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: C1556 − 11a (Reapproved 2016)

Standard Test Method for

Determining the Apparent Chloride Diffusion Coefficient of
Cementitious Mixtures by Bulk Diffusion1
This standard is issued under the fixed designation C1556; 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* 2.2 NORDTEST Standards:

1.1 This test method covers the laboratory determination of NT BUILD 443 Approved 1995-11, Concrete, Hardened:
the apparent chloride diffusion coefficient for hardened cemen- Accelerated Chloride Penetration (in English)3
titious mixtures. 3. Terminology
1.2 The values stated in SI units are to be regarded as 3.1 Definitions:
standard. No other units of measurement are included in this 3.1.1 For definitions of terms used in this test method, refer
standard. to Terminology C125.
1.3 This standard does not purport to address all of the 3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the 3.2.1 apparent chloride diffusion coeffıcient, Da, n—a chlo-
responsibility of the user of this standard to establish appro- ride transport parameter calculated from acid-soluble chloride
priate safety and health practices and determine the applica- profile data obtained from saturated specimens exposed to
bility of regulatory limitations prior to use. chloride solutions, without correction for chloride binding, that
provides an indication of the ease of chloride penetration into
2. Referenced Documents
cementitious mixtures.
2.1 ASTM Standards:2
3.2.2 chloride binding, v—the chemical process by which
C31/C31M Practice for Making and Curing Concrete Test
chloride ion is removed from solution and incorporated into
Specimens in the Field
cementitious binder hydration products.
C42/C42M Test Method for Obtaining and Testing Drilled
3.2.2.1 Discussion—Chloride binding is primarily associ-
Cores and Sawed Beams of Concrete
ated with hydration products formed by the aluminate phase of
C125 Terminology Relating to Concrete and Concrete Ag-
cement and mixtures containing ground granulated blast fur-
gregates
nace slag.
C192/C192M Practice for Making and Curing Concrete Test
Specimens in the Laboratory 3.2.3 chloride penetration, v—the ingress of chloride ions
C670 Practice for Preparing Precision and Bias Statements due to exposure to external sources.
for Test Methods for Construction Materials 3.2.4 exposure liquid, n—the sodium chloride solution in
C1152/C1152M Test Method for Acid-Soluble Chloride in which test specimens are stored prior to obtaining a chloride
Mortar and Concrete profile.
C1202 Test Method for Electrical Indication of Concrete’s 3.2.5 exposure time, n—the time that the test specimen is
Ability to Resist Chloride Ion Penetration stored in the solution containing chloride ion.
3.2.6 initial chloride-ion content, Ci , n—the ratio of the
1
This test method is under the jurisdiction of ASTM Committee C09 on mass of chloride ion to the mass of concrete for a test specimen
Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee that has not been exposed to external chloride sources.
C09.66 on Concrete’s Resistance to Fluid Penetration.
Current edition approved April 1, 2016. Published May 2016. Originally 3.2.7 profile grinding, v—the process of grinding off and
approved in 2003. Last previous edition approved in 2011 as C1556 – 11a. DOI: collecting a powder sample in thin successive layers from a test
10.1520/C1556-11AR16. specimen using a dry process.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Published by NORDTEST, P.O. Box 116 FIN-02151 ESPOO Finland, Project
the ASTM website. 1154-94, e-mail: nordtest @vtt.fi, website: http://www.vtt.fi/nordtest

