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Contact ASTM International (www.astm.org) for the latest information
Designation: C311 – 11
Standard Test Methods for
Sampling and Testing Fly Ash or Natural Pozzolans for Use
in Portland-Cement Concrete1
This standard is issued under the fixed designation C311; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (ϵ) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* notes (excluding those in tables) shall not be considered as
1.1 These test methods cover procedures for sampling and requirements of this standard.
testing fly ash and raw or calcined pozzolans for use in 2. Referenced Documents
portland-cement concrete.
2.1 ASTM Standards:2
1.2 The procedures appear in the following order:
C33 Specification for Concrete Aggregates
C109/C109M Test Method for Compressive Strength of
Sections
Sampling 7
Hydraulic Cement Mortars (Using 2-in. or [50-mm] Cube
CHEMICAL ANALYSIS Specimens)
Reagents and apparatus 10 C114 Test Methods for Chemical Analysis of Hydraulic
Moisture content 11 and 12
Loss on ignition 13 and 14 Cement
Silicon dioxide, aluminum oxide, iron oxide, calcium oxide, C150 Specification for Portland Cement
magnesium oxide, sulfur trioxide, sodium oxide C151 Test Method for Autoclave Expansion of Hydraulic
and potassium oxide 15
Available alkali 16 and 17 Cement
Ammonia 18 C157/C157M Test Method for Length Change of Hardened
PHYSICAL TESTS Hydraulic-Cement Mortar and Concrete
Density 19
Fineness 20 C185 Test Method for Air Content of Hydraulic Cement
Increase of drying shrinkage of mortar bars 21-23 Mortar
Soundness 24 C188 Test Method for Density of Hydraulic Cement
Air-entrainment of mortar 25 and 26
Strength activity index with portland cement 27-30 C204 Test Methods for Fineness of Hydraulic Cement by
Water requirement 31 Air-Permeability Apparatus
Effectiveness of Fly Ash or Natural Pozzolan in C226 Specification for Air-Entraining Additions for Use in
Controlling Alkali-Silica Reactions 32
Effectiveness of Fly Ash or Natural Pozzolan in the Manufacture of Air-Entraining Hydraulic Cement
Contributing to Sulfate Resistance 34 C227 Test Method for Potential Alkali Reactivity of
Cement-Aggregate Combinations (Mortar-Bar Method)
1.3 The values stated in SI units are to be regarded as the C430 Test Method for Fineness of Hydraulic Cement by the
standard. The values given in parentheses are provided for 45-µm (No. 325) Sieve
information purposes only. C441 Test Method for Effectiveness of Pozzolans or
1.4 This standard does not purport to address all of the Ground Blast-Furnace Slag in Preventing Excessive Ex-
safety concerns, if any, associated with its use. It is the pansion of Concrete Due to the Alkali-Silica Reaction
responsibility of the user of this standard to establish appro- C604 Test Method for True Specific Gravity of Refractory
priate safety and health practices and determine the applica- Materials by Gas-Comparison Pycnometer
bility of regulatory limitations prior to use. C618 Specification for Coal Fly Ash and Raw or Calcined
1.5 The text of this standard references notes and footnotes Natural Pozzolan for Use in Concrete
that provide explanatory information. These notes and foot- C670 Practice for Preparing Precision and Bias Statements
for Test Methods for Construction Materials
C778 Specification for Sand
1
These test methods are under the jurisdiction of ASTM Committee C09 on
Concrete and Concrete Aggregates and are the direct responsibility of Subcommit-
2
tee C09.24 on Supplementary Cementitious Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2011. Published April 2011. Originally contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM
approved in 1953. Last previous edition approved in 2007 as C311–07. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C0311-11. the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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C311 – 11
C1012 Test Method for Length Change of Hydraulic- 5. Materials
Cement Mortars Exposed to a Sulfate Solution 5.1 Graded Standard Sand—The sand used for making test
C1157 Performance Specification for Hydraulic Cement specimens for the activity index with lime or portland cement
C1437 Test Method for Flow of Hydraulic Cement Mortar shall be natural silica sand conforming to the requirements for
D1426 Test Methods for Ammonia Nitrogen In Water graded standard sand in Specification C778.
D4326 Test Method for Major and Minor Elements in Coal
NOTE 1—Segregation of Graded Sand—The graded standard sand
and Coke Ash By X-Ray Fluorescence should be handled in such a manner as to prevent segregation, since
2.2 ACI Document:3 variations in the grading of the sand cause variations in the consistency of
ACI 201.2R Guide to Durable Concrete the mortar. In emptying bins or sacks, care should be exercised to prevent
the formation of mounds of sand or craters in the sand, down the slopes
of which the coarser particles will roll. Bins should be of sufficient size to
3. Terminology
permit these precautions. Devices for drawing the sand from bins by
3.1 Definitions of Terms Specific to This Standard: gravity should not be used.
3.1.1 composite sample—a sample that is constructed by 5.2 Hydrated Lime— The hydrated lime used in the tests
combining equal portions of grab or regular samples. shall be reagent-grade calcium hydroxide, 95 % minimum
3.1.2 established source—a source for which at least six calculated as Ca(OH)2 (Note 2), and have a minimum fineness
months of continuous production quality assurance records of 2500 m2/kg as determined in accordance with Test Method
from a test frequency required for a new source are available, C204.
sampled at the source.
