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 issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: C1152/C1152M − 20

Standard Test Method for

Acid-Soluble Chloride in Mortar and Concrete1
This standard is issued under the fixed designation C1152/C1152M; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope* Cores and Sawed Beams of Concrete

2
1.1 This test method provides procedures for the sampling C114 Test Methods for Chemical Analysis of Hydraulic
and analysis of hydraulic-cement mortar or concrete for Cement
chloride that is acid soluble under the conditions of test. In C125 Terminology Relating to Concrete and Concrete Ag-
most cases, acid-soluble chloride is equivalent to total chloride. gregates
C670 Practice for Preparing Precision and Bias Statements
1.2 The values stated in either SI units or inch-pound units for Test Methods for Construction Materials
are to be regarded separately as standard. Some values have C702/C702M Practice for Reducing Samples of Aggregate
only SI units because the inch-pound equivalents are not used to Testing Size
in practice. C823/C823M Practice for Examination and Sampling of
NOTE 1—Sieve size is identified by its standard designation in Speci-
Hardened Concrete in Constructions
fication E11. The alternative designation in parentheses is for information
only and does not represent a different standard sieve size. C1084 Test Method for Portland-Cement Content of Hard-
ened Hydraulic-Cement Concrete
1.3 The text of this standard references notes and footnotes
D1193 Specification for Reagent Water
that provide explanatory information. These notes and foot-
E11 Specification for Woven Wire Test Sieve Cloth and Test
notes shall not be considered as requirements of this standard.
Sieves
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3. Terminology
responsibility of the user of this standard to establish appro- 3.1 Definitions:
priate safety, health, and environmental practices and deter- 3.1.1 For definitions of terms used in this test method, refer
mine the applicability of regulatory limitations prior to use. to Terminology C125.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard- 4. Significance and Use
ization established in the Decision on Principles for the
4.1 The amount of acid-soluble chloride in most hydraulic-
Development of International Standards, Guides and Recom-
cement systems is equal to the total amount of chloride in the
mendations issued by the World Trade Organization Technical
system. However, some organic substances that may be intro-
Barriers to Trade (TBT) Committee.
duced into mortar or concrete contain chloride that is initially
2. Referenced Documents acid-insoluble that can eventually ionize and thus become
acid-soluble or water-soluble after a period of exposure in the
2.1 ASTM Standards:3 very alkaline cement system.
C42/C42M Test Method for Obtaining and Testing Drilled
4.2 Sulfides are known to interfere with the determination of
chloride content. Blast-furnace slag aggregates and cements
1
contain sulfide sulfur in concentrations that can cause such
This test method is under the jurisdiction of ASTM Committee C09 on
Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee interference and produce erroneously high test results. Treat-
C09.69 on Miscellaneous Tests. ment with hydrogen peroxide, as discussed in Test Methods
Current edition approved June 1, 2020. Published July 2020. Originally approved C114, is used to eliminate such interference.
in 1990. Last previous edition approved in 2012 as C1152/C1152M – 04 (2012)ε1.
DOI: 10.1520/C1152_C1152M-20. 4.3 There are aggregates that contain chloride that is not
2
This test method is based on a report by Clear, K. C., and Harrigan, E. T., available for corrosion. Such chloride will be detected by the
“Sampling and Testing for Chloride Ion in Concrete,” Report No. FHWA-RD77-85,
Federal Highway Administration, Washington, DC, August 1977 (available as PB
use of this method.4
275-428/AS National Technical Information Services).
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM For more information, see Hope, B. B., Page, J. A., and Poland, J. S., “The
Standards volume information, refer to the standard’s Document Summary page on Determination of the Chloride Content of Concrete,” Cement and Concrete
the ASTM website. Research, Vol 15, No. 5, Pergamon Press, New York, September 1985, pp. 863–870.