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

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 C1556 − 11a (2016)
3.2.8 surface chloride content, Cs, n—the theoretical ratio of 6. Apparatus
the mass of chloride ion to the mass of concrete at the interface 6.1 Balance, accurate to at least 60.01 g.
between the exposure liquid and the test specimen.
6.2 Thermometer, accurate to at least 61.0 °C.
4. Summary of Test Method 6.3 Controlled Temperature Laboratory or Chamber. The
4.1 Obtain a representative sample of the cementitious laboratory or chamber shall maintain the temperature of a
mixture prior to exposure to chloride ion. Separate each sample water bath at 23 6 2 °C.
into a test specimen and an initial chloride-ion content speci- 6.4 Plastic Container, with tight-fitting lid. Select a con-
men. Crush the initial chloride-ion content specimen and tainer size in accordance with provisions in 9.1.2.
determine the initial acid-soluble chloride-ion content. Seal all
sides of the test specimen, except the finished surface, with a 6.5 Equipment for grinding off and collecting powder from
suitable barrier coating. Saturate the sealed specimen in a concrete, mortar, or grout specimens in layers of approximately
calcium hydroxide solution, rinse with tap water, and then 2 mm thickness. Refer to Figs. 1 and 2 for examples of
place in a sodium chloride solution. After a specified exposure satisfactory equipment (see Note 3).
time, the test specimen is removed from the sodium chloride NOTE 3—A lathe or milling machine equipped with a short-barrel
carbide-tipped, or diamond-tipped, core drill bit has been found satisfac-
solution and thin layers are ground off parallel to the exposed tory for profile grinding.
face of the specimen. The acid-soluble chloride content of each
layer is determined. The apparent chloride diffusion coefficient 6.6 Resealable Polyethylene Bags, 200- to 300-mm wide by
and the projected surface chloride-ion concentration are then 250- to 300-mm long, and sheet thickness not less than 0.1
calculated using the initial chloride-ion content, and at least six mm.
related values for chloride-ion content and depth below the 6.7 Equipment for crushing concrete, mortar or grout. Suit-
exposed surface. able equipment is described in Test Method C1152/C1152M.
5. Significance and Use 6.8 Equipment for chloride analysis as described in Test
Method C1152/C1152M.
5.1 This test method is applicable to cementitious mixtures
that have not been exposed to external chloride ions, other than 6.9 Slide Caliper, accurate to at least 6 0.1 mm.
the negligible quantity of chloride ion exposure from sample
7. Reagents and Materials
preparation using potable water, prior to the test.
7.1 Distilled or De-ionized Water.
5.2 The calculation procedure described in this test method
is applicable only to laboratory test specimens exposed to a 7.2 Calcium Hydroxide [Ca(OH)2], technical grade.
sodium chloride solution as described in this test method. This 7.3 Calcium Hydroxide Solution, saturated, (approx. 3 g/L).
