Rebelo Jonathan 201406 MASc Thesis PDF
Rebelo Jonathan 201406 MASc Thesis PDF
Rebelo Jonathan 201406 MASc Thesis PDF
by
Jonathan Rebelo
Jonathan Rebelo
Civil Engineering
University of Toronto
2014
Abstract
The purpose of this research was to determine the accuracy of two test methods used in
measuring the water to cement ratio (w/c) of fresh and hardened concrete. The microwave oven
test based on a current ASTM Draft was used in determining the w/c of fresh concrete while the
modified Norwegian PF-method was used to determine the w/c of hardened concrete. The
microwave oven evaporates the water of a 1500 gram sample of fresh concrete to determine a
w/c and can accurately measure the w/c within 0.05 of the true value. The modified PF-method
uses an absorption method similar to ASTM C97 and Powers’ hydrations models to determine
the w/c of hardened concrete. 100mm diameter concrete cores were prepared from slabs and
50mm thick concrete cylinders were tested. The results from this hardened concrete test had a
ii
Acknowledgments
I would like to thank my supervisor, Professor R. Doug Hooton, for his support and guidance and
for giving me the opportunity to conduct this research. I would also like to give a special thanks
to Olga Perebotova for her help within the laboratories and a special thanks to Ardavan, Eric, and
Majella for all their help.
I would also like to thank the Industrial Research Chair of the Natural Sciences and Engineering
Research Council of Canada and the Cement Association of Canada (NSERC/CAC) for their
financial support. In addition, I thank Holcim Canada, CBM Aggregates, and Euclid Chemical
for generously supplying all the concrete materials used.
I would like to acknowledge my parents for supporting me during my academic studies and to
thank all my close friends who have supported me along the way; it was much appreciated.
iii
Table of Contents
Acknowledgments.......................................................................................................................... iii
Chapter 1 ......................................................................................................................................... 1
1 Introduction ................................................................................................................................ 1
Chapter 2 ......................................................................................................................................... 4
iv
3.2 Materials ........................................................................................................................... 26
vi
List of Tables
Table 3.1: Cement Chemical Analysis .......................................................................................... 26
Table 4.1: Hand Batched Mix Designs for Preliminary Microwave Testing ............................... 50
Table 4.9: Phase Two ASTM Draft vs Extended Drying Regime effects on W/C ...................... 56
Table 4.10: Phase Three Microwave Specific Mix Design Summary .......................................... 57
Table 4.13: Phase Three ASTM Draft vs Extended Drying Regime Effects on W/C .................. 59
vii
Table 4.16: Modified Test Trial 1 for W/C=0.402 ....................................................................... 63
Table 4.17: Summary of Modified Test Trial 1 Results for W/C=0.402 ...................................... 64
Table 4.19: Summary of Modified Test Trial 2 Results for W/C=0.405 ...................................... 65
Table 4.20: Repeat Testing of Trial 2 with Induced Micro-Cracks for W/C=0.405 .................... 65
Table 4.23: Finalized PF-Method Testing for Concrete with W/C=0.412 ................................... 68
Table 4.25: Batch Mass Summary for Phase One Mixes ............................................................. 74
viii
Table 4.36: C-0.65 Average W/C Results .................................................................................... 84
Table 4.52: Percent Error for Low W/C Concretes .................................................................... 106
Table 4.53: Percent Error in Estimation of W/C for Hardened Concrete in Phase One ............. 107
ix
List of Figures
Figure 2-1: Structural and Physical Properties of Hardened Portland Cement Paste (Neville,
2010) ............................................................................................................................................... 5
Figure 2-2: Relation Between Strength of Concrete and Water Content (Abrams, 1919) ............. 6
Figure 2-3: Nomograph Used to Determine the W/C for a Target Compressive Strength
(Teychenne, 1997) .......................................................................................................................... 8
Figure 2-4: Sellevold's Paste Porosity as a Function of W/C and Hydration (Sellevold, 2005)... 22
Figure 3-5: Ultimate Degree of Hydration Curve Based on R.H. Mills’ Model .......................... 43
Figure 3-6: Simulated and Measured Degree of Hydration from Cement # F (Meyer, 2009) ..... 44
Figure 3-7: Simulated and Measured Degree of Hydration for Cement #A (Meyer, 2009) ......... 45
Figure 4-2: Water Uptake Over Time for Samples Cast on November 28th ................................ 69
Figure 4-3: November 28th Water Saturation Duration for 0.453 W/C Concrete ........................ 69
Figure 4-4: Water Uptake Over Time for Samples Cast on January 14th .................................... 70
Figure 4-5: January 14th Water Saturation Duration for 0.453 W/C Concrete ............................. 70
Figure 4-7: Measured W/C Distribution for Phase One Concrete ................................................ 90
x
Figure 4-8: Graphical Representation of the Effects of Cylinder Location in Phase Two ......... 101
Figure 4-9: Graphical Representation of Concrete Core vs. Cylinders ...................................... 103
Figure 4-10: Average W/C Results for All Cores and Cylinders ............................................... 104
Figure 4-11: Measured W/C Distribution for Phase Two Concrete ........................................... 105
Figure 4-12: Percent Error for Low W/C Concretes ................................................................... 106
Figure 4-13: Percent Error in Phase One for Varying W/C ........................................................ 107
Figure 4-14: Optical Aid in Determining the W/C of Hardened Concrete Using Equation [3-15]
..................................................................................................................................................... 109
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1
Chapter 1
1 Introduction
1.1 Water to Cement Ratio: Background
Changes in the water to cement ratio (w/c) of concrete can greatly influential the strength and
durability of concrete elements (Abrams, 1919). When comparing two concrete mix designs
with similar mix proportions, the one with the lower w/c will generally be stronger and less
permeable than the higher w/c concrete. In 1919, Duff Abrams deduced that the modification of
the w/c ratio of a concrete sample had the largest contributor to the compressive strength of the
sample (Abrams, 1919). This relationship was so powerful that Abrams and Powers both
derived equations estimating the compressive strength of concrete based on w/c (Mehta, 1986).
Therefore, when designing concrete, a firm understanding of the w/c must be known.
The addition of water to the calcium silicates and aluminates found in standard Portland cement
form hydration products that harden over time and provide the structural and durability
properties of cement paste (Neville, 2010). When cement is mixed with water, the cement
particles begin to hydrate. Large calcium hyrdoxide cystals and smaller fibrous calcium silicate
begin to form, which then grow larger and eventually interconnect with other hydrates, where
they grow even larger forming a dense matrix of hydration products. As the matrix further reacts
the hydrates occupy more of the aqeuous space and reduces the sample’s overall porosty (Mehta,
1986).
In general, concrete with a higher porosity will result in poorer performance as compared to a
lower porosity concrete with similar mix proportions. As more water is added to cement, the
particles get spaced further apart, causing a lower concentration of cement grians thoughout the
medium. This increases the distance required for the prismatic hydration products to intersect
each other, casuing larger voids between cyrstals; therefore, increasing the porosity (Neville,
2010). Since voids do not contibrute to strength, a more porous concrete will have a lower
structural capacity compared to a denser concrete. In addition, higher porosity concrete are more
suseptable to chemical attack. Monitoring the w/c of concrete is one way of controlling its
permeability (Abrams, 1919).
2
Concrete is normally ordered with a target slump range to allow for proper placement of the
material. Before the advent of water-reducing admixtures, water was primarily added to increase
the slump of concrete to increase workability; however, this increased the overall w/c of
concrete; weakening the concrete strength and performance. In current common practice, low
w/c mix designs include water-reducing admixtures to achieve a proper slump range while
maintaing its high strength and performance requirements. Unfortunately, from visual inspection
of both fresh and hardened concrete, it is difficult to distingush concrete made with a low w/c
with water-reducers from a concrete with a higher w/c without water reducers. Therefore, a test
to accurately measure the w/c of fresh and hardened concrete is required.
Currently, accelerated compressive strength tests are used for determining the quality of
concrete; however, by the time these tests are complete, the concrete will have hardened and if
the performance criteria are not met, it may need to be removed or remedied. This may cause
large lawsuits, loss of money and delayed schedules. Therefore, determining the w/c of fresh and
hardened concrete could be very useful in ensuring a specific level of quality and to estimate its
potential strength and durability.
3
Currently, the ASTM C09 committee on concrete has created a draft for the microwave oven
test, however it has not receive full technical committee approval. This project is designed to
provide additional research for the adoption of this test as a standard. Various concrete mixes
were tested using the procedure outlined in the ASTM draft to measure the accuracy of the
measured w/c as compared to the designed value. Alternative procedures were evaluated to
improve the efficiency of this test method.
The hardened test expands on the work completed by Erik J. Sellevold at the Norwegian
University of Science and Technology (Sellevold, 2005). It combines his use of Powers’
hydration models (Powers, 1968) and the procedure outlined in the PF-method created by
Vuorinen in the 1970s to calculate the w/c of hardened concrete (Sellevold, 2005). Concrete
cylinders were batched with varrying w/c and slag replacement precentages to see if this method
can accuraetly estimate the w/c of hardened concretes. Cores from slabs were also used to better
mimic field results.
4
Chapter 2
2 Literature Review
This literature review first discusses the effects of w/c versus strength and durability, as both
properties are strongly related to each other. Following is a brief overview of how concrete is
designed in the concrete industry and how unaccounted water can be added during the
manufacturing, transportation, and placement of concrete. A discussion about past and current
methods used to determine the w/c of fresh concrete follows, including the history of the
microwave oven test and where it stands currently in the industry. A brief evaluation of current
methods used to measure the w/c of hardened concrete follows with an in-depth analysis of the
modified PF-method that Sellevold used to estimate the w/c of hardened concrete (Sellevold,
2005).
S = Soe-kp [2.1]
Where So is the strength at zero porosity, and k is a constant determined for each material
(Mehta, 1986). In general, this formula applies to most homogenous solid materials such as iron,
plaster of Paris, autoclaved cement, aggregates, etc.
Powers understood this principle and tested the 28 day compressive strengths of three different
mortars with varying porosities. Figure 2-1 shows his findings as published in the Journal of
American Ceramic Society in 1958 (Neville, 2010).
5
Figure 2-1: Structural and Physical Properties of Hardened Portland Cement Paste
(Neville, 2010)
As observed in Figure 2-1, Powers derived a formula for the compressive strength (fc) from the
line of best fit; his equation is similar to the fundamental relationship between strength and
porosity as described in Equation [2.1].
fc = a x3 [2.2]
Where a is the strength of the material at zero porosity and x is the ratio of solid material to the
total space of the sample. In Figure 2-1, the gel/space ratio represents x and a was determined as
234MPa (34,000 psi). Therefore the line of best fit is:
fc = 234(1-p)3 (MPa) [2.4] ,where p represents the porosity of the mortar sample
6
The importance of Equation [2.4] and Figure 2-1 were to show the strong relationship between
the porosity and compressive strength of cement pastes. In general, as porosity decreases,
strength will increase and as porosity increases the strength decreases.
In 1918, Abrams completed a study to determine the strength capacity of various concrete mixes
at the Structural Materials Research Laboratory, Lewis Institute in Chicago. Abrams completed a
total of 50,000 tests in a three year period of which a large portion of these tests were
compression tests of concrete and mortar. The three main factors were considered: the mix
water; the size and gradation of aggregates; and cement content. From their results, they
concluded that the most influential design condition was the water content (Abrams, 1919). As
long as aggregates were not structurally defective and were clean, changes to the aggregate
content or overall density had very minimal effect in comparison to small changes to the w/c.
Abrams concluded: when given sufficient water to create workable mixes, the water content of a
concrete mix design was the main contributor to strength development (Abrams, 1919). Abrams
plotted his strength data for concretes in Figure 2-2 to compare the w/c to compressive strength
(Abrams, 1919).
Figure 2-2: Relation Between Strength of Concrete and Water Content (Abrams, 1919)
7
S= 14000/7x [2.5]
Where S was the compressive strength in pounds per square inch and x was the w/c. After further
analysis and modifications to Equation [2.5], Abrams created Equation [2.6] otherwise known
as: Abrams’ Water/Cement Ratio Rule.
(MPa) [2.6]
Where fc is the compressive strength of the concrete, w/c is the water cement ratio and k1 and k2
are constants dependent on the cement type, age of testing, curing regimes, etc. (Abrams, 1919).
The k1 and k2 constants were determined by performing calibration compression tests on similar
concrete. Much of Abrams work was spent maximizing the efficiency of concrete mixes to
reduce costs in the manufacturing (Abrams, 1919). By determining that the w/c ratio was one of
the largest contributors to the compressive strength, his universal equation could then be used to
simplify mix proportioning to achieve targeted compressive strengths (Banu, 1996). This led to
nomographs such as Figure 2-3 to be created to estimate the compressive strength of concretes
based on its designed w/c (Teychenne, 1997).
8
Figure 2-3: Nomograph Used to Determine the W/C for a Target Compressive Strength
(Teychenne, 1997)
In summary, as water content increases in concrete, the cement grains are spaced out further
resulting in a higher porosity. Pores can not withstand physical strain, therefore lowering the
overall strength capacity of the concrete as shown in Abrams’s law. In addition, as porosity
increases, concrete is more susceptible to ingress of aggressive chemicals and lowers the
durability.
will minimize production cost and do not disclose the mix design in order to protect their
competitive edge within the industry. Prescription-based specifies that the owner will assume
control of the concrete mix design, and will state the mix proportions per cubic meter. It is the
duty of the supplier to disclose all information and demonstrate that the concrete complies with
the mix design prescribed by the owner (CSA A23.1 Annex J, 2009).
As stated earlier, unless agreed upon in a performance-based contract, the concrete manufacturer
is not required to disclose the mix design to the recipient. The liability for the delivery and use of
inferior concrete would fall upon the manufacturer; however, it is difficult for an owner to
quantify the strength and durability of concrete without a mix design. The current method to
verify if the proper concrete is placed is to perform compressive strength tests of concrete
cylinders cast from the concrete batch. However, by the time the results are received the concrete
that was tested would have already been poured and hardened. If the concrete fails to meet the
performance requirements, costly remedial work may be required hindering the success of the
project, creating a legal dispute between the owner and the manufacture.
When using a prescriptive-based system, a full mix design would be available showing the
cement content, aggregate contents, aggregate natural moisture, and free water content. Both
systems have their advantages and disadvantages, but both must have quality control measures in
place to ensure quality concrete.
CSA A23.1 allows the addition of water to a concrete truck if the measured slump is
unsatisfactory for the placement of the material. Concrete placers are allowed to add up to 10%
additional mixing water, as long as it does not exceed the specified w/c (CSA A23.1 Annex J,
2009). As workability increases through the addition of water, the level of difficulty decreases
when placing fresh concrete; a concrete placing may purposely add water to a concrete mix to
eases their work. Without careful supervision of these actions, excessive water may be added,
reducing the overall performance of the concrete.
