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Designation: G 180 – 04

Standard Test Method for


Initial Screening of Corrosion Inhibiting Admixtures for
Steel in Concrete1
This standard is issued under the fixed designation G 180; 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 3. Terminology
1.1 This test method describes a procedure for determining 3.1 Definitions—For definitions of terms used in this prac-
the effects of chemical admixtures on the corrosion of metals in tice see Terminology G 15.
concrete. This test method can be used to evaluate materials
intended to inhibit chloride-induced corrosion of steel in 4. Significance and Use
concrete. It can also be used to evaluate the corrosivity of 4.1 This test method provides a means for assessing
admixtures by themselves or in a chloride environment. This corrosion-inhibiting concrete admixtures.
test is not applicable for emulsions. 4.2 This test method is useful for development of admix-
1.2 Units—The values stated in SI units are to be regarded tures intended to reduce corrosion of reinforcing steel in
as standard. No other units of measurement are included in this concrete.
standard. 4.3 This test method is useful in determining the corrosivity
1.3 This standard does not purport to address all of the of admixtures toward steel reinforcing if the admixture sample
safety concerns, if any, associated with its use. It is the is compared to a control without admixtures.
responsibility of the user of this standard to establish appro- 4.4 Good performance, a reduction in corrosion rate versus
priate safety and health practices and determine the applica- chloride alone by at least one order of magnitude in this test, is
bility of regulatory limitations prior to use. a strong indication that an admixture is a corrosion inhibitor.
However, poor performance requires additional testing to
2. Referenced Documents determine if the admixture improves corrosion resistance.
2.1 ASTM Standards: 2 4.5 This method is a screening test and shall not be used to
C 150 Specification for Portland Cement predict performance in the field. However, it is useful to
C 670 Practice for Preparing Precision Statements for Test determine which admixtures shall be included into long-term
Methods for Construction Materials evaluation programs.
D 632 Specification for Sodium Chloride 4.6 The filtering process makes this test not suitable for the
E 691 Practice for Conducting an Interlaboratory Study to evaluation of emulsions.
Determine the Precision of a Test Method
G 3 Practice for Conventions Applicable to Electrochemical 5. Apparatus
Measurements in Corrosion Testing 5.1 The test cell as described in Test Method G 5.
G 5 Test Method for Making Potentiostatic and Potentiody- 5.2 Potentiostat, as described in Test Method G 5, capable
namic Anodic Polarization Measurements of varying potential at a constant scan rate and measuring the
G 15 Terminology Relating to Corrosion and Corrosion resulting current.
Testing 5.3 A method of recording the varying potential and result-
G 59 Test Method for Conducting Potentiodynamic Polar- ing current is needed.
ization Resistance Measurements 5.4 Electrode holder such as described in Fig. 3 of Test
Method G 5.
5.5 Electrodes:
1
This test method is under the jurisdiction of ASTM Committee G01 on 5.5.1 Working electrode, prepared from a 12.7 mm length of
Corrosion of Metals and is the direct responsibility of Subcommittee G01.14 on
Corrosion of Metals in Concrete, Mortar, or Cement. 9.5 mm diameter rod stock. Carbon steel C1215 should be
Current edition approved July 1, 2004. Published July 2004. used.
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 NOTE 1—If specimen forms are used other than those called for by this
Standards volume information, refer to the standard’s Document Summary page on test method, for example flat sheet specimens, care should be taken not to
the ASTM website. introduce crevices which can lead to erroneous results.

