Fly Ash Handbook (FAH)

Transcription

1 Fly Ash Handbook (FAH) Supplementary file to accompany the FHWA/IN/ JTRP-2017/11 report Updating Physical and Chemical Characteristics of Fly Ash for Use in Concrete by P. Tanikella and J. Olek.

2 Fly Ash Handbook (FAH) Supplementary file to accompany the FHWA/IN/JTRP-2017/11 report Updating Physical and Chemical Characteristics of Fly Ash for Use in Concrete by P. Tanikella and J. Olek. This document contains supplementary information regarding the characteristics of twenty fly ashes used in the study. The list of the names of all fly ashes, along with the supplier and source information is provided in Table 1. This supplementary file contains the following sections: Section I Section II Section III Section IV Detailed Summary of the Characteristics of Fly Ashes Discussion Conclusions Fly Ash Data Sheets Table 1. Summary of names and supplier/source information for all fly ashes used in the study No. Fly ash Name Class Supplier Source 1 Baldwin C Headwaters Resources Baldwin Power Plant, IL 2 Edwards C Edwards, IL 3 Hennepin C Hennepin Power Station, IL 4 Schahfer C Schahfer Unit 15, IL 5 Vermilion C Vermilion, IL 6 Miller C Holcim Inc. Miller Plant, AL 7 Joliet C Lafarge North America Joliet, IL 8 Kenosha C Kenosha, WI 9 Rockport C Rockport, IL 10 Will County C Will County, IL 11 Joppa C Mineral Resource Joppa, IL 12 Labadie C Technologies Labadie Power Plant, MO 13 Mill Creek F Mill Creek, WA 14 Petersburg F Petersburg, IN 15 Rush C Rush Island Power Plant, Festus, MO Island 16 Trimble F Trimble County Power Station, Bedford, KY 17 Elmersmith F Fly Ash Direct Elmer Smith Station, Owensboro, KY 18 Miami7 F Miami Fort Unit #7, North Bend, OH 19 Miami8 F Miami Fort Unit #8, North Bend, OH 20 Zimmer F Zimmer Power Station, Moscow, OH 2

3 SECTION I DETAILED SUMMARY OF THE CHARACTERISTICS OF FLY ASHES I.1.1 Chemical Analysis I.1 Baldwin Headwaters Resources, Baldwin Power Plant, Baldwin, IL I Results of Total Chemical Analysis The results of the total chemical analysis results from experiments for the Baldwin fly ash are shown in Table I.. The results of the analyses were used to calculate the Derived Parameters values shown in Table I.2. Other pertinent information for this fly ash is shown in Table I.3 under the heading Results of Analyses. Table I.1 Total Chemical Analysis - Baldwin Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.25 Na2O, % 1.93 K2O, % 0.47 SO3, % 1.55 MgO, % 5.90 Total Table I.2 Derived Parameters - Baldwin Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

4 Table I.3 Results of Analyses - Baldwin Fly Ash Loss on ignition, % 0.49 Total SO3, % 1.55 Soluble SO3, % 0.28 Percentage of the total SO3 that is soluble 18% Soluble Na2O, % 0.05 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 2.24 Soluble alkalies, as equivalent Na2O, % 0.06 Percentage of the alkalies that are soluble 2.7% I Chemical Analysis Interpretations This fly ash is classified as a Class C fly ash according to its composition, with a total SiO 2+Al 2O 3+Fe 2O 3 content of 60% (<70%, in ASTM C 618 specification ). The CaO content is 25%. The MgO content (5.90%) is rather high as compared to other Class C fly ash presented in this report. The contents of other elements are not unusual and the loss on ignition result is similar to the results obtained for other Class C fly ashes tested here. The alkali content is about 2%, nearly all of it is insoluble, and is likely contained in the glass. I.1.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics determined for Baldwin fly ash. The particle size distribution of this fly ash is presented in Figure I.1; a comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.2. Parameters related to particle size for this fly ash are shown in Table I Baldwin 80 % smaller Diameter (µm) Figure I.1 Particle Size Distribution - Baldwin Fly Ash 4

5 25 20 Miller Baldwin % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.2 Relative Particle Size Distribution - Baldwin Fly Ash Table I.4 Particle Size Parameters - Baldwin Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 6102 I Particle Size Distribution Interpretation This is a fairly ordinary particle size distribution, similar to the typical (Miller) fly ash used as the reference on the bar chart, especially for the particles smaller than 5 μm. The mean particle size of 22 μm is also close to that of Miller fly ash (~25 μm). It is observed that there are a bit more particles falling in the range of 5 to 26 μm and a bit less in the range of 26 to 100 μm, while the percentage of particles >45 μm (about 16%) is smaller (~19% of Miller fly ash). As a result, this fly ash appears a little finer than the typical fly ash. I.1.3 Measurements of Physicochemical Parameters This section contains the test results of content for magnetic particles and X-ray diffraction (XRD) analysis for the Baldwin fly ash. The X-ray diffraction pattern obtained for this fly ash is presented in Figure I.3. The crystalline components detected include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These components are normally found in Class C fly ashes. A hump, 5

6 representing a calcium-aluminate type of glass with a maximum near 2θ=~32 is visible. No magnetic particles were found in this fly ash Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.3 X-Ray Diffraction Results - Baldwin Fly Ash I.1.4 Scanning Electron Micrographs The four micrographs chosen as representative of the larger set obtained for this fly ash are described below. Figure I.4(a) shows a micrograph of the Baldwin fly ash taken at a magnification of 600, and showing the great disparity in sizes of the individual particles in this fly ash. There are two large spheres shown here, about 40 µm in size, each one shows a smooth surface and the other appears to be rather rough. Both spheres have very small particles deposit on their surfaces. Hundreds of smaller fly ash particles are also present in the area depicted in the micrograph. Many appear to be 1 µm or smaller in diameter. A different field of the Baldwin fly ash taken at a slightly lower magnification (400 ) is shown in Figure I.4(b). A large irregular grain (almost 200 µm in size) is present in the center of this micrograph. Similar large irregular grains were found in most of the micrographs taken for this fly ash. Figure I.4(c) shows one of an incompletely spherical plenosphere about 40µm in size. Most of the smaller particles inside the plenosphere are clean spheres with smooth surfaces. 6

7 An unusually thin and long carbon residue grain (confirmed by EDX examination) is shown in Figure I.4(d). This carbon particle is longer than 200 µm, but its width is less than 20 µm. I.1.5 Strength Activity Index Laboratory trials carried out for mortar made with this fly ash following the standard ASTM 311 procedure, gave a strength being 84% of that of the control mortar at the age of 7 days. The strength was 127% of the control mortar at the age of 28 days, following the standard test method specified in ASTM C 311. The strength activity index of this fly ash at 7 days is the lowest among all the other Class C fly ashes. However, the index increases to 127% at 28 days, indicating noticeable reactivity with cement at later ages. The water requirement of this fly ash is 93%, which is the lowest among those of all the fly ashes tested in this study. I.1.6 Summary This fly ash is a high-calcium fly ash of typical chemical composition, except for a little higher content of magnesium. It has the usual reactive components characteristic of Class C fly ashes most of which are reactive and it has the calcium aluminate type glass structure. Occasionally extremely large grains (around 200 µm in size) are common in this fly ash, and quite a few oversized carbon particles are also present. They are probably responsible for the large mean particle size found in particle size distribution experiment. The strength of fly ash bearing mortar is relatively low. But, the substantial potential reactivity is evident by 28 days. 7

8 (a) 600 (b) 400 8

9 (c) 2000 (d) 300 Figure I.4 SEM Micrographs of Baldwin Fly Ash as Magnification of 600, (b) 400, (c) 2000, (d) 300 (a) 9

10 I.2 Edwards Headwaters Resources, Edwards Power Station, Bartonville, IL I.2.1 Chemical Analysis I Results of Total Chemical Analysis The results of these analyses for the Edwards fly ash are shown in Table I.5. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.6. Other pertinent information for this fly ash is shown in Table I.7 under the heading Results of Analyses. Table I.5 Total Chemical Analysis - Edwards Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % Na2O, % 1.38 K2O, % 0.38 SO3, % 2.73 MgO, % 4.92 Total Table I.6 Derived Parameters - Edwards Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

11 Table I.7 Results of Analyses - Edwards Fly Ash Loss on ignition, % 0.43 Total SO3, % 2.73 Soluble SO3, % 0.75 Percentage of the total SO3 that is soluble 27% Soluble Na2O, % 0.09 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 1.63 Soluble alkalies, as equivalent Na2O, % 0.10 Total alkalies, as equivalent Na2O, % 6.1% I Chemical Analysis Interpretations Based on these results, this fly ash would be properly classified as Class C in the ASTM C 618 specifications (SiO 2+Al 2O 3+Fe 2O 3 =62.47% < 70%). The CaO content is about 24%, much higher than the Baldwin ash, average of Class C fly ashes. At 10%, the iron oxide content of this fly ash is much higher than that of other Class C fly ashes used in this study. The SO 3 content (2.73%) is a little high, however less than 30% of it is soluble. At 1.63%, the alkali content of this fly ash is lower than any of the other Class C fly ashes tested here. However, a relatively high (~6%) of these alkalies are soluble. I.2.2 Physical Characteristics I Results from Experiments This section presents the results of the physical characteristics evaluations of the Edwards fly ash. Particle size distribution of this fly ash is presented in Figure I.5, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.6. Parameters related to particle size for this fly ash are shown in Table I Edwards 80 % smaller Diameter (µm) Figure I.5 Particle Size Distribution - Edwards Fly Ash 11

12 30 25 Miller Edwards 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.6 Relative Particle Size Distribution - Edwards Fly Ash Table I.8 Particle Size Parameters - Edwards Fly Ash % > No.325 sieve (Supplier Certificate), % 8.90 % > 45 µm (LPSD), % 9.22 Mean particle size (LPSD), µm Specific Area (LPSD), cm 2 /g Blaine fineness, cm 2 /g 7306 I Particle Size Distribution Interpretation This fly ash is finer than the typical (Miller) fly ash. The mean particle size of 15 μm is smaller than that of the Miller fly ash (~25 μm) and the percentage of particles >45 μm (9%) is far smaller (~19% of the Miller fly ash). Furthermore, as indicated in Figure I.6, the cumulative percentage of particles smaller than 13 μm is roughly 15% higher than that of the typical (Miller) fly ash. It is clear that particle size distribution of the Edwards fly ash is skewed toward the finer size. 12

13 I.2.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Edwards fly ash. X-ray diffraction analysis results for this fly ash are given in Figure I.7. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), merwinite (Ca 3Mg(SiO 4) 2) and magnetite (Fe 3O 4). A hump, the latter component presumably is responsible for the magnetic particle content, otherwise the crystalline components are typical for class C fly ashes, representing a calcium-aluminate type of glass with a maxiumum at 2θ=~32 is also visible. The measured weight content of magnetic particles in this fly ash was 3.4% Counts (6) (6) : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO 6: Magnetite Fe3O4 Figure I.7 X-Ray Diffraction Results - Edwards Fly Ash I.2.4 Scanning Electron Micrographs A set of four of the micrographs for this fly ash chosen as representative of the morphology of the particles were obtained. These micrographs are presented in Figure I.8. Figure I.8(a) shows an area containing typical spherical fly ash particles taken at a magnification of 500. These particles range in sizes from less than 1µm to more than 10µm. A few irregular 13

14 particles also can be seen. Most of the particles are smooth. The fuzzy looking particle located just alone in the middle of the micrograph is actually a cluster of extremely fine particles. Figure I.8(b) shows an area similar to the previous one, taken at a higher magnification. Most particles are smooth but fine deposits can be observed on a few of the large particles. There are also some irregular, non-spherical grains present in this area. Corresponding to the appreciable content of iron oxide found in XRD result, a few detectable iron oxide grains were found in this fly ash. One of them is seen in Figure I.8(c) appearing as the thin plate in the upper right corner. Such particles are not commonly seen in Class C fly ashes. An unusually large solid carbon residue grain is shown in Figure I.8(d). It is almost 200µm long and is much larger than other particles present in this fly ash. I.2.5 Strength Activity Index The 7 day strength is 89% of that of the control mortar. However, the 28 day strength of the Edwards fly ash mortar was 133% of that of the control mortar indicating that substantial delayed reactivity must have taken place. The water requirement of this fly ash is 93%, which is the lowest among those of all the fly ashes tested in this study. I.2.6 Summary This fly ash is a Class C fly ash with an appreciable content of iron oxide, an unusual feature of Class C fly ashes. As a result, a certain amount of magnetite could be detected from XRD analysis, which is also not common for a Class C fly ash. This fly ash is relatively fine compared to the typical (Miller) fly ash. Fairly large carbon particles are also found in this fly ash, but there are no other extremely large irregular grains. The addition of this fly ash also reduces the strength of mortar at the age of 7 days but it substantially increases at 28 days. 14

15 (a) 500 (b)

16 (c) 1000 (d) 360 Figure I.8 SEM Micrographs of Edwards Fly Ash as Magnification of 500, (b) 800, (c) 1000, (d) 360 (a) 16

17 I.3.1 Chemical Analysis I.3 Hennepin Headwaters Resources, Hennepin Power Station, Hennepin, IL I Results of Total Chemical Analysis The results of total chemical analysis results for the Hennepin fly ash are shown in Table I.9. The results of these analyses were used to calculate the Derived Parameters values shown in Table I.10. Other pertinent information for this fly ash is shown in Table I.11 under the heading Results of Analyses. Table I.9 Total Chemical Analysis - Hennepin Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 5.91 Na2O, % 1.57 K2O, % 0.64 SO3, % 1.43 MgO, % 4.93 Total Table I.10 Derived Parameters - Hennepin Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

18 Table I.11 Results of Analyses - Hennepin Fly Ash Loss on ignition, % 0.61 Total SO3, % 1.43 Soluble SO3, % 0.35 Percentage of the total SO3 that is soluble 24% Soluble Na2O, % 0.08 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 1.99 Soluble alkalies, as equivalent Na2O, % 0.09 Total alkalies, as equivalent Na2O, % 4.5% I Chemical Analysis Interpretations Based on the fact that the total SiO 2+Al 2O 3+Fe 2O 3 content is 66% (<70%, in the ASTM C 618 specification), this fly ash would be proper to be classified as Class C. The CaO content is 22%, slightly lower than average for a Class C fly ash. The loss on ignition (0.61%) is still low. I.3.2 Physical Characteristics I Experimental Results This section contains the results of the physical characteristics determined for the Hennepin fly ash. Particle size distribution of this fly ash is presented in Figure I.9, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.10. Parameters related to particle size for this fly ash are shown in Table I Hennepin 80 % smaller Diameter (µm) Figure I.9 Particle Size Distribution - Hennepin Fly Ash 18

19 25 20 Miller Hennepin % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.10 Relative Particle Size Distribution - Hennepin Fly Ash Table I.12 Particle Size Parameters - Hennepin Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 5125 I Particle Size Distribution Interpretation This is also a finer fly ash when compared to the typical (Miller) fly ash. As shown in Figure I.10, the main differences between the two fly ashes lie in the particle range of 1 to13 μm (~13%) and 26 to 100 μm (~10%). The mean particle size of this fly ash is about 17 μm and the percentage of particles >45 μm is about 12%. Both of the values appear smaller than those of the typical fly ash, which are respectively about 25 μm and 19%. I.3.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Hennepin fly ash. 19

20 The measured weight content of magnetic particles of this fly ash was 0.07%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.11. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). There are normal crystalline components found in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.11 X-Ray Diffraction Results - Hennepin Fly Ash I.3.4 Scanning Electron Micrographs Of the micrographs taken for this particular fly ash, a set of four are chosen as representative of the morphology of the particles and are presented. They are described below. Two irregular grains decorated with rough deposits and a lot of much finer spherical particles are shown in Figure I.12(a), which is taken at a rather low magnification of 300. Other than the two grains that are nearly 100 µm in size, the rest of particles are smaller than 20 µm, or some may even be smaller than 1 µm. In addition, they are mostly smooth and clean. As shown in Figure I.12(b), shows a typical area taken at a much higher magnification of Here one can clearly see a few fine particles smaller than 1 µm. Again, most of the particles appear smooth and clean, including the larger irregular piece on the left upper part of the micrograph. 20

21 The appearance of irregular large complex grains is shown in Figure I.12(c). This grain is extremely large with a length over 200 µm. Quite a few similar grains were found in this particular fly ash. A layered grain is present in Figure I.12(d). There is a clear hemisphere shape hole left in this fragment, which appears relatively clean except for some very fine particles deposits. I.3.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a strength of 88% that of the control mortar at the age of 7 days, and 137% at the age of 28 days, following the standard test method in ASTM C 311. The water requirement of this fly ash is 93%, which is the lowest among those of all the fly ashes tested in this study. I.3.6 Summary This Class C fly ash has common chemical composition as well as the usual reactive crystalline components characteristic of Class C fly ashes. The ignition is a little higher as compared to other Class C fly ashes in this study yet still low. This fly ash is finer than the typical (Miller) fly ash and the presence of those fine particles has been confirmed by SEM examination. However, quite a few of complex grains with size over 200 µm are also found, which could have compromised the fineness of this fly ash. The strength of mortar containing this fly ash shows lower than that of the control mortar at the age of 7 days; however, it becomes much higher at the age of 28 days, showing the rather high potential reactivity of this fly ash during the period. 21

22 (a) 300 (b)