3.1.3 grab sample—a sample that is taken in a single NOTE 2—The calcium hydroxide should be protected from exposure to
carbon dioxide. Material remaining in an opened container after a test
operation from a conveyor delivering to bulk storage, from should not be used for subsequent tests.
bags, or from a bulk shipment. Such a sample may, or may not,
reflect the composition or physical properties of a single lot of 5.3 Portland Cement— The portland cement used in the
fly ash or natural pozzolan. This type of sample can be used to Strength Activity Index with Portland Cement test shall comply
characterize small amounts of material. with the requirements of Specification C150 and have a
3.1.4 jobsite or new source—a source for which less than minimum compressive strength of 35 MPa (5000 psi) at 28
six months of production records are available, sampled at the days and total alkalies (Na2O + 0.658 K 2O) not less than
source. 0.50 % nor more than 0.80 %.
3.1.5 lot—specific quantity of fly ash or natural pozzolan 5.3.1 The use of a locally available portland cement in the
offered for inspection at any one time. A lot may be one storage Strength Activity Index or a project cement that does not meet
bin or the contents of one or more transport units representing the requirements of the section on Materials is permitted when
material drawn from the same storage bin. the variations from the requirements of the section on Materials
are reported and when the use of such portland cement is
3.1.6 regular sample—a sample that is constructed by
requested.
combining equal portions of grab samples that were taken at
predetermined times or locations from any single lot of 6. Sample Type and Size
material.
6.1 Grab samples and regular samples shall have a mass of
at least 2 kg (4 lb).
4. Significance and Use
6.2 Grab samples or regular samples taken at prescribed
4.1 These test methods are used to develop data for com- intervals over a period of time (see Table 1), may be combined
parison with the requirements of Specification C618. These test to form a composite sample representative of the fly ash or
methods are based on standardized testing in the laboratory and natural pozzolan produced during that period of time.
are not intended to simulate job conditions. 6.3 Composite samples shall have a mass of at least 4 kg (8
4.1.1 Strength Activity Index—The test for strength activity lb).
index is used to determine whether fly ash or natural pozzolan 6.4 The sampling shall be done by, or under the direction of,
results in an acceptable level of strength development when a responsible representative of the purchaser.
used with hydraulic cement in concrete. Since the test is
performed with mortar, the results may not provide a direct
TABLE 1 Minimum Sampling and Testing FrequencyA
correlation of how the fly ash or natural pozzolan will
contribute to strength in concrete. Jobsite or New Established
Test Sample Type
SourceB SourceB
4.1.2 Chemical Tests— The chemical component determi-
Moisture content Regular Daily or each Daily or each
nations and the limits placed on each do not predict the Loss on ignition 90 Mgc 360 MgC
performance of a fly ash or natural pozzolan with hydraulic Fineness (100 Tons) (400 Tons)
cement in concrete, but collectively help describe composition Density and the other Composite Monthly or each Monthly or each
tests in Specification 1 800 MgC (2 000 2 900 MgC
and uniformity of the material. C618, Tables 1 and 2 Tons) (3 200 Tons)
A
It should be noted that the minimum test frequency given in Table 1 is not
necessarily the frequency needed for quality control programs on some fly ash or
natural pozzolans.
3 B
Available from American Concrete Institute (ACI), P.O. Box 9094, Farmington For definitions, refer to the Terminology section.
C
Hills, MI 48333-9094, http://www.aci-int.org. Whichever comes first.
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C311 – 11
7. Sampling Procedure MOISTURE CONTENT
7.1 The fly ash or natural pozzolan may be sampled by any 11. Procedure
one of the following methods:
11.1 Dry a weighed sample, as received, to constant weight
7.1.1 From Bulk Storage at Point of Discharge or from Rail in an oven at 105 to 110 °C (221 to 230 °F).
Cars and Road Tankers—A sample may be taken by siphon
tube during loading or by sampling tube from each loaded car 12. Calculation
or tanker. If the load is sampled at the point of discharge into 12.1 Calculate the percentage of moisture to the nearest
the rail car or tanker, the top surface shall be removed to a 0.1 %, as follows:
depth of at least 200 mm (8 in.) before sampling. The sample Moisture content, %5~A/B!3100 (1)
shall be identified with at least the date and shipment number.
7.1.2 From Bags in Storage—The regular sample shall where:
comprise increments of equal size taken by sampling tube from A = mass loss during drying, and
three bags selected at random from one lot of bagged material. B = mass as received.
