Designation: C 265 – 01

Standard Test Method for

Water-Extractable Sulfate in Hydrated Hydraulic Cement
Mortar1
This standard is issued under the fixed designation C 265; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope D 1193 Specification for Reagent Water3

1.1 This test method covers the measurement of water- E 11 Specification for Wire-Cloth and Sieves for Testing
extractable SO3 in hardened hydraulic cement mortar. This Purposes4
measurement is assumed to represent unreacted, available IEEE/ASTM SI-10 Standard for Use of the International
sulfate remaining in the mortar. System of Units (SI): The Modern Metric System4
1.1.1 Warning: Fresh hydraulic cementious mixtures are 3. Terminology
caustic and may cause chemical burns to skin and tissue upon
prolonged exposure. 3.1 Definitions—The terms used in this test method are
1.2 The values stated in SI units are to be regarded as the defined in accordance with Terminology C 219.
standard. The values given in parentheses are for information 4. Significance and Use
only.
1.3 Values in SI units were obtained by measurement in SI 4.1 This test method is intended for use by manufacturers of
units or by appropriate conversion using the Rules for Conver- hydraulic cement and those interested in research on a suitable
sion and Rounding given in IEEE/ASTM SI-10 Standard of method for determining whether calcium sulfate has or has not
measurements made in other units. been added in an amount considered to be optimum. Also, for
1.4 This standard does not purport to address all of the any such cement having an above optimum SO3 content, this
safety concerns, if any, associated with its use. It is the test method establishes whether that excess exceeds the limit
responsibility of the user of this standard to establish appro- allowed in Specification C 595. This test method also can
priate safety and health practices and determine the applica- provide useful information on other hydraulic cements, such as
bility of regulatory limitations prior to use. those specified in Specifications C 150 and C 1157.

2. Referenced Documents 5. Apparatus

2.1 ASTM Standards: 5.1 Sieve—A 2.36-mm (No.8) sieve conforming to Specifi-
C 109/C 109M Test Method for Compressive Strength of cation E 11.
Hydraulic Cement Mortars (Using 2-in. or 50-mm Cube 5.2 Mixer, Bowl, and Paddle—An electrically driven me-
Specimens)2 chanical mixer equipped with a paddle and bowl, as specified
C 114 Test Methods for Chemical Analysis of Hydraulic in the Apparatus section of Practice C 305.
Cement2 5.3 Polyethylene Containers—Watertight polyethylene bags
C 150 Specification for Portland Cement2 of 1-L (1-qt) capacity or approximately 360-mm (14-in.) sheet
C 219 Terminology Relating to Hydraulic Cement2 material, made using polyethylene at least 0.10-mm (0.004-in.)
C 305 Practice for Mechanical Mixing of Hydraulic Cement in thickness.
Pastes and Mortars of Plastic Consistency2 5.4 Mortar and Pestle—A mortar of 1.5-L (11⁄2-qt) size, and
C 595 Specification for Blended Hydraulic Cements 2 a pestle, both of which shall be iron or porcelain.
C 778 Specification for Standard Sand2 5.5 Water Bath—A water bath thermostatically controlled at
C 1157 Performance Specification for Hydraulic Cement 23.0 6 0.15°C .
[Metric]2 6. Reagents and Materials
6.1 Mixing Water—Reagent water conforming to the nu-
merical limits of Type II of Specification D 1193.
1
This test method is under the jurisdiction of ASTM Committee C01 on Cement
and is the direct responsibility of Subcommittee C01.28 on Sulfate Content.
Current edition approved Aug. 10, 2001. Published October 2001. Originally
3
published as C 265 – 51 T. Last previous edition C 265 – 99. Annual Book of ASTM Standards, Vol 11.01.
2 4
Annual Book of ASTM Standards, Vol 04.01. Annual Book of ASTM Standards, Vol 14.02.