23 (c) 300 (d) 1000 Figure I.12 SEM Micrographs of Hennepin Fly Ash as Magnification of 300, (b) 1000, (c) 300, (d)1000 (a) 23

24 I.4 Schahfer Headwaters Resources, Schahfer Power Station Unit 15, Wheatfield, IN I.4.1 Chemical Analysis I Results of Total Chemical Analysis The results of total chemical analysis for the Schahfer fly ash are shown in Table I.13. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.14. Other pertinent information for this fly ash is shown in Table I.15 under the heading Results of Analyses. Table I.13 Total Chemical Analysis - Schahfer Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.76 Na2O, % 1.35 K2O, % 0.73 SO3, % 1.42 MgO, % 4.29 Total Table I.14 Derived Parameters - Schahfer Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

25 Table I.15 Results of Analyses - Schahfer Fly Ash Loss on ignition, % 0.44 Total SO3, % 1.42 Soluble SO3, % 0.48 Percentage of the total SO3 that is soluble 34% Soluble Na2O, % 0.03 Soluble K2O, % Total alkalies, as equivalent Na2O, % 1.83 Soluble alkalies, as equivalent Na2O, % 0.03 Total alkalies, as equivalent Na2O, % 1.6% I Chemical Analysis Interpretations According to ASTM C 618 specification, this fly ash would be classified as Class C, although the total SiO 2+Al 2O 3+Fe 2O 3 content is 68% (<70%) approaching the required minimum content for Class F in the specification. The CaO content is 21% which is lower than typical Class C fly ashes. The other elements content are typical as for a Class C fly ash and the loss on ignition (0.44%) is also common among the Class C fly ashes in this study. I.4.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Schahfer fly ash. Particle size distribution of this fly ash is presented in Figure I.13, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.14. Parameters related to particle size for this fly ash are shown in Table I Schahfer 80 % smaller Diameter (µm) Figure I.13 Particle Size Distribution - Schahfer Fly Ash 25

26 25 20 Miller Schahfer % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.14 Relative Particle Size Distribution - Schahfer Fly Ash Table I.16 Particle Size Parameters - Schahfer Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 6428 I Particle Size Distribution Interpretation This particle size distribution is different from fly ashes described before. It is shown in Figure I.14 that there are fewer particles smaller than 1 μm than that of the typical (Miller) fly ash. However, there are still more particles falling in the range of 1 to 26 μm. As a result, a mean particle size of 19 μm and 10% of >45 μm particles of the Schahfer fly ash indicate that it is finer than the typical fly ash. 26

27 I.4.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Schahfer fly ash. The measured weight content of magnetic particles of this fly ash was 2.7% but no XRD peaks for these oxides were found. X-Ray Diffraction analysis results for this fly ash are given in Figure I.15. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.15 X-Ray Diffraction Results - Schahfer Fly Ash I.4.4 Scanning Electron Micrographs A set of four micrographs chosen as representative of those obtained for this fly ash are described below. 27

28 A fairly special kind of Si-Al bearing thin plate particle, found to be rich in Si and Al by EDX is shown in Figure I.16(a), with appearance of thin plates. It was only found in this particular fly ash by far. There is another large and almost spherical particle, with a diameter close to 40 µm. It is seen that there are many rather fine particles, mostly spherical and smooth. The micrograph shown in Figure I.16(b) is similar to the previous one, except that there is an extremely large grain present. Similar to the Hennepin fly ash described before, An appreciable content of these complex grains with a size about 200 µm were found in this fly ash as was found in the Hennepin fly ash. This particle is most likely an unburned carbon residue. Another large grain is shown in Figure I.16(c) at the same magnification. The difference from the previous grain is that it is much smaller and appears as different structure. While the previous grain seems to be solid from the micrograph, this grain shows a less compact structure with pockets containing tiny fly ash particles. The micrograph present in Figure I.16(d), taken at a much higher magnification of 2000, shows a remnant of unburned carbon, which is very different from those carbon residue found in previous fly ashes. It is part of a structure called Swiss cheese, though not so representative, with a lot of tiny fly ash particles embedded and apparent holes in which those spherical particles were formed. I.4.5 Strength Activity Index The strength activity index tested for this particular fly ash is 84% at the age of 7 days and 119% at the age of 28 days of the control mortar, as results from the specific test method in ASTM C 311. As compared to all the other Class C fly ashes tested in this study, the strength activity index of 7 days age of this fly ash appears to be the lowest, while that of 28 days is close to the lowest. This fact indicates that this Class C fly ash highly reduces the strength of mortar at early age and has a certain potential reactivity at later age, yet not very high. The water requirement of this fly ash is 93%, which is the lowest among those of all the fly ashes tested here. I.4.6 Summary This is a common Class C fly ash with usual reactive crystalline components and typical calcium aluminate type glass structure, though the combination content of SiO 2, Al 2O 3 and Fe 2O 3 is close to the limit indicated in ASTM C 618 specification. This fly ash is also finer than the typical (Miller) fly ash. There are a few of oversize grains (>200 µm) found in this fly ash when examined by SEM. In addition, some carbon residue grains shaped as Swiss Cheese are present. The addition of this fly ash has a major negative effect on the early strength of the mortar. The limited enhancement of the strength at the age of 28 days indicates a not very high reactivity of this fly ash during the period. 28

29 29

30 (a) 800 (b)

31 (c) 600 (d) 2000 Figure I.16 SEM Micrographs of Schahfer Fly Ash as Magnification of 800, (b) 600, (c) 600, (d) 2000 (a) 31

32 I.5.1 Chemical Analysis I.5 Vermilion Headwaters Resources, Vermilion Station, Oakwood, IL I Results of Total Chemical Analysis The results of the total chemical analysis for Vermilion fly ash are shown in Table I.17. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.18. Other pertinent information for this fly ash is shown in Table I.19 under the heading Results of Analyses. Table I.17 Total Chemical Analysis - Vermilion Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.19 Na2O, % 1.50 K2O, % 0.62 SO3, % 1.40 MgO, % 4.55 Total Table I.18 Derived Parameters - Vermilion Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 1.91 Table I.19 Results of Analyses - Vermilion Fly Ash Loss on ignition, % 0.43 Total SO3, % 1.40 Soluble SO3, % 0.22 Percentage of the total SO3 that is soluble 16% Soluble Na2O, % 0.06 Soluble K2O, % Total alkalies, as equivalent Na2O, % 1.91 Soluble alkalies, as equivalent Na2O, % 0.07 Total alkalies, as equivalent Na2O, % 3.7% 32

33 I Chemical Analysis Interpretations This is another typical Class C fly ash in terms of its chemical analysis, since the total SiO 2+Al 2O 3+Fe 2O 3 content of 64% meets the applicable requirement for the Class C fly ash given in ASTM C 618 specification. The CaO content is 24%, average of a Class C fly ash. The content of other elements are moderate and so is the loss on ignition. I.5.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Vermilion fly ash. Particle size distribution of this fly ash is presented in Figure I.17, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.18. Parameters related to particle size for this fly ash are shown in Table I Vermilion 80 % smaller Diameter (µm) Figure I.17 Particle Size Distribution - Vermilion Fly Ash 33

34 30 25 Miller Vermilion 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.18 Relative Particle Size Distribution - Vermilion Fly Ash Table I.20 Particle Size Parameters - Vermilion Fly Ash % > No.325 sieve (Supplier Certificate), % 6.40 % > 45 µm (LPSD), % 7.64 Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 5536 I Particle Size Distribution Interpretation As shown in Figure I.18, the cumulative percentage of particles smaller than 13 μm of this fly ash is about 17% higher than that of the typical (Miller) fly ash. At the same time, a difference of 15% could be estimated for the percentage of particles larger than 26 μm. The mean particle size of 14 μm is noticeable smaller than the Miller fly ash (~25 μm). In addition, particles larger than 45 μm in this fly ash are far more less than in the Miller fly ash (~19%). I.5.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Vermilion fly ash. The measured weight content of magnetic particles of this fly ash was 0.26%. 34

35 X-Ray Diffraction analysis results for this fly ash are given in Figure I.19. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.19 X-Ray Diffraction Results - Vermilion Fly Ash I.5.4 Scanning Electron Micrographs Of the micrographs obtained for this fly ash, four micrographs were chosen as being representative and they are described below. A representative collection of medium size to finer fly ash particles is shown in Figure I.20(a), taken at a magnification of 600. It is found that particles present in this fly ash appears are much finer than that in previous fly ashes, and most of them are spherical and smooth. 35

36 The area shown in Figure I.20(b) is similar to the previous one, except that it was taken at a higher magnification and some particles with rough-textured surface could be seen. Meanwhile, a few of irregular grains are also found here, but still in a small size, the same as those spherical particles. Figure I.20(c) shows some unusually large and rare bulks, which all appear being made of half of fuzzy surface and half of relatively smooth surface. However, they are not very common in this fly ash. Therefore, this is not the typical feature. Similarly, several extremely large irregular grains were found in this fly ash, as one of them shown in Figure I.20(d). Nevertheless, they are much less compared to previous fly ashes, such as the Hennepin and Schahfer fly ash. I.5.5 Strength Activity Index Trials carried out with this fly ash gave a strength being 85% of the control mortar at the age of 7 days, while being 137% at the age of 28 days, following the standard test method in ASTM C 311. The big difference between the two strength activity indices indicates the substantial potential reactivity of this fly ash with cement at later age. In addition, the water requirement of this fly ash is 93%, which is the lowest among all the fly ashes tested. I.5.6 Summary This is a rather fine Class C fly ash with typical chemical composition and usual reactive crystalline components and calcium aluminate type glass structure. Most particles detected in this fly ash are spherical and smooth, yet with a very small number of large and irregular grains. The results of strength activity index at 7 days and 28 days show a substantial potential reactivity of this fly ash with cement during the period. 36

37 (a) 600 (b)

38 (c) 500 (d) 600 Figure I.20 SEM Micrographs of Vermilion Fly Ash as Magnification of 600, (b) 800, (c) 500, (d) 600 (a) 38

39 I.6.1 Chemical Analysis I.6 Miller Holcim, Inc., Miller Plant of Alabama Power, West Jefferson, AL I Results of Total Chemical Analysis The results of the total chemical analysis for the Miller fly ash are shown in Table I.21. The results of these analyses were used to calculate the Derived Parameters values shown in Table I.22. Other pertinent information for this fly ash is shown in Table I.23 under the heading Results of Analyses. Table I.21 Total Chemical Analysis - Miller Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.03 Na2O, % 1.73 K2O, % 0.53 SO3, % 1.97 MgO, % 5.64 Total Table I.22 Derived Parameters - Miller Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.08 Table I.23 Results of Analyses - Miller Fly Ash Loss on ignition, % 0.44 Total SO3, % 1.97 Soluble SO3, % 0.52 Percentage of the total SO3 that is soluble 26% Soluble Na2O, % 0.08 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 2.08 Soluble alkalies, as equivalent Na2O, % 0.09 Total alkalies, as equivalent Na2O, % 4.3% 39

40 I Chemical Analysis Interpretations Based on the chemical composition and applicable requirements in ASTM C 618 specification, this fly ash is fairly a typical Class C fly ash in most respects. The total SiO 2+Al 2O 3+Fe 2O 3 content is about 60% (<70%) and contents of other elements are mostly typical, expect that the MgO content (5.64%) is a little high. Loss on ignition is as low as most Class C fly ashes tested here. The alkali content (2.08%) is moderate, and mostly insoluble. I.6.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Miller fly ash. Cumulative curve of particle size distribution of this fly ash is presented in Figure I.21, while the particle frequency distribution is given in Figure I.22. Parameters related to particle size for this fly ash are shown in Table I Miller 80 % smaller Diameter (µm) Figure I.21 Particle Size Distribution - Miller Fly Ash 40

41 25 Miller 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.22 Relative Particle Size Distribution - Miller Fly Ash Table I.24 Particle Size Parameters - Miller Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 4851 I Particle Size Distribution Interpretation This fly ash has been selected as the typical fly ash for using to examine the relative particle size distribution of all the other fly ashes. The fineness reported from supplier certificate is 19.80% retained when wet-sieved on 45 μm sieve, which is very close to the percentage of >45 μm particles (19.0%) as shown in Figure I.22. The mean particle size of 25 μm is about the average of all the fly ashes tested in this study and the distribution pattern is typical. The bar chart plot shows a reasonable particle size distribution in the different size range groupings used. 41

42 I.6.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Miller fly ash. No magnetic particles were found in this fly ash. X-Ray Diffraction analysis results for this fly ash are given in Figure I.23. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4) and merwinite (Ca 3Mg(SiO 4) 2). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.23 X-Ray Diffraction Results - Miller Fly Ash 42

43 I.6.4 Scanning Electron Micrographs The four micrographs discussed below were chosen as representative of those obtained of this fly ash. The micrograph presented in Figure I.24(a), targeted on a typical area, shows the different kinds of particles in this fly ash. Relatively large particle with rough surface and fine deposits is found in this area, while lots of finer spheres are present and mostly smooth. The rough particle was examined and found to have a high content of magnesium. This is another typical area, showing several irregular grains with mostly smooth and relatively clean surface, as presented in Figure I.24(b). The sharp-cornered grain on the right of this area is a fragment of unburned carbon residue. There seems very small amount of carbon residue found in this fly ash. This micrograph in Figure I.24(c) taken at a higher magnification shows most of the medium size to fine fly ash particles. It is observed that some clusters of fine particles. Again, most of them are smooth and relatively clean. The final micrograph as in Figure I.24(d), taken at a low magnification of 300, shows one of the very large grains representative of oversize material, in this case a complex rugged-surface grain with lots of tiny fly ash particles deposits. I.6.5 Strength Activity Index The strength activity index tested for this particular fly ash is 90% at the age of 7 days and 123% at the age of 28 days, as results from the specific test method in ASTM C 311. Again, the difference between the two strength activity indices shows the certain potential reactivity of this fly ash with cement at later age. In addition, the water requirement of this fly ash is 95%. I.6.6 Summary This is fairly a typical Class C fly ash in most respects, except a little high content of Magnesium. As a result, the rough content of merwinite and periclase showing in the XRD analysis seems a bit higher. Other than that, the reactive crystalline components and calcium aluminate type glass structure of this fly ash detected using XRD appears normal. This fly ash has been chosen as the typical fly ash used in comparison for other fly ashes due to its reasonable particle size distribution in the different size range groupings used in this report. The addition of this fly ash reduces the strength of mortar as 10% at 7 days and enhances it as 23% at 28 days, showing an average potential reactivity of this fly ash among all the Class C fly ashes tested in this study. 43

44 (a) 500 (b)

45 (c) 880 (d) 300 Figure I.24 SEM Micrographs of Miller Fly Ash as Magnification of 500, (b) 580, (c) 880, (d) 300 (a) 45

46 I.7.1 Chemical Analysis I.7 Joliet Lafarge North America, Joliet Station, Joliet, IL I Results of Total Chemical Analysis The results of the total chemical analysis for the Joliet fly ash are shown in Table I.25. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.26. Other pertinent information for this fly ash is shown in Table I.27 under the heading Other Analysis. Table I.25 Total Chemical Analysis - Joliet Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.41 Na2O, % 3.70 K2O, % 0.34 SO3, % 2.45 MgO, % 5.83 Total Table I.26 Derived Parameters - Joliet Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 3.92 Table I.27 Other Analysis - Joliet Fly Ash Loss on ignition, % 0.49 Total SO3, % 2.45 Soluble SO3, % 1.28 Percentage of the total SO3 that is soluble 52% Soluble Na2O, % 0.31 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 3.92 Soluble alkalies, as equivalent Na2O, % 0.32 Total alkalies, as equivalent Na2O, % 8.2% 46

47 I Chemical Analysis Interpretations This fly ash is classified as a Class C fly ash with a total SiO 2+Al 2O 3+Fe 2O 3 content of 56% (<70%, in ASTM C 618 specification). The CaO content was 27%, slightly larger than most Class C fly ashes in this study. The MgO content (5.83%) is fairly high. So is the SO 3 content (2.45%), essentially half of it soluble. The alkali content (3.92%) is fairly high, almost twice as much as most Class C fly ashes tested here and about 8% of it soluble. I.7.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Joliet fly ash. Particle size distribution of this fly ash is presented in Figure I.25, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.26. Parameters related to particle size for this fly ash are shown in Table I Joliet 80 % smaller Diameter (µm) Figure I.25 Particle Size Distribution - Joliet Fly Ash 47

48 30 25 Miller Joliet 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.26 Relative Particle Size Distribution - Joliet Fly Ash Table I.28 Particle Size Parameters - Joliet Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % 7.79 Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 5356 I Particle Size Distribution Interpretation This particle size distribution shows substantial differences from the typical Miller fly ash in the range of 5 to 13 μm (~10% higher) and >45 μm (~12% lower). These facts make this fly ash a finer one when compared to the Miller fly ash, though percentages of particles in other ranges appear close for both. The mean particle size of 14 μm of this fly ash is fairly smaller than that of the Miller fly ash (~25 μm). I.7.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Joliet fly ash. The measured weight content of magnetic particles of this fly ash was 0%. 48

