Designation: C 1152/C 1152M – 04

Standard Test Method for

Acid-Soluble Chloride in Mortar and Concrete1
This standard is issued under the fixed designation C 1152/C 1152M; 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 ened Hydraulic-Cement Concrete

1.1 This test method2 provides procedures for the sampling D 1193 Specification for Reagent Water
and analysis of hydraulic-cement mortar or concrete for E 11 Specification for Wire Cloth and Sieves for Testing
chloride that is acid soluble under the conditions of test. In Purposes
most cases, acid-soluble chloride is equivalent to total chloride. 3. Significance and Use
1.2 The text of this standard references notes and footnotes
that provide explanatory information. These notes and foot- 3.1 The amount of acid-soluble chloride in most hydraulic-
notes shall not be considered as requirements of this standard. cement systems is equal to the total amount of chloride in the
1.3 This standard does not purport to address all of the system. However, some organic substances that may be intro-
safety concerns, if any, associated with its use. It is the duced into mortar or concrete contain chloride that is initially
responsibility of the user of this standard to establish appro- acid-insoluble that can eventually ionize and thus become
priate safety and health practices and determine the applica- acid-soluble or water-soluble after a period of exposure in the
bility of regulatory limitations prior to use. very alkaline cement system.
1.4 The values stated in either SI units or inch-pound units 3.2 Sulfides are known to interfere with the determination of
are to be regarded separately as standard. Within the text, the chloride content. Blast-furnace slag aggregates and cements
inch-pound units are shown in brackets. The values stated in contain sulfide sulfur in concentrations that can cause such
each system are not exact equivalents; therefore, each system interference and produce erroneously high test results. Treat-
shall be used independently of the other. ment with hydrogen peroxide, as discussed in Test Methods
C 114, is used to eliminate such interference.
2. Referenced Documents 3.3 There are aggregates that contain chloride that is not
2.1 ASTM Standards: 3 available for corrosion. Such chloride will be detected by the
C 42/C 42M Test Method for Obtaining and Testing Drilled use of this method.4
Cores and Sawed Beams of Concrete 4. Apparatus
C 114 Test Methods for Chemical Analysis of Hydraulic
Cement 4.1 Sampling Equipment
C 670 Practice for Preparing Precision and Bias Statements 4.1.1 The apparatus required for obtaining samples by
for Test Methods for Construction Materials coring or sawing is described in Test Method C 42/C 42M.
C 702 Practice for Reducing Samples of Aggregate to 4.1.2 Use the following apparatus for sampling by drilling
Testing Size (pulverization):
C 823 Practice for Examination and Sampling of Hardened 4.1.2.1 Rotary Impact Drill and drill or pulverizing bits of
Concrete in Constructions sufficient diameter to provide a representative sample of
C 1084 Test Method for Portland-Cement Content of Hard- sufficient size for testing.
4.1.2.2 Spoon or other suitable means to remove pulverized
sample material from drill hole without contamination.
1
4.1.2.3 Sample Containers capable of maintaining samples
This test method is under the jurisdiction of ASTM Committee C09 on
Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee
in an uncontaminated state.
C09.69 on Miscellaneous Tests. 4.2 Sample Processing Apparatus—The apparatus required
Current edition approved June 1, 2004. Published July 2004. Originally approved for processing samples shall be chosen for its suitability for the
in 1990. Last previous edition approved in 2003 as C 1152 – 03. purposes of the investigation, and frequently includes a con-
2
This test method is based on a report by Clear, K. C., and Harrigan, E. T.,
“Sampling and Testing for Chloride Ion in Concrete,” Report No. FHWA-RD77-85, crete saw and one or more pulverizers.
Federal Highway Administration, Washington, DC, Aug. 1977 (Available as PB
275-428/AS National Technical Information Services).