The sample shall be identified with date and lot number. LOSS ON IGNITION
7.1.3 From Conveyor Delivering to Bulk Storage—Take
one sample of 2 kg (4 lb) or more of the material passing over 13. Procedure
the conveyor. This may be secured by taking the entire test 13.1 Determine loss on ignition in accordance with the
sample in a single operation, known as the grab sample procedures outlined in Test Methods C114, except that the
method, or by combining several equal portions taken at material remaining from the determination of moisture content
regular intervals, known as the regular sample method. Auto- shall be ignited to constant mass in an uncovered porcelain, not
matic samplers may be used to obtain samples. platinum, crucible at 750 6 50 °C (1382 6 190 °F).
7.2 Samples shall be treated as described in Section 8.
14. Calculation
NOTE 3—Some methods of loading or delivery of fly ash or natural 14.1 Calculate the percentage of loss on ignition to the
pozzolan, particularly from an airstream or conveyor belt, may create nearest 0.1, as follows:
stratification or segregation in the material stream. Sampling techniques
must be designed to ensure that the sample is representative of the material Loss on ignition, %5~A/B!3100 (2)
shipped.
where:
8. Preparation and Storage of Samples A = loss in mass between 105 and 750 °C (221 and 1382
°F),
8.1 Prepare composite samples for the tests required in B = mass of moisture-free sample used.
Section 9, by arranging all grab or regular samples into groups
covering the period or quantity to be represented by the SILICON DIOXIDE, ALUMINUM OXIDE, IRON OXIDE,
sample. Take equal portions from each, sufficient to produce a CALCIUM OXIDE, MAGNESIUM OXIDE, SULFUR
composite sample large enough for the tests required. Mix the TRIOXIDE, SODIUM OXIDE AND POTASSIUM OXIDE
composite sample thoroughly.
15. Procedure
8.2 Samples shall be stored in clean, airtight containers
15.1 Determine the percentages of these oxides as required
identified with the source and lot or period of time represented.
in accordance with the applicable sections of Test Methods
Untested portions of the sample shall be retained for at least
C114 for materials having an insoluble residue greater than
one month after all test results have been reported.
1 % (Note 4). Analysts performing sodium oxide and potas-
sium oxide determinations shall observe the precautions out-
9. Testing Frequency lined in the applicable section of Performance Specification
9.1 General—When required, the purchaser shall specify C1157 (refer to the section on Test Methods). Most pozzolans
the amount of testing for available alkalies, reactivity with dissolve completely in lithium borate fluxes.
cement alkalies, drying shrinkage, and air-entrainment. Make NOTE 4—Rapid and instrumental methods may be employed similar to
all other tests on regular or composite samples chosen as those in Test Methods C114 and D4326.
specified in Table 1.
AVAILABLE ALKALI
CHEMICAL ANALYSIS
16. Procedure
10. General 16.1 Weigh 5.0 g of the sample and 2.0 g of hydrated lime
on a piece of weighing paper, carefully mix using a metal
10.1 All apparatus, reagents and techniques shall comply spatula, and transfer to a small plastic vial of approximately
with the requirements of Test Methods C114. 25-mL capacity. Add 10.0 mL of water to this mixture, seal the
10.2 Purity of Water— Unless otherwise indicated, refer- vial by securing the cap or lid to the vial with tape (Note 5),
ences to water shall be understood to mean distilled water or blend by shaking until the mixture is uniform, and store at
water of equal purity. 38 6 2 °C.
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C311 – 11
NOTE 5—To ensure that moisture loss from the paste does not occur, NW = ammonia concentration of the water extract deter-
place the sealed vial in a sealable container (such as a small sample or
mined by Test Methods D1426, mg/L,
mason jar), add sufficient water to cover the bottom of the container, and
seal.
VW = volume of water used for extracting ammonia from
the fly ash sample, mL, and
16.2 Open the vial at the age of 28 days and transfer the Wfa = Mass of fly ash sample used in the test, g.
contents to a 250-mL casserole. Break up and grind the cake
with a pestle, adding a small amount of water, if necessary, so PHYSICAL TESTS
that a uniform slurry containing no lumps is obtained (Note 6).
Add sufficient water to make the total volume 200 mL. Let DENSITY
stand 1 h at room temperature with frequent stirring. Filter 19. Procedure
through a medium-textured filter paper onto a 500-mL volu-
19.1 Determine the density of the sample in accordance
metric flask. Wash thoroughly with hot water (eight to ten
with the procedure described in Test Method C188 or Test
times).
Method C604 as modified below.
NOTE 6—At times it may be necessary to break the vial and peel off the 19.2 For Test Method C188, follow the procedure except
plastic from the solid cake. In such cases, care should be exercised to use a quantity of fly ash or natural pozzolan weighed to the
avoid the loss of material and to remove all solid material from the
nearest 0.05 g, of about 50 g.
fragments of the vial. If the cake is too hard to break up and grind in the
casserole, a mortar should be used. 19.3 For Test Method C604 use an amount of material that
is appropriate for the instrument.