49 X-Ray Diffraction analysis results for this fly ash are given in Figure I.27. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These are the typical components present in a Class C fly ash. A hump, representing a calcium-aluminate type of glass with a maxiumum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.27 X-Ray Diffraction Results - Joliet Fly Ash I.7.4 Scanning Electron Micrographs Four micrographs chosen as representative of the larger set obtained in this work are described below. There is a representative area observed in this fly ash shown in Figure I.28(a) taken at a relatively high magnification of One thing should be notified is that fully separate particles are hardly found in this depicted area. There are always several particles stuck together, either large or tiny. Most of the particles shown have smooth surface. In Figure I.28(b), there is a similar area taken at the same magnification as the previous micrograph. Finer spherical particles appear, and the largest particle is smaller than 15 μm in diameter. In addition, a hollow particle with quite a few tiny fly ash particles inside is present in the right upper area. 49

50 This micrograph shown in Figure I.28(c) taken at a much higher magnification shows a close examination of the hollow particle shown previously. The shell of the hollow particle was found to have a high content of sodium. Here we could find both smooth spheres and rugged-surface particles with small particles deposited on. An extremely large carbon grain was found in this fly ash sample as shown in Figure I.28(d), taken at a higher magnification of It appears porous structure and entraps many small fly ash spheres. I.7.5 Strength Activity Index The strength activity index tested for this particular fly ash is 89% at the age of 7 days and 117% at the age of 28 days, as results from the specific test method in ASTM C 311. As compared to all the other Class C fly ashes tested in this study, the strength activity index of 7 days age of this fly ash appears to be average, while that of 28 days is the lowest. This fact indicates the limited potential reactivity of this Class C fly ash in this period. In addition, the water requirement of this fly ash is 94%. I.7.6 Summary This is a Class C fly ash with rather high content of Magnesium and fairly high content of alkalies. As a result, a relatively high content of merwinite and periclase roughly shows in the results of XRD analysis while the content of alkalies in particles of this fly ash could be examined by EDX in SEM. This fly ash is finer than the typical (Miller) fly ash. The strength activity index of this fly ash at the age of 28 days is the lowest among those of all the Class C fly ashes tested in this study. It indicates a limited potential reactivity of this fly ash with cement. 50

51 (a) 1000 (b)

52 (c) 3000 (d) 1200 Figure I.28 SEM Micrographs of Joliet Fly Ash as Magnification of 1000, (b) 1000, (c) 3000, (d) 1200 (a) 52

53 I.8 Kenosha Lafarge North America, Pleasant Prairie Power Station, Kenosha, WL I.8.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Kenosha fly ash are shown in Table I.29. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.30. Other pertinent information for this fly ash is shown in Table I.31 under the heading Results of Analyses. Table I.29 Total Chemical Analysis - Kenosha Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 5.87 Na2O, % 1.80 K2O, % 0.58 SO3, % 1.11 MgO, % 5.52 Total Table I.30 Derived Parameters Kenosha Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.18 Table I.31 Results of Analyses - Kenosha Fly Ash Loss on ignition, % 0.38 Total SO3, % 1.11 Soluble SO3, % 0.53 Percentage of the total SO3 that is soluble 48% Soluble Na2O, % 0.03 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 2.18 Soluble alkalies, as equivalent Na2O, % 0.04 Total alkalies, as equivalent Na2O, % 1.8% 53

54 I Chemical Analysis Interpretations Based on the total SiO 2+Al 2O 3+Fe 2O 3 content of 64% (<70%, in ASTM C 618 specification), this fly ash is also classified as Class C. The CaO content was found to be 23%, typical of a Class C fly ash. The SO 3 content is lower than the contents of most other Class C fly ashes tested here, with half of it soluble. Other elements content of this fly ash is normal and again, loss on ignition is also low. The alkali content (about 2%) is moderate with mostly insoluble. I.8.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Kenosha fly ash. Particle size distribution of this fly ash is presented in Figure I.29, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.30. Parameters related to particle size for this fly ash are shown in Table I Kenosha 80 % smaller Diameter (µm) Figure I.29 Particle Size Distribution - Kenosha Fly Ash 54

55 30 25 Miller Kenosha 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.30 Relative Particle Size Distribution - Kenosha Fly Ash Table I.32 Particle Size Parameters - Kenosha Fly Ash % > No.325 sieve (Supplier Certificate), % -- % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 4452 I Particle Size Distribution Interpretation There are some differences lying in the range of 1 to 5 μm (~5%) and >45 μm (~8%) when comparing this fly ash to the typical Miller fly ash. It is shown in Figure I.30 that particles smaller than 26 μm in this fly ash are a bit more than in the Miller fly ash, while particles larger than 26 μm show a bit less. In other words, the distribution curve of this fly ash is skewed a little to the finer part as compared to that of the typical fly ash. The mean particle size of 17 μm is smaller. Therefore, this fly ash is also finer than the Miller fly ash. I.8.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Kenosha fly ash. No magnetic particles were found in this fly ash. 55

56 X-Ray Diffraction analysis results for this fly ash are given in Figure I.23. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These are the common crystalline components in Class C fly ashes. These are the common crystalline components in Class C fly ashes, except lime and anhydrite. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 4: Periclase MgO 5: Lime CaO Figure I.31 X-Ray Diffraction Results - Kenosha Fly Ash 2θ I.8.4 Scanning Electron Micrographs A set of four micrographs were selected as representative of those obtained for this fly ash. They are described below. An overall idea of the kinds and sizes of particles present in this fly ash is provided in Figure I.32(a). One can find large spherical particles with smooth surface, irregular grains, hollow particles and hundreds of tiny fly ash particles mostly clean. As shown in Figure I.32(b), this micrograph taken at a higher magnification shows two specific extremely large grains found in this fly ash. The one present at the upper area appears more porous and seems to have melted surface, while the other grain seems more solid. There are a lot of tiny particles entrapped in both grains. 56

57 Here is another unusual grain shown in Figure I.32(c). This grain seems containing a lot of small spheres inside, and the shape is highly irregular but relatively smooth. A substantial feature of this fly ash is shown in Figure I.32(d), which is taken at a very low magnification of only 140. It is an unburned carbon and is enormous compared to the size of fly ash particles. Actually, it is even visible during the preparation. I.8.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave the strength activity index being 96% at the age of 7 days and being 121% at the age of 28 days. The difference between the two indices is similar to the previous (Joliet) fly ash, indicating a fairly limited potential reactivity of the Kenosha fly ash during this period. Again, the water requirement of this fly ash is 94%. I.8.6 Summary This Class C fly ash has a rather normal chemical composition, only that the content of SO 3 is relatively low among those of all Class C fly ashes tested in this study. The reactive crystalline components and calcium aluminate type glass structure of this fly ash detected in XRD analysis also seems to be usual. This fly ash is finer than the typical (Miller) fly ash. A certain amount of extreme large pieces of unburned carbon are found in this fly ash by SEM. The addition of this fly ash reduces the strength of mortar at only 4% at 7 days, which indicates that this fly ash has a rather low negative effect on the early strength of mortar. 57

58 (a) 600 (b)

59 (c) 800 (d) 140 Figure I.32 SEM Micrographs of Kenosha Fly Ash as Magnification of 600, (b) 800, (c) 800, (d) 140 (a) 59

60 I.9.1 Chemical Analysis I.9 Rockport Lafarge North America, Rockport Power Station, Rockport, IN I Results of Total Chemical Analysis The results of the total chemical analysis for the Rockport fly ash are shown in Table I.33. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.34. Other pertinent information for this fly ash is shown in Table I.35 under the heading Results of Analyses. Table I.33 Total Chemical Analysis - Rockport Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 5.95 Na2O, % 1.71 K2O, % 1.14 SO3, % 0.99 MgO, % 3.72 Total Table I.34 Derived Parameters - Rockport Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.46 Table I.35 Other Analysis - Rockport Fly Ash Loss on ignition, % 1.05 Total SO3, % 0.99 Soluble SO3, % 0.45 Percentage of the total SO3 that is soluble 46% Soluble Na2O, % 0.03 Soluble K2O, % 0.02 Total alkalies, as equivalent Na2O, % 2.46 Soluble alkalies, as equivalent Na2O, % 0.04 Total alkalies, as equivalent Na2O, % 1.6% 60

61 I Chemical Analysis Interpretations The total SiO 2+Al 2O 3+Fe 2O 3 content of 67% (<70%) results in the classification of Class C for this fly ash, according to the requirement given in ASTM C 618. Among all the Class C fly ashes tested in this study, the Rockport fly ash has the lowest CaO content (16%) and the lowest SO 3 content (0.99%), while the loss on ignition (1.05%) of it appears to be the highest. Contents of other elements show no significant difference from typical Class C fly ash. Again, the alkali content (2.46%) is moderate with mostly insoluble. I.9.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Rockport fly ash. Particle size distribution of this fly ash is presented in Figure I.33, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.34. Parameters related to particle size for this fly ash are shown in Table I Rockport 80 % smaller Diameter (µm) Figure I.33 Particle Size Distribution - Rockport Fly Ash 61

62 25 20 Miller Rockport % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.34 Relative Particle Size Distribution - Rockport Fly Ash Table I.36 Particle Size Parameters - Rockport Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 4354 I Particle Size Distribution Interpretation This is by far the first fly ash that appears to have more particles larger than 45 μm (~5%) than the typical (Miller) fly ash, as shown in Figure I.34. At the same time, percentage of particles smaller than 1 μm in this fly ash is smaller, while in other particle ranges, the percentages of particles in the two fly ashes roughly remain the same. As a result, this fly ash appears a little coarser than the typical fly ash. Actually, the Rockport fly ash is the coarsest one among all the Class C fly ashes tested in this study. This fact is also indicated by the mean particle size of 32 μm for this fly ash. I.9.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Rockport fly ash. No magnetic particles were found in this fly ash. 62

63 X-Ray Diffraction analysis results for this fly ash are given in Figure I.35. The crystalline components detected in this fly ash include: quartz (SiO 2), anhydrite (CaSO 4), merwinite (Ca 3Mg(SiO 4) 2, periclase (MgO), and magnetite (Fe 3O 4). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts (5) (5) : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Magnetite Fe3O4 Figure I.35 X-Ray Diffraction Results - Rockport Fly Ash I.9.4 Scanning Electron Micrographs The following four micrographs were chosen as representative of the larger set obtained for this fly ash. This area shows a well-distribution in particle size of this fly ash in Figure I.36(a) taken at a magnification of The particles mostly are spherical with smooth and clean surface, though there are some exceptions. In contrary to the previous micrograph, Figure I.36(b) shows a rather large grains with almost 200 μm in size for the largest one. The surface of those grains is fairly uneven, and it seems that some of the holes held fly ash particles before, which could have been shaken off. 63

64 There are also smaller irregular grains, as shown in Figure I.36(c). Smooth surface of most particles could be clearly seen here. Figure I.36(d) shows a bulk of unburned carbon residue found in this fly ash. It is filled with hundreds of tiny particles. Though most of the surface has been burned away, the outline of the original fragment is still distinguishable. I.9.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a strength being 105% of the control mortar at the age of 7 days, while being 134% at the age of 28 days, following the standard test method indicated in ASTM C 311. This fly ash appears to have positive effect on the early age strength of mortar, since its strength activity index is by far the first one that exceeds 100%, which means the strength of mortar containing this fly ash is higher than the control mortar even at 7 days age. In addition, the water requirement of this fly ash is 95%. I.9.6 Summary This Class C fly ash has the lowest content of CaO among all the Class C fly ashes tested in this study and it is extremely difficult to identify lime in XRD pattern of this fly ash. This fly ash also has the lowest content of SO 3 and the highest loss on ignition among all those Class C fly ashes. There is a small amount of magnetite showing in XRD analysis despite of the not very high iron content in chemical analysis. This fly ash is the coarsest one among all the Class C fly ashes here. The strength activity index exceeds 100% even at the age of 7 days, which means a positive effect of this fly ash on the early strength of mortar. 64

65 (a) 1000 (b)

66 (c) 600 (d) 600 Figure I.36 SEM Micrographs of Rockport Fly Ash as Magnification of 1000, (b) 300, (c) 600, (d) 600 (a) 66

67 I.10.1 Chemical Analysis I.10 Will County Lafarge North America, Will County, Romeoville, IL I Results of Total Chemical Analysis The results of the total chemical analysis results for the Will County fly ash are shown in Table I.37. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.38. Other pertinent information for this fly ash is shown in Table I.39 under the heading Results of Analyses. Table I.37 Total Chemical Analysis - Will County Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.47 Na2O, % 2.82 K2O, % 0.37 SO3, % 2.61 MgO, % 5.78 Total Table I.38 Derived Parameters - Will County Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 3.06 Table I.39 Results of Analyses - Will County Fly Ash Loss on ignition, % 0.35 Total SO3, % 2.61 Soluble SO3, % 0.43 Percentage of the total SO3 that is soluble 16% Soluble Na2O, % 0.17 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 3.06 Soluble alkalies, as equivalent Na2O, % 0.18 Total alkalies, as equivalent Na2O, % 5.9% 67

68 I Chemical Analysis Interpretations According to the requirements given in ASTM C 618, this fly ash is clearly classified as Class C, with a total SiO 2+Al 2O 3+Fe 2O 3 content of 57% (<70%) and a fairly high CaO content of 27%. The MgO content (5.78%) is a little higher than most of Class C fly ashes in this study. The SO 3 content (2.61%) is a little high yet only 16% of it soluble. The alkali content (about 3%) is also fairly high with mostly insoluble. I.10.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Will County fly ash. Particle size distribution of this fly ash is presented in Figure I.37, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.38. Parameters related to particle size for this fly ash are shown in Table I Will County 80 % smaller Diameter (µm) Figure I.37 Particle Size Distribution - Will County Fly Ash 68

69 30 25 Miller Will County 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.38 Relative Particle Size Distribution - Will County Fly Ash Table I.40 Particle Size Parameters - Will County Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % 8.80 Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 5097 I Particle Size Distribution Interpretation Particle size distribution of this fly ash is obviously skewed to the finer range when compared to that of the typical (Miller) fly ash, as indicated in Figure I.38. While percentage of particles of this fly ash falling in the range of 13 to 26 μm is pretty the same as that of the Miller fly ash, the particles of the size <13 μm appear to be present more (~13%) and those of the size >45 μm appear to be present less. The mean particle size of this relatively fine fly ash is about 15 μm. I.10.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Will County fly ash. No magnetic particles were found in this fly ash. 69

70 X-Ray Diffraction analysis results for this fly ash are given in Figure I.39. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), and merwinite (Ca 3Mg(SiO 4) 2). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO Figure I.39 X-Ray Diffraction Results - Will County Fly Ash I.10.4 Scanning Electron Micrographs The following four micrographs were selected as representative of the larger set obtained in this work. Figure I.40(a) shows a representative area in this fly ash. The variety of particles is shown as the form of spherical particles with smooth and fairly clean surface, irregular grain with clean surface as well as rather decorated surface. Additionally, pieces of unburned carbon residue could also be found here. There is also a typical area of this fly ash, as shown in Figure I.40(b), taken at a lower magnification. There are several larger grains with rough surface and with small particles deposited on. Other than that, there are quite a few fairly small spherical particles. 70

71 A specific particle with well-textured surface is examined and shown in Figure I.40(c) taken at a very high magnification. It appears that the rugged surface has a high content of SO 3 and magnesium (confirmed by EDX examination). Unburned carbon residue seems very hard to find in this fly ash. However, there are two small ones shown in Figure I.40(d). I.10.5 Strength Activity Index The strength activity index for this fly ash is 103% at the age of 7 days and 140% at the age of 28 days. Similar to the previous (Rockport) fly ash, the index higher than 100% at 7 days age indicates that the addition of this particular fly ash has a very good effect on the early age strength of mortar. Moreover, the index at 28 days age appears to be the highest among those of all fly ashes in this study, showing a significant potential reactivity of this fly ash at late age. In addition, the water requirement of this fly ash is 94%. I.10.6 Summary This fly ash is classified as Class C, with a little high content of calcium, magnesium, SO 3 and fairly high content of alkalies, when compared to the other Class C fly ashes studied in this report. The reactive crystalline components and calcium aluminate type glass structure of this fly ash are found to be normal in XRD analysis. There is very few pieces of carbon residue present as examined by SEM. Similar to the previous (Rockport) fly ash, the effect of this fly ash on the early strength of mortar is also positive. Besides, the strength activity index tested at the age of 28 days appears the highest among all the results of other fly ashes in this study. It indicates that this fly ash would be excellent considering its reactivity with cement. 71

72 (a) 1000 (b)

73 (c) 500 (d) 1000 Figure I.40 SEM Micrographs of Will County Fly Ash as Magnification of (a) 1000, (b) 560, (c) 500, (d)

74 I.11 Joppa Mineral Resource Technologies, Joppa Power Generation Station, Joppa, IL I.11.1 Chemical Analysis I Results of Total Chemical Analysis The results of total chemical analysis for the Joppa fly ash are shown in Table I.41. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.42. Other pertinent information for this fly ash is shown in Table I.43 under the heading Other Analysis. Table I.41 Total Chemical Analysis - Joppa Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.36 Na2O, % 1.99 K2O, % 0.49 SO3, % 1.72 MgO, % 5.01 Total Table I.42 Derived Parameters - Joppa Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.31 Table I.43 Results of Analyses - Joppa Fly Ash Loss on ignition, % 0.35 Total SO3, % 1.72 Soluble SO3, % 0.07 Percentage of the total SO3 that is soluble 4% Soluble Na2O, % 0.09 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 2.31 Soluble alkalies, as equivalent Na2O, % 0.10 Total alkalies, as equivalent Na2O, % 4.3% 74