calculation procedure is not applicable to specimens exposed to
chloride ions during cyclic wetting and drying. 7.4 Sodium Chloride [NaCl], technical grade.
7.5 Exposure Liquid—An aqueous NaCl solution prepared
NOTE 1—The diffusion of ionic species in concrete occurs within the
fluid-filled pores, cracks and void spaces. The concentration and valence with a concentration of 165 6 1 g NaCl per L of solution.
of other ionic species in the pore fluid also influence the rate of chloride 7.6 Two-component Polyurethane or Epoxy-resin Based
diffusion, and therefore, the apparent diffusion coefficient as determined
Paint, capable of forming a barrier membrane that is resistant
by this test procedure.
to chloride ion diffusion.
5.3 In most cases, the value of the apparent chloride
diffusion coefficient for cementitious mixtures changes over 8. Test Specimens
time (see Note 2). Therefore, apparent diffusion coefficients
8.1 Drilled cores, molded cylinders, or molded cubes are
obtained at early ages may not be representative of perfor-
acceptable test specimens. One sample consists of at least two
mance in service.
NOTE 2—The rate of change of the apparent diffusion coefficient for test specimens representative of the cementitious mixture
cementitious mixtures containing pozzolans or blast-furnace slag is under test (see Note 4). Specimens must be free of defects such
typically different than that for mixtures containing only portland cement. as voids or cracks visible to the unaided eye (see Note 5). The
5.4 The apparent chloride diffusion coefficient is used in minimum dimension across the finished surface of each test
Fick’s second law of diffusion to estimate chloride penetration specimen must be at least 75 mm, but not less than three times
into cementitious mixtures that are in a saturated condition. the nominal maximum aggregate particle size. The specimen
depth must be at least 75 mm.
5.5 The apparent chloride diffusion coefficient is commonly NOTE 4—The material between the exposed surface and the outermost
used in chloride ingress models based on Fick’s second law of layer of reinforcement is often of interest because it is here that the
diffusion. The apparent diffusion coefficient determined by this protection against chloride penetration is needed. Furthermore, the quality
method includes bound chloride, so proper use of the apparent of the material in this particular area can deviate from that in the rest of
the system, as this region is often affected by construction practices.
chloride diffusion coefficient to predict chloride ingress re- NOTE 5—Specimens with voids deeper than the profile layer thickness
quires consideration of chloride binding. can increase the apparent rate of chloride penetration, and increases test
5.6 The resistance to chloride penetration is affected by such variability.
factors as the environment, finishing, mixture composition, 8.2 Unless otherwise specified, provide 28 days of labora-
workmanship, curing, and age. tory standard moist curing in accordance with Practice C31/