16.3 Neutralize the filtrate with dilute HCl (1 + 3), using 1 19.3.1 Determine the density of the material as received. Do
to 2 drops of phenolphthalein solution as the indicator. Add not prepare sample as described in Section 6 of Test Method
exactly 5 mL of dilute HCl (1 + 3) in excess. Cool the solution C604.
to room temperature and fill the flask to the mark with distilled 19.4 In the final report of the density value, indicate which
water. Determine the amount of sodium and potassium oxides test method was used in measuring density.
in the solution using the flame photometric procedure, de-
scribed in Test Methods C114, except that the standard FINENESS, AMOUNT RETAINED WHEN WET-SIEVED ON
solutions shall be made up to contain 8 mL of calcium chloride A45-µm (NO. 325) SIEVE
(CaCl2) stock solution per litre of standard solution, and the
solution as prepared shall be used in place of the solution of 20. Procedure
cement. 20.1 Determine the amount of the sample retained when
wet-sieved on a 45-µm (No. 325) sieve, in accordance with
NOTE 7—The standard solutions made up with 8 mL of calcium
chloride (CaCl2) stock solution contain the equivalent of 504 ppm of CaO. Test Method C430, with the following exceptions.
Tests have shown that this amount closely approximates the amount of 20.1.1 Calibrate the 45-µm (No. 325) sieve using a cement
calcium dissolved in the test solution. standard (SRM 114). Calculate the sieve correction factors as
follows:
17. Calculation and Report
CF5std2obs (5)
17.1 Calculate the results as weight percent of the original
sample material. Report as equivalent percentage of sodium where:
oxide (Na2O), calculated as follows: CF = the sieve correction factor, %, (include a negative
Equivalent Na 2O, % 5 Na2O, %10.658 3 K2O, % (3)
sign when appropriate),
std = the certified residue value for the SRM, %, and
AMMONIA obs = the observed residue value for the SRM, %.
20.1.2 Calculate the fineness of the fly ash or natural
18. Procedure pozzolan to the nearest 0.1 % as follows:
18.1 Weigh 1.00 g of the fly ash sample into a 125 mL RC5RS1CF (6)
Erlenmeyer flask. Add 100 mL of ammonia-free water. Place a
neoprene rubber stopper on the flask and swirl the contents to where:
thoroughly mix the sample and the water. RC = corrected sieve residue, %,
18.2 Filter the mixture using a medium-textured filter paper RS = observed residue for the test sample, %, and
and save the filtrate for the ammonia determination. CF = the sieve correction factor, %.
18.3 Determine the concentration of ammonia in the filtrate If the residue retained for the test sample is equal to zero
in accordance with the procedures outlined in Test Methods (RS = 0), then the sieve correction factor shall not be added to
D1426, Method A–Direct Nesslerization or Method B–Selec- the test result to calculate the corrected sieve residue. In such
tive Ion Electrode. cases, the corrected fineness shall be reported as zero.
18.4 Calculate the ammonia concentration of the fly ash as NOTE 8—Test Method C430 has been adopted for testing fly ash
follows: fineness. However, certain requirements, such as cleaning of sieves and
Ammonia, mg/kg 5 NW 3 VW/Wfa (4) interpretation of the test results, are sometimes not appropriate for fly
ashes.
20.2 Numerical examples for calibrating a fineness sieve
where: and calculating the corrected fineness.
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C311 – 11
20.2.1 Calibrating a fineness sieve (NIST standard reference where:
material SRM 114p was used in this example): S = drying shrinkage of test or control speci-
Certified residue retained on a 452µm sieve mens, %,
5 8.24 % ~obtained from standard certificate! initial CRD = difference between the comparator reading
of the specimen and the reference bar at 7
Measured residue retained on a 452µm sieve days of moist curing,
5 7.12 % ~measured in the laboratory! CRD = difference between the comparator reading
of the specimen and the reference bar at 28
Correction factor ~CF! 5 standard value ~std! – observed value ~obs! days of drying, and
5 8.24 – 7.12 G = the gage length of the specimens 250 mm (10
5 1.12 % in.).
20.2.2 Calculating a corrected fineness value for a cali- 23.2 Report the results to the nearest 0.01. If the average
brated sieve (fly ash A was used in this example): drying shrinkage of the control specimens is larger than the
average drying shrinkage of the test specimens, prefix a minus
Amount of fly ash A retained on the sieve: Rs
5 15.2 % ~expressed as a % of sample mass!
sign to the increase of drying shrinkage of mortar bars
reported.