3 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or For more information, see “The Determination of the Chloride Content of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Concrete,” by Brian B. Hope, John A. Page and John S. Poland, Cement and
Standards volume information, refer to the standard’s Document Summary page on Concrete Research, Volume 15, Number 5, Pergamon Press, New York, September
the ASTM website. 1985, pp. 863-870.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 C 1152/C 1152M – 04
4.2.1 Samples more than 25 mm (1 in.) in maximum 5.1.6 Silver Nitrate, Standard Solution (0.05 N (AgNO3))—
dimension shall be reduced in size by use of a jaw crusher or Dissolve 8.4938 g of silver nitrate in water. Dilute to 1 L in a
broken into smaller pieces by hammering carefully to avoid volumetric flask and mix thoroughly. Standardize against 5.00
loss of smaller pieces. mL of standard 0.05 N sodium chloride solution diluted to 150
4.2.2 Crush particles less than 25 mm (1 in.) in maximum mL with water following the titration test method given in 8.1
dimension using a rotating puck grinding apparatus, or by beginning with the second sentence. The exact normality shall
using a disk pulverizer, or mortar and pestle operated to restrict be calculated from the average of three determinations as
to negligible levels the loss of fine particles. follows:
4.2.3 Sieve, 850-µm [No. 20], which shall comply with N = 0.25/V, where:
Specification E 11.
4.3 Chloride Determination
4.3.1 Balance, shall be capable of reproducing results N = normality of AgNO3 solution,
0.25 = milliequivalents NaCl (5.0 3 0.05 N), and
within 0.0002 g with an accuracy of 6 0.0002 g. Direct-
V = volume of AgNO3 solution, mL.
reading balances shall have a sensitivity not exceeding 0.0001
g. Conventional two-pan balances shall have a maximum
Commercially available standard solutions may be used pro-
sensibility reciprocal of 0.0003 g. Any rapid weighing device
vided the normality is checked according to the standardization
that may be provided, such as a chain, damped motion, or
procedure.
heavy riders, shall not increase the basic inaccuracy by more
5.1.7 Methyl Orange Indicator—Prepare a solution contain-
than 0.0001 g at any reading and with any load within the rated
ing 2 g of methyl orange per litre of 95 % ethyl alcohol.
capacity of the balance.
5.1.8 Nitric Acid (1+1).
4.3.2 Stirrer, magnetic variable speed, with a TFE-
5.1.9 Hydrogen Peroxide (30 %).
fluorocarbon coated magnetic stirring bar.
4.3.3 Chloride, Silver/Sulfide Ion Selective Electrode, or a 6. Sampling
silver billet electrode coated with silver chloride (see Note 1) 6.1 Select the sample per Practice C 823 or as required for
with an appropriate reference electrode. the purpose of the investigation.
4.3.4 Potentiometer, with millivolt scale readable to 1 mV 6.1.1 Because of the small nominal maximum size of the
or better. A digital readout is preferred but not required. aggregate in a mortar, pieces of mortar having a mass of 10 g
NOTE 1—See Note 67 of Test Methods C 114 for a discussion of or more will be representative of a rather large volume of
suitable electrodes and coating methods. mortar.
4.4 Glazed Paper—Paper to which fine particles do not 6.1.2 Take concrete cores in accordance with Test Method
adhere, for use as described in 7.1. C 42/C 42M unless otherwise specified.
NOTE 2—Concrete cores taken in accordance with Test Method C 42/
5. Reagents C 42M may be cut longitudinally to provide a 12-mm [1⁄2-in.] thick section
5.1 Purity of Reagents—Reagent grade chemicals shall be generally representative of the core, or cut laterally into 12-mm [1⁄2-in.]
used in all tests. Unless otherwise indicated, it is intended that thick disks representative of the concrete core at various depths. Concrete
farthest from a surface into which chloride has penetrated often provides
all reagents shall conform to the specifications of the Commit-
chloride data close to that of the originally placed fresh concrete. The
tee on Analytical Reagents of the American Chemical Society5. cooling water from core cutting may dissolve some of the chloride.