75 I Chemical Analysis Interpretations This fly ash also has a high CaO content of 26% and would be classified as Class C results from the total SiO 2+Al 2O 3+Fe 2O 3 content of 60% (<70%, in ASTM C 618 specification). The CaO content was found to be 26%. The SO 3 content (1.72%) is moderate yet nearly none of it soluble. The alkali content (2.31%) is also common for a Class C fly ash. There is nothing unusual for other elements content of this fly ash. I.11.1 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics determined for the Joppa fly ash. Particle size distribution of this fly ash is presented in the Figure I.41; while a comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.42. Parameters related to particle size for this fly ash are shown in Table I Joppa 80 % smaller Diameter (µm) Figure I.41 Particle Size Distribution - Joppa Fly Ash 75

76 30 25 Miller Joppa 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.42 Relative Particle Size Distribution - Joppa Fly Ash Table I.44 Particle Size Parameters - Joppa Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 4371 I Particle Size Distribution Interpretation Again, the particle size distribution shown in Figure I.42 also indicates this is a relatively finer fly ash when compared to the typical Miller fly ash. Examination of the size distribution bar chart shows that 13 μm is a substantial particle size for this comparison. Particles smaller than 13 μm are found more in this fly ash while particles larger than that are found more in the typical Miller fly ash. The mean particle size of 18 μm more or less indicates the difference of particle size distribution between these two fly ashes. I.11.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Joppa fly ash. The measured weight content of magnetic particles of this fly ash was 0.31%. 76

77 X-Ray Diffraction analysis results for this fly ash are given in Figure I.43. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), merwinite (Ca 3Mg(SiO 4) 2) and magnetite (Fe 3O 4). There are the typical components present in a Class C fly ash. A hump, representing a calcium-aluminate type of glass with a maxiumum at 2θ=~32 is visible Counts : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO 6: Magnetite Fe3O4 Figure I.43 X-Ray Diffraction Results - Joppa Fly Ash I.11.4 Scanning Electron Micrographs A set of four micrographs were chosen as representative of the larger set taken in this work, and are described below. Figure I.44(a) shows one of the relatively rare areas where nearly all of the particles are spherical. They range from 20 μm to 1 μm. Most of the particles are with smooth and clean surface. There is a somewhat more typical area shown in Figure I.44(b), taken at a much lower magnification of 320. There are appreciable numbers of irregular grains, including an extremely long rod of unburned carbon residue. Meanwhile, lots of small to tiny particles are shown. A specific irregular grain is shown in Figure I.44(c). It has rugged surface and many fine particles are deposited on it. Just above it, there is a single large spherical particle appears smooth and fairly clean, which is typical in this fly ash. 77

78 Figure I.44(d) shows a fragment of unburned carbon residue. It seems fairly clean on the surface and with a lot of fine fly ash particles inside. I.11.5 Strength Activity Index The results from trials carried out with this fly ash using Portland cement show a highest strength activity index at the age of 7 days among those of all the fly ashes studied, being 107%. The value of 136% is also high as the strength activity index at the age of 28 days. The water requirement of this fly ash is 94%, which is close to the lowest one among those of all the fly ashes here in this study. I.11.6 Summary This Class C fly ash has a reasonably typical chemical composition, except for a relatively high content of iron. The presence of magnetite in this fly ash has been indicated by XRD analysis. The other reactive crystalline components and calcium aluminate type glass structure appears to be normal for a Class C fly ash. This fly ash is also finer than the typical (Miller) fly ash. Particles detected in SEM are mostly smooth and clean. The results of strength activity index show a very nice positive effect of this fly ash on the strength of mortar at both the early age and the late age. 78

79 (a) 1000 (b)

80 (c) 1500 (d) 2000 Figure I.44 SEM Micrographs of Joppa Fly Ash as Magnification of 1000, (b) 320, (c) 1500, (d) 2000 (a) 80

81 I.12 Labadie Mineral Resource Technologies, Labadie Power Plant, Labadie, MO I.12.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Labadie fly ash are shown in Table I.45. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.46. Other pertinent information for this fly ash is shown in Table I.47 under the heading Results of Analyses. Table I.45 Total Chemical Analysis - Labadie Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.46 Na2O, % 1.54 K2O, % 0.61 SO3, % 2.13 MgO, % 4.86 Total Table I.46 Derived Parameters - Labadie Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

82 Table I.47 Results of Analyses - Labadie Fly Ash Loss on ignition, % 0.25 Total SO3, % 2.13 Soluble SO3, % 1.14 Percentage of the total SO3 that is soluble 54% Soluble Na2O, % 0.05 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 1.94 Soluble alkalies, as equivalent Na2O, % 0.06 Total alkalies, as equivalent Na2O, % 3.1% I Chemical Analysis Interpretations Based on the results of above chemical analysis, it would be proper to classify this fly ash as Class C, according to the requirements given in ASTM C 618 (SiO 2+Al 2O 3+Fe 2O 3=63% < 70%). The CaO content is 24%, typical of a Class C fly ash. The loss on ignition (0.25%) is lower than those of most of the Class C fly ashes studied here. It is common for other elements content of this fly ash. The SO 3 content (2.13%) is moderate with more than half soluble. I.12.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Labadie fly ash. Particle size distribution of this fly ash is presented in Figure I.45, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.46. Parameters related to particle size for this fly ash are shown in Table I Labadie 80 % smaller Diameter (µm) 82

83 Figure I.45 Particle Size Distribution - Labadie Fly Ash Miller Labadie % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.46 Relative Particle Size Distribution - Labadie Fly Ash Table I.48 Particle Size Parameters - Labadie Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 6279 I Particle Size Distribution Interpretation This is a relatively fine fly ash, as indicated by the small value of the mean particle size (17 μm) and the relatively higher content of particles falling in the range of 1 to 13 μm (~15% higher than that of the typical fly ash). At the same time, the different cumulative percentage of particles in the size range of >13 μm between the two fly ashes is also roughly 15%, as shown in Figure I.46. I.12.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Labadie fly ash. 83

84 The measured weight content of magnetic particles of this fly ash was 0%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.47. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), merwinite (Ca 3Mg(SiO 4) 2) and magnetite (Fe 3O 4). These are the common crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts θ 1: Quartz SiO2 1 Q t SiO 4: Periclase MgO 2: Anhydrite CaSO4 5: Lime CaO 3: Merwinite Ca3Mg(SiO4)2 6: Magnetite Fe3O4 Figure I.47 X-Ray Diffraction Results - Labadie Fly Ash I.12.4 Scanning Electron Micrographs Four micrographs were chosen as representative of the larger set obtained in this work, and are described below. A relatively representative area is depicted in Figure I.48(a). Most of the particles shown are fine and smooth, except for one large irregular grain on the right corner of this area, also with smooth surface. 84

85 Figure I.48(b) shows an extremely large grain found to be common in this fly ash, somewhat similar to those found in previous fly ashes. There are also a lot of fine fly ash particles depositing on the grain. In Figure I.48(c), taken at a very high magnification of 3000, a specific particle with well-textured surface is shown and examined by EDX. It turns out that the rugged surface has a very high content of SO 3. Figure I.48(d) shows a very good example of hemispherical particle, with a lot of various size of fly ash particles filled inside. I.12.5 Strength Activity Index The strength activity index tested for this fly ash is 92% at the age of 7 days and 119% at the age of 28 days, according to the standard test method indicated in ASTM C 311. The difference between indices at the two ages of this fly ash is smaller than most of those of the other Class C fly ashes in this study and therefore indicates the fairly limited potential reactivity of this fly ash. In addition, the water requirement of this fly ash is 96%. I.12.6 Summary This is a Class C fly ash with very low loss on ignition. There are no special characteristics in chemical composition, yet in XRD analysis, a rather low content of magnetite could be identified from the pattern. This fly ash is finer than the typical (Miller) fly ash. Large grains with deposits on are found to be common in this fly ash. The results from the strength activity index test indicate a fairly limited potential reactivity of this fly ash with cement during the period tested. 85

86 (a) 600 (b)

87 (c) 3000 (d) 3000 Figure I.48 SEM Micrographs of Labadie Fly Ash as Magnification of 600, (b) 800, (c) 3000, (d) 3000 (a) 87

88 I.13 Mill Creek Mineral Resource Technologies, Mill Creek Station, Louisville, KY I.13.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Mill Creek fly ash are shown in Table I.49. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.50. Other pertinent information for this fly ash is shown in Table I.51 under the heading Results of Analyses. Table I.49 Total Chemical Analysis - Mill Creek Fly Ash CaO, % 5.42 SiO2, % Al2O3, % Fe2O3, % Na2O, % 0.60 K2O, % 2.97 SO3, % 1.12 MgO, % 1.05 Total Table I.50 Derived Parameters - Mill Creek Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

89 Table I.51 Other Analysis - Mill Creek Fly Ash Loss on ignition, % 1.38 Total SO3, % 1.12 Soluble SO3, % 0.69 Percentage of the total SO3 that is soluble 62% Soluble Na2O, % 0.04 Soluble K2O, % 0.06 Total alkalies, as equivalent Na2O, % 2.55 Soluble alkalies, as equivalent Na2O, % 0.08 Total alkalies, as equivalent Na2O, % 3.1% I Chemical Analysis Interpretations This fly ash would be properly classified as Class F fly ash, since the total SiO 2+Al 2O 3+Fe 2O 3 content of 86%, meeting the requirement given in ASTM C 618 (>70%). The SiO 2 content (47.48%) is a little high while the CaO content (5.42%) is moderate. There is nothing unusual for other elements content as of a Class F fly ash. The loss on ignition of this fly ash is the lowest when compared to other Class F fly ashes tested in this study. I.13.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Mill Creek fly ash. Particle size distribution of this fly ash is presented in Figure I.49, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.50. Parameters related to particle size for this fly ash are shown in Table I Mill Creek 80 % smaller Diameter (µm) Figure I.49 Particle Size Distribution - Mill Creek Fly Ash 89

90 30 25 Miller Mill Creek 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.50 Relative Particle Size Distribution - Mill Creek Fly Ash Table I.52 Particle Size Parameters - Mill Creek Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 3739 I Particle Size Distribution Interpretation This is a very different particle size distribution from that of all the previous fly ashes described before. However, it is typical for the Class F fly ashes studied in this project. The main difference for Class F fly ashes from Class C fly ashes is the deficiency of particles in the finer categories (0 to 5 μm) and substantial content of coarser particles. The mean particle size of this fly ash is 26 μm, which appears not so much difference from that of the typical (Miller) fly ash (25 μm). It is probably due to the particles of main size in this fly ash concentrate in the range of 13 to 26 μm. Meanwhile, the percentage of particles larger than 45 μm, about 20% calculated in Figure I.50, is also close to that of the Miller fly ash. It should be noticed that the content of particles larger than 100 μm in this fly ash is actually less than that of the typical fly ash. I.13.3 Measurements of Physicochemical Parameters 90

91 This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Mill Creek fly ash. The measured weight content of magnetic particles of this fly ash was 24.90%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.51. The crystalline components detected in this fly ash include: quartz (SiO 2), anhydrite (CaSO 4), mullite (Al 6Si 2O 13), hematite (Fe 2O 3), and magnetite (Fe 3O 4). A hump, representing a silica type of glass with a maximum at 2θ=~24 is visible Counts 1000 (4) (4) (3) 5 (4) : Quartz SiO2 2: Anhydrite CaSO4 3: Mullite Al6Si2O13 2θ 4: Hematite Fe2O3 5: Magnetite Fe3O4 Figure I.51 X-Ray Diffraction Results - Mill Creek Fly Ash I.13.4 Scanning Electron Micrographs A set of four of the micrographs obtained for this fly ash were chosen as being representative, and are described below: Figure I.52(a) shows an area of mostly spherical fly ash particles, some of which are with rough surface, while others are smooth. The particles in this area range from less than 1 µm to almost 20µm. Figure I.52(b) was taken at a relatively low magnification to show a variety of particles present in this fly ash. In addition to the spherical solid particles, there are some hollow and incomplete spheres as 91

92 well as some irregular particles. The particle with rough surface is presumable magnetic particle and it is typical in this fly ash. Large piece of carbon residue is shown in Figure I.52(c). It is more than 100µm in size, and is probably responsible for the coarse fineness results. Figure I.52(d) shows one of the larger grains, an incompletely spherical partly hollow particle about 20µm. The particles inside are smaller spherical particles and also irregular grains. I.13.5 Strength Activity Index As a Class F fly ash, the results for strength activity index of this fly ash is surprising high, as being 95% at the age of 7 days and being 126% at the age of 28 days, especially for the early age. The result of 7 days age appears to be the highest when compared to those of all other Class F fly ashes, even higher than most of the Class C fly ashes. At the same time, the result of 28 days age still remains to be the highest among those of all Class F fly ashes, yet becomes lower than most of the Class C fly ashes. This fact indicates that this fly ash works better when the early strength of mortar is important, as compared to other Class F fly ashes. However, this fly ash still has a limited potential reactivity as being Class F. I.13.6 Summary This is a Class F fly ash with a little higher content of SiO 2 and the lowest loss on ignition among all the Class F fly ashes tested in this study. The reactive crystalline compounds and a silica type of glass structure detected in XRD are found to be normal as to Class F fly ash. This fly ash is rather coarse with a very different particle size distribution pattern from that of the typical (Miller) fly ash. Large pieces of carbon residue are easily found in this fly ash using SEM, which may be responsible for the relatively coarse particle size distribution. The strength activity index test shows that this fly ash has very less negative effect on the strength of mortar at early age and a surprisingly good potential reactivity with cement at the late age. That is not common for a Class F fly ash. 92

93 (a) 1000 (b)

94 (c) 210 (d) 2000 Figure I.52 SEM Micrographs of Mill Creek Fly Ash as Magnification of 1000, (b) 400, (c) 210, (d) 2000 (a) 94

95 I.14 Petersburg Mineral Resource Technologies, Petersburg Power Station, Petersburg, IN I.14.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Petersburg fly ash are shown in Table I.53. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.54. Other pertinent information for this fly ash is shown in Table I.55 under the heading Results of Analyses. Table I.53 Total Chemical Analysis - Petersburg Fly Ash CaO, % 1.86 SiO2, % Al2O3, % Fe2O3, % Na2O, % 0.67 K2O, % 2.46 SO3, % 0.54 MgO, % 0.88 Total Table I.54 Derived Parameters - Petersburg Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.29 Table I.55 Results of Analyses - Petersburg Fly Ash Loss on ignition, % 1.39 Total SO3, % 0.54 Soluble SO3, % 0.87 Percentage of the total SO3 that is soluble 100% Soluble Na2O, % 0.04 Soluble K2O, % 0.05 Total alkalies, as equivalent Na2O, % 2.29 Soluble alkalies, as equivalent Na2O, % 0.07 Total alkalies, as equivalent Na2O, % 3.1% 95

96 I Chemical Analysis Interpretations This fly ash is clearly classified as Class F, since the total SiO 2+Al 2O 3+Fe 2O 3 content is over 90% (>70%, in ASTM C 618 specification). The CaO content (1.86%) is fairly low. The iron oxide content (25.29%) of this fly ash is the highest among those of all the Class F fly ashes tested here. The SO 3 content (0.54%) is a little low but all of it immediately soluble. This fly ash has a lower loss on ignition when compared to most of Class F fly ashes in this study. I.14.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics determined for the Petersburg fly ash. Particle size distribution of this fly ash is presented in Figure I.53, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.54. Parameters related to particle size for this fly ash are shown in Table I Petersburg 80 % smaller Diameter (µm) Figure I.53 Particle Size Distribution - Petersburg Fly Ash 96

97 40 35 Miller Petersburg 30 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.54 Relative Particle Size Distribution - Petersburg Fly Ash Table I.56 Particle Size Parameters - Petersburg Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g 9849 Blaine fineness, cm 2 /g 2391 I Particle Size Distribution Interpretation Particle size distribution of this fly ash shows great difference from the typical (Miller) fly ash, mainly due to the deficiency of particles in the range of 0 to 5 μm and the excessive particles in the range of 13 to 26 μm. The content of >45 μm particles seems fairly close to that of the Miller fly ash. The mean particle size of this fly ash is 28 μm, which is a little larger than that of the typical fly ash. Therefore, it would be proper to conclude that this is a coarser fly ash when compared to the typical fly ash. I.14.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Petersburg fly ash. The measured weight content of magnetic particles of this fly ash was 37.72%. 97

98 X-Ray Diffraction analysis results for this fly ash are given in Figure I.55. The crystalline components detected in this fly ash include: quartz (SiO 2), mullite (Al 6Si 2O 13), hematite (Fe 2O 3), and magnetite (Fe 3O 4). A hump, representing a silica type of glass with a maximum near 2θ=~24 is visible Counts (2) 3 (3) 4 2 (2) (4) 2 2 (3) : Quartz SiO2 2: Mullite Al6Si2O13 2θ 3: Hematite Fe2O3 4: Magnetite Fe3O4 Figure I.55 X-Ray Diffraction Results - Petersburg Fly Ash I.14.4 Scanning Electron Micrographs The four micrographs described below were chosen as representative of the larger set obtained for this fly ash. Figure I.56(a), taken at a relatively low magnification of 500, shows a variety of particles of the various kinds that occur in this fly ash. Most of the particles shown are spherical, except the obvious piece of fragment in the middle of this area, which is the unburned carbon residue. There is also another piece of carbon residue with very different appearance on the left corner, present with tiny fly ash spheres embedded in them. A great disparity in sizes of the individual particles in this fly ash is shown in Figure I.56(b). There is a very large spherical particle with over 40 µm in size. The surface is rather smooth though with small particles deposited on. On the right part of this area, one can find thin rod and clusters of small particles. Details of particles are shown more clearly in Figure I.56(c), taken at a higher magnification. There are some spherical particles with rough surface. Meanwhile, there are also some small particles 98