Corrected sieve residue for fly ash A: Rc 5 Rs 1 CF
5 15.2 1 1.12
SOUNDNESS
5 16.3 %
24. Procedure
INCREASE OF DRYING SHRINKAGE OF MORTAR BARS 24.1 Conduct the soundness test in accordance with Test
Method C151, except that the specimens shall be molded from
21. Test Specimen
a paste composed of 25 parts by weight of fly ash or natural
21.1 Prepare test specimens in accordance with the proce- pozzolan and 100 parts by weight of a portland cement
dures described in Test Method C157/C157M, except mold conforming to Specification C150.
three mortar bars from both the control mix and the test mix
using the following proportions: AIR-ENTRAINMENT OF MORTAR
Control Mix Test Mix 25. Procedure
Portland cement, g 500 500
Fly ash or natural None 125 25.1 Using portland cement conforming to the requirements
pozzolan, g
Graded standard sand, g 1375 1250
for Type I or Type II of Specification C150, prepare a test
Water sufficient to produce a flow of 100 to 115 % mixture in accordance with Test Method C185, using the
following proportions:
Test Mix
Portland cement, g 300
22. Procedure Fly ash or natural pozzolan 75
22.1 Cure and measure the test specimens in accordance 20–30 standard sand, g 1125
Water, mL, sufficient to give a flow of 80 to 95 Y
with Test Method C157/C157M, except that the moist-curing Neutralized Vinsol resin solution, mL,A sufficient Z
period (including the period in the molds) shall be 7 days, and to produce an air content of 18 6 3 %
the comparator reading at the age of 24 6 1⁄2 h shall be omitted.
A
Immediately after taking the comparator reading at the end of The amount of Vinsol resin solution used shall be considered as part of the
mixing water.
the 7-day moist-curing period, store the specimens in accor-
dance with Test Method C157/C157M, and after 28 days of air
storage, take a comparator reading for the specimens in 25.2 The neutralized Vinsol resin solution used in this
accordance with Test Method C157/C157M. section on Air-Entrainment of Mortar shall be either a com-
mercial neutralized Vinsol resin solution or a neutralized
23. Calculation and Report Vinsol resin solution prepared in accordance with Specification
23.1 Calculate the increase in drying shrinkage of the C226. If it is necessary to dilute either of these solutions, use
mortar bars, Si, as follows: distilled or demineralized water. (Note 9.)
Si5St2Sc (7)
NOTE 9—Dissolved minerals in drinking water may precipitate Vinsol
where: resin solutions and greatly diminish its air-entraining characteristics.
St = average drying shrinkage of the test specimens calcu- 25.3 Prepare two test mixtures with sufficient neutralized
lated as follows, and Vinsol resin to produce an air content of 15 to 18 % in the first
Sc = average drying shrinkage of the control specimens mix and 18 to 21 % in the second mix. Then, determine by
calculated as follows: interpolation the amount of Vinsol resin, expressed as weight
@initial CRD 2 CRD# 3 100 percent of the cement, required to produce an air content of
S5 G (8) 18 %.
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C311 – 11
26. Calculation from the moist room or closet and remove the cubes from the
26.1 Calculate the air content of the test mixtures as molds. Place and store the cubes in saturated lime water as
follows: specified in Test Method C109/C109M.
Air content, volume %5100[12~Wa/W c!# (9) NOTE 10—Take care to ensure against zones of stratification or pockets
of variation in temperature in the curing chamber.
Wa5W/400 (10)
300111251751~300 3 P 3 0.01! 29. Compressive Strength Test
Wc5 (11)
FS D S D S D S
300 1125 75
3.15 1 2.65 1 D 1
300 3 P 3 0.01
1 DG 29.1 Determine the compressive strength, as specified in
Test Method C109/C109M, of three specimens of the control
where: mixture and three specimens of the test mixture at ages of 7
Wa = actual weight per unit of volume of mortar as days, or 28 days, or both, depending upon how many speci-
determined by Test Method C185, g/mL, mens were molded as prescribed in the section on Number of
W = weight of the specified 400 mL of mortar (see Test Specimens.
Method C185), g,
Wc = theoretical weight per unit of volume, calculated on 30. Calculation
an air-free basis and using the values for density and 30.1 Calculate the strength activity index with portland
quantities of the materials in the mix, g/mL, cement as follows:
P = percentage of mixing water plus Vinsol resin solution Strength activity index with portland cement =
based on weight of cement, and (A/B) 3 100 (11)
D = density of fly ash or natural pozzolan in the mixture,
Mg/m3.
where:
STRENGTH ACTIVITY INDEX WITH PORTLAND CEMENT A = average compressive strength of test mixture cubes,
MPa (psi), and
27. Specimens B = average compressive strength of control mix cubes,
27.1 Mold the specimens from a control mixture and from a MPa (psi).
test mixture in accordance with Test Method C109/C109M.
The portland cement used in the Strength Activity Index test WATER REQUIREMENT
shall comply with the requirements of Specification C150 and
with the alkali and strength limits given in the section on 31. Calculation
Materials. In the test mixture, replace 20 % of the mass of the 31.1 Calculate the water requirement for the Strength Ac-
amount of cement used in the control mixture by the same mass tivity Index with Portland Cement as follows:
of the test sample. Make six-cube batches as follows: Water requirement, percentage of control =
27.1.1 Control Mixture: (Y/242 3 100) (12)
where:
500 g of portland cement Y = water required for the test mixture to be 65 of control
1375 g of graded standard sand
242 mL of water flow.
