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US Army Corps
of Engineers
UI I iIIiIIt llIii
Nlil
Waterways Experiment
Station
DTIC
SELECIE~
SEP2aS9 3
93-22422
1347'C QtTALrm'
Final report
Approved for public release; distribution is unlimited
Preface............................................. iv
l-Introduction .. ..................................... I
2-Fineness Uniformity . ................................ 2
Relationship Between Fineness Uniformity Statistic
and Within-Source Variation .......................... 2
Effect of Sampling Procedures on Levels of Within-Source Variation . 3
Discussion of Sampling Procedures ........................ 4
Importance of Fineness Uniformity on Strength ............... 5
3-Evaluation of Butler and Kanare's Correction ................. 8
Calibration of 45-pm Sieve .............................. 8
4-General Discussion and Conclusions ...................... 10
References . ........................................ 11
SF 298
Iil
Preface
The work described in this report was conducted by the Structures Labo-
ratory (SL), U.S. Army Engineer Waterways Experiment Station (WES) for
the U.S. Army Corps of Engineers (USACE) under Civil Works Investiga-
tional Study Work Unit 32680, "Relatig Variations in Properties of Cements
and Pozzolans to Changes in Concrete." Dr. Tony Liu (CECW-EG) was the
USACE Technical Monitor.
All work was conducted under the general supervision of Mr. Bryant
Mather, Director, SL; Mr. James T. Ballard, Assistant Director, SL; and
Mr. Kenneth L. Saucier, Chief, CTD, SL.
Dr. Robert W. Whalin was the Director of WES. Commander was COL
Bruce K. Howard, EN.
iv
1 Introduction
Ch~apter 1 Introduction 1
2 Fineness Uniformity
D - im-xi
where D is the maximum difference between the mean of the previous ten
samples (iro) and the value for the sample currently under test (x-). This
requirement is set at 5 percent by C 618. In order to estimate the frequency
with which D will exceed the 5 percent requirement, the variance in D (s2D)
must be determined. The variance for a given source is related to the within-
source variance among samples (s2), as follows:
' . + $2 _ 1.1S2
10
2sD- . IWo
s z 2.38%
The rclevant Spccfiion, ASTM C 618 cites ASTM Mcthods C 311 for sampling require-
merts, C 311 requires that any sample tested for finencas not reprcsent more than 400 tons.
1Th,; conclusion to be drawn from this analysis is that the high number of
specification failures in the fineness uniformity property are expected given
the size of the within-source variation common to many fly ash sources when
sampled by grab samples. These fly ash sources are commonly used by the
Corps of Engineers and are believed to perform satisfactorily.
The result of the forgoing analysis is that type of sampling, composite vs.
grab, is an important factor in determining likelihood of compliance with
specification requirements. ASTM C 311 gives no guidance on sampling
except that it allows a sample to be either composite or grab, and it should not
represent more than 400 tons of fly ash. The composi . sampling practiced by
some fly ash producers probably exceeds the limit of 400 tons per sample. If
grab sampling is to remain a legitimate sampling technique for monitoring
uniformity, then either the specification limit must be increased or some pro-
ducers must reduce the variability of their product.
5
Chapter 2 Finenees Uniformity
In order to gain some insight into the direct effect of fineness uniformity
on strength, fineness was analyzed against the pozzolanic activity index (PAI),
as described in ASTM C 311-89. This is a test that compares strength of a
portland cement-fly ash mortar to the strengtn of the equivalent portland-
cement mortar. Fly asb represents 35 percent of the cementitious material, by
volume. Results are expressed as a percentage of control. Water content of
both mortars is adjusted to a constant flow, so the indirect effect of fineness
on water demand is accounted for. Strengths are measured after 28 days of
curing at 100 "F, consequently, this test best measures relatively long-term
strength-development potential of materials. A subsample of the WES test
data described above was also used to perform this analysis. These data were
chosen from sources that represented extremes in fineness as well as from
some that represented the more common intermediate values. Six sources
were represented. The PAI test conducted at 380C (1000F) was a require-
ment of C 618 and C 311 in 1988. It is not included at present. The data
obtained from it are regarded as useful for the purposes of this report.
Ravina (1980) did a similar analysis based on fly ash collected from vari-
ous precipitator fields of in a single source. Fineness varied from 9.7 percent
to 35 percent.
Results from both sets of data are presented in Figure 2. The WES data
shows considerable scatter about the linear regression line, due to effects of
different cements and fly ashes, as well as to other unidentified sources of
systematic error, and to random testing error. The slope of the regression
line indicates that, on the average, one should expect a decrease in PAI of
about 1.2 percent for every 1 percent increase in fineness. The Ravint data
shows less error about its regression line, due probably to the better control
on materials used in testing. The slope of this regression indicates a decrease
in strength of 2.1 percent for every 1 percent increase in fineness. The aver-
age slope from the two analyses is 1.6 percent.