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 C1556 − 11a (2016)

FIG. 1 Profile Grinding Using a Milling Machine

FIG. 2 Profile Grinding Using a Lathe

C31M or C192/C192M prior to sample preparation for immer- 8.3 For drilled cores obtained according to Test Method
sion in the exposure liquid. C42/C42M, prepare the test specimen by cutting off the
8.2.1 Describe any variance from standard curing practice outermost 75 mm of the core. The test specimen thus obtained
in the report.

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 C1556 − 11a (2016)
has one face that is the original finished surface, and the other blot the surface dry with a paper towel, and determine the mass
face that is a sawn surface as shown in Fig. 3. of the specimen in the surface-dry condition.
8.4 For specimens prepared in accordance with Practice 8.10 The test specimen is immersed in a saturated calcium
C31/C31M or C192/C192M, the test specimen is prepared by hydroxide water bath until the mass does not change by more
cutting parallel to the finished surface. The top 75 mm is used than 0.1 % in 24 h (see Note 7). An acceptable alternative
as the test specimen (see Fig. 3). procedure is to vacuum saturate the specimens with saturated
8.5 From the remainder of the drilled core, or molded calcium hydroxide solution using a vacuum chamber similar to
specimen, cut a slice that is at least 20-mm thick. Use this slice the system described in Test Method C1202.
NOTE 7—Typically, the mass of moist-cured specimens stabilizes within
to determine the initial chloride-ion content, Ci either by 48 h.
crushing the entire slice or by grinding off a layer at least 2-mm
thick. Alternately, if the profile from the diffusion test specimen 9. Procedure
is ground deep enough such that the last 2 successive layers
taken have chloride contents within 0.01 % by mass of 9.1 Exposure:
concrete of each other, it is permitted to extrapolate the best-fit 9.1.1 Remove the saturated test specimen from the calcium
equation of the chloride profile to obtain the initial chloride-ion hydroxide water bath, immediately rinse the specimen surface
content, Ci. with tap water, place the specimen in the exposure container,
fill the container with the exposure liquid, and then seal the
8.6 Rinse the specimens with tap water immediately after container. Place the container in a temperature-controlled
cutting. Scrub the surface with a stiff nylon brush, and rinse chamber or room maintained at 23 6 2°C. Record the start date
again. Prior to sealing specimen surfaces, air dry until no and start time to the nearest hour.
moisture can be removed from the surface with a dry paper 9.1.2 It is permitted to place multiple specimens in a single
towel (see Note 6). container as long as the specimens are placed in the container
8.6.1 Exposure specimens must be surface-dry but inter- such that the entire exposure surface is unobstructed. Maintain
nally moist prior to sealing. This condition is satisfied by the exposed surface area to exposure liquid volume ratio within
standard moist-cured specimens allowed to air dry for no more the range of 50 6 30 cm2/L (see Note 8).
than 24 h in laboratory air maintained at 23 6 2 °C and 50 6
3 % RH. NOTE 8—The volume of exposure liquid required for nominal 100-mm
diameter cylinder or core exposure specimens is approximately one liter
NOTE 6—Specimens cured in a saturated calcium hydroxide water bath per specimen.
are normally covered by residual lime particles. If this residue is not 9.1.3 The specimens must remain in the exposure liquid for
removed and test specimens are allowed to temporarily dry in air, a
calcium carbonate layer can form on the surface of the specimen. This at least 35 days (see Note 9).
carbonate layer may interfere with the test result, which is why cleansing NOTE 9—The exposure time should be extended for mixtures such as
and rinsing with tap water after cutting or removal from the saturated those that are more mature, were made with low w/cm, or high-
calcium hydroxide water bath is required. performance mixtures containing supplementary cementitious materials.
8.7 Seal all sides of the exposure specimen except for the 9.1.4 If evaporation of water from the exposure liquid or a
finished surface following the procedure described in Test container leak allows the specimen surface to dry during the
Method C1202. exposure time, the test is not valid (see Note 10).
8.8 Determine the initial mass of the test specimen when the NOTE 10—It is suggested to monitor the mass of the sealed container if
coating has hardened. evaporation of water from the exposure solution is expected.
8.9 Immerse the test specimen in the saturated calcium 9.1.5 Record the exposure time to the nearest hour.
hydroxide water bath at 23 6 2°C in a tightly closed plastic
9.2 Profile Grinding:
container. The container must be filled to the top to prevent
9.2.1 Remove the test specimen from the exposure liquid,
carbonation. After 24 h of immersion, remove the specimen,
rinse with tap water, and dry for at least 24 h in laboratory air
maintained at 23 6 2°C and 50 6 3 % RH.
9.2.2 When grinding is to be performed longer than 48 h
after removal from the exposure solution, store the specimens
in watertight resealable polyethylene bags until time of grind-
ing. When grinding is to be performed longer than 7 days after
removal from the exposure solution, store the bagged speci-
mens in a freezer maintained at -15 °C (65 °C) until time of
grinding.
9.2.3 Obtain the powder samples by grinding off material in
layers parallel to the exposed surface. Unless the coating is
removed by sawing or by using a chisel, do not grind closer
than 5 mm from the edge of the specimen to avoid edge effects
and disturbances from the coating.
9.2.4 For the minimum exposure time of 35 days, grind off
FIG. 3 Sketch of Specimens Obtained from a Typical Sample at least eight layers in accordance with Table 1. For longer

