Sampling and Testing Fly Ash or Natural Pozzolans For Use in Portland-Cement Concrete
Sampling and Testing Fly Ash or Natural Pozzolans For Use in Portland-Cement Concrete
Sampling and Testing Fly Ash or Natural Pozzolans For Use in Portland-Cement Concrete
3.2 Definitions of Terms Specific to This Standard: 5.2 Hydrated Lime—The hydrated lime used in the tests
3.2.1 composite sample, n—a sample that is constructed by shall be reagent-grade calcium hydroxide, 95 % minimum
combining equal portions of grab or regular samples. calculated as Ca(OH)2 (Note 3), and have a minimum fineness
of 2500 m2/kg as determined in accordance with Test Method
3.2.2 established source, n—a source for which at least six C204.
months of continuous production quality assurance records
from a test frequency required for a new source are available, NOTE 3—The calcium hydroxide should be protected from exposure to
carbon dioxide. Material remaining in an opened container after a test
sampled at the source.
should not be used for subsequent tests.
3.2.3 grab sample, n—a sample that is taken in a single 5.3 Portland Cement—The portland cement used in the
operation from a conveyor delivering to bulk storage, from Strength Activity Index with Portland Cement test shall comply
bags, or from a bulk shipment. with the requirements of Specification C150 and have a
3.2.3.1 Discussion—A grab sample may or may not reflect minimum compressive strength of 35 MPa (5000 psi) at 28
the composition or physical properties of a single lot of fly ash days and total alkalies (Na2O + 0.658 K2O) not less than
or natural pozzolan. This type of sample can be used to 0.50 % nor more than 0.80 %.
characterize small amounts of material. 5.3.1 The use of a locally available portland cement in the
3.2.4 new source, n—a source for which less than six Strength Activity Index or a project cement that does not meet
months of production records are available, sampled at the the requirements of the section on Materials is permitted when
source. the variations from the requirements of the section on Materials
3.2.5 regular sample, n—a sample that is constructed by are reported and when the use of such portland cement is
combining equal portions of grab samples that were taken at requested.
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).
3
Available from American Concrete Institute (ACI), P.O. Box 9094, Farmington 6.2 Grab samples or regular samples taken at prescribed
Hills, MI 48333-9094, http://www.aci-int.org. intervals over a period of time (see Table 1), may be combined
10. General
to form a composite sample representative of the fly ash or 10.1 All apparatus, reagents and techniques shall comply
natural pozzolan produced during that period of time. with the requirements of Test Methods C114.
6.3 Composite samples shall have a mass of at least 4 kg (8
10.2 Purity of Water—Unless otherwise indicated, refer-
lb).
ences to water shall be understood to mean distilled water or
6.4 The sampling shall be done by, or under the direction of, water of equal purity.
a responsible representative of the purchaser.
MOISTURE CONTENT
7. Sampling Procedure
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 mass in
7.1.1 From Bulk Storage at Point of Discharge or from Rail an oven at 110 6 5 °C [230 6 10 °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
the rail car or tanker, the top surface shall be removed to a 12.1 Calculate the percentage of moisture to the nearest
depth of at least 200 mm (8 in.) before sampling. The sample 0.1 %, as follows:
shall be identified with at least the date and shipment number.
7.1.2 From Bags in Storage—The regular sample shall Moisture content, % 5 ~ A/B ! 3 100 (1)
comprise increments of equal size taken by sampling tube from
three bags selected at random from one lot of bagged material. where:
The sample shall be identified with date and lot number. A = mass loss during drying, and
7.1.3 From Conveyor Delivering to Bulk Storage—Take one B = mass as received.
sample of 2 kg (4 lb) or more of the material passing over the
conveyor. This may be secured by taking the entire test sample LOSS ON IGNITION
in a single operation, known as the grab sample method, or by
combining several equal portions taken at regular intervals, 13. Procedure
known as the regular sample method. Automatic samplers may 13.1 Determine loss on ignition in accordance with the
be used to obtain samples. procedures outlined in Test Methods C114, except that the
7.2 Samples shall be treated as described in Section 8. material remaining from the determination of moisture content
shall be ignited to constant mass in an uncovered porcelain, not
NOTE 4—Some methods of loading or delivery of fly ash or natural
pozzolan, particularly from an airstream or conveyor belt, may create platinum, crucible at 750 6 50 °C.
stratification or segregation in the material stream. Sampling techniques
must be designed to ensure that the sample is representative of the material 14. Calculation
shipped.
14.1 Calculate the percentage of loss on ignition to the
8. Preparation and Storage of Samples nearest 0.1, as follows:
8.1 Prepare composite samples for the tests required in
Section 9, by arranging all grab or regular samples into groups Loss on ignition, % 5 ~ A/B ! 3 100 (2)
covering the period or quantity to be represented by the
where:
sample. Take equal portions from each, sufficient to produce a
composite sample large enough for the tests required. Mix the A = loss in mass between 110 and 750 °C,
B = mass of moisture-free sample used.
composite sample thoroughly.
