ASTM C1084-97
(Test Method)Standard Test Method for Portland-Cement Content of Hardened Hydraulic-Cement Concrete
Standard Test Method for Portland-Cement Content of Hardened Hydraulic-Cement Concrete
SCOPE
1.1 This test method covers the determination of portland-cement content of a sample of hardened hydraulic-cement concrete.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information purposes only.
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. Disposal of some or all of the chemicals used in this method may require adherence to EPA or other regulatory guidelines.
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Designation: C 1084 – 97
Standard Test Method for
Portland-Cement Content of Hardened Hydraulic-Cement
Concrete
This standard is issued under the fixed designation C 1084; 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 procedures and an extraction procedure. Each procedure re-
quires a substantial degree of chemical skill and relatively
1.1 This test method covers the determination of portland-
elaborate chemical instrumentation. Except for the influence of
cement content of a sample of hardened hydraulic-cement
known interferences, determined cement contents are normally
concrete.
equal to, or slightly greater than, actual values except for the
1.2 The values stated in SI units are to be regarded as the
Maleic Acid procedure where results can also be significantly
standard. The values given in parentheses are provided for
low when the paste is carbonated (Note 1).
information purposes only.
1.3 This standard does not purport to address all of the
NOTE 1—With certain limitations, the procedure is also applicable for
safety concerns, if any, associated with its use. It is the estimating the combined content of portland cement and pozzolan or slag
in concretes made with blended hydraulic cement and blends of portland
responsibility of the user of this standard to establish appro-
cement with pozzolans or slags. The results of this test method when
priate safety and health practices and determine the applica-
applied to concretes made with blended cements or pozzolans depend on
bility of regulatory limitations prior to use. Disposal of some or
the composition of the pozzolan, the age of the concrete, the extent of
all of the chemicals used in this method may require adherence
reaction of the pozzolan and the fact that this test method may determine
to EPA or other regulatory guidelines.
only the portland-cement component of a blended cement. The test
method should be applied to determination of the blended cement content
2. Referenced Documents
or the pozzolanic content only by use of calibration concrete samples or
other information. Earlier versions of this test method can provide useful
2.1 ASTM Standards:
6 7
information as detailed by Hime and Minnick.
C 42 Test Method for Obtaining and Testing Drilled Cores
and Sawed Beams of Concrete
4. Interferences
C 114 Test Methods for Chemical Analysis of Hydraulic
4.1 Many constituents of concrete may interfere with the
Cement
analysis of the concrete for portland-cement content. The
C 670 Practice for Preparing Precision and Bias Statements
following limited lists of materials have been provided as a
for Test Methods for Construction Materials
guide. The rocks, minerals or mineral admixtures listed will
C 823 Practice for Examination and Sampling of Hardened
interfere with the cement content determination to the extent of
Concrete in Constructions
their solubility during the dissolution procedure used. The
C 856 Practice for Petrographic Examinations for Hardened
solubility of rocks, minerals or mineral admixtures may depend
Concrete
4 on the fineness of the test sample, the water-cement ratio of the
D 1193 Specification for Reagent Water
concrete, the extent of hydration, and the age of the concrete
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
2 (extended exposure to the high pH of the concrete may affect
poses
5 the solubility of some minerals).
E 832 Specification for Laboratory Filter Papers
4.2 Substances Affecting Calcium Oxide Sub-procedure:
3. Significance and Use 4.2.1 The following are soluble in even the cold dilute
hydrochloric acid of this procedure and will contribute a high
3.1 This test method consists of two independent proce-
bias to the cement content calculated from the soluble calcium
dures: an oxide-analysis procedure that consists of two sub-
oxide: limestone, marble, dolomitic limestone, calcareous
This method is under the jurisdiction of ASTM Committee C-9 on Concrete and
Concrete Aggregatesand is the direct responsibility of Subcommittee C09.69 on Hime, W. G., “Cement Content,” Significance of Tests and Properties of
Miscellaneous Tests. Concrete and Concrete-Making Materials, ASTM STP 169B, ASTM, 1978, pp.
Current edition approved Jan. 10, 1997. Published July 1997. Originally 462–470, and “Analyses for Cement and Other Materials in Hardened Concrete,”
published as C 1084 – 87. Last previous edition C 1084 – 92. Chapter 29, Significant of Tests and Properties of Concrete and Concrete-Making
Annual Book of ASTM Standards, Vol 04.02. Materials, ASTM STP 169C, 1994, pp. 315–319.
3 7
Annual Book of ASTM Standards, Vol 04.01. Minnick, L. J., “Cement-Content, Hardened Concrete,” Significance of Tests
Annual Book of ASTM Standards, Vol 11.01. and Properties of Concrete and Concrete-Making Materials, ASTM STP 169A,
Annual Book of ASTM Standards, Vol 15.09. ASTM, 1966, p. 326–329.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
C 1084
sandstone, calcareous chert, and caliche encrusted and calcite in Specification E 832.
or dolomite coated rocks. 5.1.9 Beakers, 1000 and 250 mL.