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use 6.1.3 Powdered concrete obtained by use of a rotary impact
without lessening the accuracy of the determination. drill is frequently used in determining chloride concentration
5.1.1 Sodium Chloride (NaCl). with depth in bridge decks, pavements, etc. Such samples may
5.1.2 Silver Nitrate (AgNO3). be unrepresentative, especially when the nominal maximum
5.1.3 Potassium Chloride (KCl), (required for silver billet coarse aggregate size is 25 mm [1 in.] or more. Thus, several
electrode only). such samples should be combined, or the data used with care.
5.1.4 Reagent Water conforming to the requirements of Procedures for this method of sampling are as follows:
Specification D 1193 for Type III reagent water. 6.1.3.1 Using the rotary impact drill, drill perpendicular to
5.1.5 Sodium Chloride, Standard Solution (0.05 N NaCl)— the concrete surface or parallel to the axis of a cored specimen
Dry sodium chloride at 105 to 110 °C to a constant mass. to a specified depth or a depth sufficient to obtain a represen-
Weigh 2.9222 g of dried reagent. Dissolve in water and dilute tative sample of the concrete mixture of at least 20 g of
to exactly 1 L in a volumetric flask and mix thoroughly. This powdered material. To prevent sample contamination, avoid
solution is the standard and requires no further standardization. contact of sample with hands and other sources of perspiration.
Clean all sampling tools prior to each sampling operation (See
Note 3). No lubricants shall be used during drilling.
5
Reagent Chemicals, American Chemical Society Specifications, American NOTE 3—Sampling tools may be cleaned with a brush, cloth, ethyl
Chemical Society, Washington, DC. For suggestions on the testing of reagents not alcohol rinse, water rinse, or other method that will not contaminate the
listed by the American Chemical Society, see Analar Standards for Laboratory sample.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, 6.1.3.2 Transfer powdered sample into sample container
MD. using a spoon or other suitable means.

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 C 1152/C 1152M – 04
7. Sample Preparation NOTE 8—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
7.1 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
coning as described in Practice C 702 from one glazed paper to 8.5 Gradually titrate, record the amount of standard 0.05 N
another at least 10 times. silver nitrate solution required to bring the millivoltmeter
reading to -60.0 mV of the equivalence point determined in the
8. Procedure water.
8.6 Continue the titration with 0.20 mL increments. Record
8.1 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 9).
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 9—Experience has shown that acceptable readings are obtained
3 mL of hydrogen peroxide (See Note 4). 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 8.7 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 8.8 Calculate the precise equivalence point of the titration
(See Note 5). Make a blank determination using 75 mL of (See Note 10) and subtract the results of the water blank (See
water in place of sample. Note 11)
NOTE 4—Slags and slag cements contain sulfide sulfur in concentra- NOTE 10—An example of recording solution, millivolt readings, and
tions that can interfere with chloride determination unless oxidized with calculation of the titration equivalence point can be found in Appendix X1
hydrogen peroxide. of Test Methods C 114.
NOTE 5—To prevent loss of chloride by volatilization, it is important to NOTE 11—For nonreferee analysis, the blank may be omitted.
keep the beaker covered during heating and digestion. Ten seconds of
boiling is sufficient. Excessive amounts of acid can erode the silver 9. Calculation
chloride coating on the silver billet electrode prematurely. A slurry that is
only slightly acidic is sufficient. 9.1 Calculate percent chloride by mass of mortar or concrete
to the nearest 0.001 % as follows:
8.2 Filter the sample through a 9-cm coarse-textured filter
C1, % = 3.545 [(V1-V2) N] W, where:
paper in a 250 mL or 500 mL Buchner funnel and filtration
flask using suction. Rinse the beaker and the filter paper twice
with small portions of water. Transfer the filtrate from the flask V1 = millilitres of 0.05 N AgNO3 solution used for sample
to a 250 mL beaker and rinse the flask once with water. The titration (equivalence point),
original beaker may be used (See Note 6). Cool the filtrate to V2 = millilitres of 0.05 N AgNO3 solution used for blank
room temperature. The volume should not exceed 175 mL. titration (equivalence point),
N = exact normality of 0.05 N AgNO3 solution,
NOTE 6—It is not necessary to clean all the slurry residue from the sides
of the beaker, nor is it necessary that the filter remove all the fine material.