Butler and Kanare (1989) have analysed sieve corrections and determined
that the correction factor should be determined by the simple difference
between the nominal value and the measured residue of the SRM:
The final test result is then calculated by adding the correction factor to the
measured fineness. Butler and Kanar's correction results in a smaller CF for
a given difference in nominal and measured residue.
The effect on the final test result of the difference between these two cor-
rection procedures is very small when little sieve correction is needed, or
when fineness of an unknown is close to the fineness of the SRM used to
correct the sieve. The effect becomes substantial as the size of the correction
factor becomes large or whea the fineness of an unknown is much different
from the fineness of the SRM.
The nominal 45-pim sieve residue for SRM fineness standards is about
10 percent, so the test results on fly ashes whose fineness is with a few per-
cent of this value are not seriously affected by the method for calculating the
The Cement and Concrete Reference Laboratory (CCRL) fly ash profi-
ciency sample numbers 7 and 8 were selected because of their relatively
coarse particle size. Thirty-eight laboratories provided enough information to
compare test results calculated from the C 430 correction procedure and the
Butler-Kanare correction procedure.
In ASTM C 670, 1d2a" is "acccuble difference between two results on test portions of the
same mateel."
9
Chapter 3 Evaluation of Butter and Kanare's Correction
4 General Discussion and
Conclusions
American Society for Testing and Materials (ASTM). (1988). "Standard test
methods for sampling and testing fly ash or natural pozzolan for use as a
mineral admixture in portland-cement concrete," Designation: C 311-88,
Concrete and Aggregates 04.02, Philadelphia, PA.
Butler, W. B., and H. M. Kanare. (1989). "Testing fly ash for fineness to
ASTM C 430: Sieve calibration." MaterialsResearch Society Symposium
Proceedings 138, 107-112.
Referene1
Table 1
Summary of Within-Source Standard Deviations, Taken From
Composite and Grab Samples, and Failures of the Uniformity
Requirement
Sid. Dev.
Nominal Composite Sid. 0ev. Grab Expected Observed
Source Class Fineness Samples (n) Samples in) Failures Failures
AR C 15 0.96 (20)
NE C 16 2.35 (20)
NV F 26 2.63 (20)
TX-I C 15 2.56(20)
WA-2 C 10 1.56(8)
Totals 60.9 55
Table 2
Comparison of Sieve Corrections Using CCRL Data
Correction Method Mean Finenes _ Standard Deviation F-test Comparison
CCRL 7
CCRL 8
10 -----
------ ---
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(D
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E
z
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0.0-0.9 1.0-1.9 2.0-2.9 3.0-3.9 >4.0
Stardard Deviation
U Composite samples EM Grab samples
-------
S12 0
C? 6
1001 03 05
40
0 10 20 30 40 50
Finenss (% retained)
WES Data Ravina Data
40
U,
30
20 ... .
I I I ,t
40
CCD El
30
20l
SI I I...i..
15
0- 10
L.
5 -
0
70 80 90 100 110 120 130 140 150
Calibration Factor
30
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24
22
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40
35 .-- _ _ _ _
I=s
20
25
15 [t1
(6) (4) (2) 0 2 4
Correction Factor, Proposed Method
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1. AGENCY USE ONLY fLeave 404n1) 2. REPORT DATE 3. REPORT TYPE AND OATES COVERED
Problems with Fineness Testing of Coal Fly Ash for Use in Concrete Study Work Unit 32680
6. AUTHOR(S)
Toy S. Poole
Available from National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161.
The specification governing use of coal fly ash in concrete (ASTM C 618) includes a fineness-
uniformity requirement. This requirement is frequently exceeded. The relationship between product
variation and the probability of exceeding this requirement was developed. It was found that a
product standard deviation in fineness (including testing error) of less than or equal to 2.38 percent
would be required to ensure that a material would meet the uniformity requirement in 95 percent of
samples. Product standard deviation is strongly dependent on sampling techniques. Many apparently-
good fly ashes fail to meet the C 618 level of uniformity when sampled by grab samples, but more
meet the requirement when analysis is done on composite samples.
An error in the calibration of sieves used in the testing of fly ash fineness and a corrective
action has been published. In this work, CCRL data collected on two very coarse samples were used
to evaluate the improvement in testing error associated with the change. The between-laboratory
standard deviation for the existing test method were found to be 4.6 percent. It was reduced to 2.4
percent when the new procedure was applied.
14. SUBJECT TERMS IS. NUMBER OF PAGES