4.2.2 The following may be soluble depending on the age 5.1.10 Magnetic stirrer, variable speed, with a TFE-
and pH of the concrete; whether the mineral present is glassy fluorocarbon-coated magnetic stirring rod, or an overhead
or crystalline, or weathered or strained; and the fineness of the stirrer with a propeller.
mineral present, and, if soluble, will bias the cement content 5.1.11 Volumetric flask, 1000 mL and 500 mL.
calculated from the soluble calcium oxide high depending on 5.1.12 Filtering flask, 2000 mL.
the calcium content of the minerals: weathered or altered 5.1.13 Vacuum pump.
plagioclase feldspar, caliche-encrusted rocks, altered volcanic 5.1.14 Watch glass, 125 mm.
rocks (with calcareous inclusions), and many other calcium
6. Reagents and Materials
containing rocks.
6.1 Soluble Silica Sub-procedure:
4.2.3 Every percent of soluble calcium oxide that is contrib-
6.1.1 Hydrochloric Acid, reagent grade, density 1.19 Mg/
uted by soluble aggregate or mineral admixtures will bias the
m .
cement content high by approximately 1.6 %.
6.1.2 Hydrochloric Acid (1:3)—Mix 300 mL of hydrochlo-
4.2.4 Silica fume may lower the acid solubility of the
ric acid into 900 mL of water.
sample and hence bias the result low.
6.1.3 Hydrochloric Acid (1:9)—Mix 100 mL of hydrochlo-
4.3 Substances affecting the Soluble Silica Sub-procedure:
ric acid into 900 mL of water.
4.3.1 The following may be soluble depending on the age
6.1.4 Sodium Hydroxide (10 g/L)—Dissolve5gof reagent
and pH of the concrete; whether the aggregate is glassy or
grade sodium hydroxide in 200 mL of water and dilute to 500
crystalline, or weathered or strained; and the fineness of the
mL.
mineral: chert, opal, chalcedony, glassy volcanic rock, strained
6.1.5 Hydrofluoric Acid, 48 %, reagent grade.
quartz (highly strained), quartzite, cataclastic rocks (mylonite,
6.1.6 Sulfuric Acid, density 1.84 Mg/m , reagent grade.
phyllonite), gneiss, schist, metagraywacke, and many other
6.2 Calcium Oxide Sub-procedure—Use reagents as re-
soluble silicon containing rocks or minerals.
quired in Test Methods C 114.
4.3.2 Every percent of soluble SiO contributed by aggre-
6.3 Maleic Acid Procedure:
gates or mineral admixtures will bias the reported cement
6.3.1 Maleic acid, technical grade.
content high by approximately 4.7 %.
6.3.2 Methanol, technical grade, anhydrous.
4.3.3 Silica fume may lower the acid solubility of the
6.3.3 Maleic acid solution—prepare a fresh solution of
sample and hence bias the result low. If the digestion time or
15 % maleic acid in methanol by dissolving and diluting
temperature are sufficient to digest all of the portland cement,
180 + 1 g of maleic acid with methanol to a final solution
the silica fume will also be solubilized and bias the calculated
volume of 1200 millilitres. Prepare this solution fresh daily.
cement content high.
Care must be taken to use methanol only in well ventilated
4.4 Substances affecting the Maleic Acid Procedure:
areas, preferably under a hood, to avoid skin contact and
4.4.1 The same substances that are soluble in the soluble
breathing vapors. Disposal of the maleic acid/methanol solu-
calcium or the soluble silica subprocedures may be soluble in
tion shall be according to applicable regulations.
the maleic acid procedure. (See 4.2.1, 4.2.2 and 4.3.1.)
6.3.4 Fuller’s earth—a clay-like material consisting of a
4.4.2 Every 1 % of the sample that is aggregate or mineral
porous colloidal aluminum silicate. Its high adsorptivity has
admixture dissolved by the maleic acid will bias the cement
been found very beneficial for decolorizing and purifying
content high by 1 %.
materials.
4.4.3 Carbonated cement paste may not be soluble in the
6.4 Water—All references to water shall be understood to
maleic acid-methanol dissolution and thus may bias the cement
mean reagent water Types I through IV of Specification
content results low.
D 1193.
4.4.4 The unhydrated iron and aluminum phases of the
portland cement may not be soluble in the maleic acid and, if
7. Sampling
not soluble, will bias the cement content low. This may be
7.1 Choose the concrete sample in accordance with the
significant at early ages and less significant at later ages.
purposes of the investigation (Note 2).
5. Apparatus
NOTE 2—A standard procedure for sampling hardened concrete is given
5.1 Choose the apparatus from applicable items given in in Practice C 823 and a standard procedure for obtaining cores is given in
Test Method C 42.