EFFECTIVENESS OF FLY ASH OR NATURAL POZZOLAN
27.1.2 Test Mixture: IN CONTROLLING ALKALI SILICA-REACTIONS (SEE
Appendix X1)
400 g of portland cement
100 g of test sample 32. Procedure
1375 g of graded standard sand
mL of water required for flow 6 5 of control mixture 32.1 Determine expansion of mortar made with a fly ash or
natural pozzolan and a test cement as a percent of expansion of
27.2 Number of Specimens: mortar made with low alkali cement in accordance with Test
27.2.1 Since Specification C618 specifies that “meeting the Method C441 as modified in the following paragraphs:
7 day or 28 day Strength Activity Index will indicate specifi- 32.1.1 Control Mixture— The control mixture will be made
cation compliance” only one age might be required. At the as required in Test Method C441 except that the control cement
option of the producer or the user after preparing six-cube shall have an alkali content (as equivalent Na2O) less than
batches, only three cubes of control and test mixtures need to 0.60 % (Note 11).
be molded for either 7 or 28 day testing. NOTE 11—Generally, the control cement should have an alkali content
as equivalent Na2O between 0.50 and 0.60 %. However, lower alkali
28. Storage of Specimens control cement may be used, if desired, to demonstrate equivalence.
28.1 After molding, place the specimens and molds (on the 32.1.2 Test Mixture Using Fly Ash or Natural Pozzolan—
base plates) in the moist room or closet at 23.0 6 2.0 °C The combined quantity of cement plus fly ash or natural
(73.4 6 3 °F) for 20 to 24 h. While in the moist room or closet, pozzolan shall total 400 g (see Appendix X1). Use 900 g of
protect the surface from dripping water. Remove the molds borosilicate glass aggregate and sufficient mixing water to
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produce a flow between 100 and 115 % as determined in that Type II cements are often used for moderate levels of exposure. Type
accordance with Test Method C1437. The cement used in the V cement is commonly used for severe exposures (see X2.2 of Appendix
test mixture shall have an alkali content greater than that of the X2).
cement in the control mixture (Note 12). 34.5 Test Mixture for Using Fly Ash or Natural Pozzolan for
NOTE 12—Generally, this test cement will have an alkali content equal Procedure B—Make the combined quantity of cement plus fly
to or higher than that used in the job. ash or natural pozzolan, by mass, the same as the total cement
used in the control mixture. The proportion of fly ash or natural
32.1.3 Store and measure specimens as required in Test
pozzolan may be varied from 15 % to 50 % of the total cement
Method C227. Measure length of specimens at ages of 1 and 14
plus fly ash or natural pozzolan by mass. Any type of portland
days.
cement may be used to prepare test mixtures.
33. Report 34.6 For either Procedure A or B, store and measure
33.1 Include in the report for each test mixture comparison specimens as required in Test Method C1012 for at least 6
made: months.
33.1.1 The 14 day expansion of the test mixture as a percent NOTE 14—Evaluation of the sulfate resistance of cementitious materials
of the control mixture at that age, for use in certain situations or critical structures may require longer
33.1.2 The identification and chemical analysis of the fly periods of storage and additional length measurements. Refer to Test
ash or natural pozzolan, Method C1012 for guidance on this matter.
33.1.3 The mass percentage of fly ash or natural pozzolan
based on the total mass of cement plus fly ash or natural 35. Report
pozzolan in the test mixture, and 35.1 In addition to the information required in Test Method
33.1.4 The alkali content of control and test mixture ce- C1012, report the following information for each mixture
ments as equivalent alkali (Na2O + 0.658 K2O). comparison made:
35.2 For Procedure A, the age and expansion as a specific
EFFECTIVENESS OF FLY ASH OR NATURAL POZZOLAN amount,
IN CONTRIBUTING TO SULFATE RESISTANCE
35.3 For Procedure B, the age and expansion as a percent of
34. Procedure the control mixture at that age,
35.4 The identification and chemical analysis including C3A
34.1 Compare the length change of mortar bars with abso-
content of the cements used in both the control and test
lute expansion limits or compare the length change of mortar
mixtures,
bars made with a control cement with the length change of
mortar bars made with fly ash or natural pozzolan and a test 35.5 The identification and chemical analysis of the fly ash
cement, in accordance with Test Method C1012, as modified in or natural pozzolan used in the test mixtures,
the following paragraphs. Results shall be evaluated using 35.6 The mass percentages of the fly ash or natural pozzolan
absolute limits (Procedure A) or the relative expansion limits based on the total mass of cement plus fly ash or natural
(Procedure B) in Specification C618, Table 2A. pozzolan in the test mixture.
34.2 Control Mixture for Procedure A—A control mixture is
not mandatory since performance measured using Procedure A PRECISION AND BIAS
is based on maximum expansion of the test mixture. If a
control mixture is made for Procedure A then proportion it as 36. Precision and Bias
required in Test Method C1012 using a cement meeting the 36.1 Strength Activity Index Test:
requirements of Specification C150, Type II or Type V.
