a given set of materials and test procedures, it may be possible to increase the apparent concrete strength by decreasing the specimen size, this does not in any way change the strength of the concrete in the structure. One particular specimen size does not give 'truer' results than any other. Thus, one should be careful to specify a particular specimen size for a given project, rather than leaving it as a matter of choice.

Specimen end conditions

According to ASTM C39: Compressive Strength of Cylindrical Concrete Specimens, the ends of the test specimens must be plane within 0.002 in. (0.05 mm). This may be achieved either by capping the ends (usually with a sulfur mortar) or by sawing or grinding. Unfortunately, different end
Table 1.11 Effect of specimen size on the compressive strength of high strength concrete Investigator Peterman and Carrasquillo16 Carrasquillo, Slate and Nilson34 Howard and Leatham32 Cook15 Burg and Ost19 Aitcin33 Moreno30 83 MPa concrete 119 MPa concrete Carrasquillo and Carrasquillo29 fc (100 x 200 mm cylinder) fc' (150 x 300 mm cylinder)

-1.1 -1.1 -1.08 -1.05 -1.01 ambiguous results -1.0 -0.93 -0.93

conditions can lead to different measured strengths, and so the end preparation for testing high strength concrete specimens should be specified explicitly for any given project. The most common method for preparing the ends of normal strength concrete is to use sulfur caps; for high strength concrete, high strength sulfur mortars are commercially available. However, if the strength of the cap is less than the strength of the concrete, the compressive load will not be transmitted uniformly to the specimen ends, leading to invalid results. Thus, for high strength concrete, in addition to high strength capping compounds, a number of other end preparation techniques are being investigated. These include grinding the specimen ends, or using unbonded systems, consisting of a pad constrained in a confining ring which fits over the specimen ends. Most compressive strength tests on high strength concrete are still carried out using a high strength capping compound. The materials available in North America will achieve compressive strengths of 12,000 psi to 13,000 psi (84MPa to 91 MPa) when tested as 2 in. (50mm) cubes.33 Peterman and Carrasquillo21 recommend the use of such capping compounds, since they give higher concrete strengths than ordinary capping compounds. Cook16 has used such compounds for concrete strengths up to 10,000 psi (7OMPa), while Moreno30 considers them to be satisfactory at strengths up to 17,000 psi (119 MPa). Burg and Ost19 report that a high strength capping material may be used with concrete strengths of up to 15,000 psi (105MPa); beyond that, the mode of failure of the cylinders changed from the normal cone failure of a columnar one. They recommend grinding of the cylinder ends for strengths beyond 15,000 psi (105MPa). Similarly, Aitcin33 has reported that above about 17,000psi (119MPa), the high strength capping material is pulverized as the specimens fail, which might well affect the measured strength. He too recommends grinding of the specimen ends for very high strength concretes. (It might be noted that end grinders for concrete cylinders are now commercially available. In 1992, the cost of such a machine was approximately US$12,000.) Because of the uncertainty with high strength capping compounds, and the costs and time involved in end grinding, a considerable amount of research has been carried out on unbonded capping systems. These consist of metal restraining caps into which elastomeric inserts are placed; the assemblies then fit over the ends of the cylinder. As the elastomeric inserts deteriorate with repeated use, they are replaced from time to time. Richardson35 used a system of neoprene inserts in aluminium caps for testing normal strength concretes in the range of 3000 psi to 6000 psi (21 MPa to 42 MPa). He found that below 4000 psi (28 MPa), the neoprene pads gave somewhat lower strengths than conventional sulfur caps, while above 4000 psi (28MPa) they gave somewhat higher strengths. Overall, however, the mean compressive strengths were not significantly different between the two systems.

