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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations isued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation:C494/C494M-19
INTERNATIONAL

Standard Specification for


Chemical Admixtures for Concrete1
This standard is issued under the fixed designation C494/C494M; 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 (s) indicates an editorial change since the last revision or reapproval.
This standand has been approved for use by agencies of the U.S. Deparmment of Defense.

1.Scope* ments of this specification. Proof of compliance shall be based


1.1 This specification covers materials for use as chemical on comparisons of the average test results from the batches of
admixtures to be added to hydraulic-cement concrete mixtures test concrete and the average test results from the batches of
for the purpose or purposes indicated for the eight types as reference concrete. Admixtures (except for Types B, C,E,and
S) shall qualify for provisional compliance if the time of
follows:
1.1.1 Type A—Water-reducing admixtures, setting, length change, and durability factor meet the physical
1.1.2 Type B—Retarding admixtures, requirements and any of the alternative compressive strength
1.1.3 Type C—Accelerating admixtures, requirements shown in parentheses in Table I are met through
1.1.4 Type D—Water-reducing and retarding admixtures, the date of provisional acceptance (see Note 4). If subsequent
test results at six months or one year fail to meet the
1.1.5 Type E—Water-reducing and accelerating admixtures, requirement of at least 100of reference strength, the
1.1.6 Type F—Water-reducing, high range admixtures, provisional compliance of the admixture to this standard is
1.1.7 Type G—Water-reducing, high range, and retarding
admixtures, and withdrawn and all users of the admixture shall be notified
1.1.8 Type S—Specific performance admixtures. immediately. Uniformity and equivalence tests of Section 6
shall be carried out to provide results against which later
1.2 Unless specified otherwise by the purchaser, test speci- comparisons shall be made.
mens for qualifying an admixture shall be made using coneret-
ing materials as described in 11.1-11.3. Non 4—Allowing for provisional compliance while retaining longer
term compressive strength requirements promotes more rapid qualification
None 1—As discussed in Appendix X2, it is recommended that, of new materials, but also provides assurance that new admixture
whenever practicable, supplementary tests be made by the purchaser using technologies will not exhibit unexpected longer term performance. The
the cement, pozzolan, aggregates, air-entraining admixture, and the alternative compressive strength requirements in Table I are based on
mixture proportions, batching sequence, and other physical conditions statistical analysis of 103 Specification C494/C494M evaluation tests. The
proposed for the specific work because the specific effects produced by alternative requirements shown in parentheses correspond to a 99%
chemical admixtures may vary with the properties and proportions of the probability of passing strength requirements at subsequent test ages,2 if
other ingredients of the concrete. For example, Types F and G admixtures any one of the requirements is met. There is no requirement that all be
may exhibit much higher water reduction in concrete mixtures having met.
higher cement contents than that listed in 12.1.1.
Non 2—The purchaser should verify that the admixture supplied for 1.3.2 Level 2-Limited retesting is described in 5.2-5.2.2.
use in the work is equivalent in composition to the admixture subjected to Proof of compliance with the requirements of Table 1 demon-
test under this specification (see Section 6, Uniformity and Equivalence). strates continued conformity of the admixture with the require-
Nore 3—Admixtures that contain sufficient amounts of chloride may ments of the specification.
accelerate corrosion of steel reinforcement. Compliance with the require-
ments of this specification does not constitute assurance of acceptability of 1.3.3 Level 3—For acceptance of a lot or for measuring
the admixture for use in reinforced concrete. uniformity within or between lots, if specified by the purchaser,
1.3 This specification provides for three levels of testing. the uniformity and equivalence tests of Section 6 shall be used.
1.3.1 Level 1-During the initial approval stage, proof of 1.4 The values stated in either SI units or inch-pound units
compliance with the performance requirements defined in are to be regarded separately as standard. The values stated in
Table 1 demonstrates that the admixture meets the require- each system are not necessarily exact equivalents; therefore, to
ensure conformance with the standard, each system shall be
used independently of the other, and values from the two
This specification is under the jurisdiction of ASTM Committee C09 on
Concrete and Concerete Aggregates and is the direct responsibility of Subcommittee
C09.23 on Chemical Admixtures.
Current edition approved Dee. 15, 2019.Published March 2020. Originally 2 Supporting data have been filed at ASTM Intemational Headquarters and may
approved in 1962. Last previous edition approved in 2017 as C494/C494M-17. beService
obtained by requesting Research Report RR:C09-1030.Contact ASTM Customer
at service@astm.org.
DOI:10.1520/C0494_C0494M-19.

*A Summary of Changes section appears at the end of this standard


CoprightOASTM Intemafional. 100 Barr Harbor Dive, PD Box C700, West Conshohocken,PA 19428-2959. United States

C494/C494M-19
systems shall not be combined. Some values have only SI units C403/C403M Test Method for Time of Setting of Concrete
because the inch-pound equivalents are not used in practice. Mixtures by Penetration Resistance
1.5 The text of this standard refers to notes and footnotes C666/C666M Test Method for Resistance of Concrete to
that provide explanatory material. These notes and footnotes Rapid Freezing and Thawing
(excluding those in tables and figures) shall not be considered C1753/C1753M Practice for Evaluating Early Hydration of
as requirements of the standard. Hydraulic Cementitious Mixtures Using Thermal Mea-
1.6 The following precautionary caveat pertains only to test surements
D75/D75M Practice for Sampling Aggregates
method Sections 11 -18 of this Specification: This standard D891 Test Methods for Specific Gravity.Apparent, of Liquid
does not purport to address all of the safety concerns, if any, Industrial Chemicals
associared with its use. It is the responsibiliry of the user ofthis D1193 Specification for Reagent Water
standard to establish appropriate safety, health, and environ- E100 Specification for ASTM Hydrometers
mental practices and determine the applicabiliry of regulatory E178 Practice for Dealing With Outlying Observations
limitarions prior to use.(Warning—Fresh hydraulic cementi- E1252 Practice for General Techniques for Obtaining Infra-
tious mixtures are caustic and may cause chemical burns to red Spectra for Qualitative Analysis
exposed skin and tissue upon prolonged exposure3) Manual of Aggregate and Concrete Testing
1.7 This international standard was developed in accor- 2.2 American Concrete Institute Standard:
danee with internationally recognized principles on standard-
ization established in the Decision on Principles for the ACl 211.1-91 (2009)Standard Practice for Selecting Pro-
Development of International Standards, Guides and Recom- portions for Normal, Heavyweight, and Mass Concrete5
mendations issued by the World Trade Organization Technical 3. Terminology
Barriers to Trade (TBT) Committee.
2. Referenced Documents 3.1 For definitions of terms used in this specification, refer
to Terminology C125.
2.1 ASTM Standards:4
C33/C33M Specification for Concrete Aggregates 3.2 Definitions of Terms Specific to This Standard:
C39/C39M Test Method for Compressive Strength of cylin- 3.2.1 accelerating admixture, n—an admixture that in-
drical Concrete Specimens creases the rate of reaction of cementitious materials thus
C78/C78M Test Method for Flexural Strength of Concrete reducing time of setting and increasing the rate of early-age
(Using Simple Beam with Third-Point Loading) strength development of concrete.
C125 Terminology Relating to Concrete and Concrete Ag- 3.2.2 reference concrete, n—concrete made without the
gregates admixture being evaluated and used as the basis for evaluating
C127/C127M Test Method for Relative Density (Specific the performance of the admixture.
Gravity) and Absorption of Coarse Aggregate
C128/C128M Test Method for Relative Density (Specific 3.2.3 retarding admixture, n—an admixture that decreases
the rate of reaction of cementitious materials thus increasing
Gravity) and Absorption of Fine Aggregate time of setting of concrete.
C136/C136M Test Method for Sieve Analysis of Fine and
Coarse Aggregates 3.2.4 test concrete, n—concrete containing the admixture
C138/C138M Test Method for Density (Unit Weight), Yield, being evaluated.
and Air Content (Gravimetric) of Concrete 3.2.4.I Discussion—In the text of this specification, the
C143/C143M Test Method for Slump of Hydraulic-Cement wording "category of concrete" refers to whether the concrete
Concrete mixture is the reference concrete or the test concrete.
C150/C150M Specification for Portland Cement 3.2.5 water-reducing admixture, n—an admixture that either
C157/C157M Test Method for Length Change of Hardened increases the slump of freshly mixed concrete without increas-
Hydraulic-Cement Mortar and Concrete ing the water content or that maintains the slump with a
C183/C183M Practice for Sampling and the Amount of reduced amount of water due to factors other than air entrain-
Testing of Hydraulic Cement ment.
C192/C192M Practice for Making and Curing Concrete Test
Specimens in the Laboratory 3.2.6 water-reducing admiture, high range, n—an admix-
C231/C231M Test Method for Air Content of Freshly Mixed ture that reduces the quantity of mixing water required to
Concrete by the Pressure Method produce concrete of a given slump by 12 or greater.
C260/C260M Specification for Air-Entraining Admixtures 3.2.7 water-reducing and accelerating admixure, n-an
for Concrete admixture that reduces the quantity of mixing water required to
produce concrete of a given slump, reduces the time of setting,
3See Section on Safety Precautions, Manual of Aggregate and Conerte Testing. and increases the rate of early-age strength development.
Annual Book of ASTM Standants, Vol. 04.02.
For referenced ASTM standards. visit the ASTM website, wwwastm.org, or
contact ASTM Customer Service at serviceeastm.org. For Anual Book of ASTM
Stondards volume information, refer to the slandand's Document Sumnury page on
the ASTM website.
5 Availahle from American Concrete Instilute(ACI), P0.Box 9094.Farmington
Hils, M148333-9094,hupe//wwwaci in.org.