36.1.1 Precision was determined from two interlaboratory
34.3 Test Mixture Using Fly Ash or Natural Pozzolan for
studies involving two Class C fly ashes, two Class F fly ashes,
Procedure A—Make the combined quantity of cement plus fly
ash or natural pozzolan, by mass, the same as the total cement
content of the control mixture described in the Making Mortars
TABLE 2 Within and Between Lab Precision Estimates for C114
section of Test Method C1012. The proportion of fly ash or Methods Applied to the Analysis of Fly AshA
natural pozzolan may be varied using from 15 % to 50 %, by
1s d2s
mass, of the total cement plus fly ash or natural pozzolan. Any Oxide
W/L B/L W/L B/L
type of portland cement may be used to prepare test mixtures.
34.4 Control Mixture for Procedure B—Make the control SiO2 0.62 0.86 1.75 2.45
Al2O3 1.46 2.29 4.12 6.48
mixture for Procedure B as required in Test Method C1012 Fe2O3
with the cement that is proposed for use in the project or a <2 % 0.12 0.11 0.34 0.31
cement that through performance or definition (Specification $2 % 0.12 0.25 0.34 0.71
CaO 0.63 0.74 1.79 2.09
C150, Section 1) is expected to give satisfactory results (or a MgO 0.20 0.21 0.55 0.61
cement for which the contribution to sulfate resistance is SO3 0.10 0.16 0.28 0.45
known and is satisfactory). Moisture 0.05 0.06 0.15 0.17
LOI 0.09 0.12 0.25 0.35
NOTE 13—The control cement should be chosen to give sulfate resis- A
The four values for SO3 were editorially corrected to reflect updated research
tance for the expected level of sulfate exposure. Experience has shown reports associated with this standard.
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C311 – 11
and one Class N pozzolan. Participating laboratories numbered 36.2.2 Precision—Within-laboratory (W/L) and between-
12 and 7 in the two studies.4 laboratory (B/L) estimates of standard deviation and estimates
36.1.2 The single-operator standard deviation for the of maximum differences expected between duplicate determi-
Strength Activity Index test has been found to be 3.7 % (1s). nations in 95 % of comparisons6 are summarized in Table 2.
This does not appear to vary either with material or with test 36.2.3 Bias—Statistically significant bias was found in the
age, over the range of 7 to 28 days. Therefore, results of two determination of CaO and MgO. CaO determinations averaged
properly conducted tests by the same operator on the same 0.46 % higher than the value certified for the SRM. MgO
material should not differ by more than 10.5 % (d2s) of the determinations averaged 0.19 % higher than the value certified
average of the two results. for the SRM.
36.1.3 The multilaboratory standard deviation for the 36.3 Ammonia:
Strength Activity Index test has been found to be 4.5 % (1s). 36.3.1 Precision of Method A (Direct Nesslerization) – The
This does not appear to vary either with material or with test single-laboratory coefficient of variation (repeatability) has
age, over the range of 7 to 28 days. Therefore, results of two been found to be 9.2 % (1s %). The reproducibility of this test
properly conducted tests in different laboratories on the same method is being determined and will be available on or before
material should not differ by more than 12.7 % (d2s) of the July 2010.
average of the two results. 36.3.2 Precision of Method B (Selective Ion Electrode) –
36.1.4 Since there is no accepted reference material suitable The single-laboratory coefficient of variation (repeatability)
for determining the bias for this procedure, no statement on has been found to be 7.4 % (1s %). The reproducibility of this
bias is being made. test method is being determined and will be available on or
36.2 Chemical Analysis: before July 2010.
36.2.1 Precision and bias estimates for the test methods in 36.3.3 Bias—Since there is no accepted reference material
Test Methods C114 when applied to the analysis of pozzolans suitable for determining the bias for these procedures, no
were calculated from an interlaboratory study involving 7 statement on bias is being made.
laboratories each analyzing 4 NIST SRM fly ashes. A research
report describing the results of this study is available from 37. Keywords
ASTM.5
37.1 fly ash; natural pozzolan
4
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:C09-1001.
5 6
Supporting data have been filed at ASTM International Headquarters and may These values represent, respectively, the (1s) and (d2s) limits as described in
be obtained by requesting Research Report RR:C09-1008. Practice C670.
APPENDIXES
(Nonmandatory Information)
X1. COMMENTARY ON SECTION 32
X1.1 Test procedures in Section 32 are designed to deter- test mixture with cements having alkali contents that do not
mine the effectiveness of fly ash, or natural pozzolan, in exceed by more than 0.05 percentage points the alkali content
preventing excessive expansion resulting from a reaction of the cement used in the test mixture.
between certain aggregates and alkalies in portland-cement
mixtures. Tests are made in accordance with Test Method C441 X1.4 Selection of the Percentage of Fly Ash or Natural
using: Pozzolan—It may be necessary to make test mixtures with
several percentages of fly ash or natural pozzolan to determine
X1.1.1 400 g of portland cement or a combined total of
the minimum amount necessary to be considered “effective” in
cement plus fly ash or natural pozzolan of 400 g,
reducing expansion to the level produced by the “control”
X1.1.2 900 g of borosilicate glass, and
low-alkali cement. The minimum amount of fly ash or natural
X1.1.3 Sufficient water to obtain a flow of 100 to 115 %.
pozzolan should be 15 % by weight of cementitious material.
