ASTM C1524-02

Standard Test Method for Water-Extractable Chloride in Aggregate (Soxhlet Method)

SCOPE
1.1 This test method provides procedures for sampling and analysis of aggregate for water-extractable chloride using a Soxhlet extractor.
Note 1—This test method is to be used when significantly high chloride content has been found in aggregates, concretes, or mortars.
1.2 The values stated in SI units are to be regarded as standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 09-Jul-2002
• ICS: 91.100.30 - Concrete and concrete products
• Technical Committee: C09 - Concrete and Concrete Aggregates
• Drafting Committee: C09.69 - Miscellaneous Tests

Relations

• Replaced By: ASTM C1524-02a - Standard Test Method for Water-Extractable Chloride in Aggregate (Soxhlet Method)
• Effective Date: 10-Dec-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: C 1524 – 02
Standard Test Method for
Water-Extractable Chloride in Aggregate (Soxhlet Method)
This standard is issued under the fixed designation C 1524; 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 Steel in Mortar and Concrete Using the Soxhlet Extractor
1.1 This test method provides procedures for sampling and
3. Significance and Use
analysis of aggregate for water-extractable chloride using a
3.1 Water-extractable chloride, when present in sufficient
Soxhlet extractor.
amount, has a potential to initiate or accelerate corrosion of
NOTE 1—This test method is to be used when significantly high
metals, such as steel, embedded in or contacting a cementitious
chloride content has been found in aggregates, concretes, or mortars.
system, such as mortar, grout, or concrete. This test method is
1.2 The values stated in SI units are to be regarded as
applicable when aggregates contain a high background of
standard.
naturally occurring chloride (see ACI 222.1–96 ). Test Method
1.3 This standard does not purport to address all of the
C 1152/C 1152M determines acid-soluble chloride and Test
safety concerns, if any, associated with its use. It is the
Method C 1218/C 1218M determines water-soluble chloride.
responsibility of the user of this standard to establish appro-
Both Test Methods C 1152/C 1152M and C 1218/C 1218M
priate safety and health practices and determine the applica-
pulverize the sample to a fine powder or fine granular material.
bility of regulatory limitations prior to use.
The Soxhlet method is intended to use nonpulverized material.
Results with some aggregates have shown that the Soxhlet
2. Referenced Documents
procedure extracts an extremely low amount of chloride, with
2.1 ASTM Standards:
most of it remaining in the rock, and therefore, it is not
C 114 Test Methods for Chemical Analysis of Hydraulic
available for corrosion.
Cement
3.2 The Soxhlet extraction apparatus consists of three sec-
C 670 Practice for Preparing Precision and Bias Statements
tions: the boiling flask, which contains reagent water at the
for Test Methods for Construction Materials
beginning of the test; the extractor, which contains the sample
C 1152/C 1152M Test Method for Acid-Soluble Chloride in
inside a thimble; and, the condenser. The extractor functions by
Mortar and Concrete
boiling the water, which condenses and drips on to the sample.
C 1218/C 1218M Test Method for Water-Soluble Chloride
When the water attains a fixed height above the sample, the
in Mortar and Concrete
extractor siphons the water from the thimble back to the boiling
D 75 Practice for Sampling Aggregates
flask. The process repeats itself until the test is terminated.
D 1193 Specification for Reagent Water
(Refer to Fig. 1.)
E 11 Specification for Wire Cloth and Sieves for Testing
4. Apparatus
Purposes
2.2 American Concrete Institute Standard:
4.1 Sampling Equipment:
ACI 222.1–96 Provisional Standard Test Method for Water-
4.1.1 The apparatus required for obtaining aggregate
Soluble Chloride Available for Corrosion of Embedded
samples is described in Practice D 75.
4.2 Sampling Processing Apparatus, the same as in Test
Method C 1218/C 1218M without pulverization.
4.3 Soxhlet Extractor Apparatus, shall have the following
minimum size and consist of the following (see Fig. 1).
4.3.1 Reflux-Type Condenser, with a 34/45-mm ground-
This test method is under the jurisdiction of ASTM Committee C09 on
Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee glass fitting to the extractor, and having a 27-mm inside
C09.69 on Miscellaneous Tests.
diameter by a 192-mm body length.
Current edition approved July 10, 2002. Published August 2002. Originally
4.3.2 Soxhlet Extraction Tube, with a 34/45-mm ground-
published as PS 118–99. Last previous edition PS 118–99.
Annual Book of ASTM Standards, Vol 04.01. glass fitting to the condenser and a 24/40-mm ground-glass
Annual Book of ASTM Standards, Vol 04.02.
Annual Book of ASTM Standards, Vol 04.03.
5 7
Annual Book of ASTM Standards, Vol 11.01. Available from American Concrete Institute (ACI), P.O. Box 9094, Farmington
Annual Book of ASTM Standards, Vol 14.02. Hills, MI 48333.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 1524
FIG. 1 Soxhlet Extraction Apparatus
fitting to the boiling flask, for holding sample thimbles 25 mm and the Procedure section of Test Method C 1218/C 1218M.
by 80 mm (diameter by height). 5.2 Reagent water is either deionized or distilled, conform-
4.3.3 A 250-mL boiling flask with a 24/40-mm ground-glass ing to the requirements of Specification D 1193 for Type III
fitting. reagent water.
4.3.4 A heating mantel, burner, or hot plate configured for
6. Sample Preparation
the flask capable of attaining 200°C.
6.1 Preparation:
4.3.5 Suitable Sample Holder, such as a porous extraction
6.1.1 For Nominal Maximum Aggregate Sizes 25.0 mm or
thimble having a 25-mm inside diameter and 80-mm external
Greater:
length.
Use a jaw crusher or hammer, and reduce the sample so that
4.4 The apparatus required for the chloride determination
the particles pass a 25.0-mm sieve and are representative of the
step is given in the test method for chloride in Test Methods
sample. Use a sample splitter or use coning and quartering to
C 114.
reduce the sample to between 200 and 500 g. Do not crush the
4.5 pH Paper, short-range 0.0-3.0.
sample to a powder. Oven dry the reduced sample at 110 6 5°C
4.6 Drying Oven, of sufficient size, capable of continuously
for2h.
heating at 110 6 5°C.
6.1.2 For Nominal Maximum Aggregate Sizes Less Than
5. Reagents
25.0 mm :
5.1 The reagents required for the chloride determination are Use a sample splitter or use coning and quartering to reduce
given in the test method for chloride of Test Methods C 114, the sample to between 200 and 500 g. Do not crush the sample
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 1524
to a powder. Oven dry the reduced sample at 110 6 5°C for 2 a stirring bar composed of polytetrafluoroethylene (PTFE) and
h. allow to stand for 1 to 2 min. While stirring, heat the covered
beaker rapidly to boiling. Do not boil for more than a few
7. Procedure
seconds. Remove from the hot plate.
7.1 Mix and cone the reduced sample three times before
NOTE 4—It is important to keep the beaker covered during heating and
sampling each replicate. Obtain a minimum mass of 30.0 g of
digestion to prevent the loss of volatile chloride.
the sample by sampling from at least four points, record the
7.1.3 Proceed in accordance wi
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