Carrasquillo and Carrasquillo29 compared a high strength sulfur capping compound to an unbonded system consisting of a polyurethane pad in an aluminium restraining ring. They found that up to about 10,000 psi (7OMPa), the unbonded system gave strengths that were 97% of those obtained with the capping compound. Beyond 10,000 psi (7OMPa), however, the unbonded system gave much higher strengths; they hypothesized that this might be due to greater end restraint of the cylinders with such a system. In subsequent work,36 they found that up to 10,000 psi (7OMPa), polyurethane pads in an aluminium cap gave results within 5% of those achieved with high strength sulfur caps, while up to 11,000 psi (77MPa), neoprene pads in steel caps gave results within 3% of those obtained with the sulfur end caps. However, they concluded that the use of either unbonded system was questionable; substantial differences in test results were obtained when two sets of restraining caps (from the same manufacturer) were used. To improve the results obtained with unbonded systems, Boulay37 developed a system in which, instead of elastomeric inserts, a mixture of dry sand and wax is used. It was found38 that the sand mixture gave results which were intermediate between those obtained with ground ends or with sulfur mortar caps. In summary, then, below about 14,000psi (98MPa), a thin, high strength sulfur mortar cap may be used successfully. Beyond that strength level, it would appear that grinding specimen ends is currently the only way to ensure valid test results.

Testing machine characteristics

In general, for normal strength concrete, the characteristics of the testing machine itself are assumed to have little or no effect on the peak load. However, for very high strength concretes the machine may well have some effect on the response of the specimen to load. From a review of the literature, Hester31 concluded that the longitudinal stiffness of the testing machine will not affect the maximum load, and this view is shared also by Aitcin.33 However, if the machine is not stiff enough, the specimens may fail explosively, and, of course, a very stiff machine (with servo-controls) is required if one wishes to determine the post-peak response of the concrete. On the other hand, Hester31 also reports that if the machine is not stiff enough laterally, compressive strengths may be adversely affected. One must also be concerned about the capacity of the testing machine when testing very high strength concretes. Aitcin33 calculated the required machine capacities for different strength levels and specimen sizes, using the common assumption that the failure load should not exceed 2/3 of the machine capacity. Some of his results are reproduced in Table 1.12. Relatively few commercial laboratories are equipped to test high strength concrete, since a common capacity of commercial testing machine is 292,500 lbs (1.3 MN). To test a 6x12 in. (15Ox 300 mm) cylinder of

Table 1.12 Machine capacity required for high strength concrete33 Failure load Specimen size 100 x 200 mm 150 x 300 mm Machine capacity

fc' = 100 MPa 0.785 MN 1.76 MN

fc' = 150 MPa 1.18 MN 2.65 MN

fc' = 100 MPa 1.2MN 2.65 MN

fc' = 150 MPa 1.75 MN 4.0 MN

Note: I M N = 225,000 lbf

21,400psi (15OMPa) concrete requires a 900,000 Ib (4.0 MN) testing machine, and relatively few machines of this size are available in commercial laboratories. This then, is probably the driving force behind the move to the smaller 4 x 8 in. (100 x 200 mm) cylinders.

Effect of loading platens

Again, for ordinary concrete, the effects of the spherically seated bearing blocks (platens) are not explicitly considered, as long as they meet the requirements of ASTM C39: Compressive Strength of Cylindrical Concrete Specimens. However, recent work at the Construction Technology Laboratories in Skokie, Illinois39 has shown that, for high strength concrete, even this cannot be ignored. Spherical bearing blocks which deform in such a way that the stresses are higher around the periphery of the specimen than at the centre, yield higher compressive strengths than blocks which deform so that the highest stresses are at the centre of the specimen, and fall off towards the edges (i.e. a 'concave' rather than a 'convex' stress distribution). Measured differences can be as high as 15% for concretes with compressive strengths greater than 16,000 psi (112 MPa).

1.5

Conclusions

In conclusion, then, it has been shown that the production of high strength concrete requires careful attention to details. It also requires close cooperation between the owner, the engineer, the suppliers and producers of the raw materials, the contractor, and the testing laboratory.32 Perhaps most important, we must remember that the well-known 'laws' and 'rules-of-thumb' that apply to normal strength concrete may well not apply to high strength concrete, which is a distinctly different material. Nonetheless, we now know enough about high strength concrete to be able to produce it consistently, not only in the laboratory, but also in the field. It is to be hoped that codes of practice and testing standards catch up with the high strength concrete technology, so that the use of this exciting new material can continue to increase.

Acknowledgements
This work was supported by the Canadian Network of Centres of Excellence on High-Performance Concrete.

References
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