99 clustering together. It is resulted from the EDX examination that the rough spheres are iron oxide, while the cluster contains iron also. Figure I.56(d) shows again the Swiss cheese structure of a piece of unburned carbon residue in this fly ash. Here, nearly all the individual spherical particles appear smooth and clean. I.14.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a rather low strength activity index of 7 days age being 82% following the standard test method specified in ASTM C 311. However, it meets the specific requirement indicated in ASTM C 618 that the strength activity index is no less than 75%. At the age of 28 days, the strength of mortar containing this fly ash shows a little higher than that of the control mortar, as the strength activity index is 104%. In addition, the water requirement of this fly ash is 94%. I.14.6 Summary This is a Class F fly ash with fairly lower CaO content and the highest iron content when compared to all the other Class F fly ashes tested in this study. The reactive crystalline compounds and a silica type of glass structure detected in XRD appear usual as a Class F fly ash. This fly ash has great different particle size distribution from the typical (Miller) fly ash and seems rather coarser. The results from the strength activity index test indicate that the addition of this fly ash significantly reduces the early strength of mortar. At the late age of 28 days, the strength of mortar containing this fly ash shows only 4% more than that of the control mortar. This fact indicates the very limited potential reactivity with cement of this Class F fly ash. 99

100 (a) 500 (b)

101 (c) 880 (d) 1200 Figure I.56 SEM Micrographs of Petersburg Fly Ash as Magnification of (a) 500, (b) 400, (c) 880, (d)

102 I.15 Rush Island Mineral Resource Technologies, Rush Island Power Plant, Festus, MO I.15.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Rush Island fly ash are shown in Table I.57. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.58. Other pertinent information for this fly ash is shown in Table I.59 under the heading Results of Analyses. Table I.57 Total Chemical Analysis - Rush Island Fly Ash CaO, % SiO2, % Al2O3, % Fe2O3, % 6.86 Na2O, % 2.02 K2O, % 0.36 SO3, % 2.40 MgO, % 5.51 Total Table I.58 Derived Parameters - Rush Island Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.26 Table I.59 Other Analysis - Rush Island Fly Ash Loss on ignition, % 0.17 Total SO3, % 2.40 Soluble SO3, % 0.05 Percentage of the total SO3 that is soluble 2% Soluble Na2O, % 0.08 Soluble K2O, % 0.01 Total alkalies, as equivalent Na2O, % 2.26 Soluble alkalies, as equivalent Na2O, % 0.09 Total alkalies, as equivalent Na2O, % 4.0% 102

103 I Chemical Analysis Interpretations The total SiO 2+Al 2O 3+Fe 2O 3 content of 58% results in the classification of this fly ash properly as Class C, since it meets the requirement given in ASTM C 618 specification (<70%). The CaO content (27.66%) is the highest value among those of all the Class C fly ashes tested here. The MgO content (5.51%) is a little high. The SO 3 content (2.40%) is also high, yet with almost none of it soluble. The loss on ignition (0.17%) appears extremely low. Actually, it is the lowest among the loss on ignition values of all the Class C fly ashes in this study. I.15.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Rush Island fly ash. Particle size distribution of this fly ash is presented in Figure I.57, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.58. Parameters related to particle size for this fly ash are shown in Table I Rush Island 80 % smaller Diameter (µm) Figure I.57 Particle Size Distribution - Rush Island Fly Ash 103

104 30 25 Miller Rush Island 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.58 Relative Particle Size Distribution - Rush Island Fly Ash Table I.60 Particle Size Parameters - Rush Island Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 5924 I Particle Size Distribution Interpretation This fly ash shows a rather similar particle size distribution to the typical Miller fly ash, as indicated in Figure I.58. Slight differences are observed in each particle range. Nevertheless, the mean particle size of 21 μm and 15% of >45 μm particles shown in Table I.60 indicate that this fly ash is a little finer than the Miller fly ash. I.15.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Rush Island fly ash. The measured weight content of magnetic particles of this fly ash was 0%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.59. The crystalline components detected in this fly ash include: lime (CaO), quartz (SiO 2), periclase (MgO), anhydrite 104

105 (CaSO 4), merwinite (Ca 3Mg(SiO 4) 2) and hematite (Fe 2O 3). These are the typical crystalline components in Class C fly ashes. A hump, representing a calcium-aluminate type of glass with a maximum at 2θ=~32 is visible Counts (6) (6) : Quartz SiO2 2: Anhydrite CaSO4 3: Merwinite Ca3Mg(SiO4)2 2θ 4: Periclase MgO 5: Lime CaO 6: Hematite Fe2O3 Figure I.59 X-Ray Diffraction Results - Rush Island Fly Ash I.15.4 Scanning Electron Micrographs The following four micrographs were selected as representative of those obtained for this fly ash. This is a representative area of this fly ash shown in Figure I.60(a). There are some irregular grains as well as the spherical particles. Most of them are smooth however commonly with smaller fly ash particle deposits. Another micrograph is taken at the same magnification as shown in Figure I.60(b). The relatively fine, mostly smooth fly ash spheres predominate here except that there is a very thin rod present on the right area. Extremely large fragments of unburned carbon residue are also found in this fly ash, one of which is shown in Figure I.60(c), taken at a very low magnification of only 150. This fragment is fairly clean, very few fly ash particles are found on the surface or inside it. There is another representative grain of oversize material shown in Figure I.60(d), also taken at a rather low magnification. It is over 200 µm in size and smooth however with many tiny fly ash particles deposited on. 105

106 I.15.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a strength being 97% of the control mortar at the age of 7 days, while being 128% at the age of 28 days. The strength activity index of 7 days age is higher than those of most of the other Class C fly ashes, indicating a relatively less negative effect of this fly ash on the early age strength when mixed with Portland cement. In addition, the water requirement of this fly ash is 96%. I.15.6 Summary This is a Class C fly ash with the highest content of CaO among all the Class C fly ashes tested in the study. The contents of MgO and SO 3 are also a little high and the loss on ignition of this fly ash appears to be the lowest among all the fly ashes here. In the XRD analysis, a small amount of hematite could be identified. This fly ash is a litter finer than the typical (Miller) fly ash. Some large fragments of carbon residue are found by SEM in this fly ash. The results from the strength activity index test indicate that this fly ash has a very low negative effect on the early strength of mortar as well as a not very high potential reactivity with cement. 106

107 (a) 1000 (b)

108 (c) 150 (d) 300 Figure I.60 SEM Micrographs of Rush Island Fly Ash as Magnification of (a) 1000, (b) 1000, (c) 150, (d)

109 I.16 Trimble Mineral Resource Technologies, Trimble County Power Station, Bedford, KY I.16.1 Chemical Analysis I Results of Total Chemical Analysis The results of the total chemical analysis for the Trimble fly ash are shown in Table I.61. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.62. Other pertinent information for this fly ash is shown in Table I.63 under the heading Results of Analyses. Table I.61 Total Chemical Analysis - Trimble Fly Ash CaO, % 2.50 SiO2, % Al2O3, % Fe2O3, % Na2O, % 0.73 K2O, % 1.97 SO3, % 0.99 MgO, % 0.86 Total Table I.62 Derived Parameters - Trimble Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.03 Table I.63 Other Analysis - Trimble Fly Ash Loss on ignition, % 1.89 Total SO3, % 0.99 Soluble SO3, % 1.09 Percentage of the total SO3 that is soluble 100% Soluble Na2O, % 0.04 Soluble K2O, % 0.05 Total alkalies, as equivalent Na2O, % 2.45 Soluble alkalies, as equivalent Na2O, % 0.07 Total alkalies, as equivalent Na2O, % 2.9% 109

110 I Chemical Analysis Interpretations Based on the fact that the total SiO 2+Al 2O 3+Fe 2O 3 content of this fly ash is 88%, it would be proper to classify it as Class F, according to the requirement (>70%) given in ASTM C 618. The CaO content (2.50%) is low. Contents of other elements are normal and the loss on ignition is also moderate when compared to those values of other Class F fly ashes in this study. I.16.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Trimble fly ash. Particle size distribution of this fly ash is presented in Figure I.61, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.62. Parameters related to particle size for this fly ash are shown in Table I Trimble 80 % smaller Diameter (µm) Figure I.61 Particle Size Distribution - Trimble Fly Ash 110

111 35 30 Miller Trimble 25 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.62 Relative Particle Size Distribution - Trimble Fly Ash Table I.64 Particle Size Parameters - Trimble Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g 8857 Blaine fineness, cm 2 /g 3253 I Particle Size Distribution Interpretation This is another coarser fly ash as compared to the typical (Miller) fly ash shown in Figure I.62. The particle size distribution has no much difference from those of the typical Class F fly ashes described previously, except for some percentage changes in certain particle range. The mean particle size of 27 μm is a little larger than the Miller fly ash, while the content of >45 μm particles is pretty close. I.16.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Trimble fly ash. The measured weight content of magnetic particles of this fly ash was 26.40%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.63. The crystalline components detected in this fly ash include: quartz (SiO 2), mullite (Al 6Si 2O 13), hematite (Fe 2O 3), and 111

112 magnetite (Fe 3O 4). A hump, representing a silica type of glass with a maximum at 2θ=~24 is visible Counts (3) 4 (2) 3 (2) 3 (2) (4) (3) : Quartz SiO2 2: Mullite Al6Si2O13 2θ 3: Hematite Fe2O3 4: Magnetite Fe3O4 Figure I.63 X-Ray Diffraction Results - Trimble Fly Ash I.16.4 Scanning Electron Micrographs A set of four micrographs were selected as representative of the larger set obtained in this work, and are described below. As shown in Figure I.64(a), this micrograph is taken at a magnification of 600. In the depicted area, those fly ash particles are well distributed. There are some irregular grains present among those spherical particles, and both kinds of them appear fairly clean. It is easy to find some thin plates of unburned carbon residue on the upper part of this area. There is another representative area shown in Figure I.64(b), taken at a higher magnification of Several types of particles are present including mostly smooth and clean spherical particles mentioned in previous micrograph, a cluster of tiny fly ash spheres and a nearly spherical but hollow grain filled with tiny particles. Figure I.64(c), taken at a much higher magnification, shows a specific grain found and examined in this fly ash. The surface looks like lots of tiny fly ash particles well agglomerated. High SO 3 content is found in these small particles. 112

113 In Figure I.64(d), a piece of fragment from unburned carbon is shown. As described before, this kind of carbon residue seems fairly common in a lot of fly ashes tested in this project. In this case, this fragment is less burned. I.16.5 Strength Activity Index The strength activity index of this fly ash at the age of 7 days being 86% is higher than those of most of the other Class F fly ashes in this study, as a result from standard test method in ASTM C 311. At the same time, the strength activity index at the age of 28 days being 109% is close to the lowest value among those of all the Class F fly ashes tested. This fact results in the lowest potential reactivity of this fly ash during this period, when compared to all the other Class F fly ashes. In addition, the water requirement of this fly ash is 97%. I.16.6 Summary This is a fairly typical Class F fly ash with reasonably chemical composition as well as normal reactive crystalline compounds and a silica type of glass structure found in XRD analysis. This fly ash is coarser than the typical (Miller) fly ash and with very different particle size distribution. Large fragments of unburned carbon are easily found in this fly ash by using SEM. The results from the strength activity index test indicate the lowest potential reactivity of this fly ash among all the Class F fly ashes tested in this study during the test period. 113

114 (a) 600 (b)

115 (c) 2500 (d) 1000 Figure I.64 SEM Micrographs of Trimble Fly Ash as Magnification of 600, (b) 1000, (c) 2500, (d) 1000 (a) 115

116 I.17.1 Chemical Analysis I.17 Elmer Smith Fly Ash Direct, Elmer Smith Station, Owensboro, KY I Results of the Total Chemical Analysis The results of the total chemical analysis for the Elmer Smith fly ash are shown in Table I.65. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.66. Other pertinent information for this fly ash is shown in Table I.67 under the heading Results of Analyses. Table I.65 Total Chemical Analysis - Elmer Smith Fly Ash CaO, % 9.31 SiO2, % Al2O3, % Fe2O3, % Na2O, % 0.80 K2O, % 2.31 SO3, % 1.71 MgO, % 0.90 Total Table I.66 Derived Parameters - Elmer Smith Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, %

117 Table I.67 Results of Analyses - Elmer Smith Fly Ash Loss on ignition, % 2.37 Total SO3, % 1.71 Soluble SO3, % 0.6 Percentage of the total SO3 that is soluble 35% Soluble Na2O, % 0.03 Soluble K2O, % 0.03 Total alkalies, as equivalent Na2O, % 2.32 Soluble alkalies, as equivalent Na2O, % 0.05 Total alkalies, as equivalent Na2O, % 2.2% I Chemical Analysis Interpretations This fly ash is classified as Class F according to ASTM C 618 specification, due to the fact that the total SiO 2+Al 2O 3+Fe 2O 3 content of this fly ash is 81% (>70%). However, the CaO content appears unusually high for a Class F fly ash. The SO 3 content (1.71%) is a little high, yet with only 35% of it soluble. The loss on ignition (2.37%) is moderate. I.17.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Elmer Smith fly ash. Particle size distribution of this fly ash is presented in Figure I.65, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.66. Parameters related to particle size for this fly ash are shown in Table I Elmer Smith 80 % smaller Diameter (µm) Figure I.65 Particle Size Distribution - Elmer Smith Fly Ash 117

118 30 25 Miller Elmer Smith 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.66 Relative Particle Size Distribution - Elmer Smith Fly Ash Table I.68 Particle Size Parameters - Elmer Smith Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g 6344 Blaine fineness, cm 2 /g 3092 I Particle Size Distribution Interpretation As shown in Figure I.66, the particle size distribution of this fly ash seems also typical. There is a slight difference from the previous Class F fly ashes discussed before. That is, the particles with size of >100 μm present in this fly ash are a little more than those in the typical Miller fly ash. Accordingly, the cumulative percentage of particles >45 μm in this fly ash (~24%) is larger when compared to that of the Miller fly ash (~19%). At the same time, the amount of particles with size of <5 μm in this fly ash are far less, almost one third as that in the Miller fly ash. The mean particle size of 33 μm and the distribution described before make it the coarsest fly ash among all the Class F fly ashes tested in this study. Blaine s fineness is less than that of many cements. I.17.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Elmer Smith fly ash. 118

119 The measured weight content of magnetic particles of this fly ash was extremely high at 32.99%. X-Ray Diffraction analysis results for this fly ash are given in Figure I.67. The crystalline components detected in this fly ash include: quartz (SiO 2), lime (CaO), anhydrite (CaSO 4), mullite (Al 6 Si 2O 13), large contents of hematite (Fe 2O 3) and magnetite (Fe 3O 4). These are the common crystalline components in Class C fly ashes except for the lime and anhydrite. A hump, representing a silica type of glass (with a maxiumum at 2θ=~24, Cu radiation) is visible Counts 1000 (4) (4) (6) (3) 5 (4) : Quartz SiO2 2: Anhydrite CaSO4 3: Mullite Al6 Si2O13 2θ 4: Hematite Fe2O3 5: Magnetite Fe3O4 6: Lime CaO Figure I.67 X-Ray Diffraction Results - Elmer Smith Fly Ash I.17.4 Scanning Electron Micrographs The four micrographs discussed below were chosen as representative of the larger set taken in this work. In Figure I.68(a), there is a representative area shown, where most kinds of particles in this fly ash can be found. Besides the smooth and relatively clean spheres, there are also irregular grains or spheres with rough surface. 119

120 Figure I.68(b) is taken at the same magnification and shows a similar area compared to the previous one, except for several pieces of fragments from unburned carbon residue. They are easily found as the angular shape and clearly left after being burned. There are some particular grains found in this fly ash, as one of them shown in Figure I.68(c). They have thin shell structure, and contain mainly silica and alumina from the examination results. The surface is fairly smooth, with small fly ash particles deposited on. There is another kind of specific particle shown in Figure I.68(a). The main particle with curved surface contains silica and calcium oxide, while the small deposits are examined to be calcium oxide only. I.17.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a strength being 84% of the control mortar at the age of 7 days, while being 110% at the age of 28 days, following the standard test method in ASTM C 311. Both the indices are at average level among those of all the Class F fly ashes. The water requirement of this fly ash is 98%, which is the highest among all the fly ashes tested. I.17.6 Summary This is a Class F fly ash with a relatively high content of calcium resulted from chemical analysis. The Fe2O3 content was unusually very high for a fly ash, even for a Class F fly ash. This resulted in an unusually high content of magnetic particles. The content of SO 3 is also a little high. As a result, a certain amount of lime and anhydrite could be easily identified from the XRD patterns of this fly ash. Other reactive crystalline compounds and a silica type of glass structure seem to be normal as for Class F fly ashes. This fly ash is coarser than the typical (Miller) fly ash. The strength activity index for this fly ash at both 7 days and 28 days are at average among all the Class F fly ashes tested in this study, showing a limited potential reactivity with cement. 120

121 (a) 1000 (b)