Unfortunately the water content of concrete arriving from a manufacturer may not always be the
same with what was defined by the batch sheet. During transportation concrete may stiffen;
resulting in a lowered workability. Truck drivers would ideally add chemical admixture to ensure
a proper slump, however, some may add water. It is quite difficult to notice what was added.
Another source of unaccounted water may be found from repeated use of the same concrete
truck. After a concrete truck has finished pouring its contents, water is used to wash the drum.
This process allows for large volumes of water to collect at the bottom of the drum. When
concrete trucks return to the plant to be loaded again, the volume of wash water remaining in the
drum must be accounted in the mix proportions; if neglected it will increase the overall w/c.
ASTMC94 (Standard Specification for Ready-Mix Concrete) states that wash water must be
measured prior to mixing, and if this measurement is impossible to retrieve, all the wash water
must be removed for an accurate total measurement of water to be made. In addition, chemical
admixtures, ice and any other additional water added including wash water must be measured
such that the total water content tolerance is within ±3% of the total amount of concrete.
From an economic standpoint, the cost of cement is considerably higher than it the cost of water;
in 2005 average mill price for US cement was around $84 per ton (EPA, 2013), while the 2012
industrial price of Toronto tap water was $1.90/ton (City of Toronto Council, 2012). It benefits a
manufacturer financially to reduce the use of cement and maximize the use of water, provided
they meet the specifications.
In summary, there are many ways water can be added to a concrete mix that could alter the
design specification of the concrete. This excess water could be added during manufacturing,
transport, or during placement. Therefore a test to measure the w/c of fresh and hardened
concrete is necessary in order to determine the true w/c of concrete.
11
The current ASTM C684 contains four methods for estimating the 28 day compressive strength
of accelerated cured concrete. This standard is the fastest available test method for determining
the strength performance of concrete and can be completed within two days of casting; however,
this is not a fresh concrete test and cannot prevent the use of inferior concrete (Ramme, 1987).
Therefore, other non-standardized test methods were analyzed.
The U.S. Army Corps of Engineers decided to implement this procedure in 1976; the Corps of
Engineers’ Seattle District Office and the Federal Highway Administration would transport all
12
the equipment necessary to operate these tests in two portable wooden trunks measuring 14” by
30” by 48”. The estimated cost in 1976 for fabrication of this equipment including labor and
material was $3,200 per unit and could be operated from the back of a pick-up truck (National
Technical Information Service, 1977). With a single operator this method could be completed in
a period of 10-15 minutes and was claimed to accurately identify the water content within 5
percent and from that determined 28 day strengths within 15 percent (National Technical
Information Service, 1977). Unfortunately, the US Army Corps discontinued the use of this test
due to the fragile glassware used in operation (Williamson, 1984), and ASTM C1079 was later
revoked as a standard in 1998.
1. Measure and tare the mass of a 0.01m3 plastic container with Plexiglas plate cover
2. Place a 10kg sample of fresh concrete in the container.
3. Fill the container with water until 0.5cm from the top rim.
4. Stir vigorously for 1-2 minutes to remove all air from the system.
5. Fill container completely with water and remove foam residue by sliding the Plexiglas
plate over the top of the container. Ensure all air is removed from under the Plexiglas
plate before continuing.
6. Measure the mass of the contents inside the 0.01m3 container.
13
To determine the underwater weight of concrete, the total mass from Step 6 was subtracted from
the total mass of water required to fill the 0.01m3 container (10kg). With the specific gravities of
the cement and aggregates, and the aggregate to cement ratio from the mix design, a w/c can be
determined using Equation [2.7] and [2.8] (Ramme, 1989).
|[ ] [ ]| [2.7]
Wa = the calculated mass of aggregate in the sample in air from mix design
Wcm = the calculated mass of cement in the sample in air from mix design
|[ ] [ ]| [2.8]
Laboratory test results showed a percent error of -15% to 8%, with a mean error of 6 percent
(Ramme, 1989). Additional testing showned that the natural moisture content of the aggregates
and specific gravity of the materials affect the overall calulcations substantially. Due to the
sensitivity to specific gravity values in the buoyancy method, the supplier data on bulk specific
gravity, percent absorption, and natural moisture contents were not accurate enough for this
testing and required independent testing to verify those values. This complicated the test
procedure, and lengthened it (Ramme, 1989). They started performing their own tests on
aggregates using a microwave oven to shorten the 110°C oven drying time from days to minutes
as outlined in ASTM C128 and C127.
The method purposed by Dunagan in 1930 (Allen, 1977) was slightly different than the method
purposed by Naik and Ramme. Dunagan used a 5kg sample of concrete and passed the coarse
and fine aggregates through a sieve to determine the aggregate contents. The accuracy of this
14
method for determining the mass of solid components (cement and aggregates) and the water
content of a 5kg sample was within ± 1 percent and ± 2 percent of the total concrete mass
respectively (Allen, 1977).
Prior to the use of the microwave oven to evaporate the water from fresh concrete, Naik used
hot-plates and conventional ovens, but these methods were too slow and helped facilitate the
hydration process and over time a portion of water would become non-evaporable water and
would lower the calculated w/c results. In addition, the time it took to evaporate all the water
using a hot plate was far too long for field use (Ramme, 1987). After using the microwave oven
to quickly evaporate the water from aggregates, it was then used to determine the water content
of fresh concrete.
Naik’s original experiment consisted of batching a 1500g sample in the lab, from which a
representative 1000g sample of the fresh concrete was then spread out thinly on a 30 cm
diameter microwave resistant glass plate. The sample was then placed in a microwave oven, and
every few minutes the sample was removed and stirred to expose trapped moisture within the
sample, and the mass measured. This process would continue until a constant mass was
determined (Ramme, 1987). The mass difference between the initial fresh concrete and the dried
concrete was considered to be the water content of the sample. Using the cement content from
the mix design, a w/c could be determined. Naik and Ramme used an Amana microwave for
their tests but the power rating was never stated (Ramme, 1987).
The first eight concrete mixes tested used 100% Portland cement with w/c ranging from 0.36-
0.73. The results varied with an error of +28% to -11%, with a mean error of 14% (Ramme,
15
1987). After re-analyzing their approach, they hand-mixed eight more samples in glass plates
used to dry the sample to know the exact mix proportions for each specimen. The average
percent error was 3.5% (Ramme, 1987). Another eight tests were done in this manner, but the
cement was eliminated. The percent error of this modification was 0.6% showing that most of
the water introduced in the system did evaporate. Two small controlled batches were hand
mixed, and allowed to stand for 30 minutes after mixing. A 2-4% increase in error was noted,
due to water evaporation after mixing, therefore, the test was recommended to be completed as
soon as the concrete was mixed (Ramme, 1987). In addition, the study showed that excessive
heating and energy level of the microwave oven had no further effects once the sample was fully
dried. Once the sample reached a constant mass, it was assumed that all the water had been
removed (Ramme, 1987). In all tests an aggregate moisture correction factor was applied, as the
microwave would evaporate the natural water content of the aggregates, which did not contribute
to the w/c of the concrete mix. This correction factor would use the mix design to determine the
mass of aggregates and determine the moisture contained within. This mass loss was subtracted
from the total mass loss to determine the free water of the mix.
In 1994, Nagi and Whiting revisited the work published by Naik and Ramme, and modified the
method to make it more field-worthy (Whiting, 1994). One noticeable difference is that they
changed the sample size to 1500 grams to better represent the concrete and they classified the
power setting of their microwave to 900Watts (Whiting, 1994). The concrete sample was
wrapped in a fiberglass cloth, placed on a glass tray immediately after mixing, and the initial
mass was measured. They initially dried the sample for a full 10 minutes, but realized the
concrete would become a dense mass with entrapped moisture at its center. A decision was made
to stop the microwave drying time at five minutes, while the concrete was still soft enough to
easily remove the course aggregate from the mortar exposing more surface area for drying. They
also took the mortar and ground it in a mortar and pestle. The sample was then placed back into
the microwave for another five minutes, taken out, weighed, placed back in the microwave for
another two minutes, and then the final mass was taken after a total of twelve minutes in the
microwave. The difference between the initial mass of the fresh concrete, and the mass after
twelve minutes of drying, was the total water loss of the sample (Whiting, 1994). An aggregate
correction factor was used in this method to account for the natural water absorbed by the
aggregates.
16
Fresh concrete samples were produced as part of a Strategic Highway Research Program (SHRP)
study. Most of the microwave oven results for determining the fresh w/c were taken from
concrete trucks designed for bridge deck overlay placement and concrete pavement section
repair. They used four types of concrete mixes with aggregate absorption values of 0.3%, 1.9%,
or 3.8%. They used conventional concrete with a moderate, high, and low slump mix by altering
the overall water content. They also tested silica fume, fly ash, and latex modified concrete.
After 12 minutes of drying in the microwave, the water recovery of these concrete types varied
between 91% and 97%; with latex modified concrete and fly-ash mixes having the lowest values
(Whiting, 1994). After evaluating these results, it was decided to extend the drying period to 14
minutes as the water recovery was too low with a 12 minute drying period (Whiting, 1994).
Therefore, the remaining test used an additional two minutes in the microwave, resulting in an
average error of only 3% (Whiting, 1994).
The North Dakota State Highway Department may have been one of the earliest organizations to
adopt the microwave oven test on projects in the field to determine the water content of fresh
concrete (Whiting, 1994). Although a current ASTM standard does not exist for this microwave
oven test, the American Association of State Highway and Transportaion Officals(AASHTO),
have standardized their own method as AASHTO T 318. This method is very similar to the one
outlined by Nagi and Whiting. The American Society of Testing and Materials (ASTM) are
developing the the microwave oven test which is based from the AASHTO T318 designation. A
brief summary of the procedure is as follows:
The water content is determined by first drying a sample of concrete to a moisture content of 0%
and then vacuum saturating the sample in a liquid of known density fill the capillary pores of the
sample. The volume of the capillary pores can be determined by measuring the mass increase of
the sample and dividing the density of the fluid (Buenfeld, 2009). The standard states that
concrete with visible signs of chemical or physical damage cannot be tested. Samples that are air
entrained, poorly compacted, or are older than five years cannot be tested (Neville, 2003).
According to the Concrete Society Technical Report, the average error in using this indirect
method to calculate the w/c is 0.1 from the actual w/c (Concrete Society, 1989). This value may
even be too conservative as other researchers feel that the degree of error is larger than 0.1 even
when performed by experienced analysts (St John, 1998).
18
For samples with a w/c lower than 0.5 a fluorescent liquid replacement method is used. The
sample preparation is very similar where a 40 x 20 x10 mm concrete sample is prepared and
glued to a glass slide; however, a less harsh drying procedure is used to prevent microcracks. The
sample is placed in a 70°C oven for 24 hours and then placed under water for 24 hrs. These steps
are repeated twice. The humidity of the sample is very important for the impregnation process
and is the leading driver for this procedure. Unfortunately concrete with low w/c can exhibit
signs of micro cracking, and if this is a concern, the drying stages can be neglected. The sample
is then placed face down in a container with fluorescent dye treated ethanol for four days,
removed and allowed to dry on a paper tissue overnight at room temperature. The sample is
lightly ground to remove excess dye. To fill larger air voids, the sample is placed in a vacuum
chamber for 20-30 seconds at 0.2 Bar subjected to a fluorescent epoxy treatment. The sample is
then placed in a plastic bag until the epoxy has hardened. The sample is then cut and ground to
0.025mm as described in the previous impregnation method (NT361, 1999).
Reference samples are made in a similar method to either impregnation method and are stored in
a dark room prior to comparison. These reference samples should have similar compositions to
the thin section but with known w/c of: 0.35, 0.4, 0.45, 0.5, 0.6, and 0.7. Once ready to examine,
19
the test samples are placed under the microscope and the fluorescent intensities are compared to
the reference samples. Once a match is determined, a new location on the test sample is picked
for analysis and the average of ten reference point comparisons is used to determine the w/c of
the sample.
This method can yield accurate results; however, the level of difficulty is high (Jakobsen, 2006).
The equipment and material needed can be expensive and tedious to execute properly. Learning
how to prepare the thin sections require training and supervision by skilled petrographers. These
procedures are very sensitive to the sample thickness, impregnation techniques, and
inconsistencies among petrographers lead to variations in determined w/c. With proper use of the
test method a standard deviation of 0.02-0.03 is possible when determining the hardened w/c of
concrete. (Jakobsen, 2006).
Alternative methods have been tested, such as using a scanning electron microscope to determine
the w/c of concrete. This test also uses epoxy impregnated samples but then bombarded the thin
sections with electrons to produce an image; the higher the atomic number, the darker the SEM
image appears (Sahu, 2004). The epoxy-impregnated pores appear dark while the cement paste is
brighter. By using reference materials and image analysis software a w/c can be determined. The
error in this technique can be comparable to standard deviations documented by the NT Build
361 method (Sahu, 2004).
Another back-scattered electron method has been used to determine the w/c of hardened concrete
and have yield errors within 0.025 of the actual water cement ratio (Buenfeld, 2009). This
method avoids the use of a reference materials by measuring the volume percent of unreacted
cement, hydration products and capillary pores using field emission scanning electron
microscopy in there backscatter mode. The cement content and free water content can then be
determined which yields the w/c (Buenfeld, 2009).
20
2.5.3 PF-Method
The PF-method was first developed by Vuorinen in the 1970’s in Finland as a test to verify the
frost resistance of concrete (Sellevold, 2005). The acronym of PF is derived from a Finnish word
“slyddportal” which translates roughly to the “protective pore ratio”. Vuorinen stated that a
concrete sample with a PF-value of 0.25 or greater would have a protective capability when
exposed to deicer salts during freeze-thaw cycles (Sellevold, 2005). The protective pores were
considered to be the air pores within concrete that would not normally be filled with water when
submerged in water. With the PF-value, concrete could then be classified for freeze thaw
resistance.
The PF-method is frequently used in Norway and is internally standardized at SINTEF (The
Foundation for Scientific and Industrial Research) in Trondheim but very minimal adoption of
this method has occurred elsewhere (Sellevold, 2005). The process outlined by Vuorinen is as
follows:
8. Pressure saturate the sample over night with at least 5MPa of water pressure
9. Measure mass of pressurized sample (WPRESSURE) as soon as possible to avoid water loss
With the mass measurements recorded in grams the PF-value could be determined using the
following formulas.
The porosity values are expressed in volume fractions of the total volume of the sample. In order
to obtain porosity in terms of paste volume the following was required:
Where Vp is the paste volume of the concrete sample. This paste volume can be determined
using the batch sheet of the concrete mix design, point counting methods, other forms of
microscopy, or assumed to be within a specific range given the concrete type (Sellevold, 2005).
The mass measurements were recorded in grams and the PF-value was determined using
Equation [2.14].