NOTE 6—To ensure that moisture loss from the paste does not occur, where:
place the sealed vial in a sealable container (such as a small sample or NW = ammonia concentration of the water extract deter-
mason jar), add sufficient water to cover the bottom of the container, and mined by Test Methods D1426, mg/L,
seal.
VW = volume of water used for extracting ammonia from
16.2 Open the vial at the age of 28 days and transfer the the fly ash sample, mL, and
contents to a 250-mL casserole. Break up and grind the cake Wfa = mass of fly ash sample used in the test, g.
with a pestle, adding a small amount of water, if necessary, so
that a uniform slurry containing no lumps is obtained (Note 7). PHYSICAL TESTS
Add sufficient water to make the total volume 200-mL. Let
DENSITY
stand 1 h at room temperature with frequent stirring. Filter
through a medium-textured filter paper onto a 500-mL volu- 19. Procedure
metric flask. Wash thoroughly with hot water (eight to ten 19.1 Determine the density of the sample in accordance
times). with the procedure described in Test Method C188 or Test
NOTE 7—At times it may be necessary to break the vial and peel off the Method C604 as modified below.
plastic from the solid cake. In such cases, care should be exercised to
avoid the loss of material and to remove all solid material from the 19.2 For Test Method C188, follow the procedure except
fragments of the vial. If the cake is too hard to break up and grind in the use a quantity of fly ash or natural pozzolan weighed to the
casserole, a mortar should be used. nearest 0.05 g, of about 50 g.
16.3 Neutralize the filtrate with dilute HCl (1 + 3), using 1 19.3 For Test Method C604 use an amount of material that
to 2 drops of phenolphthalein solution as the indicator. Add is appropriate for the instrument.
exactly 5 mL of dilute HCl (1 + 3) in excess. Cool the solution 19.3.1 Determine the density of the material as received. Do
to room temperature and fill the flask to the mark with distilled not prepare sample as described in Section 6 of Test Method
water. Determine the amount of sodium and potassium oxides C604.
in the solution using the flame photometric procedure, de- 19.4 In the final report of the density value, indicate which
scribed in Test Methods C114, except that the standard test method was used in measuring density.
solutions shall be made up to contain 8 mL of calcium chloride
(CaCl2) stock solution per litre of standard solution, and the FINENESS, AMOUNT RETAINED WHEN WET-SIEVED ON
solution as prepared shall be used in place of the solution of A45-µm (NO. 325) SIEVE
cement.
20. Procedure
NOTE 8—The standard solutions made up with 8 mL of calcium
chloride (CaCl2) stock solution contain the equivalent of 504 ppm of CaO. 20.1 Determine the amount of the sample retained when
Tests have shown that this amount closely approximates the amount of wet-sieved on a 45-µm (No. 325) sieve, in accordance with
calcium dissolved in the test solution. Test Method C430, with the following exceptions.
where:
CF = the sieve correction factor, %, (include a negative
sign when appropriate), 22. Procedure
std = the certified residue value for the SRM, %, and
obs = the observed residue value for the SRM, %. 22.1 Cure and measure the test specimens in accordance
with Test Method C157/C157M, except that the moist-curing
20.1.2 Calculate the fineness of the fly ash or natural period (including the period in the molds) shall be 7 days, and
pozzolan to the nearest 0.1 % as follows: the comparator reading at the age of 24 6 1⁄2 h shall be omitted.
Immediately after taking the comparator reading at the end of
R C 5 R S 1CF (6) the 7-day moist-curing period, store the specimens in accor-
dance with Test Method C157/C157M, and after 28 days of air
where: storage, take a comparator reading for the specimens in
RC = corrected sieve residue, %, accordance with Test Method C157/C157M.
RS = observed residue for the test sample, %, and
CF = the sieve correction factor, %. 23. Calculation and Report
If the residue retained for the test sample is equal to zero 23.1 Calculate the increase in drying shrinkage of the
(RS = 0), then the sieve correction factor shall not be added to mortar bars, Si, as follows:
the test result to calculate the corrected sieve residue. In such
cases, the corrected fineness shall be reported as zero. Si 5 St 2 Sc (7)
NOTE 9—Test Method C430 has been adopted for testing fly ash where:
fineness. However, certain requirements, such as cleaning of sieves and
interpretation of the test results, are sometimes not appropriate for fly St = average drying shrinkage of the test specimens calcu-
ashes. lated as follows, and
Sc = average drying shrinkage of the control specimens
20.2 Numerical examples for calibrating a fineness sieve
calculated as follows:
and calculating the corrected fineness.