W = mass of sample, g.
The titration may take place in a solution that contains a small amount of 9.2 Other useful measures of chloride concentration can be
solid matter. obtained as follows:
9.2.1 For calculating kilograms of chloride per cubic metre
8.3 For instruments equipped with a dial readout it is
[pounds of chloride per cubic yard] of concrete (see Note 12),
necessary to establish an approximate 9equivalence point9 by
multiply percent chloride by D1/100 or D2/100 to the nearest
immersing the electrodes in a beaker of water and adjusting the
0.1 kg/m3[lb/yd3], where:
instrument to read about 20 mV lower than mid-scale. Record
the approximate millivoltmeter reading. Remove the beaker
and wipe the electrodes with absorbent paper. D1 = oven dry density as determined in the section on
8.4 Pipet 2.00 mL of standard 0.05 N NaCl solution into the Concrete Density in Test Method C 1084, kg/m3[lb/
cooled sample beaker (See Note 7). Place the beaker on a yd3].
magnetic stirrer and add a TFE-fluorocarbon coated stir bar. D2 = saturated-surface-dry density as determined in the
Immerse the electrodes into the solution, taking care that the section on Concrete Density in Test Method C 1084,
stir bar does not strike the electrodes. Begin stirring gently. kg/m3[lb/yd3].
Place the delivery tip of the 10 mL buret filled to the zero mark
with standardized 0.05 N AgNO3 in (preferably) or above the Report which density was used in the calculation.
sample solution (See Note 8).
NOTE 12—In the case of drilled samples or where the actual density can
NOTE 7—It is advisable to maintain constant temperature during not be determined: U = density of mortar or concrete, kg/m3[lb/yd3]. The
measurement, as the solubility of silver chloride varies markedly with air dry density of normal weight concrete for most purposes can be
temperature at low concentrations. assumed to be 2263 kg/m3[3815 lb/yd3].

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 C 1152/C 1152M – 04
9.2.2 For calculating percent chloride by mass of cement, properly conducted tests in the same laboratory on the same
multiply percent chloride by 100/P, where: material should not differ by more than 0.0042 % (b).
10.1.2 The multilaboratory standard deviation has been
found to be 0.0021 % (a). Therefore, results of two properly
P = percent cement by mass in the mortar or concrete, as
conducted tests from two different laboratories on samples of
known or determined in accordance with Test Method
the same material should not differ by more than 0.0059 % (b).
C 1084.
9.2.3 For calculating equivalent flake calcium chloride (cal- NOTE 13—The numbers (a) and (b) represent, respectively, the (1S) and
cium chloride dihydrate) concentrations, multiply percent chlo- (D2S) limits as described in Practice C 670. This precision statement
ride by 2.07. applies to tests of samples prepared and ground by a single laboratory. For
this reason, test results will vary depending upon the method of obtaining
10. Precision and Bias the sample and the size of the sample before it is crushed and reduced to
pass the 850-µm [No. 20] sieve, or pulverized. The effect may be small for
10.1 Precision6 large concrete cores or from mortars sectioned vertically to appreciable for
10.1.1 The single laboratory standard deviation has been large aggregate concretes sampled by rotary impact drilling with small
found to be 0.0015 % chloride (a). Therefore, results of two diameter drills.
10.2 Bias—Since there is no accepted reference material
6
A copy of the research report used to develop the precision statement is suitable for determining the bias for the procedure in this test
available from ASTM Headquarters. Request RR:C9-1003. method, no statement on bias is being made.

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