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

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 C1152/C1152M − 20
5. Apparatus tee on Analytical Reagents of the American Chemical Society.5
Other grades may be used, provided it is first ascertained that
5.1 Sampling Equipment:
the reagent is of sufficiently high purity to permit its use
5.1.1 The apparatus required for obtaining samples by without lessening the accuracy of the determination.
coring or sawing is described in Test Method C42/C42M. 6.1.1 Sodium Chloride (NaCl).
5.1.2 Use the following apparatus for sampling by drilling 6.1.2 Silver Nitrate (AgNO3).
(pulverization): 6.1.3 Potassium Chloride (KCl), (required for silver billet
5.1.2.1 Rotary Impact Drill and drill or pulverizing bits of electrode only).
sufficient diameter to provide a representative sample of 6.1.4 Reagent Water conforming to the requirements of
sufficient size for testing. Specification D1193 for Type III reagent water.
5.1.2.2 Spoon or other suitable means to remove pulverized 6.1.5 Sodium Chloride, Standard Solution (0.05 N NaCl)—
sample material from drill hole without contamination. Dry sodium chloride at 105 to 110 °C to a constant mass.
Weigh 2.9222 g of dried reagent. Dissolve in water and dilute
5.1.2.3 Sample Containers capable of maintaining samples to exactly 1 L in a volumetric flask and mix thoroughly. This
in an uncontaminated state. solution is the standard and requires no further standardization.
5.2 Sample Processing Apparatus—The apparatus required 6.1.6 Silver Nitrate, Standard Solution (0.05 N (AgNO3))—
for processing samples shall be chosen for its suitability for the Dissolve 8.4938 g of silver nitrate in water. Dilute to 1 L in a
purposes of the investigation, and frequently includes a con- volumetric flask and mix thoroughly. Standardize against 5.00
crete saw and one or more pulverizers. mL of standard 0.05 N sodium chloride solution diluted to 150
5.2.1 Samples more than 25 mm (1 in.) in maximum mL with water following the titration test method given in 9.1
dimension shall be reduced in size by use of a jaw crusher or beginning with the second sentence. The exact normality shall
broken into smaller pieces by hammering carefully to avoid be calculated from the average of three determinations as
loss of smaller pieces. follows:
5.2.2 Crush particles less than 25 mm (1 in.) in maximum N 5 0.25⁄V
dimension using a rotating puck grinding apparatus, or by where:
using a disk pulverizer, or mortar and pestle operated to restrict N = normality of AgNO3 solution,
to negligible levels the loss of fine particles. 0.25 = milliequivalents NaCl (5.0 × 0.05 N), and
5.2.3 Sieve, 850-µm (No. 20), which shall comply with V = volume of AgNO3 solution, mL.
Specification E11. Commercially available standard solutions may be used
5.3 Chloride Determination: provided the normality is checked according to the standard-
ization procedure.
5.3.1 Balance, shall be capable of reproducing results
6.1.7 Methyl Orange Indicator—Prepare a solution contain-
within 0.0002 g with an accuracy of 6 0.0002 g. Direct-
ing 2 g of methyl orange per litre of 95 % ethyl alcohol.
reading balances shall have a sensitivity not exceeding 0.0001
6.1.8 Nitric Acid (1+1).
g. Conventional two-pan balances shall have a maximum
6.1.9 Hydrogen Peroxide (30 %).
sensibility reciprocal of 0.0003 g. Any rapid weighing device
that may be provided, such as a chain, damped motion, or 7. Sampling
heavy riders, shall not increase the basic inaccuracy by more
7.1 Select the sample in accordance with Practice C823/
than 0.0001 g at any reading and with any load within the rated
C823M or as required for the purpose of the investigation.
capacity of the balance.
7.1.1 Because of the small nominal maximum size of the
5.3.2 Stirrer, magnetic variable speed, with a TFE- aggregate in a mortar, pieces of mortar having a mass of 10 g
fluorocarbon coated magnetic stirring bar. or more will be representative of a rather large volume of
5.3.3 Chloride, Silver/Sulfide Ion Selective Electrode, or a mortar.
silver billet electrode coated with silver chloride (see Note 2) 7.1.2 Take concrete cores in accordance with Test Method
with an appropriate reference electrode. C42/C42M unless otherwise specified.
5.3.4 Potentiometer, with millivolt scale readable to 1 mV NOTE 3—Concrete cores taken in accordance with Test Method
or better. A digital readout is preferred but not required. C42/C42M may be cut longitudinally to provide a 12-mm [1⁄2-in.] thick
section generally representative of the core, or cut laterally into 12-mm
NOTE 2—See Note 67 of Test Methods C114 for a discussion of suitable [1⁄2-in.] thick disks representative of the concrete core at various depths.
electrodes and coating methods. Concrete farthest from a surface into which chloride has penetrated often
provides chloride data close to that of the originally placed fresh concrete.
5.4 Glazed Paper—Paper to which fine particles do not The cooling water from core cutting may dissolve some of the chloride.
adhere, for use as described in 8.1.
5
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
6. Reagents Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical
6.1 Purity of Reagents—Reagent grade chemicals shall be
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
used in all tests. Unless otherwise indicated, it is intended that U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
all reagents shall conform to the specifications of the Commit- copeial Convention, Inc. (USPC), Rockville, MD.