20.2.1 Calibrating a fineness sieve (NIST standard reference @ initial CRD 2 CRD# 3 100
S5 (8)
material SRM 114p was used in this example): G
(Nonmandatory Information)
X1.1 Test procedures in Section 32 are designed to deter- delineate any increase in expansion. The fly ash or natural
mine the effectiveness of fly ash, or natural pozzolan, in pozzolan percentage used may need to be sufficiently high to
preventing excessive expansion resulting from a reaction demonstrate that the percentage exceeds the pessimum if such
between certain aggregates and alkalies in portland-cement pessimum exists for the combination.
mixtures. Tests are made in accordance with Test Method C441
using: X1.6 Selection of the Low Alkali Control Cement—The test
X1.1.1 400 g of portland cement or a combined total of procedure in this test method and requirements in Specification
cement plus fly ash or natural pozzolan of 400 g, C618 are designed to measure the relative effectiveness of the
fly ash or natural pozzolan in reducing expansion due to
X1.1.2 900 g of borosilicate glass, and alkali-silica reactions. The effectiveness is a function of both
X1.1.3 Sufficient water to obtain a flow of 100 to 115 %. the alkali content of the cement used in the test mixture and the
percentage of fly ash or natural pozzolan. The higher the alkali
X1.2 The control mixture is made with a low-alkali portland content of the test mixture cement and the lower the percentage
cement. The test mixture, made of a test percentage of the fly of fly ash or natural pozzolan used, the more effective the fly
ash or natural pozzolan, can be made with the same cement or ash or natural pozzolan. This test procedure and the 100 %
any other cement having an equivalent alkali content greater criterion of Specification C618 can be used as a guide to
than 0.60 %. enhance field performance of job mixtures if it is assumed that
X1.3 Interpretation of Results—The fly ash or natural use of the low alkali control cement will prevent excessive
pozzolan should be considered “effective” when used at expansion in service with materials proposed for use in the job.
percentages equal to or greater than the percentages used in the This is the situation when the aggregates proposed for use
test mixture with cements having alkali contents that do not contain rapidly reactive constituents but do not exceed 0.05 %
exceed by more than 0.05 percentage points the alkali content expansion in three months or 0.10 % expansion in six months
of the cement used in the test mixture. when tested with the control cement in Test Method C227. In
such instances the control cement used in this test method
X1.4 Selection of the Percentage of Fly Ash or Natural should have an alkali content as required to control the
Pozzolan—It may be necessary to make test mixtures with expansive reactions of the aggregates being used, for example
several percentages of fly ash or natural pozzolan to determine in the 0.50 to 0.60 % range. See the appendix to Specification
the minimum amount necessary to be considered “effective” in C33.
reducing expansion to the level produced by the “control”
low-alkali cement. The minimum amount of fly ash or natural X1.6.1 Certain reactive aggregates have been identified
pozzolan should be 15 % by mass of cementitious material. which produce deleterious expansion after many years of
service when used with cements with equivalent alkali contents
X1.5 Selection of the Alkali Content of the Cement Used in well below 0.60 %. Often these reactive aggregates do not
the Test Mixture—In some instances it may not be necessary to produce expansions in Test Method C227 exceeding those
demonstrate that the fly ash or natural pozzolan will reduce discussed in the appendix of Specification C33 until a much
expansion, but rather that it will not increase expansion. In this later age, perhaps one or two years. In such instances the use
instance the test and control mixtures should be made with the of a control cement with an alkali content significantly less
same low alkali cement used in the control mixture to better than 0.60 % is appropriate.
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
cement when the sulfate content, expressed as SO4, is 0.10 to proposed for use in the project 6 2 %, and that the C3A content
0.20 percent in soils or 150 to 1500 ppm in waters. ACI 201.2R of the project cement be equal to, or less than, that which was
recommends Type V cements when the sulfate content, ex- used in the test mixtures. See Appendix X1, Technical
pressed as SO4, is 0.20 to 2.0 % in soils, or 1500 to 10 000 ppm Background, Test Method C1012.
in waters. The test mixtures for both procedures may be made
X2.4 Selection of the Percentage of Fly Ash or Natural
with varying percentages of fly ash or natural pozzolan. Test
Pozzolan—It may be necessary to make test mixtures with
mixtures can use cements with equal or higher or lower C3A
several percentages of fly ash or natural pozzolan to determine
contents that might not have given satisfactory results when
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.
SUMMARY OF CHANGES
Committee C09 has identified the location of selected changes to these test methods since the last issue,
C311–11b, that may impact the use of these test methods. (Approved February 1, 2013)
(1) Section 1.3 was revised to conform to a combined standard. (4) Revised standard temperature and drying oven tempera-
(2) The term “weight” is replaced with “mass” where used in tures to agree with C09 standards. Other temperatures are
the standard. expressed in SI only.
(3) Standard room and drying temperatures defined by C09.95
coordination document are inserted where needed. Other tem-
peratures are expressed in SI only.
Committee C09 has identified the location of selected changes to these test methods since the last issue,
C311–11a, that may impact the use of these test methods. (Approved December 1, 2011)
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