C494/C494M-19
3.2.8 water-reducing and retarding admixture, n—an ad- oven drying, and relative density (specific gravity) of the
mixture that reduces the quantity of mixing water required to supplied admixture are within the limits in Section 6 when
produce concrete of a given slump and increases the time of compared with the initial sample tested under Level 1 of this
setting of concrete. specification.
3.2.9 water-reducing, high-range, and retarding admixure,
n—an admixture that reduces the quantity of mixing water 6.Uniformity and Equivalence
required to produce concrete of a given slump by 12or 6.1 If specified by the purchaser, the uniformity of a lot, or
greater and inereases the time of setting of concrete. the equivalence of diferent lots from the same source shall be
3.2.10 specific performance adnixure, n—an admixture established by complying with the following requirements:
that provides a desired performance characteristic(s) other than 6.1.1 Infrared Analysis—The infrared absorption spectra of
reducing water content, or changing the time of setting of the initial sample and the test sample, obtained as specified in
concrete, or both, without any adverse effects on fresh, 18.1, shall be equivalent. Two infrared absorption spectra are
hardened and durability properties of concrete as specified considered equivalent if the same infrared absorption frequen-
herein, excluding admixtures that are used primarily in the cies at the same relative intensities are present in both spectra.
manufacture of dry-cast concrete products. Refer to Appendix X3 for additional guidance.
3.2.10.1 Discussion—Other specific performance character- 6.1.2 Residue by Oven Drying (Liquid Admixtures)—When
isties include, but are not limited to, shrinkage reduction, dried as specified in 18.2, the oven-dried residues of the initial
mitigation of alkali-silica reaction, and viscosity modification. sample and of subsequent samples shall be within ±12 of
Admixtures used for the purposes of reducing water content or the mid-point of the manufacturer's stated range, but not
changing the time of setting of concrete are classified within exceeding the manufacturer's stated limits.
the Type A through Type G grouping. Plasticizing,water- Non 5—As an example, for an admixture produced with a residue
repellent, and efflorescence-controlling admixtures are ex- range from 27 to 35?the manufacturer would provide maximum
amples of admixtures that are used in the manufacture of acceptable limits of 27.3 to 34.7?representing ±12 of the mid-point
dry-cast concrete products. of the limits, where the mid-point is 31.0%.
6.1.3 Residue by Oven Drying(Nonliquid Admixtures)-
4.Ordering Information When dried as specified in 18.3, the oven-dried residues of the
4.1 The purchaser shall specify the type of chemical admix- initial sample and of the subsequent samples shall be within a
range of variation not greater than ±4 percentage points.
ture desired, and in the case of a Type S admixture the specific 6.1.4 Relative Density (Specific Gravity)(Liquid
performance characteristic(s) required.
Admixtures)—When tested as specified in 18.4, the relative
5.General Requirements density (specific gravity) of the initial sample and subsequent
test samples shall not differ from the mid-point of the manu-
5.1 For initial compliance with this specification, test con- facturer's stated range by more than 10 of the difference
crete made with one of the admixtures shown in 1.1 shall between the mid-point of the manufacturer's stated range and
conform to the respective requirements prescribed in Table 1. that of reagent water. If 10of the difference between the
5.2 The purchaser is allowed to require a limited retesting to relative density (specific gravity) of the initial sample and
confirm current compliance of the admixture to specification water is less than 0.01, use the value 0.01 as the maximum
requirements. The limited retesting covers physical properties allowable difference. Reagent water conforming to Specifica-
and performance of the admixture. tion DI193, Types III or IV, and prepared by distillation ion
5.2.1 The physical properties retesting shall consist of exchange, reverse osmosis, electrodialysis, or a combination of
these procedures is adequate.
uniformity and equivalence tests for infrared analysis, residue
by oven drying, and relative density (specific gravity). 6.2 If the nature of the admixture or the analytical capability
5.2.2 The performance property retesting shall consist of of the purchaser make some or all of these procedures
water content of fresh concrete, setting time, and compressive unsuitable, other requirements for uniformity and equivalence
strength at 3, 7, and 28 days. from lot to lot or within a lot shall be established by agreement
5.3 At the request of the purchaser, the manufacturer shall between the purchaser and the manufacturer.
state in writing the chloride content of the admixture. 7.Packaging and Marking
5.4 At the request of the purchaser, the manufacturer shall 7.1 If the admixture is delivered in packages or containers,
provide data to substantiate the specific performance charac-
teristic(s) stated by the manufacturer for a Type S admixture. the proprictary name of the admixture, the type under this
specification, and the net mass or volume shall be plainly
5.5 Tests for uniformity and equivalence, as indicated in marked thereon. Similar information shall be provided in the
Section 6, shall be made on the initial sample and the results shipping advices accompanying packaged or bulk shipments of
retained for reference and comparison with the results of tests admixtures.
of samples taken from elsewhere within the lot or subsequent
lots of admixture. 8.Storage
5.6 At the request of the purchaser, the manufacturer shall 8.1 The admixture shall be stored in such a manner as to
state in writing that the infrared analysis spectrum, residue by permit access for inspection and identification of each