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 C1152/C1152M − 20
7.1.3 Powdered concrete obtained by use of a rotary impact NOTE 7—It is not necessary to clean all the slurry residue from the sides
drill is frequently used in determining chloride concentration of the beaker, nor is it necessary that the filter remove all the fine material.
The titration may take place in a solution that contains a small amount of
with depth in bridge decks, pavements, etc. Such samples may solid matter.
be unrepresentative, especially when the nominal maximum
coarse aggregate size is 25 mm (1 in.) or more. Thus, several 9.3 For instruments equipped with a dial readout it is
such samples should be combined, or the data used with care. necessary to establish an approximate “equivalence point” by
Procedures for this method of sampling are as follows: immersing the electrodes in a beaker of water and adjusting the
7.1.3.1 Using the rotary impact drill, drill perpendicular to instrument to read about 20 mV lower than mid-scale. Record
the concrete surface or parallel to the axis of a cored specimen the approximate millivoltmeter reading. Remove the beaker
to a specified depth or a depth sufficient to obtain a represen- and wipe the electrodes with absorbent paper.
tative sample of the concrete mixture of at least 20 g of 9.4 Pipet 2.00 mL of standard 0.05 N NaCl solution into the
powdered material. To prevent sample contamination, avoid cooled sample beaker (see Note 8). Place the beaker on a
contact of sample with hands and other sources of perspiration. magnetic stirrer and add a TFE-fluorocarbon coated stir bar.
Clean all sampling tools prior to each sampling operation (see Immerse the electrodes into the solution, taking care that the
Note 4). No lubricants shall be used during drilling. stir bar does not strike the electrodes. Begin stirring gently.
NOTE 4—Sampling tools may be cleaned with a brush, cloth, ethyl Place the delivery tip of the 10 mL buret filled to the zero mark
alcohol rinse, water rinse, or other method that will not contaminate the with standardized 0.05 N AgNO3 in (preferably) or above the
sample. sample solution (see Note 9).
7.1.3.2 Transfer powdered sample into sample container NOTE 8—It is advisable to maintain constant temperature during
using a spoon or other suitable means. measurement, as the solubility of silver chloride varies markedly with
temperature at low concentrations.
8. Sample Preparation NOTE 9—If the tip of the buret is out of the solution, any adhering
droplet should be rinsed into the beaker with a few millilitres of water
8.1 Pulverize the sample so that all the material will pass a following each titration increment.
850-µm (No. 20) sieve. Thoroughly blend the material by
9.5 Gradually titrate, record the amount of standard 0.05 N
coning as described in Practice C702/C702M from one glazed
silver nitrate solution required to bring the millivoltmeter
paper to another at least 10 times.
reading to –60.0 mV of the equivalence point determined in the
water.
9. Procedure
9.6 Continue the titration with 0.20 mL increments. Record
9.1 Determine the mass of approximately 10 g of sample to
the buret reading and the corresponding millivoltmeter reading.
the nearest 0.01 g and transfer to a 250 mL beaker. Disperse the
Allow sufficient time between each addition for the electrodes
sample with 75 mL of water. Slowly add 25 mL of dilute (1+1)
to reach equilibrium with the sample solution (see Note 10).
nitric acid and stir with a glass rod, breaking up any lumps of
sample. If the smell of hydrogen sulfide is strongly present, add NOTE 10—Experience has shown that acceptable readings are obtained
3 mL of hydrogen peroxide (see Note 5). Add 3 drops of when the minimum scale reading does not change within a 5-s period.
methyl orange indicator to the beaker and stir. Cover the beaker 9.7 As the equivalence point is approached, the equal
with a watch glass and allow to stand for 1 to 2 minutes. If the additions of silver nitrate solution will cause larger and larger
solution above the settled solids is not pink colored, add more changes in the millivoltmeter readings. Past the equivalence
nitric acid dropwise while stirring until a pink or reddish color point, the change per increment will decrease. Continue to
persists, then add 10 additional drops of nitric acid and stir. titrate until three readings past the approximate equivalence
Heat the covered beaker rapidly to boiling and remove from point have been recorded.
hot plate. Do not allow sample to boil more than a few seconds
(see Note 6). Make a blank determination using 75 mL of water 9.8 Calculate the precise equivalence point of the titration
in place of sample. (see Note 11) and subtract the results of the water blank (see
Note 12)
NOTE 5—Slags and slag cements contain sulfide sulfur in concentra-
tions that can interfere with chloride determination unless oxidized with NOTE 11—An example of recording solution, millivolt readings, and
hydrogen peroxide. calculation of the titration equivalence point can be found in Appendix X1
NOTE 6—To prevent loss of chloride by volatilization, it is important to of Test Methods C114.
keep the beaker covered during heating and digestion. Ten seconds of NOTE 12—For nonreferee analysis, the blank may be omitted.
boiling is sufficient. Excessive amounts of acid can erode the silver
chloride coating on the silver billet electrode prematurely. A slurry that is 10. Calculation
only slightly acidic is sufficient.
9.2 Filter the sample through a 9-cm coarse-textured filter 10.1 Calculate percent chloride by mass of mortar or con-
paper in a 250 mL or 500 mL Buchner funnel and filtration crete to the nearest 0.001 % as follows:
flask using suction. Rinse the beaker and the filter paper twice C1, % 5 3.545@ ~ V 1 2 V 2 ! N # ⁄W
with small portions of water. Transfer the filtrate from the flask where:
to a 250 mL beaker and rinse the flask once with water. The
V1 = millilitres of 0.05 N AgNO3 solution used for sample
original beaker may be used (see Note 7). Cool the filtrate to
titration (equivalence point),
room temperature. The volume should not exceed 175 mL.