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 C1556 − 11a (2016)
TABLE 1 Recommended Depth Intervals (in mm) for Powder GrindingA
w/cm 0.25 0.30 0.35 0.40 0.50 0.60 0.70
Depth 1 0-1 0-1 0-1 0-1 0-1 0-1 0-1
Depth 2 1-2 1-2 1-2 1-3 1-3 1-3 1-5
Depth 3 2-3 2-3 2-3 3-5 3-5 3-6 5-10
Depth 4 3-4 3-4 3-5 5-7 5-8 6-10 10-15
Depth 5 4-5 4-6 5-7 7-10 8-12 10-15 15-20
Depth 6 5-6 6-8 7-9 10-13 12-16 15-20 20-25
Depth 7 6-8 8-10 9-12 13-16 16-20 20-25 25-30
Depth 8 8-10 10-12 12-16 16-20 20-25 25-30 30-35
A
Luping, Tang and Sørensen, Henrik, “Evaluation of the Rapid Test Methods for Measuring the Chloride Diffusion Coefficients of Concrete,” NORDTEST Project No.
1388-98, Swedish National Testing and Research Institute, SP Report 1998:42.

NOTE 1—For cementitious mixtures with pozzolan or slag, the depth intervals in the column one place to the left should be applied. For example, use
the depth intervals for w/cm = 0.35 for silica fume concrete with w/cm = 0.40.

exposure times, select depth increments such that a minimum Cs = projected chloride concentration at the interface
of 6 points span the range from 1 mm below the exposed between the exposure liquid and test specimen that
surface to a depth with a chloride-ion content equal to, or is determined by the regression analysis, mass %,
slightly greater than, the initial chloride-ion content. Ci = initial chloride-ion concentration of the cementi-
9.2.5 The following alternate profiling procedure is permit- tious mixture prior to submersion in the exposure
ted if the exposure time is sufficient to allow chloride penetra- solution, mass %,
tion deeper than 40 mm. Slice the test specimen parallel to the x = depth below the exposed surface (to the middle of a
exposure surface using a water-cooled diamond saw in 5- to 6- layer), m,
mm increments, minimizing the time specimens are exposed to Da = apparent chloride diffusion coefficient, m2/s,
water. Dry the slices for 24 h in laboratory air, then crush and t = the exposure time, s, and
prepare the powder sample as described in Test Method erf = the error function described in Eq 2.
C1152/C1152M. z

9.2.6 Obtain a sample of at least 10 g of powder from each erf ~ z ! 5 2/ =π· * exp~ 2u ! du
0
2
(2)
layer. Determine the distance from the exposure surface to the
10.1.2 Tables with values of the error function are given in
mid-depth of each layer. For example, the layer thickness and
standard mathematical reference books.4 The error function is
mid-depth are determined from measurements of the specimen
also included as a library function in most electronic calcula-
before and after powder sample collection. Calculate the depth
tion software.
below the exposed surface as the average of five uniformly
10.1.3 The test results are:
distributed measurements using a slide caliper.
10.1.3.1 The initial chloride concentration, Ci (mass %),
9.3 Chloride Analysis: stated to three significant digits.
9.3.1 Determine the acid-soluble chloride-ion content of the 10.1.3.2 The projected surface chloride concentration at the
powder samples, Cx (mass %), to 60.001 % according to Test exposed surface, Cs (mass %), stated to three significant digits.
Method C1152/C1152M. 10.1.3.3 The apparent chloride diffusion coefficient, Da
9.3.2 Obtain the initial chloride-ion content, Ci (mass %), (m2/s), stated to 2 significant digits.
from the 20-mm thick slice by crushing and prepare a powder
10.2 Non-linear Regression Analysis—Perform the regres-
sample as described in Test Method C1152/C1152M.
sion analysis by minimizing the sum given in Eq 3. Refer to
9.4 Record any deviations from the requirements of this Fig. 4 for clarification.
method. N N

10. Calculations S5 ( ∆C ~ n ! 5 ( ~ C
n52
2
n52
m ~ n ! 2 C c ~ n !! 2 (3)

10.1 Test Results: where:

10.1.1 Determine the values of surface concentration and S = sum of squares to be minimized, (mass %)2,
apparent chloride diffusion coefficient by fitting Eq 1 to the N = the number of layers ground off,
measured chloride-ion contents by means of a non-linear ∆C(n) = difference between the measured and calculated
regression analysis using the method of least squares. Omit the chloride concentration of the nth layer, mass %,
chloride-ion content determined from the exposure surface Cm(n) = measured chloride concentration of the nth layer,
layer in the regression analysis. All other chloride-ion content mass %, and
measurements are included in the regression analysis. Cc(n) = calculated chloride concentration in the middle of

C ~ x,t ! 5 C s 2 ~ C s 2 C i ! ·erf S= D
x
4·D a ·t
(1)
the nth layer, mass %.
10.3 Other Calculations:
where:
C(x,t) = chloride concentration, measured at depth x and 4
Beyer, W. H., ed., CRC Handbook of Mathematical Sciences, 5th Edition, CRC
exposure time t, mass %, Press, Boca Raton, FL, 1978.