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

1
G 180 – 04
5.6 Auxiliary Electrodes: NOTE 4—An example of a polarization resistance curve is given in the
5.6.1 Two graphite rods or platinized-niobium or platinum Appendix as Fig. X1.4.
mesh. 8. Interpretation of Results
5.7 Reference Electrodes:
5.7.1 A saturated calomel electrode with a controlled rate of 8.1 An admixture is behaving as a corrosion inhibitor in this
leakage (about 3 µL/h) is recommended. test method if the average log10(1/Rp) value is 1.0 or less than
that of the chloride only average.
6. Reagents and Materials 8.2 If the admixture does not reduce average 1/Rp by an
6.1 Type I/II cement (C3A content between 6 and 10 %), order of magnitude another test method is needed to determine
according to Specification C 150. if it is an inhibitor.
6.2 Filter paper with 1.1 µm retention. 8.3 An admixture that increases average 1/Rp by an order of
6.3 Teflon stir bars. magnitude over a slurry without chloride or inhibitor is
6.4 Carbon steel C1215 samples.3 corrosive.
6.5 Sodium chloride, reagent grade, according to Specifica- NOTE 5—The change in log10(1/Rp) by 1.0 is an order of magnitude
tion D 632. change in 1/Rp. Log values are useful in comparing corrosion rates since
6.6 Calcium hydroxide, reagent grade. rates from different specimens or conditions can differ by orders of
6.7 Admixtures to be tested. magnitude making a linear scale less useful.
6.8 Carbon dioxide free compressed air.4
9. Report
7. Experimental Procedure 9.1 Report the following information:
7.1 Prepare a cement slurry consisting of 1000 g of water 9.1.1 Value of the open circuit potential (OCP) versus SCE,
and 200 g cement. Mix thoroughly, stir for 60 min and filter. and
9.1.2 Corrosion rate given by 1/Rp in µS/cm2.
NOTE 2—An admixture should be added at a quantity consistent with its
addition rate in concrete. 35 to 965 mL of water is equivalent to 5 L/m3 10. Precision and Bias
in concrete. If other dosages are desired, proportion them based on this
ratio. 10.1 Based on the pooled estimates of precision, the follow-
ing statement of precision and bias5 can be made:
7.2 Filter, and add 4 g/L calcium hydroxide and stir a further
10.1.1 Interlaboratory Test Program—An interlaboratory
30 min.
study of a pore solution test for corrosion inhibiting admixtures
7.3 Setup a standard electrochemical cell according to Test
for steel reinforcement in concrete was conducted in 2001.
Method G 5 and fill it with 900 mL of filtered slurry solution.
Each of six laboratories tested two randomly drawn samples of
Purge the cell with carbon dioxide free air. Air flow rate should
each of four materials (two sodium chloride solutions, 0.5M
be at least 300 cc/min.
and 1.0M, each with and without 35 mL/L of a solution
7.4 Degrease the metal sample by cleaning ultrasonically in
containing 30 % calcium nitrite). Practice E 691 was followed
hexane for 2 min. If an ultrasonic bath is not available, soak the
for the design and analysis of the study.
samples in hexane and wipe dry. Make sure the sample is
10.1.2 Single-Operator Precision—The single operator
thoroughly dried before mounting it on the electrode holder.
standard deviation of the logarithm to the base 10 of a single
7.5 While purging the cell with carbon dioxide free air,
test result is 0.36. Therefore, log10(1/Rp) values of two properly
precondition the electrode in the solution for 24 h.
conducted tests by the same operator should not differ by more
7.5.1 Add NaCl to the solution obtained in 7.3 (having been
than 1.0.
purged for 24 h with CO2-free air), to obtain a 0.5 or a 1M
10.1.3 Interlaboratory Precision—The interlaboratory stan-
solution, and continue purging for a further 4 h.
dard deviation of the logarithm to the base 10 of a single test
NOTE 3—The multi-laboratory test was run at the two different chloride result is 0.44. Therefore, log10(1/Rp) values of two properly
levels to develop the precision statement. The higher chloride level would conducted tests in different laboratories should not differ by
be representative of a more severe exposure. more than 1.24.
7.5.2 Measure the open circuit potential. NOTE 6—These numbers represent, respectively, the (1s) and (2ds)
7.5.3 Measure the polarization resistance (Rp) by recording limits as described in Practice C 670.
the potentiodynamic polarization curve at a scan rate of 0.167
mV/s, from –20 mV to +20 mV versus open circuit potential. 10.2 Bias—Since there is no accepted reference material
7.5.4 Plot the polarization resistance curve as a linear suitable for determining the bias in this test method, no
potential-current density plot as shown in Practice G 3. statement on bias is made.
7.5.5 Determine the polarization resistance Rp, as the tan- 11. Keywords
gent of the curve at i = 0, as described in Test Method G 59.
The corrosion rate is expressed as 1/Rp in µS/cm2. 11.1 admixtures; cement; corrosion inhibitors; slurry;
solution

3
The samples are cylindrical in shape, with 5.1 cm2 exposed area, and can be
5
purchased from Metal Samples, AL, sample type P/N410. Supporting data have been filed at ASTM Headquarters. Request RR:G01-
4
A CO2 free air gas generator (typically used for FT-IR equipment) can be used. 1021.