122 (c) 2000 (d) 2000 Figure I.68 SEM Micrographs of Elmer Smith Fly Ash as Magnification of (a) 1000, (b) 1000, (c) 2000, (d)

123 I.18.1 Chemical Analysis I.18 Miami 7 Fly Ash Direct, Miami Fort Unit #7, North Bend, OH I Results of Total Chemical Analysis The results of the total chemical analysis for the Miami 7 fly ash are shown in Table I.69. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.70. Other pertinent information for this fly ash is shown in Table I.71 under the heading Results of Analyses. Table I.69 Total Chemical Analysis Miami 7 Fly Ash CaO, % 1.25 SiO2, % Al2O3, % Fe2O3, % 4.96 Na2O, % 0.36 K2O, % 2.79 SO3, % 0.21 MgO, % 0.85 Total Table I.70 Derived Parameters Miami 7 Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.20 Table I.71 Results of Analyses Miami 7 Fly Ash Loss on ignition, % 2.31 Total SO3, % 0.21 Soluble SO3, % 0.42 Percentage of the total SO3 that is soluble -- Soluble Na2O, % 0.02 Soluble K2O, % 0.02 Total alkalies, as equivalent Na2O, % 2.20 Soluble alkalies, as equivalent Na2O, % 0.03 Total alkalies, as equivalent Na2O, % 1.4% 123

124 I Chemical Analysis Interpretations Based on the chemical analysis above and following the requirements given in ASTM C 618, it is proper to conclude that this is a Class F fly ash with rather unusual chemical composition. While the total SiO 2+Al 2O 3+Fe 2O 3 content is normally over 90%, but the Fe 2O 3 content (4.96%) is smaller and the Al 2O 3 content (29.45%) is larger than the typical values shown in other Class F fly ashes, which basically around 25% and 20%. Moreover, the SiO 2 content (55.89%) is extremely high. The CaO content is very small and the SO 3 content (0.21%) is fairly low, and all of it soluble. The alkali content is typical (2.20%) and most of it insoluble. I.18.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Miami 7 fly ash. Particle size distribution of this fly ash is presented in Figure I.69, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.70. Parameters related to particle size for this fly ash are shown in Table I Miami 7 80 % smaller Diameter (µm) Figure I.69 Particle Size Distribution - Miami7 Fly Ash 124

125 30 25 Miller Miami 7 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.70 Relative Particle Size Distribution Miami 7 Fly Ash Table I.72 Particle Size Parameters Miami 7 Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 4088 I Particle Size Distribution Interpretation As shown in Figure I.70, the main differences between the particle size distribution of this fly ash and that of the typical (Miller) fly ash remain in the cumulative percentages of particles in the range of smaller than 5 μm and 13 to 100 μm. As a result, the mean particle size of this fly ash (~30 μm) is a little larger than that of the Miller fly ash (~25 μm). Meanwhile, the percentage of particles with the size >45 μm from LPSD (~24%) shown in Table I.72 is also higher than that of the Miller fly ash (~19%). Therefore, this fly ash appears a little coarser than the typical fly ash. I.18.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Miami 7 fly ash. The measured weight content of magnetic particles of this fly ash was 3.68%, but no crystalline magnetic components were detected. 125

126 X-Ray Diffraction analysis results for this fly ash are given in Figure I.71. The crystalline components detected in this fly ash include: quartz (SiO 2), and mullite (Al 6 Si 2O 13). No iron oxide peaks were detected. A hump, representing a silica type of glass with a maximum at 2θ=~24 is visible Counts θ 1: Quartz SiO2 2: Mullite Al6 Si2O13 Figure I.71 X-Ray Diffraction Results Miami 7 Fly Ash I.18.4 Scanning Electron Micrographs Of the micrographs taken for this fly ash, four micrographs were selected as being representative and are described below. Figure I.72(a) shows a very typical area of this fly ash, including almost all kinds of particles and grains. It is obvious that irregular grains are substantial in this fly ash, compared to those clean and smooth spherical particles. In the current area present, it is easy to find some shell fragment presumably from a hollow sphere, unburned carbon residue with Swiss cheese structure, as well as irregular and combined fly ash grains. Here is another typical area of this particular fly ash. In Figure I.72(b), taken at the same magnification as previous one, the predomination of unburned carbon residue is evident. Moreover, these fragments of carbon residue are much larger in size compared to those fly ash spheres. 126

127 Figure I.72(c) shows several very large pieces of fragment. As described before, they are assumed once to be part of the large hollow fly ash particles. It contains mainly silica and alumina from the EDX examination results. The appearance of one particular grain at a low magnification is shown in Figure I.72(d). It is over 100 µm in size and apparently hollow, with lots of small fly ash particles inside. Again, besides this large particle, irregular grains and cluster of tiny fly ash particles are present in this area. I.18.5 Strength Activity Index Similar to the previous (Elmer Smith) fly ash, the strength activity index of this fly ash at the age of 7 days being 84% is at average level among those of all the other Class F fly ashes. However, the strength activity index at the age of 28 days being 118% is fairly high. This results in the biggest difference present between the two indices of this fly ash and hence the highest potential reactivity during this period, as compared to those of all the other Class F fly ashes. In addition, the water requirement of this fly ash is 98%, which is the highest among all the fly ashes tested. I.18.6 Summary This is a Class F fly ash but one with an extremely low content of iron oxide, even lower than those of most Class C fly ashes in this study. On the other hand, the content of silica and alumina are extremely high. Accordingly, there are only two reactive crystalline compounds, quartz and mullite in the XRD patterns for this fly ash. This fly ash is a little coarser than the typical (Miller) fly ash. Large fragments of unburned carbon are easily found by SEM. The results of the strength activity index for this fly ash indicate the highest potential reactivity than any of the other Class F fly ashes tested here. 127

128 (a) 400 (b)

129 (c) 360 (d) 400 Figure I.72 SEM Micrographs of Miami 7 Fly Ash as Magnification of 400, (b) 400, (c) 360, (d) 400 (a) 129

130 I.19.1 Chemical Analysis I.19 Fly Ash No.19: Miami 8 Fly Ash Direct, Miami Fort Unit #8, North Bend, OH I Results of Total Chemical Analysis The results of thetotal chemical analysis for the Miami 8 fly ash are shown in Table I.73. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.74. Other pertinent information for this fly ash is shown in Table I.75 under the heading Results of Analyses. Table I.73 Total Chemical Analysis Miami 8 Fly Ash CaO, % 3.98 SiO2, % Al2O3, % Fe2O3, % 4.62 Na2O, % 0.88 K2O, % 2.54 SO3, % 0.45 MgO, % 1.44 Total Table I.74 Derived Parameters Miami 8 Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 2.55 Table I.75 Results of Analyses Miami 8 Fly Ash Loss on ignition, % 2.43 Total SO3, % 0.45 Soluble SO3, % 0.76 Percentage of the total SO3 that is soluble -- Soluble Na2O, % 0.04 Soluble K2O, % 0.02 Total alkalies, as equivalent Na2O, % 2.55 Soluble alkalies, as equivalent Na2O, % 0.05 Total alkalies, as equivalent Na2O, % 2.0% 130

131 I Chemical Analysis Interpretations The chemical composition of this fly ash appears very similar to that of the Miami 7 fly ash, probably due to the same coal source. While the CaO content (4%) is a little higher than the Miami 7 fly ash and the total SiO 2+Al 2O 3+Fe 2O 3 content is a little lower (96%), it is no doubt to also classify this fly ash to Class F (according to ASTM C 618 specification). The SO 3 content (0.45%) is low, with all of it soluble. I.19.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Miami 8 fly ash. Particle size distribution of this fly ash is presented in Figure I.73, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.74. Parameters related to particle size for this fly ash are shown in Table I Miami 8 80 % smaller Diameter (µm) Figure I.73 Particle Size Distribution Miami 8 Fly Ash 131

132 30 25 Miller Miami 8 20 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.74 Relative Particle Size Distribution Miami 8 Fly Ash Table I.76 Particle Size Parameters Miami 8 Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 3600 I Particle Size Distribution Interpretation Similar to the chemical similarity found between the present fly ash and previous fly ash (Miami 7), there are almost the same particle size distribution curves for both, as shown in Figure I.70 and Figure I.74. Moreover, they have fairly the same percentage of >45 μm particles from LPSD as shown in Table I.72 and Table I.76, which is 24% and 23% respectively. The mean particle size of 32 μm of this fly ash is also a little larger than the typical (Miller) fly ash. All the above facts indicate this is another coarser fly ash when compared to the typical fly ash. I.19.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Miami 7 fly ash. The measured weight content of magnetic particles of this fly ash was 4.18%. 132

133 X-Ray Diffraction analysis results for this fly ash are given in Figure I.71. The crystalline components detected in this fly ash include: quartz (SiO 2), and mullite (Al 6 Si 2O 13). A hump, representing a silica type of glass with a maximum at 2θ=~24 is visible Counts θ 1: Quartz SiO2 2: Mullite Al6 Si2O13 Figure I.75 X-Ray Diffraction Results Miami 8 Fly Ash I.19.4 Scanning Electron Micrographs Four micrographs were chosen as representative of the larger set taken in this work, and are described below. Figure I.76(a) shows a very typical area of this fly ash. On the contrary to the similarity of chemical composition and particle size distribution between this fly ash and Miami 7, it is surprisingly found that the morphologies of those two fly ashes are very different. In this area, it is evident that most of the particles present are smooth and clean. Moreover, the spherical particles are much more than the irregular gains. There is another typical area shown in Figure I.76(b) taken at a little higher magnification. There is a very large spherical particle over 50 µm in size. Other than that, lots of particles seem much smaller, however also with smooth and clean surface. Several irregular grains and broken shell can be found, but again, in a rather limited amount. There is a noticeable grain shown in Figure I.76(c). It is on the left corner of this area. It appears to be an irregular fly ash grain; however, it is actually the unburned carbon residue from the examination result. It is the most integral carbon grain found so far. 133

134 In Figure I.76(d), a fragment of unburned carbon residue with more common appearance is shown. These are the similar structure to the ones found in Miami 7 fly ash, but in a much less amount. I.19.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a strength being 85% of the control mortar at the age of 7 days, while being 112% at the age of 28 days, following the standard test method in ASTM C 311. Again, both the indices are at average level among those of all the Class F fly ashes. The water requirement of this fly ash is 98%, which is the highest among all the fly ashes tested. I.19.6 Summary Similar to the previous (Miami 7) fly ash, this Class F fly ash is also with extremely low content of iron oxide and fairly high content of silica and alumina. In XRD analysis, there are also only two reactive crystalline compounds detected as well as a silica type of glass structure. This fly ash is also a little coarser than the typical (Miller) fly ash. However, it is surprisingly found that the morphology of this fly ash is far different from that of the previous fly ash. For this fly ash, most of the particles present are smooth and clean. Besides, similar large fragments of unburned carbon are also found in this fly ash, yet with a much less number compared to that of the previous fly ash. The results of the strength activity index indicate the average potential reactivity with cement of this fly ash, as compared to those of all the other Class F fly ashes tested here. 134

135 (a) 400 (b)

136 (c) 720 (d) 1000 Figure I.76 SEM Micrographs of Miami 8 Fly Ash as Magnification of 400, (b) 840, (c) 720, (d) 1000 (a) 136

137 I.20.1 Chemical Analysis I.20 Fly Ash No.20: Zimmer Fly Ash Direct, Zimmer Power Station, Moscow, OH I Results of Total Chemical Analysis The results of the total chemical analysis results for the Zimmer fly ash are shown in Table I.77. The results of this analysis were used to calculate the Derived Parameters values shown in Table I.78. Other pertinent information for this fly ash is shown in Table I.79 under the heading Results of Analyses. Table I.77 Total Chemical Analysis - Zimmer Fly Ash CaO, % 4.94 SiO2, % Al2O3, % Fe2O3, % Na2O, % 0.44 K2O, % 1.52 SO3, % 3.07 MgO, % 4.81 Total Table I.78 Derived Parameters - Zimmer Fly Ash Total SiO2+ Al2O3+ Fe2O3, % Total alkalies, as equivalent Na2O, % 1.44 Table I.79 Results of Analyses - Zimmer Fly Ash Loss on ignition, % 1.48 Total SO3, % 3.07 Soluble SO3, % 2.08 Percentage of the total SO3 that is soluble 68% Soluble Na2O, % 0.03 Soluble K2O, % 0.02 Total alkalies, as equivalent Na2O, % 1.44 Soluble alkalies, as equivalent Na2O, % 0.04 Total alkalies, as equivalent Na2O, % 2.8% 137

138 I Chemical Analysis Interpretations This fly ash, with the total SiO 2+Al 2O 3+Fe 2O 3 content of 82% (>70%) and a relative high Fe 2O 3 content (24.90%) would be proper to be classified as Class F, according to ASTM C 618 specification. The MgO content (4.81%) is unusually high as for a Class F fly ash, so is the SO 3 content (3.07%), with 68% soluble. The alkali content (1.44%) is fairly low. I.20.2 Physical Characteristics I Results from Experiments This section contains the results of the physical characteristics evaluations of the Zimmer fly ash. Particle size distribution of this fly ash is presented in Figure I.77, while the comparison of particle size distribution between this fly ash and the typical (Miller) Class C fly ash is given in Figure I.78. Parameters related to particle size for this fly ash are shown in Table I Zimmer 80 % smaller Diameter (µm) Figure I.77 Particle Size Distribution - Zimmer Fly Ash 138

139 35 30 Miller Zimmer 25 % By Weight to 1 1 to 5 5 to to to to to 200 Diameter (µm) Figure I.78 Relative Particle Size Distribution - Zimmer Fly Ash Table I.80 Particle Size Parameters - Zimmer Fly Ash % > No.325 sieve (Supplier Certificate), % % > 45 µm (LPSD), % Mean particle size (LPSD), µm Specific Area (LPSD),cm 2 /g Blaine fineness, cm 2 /g 3782 I Particle Size Distribution Interpretation As shown in Figure I.78, the particle size distribution indicates that this fly ash is relatively coarser than the typical (Miller) fly ash, though there are less particles with the size of >45 μm appear to present in this fly ash (~18%) than in the Miller fly ash (~19%). The mean particle size of this fly ash is 26 μm, a little bit larger than that of the Miller fly ash (~25 μm). In fact, this fly ash is a relatively finer fly ash among all the Class F fly ashes tested in this study. I.20.3 Measurements of Physicochemical Parameters This section contains the test results of content of magnetic particles and X-Ray Diffraction (XRD) analysis for the Zimmer fly ash. The measured weight content of magnetic particles of this fly ash was 35.32%. 139

140 X-Ray Diffraction analysis results for this fly ash are given in Figure I.67. The crystalline components detected in this fly ash include: quartz (SiO 2), periclase (MgO), anhydrite (CaSO 4), mullite (Al 6 Si 2O 13), hematite (Fe 2O 3) and magnetite (Fe 3O 4). A hump, representing a silica type of glass with a maximum near 2θ=~24 is visible Counts (4) 5 (3) (3) 6 (6) (3) (3) (3) : Quartz SiO2 2: Anhydrite CaSO4 3: Mullite Al6 Si2O13 2θ 4: Hematite Fe2O3 5: Magnetite Fe3O4 6: Periclase MgO Figure I.79 X-Ray Diffraction Results - Zimmer Fly Ash I.20.4 Scanning Electron Micrographs The following four micrographs were chosen as representative of the larger set obtained for this fly ash and are described below. An overall view of this fly ash is shown in Figure I.80(a). It is easy to find different types of those particles and grains, including solid spheres, hollow particles, irregular grains, thin rod, as well as clusters of tiny small particles. This micrograph shown in Figure I.80(b) is taken at a little higher magnification, so the details of the typical particles are shown more clearly. The third sphere from the top on the left with slight rough surface is presumable to be magnetic particle, since the only compound found in it is iron oxide. The irregular grain in the middle of this area, which appears with a lot of tiny fly ash particles deposited on, contains high content of magnesium. 140

141 Another view of the particles at a higher magnification is shown in Figure I.80(c). The large rough particle on the upper part has a high content of ion. Again, the irregular grain with very rough surface has a fairly high content of magnesium. Unburned carbon residue seems hard to find in this fly ash, though there is one shown in Figure I.80(d). It is a small fragment, probably from the carbon mostly burned away. I.20.5 Strength Activity Index Trials carried out with this fly ash using Portland cement gave a very poor result in the strength activity index at the age of 7 days, as the strength recorded is only 70% of the control mortar. Although at the age of 28 days, the strength of mortar containing this particular fly ash increased and reached 96% of that of the control mortar, these results failed to meet the requirements specified in ASTM C 618 that both of the strength activity index at 7 days and 28 days should be no less than 75%. In fact, the strength activity index of this fly ash is the lowest value among values of all the fly ashes tested in this study, at both 7 days and 28 days. The water requirement of this fly ash is 98%, which is the highest among those of all the fly ashes tested. I.20.6 Summary This is a Class F fly ash with unusually high content of magnesium and SO 3 that a certain amount of periclase and anhydrite could be identified in XRD analysis. This fly ash is a little coarser than the typical (Miller) fly ash yet it is actually relatively fine among all those Class F fly ashes in this study. Most particles detected in this fly ash by SEM appear rough and irregular, which may be responsible for the high water requirement of this fly ash. In addition, the strength activity index of this fly ash at 7 days fails to meet the requirement specified in ASTM C 618. Even at 28 days, the strength of mortar containing this fly ash still shows lower than the control mortar. This is the only case of all the fly ashes studied in this report. Therefore, this fly ash would not be recommended to projects where strength, at both early and late age, is big concern. 141