C494/C494M-19
TABLE 1 Physical RequirementsB
Type D, Type E. Type F. Type G,
Type A. Type B. Type C. Water- Water- Water- Water- Type s
Water-
Retarding Accelerating Reducing and Reducing and Reducing
Beducing Specitic Perfor-
Reducing High-Range
Retarding Accelerating High-Range and mance
Retarding
Water content, max. 95 95 95 88 88
of reference^
Time of setting, allowable
deviation from reference,
h:min:
Initial: at least 1:00 later 1:00 earier 1:00 later 1:00 earier 1:00 later
not more than 1:00 earier 3:30 later 3:30 earliet 3:30 later 3:30 earlier 1:00 earier 3:30 later 1:00 earlier
nor 1:30 nor 1:30 nor 1:30
later later later
Final: at least 1:00 earlier 1:00 eartier
not more than 1:00 earier 3:30 later 3:30 later 1:00 earlier 3:30 later 1:00 earier
nor 1:30 nor 1:30 nor 1:30
later later later
Compressive strength,min,
of reference:
1 day 140 125
3 days 110 90 125 110 125 125 125 90
7 days 110 90 100 110 110 115 115 90
28 days 110
(120)°
90 100 110
(120)0
110 110
(120)°
110
(120)C
90
90 days (117)0 rva n/a (117)° n/a (117)° (117)° n/a
6 months 100 90 90 100 100 100 100 90
(113)° (113)° (113)° (113)°
1 year 100 90 90 100 100 100 100 90
Flexural strength, min,
reference:c
3 days
7 days
100 90 110 100 110 110 110 90
100 90 100 100 100 100 100 90
28 days 100 90 90 100 100 100 100 90
Length change, max
shrinkage (altermative
requirements):
Percent of reference 135 135 135 135 135 135 135 135
Increase over reference 0.010 0.010 0.010 0.010 0.010 0.010 0.010 0.010
Relative durabilily factor, min 80 80 80 80 80 80 80 80
of reference
A Requirements in this table apply to the averages of three or more test results for each category of concrete. Comparisons are not to be made between pairs of single
test results of reference and test concretes. The indicated maximum water contents are not to be interpreted as requiring exactly that amount; they are maximum values
and testing at lower water content is permitted. Further, there is no requirement that either test or reterence concretes be prepared at the same water contents. Because
requirements in this specification apply to the average test results for each category of concrete, adjustment of mixtures within the tolerances of this specification are
permitted if necessary to make the averages fall within requirements.
B The values in the table include allowance for normal variation in test results. The objective of the 90 ompressive strength requirement for a Type B and Type S
admixture is to require a level of performance comparable to that of the reference concrete while allowing for variability in test results.
C The compressive and fexural strength of the concrete containing the admixture under test at any test age shall be not less than 90 of that attained at any previous
test age. The objective of this limit is to require that the compressive or fiexural strength of the concrete containing the admixture under test shall not decrease with age.
DAlternative requirement. If the physical requirements are met and any of the measured relative strengths are greater than the requirement in parentheses, the admixture
shall be considered provisionally to meet the requirements of this specification unti the one-year strength test results are obtained.
Altemative requirements, see 17.1.4. The of reference limit applies if length change of reference concrete is 0.030 or greater;increase over reference limit applies
if length change of reference concrete is less than 0.030%
This requirement is applicable only if the admixture is intended for use in air-entrained concrete that may be exposed to freezing and thawing while wet.

shipment, and in an environment that will protect the admix- one obtained in a single operation.A composite sample is one
ture from dampness and freezing. obtained by combining three or more grab samples.
9.Sampling and Inspection 9.3 For the purposes of this specification, it is recognized
that samples will be taken for two reasons:
9.1 The purchaser shall be provided the opportunity for 9.3.1 Compliance Tests—A sample obtained for the purpose
sampling and inspection, either at the point of manufacture or
of demonstrating compliance of a source or lot of admixture
at the site of the work, as specified by the purchaser. shall meet the applicable requirements of this specification as
9.2 Samples shall be either"grab" or "composite" samples, described in 5.1 through 5.2.2. The sample used to determine
as specified or required by this specification. A grab sample is conformance with the requirements of this specification shall


C494/C494M-19
be a composite of grab samples taken from multiple locations the purchaser and the purchaser has the right to reject the
such that the composite sample will be representative of the lot. admixture if it fails to conform to any of the applicable
9.3.2 Uniformity and Equivalence Tests—If specified by the requirements of this specification.
purchaser, samples taken for the purpose of evaluating the 10.4 Packages or containers varying more than 5 rom the
uniformity of a single lot, or equivalence of different lots from specified mass or volume are allowed to be rejected. If the
one source shall be tested as provided in Section 6. Such average mass or volume of 50 packages taken at random is less
samples shall be composite samples from individual lots if than that specified, the entire shipment is allowed to be
different lots from the same source are being compared. If the rejected.
uniformity of a single lot is being evaluated, grab samples shall
be used. 10.5 If the admixture is to be used in non-air-entrained
concrete, the purchaser has the right to reject the admixture if
9.4 Liquid Admixtures—Liquid admixtures shall be agitated the test concrete containing it has an air content greater than
to a homogeneous condition before sampling. Grab samples 3.5 ?If the admixture is to be used in air-entrained concrete,
taken for compliance or uniformity testing shall represent a the purchaser has the right to reject the admixture if the test
unit shipment or a single production lot. Each grab sample concrete containing it has an air content greater than 7.0 %.
shall have a volume of at least 0.5 L [1 pt]. At least three grab
samples shall be taken. Composite samples shall be prepared TEST METHODS
by mixing the selected grab samples and sampling the resultant Nore 6—These tests are based on arbitrary stipulations that make
homogeneous mixture to provide at least 4L [1 gal] for possible highly standardized testing in the laboratory and are not intended
compliance tests. Grab samples shall be taken from different to simulate actual job conditions. Refer to Appendix X1 for a discussion
locations distributed throughout the quantity to be represented. of the required testing program and how test results are evaluated. Testing
9.4.1 Admixtures in bulk storage tanks shall be sampled personnel should be certified to perform the required tests.
equally from the upper, intermediate, and lower levels by
means of drain cocks in the sides of the tanks or a weighted 11. Materials
sampling bottle fitted with a stopper that can be removed after 11.1 Cement—The cement used in any series of tests shall
the bottle is lowered to the desired depth. be a Type I or Type II cement conforming to Specification
9.4.2 Samples shall be stored in airtight containers that are C150/Ci50M, or a blend of two or more cements. Each cement
resistant to attack by the admixture. of the blend shall conform to the requirements of either Type I
9.5 Non-liquid Admixtures—Grab samples taken for com- or Type II of Specification C150/C150M, If the air content of
the reference concrete made without an air-entraining
pliance or uniformity testing shall represent not more than
2 Mg [2 tons] of admixture and each grab sample shall be at admixture, tested as prescribed in I4.3, is more than 3.5%,
least 1 kg [2 Ib]. At least four grab samples shall be taken. select a different cement, or blend, so that the air content of the
reference concrete does not exceed 3.5 %.
Composite samples shall be prepared by mixing the grab
samples selected and the resultant homogeneous mixture 11.2 Aggregates—The fine and coarse aggregates used in
sampled to provide at least 2.5 kg [5 Ib] for the composite any series of tests shall come from single lots of materials that
sample. Grab samples shall be taken from different locations conform to the requirements of Specification C33/C33M,
distributed throughout the quantity to be represented. except that the grading of the aggregates shall conform to the
9.5.I Samples of packaged admixtures shall be obtained by requirements in 11.2.2 and 11.2.3:
means of a tube sampler as described in Practice C183/C183M. 11.2.1 Physical Properties—Determine the relative density
9.5.2 Samples shall be stored in moisture-proof, airtight and absorption of the coarse aggregate in accordance with Test
containers. Method C127/C127M and of the fine aggregate in accordance
9.6 Samples shall be mixed to a homogeneous condition with Test Method C128/C128M.
before testing. If recommended by the manufacturer, the entire 11.2.2 Fine Aggregate Grading—Determine the grading and
sample of a non-liquid admixture shall be dissolved in water fineness modulus of the fine aggregate in accordance with Test
before testing. Method C136/C136M, The grading shall conform to the
following requirements:
10.Rejection Sieve Mass Percent
10.1 For initial compliance testing, the purchaser is allowed Passing
4.75 mm(No.4) 100
to reject the admixture if it fails to meet any of the applicable 1.18mm(No.16) 65 to 75
requirements for this specification. 300 μm(No.50) 12 to 20
150μm(No. 100) 2 to 5
10.2 For limited retesting, the purchaser has the right to 11.2.3 Coarse Aggregate Grading—The coarse aggregate
reject the admixture if it fails to meet any of the requirements shall meet the requirements for size number 57 of Specification
of the Uniformity and Equivalence Section and of the appli- C33/C33M.Use accepted practices in loading and delivery to
cable parts of Table 1. avoid segregation.
10.3 An admixture stored at the point of manufacture, for 11.2.4 Preparation of Coarse Aggregate—Coarse aggregate
more than six months before shipment, or an admixture in local from the same lot shall be used for each batch of reference
storage in the hands of a vendor for more than six months, after concrete and each batch of test concrete. The quantity of
completion of tests, shall be retested before use if requested by concrete for Level I testing includes at least three batches of the