[2.14]
The PF-value would then be used to determine the frost resistance of a concrete sample.
Sellevold and Farstad conducted research at the Norwegian University of Science and
Technology and at the Norwegian Building Research Institute in Oslo, Norway on the validity of
the PF-method and conducted their own experiments to modify this method to determine the w/c
ratio of hardened concrete (Sellevold, 2005). By applying Powers’ models of cement paste
porosity and hydration kinetics, they developed a way to use the PF-method to not only measure
frost resistance of hardened concrete but also to determine the w/c of concrete (Sellevold, 2005).
Powers found that as cement hydrates, the water experiences a chemical shrinkage of 25.4%
when converted into chemically bound water (wn) (Powers, 1968). Powers derived Equation
[2.15] to express how the degree of hydration influenced the chemically bound water fraction. At
full hydration, the chemically bound water can be assumed to weigh 0.23g per gram of cement
(Powers, 1968).
𝛼 = wn / 0.23 [2.15]
22
By assuming that the paste volume will stay constant throughout the hydration process, Sellevold
deduced that the paste porosity (Ɛp) can be determined as a volume fraction of a concrete sample
as shown in Equation [2.17] (Sellevold, 2005).
ε p w c wn 0.254wn [2.16]
w c 1 3.15
ε p w c 0.172 [2.17]
w c 0.321
These equations are based on using a Portland cement with an absolute density of 3.15 and
Equation [2.17] is the main formula Sellevold uses in determining the w/c for hardened concrete.
Sellevold plotted Equation [2.17] and used his Figure 2-4 as a quick tool to calculate the w/c of
any given sample given estimates for the degree if hydration and paste content.
Figure 2-4: Sellevold's Paste Porosity as a Function of W/C and Hydration (Sellevold, 2005)
23
Sellevold conducted the PF-method to determine the suction porosity (Pa) of a sample and then
estimate a paste volume for the test specimen to determine the paste suction porosity (Ɛa). He
then equated the Ɛa to the total paste porosity (Ɛp) found in Figure 2-4 and with an estimation of
the degree of hydration; he determined the w/c of hardened concrete samples.
In an example illustrated in his 2005 paper, he estimated a realistic range for the degree of
hydration of cement in a 10 year structure to be between 0.65-0.85 (Sellevold, 2005). He
conducted the test using his estimated range for degree of hydration (𝝰) and noted that the
sensitivity of estimating the 𝝰 would only affect the results by a standard deviation of 0.02 from
the measured w/c (Sellevold, 2005). He also estimated a range for the paste volume to be 0.27-
0.31. Without knowledge of the mix design, he concluded a total standard deviation of 0.05 for
the calculated w/c can be expected when using the range for the paste volumes assumed above
(Sellevold, 2005).
Sellevold analyzed concrete using the PF-method on a Norwegian project. A total of 31 concrete
mixes were tested using different amounts of silica fume, and other binders. During the first
phase of the project, 17 concrete batches were tested, with a mean deviation of 0.02 w/c and the
remaining 14 batches in phase two of the project had a standard deviation of 0.05. In addition,
the values of the calculated w/c of these concrete better correlated to the 28 day strength tested,
showing some inconsistencies in the manufacturing process (Sellevold, 2005).
Sellevold’s method of estimating ranges for the degree of hydration and paste content (Sellevold,
2005) could be improved upon as other methods are available in determining these values. The
estimation of paste volume can be determined by a modified point count method similar to
ASTM C457 or from summing the volumetric quantities from a mix design, and R.H. Mills’
model for the ultimate degree of hydration can be used to estimate the degree of hydration of
concrete (Meyer, 2009).
The degree of hydration is largely influenced by the w/c of a concrete mix. In theory a w/c of 0.4
would allow for full hydration of cement; however, due to low internal relative humidity within
concrete the hydration is hindered. As cement hydrates it prevents the transport of water to
anhydrous cement particles (Meyer, 2009). R.H. Mills’ derived Equation [2.18] to better
represent the ultimate degree of hydration.
24
𝛼 [2.18]
If sufficient water was added during hydration then the limiting factor for practical degree of
hydration is the space required for hydration products (Byard, 2012).
𝛼 [2.19]
Therefore Sellevold’s Equation [2.17] could be modified to include a more realistic degree of
hydration based on Equation [2.18]. Equation [2.20] illustrates this.
Ɛp = [2.20]
Equation [2.20] takes into consideration a more realistic degree of hydration based on the w/c of
a given concrete sample. With a better estimate of the paste content, better estimates for w/c can
be made using Equation [2.20].
25
Chapter 3
3 Experimental Program
3.1 Introduction
This experimental program required the use of fresh and hardened concrete prepared at the
University of Toronto’s concrete laboratory. Fresh concrete samples were prepared as outlined in
ASTM C192, the Standard Practice for Making and Curing Test specimens in the Laboratory.
Once the mixing was complete, the slump (ASTM C143), density, and air content (ASTM C138)
tests were conducted. A high-range water reducer was added during mixing to achieve a
workable mix for proper placement during casting. The air content and measured density were
measured to calculate the yield of the concrete mix and to determine true paste content.
Directly after mixing, a fresh concrete sample was subjected to a testing procedure to determine
the w/c of the mix. During testing of the fresh concrete, cylinders were cast using pre-lubricated
100mm diameter by 200mm tall cylinder molds. In the later phases of this experimental
program, concrete slabs were cast using pre-lubricated wooden molds measuring 300mm x
200mmx 90mm. The concrete filled molds were then covered in a wet burlap cloth, followed by
a plastic sheet to maintain a moist environment. The following day, the samples were de-molded
and placed in a fog room, where the temperature was maintained at 23°C and 100% relative
humidity.
After a specified curing interval in the fog room, the concrete cylinders and slabs were then
prepared for use in the hardened concrete testing regime. At 28 days, concrete cylinders were
subjected to an uniaxial compression test (ASTM C39) to determine the compressive strength of
each mix design.
26
3.2 Materials
The materials used for batching included: CSA A3001 general use cement (GU), slag, water,
coarse and fine aggregate, and a high range water reducing admixture.
Physical properties for the slag were provided by Holcim Canada as is displayed in Table 3.2.
27
Physical Analysis
Residue 45 um (%) 1.37
Blaine (m2/kg) 668
Autoclave Exp. (%) 0.03
Air Content (%) 5.57
Compressive Strength
50:50 cement : slag
7 Day (MPa) 22.9
7 Day Slag Activity Index % 79.1
28 Day (MPa) 40.0
28 Day Slag Activity Index % 109.4
3.2.3 Aggregate
The fine aggregate was obtained from St. Marys Cement’s Sunderland quarry. The coarse
aggregate was delivered by Holcim Canada from their Milton quarry. The Ontario Provincial
Standard Specification for Material Specification for Aggregates (OPSS.MUNI 1002), outlines
the requirements for the fine and coarse aggregate gradation. Essentially, it defines the upper and
lower limits for gradation of aggregates used in concrete. For this project, a sieve analysis was
conducted for the aggregates used in the laboratory and compared to the OPSS.MUNI 1002
guidelines. Table 3.3 shows the sieve analysis of the fine aggregate and Figure 3.1 shows how it
compared to the OPSS grading envelope.
28
Sieve Size Percent Passing (%) Percent Retained (%) OPSS.MUNI 1002 (%)
80
60
40
20
0
1
Pan 2
75µm 3
150µm 4
300µm 5
600µm 6
1.18cm 7
2.36mm 8
4.75mm 9
9.5mm
Sieve Size
Upper Limit Fine Aggregate Gradration Lower Limit
Sieve Size Percent Passing (%) Percent Retained (%) OPSS.MUNI 1002 (%)
80
60
40
20
0
0
Pan 1
4.75mm 2
9.5mm 3
16mm 4
19mm 5
26.5mm
Sieve Size
Upper Limit Coarse Aggregate Gradation Lower Limit
The gradation of the coarse aggregate lays very close to the lower limit of the OPSS guideline
and just barely fails the percentage passing requirement for the 9.5mm sieve. The absorption
content of this aggregate was 1.42%. These aggregates were used for all of the concrete mixed.
30
3.3 Procedure
3.3.1 Concrete Production
ASTM C192 (Making and Curing Concrete Test Specimens in the Laboratory) was used for the
production of the concrete.
A one kilogram sample of coarse aggregate from each sealed container was then be placed in a
drying pan, weighed and then placed in a 110°C oven overnight. The next morning, the dry mass
was measured, and the moisture content for each container of coarse aggregate was determined.
These moisture contents were then compared to the absorption of the aggregate and an
adjustment to the mix water was made to account for the design w/c.
The fine aggregate was prepared in a similar fashion, but were not pre-washed before mixing.
The top layer of the fine aggregate pit would normally be drier due to the dry climate of the
laboratory; therefore, the aggregates were tilled before extraction. The fine aggregate was then
placed in a sealed container to prevent evaporation. After a minimum of six hours, the sealed
containers were opened, the aggregates were stirred with a metal rod, and a kilogram sample
from each bucket was placed in a drying pan. The wet mass was measured, and then placed in a
110°C oven overnight. The next morning, the dry mass was measured, and the moisture content
for each sealed bucket was determined. An adjustment to the batch water was then be made to
maintain the proper w/c.
32
Cement and slag were batched the day of mixing. The adjusted water content was measured and
placed in a sealed container to prevent evaporation. HRWR was poured into a graduated cylinder
to easily measure the amount added during mixing. Prior to mixing, concrete cylinder molds
were lightly lubricated with used hydraulic oil to ease the de-molding process; wooden concrete
slab molds were constructed, secured, and lubricated in the same fashion.
After all the concrete materials were prepared, the mixing drum, blades, sampling tools, and
fresh concrete testing equipment were dampened. As outlined in ASTM C192, the coarse
aggregate and some of the mix water was placed in the drum prior to starting the mixer. While
mixing, the sand, cementitious materials, and the remaining water were added in that order. After
all the material was added, the mixer was run for three minutes. After which the concrete was
allowed to rest for three minutes followed by a final two minute mixing cycle. Depending on the
apparent stiffness of the concrete, HRWR was added during mixing to achieve a workable slump
for placement.
Immediately after mixing, a sample was taken aside to be used in the microwave oven test which
was performed in conjunction with the standard fresh concrete testing. The slump test was
completed first in accordance with ASTM C143.
The fresh density of the concrete was measured using ASTM C138. A steel cylindrical container
conveniently used for determining the air content of concrete was used as the vessel to house the
fresh concrete. The air content was measured using a type B air meter detailed in ASTM C231.
An aggregate correction factor of 1% was determined for the aggregate blend used. None of the
33
concrete casts were air entrained and the exact air content was not necessary when following the
procedure to determine the w/c of the fresh and hardened concrete.
After completing the fresh concrete testing, cylinders and slabs were prepared in accordance with
ASTM C192. Concretes were placed into lightly lubricated 100x200mm cylindrical molds in
three layers and tampered 25 times per layer; a rubber mallet was used to help further consolidate
the cylinders. In later batches, slabs were also prepared, but were prepared in two layers and
tampered 42 times per layer as outlined in Table 2 of ASTM C192. The fresh concrete molds
were covered with damp burlap, and then wrapped with a plastic sheet to maintain a wet
environment during setting. The following day (24± 8h) the samples were de-molded, labeled,
and then placed in a moist room where the temperature was maintained at 23 ± 2° C at 100%
relative humidity. These samples were kept in the moist room until the day of testing.
34
3.3.2.2 Procedure
1. Cut a piece of fibre glass cloth to lie over the glass tray with enough overhang to
completely wrap the concrete specimen. For a 23cm (9 inch) glass tray a 50 cm x 50 cm
piece of fibreglass is recommended.
2. Determine the mass of the tray and fibreglass cloth together (WT). All corresponding
measurements must be measured to an accuracy of at least 0.1 gram.
3. Place the center of the fibre glass at the center of the glass tray allowing for adequate
overhang. Place a representative 1500 ± 10 gram sample of fresh concrete onto the fibre
glass and fold over the fibre glass cloth to completely encase the concrete.
4. Measure the mass of the concrete, tray and fibreglass combined (WS).
35
5. Place the tray with the freshly wrapped concrete into the microwave for an initial drying
period of five minutes.
6. After the drying interval, remove the sample out of the microwave, pull back the fibre
glass cloth and use a metal scrapper to separate the coarse aggregate from the mortar to
maximize the exposed area of the specimen. Pay special attention to avoiding losing any
material.
7. Rewrap the sample and place it back in the microwave for another five minutes of drying.
8. Remove the sample from the microwave and measure the mass of the concrete, tray and
fibreglass together. Place the sample back in the microwave to dry for another two
minutes
9. Repeat step 8 until a mass difference between drying intervals is less than 1 gram.
10. Document the final mass of the tray, cloth and dry concrete (WE).
3.3.2.3 Calculations
The fresh concrete sample mass (WF) can be measured by subtracting the total mass of the fresh
concrete, fibre glass, and tray (WS), by the mass of the tray and fibre glass (WT). The final dried
concrete sample mass (WD) can be determined by subtracting the end mass (WE) by the total
starting mass (WT).
WF = WS - WT [3.1]
WD = WE - WT [3.2]
The total water content (TWC) of the concrete sample is the mass of all the water evaporated
due to the microwave oven drying process.
The TWC includes the free water of the mix, and the natural moisture content of aggregates;
however, the w/c of concrete is determined by the amount of free water in the system when the
aggregates are at surface saturated dry (SSD) conditions. In other words, a small percentage of
the mass loss is attributed by the evaporation of the absorbed moisture content of the aggregates
which is not accounted for when determining the w/c of a mix design. Therefore an aggregate
correction factor (ACF) must be applied to each test in order to estimate the total free water
content (FWC) and avoid measuring an inflated experimental w/c.
Using mass ratios between the mix design and sample size (WS), an estimation of the aggregate
sample mass can be determined. By measuring the natural moisture absorption percentage for
each aggregate at SSD, the addition of the fine and coarse aggregate water contents will yield the
ACF.
Therefore,
Once again, the use of the mix design is necessary for determine the cement content of the
concrete specimen. Using a mass ratio comparing the test specimen with the mix design, the
sample’s cement content (CC) can be determined. Using the adjusted water content of the
specimen and the CC, a microwave water cement ratio (MWC) can be determine.
A comparison can then be made to the actual water cement ratio (AWC) to the MWC. In terms
of percent difference:
TWC = WF – WD
=1518.8g -1399.4g
=1194.4g
= 13.04g
= 119.4g - 13.04g
= 106.36g
38
MWC = FWC/CC
= 106.36g / 239.00g
= 0.445
Difference: (-0.008)
= (0.445-0.453)/0.453 x 100%
= (-1.7 %)
3.3.3.1 Apparatus
1. Concrete saw capable of cutting 100mm diameter concrete cylinders
5. Scales calibrated to measure within 0.01g and capable to withstand 800-1100g samples
3.3.3.2 Procedure
1. Retrieve sample from moist room
3. Label concrete specimen: T for Top, C for Center, B for Bottom, Date, Concrete
Identification Number, etc…
4. For slabs: Use coring machine to cut cores from slabs as seen in Figure 3-4.
40
5. After all samples are cut and properly labeled, they are placed in 105 °C oven for a
minimum of 48 hours.