Copyright © ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

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 C 265
6.2 Graded Sand—Sand conforming to the requirements for Complete filtration within a period of 2 min. Filter again,
graded sand in Specification C 778. whether the filtrate is turbid or not, using a new dry filter paper
without suction.
7. Temperature and Relative Humidity
7.1 Maintain the temperature of the molding room at 23.0 6 11. Analysis of the Extract
2.0°C . Adjust the temperature of the dry materials and the 11.1 Transfer 50.0 mL of the clear extract by means of a
mixing water, prior to mixing, so that the temperature of the 50-mL pipet to a 400-mL beaker, dilute with distilled water to
mortar, immediately upon completion of mixing is 23 6 1°C . about 250 mL, and add 5 mL of concentrated hydrochloric acid
7.2 Maintain the relative humidity of the laboratory so that (HCl, sp gr 1.19). Heat to boiling, and proceed in accordance
it is not less than 50 %. with the sulfur trioxide determination section of Test Methods
8. Preparation of Test Mortar C 114. Perform a blank on the reagents in use in the analysis.
11.1.1 After the BaCl2 solution is added in accordance with
8.1 Proportion the mortar in accordance with the instruc-
the sulfur trioxide determination section of Test Methods
tions for a six-cube batch given in the section on Composition
C 114, boil the solution vigorously for 15 min.
of Mortars of Test Method C 109, except use a water-
cementious material ratio of 0.5, by mass. Mix mechanically in 11.2 When the amount of filtrate is insufficient to provide a
accordance with Procedure for Mixing Mortars of Practice 50-mL aliquot, use 25 mL of the extract and a factor twice that
C 305. given in Section 12.
8.2 Split the batch immediately after mixing then place
approximately 450 g of mortar in each of the two polyethylene 12. Calculation and Report
containers. Obtain the temperature of each portion to ensure 12.1 Calculate the SO3 content to the nearest 0.01 g/L of
that it is within the range 23 6 1°C . If bags are used, twist the solution, as follows:
neck of each and seal with a rubber band; double the neck over SO3, g/L 5 W 3 6.86 (1)
and seal with a second band. If sheets are used to contain the
samples, gather the corners and edges to make a bag and seal where:
in similar manner. W = grams of barium sulfate (BaSO4) precipitated.
12.2 Report the average of the two determinations.
9. Storage of Test Mortar
9.1 Immediately immerse both containers in the water bath 13. Precision and Bias
maintained at (23.0 6 0.15°C) .
13.1 Precision—The single-operator (within-laboratory)
10. Preparation of Cement Extract standard deviation has been found to be 0.077 g/L SO3
throughout the range of 0.20 to 0.85 g/L SO3. Therefore, results
10.1 At 24 6 1⁄4 h after the instant the cement and water
of two properly conducted tests by the same operator on
were mixed together, remove the containers successively from
water-extractable SO3 in hardened hydraulic cement mortars of
the water bath, pulverizing each sample in turn with the pestle
the same material should not differ from each other by more
in the mortar as rapidly as possible. Immediately upon removal
than 0.22 g/L SO3. The multi-laboratory (between-laboratory)
from the water bath treat each sample individually as follows:
standard deviation has been found to be 0.137g/L SO3 through-
First pulverize approximately one third of the specimen until
out the range of 0.20 to 0.85 g/L SO3. Therefore, results of two
most of it passes the 2.36-mm (No. 8) sieve. Return the coarse
properly conducted tests on the same material, from two
residue to the mortar and grind another one third of the
different laboratories on water-extractable SO3 in hardened
specimen as before. Repeat the process until all of the
hydraulic cement mortars should not differ from each other by
specimen is pulverized to pass the 2.36-mm (No. 8) sieve.
more than 0.39 g/L SO3.
Place 400 g of the pulverized material in a 400-mL beaker and
add 100 mL of water at a temperature of 23.0 6 0.6°C . 13.2 Bias—No justifiable statement can be made on the bias
Quickly mix to uniform consistency with a spatula; then stir of the procedure in this test method for measuring the
mechanically for 2 min. Use a stirrer of such a type and speed water-extractable SO3 in hardened hydraulic cement mortars,
that all particles of the slurry are suspended, with no settling because no reference samples are available.
and no appreciable increase of the temperature of the slurry
occurs. 14. Keywords
10.2 Filter the slurry on a dry No. 2A Büchner funnel with 14.1 hydraulic cement; optimum sulfate content; sulfate;
the aid of suction using a dry 90-mm, medium, ashless paper. sulfate content

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 C 265
For additional useful information on details of cement test methods, reference may be made to the “Manual of Cement
Testing,” Annual Book of ASTM Standards, Vol 04.01.

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