C494/C494M-19
reference concrete and at least three batches of each test of total aggregate, or both, while maintaining the yield and
concrete being evaluated. If reference conerete and companion slump in the required ranges.
test concrete batches are made the same day, it is permitted to 12.2 Adding Admixture to Test Concrete—Except for a Type
use the same reference concrete to evaluate more than one test S admixture, add the admixture in the manner recommended
concrete. The quantity of coarse aggregate for one set of tests by the manufacturer and in the amount necessary to comply
shall be sufficient to make all batches of concrete and provide with the applicable requirements of the specifications for water
a sample for performing a sieve analysis.
11.2.4.1 Obtain tared containers, one for each batch of reduction or time of setting, or both. If desired by the person or
agency for whom the tests are being performed, the admixture
concrete to be made and one for the sieve analysis sample. One is allowed to be added in an amount such as to produce a
or more spare containers are recommended in case a concrete specific time of setting of the concrete mixture within the limits
batch has to be discarded. Prepare coarse aggregate for a set as of the applicable provisions of this specification. A Type S
follows: Fill tared containers so that each batch will contain admixture shall be tested at a dosage within the range recom-
similar particle grading. Accomplish this by taking scoopfuls mended by the manufacturer for field use.
from the stockpile and placing them successively into each 12.2.1 Non-Air-Entrained Concrete—If the admixture is to
container until all containers have their required mass. See the be tested for use only in non-air-entrained concrete, the average
Appendix of Practice D75/D75M, Sampling from Stockpiles, air contents of the test concrete and the reference concrete shall
and the Manual of Aggregate and Concrete Testing for guid- not exceed 3.5 ?nd the difference between the average air
ance on procedures to mitigate segregation. contents of the two categories shall not exceed 1.0 percentage
11.2.5 Verification of Grading—Test the coarse aggregate point. If necessary, the air-entraining admixture shall be added
samples representing each set in accordance with Test Method to the reference concrete to obtain an air content within I
C136/C136M.Discard any set for which the sample does not percentage point of the test concrete. Tests for resistance to
comply with size 57 requirements of Specification C33/C33M. cyclic freezing and thawing shall not be made.
None 7—The results required for demonstrating compliance under this 12.2.2 Air-Entrained Concrete—If the admixture is to be
specitication depend on the uniformity of the aggregate samples prepared tested for use in air-entrained concrete that will be exposed to
and used. freezing and thawing while wet, the air content of the reference
11.3 Air-Entraining Admixure—The air-entraining admix- concrete and test concrete shall be 6.0± 1.0 ?he difference
ture used in the concrete mixtures specified in Section 12 shall between the average air content from the batches of the
conform to Specification C260/C260M. reference concrete and the average air content from the batches
11.4 Preparation and Batching—Prepare and weigh all of the test concrete shall not exceed 0.5 percentage points. Air
materials in accordance with Practice C192/C192M. contents of individual pairs of batches of test and reference
concretes are nof required to fall within the 0.5 requirement.
12.Proportioning of Concrete Mixtures Tests for resistance to cyclic freezing and thawing shall be
12.1 Proportions—Concrete shall be proportioned using conducted in accordance with Test Method C666/C666M,
Procedure A.
ACI 211.1 to conform to the requirements described in 12.1.1
12.1.4.After evaluation of the trial mixtures, aggregate 13.Mixing
proportions shall be adjusted as needed to obtain workable, 13.1 Machine mix the concrete in accordance with Practice
cohesive mixtures with the correct yield to obtain the required C192/C192M.
cement contents.
12.1.1 The cement content of each batch, based on actual 14.Tests and Properties of Freshly Mixed Concrete
yield, shall be 307±3kg/m3[517±51b/yd']. The average 14.1 Samples of freshly mixed concrete from at least three
cement content of the batches of test concrete shall be within separate batches for each category of concrete shall be tested in
3kg/m3[5lb/yd'] of the average cement content of the batches accordance with the methods described in 14.2-14.5.
of reference concrete.
12.1.2 For the first trial mixture, refer to the table on volume 14.2 Slump—Test Method C143/C143M.
of coarse aggregate per unit volume of conerete in ACl 211.1 14.3 Air Content—Test Method C231/C231M.
for guidance on the amount of coarse aggregate to use, given a 14.4 Density of Fresh Concrete—Test Method C138/
nominal maximum size of 25.0 mm [l in.] and the fineness C138M.
modulus of the fine aggregate being used. 14.5 Time of Setting—Test Method C403/C403M, except
12.1.3 For the non-air-entrained mixtures, the air content
used in calculating the proportions shall be 1.5 ?For the that the temperature of each of the ingredients of the concrete
air-entrained mixtures, the air content used for this purpose mixtures, just before mixing, and the temperature at which the
time-of-setting specimens are stored during the test period shall
shall be 5.5%.
12.1.4 Adjust the water content to obtain a slump of 90± be 23.0±2.0℃[73.5±3.5°F]. Compare the average of the
15 mm [3?2 in.]. The workability of the concrete mixture results from the specimens of the test concrete with the average
shall be suitable for consolidation by hand rodding and the of the results from the specimens of the reference concrete.
concrete mixture shall have the minimum water content 14.6 Water Content:
possible. Achieve these conditions by final adjustments in the 14.6.1 Report the water-cement ratio of the concrete, com-
proportion of fine aggregate to total aggregate or in the amount puted to the nearest 0.001, as follows: Determine the net mass