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G 180 – 04

APPENDIX

(Nonmandatory Information)

X1. PRECISION CALCULATIONS

X1.1 Information on the precision of the results obtained by TABLE X1.1 Statistical Analysis of Corrosion Potential Data
this test method was derived from an interlaboratory test with Practice E 691 Interlaboratory Data Analysis Software
two samples for each molarity tested, per laboratory. Six The number of laboratories, materials, and determinations in this study DOES
meet the minimum requirements for determining precision prescribed in Practice
laboratories participated in the study. Statistical analysis of the E 691:
data was performed using Practice E 691 Interlaboratory Data This Practice E 691
Analysis Software. Results are shown in the attached Table A Study Minimum
for 1/Rp measurements. Values of repeatability (Sr, r), and Laboratories 6 6
Materials 4 3
reproducibility (SR, R) are for the logarithm (base 10) of 1/Rp, Determinations 2 2
where Sr, r, SR, and R are defined as follows:
Precision Statement for Test Method
Precision and Reproducibility of Log10(1/Rp) for Each Material
Precision, characterized by repeatability (Sr, r) and reproducibility (SR, R) has
Sr = repeatability standard deviation [log(µS/cm2] (1s), been determined for the materials to be:
r = 95 % repeatability limit within a laboratory [log(µS/ Material Average Sr SR r R
cm2] (2ds), (All dimensions are Log10(µS/cm2)

SR = reproducibility standard deviation [log(µS/cm2] (1s), 0.5M NaCl 1.65 0.38 0.59 1.05 1.64
0.5M NaCl + Ca(NO2)2 0.42 0.34 0.40 0.95 1.11
and 1.0M NaCl 1.66 0.17 0.23 0.49 0.66
R = 95 % reproducibility limit between laboratories 1.0M NaCl + Ca(NO2)2 0.49 0.43 0.43 1.20 1.20
[log(µS/cm2] (2ds). Precision and Reproducibility of Log10(1/Rp) Pooled Over All Materials
Average Sr SR r R
X1.2 This study meets the minimum requirements for (All dimensions are Log10(µS/cm2)
determining precision prescribed in Practice E 691 in terms of 1.06 0.36 0.44 1.00 1.24
the number of laboratories, materials and determinations (see where:
Appendix X1, Table X1.1). Sr = repeatability standard deviation
r = 95 % repeatability limit (within laboratory)
SR = reproducibility standard deviation
X1.3 Fig. X1.1 is a graph of r and R versus average R = 95 % reproducibility limit (between laboratories)
[log10(1/Rp) + 1]. Because the ASTM data analysis software
does not accept negative numbers, a value of 1 was added to
every log10(1/Rp) value. Adding a constant to all values does
not change the standard deviation estimates. It does, however, respectively. The h statistic examines consistency of test results
change the calculated averages. In Table X1.1, the average from laboratory to laboratory. The k statistic examines consis-
values were corrected by subtracting 1 from the software tency of within-laboratory precision from laboratory to labo-
output. In Fig. X1.1, the average values were not corrected. ratory. In these plots, the horizontal lines are the critical values
There is no indication that precision varies systematically with for h and k at the 0.5 % statistical significance level. There are
average level. Therefore, pooled estimates of precision were a couple of excursions beyond the critical values for h or k in
determined which should be valid over the range of 1/Rp each plot, but there are no consistent patterns of concern in the
encompassed in the interlaboratory study. plots. Therefore, the data appear consistent for purposes of this
analysis.
X1.4 The consistency statistics for log10(1/Rp) by labora-
tory and by material, are shown in Figs. X1.2 and X1.3, X1.5 Example of a polarization resistance curve:

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G 180 – 04

FIG. X1.1 r and R versus Material Averages


Analysis: Log10(1/Rp) + 1

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G 180 – 04

FIG. X1.2 Consistency Statistics by Laboratory


Analysis: Log10(1/Rp) + 1

FIG. X1.3 Consistency Statistics by Material


Analysis: Log10(1/Rp) + 1

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G 180 – 04

FIG. X1.4 Polarization Resistance Curve

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