6. The dry mass (Dm) is measured and then submerged in water for a minimum of four days.
7. After cooling in room temperature, place samples in a sealed container filled with water.
8. After a minimum of four days, measure the suspended mass (Sm) of the sample, followed
by the wet mass (Wm) at SSD conditions.
3.3.3.3 Calculations
Archimedes' principle dictates that an object submerged in a liquid is subjected to a buoyancy
force (Fb) equal to the weight of the liquid displaced (Archimedes, 1897). In other words:
Where D is the density of the liquid, g is the acceleration due to gravity, and V is the volume of
the immersed object. Knowing that weight can be expressed as the product of mass and the
acceleration due to gravity, Equation [3.7] can be modified to Equation [3.8].
41
Due to concrete's porous nature, the Mass air term will be represented by the SSD mass (Wm),
while the Mass suspended will be replaced with the suspended mass (Sm) at full saturation.
Therefore Equation [3.8] becomes:
Wm- Sm = D V [3.9]
Given that water was used as the suspension liquid with a density of 1g/cm3 and if all
measurements are recorded in grams, Equation [3.9] can be simplified to:
Therefore, the volume of the concrete sample being tested can be easily determined by
subtracting the SSD mass of the sample’s suspended mass. The suction porosity (Ps) of the
concrete sample represents the amount of water that is absorbed by the concrete in terms of a
total volume percent. It can be calculated by the difference between the dry and wet mass over
the total volume determined in Equation [3.10].
Ps = Wm - Dm / V [3.11]
With the volume percent of water uptake (Ps) from each sample and using the concrete mix
design to determine the paste volume fraction (Vp), an experimental paste porosity (εp) can be
determined:
Ԑp = Ps/Vp [3.12]
The experimental paste porosity represents the total water uptake from within the paste of the
concrete. From a macroscopic perspective, this is the volume of water that is being absorbed by
the capillary pores of the cement matrix.
Erik Sellevold derived an equation to determine the theoretical paste porosity (Ԑ′p) of a
concrete sample based on the work of Powers (Sellevold, 2005).
42
[3.13]
Where Ԑ′p is measured in volume percent of the total concrete sample, 𝝰 is the degree of
hydration, and Wn is the chemically bound water of cement paste. By equating the theoretical
and experimental paste porosities from Equations [3.13] and [3.12], Sellevold claimed a realistic
w/c prediction could be calculated (Sellevold, 2005).
In order to use Equation [3.13], the degree of hydration (𝝰) must be known. The degree of
hydration is dependent on both the w/c and the space available to accommodate the hydration
products (Lam, 2000). Therefore, practical limits such as the ultimate degree of hydration (𝝰u)
as outlined by R.H. Mills can be a good representation of the degree of hydration of matured
concrete samples (Byard, 2012).
[3.14]
A graphical representation of Equation [3.14] can be seen in Figure 3-5 for the range of samples
tested.
43
0.8
0.78
0.76
0.74
0.72
0.7
0.68
0.4 0.45 0.5 0.55 0.6 0.65 0.7
W/C
Figure 3-5: Ultimate Degree of Hydration Curve Based on R.H. Mills’ Model
As can be seen the ultimate degree of hydration ranges between 0.69-0.81percent for w/c
between 0.4 and 0.7.
By using the ultimate degree of hydration in equation [3.14], the formula for theoretical paste
porosity yields the following:
[ ]
[3.15]
Equation [3.15] hold true if sufficient time is allowed for hydration. This design procedure was
created for pre-existing concrete structures with many years of service, where the degree of
hydration was assumed to be near the practical ultimate limit. However, with this testing regime,
the ultimate degree of hydration may not be achieved for the 28 day samples, and special
consideration is required for the testing of these samples.
Hydration testing completed on similar cement type conducted at Columbia University in New
York showed that within the first 28 days, most of the cement paste has already hydrated and the
44
rate of hydration dramatically decreases as time progresses. Figure 3.6 is taken from the report
(Meyer, 2009).
Figure 3-6: Simulated and Measured Degree of Hydration from Cement # F (Meyer, 2009)
The figure was chosen in particular as the cement chemistry was similar to that which was used
in this research project. An assumption of similar hydration kinetics was made.
Cement #F: C3S= 0.567 C2S= 0.172 C3A= 0.067 C4AF= 0.079 (vol. fraction)
Cement Used: C3S= 0.583 C2S= 0.111 C3A= 0.097 C4AF= 0.069 (vol. fraction)
As can be seen from Figure 3.6, the time function of the hydration curve is plotted on a
logarithmic scale showing that the degree of hydration increases greatly during the early stages
of hydration, and that rate decreases and plateaus as time progresses. From a visual inspection
the degree of hydration does not increase much more past 1000hrs (42 days), and starts to
45
plateau. At 28 days (670hrs), the degree of hydration appears to be close to 95% of its maximum
value.
Additional testing using another cement type similar to the one used in this research project
displayed very similar results. The following graph was taken from the same research paper.
Figure 3-7: Simulated and Measured Degree of Hydration for Cement #A (Meyer, 2009)
Cement #A: C3S= 0.514 C2S= 0.226 C3A= 0.111 C4AF= 0.079 (vol. fraction)
Cement Used: C3S= 0.583 C2S= 0.111 C3A= 0.097 C4AF= 0.069 (vol. fraction)
Most of the hydration occurred in the first few days and began to plateau near the end of Figure
3-7. At 28 days, it appeared that 95% of the total hydration had occurred. Therefore, a k-factor
will be applied to reflect the age of the sample. At 28 days, the k-factor will be 0.95 and at 56
days or older it will be 1.0.
46
A sensitivity analysis performed by Sellevold had shown that the degree of hydration ranging
from 0.65 to 0.85 would affect the calculated w/c by a standard deviation of 0.02 (Sellevold,
2005). With w/c ranging between 0.4 and 0.7, R.H. Mills determined that the practical degree of
hydration is 0.69-0.81, which is well in-between the standard deviation of 0.02 predicted by
Sellevold.
Therefore, the ultimate degree of hydration as modelled by R.H. Mills was used for concrete
older than 56 days and 95% of the ultimate degree of hydration was used for concrete at 28 days.
This method will reduce the complexity of this test method as concrete received from the field
will not contain information regarding the degree of hydration and an estimate will need to be
made.
Equation [3.15] can now be modified with a k-factor to express the age of the concrete sample.
[ ]
[3.16]
By equating the theoretical and experimental paste porosity, and iterative process can be used to
determine the w/c of the hardened concrete sample:
[3.17]
[ ]
[3.18]
A computer program was made to rapidly determine the w/c as described in Equation [3.18].
47
=434.61 cm3
=0.1254 g/cm3
Ɛp = Ps/Vp =(0.1254/0.3054)
=0.4106
[ ]
, where k is 0.95
After iterations:
Difference = (-0.034)
Chapter 4
The next step was to introduce fine and coarse aggregates to measure the accuracy of the
microwave oven test for concrete use. Four mixes were batched using a mixing bowl and a
spatula. Due to the thin layer of cement paste that was lost coating the mixing equipment, larger
than required mix designs were created to account for the cement paste lost. Table 4.1 shows the
mix designs tested. The focus of these batches was to isolate the water content and see if the test
was valid throughout a larger range of w/c. The fine and coarse aggregates were deliberately
oven dried at 110°C to achieve a moisture content of 0%, ensuring that the measured mix water
was the total water content of the sample. The w/c* listed in Table 4.1 is the w/c based only on
the ratio of cement and water added.
50
Table 4.1: Hand Batched Mix Designs for Preliminary Microwave Testing
Mass Measured (g)
Total Total
W/C* Coarse Total Mass
Cement Water Fine Aggregate
Aggregate Mixed
Added Added
0.4 305.40 122.2 523.1 799.4 1750
0.5 269.60 134.8 443.3 662.2 1510
0.6 324.40 194.6 486.9 744.1 1750
0.7 287.00 200.9 400.3 611.8 1500
After the concrete was mixed, a representative sample was wrapped in a fibre glass cloth, placed
on a glass tray, measured, and placed in the microwave. After five minutes of heating, the sample
was removed and prodded with a steel spoon to break apart the mortar from the coarse aggregate.
It was then placed back in the microwave oven for another five minutes before being measured
again. Afterwards, the sample was placed in the microwave to heat for two minute intervals and
then weighed. When the mass did not change by more than 1 gram, the test was complete and the
final mass was used to determine the mass loss.
Table 4.2 shows the fresh concrete sample size for each w/c tested and the progression of mass
loss due to water evaporation over time (T). The 0.4 and 0.5 w/c mixes required a 14 minute
drying time as the mass change between 12 minutes and 14 minutes were less than one gram.
The 0.6 and 0.7 w/c mixes needed an additional 4 minutes in the microwave as the mass of water
needed to evaporate was much higher. As can be seen in Table 4.2, the mass loss equates closely
to the actual water content added to the system; this showed that the microwave oven test does
work for concrete and can be accurate.
51
The capacity of the concrete mixer used in these batches was 20L; after mixing, concrete was
sampled for the microwave oven test. The results of the microwave oven test are presented in
Table 4.4.
Time Of
Sample Sample Aggregate Sample
Testing
ID Batched Size Mass Correction Cement Microwave W/C Error
After
# W/C Tested Loss Factor Content W/C Diff. (%)
Mixing
(g) (g) (g) (g)
(min)
P1 0 0.402 1498.4 113.1 14.3 259.2 0.381 -0.021 5.1
P2 0 0.412 1506.1 109.3 12.4 256.8 0.377 -0.035 8.5
P3 0 0.415 1507.8 98.3 13.2 215.2 0.395 -0.020 4.8
P3 15 0.415 1001.2 65.0 8.8 142.9 0.394 -0.022 5.3
P4 0 0.453 1508.8 112.0 13.0 237.8 0.416 -0.036 8.0
P4 15 0.453 1005.3 77.2 8.7 158.4 0.433 -0.020 4.5
P4 30 0.453 2003.1 146.8 17.3 315.6 0.410 -0.042 9.4
P4 50 0.453 1501.7 109.0 12.9 236.6 0.406 -0.047 10.3
P4 70 0.453 498.8 38.7 4.3 78.6 0.438 -0.015 3.3
52
The ID# represents the identification number of each concrete batch. The “P” refers to
preliminary testing, and the number represents the sequence of batching. The sample mass loss is
the difference between the fresh mass of concrete and the final microwave dry mass. The
aggregate correction factor column shows the mass loss due to the evaporation of water within
the aggregates, and the sample’s cement content is determined by a mass ratio of the sample size
and the mix designs found in Appendix A.
The percent error is considerably small; on average the percent error is 6.6. P1 and P2 were the
first two tests completed as described in the experimental procedure section. The calculated
microwave w/c from the test would have yielded 0.436, and 0.426 respectively but this included
the mass loss attributed to the moisture absorption of the aggregates. After applying the
aggregate correction factor, the calculated w/c became 0.381, and 0.395, which if compared to
the actual w/c of 0.402 and 0.412, is a minimal difference.
Two microwave tests were completed in succession from mix P3. Due to the limitation of only
having one microwave oven during testing, the first test used concrete sampled right after
mixing, while the second was kept in a sealed container until the first test was complete. Table
4.4 shows the start time for each test. In order to measure the effects of varying sample sizes, the
first P3 test had a standard sample size of 1508g while the second had 1001g.
Similarly, five consecutive tests were completed with mix P4 concrete to further measure the
effects of sample size. Concrete from mix P4 was stored in a sealed container and sampled after
the completion of the previous test. Samples with 1500 grams and 1000g needed a minimum of
14 minute to dry in the microwave oven, and minimal precautions were needed when gathering a
representative sample from the mix. The 500g sample only required 12 minutes within the
microwave and with adjustments could be shortened, however it was difficult to ensure a
representative sample containing a proper cement paste to aggregate ratio. When completing
testing for 2000 grams, the higher water content extended the drying time to 20 minutes. A
summary of the mass loss at each drying interval is displayed in Table 4.5.
53
After testing, the samples were placed in a 110°C oven to measure any additional mass loss.
None was observed, concluding that the microwave oven test completely eliminates all
evaporable water from the system. After becoming familiar with the testing procedures, it was
thought that a 1500g ± 10g sample was the easiest to implement in the field, provided a fair
representation of the mix design, and required a short drying interval. In addition, if the fresh
concrete samples are kept in a sealed container, this test can be performed after an hour of
mixing, and can yield the same results as a tested complete right after mixing. This is illustrated
in Table 4.4 for the two P4 concrete samples tested directly after mixing, and 50 minutes after
mixing with a starting mass around 1500g. With this knowledge, larger ranges of w/c concrete
were tested.
The ID# represents the identification number for each mix design. The microwave oven test was
completed for each mix design. Some mix designs were tested multiple times in quick succession
as only one microwave oven was available for testing. Therefore some tests started directly after
mixing, 30 minutes after mixing, or 55 minutes after mixing was complete. The results are
summarized in Table 4.7.
The results appear to provide good estimates for concrete with w/c ratios below 0.5. Segregation
caused at w/c higher than 0.5 created difficulties when trying to gathering a representative
sample. A summary of the mass loss for each test during the entire drying process is presented in
Table 4.8.
In general, lower w/c concrete required less time to be dried. Unfortunately, during C-0.55, the
scale used was malfunctioning, and the mass readings between 12min and 18min fluctuated, but
after replacing the scale, the final mass was determined at 22 minutes.
The underlined mass readings in Table 4.8 show the first instance where the mass loss between
drying intervals was less than one gram. According to the ASTM draft, the underlined mass
reading was used as the final dry mass and would act as the termination of the test. The values
after the underlined text show the mass of the sample when the microwave drying intervals were
continued until a mass loss between consecutive readings was less than 0.5g was obtained.
Table 4.9 shows the measured w/c according to the ASTM draft, where the final dry mass used is
seen as the underlined text in Table 4.8, and the calculated w/c for the same concrete sample
56
subjected to an extended drying period. The final column shows the difference between the two
calculated microwave w/c.