C494/C494M-19
of water in the batch as the mass of water in the batch in excess E178 to establish if a test result is a statistical outlier. It is
of that present as absorbed water in the aggregates. Determine permitted to substitute outliers with test results from replace-
the water-cement ratio by dividing the net mass of water by the ment specimens. The test result reported for each category of
mass of cement in the batch. concrete and test age shall be the average of the individual test
14.6.2 Calculate the volume of concrete in the batch by determinations of the specimens tested. If one specimen or one
dividing the total mass of the materials in the batch by the test determination is discarded without replacement, it shall be
density measured in accordance with Test Method C138/ the average of the remaining test determinations. If more than
C138M.Record the volume to the nearest 0.001 m3[0.1 ft3]. one specimen representing a given test at a given age is found
14.6.3 Calculate the water content, in units of kg/m3[lb/ft'], faulty either before or after testing and replacement specimens
of each batch by dividing the net mass of water in the batch by are not available, the test results shall be disregarded and the
the volume of the batch. Calculate the relative water content of test shall be repeated.
the test concrete as a percentage of the water content of the
reference concrete by dividing the average water content of the Nore 9—Examples of faulty specimens include specimens with evi-
batches of the test concrete by the average water content of the dence of incomplete consolidation, specimens damaged during mold
batches of the reference concrete and multiplying the quotient removal, or defective placement of gage studs in length change prisms.
by 100%.
16.Test Specimens of Hardened Concrete
15. Preparation of Test Specimens 16.1 Number of Specimens—Make at least three batches for
15.1 As required by Section 16, make specimens for tests of each category of concrete to be compared. For each batch,
hardened concrete, representing each test and test age from at make at least two test specimens for freezing and thawing tests
least three separate batches for each category of concrete. Table and at least one test specimen for each other type of test and
2 shows the minimum number of specimens to be made from test age indicated in Table 2.The number of test ages for
three batches of each category (see Note 8). Make at least one
specimen for each test and test age from each batch of
compressive strength includes test ages for demonstrating
concrete, except make at least two specimens for the freezing provisional compliance.
and thawing test from each batch of concrete. The preparation 16.2 Types of Specimens—Specimens shall be prepared in
of all specimens can be completed in one, two, or three days of accordance with the following:
mixing, provided the same number of batches of test concrete 16.2.1 Compressive Strength—Make and cure 150 by
and reference concrete are made on the same day. 300 mm [6 by 12 in.] or 100 by 200 mm [4 by 8 in.] cylinders
NonE 8—More than the minimum number of specimens should be in accordance with Practice C192/C192M.
prepared for tests of hardened concrete to provide replacements for 16.2.2 Flexural Strength—Make and cure beams with a
specimens that may be found to be faulty or not consolidated properly (see
15.2). cross-section of 75 by 75 mm [3 by 3 in.] in accordance with
Practice C192/C192M.
15.2 Examination of Specimens—Visually examine all 16.2.3 Resistance to Freezing and Thawing—Prisms shall
specimens after removal from their molds. If any specimen is
found to be faulty, it shall be discarded (see Note 9). In be made and cured in accordance with the applicable require-
addition, measure and record the mass of each type of ments of Practice C192/C192M.Prism dimensions shall be as
specimen. Note any specimen that appears to have a low mass, required by Test Method C666/C666M. The air content of the
which may indicate inadequate consolidation. Visually exam- mixtures shall be as specified in 12.2.2.
ine specimens after testing and note any unexpected condi- 16.2.4 Length Change—Make and cure test specimens in
tions. If test results for such noted specimens are statistical accordance with Test Method C157/C157M. The moist-curing
outliers, discard the results for those specimens. Use Practice period, including the period in the molds, shall be 14 days.
TABLE 2 Minimum Number of Specimens
Test Number of Test Ages Number of Categorles of Batches for Each Number of Specimens, min
Concrete Category of Concrete
Water content 2 3 A
Slump 2 3
Air content

2 3
Time of seting 2 3 6
Compressive strength

Nn
Types B,C, E,and S 5 2 3 30
Types A and D 6° 3 36
Types F and G 70 3 42
Flexural strength 3 3 18
Freezing and thawing 3 12°
Length change 3 6
ADetermined on each batch of cancrete mixed.
日See 14.5.
CIncludes test ages for demonstrating provisional compliance.
P Two specimens per batch. For other tests of hardened concrete, one specimen per test age for each batch.


C494/C494M-19
17.Tests on Hardened Concrete drying of specimens from the test concrete shall be not more
17.1 Test specimens of hardened concrete (see Table 1) in
than 0.010 percentage units greater than that of the reference
accordance with the following methods: concrete.
17.1.I Compressive Strength-Test Method C39/C39M. Nore 10—Because the specific efects produced by chemical admix-
Test specimens at ages of 1 (Types F and G only),3.7,and 28 tures may vary with the properties of the other ingredients of the concrete,
results of length change tests using aggregates of such a nature that the
days, 6 months, and 1 year. Test specimens at 90 days if length change on drying is low may not accuratcly indicate relative
compliance to the alternative requirement for provisional performance to be expected with other aggregates having properties such
compliance is desired. For each test age, calculate the com- as to produce concrete of high length change on drying.
pressive strength of the test concrete as a percentage of the 18.Uniformity and Equivalence Tests
compressive strength of the reference concrete as follows: 18.1 Infrared Analysis—This test procedure is intended to
17.1.1.1 Divide the average compressive strength of the compare qualitatively the composition of different samples and
specimens made from the test concrete batches at a given test results should not be interpreted quantitatively (see Note 11).
age by the average compressive strength of the specimens Perform the infrared analysis in accordance with 18.1.1,18.1.2,
made from the reference concrete batches at the same test age and 18.1,3, which provides a specific procedure for the infrared
and multiply the quotient by 100%. analysis of admixtures (see Note 12), or alternately by one of
17.1.1.2 If the results of the tests are required in a period of the methods described in Practice E1252. If one of the methods
time that will not permit curing of specimens to ages of six from Practice E1252 is used to verify lot-to-lot uniformity,
months and one year, the tests at those ages are permitted to be agreement shall be reached between the purchaser and the
waived. manufacturer on the specific method to be used to conduct the
17.1.2 Flexural Srength—Test Method C78/C78M. Test infrared analysis.
specimens at ages 3, 7, and 28 days. Caleulate the fexural Nore I1—Refer to Appendix X3 for guidance on infrared analysis.
strength of the test concrete as a percentage of the flexural 18.1.1 Liquid Admixtures—Determine the dissolved solids
strength of the reference concrete as follows: concentration by oven drying in accordance with 18.2 and
17.1.2.1 Divide the average flexural strength of the speci- dilute an aliquot of the liquid admixture sample with distilled
mens made from the test concrete at a given test age by the water to yield a dissolved solids concentration of about
average flexural strength of the specimens made from the 0.015 g/mL, for example, a 5-mL aliquot diluted to 200 mL.
reference concrete at the same test age, and multiply the Pipet 5 mL of the diluted solution and add it to a petri dish with
quotient by 100%. 2.5 g of potassium bromide of a grade suitable for use in
17.1.3 Resistance to Freecing and Thawing—Comparison infrared analysis and 5 mL of distilled water. Stir and mix to
tests of the test concrete and of the reference concrete shall be dissolve. Place in a drying oven (18.2.1.1) and dry for 17±
made concurrently using Procedure A of Test Method C666/ Vh at 105±3℃[221±5°F],Cool and transfer the dried
C666M.Place specimens under test at the age of 14 days. residue to a mortar and grind to a fine powder. Work quickly to
Calculate the average durability factors of the specimens for all avoid moisture pick-up. Weigh 0.I g of the powder and 0.4g
batches of each category of concrete. Calculate the relative of potassium bromide of a grade suitable for use in infrared
durability factor by dividing the average durability factor of the analysis. Mix in an electric amalgamator for 30 s using
test concrete by the average durability factor of the reference stainless steel capsule and balls. Proceed in accordance with
concrete and multiplying the quotient by 100%, 18.1.3,
17.1.4 Length Change—Test specimens shall consist of 18.1.2 Non-liquid Admixtures—Grind 10 g to a fine powder
molded prisms made and tested in accordance with Test with mortar and pestle. Transfer the sample to a petri dish,
Method C157/C157M except that the moist curing period, place in a drying oven (18.2.1.1) and dry for 17± 94 h at 105
±3℃[221±5°F].Weigh 0.004 to 0.006 g of the dry powder
including the period in the molds, shall be 14 days. Then store and 0.995 g of potassium bromide of a grade suitable for use in
the specimens in air under conditions specified in the section
on Air Storage of Test Method C157/C157M for a period of 14 infrared analysis. Mix in an electric amalgamator for 30 s using
days, at which time determine the length change of each stainless steel eapsule and balls. Proceed in accordance with
specimen. Consider the drying shrinkage to be the length 18.1.3.
change during the drying period, based on an initial measure- 18.1.3 To prepare a disk for infrared analysis, weigh 0.300
ment at the time of removal of the specimen from the mold,
g of the mixture prepared in 18.1.I or 18.1.2 and transfer into
a suitable die. If an evacuable die is used, apply vacuum for
and express it as percent to the nearest 0.001 ased on the 2 min before pressing. Maintain the vacuum and press for
specimen gage length. If the average length change of the 3 min with suitable force to produce a disk about 1 mm thick.
specimens from the reference concrete after 14 days of drying Remove the disk from the die, insert into the infrared spectro-
is 0.030 or greater, the average length change on drying of photometer and obtain the infrared absorption spectrum.
the specimens from the test concrete, expressed as percent of
the length change of the reference concrete, shall not exceed Nore 12-It is important that the same procedures be used on all
the maximum specified in Table I. If the average length change samples to be compared with each other and preferably that they be
conducted by the same analyst. Major changes in infrared spectra may
of the specimens from the reference concrete after 14 days of result from (a) water content differences due to drying variations,(b)
drying is less than 0.030?he average length change on water picked up by hygroscopic materials,(c)reaction between the