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 C1152/C1152M − 20

V2 = millilitres of 0.05 N AgNO3 solution used for blank 11. Precision and Bias
titration (equivalence point), 11.1 Precision:
N = exact normality of 0.05 N AgNO3 solution, and
W = mass of sample, g. 11.1.1 Single-Operator Precision—The single-operator
standard deviation has been found to be 0.0015 % chloride.
10.2 Other useful measures of chloride concentration can be
Therefore, results of two properly conducted tests by the same
obtained as follows:
10.2.1 For calculating kilograms of chloride per cubic metre operator on the same material are not expected to differ by
[pounds of chloride per cubic yard] of concrete (see Note 13), more than 0.0042 %.6
multiply percent chloride by D1/100 or D2/100 to the nearest 11.1.2 Multilaboratory Precision—The multilaboratory
0.1 kg/m3 [lb/yd3], standard deviation has been found to be 0.0021 %. Therefore,
results of two properly conducted tests by two different
where:
laboratories on specimens of the same material are not ex-
D1 = oven dry density as determined in the section on pected to differ by more than 0.0059 %.6
Concrete Density in Test Method C1084, kg/m3 [lb/
yd3], and NOTE 14—These precision statements apply to tests of samples pre-
D2 = saturated-surface-dry density as determined in the sec- pared and ground by a single laboratory. For this reason, test results will
tion on Concrete Density in Test Method C1084, kg/m3 vary depending upon the method of obtaining the sample and the size of
[lb/yd3]. the sample before it is crushed and reduced to pass the 850-µm (No. 20)
sieve, or pulverized. The effect may be small for large concrete cores or
Report which density was used in the calculation. from mortars sectioned vertically to appreciable for large aggregate
NOTE 13—In the case of drilled samples or where the actual density can concretes sampled by rotary impact drilling with small diameter drills. A
not be determined: U = density of mortar or concrete, kg/m3 [lb/yd3]. The copy of the research report used to develop the precision statements is
air dry density of normal weight concrete for most purposes can be available by request.7
assumed to be 2263 kg/m3 [3815 lb/yd3].
11.2 Bias—Since there is no accepted reference material
10.2.2 For calculating percent chloride by mass of cement, suitable for determining the bias for the procedure in this test
multiply percent chloride by 100/P, method, no statement on bias is being made.
where:
P = percent cement by mass in the mortar or concrete, as
known or determined in accordance with Test Method
C1084. 6
These numbers represent the difference limits (d2s) as described in Practice
C670.
10.2.3 For calculating equivalent flake calcium chloride 7
Supporting data have been filed at ASTM International Headquarters and may
(calcium chloride dihydrate) concentrations, multiply percent be obtained by requesting Research Report RR:C09-1003. Contact ASTM Customer
chloride by 2.07. Service at [email protected].

SUMMARY OF CHANGES

Committee C09 has identified the location of selected changes to this standard since the last issue
(C1152/C1152M – 04 (2012)ε1) that may impact the use of this standard. (Approved June 1, 2020.)

(1) Revised 2.1 and Section 11. (2) Added Section 3.

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