Table 4.9: Phase Two ASTM Draft vs Extended Drying Regime effects on W/C
Microwave W/C Microwave W/C Difference
Sample Designed According to ASTM Extended Drying Between
ID #
Size W/C Draft Regime Microwave
(mass loss < 1.0g) (mass loss < 0.5 g) W/C
C-0.45 1500.9 0.453 0.414 0.416 0.002
C-0.45 1540.8 0.453 0.422 0.426 0.004
C-0.45 1518.8 0.453 0.439 0.446 0.007
C-0.5 1517.7 0.499 0.465 0.473 0.008
C-0.5 1512.0 0.499 0.549 0.552 0.003
C-0.55 1506.2 0.549 0.465 0.469 0.004
C-0.55 1505.3 0.549 0.471 0.471 0.000
C-0.6 1510.5 0.600 0.519 0.529 0.010
C-0.6 1500.2 0.600 0.463 0.472 0.009
C-0.65 1516.9 0.649 0.489 0.495 0.006
C-0.7 1551.0 0.699 0.608 0.613 0.005
C-0.45S 1541.7 0.452 0.379 0.389 0.010
Although extending the termination of the test from a mass loss of 1.0g to 0.5g had a minimal
difference on the overall w/c, it did benefit the results. If time permits, the test should be
continued until a mass difference between consecutive readings is less than 0.5g. This will
ensure that all water will have evaporated and prevent premature termination.
0.5S represents that 25% slag was used as a cement replacement. The summary of the mix
designs are provided in Table 4.10 and a full mix design can be found in Appendix A.
The microwave test was completed right after mixing, and was done twice per batch. The first
commenced right after mixing finished, and the second test commenced after the first was
complete. The concrete used for the second microwave test was kept in an open container prior
to testing. After testing, the concrete specimens were then placed in a metal tray, weighed, and
placed in a 110°C oven over night, to measure any additional mass lost from entrapped water.
Table 4.11 provides a summary of the test results.
Start
time Total Agg. Sample Microwave
Designed Sample Error
ID# after Water Water Cement Oven Diff
W/C Size (%)
mixing Loss Loss Content W/C
(min)
After becoming familiar with conducting the test method, the microwave determined w/c was
very similar to the design value. The measured w/c from the first test was higher than the second
tests as the second test was performed 30 minutes after the first, allowing for water to evaporate
and lowering the total water content of the sample. This was deliberately done to show that time
of testing is important when working with fresh concrete. The 110°C oven dried masses showed
no signs of additional mass loss.
Once again, the recorded mass during each test is displayed in Table 4.12. The underlined value
in red text illustrates shows the termination of the test according to the ASTM draft, and for the
interest of research, the drying cycle was extended further to measure all potential evaporable
water.
Table 4.13 shows the w/c as was determined by the ASTM draft’s recommendation to stop
drying when the first mass loss between readings is less than 1 g. The extended drying column
shows the measure w/c if the microwave test was continued until a mass loss less than 0.5g was
obtained. The difference between both measured w/c is shown in the final column of Table 4.13.
59
Table 4.13: Phase Three ASTM Draft vs Extended Drying Regime Effects on W/C
Microwave W/C Microwave W/C Difference
Sample Designed According to ASTM Extended Drying Between
ID #
Size W/C Draft Regime Microwave
(mass loss < 1.0g) (mass loss < 0.5 g) W/C
S-0.4 1504.7 0.408 0.391 0.398 0.007
S-0.4 1502.8 0.408 0.377 0.380 0.003
S-0.45 1498.0 0.451 0.436 0.437 0.002
S-0.45 1538.9 0.451 0.413 0.413 0.000
S-0.5 1512.2 0.499 0.487 0.491 0.004
S-0.5 1508.1 0.499 0.454 0.454 0.000
S-0.5S 1526.5 0.509 0.475 0.481 0.006
S-0.5S 1532.6 0.509 0.450 0.463 0.013
Extending the drying program of this microwave test to stop testing when a mass loss between
consecutive readings is less than 0.5g does improve the results. However, if time is limited, the
ASTM draft provides a reasonable w/c measurement.
Microwave
0.429 0.470 0.513 0.501 0.495 0.613 0.389
W/C
Actual
0.453 0.499 0.549 0.600 0.649 0.699 0.452
W/C
After repeating the microwave oven test on low w/c mixes, it was clear that this test method can
be used to accurately measure the w/c. Table 4.15 present the summary of concrete samples
tested in Phase Three.
Microwave
0.398 0.437 0.491 0.481
W/C
Figure 4-1 displays the percent error of the microwave oven test tabulated in Table 4.15.
Concrete with a C- are from phase two of testing, while concrete with an S- are from phase three.
The number value next to the letter represents the w/c of each concrete, and the S in C-0.45S and
S-0.5S represent 25% slag replacement within the mix.
61
S-0.5S -5.5
S-0.5 -1.6
S-0.45 -3.1
S-0.4 -2.5
C-0.45S -13.9
C-0.55 -6.6
C-0.5 -5.8
C-0.45 -5.2
1. Retrieve a core sample from a concrete element and cut to a thickness of 20-40mm
5. Place sample in pressure-saturation chamber over night at 5MPa for PF-value purposes
7. Dry sample in an 110°C oven for a minimum of two days and then measure the dry mass
The water saturation portion of this test followed the same procedure used in ASTM C1202
(Rapid Chloride Permeability Test). Essentially, the concrete samples was placed in a sealed
chamber under a vacuum to remove the air from the pores of the concrete, then de-aerated water
63
was added under a suction pressure of 80kPa driving the water into the pores of the concrete.
This process was thought to hasten the water saturation process to one day as opposed to
Sellevold’s four day saturation period. To determine the PF-value of the concrete sample, the
saturated sample was placed under pressure overnight at 5MPa.
The first concrete tested was cast on July 5th 2012 and the full mix design can be found in
Appendix A. In summary, the paste volume fraction (Vp) was 0.3102, with a design w/c of
0.402, and a batch size of 17.2 L. In total five concrete cylinders were taken out of the moist
room after 28, 56, and 112 days of curing and a 50mm thick sample was cut out of the center of
each core and tested. Results are shown in Table 4.16:
As can be seen, the average water uptake decreased as the sample matured. This may be due to
capillary pores becoming more discontinuous as concrete further hydrates, preventing water from
flowing easily into the sample. A second concrete mix design was tested in order to validate
these results and to see if the percent error would decrease.
The second trial batch of concrete was cast on September 19, 2012, and the full mix design is
provided in Appendix A. In summary, the paste volume fraction was 0.3038, with a designed w/c
of 0.4051 and a yield of 19.6 L. Once again the samples measured 50mm and were cut from the
center of 28 and 56 day, 100mm diameter, concrete cylinders.
These results showed significant error in estimating the w/c. On a positive note, similar trends
were visible. The predicted w/c value decreased as the concrete matured. This shows that the
concrete pores are becoming more discontinuous and is was reflected by a decrease in water
uptake during the test. It became apparent that Sellevold’s approach in drying the samples prior
to saturation may have been done deliberately to induce micro-cracks, allowing for the
transportation of water throughout the entire concrete medium. With these results, steps were
made to revert back to Sellevold’s original approach of oven drying first and then saturating
(Sellevold, 2005).
Table 4.20: Repeat Testing of Trial 2 with Induced Micro-Cracks for W/C=0.405
56 Day Repeat Test Sample 1 Sample 2 Calculations Sample 1 Sample 2
3
Submerged Mass (g) 1011.22 984.9 V (cm ) 412.82 401.50
Suspended Mass (g) 598.4 583.4 Ps 0.115 0.113
Vacuum Saturated (g) 1012.07 986.4 Vp 0.304 0.304
Oven Dry Mass (g) 963.63 939.61 Ep 0.380 0.372
Water Cement Ratio 0.386 0.376 E'p 0.379 0.372
66
These results show that the creation of micro-cracks prior to water saturation allowed water to
flow into all the capillary pores of the sample. The micro-cracks acted as transport channels into
what were previously inaccessible pores. Errors in the w/c estimate were reduced from 28.1%
down to 5.9%. Therefore, it was determined that inducing micro-cracks was necessary in
determining the w/c of the hardened concrete.
The concrete samples used for this thickness test were cast on October 3rd, 2012. They were
tested after 28 days of moist curing, and samples were cut as close to the center as possible. Each
sample slice was cut from the same concrete cylinder. The paste fraction was 0.3083, the batch
size was 19.5L and the designed w/c was 0.412. The full mix design can be found in Appendix
A. The results are shown in Table 4.22.
67
These results show that samples with thicknesses between 30mm and 50 mm resulted in minimal
differences in the w/c. The 20mm sample had the largest error and that may be due to the
nominal size of coarse aggregate being 19mm. These results show that it is not recommended to
use a sample thickness similar to the aggregate size. Reverting back to the idea of using a similar
thickness which is used in the permeability test and that very minimal differences were seen
between 30, 40, and 50mm samples, it was decided to use a thickness of 50mm for all further
testing.
Four 50mm thick cylinder slices were cut from a cylinder of the same concrete batch used to
determine the sample thickness in Table 4.22. Each 50mm sample was cut from the center of the
sample, and tested right after obtaining the results from the multiple thickness test. Therefore,
these samples were tested 5 weeks after casting. Once again this concrete was batched on
October 3rd, 2012 and had a design water cement ratio of 0.412. Table 4.23 show the results.
68
These results helped validate that 50mm slices could be used, and that inducing micro-cracks by
drying first could yield accurate results. With the order of testing, and sample size determined,
the remaining variable tested was the duration of saturation and desiccation.
# 1 Top
56
#2 Center
54
#3 Bottom
52 #2 Top
50 #2 Centre
#2 Bottom
48
#3 Top
46 # Centre
0 1 2 3 4 5 6 7 8
#3 Bottom
Days Saturated
Figure 4-2: Water Uptake Over Time for Samples Cast on November 28th
0.490
#2 Center
0.470 #3 Bottom
0.450 #2 Top
0.430 #2 Centre
#2 Bottom
0.410
#3 Top
0.390
0 1 2 3 4 5 6 7 8 # Centre
Figure 4-3: November 28th Water Saturation Duration for 0.453 W/C Concrete
70
55
54 #2 Center
53 #3 Bottom
52 #2 Top
51 #2 Centre
50
#2 Bottom
49
#3 Top
48
0 1 2 3 4 5 6 7 8 9 # Centre
Days Saturated #3 Bottom
Figure 4-4: Water Uptake Over Time for Samples Cast on January 14th
0.420 #2 Center
0.415 #3 Bottom
0.410 #2 Top
0.405 #2 Centre
0.400 #2 Bottom
0.395 #3 Top
0.390 # Centre
0 1 2 3 4 5 6 7 8 9 #3 Bottom
Days Saturated
Figure 4-5: January 14th Water Saturation Duration for 0.453 W/C Concrete
71
It is interesting to note that the November 28th samples’ water uptake from three to six days does
not increase by much more than 1 gram on average. From five to eight days, the January 14 th
samples do not change much more than 1 gram on average. Close to 95% of the water uptake
occurs within the first day of saturation, and the remaining days only add to a small fraction to
further saturation. These results were also displayed in terms of w/c. The calculated w/c does not
vary to a great degree over time. Following Sellevold’s procedure, a four day saturation period
should be used as a minimum value. If the sample can be placed under saturation for longer, it
would not dis-benefit the test.
More importantly, if all excess water is not removed from the surface of a sample when
measuring the SSD mass, this mass gain will affect the overall w/c calculation greater than an
extra day of saturation. Conversely, if a sample is allowed to dry past SSD conditions due to
evaporation prior to measuring, the mass loss also affects the w/c calculation. Therefore, a
minimum of four days of saturation is recommended with special attention required during the
measurement of the SSD wet mass.
Extensive drying measurements where not conducted as after two days of drying, minimal mass
losses were measured; on average mass loss less than1g was viewed between day two and three.
On the fourth day, the mass loss was less than 0.5g per day on average. Therefore, it is
recommended to use a minimum of 48 hours in a 105°C oven with a preferred desiccation time
of three days; however, if time permits, longer drying periods will not adversely affects the test
procedure.
It is interesting to note that the January 14th samples with the lowest water uptake were from the
bottom portions of the concrete cylinder and had the lowest calculated w/c. The opposite can be
seen for the top slices, as Figure 4-4 shows, the top samples gave higher w/c compared to the
other samples. This is evidence of segregation from consolidation of the cylinder during casting.
72
The pressure-saturation process itself is also difficult to implement, as in order to achieve SSD
conditions, the sample would need to be patted dry with a wet cloth. However, this process
requires time, and the pressurized water from within the pores will squeeze out of the sample.
Alternatively, this pressure saturation method could be used to accelerate the saturation period of
concrete samples. By submerging the sample using this pressure chamber, it could negate the
need for a minimum four day saturation period, replacing it with a one-day pressure saturation
period. However, further testing of this was required as only minimal research was complete
regarding this “shortcut”.
In summary, it is not clear what the PF-value truly measures, as micro-cracks within a concrete
sample make distinguishing the capillary porosity from the entrained air void porosity difficult.
Given a longer saturation period, the air porosity value would decrease while the capillary
porosity would increase, and the opposite could be said with a shorter saturation period.
Therefore, since the primary scope of this research project was to determine the w/c of hardened
concrete, the PF-value portion to determine air porosity was no longer studied.
73
The C in the ID# distinguishes that only cylinders were cast from the fresh concrete and the
numbers represent the w/c. The mixes were designed to isolate varying w/c. The sand and coarse
aggregate are expressed at SSD conditions. HRWR was added during mixing to achieve a
workable slump, and is accounted for in the total mix design.
Jan 14-13 C-0.45 0.453 378.4 0.0 170.0 730.4 1124.5 1.3
Jan 17-13 C-0.5 0.499 381.0 0.0 190.2 698.3 1101.5 0.00
Feb 13-13 C-0.55 0.549 373.9 0.0 205.4 685.3 1081.0 0.00
Feb 13-13 C-0.6 0.600 381.2 0.0 228.6 664.9 1031.4 0.00
Feb 21-13 C-0.65 0.649 390.0 0.0 253.2 600.9 1022.6 0.00
Feb 21-13 C-0.7 0.699 389.5 0.0 272.4 582.0 990.3 0.00
Feb 27-13 C-0.45S 0.452 284.2 94.7 170.2 727.5 1119.3 0.9
Table 4.25 shows the exact quantity of each material used in the concrete mixer, and displays the
experimental yield for each batch after completing a theoretical density test. When creating the
mix designs, the water content was the only parameter that increased to achieve higher w/c
concretes. This was done to isolate the change in water content to observe its effect on the w/c
calculations. Full mix designs can be found in Appendix A.
74
All of the batches under yielded resulting in a denser concrete then estimated. From this
information, relative density and yield adjustments were made. The key variable needed from
these yield adjustments were the paste volumes, as this value would greatly influence the results.
These adjustments can be found in Table 4.26.
From these batches, concrete cylinders were made, cut into three 50mm slices, labeled properly,
and subjected to the hardened w/c test procedure.