8.
C494/C494M-19
potassium bromide and some other compound present, and (d) differences samples of two different admixtures.
in time between formation of the disk and its use. Also, the threshold for Nom: 15—Testing Type C and E admixtures, which commonly contain
detection of individual components by infrared absorption varies widely. calcium salts, for oven-dried residue using the oven-dry method can yield
depending upon the identity and concentration of accompanying sub- inconsistent values. This is because these salts can retain bound water of
stances. For example, significant amounts of saccharides may be present hydration in an unpredictable manner upon drying. Purchasers and users
in a lignosulfonate admixture without their presence being indicated by of these types of chemical admixtures should preferably use the relative
this method. density (specific gravity) test to determine uniformity and equivalence.
18.2 Residue by Oven Drying (Liquid Admixtures): 18.3 Residue by Oven Drying(Nonliquid Admixtures):
18.2.1 Place 25 to 30 g of standard Ottawa sand (20 to 30 18.3.1 Place about 3 g of the nonliquid admixture into a
mesh) in a wide-mouth, low-form (about 60 mm inside dried and tared glass-stoppered weighing bottle (similar to the
diameter and 30 mm in height) glass weighing bottle provided one described in 18.2.1). Stopper and determine the mass of the
with a ground-glass stopper. Place the weighing bottle and bottle and contents to the nearest 0.01 g. Remove the stopper
stopper, with stopper removed, in a drying oven (18.2.1.1) and and immediately place both bottle and stopper in a drying oven
dry for 17±V4hat 105±3℃[221±5°F](Note 13).Insert (18.2.1.1). Dry for 17±14h at 105±3℃[221±5°F].At
the stopper in the weighing bottle, transfer to a desiccator, cool the end of the drying period, stopper the weighing bottle,
to room temperature, and weigh to the nearest 0.01 g. Remove transfer to the desiccator, cool to room temperature, and weigh
the stopper and, using a pipet, evenly distribute 4 mL of the to the nearest 0.01 g.
liquid admixture over the sand. Insert the stopper to avoid loss 18.3.2 Calculation:
by evaporation and weigh to the nearest 0.01 g. Remove the 18.3.2.1 Record the following masses:
stopper and place both the bottle and stopper in a drying oven
(18.2.1.1). Dry for 17± hat105±3℃[221±5°F].At mi = mass of tared stoppered weighing bottle and sample
the end of the drying period, stopper the weighing bottle, before drying,
transfer to a desiccator, cool to room temperature, and weigh to m?= mass of empty, stoppered weighing bottle.
m3 = mass of sample=(m?-m?),
the nearest 0.01 g. m4 = mass of tared stoppered weighing bottle and sample
NonE 13—For laboratories conducting this test as a routine operation. after drying, and
previously dried sand and weighing boltles can be maintained in desic- ms = mass of oven-dried residue =m?-m?.
cators so that they are immediately available for use when a sample is to 18.3.2.2 Calculate the oven-dried residue by using the
be tested.
18.2.1.1 Drying Oven—The drying oven shall be either a following equation:
forced circulation type or one with provision for free access of Residue by oven drying (mass percent)=
ms ×100
(2)
air. There shall be precise control of temperature and time of m;
drying so that the degree of volatilization of the material other 18.3.3 Precision Statement—The maximum multilaboratory
than water from sample to sample will not vary. coefficient of variation for residue by oven-drying (non-liquid
18.2.2 Calculation: admixture) has been found to be 1.40 ?Therefore, results of
18.2.2.1 Record the following masses: tests by two different laboratories on identical samples of an
m?= mass of stoppered botle with sand and sample. admixture are not expected to differ from each other by more
m = mass of stoppered bottle with sand, than 4.0 of their average (Note 14). The maximum single-
m3 =m?-m?=mass of sample, operator coefficient of variation for residue by oven drying
m = mass of stoppered bottle with sand and dried residue, (non-liquid admixture) has been found to be 0.48 ?herefore,
and results of two properly conducted tests by the same operator on
ms = m?-m?=mass of dried residue. the same material are not expected to differ by more than 1.4 %
18.2.2.2 Calculate the residue by using the following equa- of their average.
tion: 18.4 Relative Density (Specific Gravity)(Liquid Admix-
tures):
Residue by oven drying (percent by mass)=
ms×100
(1) 18.4.1 Determine the relative density (specific gravity)at
m 25.0±1.0 ℃[77.0±2.0°F] of a liquid admixture using
18.2.3 Precision Statement—The maximum multilaboratory hydrometers complying with Specification E100. Hydrometers
No. 112H through 117H will cover the range for most
coefficient of variation for residue by oven drying (liquid
admixtures) has been found to be 1.25 ?Therefore, results of determinations. A 250-mL graduated cylinder, and a water bath
tests by two different laboratories on identical samples of an capable of maintaining 25.0±1.0℃[77,0±2.0°F] will also
admixture are not expected to differ from each other by more be required. Alternatively, determine relative density (specific
than 3.5 of their average (Note 14). The maximum single- gravity) by using the pyenometer method in accordance with
operator coefficient of variation has been found to be 0.6%. Test Methods D891.
Therefore, results of two properly conducted tests by the same Nore 16—The pycnometer method is more accurate and precise
operator on the same material are not expected to differ by compared with the hydrometer method, and is the preferred method in
more than 1.7%. case of disputes. The hydrometer method is less aecurate and precise, but
is simpler and faster to perform and is often satisfactory. If the admixture
NonE 14—The precision statements are based on the maximum is too viscous to permit the hydrometer to float freely, the pyenometer
variation of tests made in 18 laboratories on sets of three duplicate method should be used.