X1.2 The control mixture is made with a low-alkali
portland cement. The test mixture, made of a test percentage of X1.5 Selection of the Alkali Content of the Cement Used in
the fly ash or natural pozzolan, can be made with the same the Test Mixture—In some instances it may not be necessary to
cement or any other cement having an equivalent alkali content demonstrate that the fly ash or natural pozzolan will reduce
greater than 0.60 %. expansion, but rather that it will not increase expansion. In this
instance the test and control mixtures should be made with the
X1.3 Interpretation of Results—The fly ash or natural same low alkali cement used in the control mixture to better
pozzolan should be considered “effective” when used at delineate any increase in expansion. The fly ash or natural
percentages equal to or greater than the percentages used in the pozzolan percentage used may need to be sufficiently high to
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C311 – 11
demonstrate that the percentage exceeds the pessimum if such contain rapidly reactive constituents but do not exceed 0.05 %
pessimum exists for the combination. expansion in three months or 0.10 % expansion in six months
when tested with the control cement in Test Method C227. In
X1.6 Selection of the Low Alkali Control Cement—The test such instances the control cement used in this test method
procedure in this test method and requirements in Specification should have an alkali content as required to control the
C618 are designed to measure the relative effectiveness of the expansive reactions of the aggregates being used, for example
fly ash or natural pozzolan in reducing expansion due to in the 0.50 to 0.60 % range. See the appendix to Specification
alkali-silica reactions. The effectiveness is a function of both C33.
the alkali content of the cement used in the test mixture and the
percentage of fly ash or natural pozzolan. The higher the alkali X1.6.1 Certain reactive aggregates have been identified
content of the test mixture cement and the lower the percentage which produce deleterious expansion after many years of
of fly ash or natural pozzolan used, the more effective the fly service when used with cements with equivalent alkali contents
ash or natural pozzolan. This test procedure and the 100 % well below 0.60 %. Often these reactive aggregates do not
criterion of Specification C618 can be used as a guide to produce expansions in Test Method C227 exceeding those
enhance field performance of job mixtures if it is assumed that discussed in the appendix of Specification C33 until a much
use of the low alkali control cement will prevent excessive later age, perhaps one or two years. In such instances the use
expansion in service with materials proposed for use in the job. of a control cement with an alkali content significantly less
This is the situation when the aggregates proposed for use than 0.60 % is appropriate.
X2. COMMENTARY ON SECTION 34
X2.1 The test procedures in Section 34 are designed to addition of fly ash or natural pozzolan influences sulfate
evaluate the performance of particular fly ashes or natural resistance. However, as referenced in Test Method C1012,
pozzolans in contributing to the resistance or durability of research has indicated that mortars meeting the expansion
concrete in a sulfate environment. Tests are made on mortars in criteria will perform adequately. Under Procedure B, the fly ash
accordance with Test Method C1012. or natural pozzolan will be considered to be able to contribute
to sulfate resistance if the expansion of the test mixture does
X2.2 The control mixture should be made with a cement not exceed that of the control mixture at an exposure time of at
that by performance or definition (Specification C150, Section
least 6 months. It is recommended that the proportion of fly ash
1.1) is expected to give satisfactory results for the anticipated
or natural pozzolan used in the test mixture be the same one
level of sulfate exposure. ACI 201.2R recommends Type II
proposed for use in the project 6 2 %, and that the C3A content
cement when the sulfate content, expressed as SO4, is 0.10 to
of the project cement be equal to, or less than, that which was
0.20 percent in soils or 150 to 1500 ppm in waters. ACI 201.2R
used in the test mixtures. See Appendix X1, Technical Back-
recommends Type V cements when the sulfate content, ex-
ground, Test Method C1012.
pressed as SO4, is 0.20 to 2.0 % in soils, or 1500 to 10 000 ppm
in waters. The test mixtures for both procedures may be made
with varying percentages of fly ash or natural pozzolan. Test X2.4 Selection of the Percentage of Fly Ash or Natural
mixtures can use cements with equal or higher or lower C3A Pozzolan—It may be necessary to make test mixtures with
contents that might not have given satisfactory results when several percentages of fly ash or natural pozzolan to determine
used alone. the amount necessary to obtain adequate resistance to different
concentrations of sulfates. Percentages used in a project should
X2.3 Interpretation of Results—The absolute expansion be within 2 % of those that are successful in the test mixtures
limits used in Procedure A make it difficult to ascertain how the or should be between two percentages that are successful.
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C311 – 11
SUMMARY OF CHANGES
Committee C09 has identified the location of selected changes to these test methods since the last issue,
C311–07, that may impact the use of these test methods. (Approved April 1, 2011)
(1) Revised Section 19.
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