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 C1556 − 11a (2016)

FIG. 4 Sample Regression Analysis

10.3.1 Plot the measured chloride contents at all points 11.1.4 Description of the tested object including specimen
versus depth below the surface. Plot the best-fit curve on the type, identification marks, mixture proportions, the date the
same graph (see Fig. 4). tested object was cast, curing regimen employed, and age at the
start of exposure.
11. Report 11.1.5 Start date and duration of the exposure time.
11.1 Report the following information if known: 11.1.6 Conditioning of the test specimens, and a description
11.1.1 Name and address of the laboratory, and the place at of the exposure conditions during the test, such as temperature,
which tests were performed, if different from the laboratory evidence of evaporation.
address. 11.1.7 Identification of the test equipment and instruments
11.1.2 Date and identification number of the test report. used.
11.1.3 Method of sampling and other circumstances (date 11.1.8 Any deviation from the test method together with
and person responsible for sampling). other information of importance for judging the result.
11.1.9 A table listing the chloride-ion content measurements
TABLE 2 Example Calculation of each layer and mid-depth for each layer.
Ci 11.1.10 A plot showing the measured chloride-ion contents
Cs (mass %) Da (m2/s) t (yr) Sum (Error)2
(mass %) for each layer and the best-fit curve from the regression
0.605 0.085 4.86E-13 1.00 2.2151E-03
analysis.
Measured Predicted Error, ∆C(n) 11.1.11 The measured value of Ci and the values of Cs, and
x (mm) (Error)2
Value Value (Meas.-Pred.) Da determined from the regression analysis.
1 0.368 0.530
2 0.450 0.458 -8.19E-03 6.72E-05
3 0.410 0.391 1.94E-02 3.76E-04 TABLE 3 Precision EstimatesA
4 0.326 0.329 -3.31E-03 1.10E-05 Single Multiple
5 0.266 0.275 -9.49E-03 9.01E-05 Coefficient Statistic
Laboratory Laboratory
6 0.231 0.230 1.25E-03 1.55E-06
Da CVB 14.2 20.2
7 0.175 0.192 -1.71E-02 2.93E-04
d2s % 39.8 56.6
8 0.183 0.162 2.08E-02 4.34E-04
Cs CV 13.3 18.1
9 0.132 0.139 -7.07E-03 5.00E-05
d2s % 37.2 50.7
10 0.124 0.122 2.16E-03 4.66E-06
A
15 0.117 0.089 2.85E-02 8.12E-04 These statistics represent the CV (1s %) and d2s % statistics as defined in
20 0.080 0.085 -5.16E-03 2.66E-05 Practice C670.
B
25 0.078 0.085 -7.00E-03 4.90E-05 Coefficient of variation.

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 C1556 − 11a (2016)
11.1.12 Date and signature. among the mixtures ranged from 0.61 to 1.0 %. Table 3
summarizes the single-laboratory and multiple-laboratory co-
12. Precision and Bias efficient of variation and maximum difference expected be-
12.1 Precision—There has been no interlaboratory study of tween duplicate determinations in 95 % of such comparisons.
this test method. However, there are precision data5 from an Therefore, the apparent diffusion coefficient results of two
interlaboratory study of NORDTEST NT Build 443, from properly conducted tests should not differ by more than 39.8 %
which this test method was developed. The report includes data of the mean value.
from two interlaboratory studies involving three concrete
12.2 Bias—Since there is no accepted reference material
mixtures and three to five laboratories participated, depending
suitable for determining the bias of this test method, no
on the mixture. Average values of Da among the mixtures
statement on bias is made.
ranged from 2.1 to 14.7 × 10-12 m2/s. Average values of Cs
13. Keywords
5
Luping, Tang and Sørensen, Henrik, “Evaluation of the Rapid Test Methods for
Measuring the Chloride Diffusion Coefficients of Concrete,” NORDTEST Project 13.1 chloride; concrete; corrosion; diffusion; ion transport;
No. 1388-98, Swedish National Testing and Research Institute, SP Report 1998:42. service life

SUMMARY OF CHANGES

Committee C09 has identified the location of selected changes to this test method since the last issue, C1556
– 11, that may impact the use of this test method. (Approved December 15, 2011.)

(1) Revised 8.5 and 9.2.4.

Committee C09 has identified the location of selected changes to this test method since the last issue, C1556
– 04, that may impact the use of this test method. (Approved October 15, 2011.)

(1) Revised 5.5 and 9.2.3.

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