C494/C494M-19
18.4.2 Place a sample in the 250-mL graduated cylinder and 19.1.2 Brand name,manufacturer's name, and lot number,
put in the hydrometer in such a manner that it floats free and character of the material, and quantity represented by the
does not touch the side of the cylinder. Place the cylinder with sample of the admixture under test,
sample and hydrometer in the constant-temperature bath until 19.1.3 Brand name, manufacturer's name, and other perti-
the temperature of the cylinder, hydrometer, and sample is nent data on the material used as the air-entraining admixture,
uniform at 25.0±1.0℃[77.0±2.0°F]. If all are at proper 19.1.4 Brand name, manufacturer's name, type, and test
temperature prior to insertion of the hydrometer, approximately data on the portland cement or cements used,
10 min should be allowed for equilibrium. If the sample shows 19.1.5 Description of, and test data on the fine and coarse
evidence of foaming, hydrometer reading should be continued aggregates used,
until constant readings are obtained. Read the hydrometer at 19.1.6 Detailed data on the concrete mixtures used, includ-
the base of the meniscus to the nearest 0.005. ing amounts and proportions of admixtures used, actual cement
18.4.2.1 If foaming is encountered during transfer of the factors, water-cement ratios, unit water contents, ratios of fine
admixture to the cylinder, sufficient time shall be allowed for to total aggregate, slump, and air content, and
the foam to dissipate or rise to the surface, where it shall be 19.1.7 In the event that, in accordance with the provisions of
removed before inserting the hydrometer. Crusting of the 17.1.1.2, some of the tests have been waived, the circum-
admixture on the hydrometer stem due to evaporation during stances under which such action was taken shall be stated.
temperature adjustment shall be avoided. 19.1.8 For a Type S admixture and if required by the
18.4.3 Precision Statement—The maximum multilaboratory purchaser, a report on the performance characteristics of the
coefficient of variation for relative density (specific gravity)(of admixture in accordance with 5.4.
liquid admixtures) has been found to be 0.316 ?Therefore, 19.1.9 On the infrared spectrum, record the procedure used
results of two different laboratories on identical samples of an for the infrared analysis. Record"ASTM C494/C494M,
admixture are not expected to differ from each other by more 18.1.1"if the potassium bromide pellet method was used. For
than 0.9 of their average (Note 14). The maximum single- methods in Practice E1252, record"ASTM E1252"on the
operator coefficient of variation has been found to be 0.09%, spectrum and include sufficient detail so that another analyst
Therefore, results of two properly conducted tests by the same would be able to obtain a similar spectrum on the same sample.
operator on the same material are not expected to differ by Non 17—If the IR spectrum is prepared according to one of the
more than 0.275%. methods in Practice E1252, the necessary steps required to obtain the
same spectrum for the same sample should be noted on the infrared
19.Report spectrum, or in a report that accompanies the infrared spectrum.
19.1 Report the following: 20.Keywords
19.1.1 Results of the tests specified in Sections 6, 14, and 20.1 accelerating: chemical admixtures; concrete; physical
17,and the relevant specification requirements with which they requirements; retarding; specific performance; testing; water
are compared, reducing

APPENDIXES
(Nonmandatory Information)
X1.SUMMARY OF TESTING PROGRAM
X1.1 The testing program to demonstrate compliance with program involving one test concrete. On any given day, the
this specification requires testing specimens made from the test same number of batches of test concrete and reference concrete
concrete that includes the admixture and comparing the aver- should be made. For example, if one test concrete is involved,
age of the test results with those obtained from specimens on a given day it is not permitted to make one batch of the
made from the reference concrete. For compliance, all criteria reference concrete and two batches of the test concrete. The
and Table 1 have to be satisfied. The testing program requires results for the individual specimens of each concrete category
making at least three batches of the reference concrete and at are averaged as shown in Fig. X1.1. The average for the test
least three batches of each test concrete, if more than one concrete specimens (7) is compared with the average for the
admixture is being evaluated in the same testing program. reference concrete specimens (R).
X1.2 Fig. X1.1 is a schematic of the minimum testing

10
C494/C494M-19

Test Concrete
Batch 1 Batch 2 Batch 3

Test Test Test


Result T1 Result T2 Result T3

T= T1+T2+73

Reference Concrete

Batch1 Batch 2 Batch 3

Test Test Test


Result R1 Result R2 Result R3

R=!R1+R2+R3

FIG. X1.1 Schematic of Minimum Testing for Each Test and Test Age

X2. VERIFICATION TESTING FOR SPECIFIC USE

X2.1 The performance of an admixture in the test concrete the same time during the batching and mixing sequence as it
prepared in accordance with this specification may not be will be added on the job. Proportion the concrete mixtures to
indicative of actual performance with the concrete mixture to have the cementitious materials content specified for use in the
be used on a specific project. Therefore, it is advisable that the work. If the maximum size of coarse aggregate is greater than
user of the admixture perform verification tests using the 25.0 mm [1 in.], screen the concrete over a 25.0-mm [1-in.]
concrete making materials and mixture proportions that will be sieve before fabricating test specimens.
used on a specific project. Practice C1753/C1753M may be
used in addition to the test methods in this specification to X2.3 Other Use Conditions—Other conditions are known to
evaluate admixture performance for the project concrete. affect the overall suitability of the concrete mixture for specific
intended uses. These include the temperature of the materials
X2.2 Materials for Tests—The effects of an admixture on or the surroundings, the relative humidity, the length of time
the time of setting and water requirement of concrete are between mixing and placing, the amount of mixing activity and
known to vary with the time of its addition during the batching other factors. These physical conditions may be incorporated
and mixing sequence. To test an admixture for use in specific into the tests with intention of revealing potential adverse
work, the cement, pozzolan, aggregates, and air-entraining interactions. As an example, the decrease of slump with time
admixture used should be representative of those proposed for (slump loss) is a characteristic that should be investigated
use in the work. Add the admixture in the same manner and at under job conditions.