Test Methods C 114 and from the following:
5.1.1 Chipmunk (jaw ore crusher).
7.2 Both the sample for cement content and for density shall
5.1.2 Disk Pulverizer.
have a minimum length and diameter of four times the nominal
5.1.3 Rotary Mill (rotating puck).
maximum size of the aggregate (Note 3).
5.1.4 Sieve, 300 um (No. 50), 1.18-mm (No. 16) and
NOTE 3—A single concrete core taken through the entire depth of the
4.75-mm (No. 4).
concrete is ordinarily an appropriate sample. This sample may be sawed
5.1.5 Ice Bath or electric cooling apparatus.
or split lengthwise to provide samples for cement content, density, and
5.1.6 Steam Bath.
petrographic examination, provided that the length and thickn ess of the
5.1.7 Funnel, Buchner-type porcelain funnel.
split samples for cement content and density meet the minimum size
5.1.8 Filter Paper, Type II, Class F and Class G as described specified in 7.2. If the split sample would not meet the minimum size
C 1084
requirement, perform the density measurement first, and then crush the
the residue, being careful that no residue is lost. Add 75 mL of
entire dry sample for cement content determination. The recommended
hot sodium hydroxide solution (10 g/L) to the residue while
mass of concrete for cement content determination is 4.5 kg (10 lb). This
stirring, macerate the filter paper, and digest, covered, on a
mass should be obtained from more than one core when the concrete depth
steam bath for 15 min. During the digestion, occasionally stir
is small and one core will not supply a mass of 4.5 kg (10 lb). If the
the mixture. Filter all solids, and wash twice with hot water
concrete sample did not have a mass of 4.5 kg (10 lb) it should be so stated
until the filtrate is neutral to litmus. Combine the filtrates.
in the final report for the cement content result.
8.1.4.4 The filtrate now contains the silica in the form of
7.3 Crush the sample for cement content determination to
silicic acid, either in true solution or in suspension in the
pass a 4.75-mm (No. 4) sieve, mix thoroughly, and obtain a
hydrochloric acid medium. To ensure analysis of only the
representative subsample for analysis by coning and quartering
soluble silicon, refilter any filtrate that is cloudy. (Allowing the
or by riffle splitting. The subsample should have a mass of 0.45
filtrate to stand overnight will usually permit suspended silica
kg (1 lb).
to settle.) The soluble silica may be analyzed by either of the
following procedures 8.1.4.4.1 or 8.1.4.4.2.
8. Cement Content Procedure
8.1.4.4.1 Analysis of soluble silica by conversion to silicon
8.1 Oxide Analysis Procedure:
tetrafluoride with hydrofluoric acid—In the case where the
8.1.1 Crush or grind the subsample prepared as described in
aggregate of the original sample contains substantial amounts
7.3 using a chipmunk (jaw ore crusher), a disk pulverizer, or a
of material that yields calcium oxide (CaO) on acid treatment,
rotary mill (rotating-puck) device, so that all of the material
add 10 mL of hydrochloric acid (density 1.19 Mg/m )tothe
passes a 300-μm (No. 50) sieve. To minimize production of
solution from 8.1.4.4. Transfer to a suitable beaker, with
very fine material, use several passes of the sample through the
several rinsings of the filter flask. Evaporate to dryness with
equipment, removing the portion passing the sieve before
great care to minimize spattering, bake at not over 120°C
regrinding the remainder of the sample. Thoroughly mix by
(248°F) for 1 h, moisten with hydrochloric acid (density 1.19
coning ten times from one paper to another.
Mg/m ), evaporate and bake again, and take up for filtration in
8.1.2 Dry the crushed or ground material in an oven at 105
75 mL of hydrochloric acid (1:3). Heat to boiling, filter through
to 115°C (220 to 240°F) for 3 h and retain the sample in a
an ashless filter paper, and wash the residue with 50 mL of hot
sealed container.
hydrochloric acid (1:9) and then with hot water until the
8.1.3 Sub-procedure to be used:
washings are free of chlorides. Determine the silica present in
8.1.3.1 The soluble silica sub-procedure shall be performed
the sample by treatment with hydrofluoric acid and sulfuric
in all cases except where a petrographic examination has
acid in accordance with the procedure given in Test Methods
indicated there are siliceous aggregates or mineral admixtures
C 114.
that will be soluble in cold hydrochloric acid.
8.1.4.4.2 Instrumental analysis of soluble silica—Transfer
8.1.3.2 The calcium oxide sub-procedure shall also be
the filtrate from 8.1.4.4 to a 500-mL volumetric flask with
employed unless the aggregate contains a significant amount of
several rinsings of the filtration flask and bring the volume in
calcareous components.
the volumetric flask to 500 mL with water. Analyze the soluble
8.1.4 Soluble Silica Sub-procedure:
silica by any instrumental method found acceptable for cement
...
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