75
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 1014.4 1068.9 634.3 434.6 0.125 0.410 0.419 -0.034 7.5
28-1 C 962.3 1013.8 603.1 410.7 0.125 0.410 0.418 -0.035 7.7
28-1 B 958.6 1008.0 600.0 408.0 0.121 0.396 0.397 -0.055 12.3
28-2 T 999.6 1053.9 625.2 428.7 0.127 0.415 0.424 -0.029 6.4
28-2 C 953.0 1003.5 596.0 407.5 0.124 0.406 0.411 -0.042 9.2
28-2 B 952.6 1002.1 596.7 405.3 0.122 0.400 0.402 -0.050 11.1
28-3 T 1031.7 1086.4 645.8 440.6 0.124 0.406 0.412 -0.041 9.1
28-3 C 952.8 1003.5 596.9 406.6 0.125 0.408 0.414 -0.039 8.5
28-3 B 949.1 999.2 594.9 404.3 0.124 0.406 0.411 -0.042 9.2
56-1 T 956.6 1004.7 596.1 408.6 0.118 0.385 0.394 -0.059 12.9
56-1 C 947.5 994.9 594.6 400.3 0.118 0.388 0.397 -0.056 12.3
56-1 B 962.0 1009.0 601.3 407.7 0.115 0.378 0.383 -0.070 15.4
56-2 T 940.7 988.8 587.5 401.3 0.120 0.393 0.404 -0.048 10.7
56-2 C 940.0 988.2 586.8 401.4 0.120 0.393 0.404 -0.048 10.7
56-2 B 959.3 1005.8 600.1 405.7 0.115 0.375 0.380 -0.073 16.1
56-3 T 961.4 1009.9 600.0 410.0 0.118 0.388 0.397 -0.056 12.4
56-3 C 960.6 1009.6 598.6 411.0 0.119 0.390 0.400 -0.053 11.7
56-3 B 966.2 1012.9 602.9 410.0 0.114 0.373 0.376 -0.076 16.8
112-1 T 979.4 1026.8 610.1 416.7 0.114 0.373 0.377 -0.076 16.7
112-1 C 980.6 1025.9 611.3 414.6 0.109 0.358 0.358 -0.095 21.0
112-1 B 972.6 1019.1 606.0 413.1 0.113 0.369 0.372 -0.081 17.8
112-2 T 981.9 1027.7 611.5 416.2 0.110 0.360 0.361 -0.092 20.3
112-2 C 984.2 1030.1 614.1 416.0 0.110 0.361 0.362 -0.091 20.1
112-2 B 970.4 1016.5 605.2 411.3 0.112 0.367 0.370 -0.083 18.4
76
Measured Actual
Average Results W/C Difference % Error
W/C W/C
28-1 0.411 0.453 0.042 -9.2
28-2 0.407 0.453 0.046 -10.2
28-3 0.412 0.453 0.041 -8.9
28-T 0.418 0.453 0.035 -7.7
28-C 0.414 0.453 0.038 -8.5
28-B 0.404 0.453 0.049 -10.9
56-1 0.391 0.453 0.061 -13.6
56-2 0.396 0.453 0.057 -12.5
56-3 0.391 0.453 0.062 -13.6
56-T 0.398 0.453 0.054 -12.0
56-C 0.400 0.453 0.052 -11.6
56-B 0.380 0.453 0.073 -16.1
112-1 0.369 0.453 0.084 -18.5
112-2 0.364 0.453 0.089 -19.6
112-T 0.369 0.453 0.084 -18.5
112-C 0.360 0.453 0.093 -20.5
112-B 0.371 0.453 0.082 -18.1
There is a small decrease of the water cement ratio from the top to bottom of the cylinder. This
could be explained by the compaction of the cylinders causing segregation. The calculated w/c
also decreases as the concrete matures, this could be due to hydration causing a denser structure
causing a decrease in the water uptake. Although the calculated w/c difference on average was
13%, the results appear to follow a reasonable trend.
77
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 900.4 962.9 564.3 398.6 0.157 0.473 0.522 0.023 4.6
28-1 C 902.8 962.7 568.0 394.8 0.152 0.459 0.496 -0.003 0.6
28-1 B 914.6 968.9 575.8 393.1 0.138 0.417 0.429 -0.070 14.1
28-2 T 897.6 959.3 564.3 395.1 0.156 0.472 0.519 0.020 4.1
28-2 C 898.3 957.0 565.1 391.9 0.150 0.452 0.485 -0.014 2.8
28-2 B 908.1 962.8 572.5 390.3 0.140 0.424 0.439 -0.060 12.1
28-3 T 915.9 977.7 575.3 402.4 0.153 0.463 0.504 0.004 0.9
28-3 C 884.9 940.5 555.6 385.0 0.145 0.436 0.459 -0.040 8.1
28-3 B 917.7 972.0 577.9 394.1 0.138 0.416 0.427 -0.072 14.4
56-1 T 914.2 977.1 570.9 406.2 0.155 0.467 0.525 0.026 5.2
56-1 C 929.8 987.6 583.8 403.8 0.143 0.432 0.464 -0.035 7.0
56-1 B 947.1 999.5 596.1 403.4 0.130 0.392 0.405 -0.094 18.9
56-2 T 927.7 989.1 580.9 408.2 0.150 0.454 0.501 0.002 0.4
56-2 C 929.7 989.1 584.0 405.1 0.146 0.442 0.481 -0.018 3.6
56-2 B 944.4 998.6 593.8 404.8 0.134 0.404 0.422 -0.077 15.5
56-3 T 918.4 980.0 575.9 404.2 0.152 0.460 0.513 0.013 2.7
56-3 C 931.7 989.9 585.2 404.7 0.144 0.434 0.468 -0.031 6.3
56-3 B 932.3 988.7 585.1 403.6 0.140 0.422 0.448 -0.051 10.2
112-1 T 931.0 995.1 583.6 411.5 0.156 0.470 0.531 0.031 6.3
112-1 C 926.5 991.0 580.2 410.8 0.157 0.474 0.537 0.038 7.7
112-1 B 947.3 1003.3 594.2 409.1 0.137 0.414 0.436 -0.063 12.6
112-2 T 951.1 1013.5 598.0 415.5 0.150 0.454 0.501 0.001 0.3
112-2 C 936.4 1000.4 588.1 412.3 0.155 0.469 0.528 0.028 5.7
112-2 B 956.5 1014.0 601.8 412.2 0.140 0.421 0.448 -0.051 10.2
112-3 T 940.0 1001.9 590.1 411.8 0.150 0.454 0.5013 0.002 0.4
112-3 C 946.6 1004.4 594.3 410.2 0.141 0.426 0.4549 -0.044 8.9
112-3 B 959.4 1012.4 603.7 408.7 0.130 0.391 0.4034 -0.096 19.2
78
Once again, a similar trend is seen with the top cylinder slices having the highest calculated
water cement ratio, while the bottom had the lowest. Overall the calculated w/c is very close to
the actual w/c with an overall percent error of 4.7%.
79
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 924.3 986.8 579.4 407.4 0.153 0.439 0.464 -0.086 15.6
28-1 C 929.5 987.8 581.6 406.2 0.144 0.411 0.419 -0.130 23.7
28-1 B 946.9 998.5 594.1 404.4 0.128 0.366 0.357 -0.192 35.0
28-2 T 905.6 967.6 567.8 399.8 0.155 0.444 0.472 -0.078 14.1
28-2 C 927.4 987.0 581.8 405.3 0.147 0.421 0.434 -0.115 20.9
28-2 B 943.9 997.5 592.5 405.0 0.132 0.379 0.374 -0.175 31.9
28-3 T 920.4 987.7 576.9 410.8 0.164 0.468 0.512 -0.038 6.8
28-3 C 925.1 981.8 580.2 401.7 0.141 0.404 0.410 -0.139 25.4
28-3 B 946.7 997.5 594.4 403.1 0.126 0.360 0.350 -0.199 36.3
56-1 T 929.7 990.7 581.8 408.9 0.149 0.427 0.456 -0.093 17.0
56-1 C 940.5 996.2 588.5 407.7 0.137 0.391 0.401 -0.148 26.9
56-1 B 944.6 998.0 592.6 405.4 0.132 0.377 0.383 -0.166 30.3
56-2 T 928.0 991.2 579.8 411.5 0.154 0.440 0.477 -0.072 13.1
56-2 C 928.7 987.2 582.0 405.1 0.144 0.413 0.434 -0.115 20.9
56-2 B 944.2 1000.0 592.8 407.2 0.137 0.392 0.403 -0.146 26.6
56-3 T 932.4 993.3 583.2 410.2 0.149 0.425 0.454 -0.095 17.4
56-3 C 933.3 993.4 583.6 409.8 0.147 0.419 0.444 -0.105 19.1
56-3 B 945.4 997.8 592.9 404.9 0.129 0.370 0.374 -0.175 31.9
112-1 T 908.6 969.7 569.9 399.7 0.153 0.437 0.473 -0.077 14.0
112-1 C 912.7 973.7 572.5 401.2 0.152 0.436 0.470 -0.079 14.4
112-1 B 926.6 981.1 581.4 399.8 0.136 0.390 0.401 -0.149 27.1
112-2 T 913.1 974.6 572.0 402.6 0.153 0.437 0.473 -0.077 14.0
112-2 C 923.6 981.3 578.8 402.5 0.143 0.410 0.429 -0.120 21.8
112-2 B 940.2 993.6 591.5 402.1 0.133 0.380 0.388 -0.162 29.5
112-3 T 930.7 989.3 583.1 406.2 0.144 0.413 0.4340 -0.115 21.0
112-3 C 925.2 982.2 580.2 402.0 0.142 0.406 0.4230 -0.126 23.0
112-3 B 928.8 984.5 584.7 399.8 0.139 0.398 0.4118 -0.137 25.0
80
During casting, the slump was naturally high (175mm) due to the high w/c ratio. Caution was
taken to avoid segregation induced by casting, however, the results showed strong signs of
segregation. During sampling it was difficult to acquire a representative sample, as water would
fall from the metal scoop. During the casting process the larger aggregates settled to the bottom
resulting in a lower calculated w/c. Although this test results are poor, they showed that this test
method could be used to observe concrete segregation.
81
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 916.8 988.2 574.5 413.7 0.173 0.463 0.503 -0.097 16.1
28-1 C 909.5 976.5 571.0 405.4 0.165 0.443 0.481 -0.118 19.7
28-1 B 937.5 994.8 587.4 407.4 0.141 0.377 0.383 -0.216 36.0
28-2 T 916.4 985.1 573.8 411.3 0.167 0.448 0.490 -0.109 18.2
28-2 C 912.0 978.2 572.4 405.8 0.163 0.437 0.472 -0.127 21.2
28-2 B 921.3 982.2 580.0 402.2 0.152 0.406 0.425 -0.175 29.2
28-3 T 879.0 956.0 549.3 406.7 0.189 0.507 0.603 0.003 0.5
28-3 C 886.1 961.4 553.8 407.6 0.185 0.496 0.578 -0.021 3.5
28-3 B 902.4 972.9 564.7 408.2 0.173 0.463 0.517 -0.083 13.8
56-1 T 920.7 991.9 576.1 415.8 0.171 0.459 0.510 -0.090 14.9
56-1 C 928.4 995.2 582.4 412.8 0.162 0.434 0.465 -0.134 22.4
56-1 B 947.9 1008.4 593.3 415.1 0.146 0.391 0.401 -0.199 33.1
56-2 T 913.0 984.0 571.5 412.5 0.172 0.462 0.514 -0.085 14.2
56-2 C 927.3 992.6 582.0 410.6 0.159 0.426 0.453 -0.146 24.4
56-2 B 943.3 1003.1 592.0 411.0 0.145 0.390 0.400 -0.199 33.3
56-3 T 926.1 993.2 580.7 412.5 0.163 0.437 0.470 -0.129 21.6
56-3 C 932.3 997.0 586.0 411.0 0.157 0.422 0.447 -0.153 25.5
56-3 B 943.4 1002.9 593.1 409.8 0.145 0.390 0.400 -0.200 33.4
112-1 T 904.7 972.5 569.5 403.0 0.168 0.451 0.496 -0.104 17.3
112-1 C 917.1 983.0 576.8 406.2 0.162 0.435 0.468 -0.132 22.0
112-1 B 929.0 989.3 585.1 404.2 0.149 0.400 0.414 -0.185 30.9
112-2 T 895.7 964.5 563.0 401.5 0.171 0.459 0.510 -0.090 14.9
112-2 C 911.5 977.4 575.1 402.4 0.164 0.439 0.475 -0.125 20.8
112-2 B 932.7 989.5 587.1 402.4 0.141 0.378 0.384 -0.216 35.9
112-3 T 910.7 978.6 573.3 405.3 0.167 0.449 0.4924 -0.107 17.9
112-3 C 911.7 976.3 574.1 402.3 0.161 0.43 0.4604 -0.139 23.2
112-3 B 931.2 992.6 585.5 407.1 0.151 0.404 0.4204 -0.179 29.9
82
Segregation occurred and is visible in the results similar to the 0.55mix. The slump was 220 mm.
It is interesting to note that this test method was able to show the extent of segregation
throughout the depth of cylinder.
83
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 897.7 962.8 558.4 404.4 0.161 0.390 0.390 -0.260 40.0
28-1 C 913.7 976.8 574.3 402.5 0.157 0.380 0.376 -0.273 42.1
28-1 B 930.4 987.0 586.0 401.0 0.141 0.342 0.327 -0.322 49.6
28-2 T 884.1 952.4 554.6 397.9 0.172 0.416 0.427 -0.222 34.3
28-2 C 893.1 959.1 559.5 399.7 0.165 0.401 0.404 -0.245 37.8
28-2 B 910.8 973.6 572.0 401.6 0.156 0.379 0.374 -0.275 42.4
28-3 T 899.2 969.3 563.0 406.3 0.173 0.419 0.430 -0.219 33.8
28-3 C 912.0 976.8 573.4 403.4 0.161 0.389 0.388 -0.261 40.2
28-3 B 927.1 987.4 583.1 404.2 0.149 0.362 0.352 -0.298 45.8
56-1 T 926.4 997.8 577.8 420.0 0.170 0.412 0.434 -0.215 33.1
56-1 C 927.2 997.4 582.1 415.3 0.169 0.410 0.430 -0.219 33.8
56-1 B 946.5 1008.3 594.3 414.1 0.149 0.362 0.364 -0.285 44.0
56-2 T 917.9 992.4 576.1 416.3 0.179 0.434 0.468 -0.182 28.0
56-2 C 929.5 997.4 583.3 414.1 0.164 0.397 0.411 -0.238 36.7
56-2 B 958.5 1018.0 603.0 415.0 0.143 0.348 0.345 -0.304 46.9
56-3 T 917.3 989.9 575.3 414.6 0.175 0.425 0.453 -0.196 30.2
56-3 C 918.5 986.4 574.9 411.5 0.165 0.400 0.415 -0.234 36.1
56-3 B 937.6 997.0 589.5 407.5 0.146 0.354 0.353 -0.297 45.7
112-1 T 908.4 988.0 571.2 416.8 0.191 0.463 0.516 -0.133 20.5
112-1 C 930.5 1000.7 586.3 414.4 0.169 0.411 0.432 -0.217 33.4
112-1 B 957.8 1019.5 604.3 415.2 0.149 0.361 0.362 -0.287 44.3
112-2 T 932.0 1007.3 585.7 421.6 0.179 0.433 0.466 -0.183 28.2
112-2 C 936.2 1006.7 590.0 416.6 0.169 0.410 0.431 -0.219 33.7
112-2 B 972.2 1033.1 612.7 420.4 0.145 0.352 0.350 -0.299 46.1
112-3 T 928.6 1005.9 583.1 422.8 0.183 0.443 0.483 -0.167 25.7
112-3 C 940.4 1014.7 591.5 423.2 0.176 0.426 0.455 -0.194 29.9
112-3 B 959.9 1026.5 603.7 422.8 0.157 0.382 0.390 -0.259 39.9
84
The slump was 225mm; segregation occurred during casting. Large pools of bleed water were
present after casting, and similar segregation trends with the calculated hardened w/c are seen.