142 (a) 400 (b)

143 (c) 1000 (d) 800 Figure I.80 SEM Micrographs of Zimmer Fly Ash as Magnification of 400, (b) 600, (c) 1000, (d) 800 (a) 143

144 SECTION II DISCUSSION Section I of this handbook presents extensive data on a suite of 20 fly ashes used in this study, 13 of them classified as the ASTM C618 Class C and 7 classified as the ASTM C618 Class F. The results collected for each fly ash were described and interpreted individually. This section of the handbook presents a general comparison of the fly ashes and summarizes their main physical and chemical characteristics. Among the 13 Class C fly ashes studied in this project, many, but not all, have very similar chemical compositions. This general compositional pattern can be described as follows: a) A combined content of silicon, aluminum and iron oxides is in the range of 56% to 65%. Only in the case of two of the fly ashes (Schahfer and Rockport) was the combined content of these oxides slightly higher (~ 68%). b) The iron oxide contents of almost all the Class C fly ashes varied very little from the typical content of ~6% with one exception. The iron oxide content of Edwards fly ash was approximately 10%, which is higher than that normally seen in Class C fly ashes. c) Typical CaO contents ranged from about 22% to 26% for most Class C fly ashes. However, CaO contents are found to be as low as 20% (Rockport) and as high as 28% (Rush Island). d) The contents of Na 2O of all Class C fly ashes presented here were found to be consistently around 0.50%. The contents of K 2O were typically in the range of 1.4~2.1% with exceptions of Joliet and Will County ashes, for which these values were, respectively, 3.7% and 2.8%. For all Class C fly ashes, both alkalis were found to be almost complete insoluble. e) The SO 3 contents of Class C fly ashes are relatively low, with the highest value being 2.7% (Edwards) and the lowest 1.0% (Rockport). The maximum SO 3 value presented in ASTM C 618 is 5% for Class C fly ash. f) The contents of MgO appears the normal range of 4~6% for all the Class C fly ashes, although the 4% MgO content of No.17 Rockport seems low for a Class C fly ash. g) The values for loss-on-ignition of almost all the Class C fly ashes are typically below 0.50% or a little higher (0.61% for No.3 Hennepin), except only one case which is quite high for a Class C fly ash (0.90% for No.17 Rockport). The 7 Class F fly ashes also appear to share some common chemical composition characteristics although again, several exceptions present. The values are quite distinct from those of the Class C ashes. Compositions for Class F fly ashes studied here are summarized as follows: a) The combined content of silicon, aluminum and iron oxides ranges from 81 to 91%. According to ASTM C 618, the Class F fly ash requirement for combined silicon, aluminum and iron oxides is not less than 70%. b) With respect to iron oxide content, 5 out of the 7 Class F fly ashes have iron oxide contents within the range of 18 to 25%. However, the other 2 Class F fly ashes (No.11 Miami 7 and No.12 Miami 8, both from the same plant, show much lower contents of iron oxide, both close to 5%. These two fly ashes have relatively high contents of silica (about 56%) and aluminum oxide 144

145 (29% for No.11 Miami 7 and 26% for No.12 Miami 8, compared to the typical content of around 20% for Class F fly ashes in this study). The CaO contents appear reasonable for almost all Class F fly ashes here except for No.10 Elmer Smith, for which the CaO content reaches 9%. This CaO content is considered to be rather high for a Class F fly ash. The XRD pattern for this fly ash includes a clear peak for CaO, which is not common in Class F fly ashes. c) The combined alkali contents seem consistent for almost all the Class F fly ashes in this study. The only exception is No.14 Zimmer, with a relatively low content of 1.4% compared to a usual content of around 2.3%. d) Contrary to alkali contents, the SO 3 contents of different Class F fly ashes vary over a broad range. A single fly ash, no. 14 Zimmer has an unusually high content (3.1%), the while others are below 1.7%. The lowest sulfate content is 0.21%, which is for No.11 Miami 7. e) The contents of MgO appear to be consistently around 0.9% for almost all the Class F fly ashes with a single exception. Similar to the sulfate content, the magnesium content of No.14 Zimmer is far higher than usual, 4.8% compared to 0.9% for other Class F fly ashes studied here. f) The loss-on-ignition values of all the Class F fly ashes in this study ranged between 1.4% and 2.4%. The results for X-ray diffraction were presented for each fly ash in Chapter 3. The XRD patterns for fly ashes vary somewhat with the variations in the chemical characteristics discussed previously in this chapter. A few unusual crystalline components were detected corresponding to unusual chemical compositions, for example, magnetite (Fe 3O 4) is identified on the XRD pattern of No.2 Edwards, which is not usual for a Class C fly ash. Similarly, Lime (CaO) is detected in No.10 Elmer Smith; it s high CaO content is unusual 9% as for Class F fly ash. As summarized above, it seems that the chemical parameters and crystalline components of the Class C and Class F fly ashes studied are different from each other, but most of them share common characteristics within their classification. However, when it comes to particle size distribution, which is also important, there are remarkable differences. The particle size distribution curves for Class C and Class F fly ashes in this study were characteristically different from each other. For the Class C fly ashes, the percentage of particles smaller than 1 μm mostly ranges in 25 ± 3%, except for low values of 20% for No. 7 Schafer and 17% for No.17 Rockport. The mean particle size for the Class C ashes was typical 9 ± 2μm, with a single exception of 15μm for No.17 Rockport. Moreover, the content of oversize material (>45μm), another important indicator regarding particle size distribution, was found to be quite consistent for these fly ashes, within the range of 13 ± 5%. The oversized material content was a little higher for No. 15 Rockport with the value of 25%. According to ASTM C 618, maximum permissible content retained on the 45 m sieve is 34% for both Class C and Class F fly ashes. All of the fly ashes met this requirement without. For Class F fly ashes, the percentage of particles smaller than 1 m appeared to be less than those for Class C fly ashes however with quite consistent, being 11 ± 1% for all Class F fly ashes except No.10 Elmer Smith, for which the value is only 7%. The mean particle size for the Class F fly ashes was 18 ± 2 m. Finally, the content of oversize material (>45 m) for all the Class F fly ashes have a value of 21 ± 3%. When compared this value with that of the Class C fly ashes, the difference for the average content of oversize material seems noticeable. However, with respect to 145

146 certain individual fly ashes, it is inappropriate to judge the fineness of the fly ash from the oversize material content indicator. For example, the content of oversize material for No.6 Miller is 19% and for No.14 Zimmer is 18%. However, the latter is actually a significantly coarser ash than the former fly ash, because of the very different particle size distribution for those particles smaller than 45 m. Finally, almost all the results of strength activity index at 7 and 28 days of fly ashes meet the requirement specified in ASTM C 618, except that the strength activity index at 7 days for No.14 Zimmer, was only 70% compared to the required minimum value of 75%. While the chemical characteristics of this fly ash are exceptional in the content of MgO and SO 3, the results of the particle size distribution indicate that No.14 Zimmer is in fact a relatively fine Class F fly ash compared to others. The possible influence factors of strength activity index required further study. However, it should be noted that at 28 day, the strength activity index of No.14 Zimmer is 96%; all the others exceed 100%. To sum up, (1) it appears that Class C fly ashes constitute a large proportion of all the fly ashes available for use in Indiana. (2) The majority of the Class C and Class F examined in this study have a consistent chemistry within their respective classes, except for a few exceptions, which might require attention and further study. (3) The fly ashes of each class are relatively consistent; the Class C ashes are significantly finer than the Class F ashes and are found to vary not much in particle size distribution. Neither have appreciable content of oversize materials. The strength activity index test is the only test performed in relation to cement in this study, showed that all except one of the fly ashes meet the strength requirement specified in ASTM C 618, and would be expected to be more or less satisfactory in concrete. SECTION III CONCLUSIONS A total of 20 fly ashes, mostly from INDOT s list of approved pozzolanic materials, have been studied and characterized to provide updating information on the basic physical and chemical characteristics of fly ashes available to INDOT and to the industry in Indiana. The following conclusions are drawn from examinations from this study: 1. Compared to the fly ashes available in Indiana in the 1980s, the proportion of Class C fly ash is currently much higher. 2. The two classes of fly ashes each show consistent chemical compositions with a few exceptions. Typically, for Class C fly ashes, compositional parameters include: a) a combined contents of silicon, aluminum and iron oxides ranging from 56 to 65%, b) iron oxide content varying very little from the typical content of 6% except for one ash, c) typical CaO contents of 22 to 26% for the majority, d) moderate total alkali contents of around 2% for most; with almost none of the alkalis soluble, e) sulfate contents below 2.7%. 146

147 Similarly, the chemical composition characteristics for Class F fly ashes could be summarized as follows: a) a combined contents of silicon, aluminum and iron oxides ranging from 81 to 91%, b) most iron oxide contents ranging from 18 to 25%, with two fly ashes close to 5%, c) typical CaO contents below 5% with one exception, d) consistent alkalis content around 2.3%, e) SO 3 contents vary in a broad range from negligible (0.2%) to 3.1%. 3. The particle size distribution results seem consistent within each of the Class C ash and Class F ash groups. The percentage of particles smaller than 1 m found in Class C fly ashes is typically 25 ± 3% but only 11 ± 1% for Class F fly ashes. The content of oversize material (>45 m) in the Class C fly ashes is 13 ± 5% but for the Class F fly ashes, it is 21 ± 3%. For Class C fly ashes, 50% by weight of is smaller than a mean size of 9 ± 2 m; for the Class F fly ashes, 50% by weight of the particles are smaller than 18 ± 2 m. The difference in the mean size between the graphs is highly significant. 4. The results from strength activity index indicate one fly ash, No.14 Zimmer did not meet the requirement specified in ASTM C 618 and thus is not recommended to use in concrete. The data provided in this report concentrated on the chemical and physical characteristics of fly ash. Further research involving both fly ash and cement would be required in order to develop a model that will allow for more optimal selection of fly ash for use in a multi-component binder system SECTION IV FLY ASH DATA SHEETS This section contains the data sheets (physical and chemical analysis reports) provided by the testing labs contracted by the ash suppliers for all but three (Miller, Kenosha and Joppa) of the fly ashes used in the project.., 147

148 Analytical Testing Service Laboratories, Inc. P.O. Box 1118, Joplin, Missouri (417) Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI June 14, 2006 Attn:Donna Re: Baldwin Unit 3 Fly Ash Sample 2000 Ton Composite - 05/01-05/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 10.30% Moisture Content 3% Max 0.07% **** Specific Gravity 2.72 Specific Gravity Variation 5% Max 1.36% Loss on Ignition 6% Max 0.23% Soundness 0.8% Max 0.02% S.A.I., 7 Days 75% Min 94.70% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si02 **** 34.34% Aluminum Oxide AI2O3 **** 21.31% Ferric Oxide Fe203 **** 6.44% Total 50% Min 62.09% Sulfur Trioxide S03 5% Max 2.05% **** Calcium Oxide CaO 25.60% **** Magnesium Oxide MgO 5.55% Available Alkalies as Na20 **** 1.33% We certify the above wasjested in accordance with ASTM C-618. Analytical Testing Service Laboratories, Inc. ~~. John K. Cupp, Manager 148

149 Analytical Testing Service Laboratories, Inc. P.O. Box 1118,Joplin, Missouri (417) Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI June 16, 2006 Attn: Donna Re: Baldwin Unit 3 Fly Ash Sample 2000 Ton Composite - 05/07-12/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 10.60% Moisture Content 3% Max 0.06% **** Specific Gravity 2.70 Specific Gravity Variation 5% Max 0.56% Loss on Ignition 6% Max 0.21% Soundness 0.8% Max 0.02% S.A.I., 7 Days 75% Min 98.60% SAI., 28 Days 75% Min % Water Req. % Control 105% Max 93.40% Silica Si02 **** 34.00% Aluminum Oxide AI2O3 **** 21.41% Ferric Oxide Fe203 **** 6.29% Total 50% Min 61.70% Sulfur Trioxide S03 5% Max 1.43% **** Calcium Oxide CaO 26.88% **** Magnesium Oxide MgO 5.39% Available Alkalies as Na20 **** 1.28% We certify the above wasjested in accordance with ASTM C-618. Analytical Testing Service Laboratories, Inc. ~~- John K. Cupp, Manager 149

150 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI June 23, 2006 Attn: Donna Re: Baldwin Unit 3 Fly Ash Sample 2000 Ton Composite - 05/15-19/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 12.50% Moisture Content 3% Max 0.05% **** Specific Gravity 2.69 Specific Gravity Variation 5% Max 0.07% Loss on Ignition 6% Max 0.25% Soundness 0.8% Max 0.02% S.A.I., 7 Days 75% Min 96.40% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.40% Silica Si02 **** 31.82% Aluminum Oxide AI2O3 **** 22.61% Ferric Oxide Fe203 **** 6.29% Total 50% Min 60.72% Sulfur Trioxide S03 5% Max 1.39% **** Calcium Oxide CaO 26.88% **** Magnesium Oxide MgO 5.89% Available Alkalies as Na20 **** 1.48% We certify the above was.tested in accordance with ASTM C-618. Analytical Testing Service Laboratories, Inc. ~~John K. Cupp, Manager 150

151 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI July 5, 2006 Attn:Donna Re: Baldwin Unit 3 Fly Ash Sample 2000 Ton Composite - OS/22-26/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 M!:!sh) 34% Max 10.80% Moisture Content 3% Max 0.06% Specific Gravity Specific Gravity Variation 5% Max 0.93% Loss on Ignition 6% Max 0.67% Soundness 0.8% Max 0.01% S.A.I., 7 Days 75% Min 98.20% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si % Aluminum Oxide AI2O % Ferric Oxide Fe % Total 50% Min 66.49% Sulfur Trioxide S03 5% Max 1.76% Calcium Oxide CaO % Magnesium Oxide MgO % Available Alkalies as Na % We certify the above was tested in accordance with ASTM C-618..~ Analytical Testing Service Laboratories, Inc. ~~. John K. Cupp, Manager 151

152 PLANT: Baldwin LOI SEIVE MOISTURE DATE % % % 05/01/ /02/ /03/ /04/ /05/ /06/ /07/ /08/ /09/ /10/ /11/ /12/ /13/ /14/ /15/ /16/ /17/ /18/ /19/ OS/20/ OS/21/ OS/22/ OS/23/ OS/24/ OS/25/ OS/26/ OS/27/ OS/28/ OS/29/ /30/ /31/

153 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI July 07,2006 Attn:Donna Re: Edwards Fly Ash Sample Monthly Composite -May 2006 ASTM C-618 Class "C" Requirements Actual Fineness (+325 Mesh) 34% Max 8.90% Moisture Content 3% Max 0.14% **** Specific Gravity 2.63 **** Specific Gravity Variation 0.11% Loss on Ignition 6% Max 0.36% Soundness 0.8% Max 0.00% S.A.I., 7 Days 75% Min 94.40% SAI., 28 Days 75% Min 99.50% Water Req. % Control 105% Max 93.00% Silica Si02 **** 33.76% Aluminum Oxide AI2O3 **** 22.58% Ferric Oxide Fe203 **** 7.87% Total 50% Min 64.21% Sulfur Trioxide S03 5% Max 2.22% **** Calcium Oxide CaO 23.88% **** Magnesium Oxide MgO 5.14% Available Alkalies Na20 **** 1.36% We certify the above was tested in accordance with ASTM C-618 and AASHTO M295. 'T Analytical Testing Service Laboratories, Inc. ~~- John K. Cupp, Manager 153

154 PLANT: EDWARDS STATION UNIT LOI SEIVE MOISTURE DATE % % 05/01/ /02/ /03/ /04/ /05/ /08/ /09/ /10/ /11/ /12/ /15/ /16/ /17/ /18/ /19/ OS/22/ OS/23/ OS/24/ OS/25/ OS/26/ /30/ /31/

155 Analytical Testing Service Laboratories, Inc. P.o. Box 1118, Joplin, Missouri (417) Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI July 13, 2006 Attn: Donna Re: Hennepin Fly Ash Sample Ton Composite - 05/14-06/05/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 12.40% Moisture Content 3% Max 0.08% **** Specific Gravity 2.70 Specific Gravity Variation 5% Max 0.04% Loss on Ignition 6% Max 0.53% Soundness 0.8% Max 0.03% S.A.I., 7 Days 75% Min 98.60% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica SiO2 **** 34.02% Aluminum Oxide AI2O3 **** 21.25% Ferric Oxide Fe203 **** 6.15% Total 50% Min 61.42% Sulfur Trioxide S03 5% Max 1.79% **** Calcium Oxide CaO 26.31% **** Magnesium Oxide MgO 5.55% Available Alkalies as Na20 **** 1.45% We certify the above was tested in accordance with ASTM C-618. Analytical Testing Service Laboratories, Inc. ~~- John K. Cupp, Manager 155

156 PLANT: HENNEPIN 325 LOI SEIVE MOISTURE DATE % % 05/01/ /02/ /03/ /04/ /05/ /06/ /07/ /08/ /09/ /10/ /11/ /12/ /13/ /14/ /15/ /16/ /17/ /18/ /19/ OS/20/ OS/21/ OS/22/ OS/23/ OS/24/ OS/25/ OS/26/ OS/27/ OS/28/ OS/29/ /30/ /31/