11
C494/C494M-19

X3.USING INFRARED ANALYSIS TO VERIFY LOT-TO-LOT UNIFORMITY


X3.1 Principle is required if comparing spectra obtained using different
X3.1.1 Infrared spectroscopy is used to identify organic and instruments and techniques.
inorganic materials by measuring the interaction of infrared X3.3 Comparing Spectra
radiation with the material. A specimen of the material is
X3.3.1 In accordance with 6.1.1, two infrared absorption
placed between an infrared source and a detector using an spectra
instrument known as an infrared spectrophotometer. The infra- are considered equivalent if the same infrared absorp-
red radiation is absorbed by the specimen at frequencies tion bands at the same relative intensities are present in both
corresponding to the vibrational frequencies of the chemical spectra. The spectra of the initial and test samples can be
bonds between specific groups of atoms (known as functional compared by visually comparing the absorption spectra that are
groups)that are present in the material. The instrument plotted on separate pieces of paper, preferably using the same
produces a graph of radiation transmitted through the specimen scale. Overlaying the two plotted spectra on a light box may
make comparison easier. If data are available in digital format,
as a function of frequency, which is called an infrared
spectrum. By convention, the frequency scale is expressed as the spectra can be plotted and compared on a computer screen.
the inverse of the wavelength in centimeters, which is known X3.3.2 Software to conduct automated comparison of two
as the wavenumberand has units of cm Typically, wavenum- spectra is available that can provide a quantitative indication of
bers in the range from 4000 to 400 em- are used to identify the their equivalence. One such method is called the hit quality
presence of different functional groups. index (HQI) value, and is a numerical measure of the closeness
X3.1.2 Historically,infrared spectra were plotted in terms of of fit between the test spectrum and the initial spectrum. The
transmittance, I/Io, where I is the intensity of radiation passing higher the HQI value, the closer the two spectra are to each
through the specimen and Io is the intensity of radiation passing other. Caution should be exercised when using HQI values to
through the blank (empty cell). With the advent of computers,
ascertain lot-to-lot uniformity. Noise and other artifacts in the
it has become more common to plot spectra in terms of spectrum can impact the HQI value. It can be a challenge to
absorbance (-logio (I/I))because absorbance is related lin- determine the minimum HQI value to indicate that the spectra
for the test sample and initial sample are equivalent and that
early to concentration. there is acceptable lot-to-lot uniformity. The HQI value is not
X3.1.3 Infrared spectroscopy provides a qualitative means a probability or a percentage, and it has no units. Therefore,
for judging the equivalence of an original sample and subse- HQI values should not be used as the sole basis for judging
quent samples obtained from different lots of a given admix- equivalence of spectra and uniformity of product.
ture. Spectral interpretation may be done by functional group
identification or by comparison of infrared spectra of unknown X3.4 Judging Equivalence
materials with those of known materials. For the purposes of
judging equivalence of different lots of an admixture, compari-
X3.4.1 The following guidelines can be used as indicators
son of spectra is used in this specification. Spectra plotted in
that the spectra of the test sample and initial sample are
terms of transmittance or absorbance are acceptable. Although equivalent:
guidance for judging equivalence is given here, a chemist with
X3.4.1.1 The spectra of the test sample and initial sample
have the same number of absorption bands.
training and experience in infrared spectroscopy should be X3.4.1.2 The wavenumbers (frequencies) of the absorption
consulted if necessary. In addition, Practice E1252 as well as bands for the spectra of the initial and test samples are the same
many textbooks and technical articles may be consulted for X3.4.1.3 The relative intensities of the absorption bands for
additional information. the spectra of the initial and test samples are similar.
X3.2 Requirements X3.4.2 Subjective judgment is involved in deciding whether
two spectra are sufficiently similar to conclude that the lot-to-
X3.2.1 As stated in Section 18, an admixture can be lot uniformity is acceptable. If differences are found between
prepared for infrared analysis by different methods. These the spectra of the initial and test samples, a repeat infrared
include preparing a potassium bromide disk containing the analysis of the test sample is recommended.
dried residue uniformly dispersed in the disk as well as the X3.4.3 Infrared spectra are affected by many factors that do
various methods cited in Practice E1252. In reporting the not translate into differences in admixture performance or
results, Section 19 requires that sufficient detail be included on composition.
the infrared spectrum so that another analyst would be able to X3.4.3.1 Admixtures derived from natural products, such as
obtain a similar spectrum on the same sample. lignosulfonates and resins, are known to have intrinsie varia-
X3.2.2 Test reports should note how test specimens were tions in their functional groups that are reflected as variations
prepared as well as how the specimens were analyzed in the in their infrared spectra.
instrument, for example, transmission (KBr pellet or Nujol X3.4.3.2 Varying amounts of water in the specimen being
mull), attenuated total reflectance, and so forth. The resolution analyzed may result in spectral changes other than the ampli-
at which the spectrum was collected also should be noted. Care tude of the bands associated with the water itself.
12
C494/C494M-19
X3.5 Examples tance as opposed to absorbance, hence the bands point down-
X3.5.1 Fig. X3.1 shows the infrared absorbance spectra for ward rather than upward. Note that wavenumbers and the
two samples of a water-reducer based on calcium lignosul- relative intensities of the absorption bands are in good agree-
fonate. The figure shows the typical patterns observed in these ment throughout the spectra. Therefore the two samples would
types of spectra. A spectrum has absorption bands of varying be considered to be equivalent.
intensities and widths. In addition, bands from different com- X3.5.3 Fig. X3.3 shows the infrared spectra of samples from
ponents in the sample may overlap one another. At the higher two lots of a mid-range water-reducing admixture. Significant
frequency (higher wavenumber) portion of the spectra in Fig. differences between the spectra are evident particularly in the
X3.1, there are bands due to stretching of O-H bonds (the high
amplitude, broad bands) and stretching of C-H bonds (the less
fingerprint region. These spectra would not be considered
similar and the two lots would not be judged to be equivalent.
intense, narrow bands). The portion of the infrared spectrum
below a wavenumber of about 1800 cm-' is known as the X3.5.4 Fig. X3.4 shows absorbance spectra of an admixture
"fingerprint region" and typically contains many and some- that were obtained from three repeated measurements at
times overlapping bands. In this example, there is a good match different times without removing the specimen from the
in the locations and intensities of the absorption bands through- spectrometer. The first measurement is shown as "Test 1"and
out the spectra for both samples; the two samples would be the last is "Test 3." As water evaporated from the specimen,
considered to be equivalent. there was a decrease in amplitude of bands due to free water at
X3.5.2 Fig. X3.2 shows infrared spectra of two samples of approximately 3400, 1640, and 550 em-', which are indicated
a naphthalene sulfonate condensate based high-range water- with the vertical dashed lines marked with"W" Some other
reducer. These spectra are plotted in terms of percent transmit- bands increased in amplitude with increased evaporation.
1.00
0.90
0.80 Initial Sample

Absorance
0.70 Fingerprint Region
0.60
0.50
0.40
0.30
0.20 Test sample
0.10
0.00
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber, cm-1
FIG. X3.1 Similar Absorption Spectra for Two Samples of Admixture Based on Calclum Lignosulfonate

13
C494/C494M-19

percntTasmi
100

品品 Initial
Sample
-Test Sample
70
60
50
40
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber,cm-1
FIG.X3.2 Similar Spectra (Percent Transmittance) for Two Samples of Admixture Based on Naphthalene Sulfonate Condensate

1.00
0.90
0.80
Initial Sample

Absorance
0.70
0.60
0.50 Test Sample
0.40
0.30
0.20
0.10
0.00
4000 3500
2500 3000
2000 1500 1000 500
Wavenumber,cm-1
FIG. X3.3 Example of Different Absorption Spectra for Two Samples of Water-Reducing Admixtures

14
C494/C494M-19
0.9
0.8
Test 1
0.7 Test 2

Absorance
0.6 Test 3
0.5 w W w
0.4
0.3
0.2
0.1
0.0
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber, cm-1
FIG. X3.4 Effect of Change in Water Content of Same Specimen Tested at Different Times Without Removal from Instrument

SUMMARY OF CHANGES

Committee C09 has identified the location of selected changes to this standard since the last issue
(C494/C494M-17) that may impact the use of this standard.(Approved Dec. 15,2019.)
(1)The specification was revised extensively.

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