85
Table 4.37 displays all the results for the concrete cast with a 0.699 w/c. Three cylinders were
tested at 28 days, three more at 56 days, and three at 112 days. Three 50mm (Top, Center, and
Bottom) samples were tested per cylinder. The paste volume fraction was 0.429. Average results
are presented in Table 4.38.
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 897.3 969.5 563.7 405.8 0.178 0.415 0.427 -0.272 38.9
28-1 C 889.1 957.9 558.5 399.4 0.172 0.402 0.406 -0.293 41.9
28-1 B 913.4 978.4 574.3 404.1 0.161 0.375 0.369 -0.330 47.2
28-2 T 887.9 960.8 557.6 403.2 0.181 0.422 0.437 -0.262 37.5
28-2 C 880.1 951.1 523.0 428.1 0.166 0.387 0.385 -0.314 44.9
28-2 B 893.3 956.5 561.7 394.8 0.160 0.373 0.367 -0.333 47.6
28-3 T 881.9 959.4 553.9 405.6 0.191 0.446 0.474 -0.225 32.2
28-3 C 894.2 964.8 561.4 403.4 0.175 0.408 0.415 -0.285 40.7
28-3 B 900.5 964.0 566.6 397.4 0.160 0.373 0.366 -0.333 47.6
56-1 T 886.9 970.4 557.1 413.3 0.202 0.471 0.531 -0.169 24.1
56-1 C 836.2 905.4 525.8 379.5 0.182 0.426 0.455 -0.244 34.9
56-1 B 905.6 974.9 568.8 406.0 0.171 0.398 0.413 -0.286 41.0
56-2 T 924.6 996.5 581.8 414.7 0.173 0.405 0.421 -0.278 39.8
56-2 C 912.1 985.5 573.0 412.5 0.178 0.415 0.437 -0.262 37.5
56-2 B 913.3 982.1 574.7 407.4 0.169 0.394 0.407 -0.293 41.9
56-3 T 918.7 991.4 578.7 412.7 0.176 0.411 0.432 -0.267 38.2
56-3 C 915.5 987.9 576.7 411.1 0.176 0.410 0.432 -0.268 38.3
56-3 B 917.2 983.1 577.7 405.4 0.163 0.379 0.386 -0.314 44.8
112-1 T 928.8 1007.4 584.4 423.0 0.186 0.433 0.467 -0.233 33.3
112-1 C 915.7 993.8 576.2 417.5 0.187 0.436 0.471 -0.228 32.6
112-1 B 907.5 982.9 570.9 412.0 0.183 0.427 0.457 -0.243 34.7
112-2 T 915.6 994.1 575.7 418.3 0.188 0.438 0.473 -0.226 32.3
112-2 C 922.9 997.9 582.3 415.6 0.181 0.421 0.448 -0.252 36.0
112-2 B 910.9 978.8 574.5 404.3 0.168 0.392 0.404 -0.295 42.3
112-3 T 925.1 1002.5 583.6 418.9 0.185 0.431 0.463 -0.236 33.8
112-3 C 924.8 998.2 582.4 415.8 0.176 0.412 0.433 -0.267 38.1
112-3 B 927.8 996.6 585.2 411.4 0.167 0.390 0.401 -0.299 42.7
86
The measured slump was 245mm. C-0.7 was very similar to C-0.65 in terms of bleed water and
segregation. The segregation is again apparent from the average results of the top, center, and
bottom measured w/c. However, larger ponds of bleed water were visible; lowering the w/c ratio
substantially. The bleed water was not measured.
87
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 988.9 1026.5 613.4 413.1 0.091 0.289 0.268 -0.183 40.6
28-1 C 982.8 1022.0 611.9 410.1 0.096 0.304 0.284 -0.168 37.2
28-1 B 970.4 1009.6 602.5 407.1 0.096 0.306 0.286 -0.166 36.7
28-2 T 984.4 1021.7 611.9 409.8 0.091 0.289 0.268 -0.183 40.6
28-2 C 987.2 1023.9 613.5 410.5 0.090 0.285 0.263 -0.188 41.7
28-2 B 978.1 1014.4 608.2 406.2 0.090 0.284 0.263 -0.188 41.7
28-3 T 985.0 1023.7 611.8 411.9 0.094 0.299 0.278 -0.173 38.4
28-3 C 980.2 1018.4 609.0 409.3 0.093 0.296 0.276 -0.176 38.9
28-3 B 973.1 1010.0 605.1 404.9 0.091 0.290 0.269 -0.182 40.4
56-1 T 992.7 1031.3 617.5 413.8 0.093 0.296 0.285 -0.167 36.9
56-1 C 998.2 1024.0 614.0 410.0 0.063 0.200 0.190 -0.262 58.0
56-1 B 975.1 1013.5 605.4 408.1 0.094 0.299 0.287 -0.164 36.4
56-2 T 997.2 1030.7 619.1 411.6 0.081 0.258 0.245 -0.207 45.7
56-2 C 992.1 1026.6 615.2 411.4 0.084 0.267 0.253 -0.198 43.9
56-2 B 980.6 1015.9 608.1 407.8 0.087 0.275 0.262 -0.189 41.9
56-3 T 1006.0 1040.8 624.9 415.9 0.084 0.266 0.253 -0.198 44.0
56-3 C 997.7 1031.3 619.2 412.1 0.082 0.259 0.246 -0.206 45.5
56-3 B 983.7 1018.1 610.5 407.6 0.084 0.268 0.255 -0.196 43.5
112-1 T 999.2 1046.3 629.2 417.1 0.113 0.358 0.358 -0.094 20.8
112-1 C 997.3 1044.1 628.8 415.3 0.113 0.358 0.357 -0.094 20.9
112-1 B 983.5 1031.7 619.2 412.5 0.117 0.371 0.374 -0.078 17.2
88
These results were difficult to analyse. The values measured were considerably lower than the
actual w/c. The 28 day test and the 56 day test yielded similar results, but the 112 day test
showed less error. Reducing the k coefficient for the degree of hydration only resulted in
lowering the overall w/c ratio in the calculations; therefore adjusting for hydration would only
increase the error. This was the first time slag was used in the testing program, and a higher
level of high range water reducer was needed to satisfy the higher water demand of the slag. The
slump of this mix was 50mm. This resulted in a mix that exhibited no signs of segregation. In
order to follow up with these results, more testing on the slag cement mixes were required.
89
0.500
Calcualted Water Cement Ratio
0.450
0.400
0.350
0.45 0.5 0.55 0.6 0.65 0.7
Designed Water Cement Ratio
It is quite clear that this test can distinguish if segregation has occurred in a cylinder.
Unfortunately, most of the calculated w/c failed to come close to the actual w/c. This was due to
severe segregation issues and excessive bleed water from high w/c concrete. C-0.5 had the
closest average results with an average error of 4.7%. C-0.45 had the second lowest average
error of 13.1%.
Figure 4-7 shows the distribution for all the concrete cores tested. The water contents per kg/m3
for each mix designs are labeled.
W/C
0.75
294.8 kg/m3
0.70
276.9 kg/m3
0.65
243.9 kg/m3
0.60
202.5 kg/m3 221.5 kg/m3
0.55
0.50
178.3 kg/m3
0.45
0.40
0.35
0.30
To better mimic site conditions, concrete slabs were cast to eliminate wall affects from cylinder
molds. The concrete slabs were cast so that four 100mm diameter core samples could be taken.
From those cores a 50mm thick section were cut from the center. The concrete slabs and
cylinders were kept in the moist room until the day of testing.
Table 4.41 shows a summary of the four concrete mix designs used in Phase Two. A full mix
design for each batch can be found in Appendix A.
May 9-13 S-0.4 0.408 375.0 0.0 149.7 754.6 1147.6 3.26
May 9-13 S-0.45 0.451 375.0 0.0 168.5 735.0 1114.7 0.72
May 16-13 S-0.5 0.499 375.0 0.0 187.2 708.3 1084.1 0.00
May 16-13 S-0.5S 0.509 281.23 93.8 187.2 705.5 1079.8 3.81
The S in the ID# represents that slabs testing was the primary focus; cylinders were made to help
supplement the data. The fine and coarse aggregates are expressed at SSD conditions, and
HRWR was added during mixing to achieve a workable slump for casting cylinders and slabs.
92
Table 4.42 show the exact mass of the materials used when batching the concrete. The batch size
was designed to cast three concrete slabs that could yield four 100mm diameter core samples
from each. The remaining concrete would then be used to cast 100mm diameter cylinders.
After mixing, the fresh density of each concrete batch was measured to determine yield. The
fresh density was then used to adjust the original mix design to determine paste content as a
volume percent of the total mix.
S-0.4 2434.9 2535.2 391.2 0.0 156.2 787.2 1197.2 3.41 0.2704
S-0.45 2405.4 2490.3 390.1 0.0 175.2 764.6 1159.6 0.75 0.2886
S-0.5 2373.4 2502.6 398.6 0.0 199.0 752.8 1152.3 0.00 0.3106
S-0.5S 2362.5 2505.2 299.7 99.9 199.5 751.6 1150.5 4.06 0.3147
A concrete slab was removed at 28 days and one at 56 days; four cores were obtained from each
slab to measure w/c. Cylinders were used to test the compressive strength of the concrete, and
the remaining cylinders were cut into three sections and tested for w/c. The third concrete slab
has not been tested as it was designed to be tested after a minimum of a year to maximize the
degree of hydration.
93
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 941.7 992.4 587.6 404.7 0.125 0.442 0.466 0.059 14.3
28-1 C 924.6 976.8 574.3 402.5 0.130 0.458 0.493 0.085 20.9
28-1 B 967.4 1013.5 603.6 409.9 0.113 0.397 0.399 -0.009 2.1
28-2 T 971.6 1015.6 608.5 407.1 0.108 0.382 0.378 -0.030 7.4
28-2 C 920.9 964.0 576.4 387.6 0.111 0.393 0.393 -0.015 3.7
28-2 B 909.1 953.8 568.0 385.8 0.116 0.409 0.416 0.008 2.1
28-3 T 977.2 1021.3 609.9 411.4 0.107 0.378 0.373 -0.035 8.5
28-3 C 988.9 1032.9 618.1 414.8 0.106 0.375 0.369 -0.039 9.7
28-3 B 936.9 978.8 585.5 393.3 0.107 0.377 0.371 -0.037 9.1
28-C1 940.0 980.9 586.8 394.1 0.104 0.366 0.358 -0.050 12.2
Core
28-C2 934.1 975.2 583.3 391.9 0.105 0.370 0.363 -0.045 11.0
28-C3 935.6 974.3 583.9 390.3 0.099 0.350 0.337 -0.071 17.3
28-C4 931.9 971.1 581.9 389.2 0.101 0.356 0.344 -0.063 15.6
56-1 T 972.9 1022.9 609.6 413.3 0.121 0.427 0.455 0.047 11.6
56-1 C 998.3 1047.7 625.7 422.0 0.117 0.414 0.435 0.027 6.6
56-1 B 968.3 1018.6 605.7 412.9 0.122 0.430 0.462 3.074 753.7
56-2 T 984.4 1035.3 617.8 417.5 0.122 0.431 0.461 0.054 13.1
56-2 C 981.0 1029.3 615.9 413.4 0.117 0.413 0.433 0.025 6.2
56-2 B 944.5 990.0 592.6 397.4 0.114 0.404 0.421 0.013 3.1
56-3 T 977.3 1026.2 613.0 413.3 0.118 0.418 0.441 0.033 8.2
56-3 C 972.7 1019.8 610.9 408.9 0.115 0.406 0.424 0.016 4.0
56-3 B 954.0 1000.0 600.1 399.9 0.115 0.407 0.424 0.016 4.0
56-C1 933.2 978.5 585.6 393.0 0.115 0.408 0.426 0.018 4.4
Core
56-C2 929.9 975.7 583.1 392.6 0.117 0.412 0.433 0.025 6.2
56-C3 931.4 976.7 583.5 393.2 0.115 0.407 0.425 0.017 4.1
56-C4 933.6 978.8 586.7 392.1 0.115 0.407 0.425 0.017 4.1
94
The 28 day core samples gave worse estimates of w/c than the 28 day cylinders, while the 56 day
core samples had better results than the cylinder samples. However, the results are quite similar,
and no major difference was visible between tests with core samples or cylinders. The average
results from all the slices tested show that the w/c was estimated fairly well.