157 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI June 14, 2006 Attn:Donna Re: Schahfer 15 Fly Ash Sample 2000 Ton Composite.- 04/29-05/05/06 ASTM C-618 Class "C" Requirements Actual Fineness (+325 Mesh) 34% Max 10.40% Moisture Content 3% Max 0.19% **** Specific Gravity 2.58 Specific Gravity Variation 5% Max 0.35% Loss on Ignition 6% Max 0.58% Soundness 0.8% Max 0.01% S.A.I., 7 Days 75% Min 91.20% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si02 **** 38.26% Aluminum Oxide AI2O3 **** 21.53% Ferric Oxide Fe203 **** 7.72% Total 50% Min 67.51% Sulfur Trioxide S03 5% Max 1.64% Calcium Oxide CaO **** 21.45% **** Magnesium Oxide MgO 4.56% Available Alkalies as Na20 **** 1.20% We certify the above was tested in accordance with ASTM C-618 and AASHTO M295. Analytical Testing Service Laboratories, Inc. ~~- John K. Cupp, Manager 157

158 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI June 16, 2006 Attn: Donna Re: Schahfer 15 Fly Ash Sample 2000 Ton Composite - 05/06-11/06 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 11.10% MoistureContent- 3% Max 0.15% **** Specific Gravity 2.53 Specific Gravity Variation 5% Max 1.46% Loss on Ignition 6% Max 0.38% Soundness 0.8% Max 0.00% S.A.I., 7 Days 75% Min 98.90% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si02 **** 39.21% Aluminum Oxide AI2O3 **** 20.84% Ferric Oxide Fe203 **** 6.86% Total 50% Min 66.91% Sulfur Trioxide S03 5% Max 1.51% Calcium Oxide CaO **** 22.17% **** Magnesium Oxide MgO 4.64% Available Alkalies as Na20 **** 1.15% We certify the above was tested in accordance with ASTM C-618 and AASHTO M295. Analytical Testing Service Laboratories, Inc. ~~- John K. Cupp, Manager 158

159 Analytical Testing Service Laboratories, Inc. P.o. Box 1118,Joplin, Missouri (417) Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI July OS, 2006 Atln: Donna Re: Schahfer 15 Fly Ash Sample 2000 Ton Composite - OS/20-25/06 ASTM C-618 Class "C" Requirements Actual Fineness (+325 Mesh) 34% Max 10.80% Moisture Content. 3% Max 0.06% **** Specific Gravity 2.59 Specific Gravity Variation 5% Max 0.93% Loss on Ignition 6% Max 0.67% Soundness 0.8% Max 0.01% S.A.I., 7 Days 75% Min 98.20% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si02 **** 36.34% Aluminum Oxide AI2O3 **** 22.71% Ferric Oxide Fe203 **** 7.44% Total 50% Min 66.49% Sulfur Trioxide S03 5% Max 1.76% **** Calcium Oxide CaO 22.02% **** Magnesium Oxide MgO 4.73% Available Alkalies as Na20 **** 1.18% We certify the above was tested in accordance with ASTM C-618 and AASHTO M295. Analytical Testing Service Laboratories, Inc. ~~ John K. Cupp, Manager 159

160 PLANT: Schahfer LOI SEIVE MOISTURE DATE % % % 05/01/ /02/ /03/ /04/ /05/ /06/ /07/ /08/ /09/ /10/ /11/ /12/ /13/ /14/ /15/ /16/ /17/ /18/ /19/ OS/20/ OS/21/ OS/22/ OS/23/ OS/24/ OS/25/ OS/26/ OS/27/ OS/28/ OS/29/ /30/ /31/

161 Analytical Testing Service Laboratories, P.o. Box 1118,Joplin, Missouri (417) Inc. Headwaters Resourses, Inc 4043 N. Euclid Ave. Bay City, MI July 05,2006 Attn: Donna Re: Dynergy Midwest Gen. Vermilion Fly Ash Sample Monthly Composite --May 2006 ASTM C-618 Class "C" Reauirements Actual Fineness (+325 Mesh) 34% Max 6.40% Moisture Content 3% Max 0.12% **** Specific Gravity 2.69 Specific Gravity Variation 5% Max 2.04% Loss on Ignition 6% Max 0.26% Soundness 0.8% Max 0.02% S.A.I., 7 Days 75% Min 96.70% S.A.I., 28 Days 75% Min % Water Req. % Control 105% Max 93.00% Silica Si02 Aluminum Oxide AI2O3 Ferric Oxide Fe203 **** 34.52% **** 21.26% **** 6.44% Total 50% Min 62.22% Sulfur Trioxide S03 5% Max 1.96% **** Calcium Oxide CaO 26.03% **** Magnesium Oxide MgO 4.89% Available Alkalies Na20 **** 1.38% We certify the above was tested in accordance with ASTM C-618. Analytical Testing Service Laboratories, Inc. ~~. John K. Cupp, Manager 161

162 PLANT: VERMilliON loi SIEVE MOISTURE DATE % % % 05/01/ /02/ /03/ /04/ /05/ /08/ /09/ /10/ /11/ /12/ /15/ /16/ /17/ /18/ /19/ OS/22/ OS/23/ OS/24/ OS/25/ OS/26/ OS/29/ /30/ /31/

163 Lafarge North America Chicago Office W. Renwick Road Lockport, IL FLY ASH SOURCE: JOLIET COMPOSITE DATE: 29-Jun to 07-Jul-06 SAMPLE IDENTIFICATION: JLX SPECIFICATIONS ASTM C 618 AASHTO M 295 CHEMICAL ANALYSIS CLASS C CLASS C SiO 2 (silicon dioxide), % = Al 2 O 3 (aluminum oxide), % = Fe 2 O 3 (iron oxide), % = 6.63 SiO 2 +Al 2 O 3 +Fe 2 O 3, % = Min 50 Min CaO (calcium oxide), % = MgO (magnesium oxide), % = 6.02 SO 3 (sulfur trioxide), % = Max 5.0 Max Moisture content, % = Max 3.0 Max Loss On Ignition, % = Max 5.0 Max Na 2 O (sodium oxide), % = 4.07 K 2 O (potassium oxide), % = 0.49 PHYSICAL ANALYSIS Fineness, amount retained on #325 sieve, % = Max 34 Max variation, points from average = -3 5 Max 5 Max Density, Mg/m 3 = 2.84 variation from average, % = 0 5 Max 5 Max Strength Activity Index with Portland Cement at 7 days, % of cement control = Min 75 Min Cement: Lafarge Alpena Type I/II Water Requirement % of cement control = Max 105 Max Soundness, autoclave expansion or contraction, % = Max 0.8 Max We hereby certify that the fly ash represented by the above chemical and physical analysis meets the requirements of ASTM C and AASHTO M ASTM C 618 Note 1 - Finely divided materials may tend to reduce the entrained air content of concrete. Hence, if a mineral admixture is added to any concrete for which entrainment of air is specified, provision should be made to ensure 8/10/2006 that the specified air content is maintained by air content tests and by use of Brian Borowski Report Date additional air-entraining admixture or use of an air-entraining admixture in Quality Assurance Manager combination with air-entraining hydraulic cement. Lafarge North America E-copy 163

164 Lafarge North America Chicago Office W. Renwick Road Lockport, IL FLY ASH SOURCE: ROCKPORT 1 COMPOSITE DATE: 3-Jun to 08-Jun-05 SAMPLE IDENTIFICATION: RP SPECIFICATIONS ASTM C 618 AASHTO M 295 CHEMICAL ANALYSIS CLASS C CLASS C SiO 2 (silicon dioxide), % = Al 2 O 3 (aluminum oxide), % = Fe 2 O 3 (iron oxide), % = 5.95 SiO 2 +Al 2 O 3 +Fe 2 O 3, % = Min 50 Min CaO (calcium oxide), % = MgO (magnesium oxide), % = 3.72 SO 3 (sulfur trioxide), % = Max 5.0 Max Moisture content, % = Max 3.0 Max Loss On Ignition, % = Max 5.0 Max Na 2 O (sodium oxide), % = 1.71 K 2 O (potassium oxide), % = 1.14 PHYSICAL ANALYSIS Fineness, amount retained on #325 sieve, % = Max 34 Max variation, points from average = -2 5 Max 5 Max Density, Mg/m 3 = 2.56 variation from average, % = 0 5 Max 5 Max Strength Activity Index with Portland Cement at 7 days, % of cement control = Min 75 Min Cement: Lafarge Alpena Type I/II Water Requirement % of cement control = Max 105 Max Soundness, autoclave expansion or contraction, % = Max 0.8 Max We hereby certify that the fly ash represented by the above chemical and physical analysis meets the requirements of ASTM C ASTM C 618 Note 1 - Finely divided materials may tend to reduce the entrained air content of concrete. Hence, if a mineral admixture is added to any concrete for which entrainment of air is specified, provision should be made to ensure 7/29/2005 that the specified air content is maintained by air content tests and by use of Brian Borowski Report Date additional air-entraining admixture or use of an air-entraining admixture in Quality Assurance Manager combination with air-entraining hydraulic cement. Lafarge North America E-copy 164

165 Lafarge North America Chicago Office W. Renwick Road Lockport, IL FLY ASH SOURCE: WILL COUNTY COMPOSITE DATE: 8-Jun to 07-Jul-06 SAMPLE IDENTIFICATION: WC SPECIFICATIONS ASTM C 618 AASHTO M 295 CHEMICAL ANALYSIS CLASS C CLASS C SiO 2 (silicon dioxide), % = Al 2 O 3 (aluminum oxide), % = Fe 2 O 3 (iron oxide), % = 6.35 SiO 2 +Al 2 O 3 +Fe 2 O 3, % = Min 50 Min CaO (calcium oxide), % = MgO (magnesium oxide), % = 5.66 SO 3 (sulfur trioxide), % = Max 5.0 Max Moisture content, % = Max 3.0 Max Loss On Ignition, % = Max 5.0 Max Na 2 O (sodium oxide), % = 2.88 K 2 O (potassium oxide), % = 0.38 PHYSICAL ANALYSIS Fineness, amount retained on #325 sieve, % = Max 34 Max variation, points from average = -2 5 Max 5 Max Density, Mg/m 3 = 2.84 variation from average, % = 0 5 Max 5 Max Strength Activity Index with Portland Cement at 7 days, % of cement control = Min 75 Min Cement: Lafarge Alpena Type I/II Water Requirement % of cement control = Max 105 Max Soundness, autoclave expansion or contraction, % = Max 0.8 Max We hereby certify that the fly ash represented by the above chemical and physical analysis meets the requirements of ASTM C and AASHTO M ASTM C 618 Note 1 - Finely divided materials may tend to reduce the entrained air content of concrete. Hence, if a mineral admixture is added to any concrete for which entrainment of air is specified, provision should be made to ensure 8/7/2006 that the specified air content is maintained by air content tests and by use of Brian Borowski Report Date additional air-entraining admixture or use of an air-entraining admixture in Quality Assurance Manager combination with air-entraining hydraulic cement. Lafarge North America E-copy 165

166 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Labadie th Street, Riverview, FL Class of Fly Ash: C Phone: (813) Sample Date: 7/25/05 to 7/29/05 Fax: (813) Date of Report: 10/6/2005 AASHTO-M Requirements for Class C ASTM C-618 Requirements for Class C Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 17.3 % 3% Max 3% Max 0.23 % ***** ***** % Max 6% Max 0.39 % 0.8% Max 0.8% Max 0.04 % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 93.0 % 75% Min 75% Min % 105% Max 105% Max 95.9 % Silica SiO2 ***** ***** % Aluminum Oxide Al2O3 ***** ***** % Ferric Oxide Fe2O3 ***** ***** 4.71 % Total 50% Min 50% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 2.64 % ***** ***** % ***** ***** 5.30 % We certify that all above test were done in accordance with ASTM C-618 * Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. CEMEX USA, Tampa Technical Center Hugh H. Wang, Ph.D Hugh H. Wang, Ph.D Corporate Technical Director 166

167 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Mill Creek th Street, Riverview, FL Class of Fly Ash: F Phone: (813) Sample Date: 9/1/05 to 9/29/05 Fax: (813) Date of Report: 12/13/2005 AASHTO-M Requirements for Class F ASTM C-618 Requirements for Class F Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 16.8 % 3% Max 3% Max 0.37 % ***** ***** % Max 6% Max 2.36 % 0.8% Max 0.8% Max % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 79.8 % 75% Min 75% Min 86.2 % 105% Max 105% Max 96.7 % Silica SiO2 ***** ***** % Aluminum Oxide Al2O3 ***** ***** % Ferric Oxide Fe2O3 ***** ***** % Total 70% Min 70% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 1.20 % ***** ***** 5.28 % ***** ***** 0.92 % We certify that all above tests were done in accordance with ASTM C-618 * Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. CEMEX USA, Tampa Technical Center Waltter Lopez, Ph.D. Waltter Lopez, Ph.D. Product Development Manager 167

168 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Petersburg th Street, Riverview, FL Class of Fly Ash: F Phone: (813) Sample Date: June Fax: (813) Date of Report: 8/25/2006 AASHTO-M Requirements for Class F ASTM C-618 Requirements for Class F Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 19.9 % 3% Max 3% Max 0.43 % ***** ***** % Max 6% Max 1.37 % 0.8% Max 0.8% Max 0.01 % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 81.7 % 75% Min 75% Min 89.9 % 105% Max 105% Max 94.2 % Silica SiO2 Aluminum Oxide Al2O3 Ferric Oxide Fe2O3 Total ***** ***** % ***** ***** % ***** ***** % 70% Min 70% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 0.96 % ***** ***** 1.79 % ***** ***** 0.78 % Available Alkalies Na20 1.5% Max ***** 0.98 % *Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. Cemex hereby certifies that this fly ash meets or exceeds the chemical and physical specifications of: X X ASTM C-618 for class f fly ash AASTHO M-295 for class f ash CEMEX USA, Tampa Technical Center Waltter Lopez, Ph.D. Waltter Lopez, Ph.D. Product Development Manager Cell: (813)

169 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Petersburg Unit # th Street, Riverview, FL Class of Fly Ash: F Phone: (813) Sample Date: 9/28/05 to 10/13/05 Fax: (813) Date of Report: 12/13/2005 AASHTO-M Requirements for Class F ASTM C-618 Requirements for Class F Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 21.4 % 3% Max 3% Max 0.46 % ***** ***** % Max 6% Max 1.23 % 0.8% Max 0.8% Max % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 81.5 % 75% Min 75% Min 88.2 % 105% Max 105% Max 96.7 % Silica SiO2 ***** ***** % Aluminum Oxide Al2O3 ***** ***** % Ferric Oxide Fe2O3 ***** ***** % Total 70% Min 70% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 0.86 % ***** ***** 1.26 % ***** ***** 0.73 % We certify that all above tests were done in accordance with ASTM C-618 * Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. CEMEX USA, Tampa Technical Center Waltter Lopez, Ph.D. Waltter Lopez, Ph.D. Product Development Manager 169

170 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Rush Island th Street, Riverview, FL Class of Fly Ash: C Phone: (813) Sample Date: 9/25/05 to 9/30/05 Fax: (813) Date of Report: 12/13/2005 AASHTO-M Requirements for Class C ASTM C-618 Requirements for Class C Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 27.4 % 3% Max 3% Max 0.36 % ***** ***** % Max 6% Max 0.25 % 0.8% Max 0.8% Max 0.05 % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 91.1 % 75% Min 75% Min 96.1 % 105% Max 105% Max 95.9 % Silica SiO2 ***** ***** % Aluminum Oxide Al2O3 ***** ***** % Ferric Oxide Fe2O3 ***** ***** 5.26 % Total 50% Min 50% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 2.34 % ***** ***** % ***** ***** 6.18 % We certify that all above tests were done in accordance with ASTM C-618 * Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. CEMEX USA, Tampa Technical Center Waltter Lopez, Ph.D. Waltter Lopez, Ph.D. Product Development Manager 170

171 Fly Ash Physical & Chemical Analysis Report Database ID Number: Cemex USA, Tampa Technical Center Fly Ash Source: MRT Trimble Co th Street, Riverview, FL Class of Fly Ash: F Phone: (813) Sample Date: September '05 Fax: (813) Date of Report: 12/13/2005 AASHTO-M Requirements for Class F ASTM C-618 Requirements for Class F Actual Fineness Retained (+325 Mesh) Moisture Content Specific Gravity Loss on Ignition Soundness 34% Max 34% Max 22.6 % 3% Max 3% Max 0.62 % ***** ***** % Max 6% Max 1.89 % 0.8% Max 0.8% Max % S.A.I., 7 Days* S.A.I., 28 Days* Water Req. % Control 75% Min 75% Min 79.6 % 75% Min 75% Min 86.3 % 105% Max 105% Max 96.7 % Silica SiO2 ***** ***** % Aluminum Oxide Al2O3 ***** ***** % Ferric Oxide Fe2O3 ***** ***** % Total 70% Min 70% Min % Sulfur Trioxide SO3 Calcium Oxide CaO Magnesium Oxide MgO 5% Max 5% Max 0.99 % ***** ***** 2.50 % ***** ***** 0.86 % We certify that all above tests were done in accordance with ASTM C-618 * Meeting the 7 or 28 day Strength Activity Index will indicate specification compliance. CEMEX USA, Tampa Technical Center Waltter Lopez, Ph.D. Waltter Lopez, Ph.D. Product Development Manager 171