95
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 957.9 1007.3 600.1 407.2 0.121 0.405 0.422 -0.029 6.5
28-1 C 940.5 992.5 587.6 404.8 0.128 0.429 0.458 0.007 1.6
28-1 B 941.2 991.7 588.3 403.4 0.125 0.418 0.442 -0.009 2.0
28-2 T 941.3 992.3 586.5 405.8 0.126 0.419 0.444 -0.008 1.7
28-2 C 937.2 988.3 584.2 404.1 0.126 0.422 0.447 -0.004 0.9
28-2 B 942.1 989.7 587.3 402.4 0.118 0.395 0.407 -0.044 9.7
28-3 T 941.4 993.8 587.7 406.1 0.129 0.430 0.461 0.010 2.2
28-3 C 930.9 980.6 580.3 400.3 0.124 0.414 0.436 -0.016 3.5
28-3 B 942.9 993.3 588.8 404.5 0.125 0.416 0.439 -0.012 2.7
28-C1 914.3 960.8 571.7 389.1 0.119 0.399 0.413 -0.038 8.4
Core
28-C2 917.0 963.2 572.4 390.8 0.118 0.394 0.407 -0.044 9.8
28-C3 922.6 968.2 577.3 390.9 0.117 0.389 0.399 -0.052 11.5
28-C4 908.1 955.3 566.8 388.4 0.122 0.406 0.423 -0.028 6.2
56-1 T 982.8 1038.8 616.8 422.0 0.133 0.443 0.481 0.030 6.7
56-1 C 958.0 1013.7 600.3 413.4 0.135 0.450 0.493 0.042 9.3
56-1 B 965.1 1019.7 605.7 414.0 0.132 0.440 0.477 0.026 5.7
56-2 T 975.7 1031.9 611.4 420.5 0.134 0.446 0.487 0.036 7.9
56-2 C 949.8 1007.5 593.2 414.3 0.139 0.464 0.519 0.067 14.9
56-2 B 959.3 1012.2 601.4 410.8 0.129 0.430 0.460 0.009 2.0
56-3 T 955.7 1014.8 597.0 417.8 0.142 0.472 0.533 0.082 18.1
56-3 C 954.0 1014.6 597.3 417.3 0.145 0.484 0.556 0.105 23.2
56-3 B 956.9 1013.5 599.5 414.0 0.137 0.457 0.505 0.054 11.9
56-C1 917.3 970.5 574.1 396.4 0.134 0.448 0.490 0.039 8.7
Core
56-C2 919.1 971.4 575.5 395.9 0.132 0.441 0.478 0.027 6.1
56-C3 929.3 980.8 584.0 396.8 0.130 0.433 0.466 0.015 3.3
56-C4 910.9 962.3 570.3 392.0 0.131 0.438 0.473 0.022 4.9
96
The average w/c results seemed to be accurate. The 56 day test samples have a larger water
uptake than the 28 day tests, resulting in a higher calculated w/c.
97
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 943.8 1001.0 590.5 410.4 0.139 0.428 0.446 -0.053 10.7
28-1 C 931.7 986.9 581.8 405.1 0.136 0.419 0.431 -0.068 13.7
28-1 B 944.9 998.5 592.2 406.3 0.132 0.405 0.411 -0.088 17.6
28-2 T 934.7 992.3 585.0 407.3 0.141 0.434 0.456 -0.044 8.7
28-2 C 932.4 987.6 584.7 402.9 0.137 0.421 0.434 -0.065 13.0
28-2 B 934.6 988.1 585.2 403.0 0.133 0.408 0.416 -0.084 16.7
28-3 T 915.9 971.0 572.5 398.5 0.138 0.424 0.440 -0.059 11.9
28-3 C 926.2 982.6 580.5 402.1 0.140 0.431 0.450 -0.049 9.8
28-3 B 930.5 983.6 582.3 401.3 0.132 0.406 0.413 -0.086 17.3
28-C1 906.0 951.1 562.8 388.3 0.116 0.357 0.344 -0.155 31.0
Core
28-C2 896.4 946.4 560.3 386.2 0.129 0.398 0.401 -0.099 19.8
28-C3 897.6 955.8 566.7 389.2 0.150 0.460 0.497 -0.002 0.4
28-C4 885.3 935.0 553.5 381.6 0.130 0.400 0.404 -0.095 19.1
56-C1 918.7 973.0 578.1 394.9 0.137 0.422 0.448 -0.051 10.3
Core
56-C2 919.6 972.6 577.3 395.3 0.134 0.412 0.432 -0.067 13.5
56-C3 919.8 972.2 577.8 394.4 0.133 0.408 0.426 -0.073 14.6
56-C4 918.1 972.8 576.0 396.8 0.138 0.424 0.450 -0.049 9.8
98
Once again the 56 day core samples have a higher w/c than the 28 day samples. But the percent
error is still high. This shows the extreme variability, as compared to the cylinder results from C-
0.5 in Phase One, the average percent error was -4.7%.
99
Dm Wm Sm V W/C %
Day- # ID Ps Ep W/C
(g) (g) (g) (cm3) Diff. Error
28-1 T 933.4 989.5 584.8 404.7 0.139 0.417 0.439 -0.070 13.7
28-1 C 916.1 977.7 573.4 404.4 0.152 0.458 0.509 -0.001 0.2
28-1 B 922.5 981.5 577.4 404.1 0.146 0.439 0.475 -0.034 6.8
28-2 T 925.1 983.5 578.7 404.9 0.144 0.434 0.466 -0.044 8.6
28-2 C 897.7 961.5 561.6 399.9 0.159 0.479 0.547 0.037 7.3
28-2 B 907.6 964.9 566.7 398.2 0.144 0.433 0.464 -0.045 8.8
28-3 T 927.9 985.6 581.2 404.4 0.143 0.429 0.459 -0.051 10.0
28-3 C 912.0 973.1 570.8 402.2 0.152 0.457 0.506 -0.004 0.7
28-3 B 915.3 971.2 571.9 399.4 0.140 0.421 0.446 -0.064 12.5
28-C1 899.9 951.1 562.8 388.3 0.132 0.397 0.410 -0.100 19.6
Core
28-C2 891.2 943.1 577.6 365.5 0.142 0.427 0.454 -0.055 10.8
28-C3 906.1 957.5 567.6 389.9 0.132 0.396 0.409 -0.101 19.8
28-C4 896.8 947.9 560.9 387.0 0.132 0.397 0.410 -0.099 19.5
56-C1 905.4 963.8 569.4 394.4 0.148 0.445 0.486 -0.023 4.5
Core
56-C2 898.9 955.2 565.7 389.5 0.144 0.434 0.467 -0.043 8.4
56-C3 897.6 956.9 563.2 393.7 0.151 0.453 0.500 -0.010 1.9
56-C4 892.4 949.2 561.1 388.1 0.146 0.440 0.476 -0.034 6.6
100
The 56 day core samples show better results for measured w/c. The 28 day core samples seem to
yield lower values of w/c. These results show that at later age, slag concrete samples can be
tested using this test method to achieve reasonable results.
101
0.500
W/C
0.450
0.400
S-0.4 S-0.45 S-0.5 S-0.5S
Figure 4-8: Graphical Representation of the Effects of Cylinder Location in Phase Two
102
This graph shows that segregation did not occur to the same extent as the Phase One results.
Although the bottom slice did for the most part have the lowest w/c, the center and the top values
alternated.
When comparing the core and cylinder results the cylinders resulted in a higher overall w/c than
the cores. This could be due to the wall effects causing an excess of cement paste on the outer
edges of the cylinder. The core samples eliminate the wall effects. Figure 4-9 displays this by
comparing the 28 and 56 day results. Unfortunately, not enough cylinders were cast to conduct a
56 day test for C-0.5 and C-0.5S. However, the 28 day results followed the trend as described
above.
103
0.550
0.500
W/C
0.450
0.400
0.350
S-0.4 S-0.45 S-0.5 S-0.5S
28-Day Core 56-Day Core 28 Cylinder 56 Cylinder
To better illustrate the trend, the average measured w/c for cylinders and cores are plotted in
Figure 4-10.
104
0.450
W/C
0.400
0.350
Figure 4-10: Average W/C Results for All Cores and Cylinders
Figure 4-11 shows the w/c distribution of all the samples tested in Phase Two.
105
W/C
0.60
0.55
0.50
0.45
0.40
0.35
0.30
S-0.4 S-0.45 S-0.5 S-0.5S
Cylinder Actual W/C Core
Figure 4-11: Measured W/C Distribution for Phase Two Concrete
106
10
Percent Error % in Terms of W/C
0
Total Top
-5 Total Centre
Total Bottom
-10 All Samples
-15
-20
Unfortunately, higher w/c concrete had high levels of segregation causing large errors in the w/c
estimates.
Table 4.53: Percent Error in Estimation of W/C for Hardened Concrete in Phase One
10
Average Percent Error in Terms of W/C
-10
Total Top
-40
-50
C-0.45 C-0.5 C-0.55 C-0.6 C-0.65 C-0.7
Testing to determine the w/c of fresh concrete failed for higher w/c; however, the test easily
showed the extent of segregation and indicated that the overall water content in each cylinder
was considerably lower than intended.
Sellevold recommended using a graph to determine w/c of hardened concrete samples based on
the degree of hydration and paste porosity (Sellevold, 2005). Figure 4-14 shows a similar graph
using the paste porosity (Ɛp) calculated in Equation [3.12] to determine the hardened w/c:
Ɛp = Ps/Vp [3.12]
Once the paste porosity Ɛp is determined it can be equated to the theoretical paste porosity Ɛ′p
determined in Equation [3.18].
[ ]
[3.18]
Equation [3.18] is graphed in Table 4-12 for w/c ranging from 0 to 1. Using the graph and
solving Equation [3.12], the hardened w/c can be determined.
109
0.7
0.65
0.6
0.55
0.5
Paste Porosity (Ɛp) [Fraction]
0.45
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Water Cement Ratio
Figure 4-14: Optical Aid in Determining the W/C of Hardened Concrete Using Equation
[3-15]
110
Compression tests were done to calculate the 28 day strength of each concrete batched. The
strengths results for all concrete samples are provided in Table 4.54.
The values measured were not as expected for the C class concrete used in Phase One. C-0.5 had
a lower compressive strength than C-0.55. Regular practice would suggest similar concrete with
a lower w/c would have a higher compressive strength. In this case it was not. When looking at
the calculated w/c from Phase One, it too showed that the calculated w/c for C-0.55 was much
lower than that of C-0.5 indicating segregation had a large impact on the water content of each
cylinder cast. In addition, C-0.65 had a higher compressive strength then C-0.6, while the
hardened concrete tests confirm C-0.65 had a lower calculated w/c relative to C-0.6. These
results are plotted on Figure 4-15 and 4-16 to better illustrate the trend.
111
60
55
50
45
Compressive Strength MPa
40
35
30
25
20
15
10
0
0.45 0.5 0.55 0.6 0.65 0.7
Water Cement Ratio
0.400
Calcualted Water Cement Ratio
0.450
0.500
The two graphs illustrate segregation during mixing and how sampling compromised the true
w/c of each cylinder, as both the compressive strength and the calculated w/c both yield similar
curves.
113
After resolving the segragtion issue and repeating the tests with a lower w/c in Phase Two, the
compressive strength tests made more sense. Figure 4-17 shows the results of all the compressive
strength testing.
50
Compressive Strength MPa
40
30
20
10
0
0.4 0.45 0.5 0.55 0.6 0.65 0.7
Water Cement Ratio
Chapter 5
5.1.2 A sample size of 1500g ±100g should be used when conducting the microwave
oven test. When compared to a smaller sample size such as 500g, the duration of
testing decreased substantially; however, it was difficult to obtain a representative
sample. The addition or removal of one piece of coarse aggregate can greatly
affect the aggregate to cement ratio at small sample sizes. When increasing the
sample size to 2000g, the duration of testing also increased as more water was
required to be heated. The AASHTO test and the ASTM-draft both recommend
using 1500g ±10g and this sample size did allow for easy sampling of a
representative sample with a relatively short drying period.
5.1.4 If time permits, the microwave heating process should continue until a mass loss
between consecutive readings is less than 0.5g. The ASTM-draft states a mass
loss of 1.0g before termination; however, tests with a longer drying time will have
improved accuracy when calculating the w/c. This may also reduce premature
termination of the test when there is still evaporable water in the system.
5.1.5 When performing the test on concrete with w/c between 0.4-0.55 with 100%
Portland cement, the deviation from the design w/c was within 0.05 and with good
practice and representative samples, the deviation was below 0.03 compared to the
design w/c.
5.1.6 This test requires the use of a concrete mix design in order to calculate an
aggregate correction factor and cement content. Without this information this test
cannot accurately determine the fresh w/c of a concrete sample. However, this test
can still be used as a tool to evaluate variability, as identical mix designs will tend
to have similar water contents. The microwave test can accurately measure the
total water content of each concrete mix to act as a quality control measure.
5.2.2 A second microwave oven could be used in order to conduct duplicate tests of the
same mix at the same time to better measure test variability.
116
5.2.3 A large assortment of aggregates should be tested to measure the effects of the
aggregate correction factor.
5.3.2 For optimal efficiency, the concrete should be initially oven dried at 105°C for a
minimum of two days. A three day drying period is recommended or until less
than 0.5g of mass loss is measured in 24 hours. The sample should be saturated in
water after the dry mass is recorded for a minimum of four days. If time permits, a
five day period is recommended or until a mass increase of less than 0.5g is
measured in 24 hours.
5.3.3 No significant difference was seen in measuring the w/c of hardened concrete
with sample thicknesses ranging from 30 to 50mm. A 100mm diameter cylinder
with a 50mm thickness is recommended.
5.3.4 Concrete batched with a w/c of 0.5 and lower had an average error less than 0.03
from the design w/c. The higher w/c concrete gave significant error. Segregation
during casting of samples with w/c above 0.55 caused large variability and
lowered the accuracy of the test results. Concrete with lower w/c and better
cohesion yielded more accurate results.
5.3.5 The slag seemed to have no significant effect on the absorption and w/c calculated
in later age concrete. The 28 day test for the mix containing slag had a much
lower measured w/c than the 56 day test, as sufficient hydration had not occurred
at early ages to obtain accurate results.
117
5.3.6 Tested core samples consistently had a lower measured w/c than the same
concrete cast in cylinders. Due to wall effects from the cylindrical molds used for
the concrete test slices, there is a larger paste to aggregate ratio along the outer
edges. This marginal increase in cement paste increased the water uptake of the
sample, increasing the measured w/c of the sample.
5.3.7 The modified PF-method used for determining the w/c of hardened concrete gave
a large degree of variability, especially for mixtures that segregate. Similar
concrete mix designs had errors of 4% to 13.1%. Even concrete samples tested
from the same concrete batches gave a wide spread of w/c values. However, for
cylinders cut into top, center, and bottom sections, a consistent trend was visible
showing the degree of segregation throughout the cylinder. The PF-method may
not be as accurate for measuring the w/c as found by Sellevold (standard deviation
of 0.05), but it is does provide an indication of concrete segregation.
5.4.2 Measure concrete with air entraining admixtures to determine if the air
entrainment will inflate the measured w/c. Use mixes with supplementary
cementing materials, such as silica fume to measure the effects of decreased
permeability on the measured w/c.
5.4.3 Compare w/c test results with optical microscopy methods such as thin section
analysis.
118
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123
Appendix A
Identification Number: P0
Mix date Sept-19-12
Batch Size 0.0202 m3
Batch Size 20.2 L
Water Cement Ratio 0.4051
Designed Paste Content 0.2947 m3
Identification Number: P1
Mix date Jul-5-12
3
Batch Size 0.0178 m
Batch Size 17.8 L
Water Cement Ratio 0.4018
3
Designed Paste Content 0.3005 m
Field Data
Identification Number: P2
Mix date Oct-3-12
Batch Size 0.0199 m3
Batch Size 19.9 L
Water Cement Ratio 0.4124
Designed Paste Content 0.3025 m3
Field Data
Identification Number: P3
Mix date 14-Nov-12
Batch Size 0.0200 m3
Batch Size 20.0 L
Water Cement Ratio 0.4154
Designed Paste Content 0.2559 m3
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data
Field Data