Standard Test Method for Insoluble Residue in Carbonate Aggregates

SCOPE
1.1 This test method covers determination of the percentage of insoluble residue in carbonate aggregates using hydrochloric acid solution to react the carbonates.  
1.2 The values stated in inch-pound 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. Specific precaution statements are given in Section 7.

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Publication Date
09-Jul-1997
Drafting Committee
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ASTM D3042-97 - Standard Test Method for Insoluble Residue in Carbonate Aggregates
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3042 – 97
Standard Test Method for
Insoluble Residue in Carbonate Aggregates
This standard is issued under the fixed designation D 3042; 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 4. Apparatus
1.1 This test method covers determination of the percentage 4.1 Sieves, U.S. standard 8-in. (203.2-mm) diameter, con-
of insoluble residue in carbonate aggregates using hydrochloric forming to Specification E 11 in the following sizes:
acid solution to react the carbonates.
⁄8-in. (9.5-mm)
No. 4 (4.75-mm)
1.2 The values stated in inch-pound units are to be regarded
No. 8 (2.36-mm)
as standard.
No. 16 (1.18-mm)
1.3 This standard does not purport to address all of the
No. 30 (600-μm)
No. 50 (300-μm)
safety concerns, if any, associated with its use. It is the
No. 100 (150-μm)
responsibility of the user of this standard to establish appro-
No. 200 (75-μm)
priate safety and health practices and determine the applica-
4.2 Balance — A balance having a minimum capacity of 15
bility of regulatory limitations prior to use. Specific precaution
kg and meeting the requirements of Specification D 4753,Class
statements are given in Section 7.
GP5.
2. Referenced Documents 4.3 Oven, of appropriate size capable of being maintained at
230 6 9°F (110 6 5°C).
2.1 ASTM Standards:
4.4 Agitation Equipment, such as a jar mill or a magnetic
C 136 Test Method for Sieve Analysis of Fine and Coarse
stirrer.
Aggregates
4.5 Bunsen Burner or Hot Plate.
C 294 Descriptive Nomenclature for Constituents of Natu-
4.6 Receiving Tank, of nonreactive material to receive wash
ral Mineral Aggregates
water and residue washed through the 8-in. (203.2-mm)
C 670 Practice for Preparing Precision and Bias Statements
2 diameter sieves.
for Test Methods of Construction Materials
4.7 Rapid Filter Paper, acid-resistant.
D 4753 Specification for Evaluating, Selecting, and Speci-
4.8 Safety Eyeglasses, Rubber Gloves, Aprons, etc.
fying Balances and Scales for Use in Testing Soil, Rock,
4.9 Borosilicate Glass Containers, for performing acid
and Related Construction Materials
leaching test.
E 11 Specification for Wire-Cloth and Sieves for Testing
4.10 pH Paper.
Purposes
5. Reagent
3. Significance and Use
5.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 The amount and size distribution of noncarbonate (in-
used in all tests. Unless otherwise indicated, it is intended that
soluble) material in carbonate aggregates is of interest to those
all reagents shall conform to the specifications of the Commit-
conducting research on the polish susceptibility of stone used
tee on Analytical Reagents of the American Chemical Society,
in pavements or on the friction properties of pavement sur-
where such specifications are available. Other grades may be
faces. In addition, some agencies utilize the test for acceptance
used, provided it is first ascertained that the reagent is of
purposes to delineate carbonate aggregates that may polish
sufficiently high purity to permit its use without lessening the
excessively and become slippery and those that will not.
accuracy of the determination.
5.2 Hydrochloric Acid (6 N)—Prepare a 6 N solution of
hydrochloric acid (HCl).
This test method is under the jurisdiction of ASTM Committee D-4 on Road
and Paving Materials and is the direct responsibility of Subcommittee D04.51 on
Aggregate Tests.
Current edition approved July 10, 1997. Published February 1998. Originally “Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
published as D 3042 – 72. Last previous edition D 3042 – 95. cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Annual Book of ASTM Standards, Vol 04.02. the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Annual Book of ASTM Standards, Vol 04.08. Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
Annual Book of ASTM Standards, Vol 14.02. Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D3042–97
6. Samples 7.7.1 If no reaction is observed upon heating, proceed with
the remainder of the test procedure.
6.1 Samples shall be representative of the sources from
7.7.2 If a reaction is observed upon heating, continue the
which they are obtained and shall be reduced to appropriate
agitation and repeat the procedure beginning at 7.7.
size by use of sample splitters or by quartering in accordance
with the Sampling Section of Test Method C 136.
7.8 When the reaction has stopped, decant the acid solution
6.1.1 Normally, the aggregate used in the test sample shall and add water to the aggregate in the glass container to
be retained after washing over the No. 4 (4.75-mm) sieve, and
thoroughly dilute the acid. The residue in the container should
passing the ⁄8-in. (9.5-mm sieve). have a pH as indicated by pH paper of more than 5.5.
6.1.2 Separate fractions or combined aggregate gradations
7.9 Wash the diluted solution and residue from the aggre-
may be tested as appropriate.
gate sample over a preweighed No. 200 sieve placed over a
6.2 Sample aggregates shall be dried to constant mass at 230
receiving tank.
6 9°F (110 6 5°C).
7.10 Thoroughly rinse the material on the No. 200 (75-μm)
6.3 An oven-dry sample weighing a minimum of 500 g shall
sieve and into the receiving tank. Dry the sieve and the residue
be used for the test.
in a 2306 9°F (110° 6 5°C) oven.
7.11 When the sieve and residue have cooled to room
7. Procedure for Determining Only the Plus No. 200 Size
temperature, weigh the sieve plus the residue and subtract the
Fraction of Insoluble Residue
original mass of the dry clean sieve to obtain the mass of the
7.1 For many applications, only the plus No. 200 (75-μm)
plus No. 200 (75-μm) sieve size residue.
size insoluble residue fraction is of interest. This section
7.12 Visually inspect the residue to determine whether or
provides a procedure for determination of the amount and size
not particle agglomeration because of the presence of plastic
distribution of only the plus No. 200 (75-μm) size insoluble
clay fractions has occurred.
residue. If the total amount of insoluble residue is desired, the
7.12.1 If agglomeration has occurred, physical reduction of
procedure given in Section 8 should be followed and the
the agglomerated particles should be performed by use of a
remainder of this section should be omitted.
mortar and rubber-tipped pestle. Care should be exercised to
7.2 Prepare and test samples in triplicate for each aggregate
prevent crushing of individual particle grains during this
sampled.
process.
7.3 Warning—Hydrogen chloride gas is released during
7.12.2 If no agglomeration has occurred, proceed with the
this procedure. Operators shall be required to wear a mask and
remainder of the test procedure.
should perform this test using the procedures set forth in 7.4.
7.13 Dry sieve the residue from the aggregate sample over
7.4 Place an aggregate sample weighing a minimum of 500
preweighed nested sieves. The nested sieves shall be of the
g in a suitable borosilicate glass container. The container shall
following series:
be vented to allow gas from the reaction to escape and to be
No. 4 (4.75-mm)
drawn away. Exercise extreme care to prevent corrosive gas
No. 8 (2.36-mm)
from entering the laboratory atmosphere. The hydrogen chlo-
No. 16 (1.18-mm)
ride gas that may be produced in the chemical reaction can be
No. 30 (600-μm)
No. 50 (300-μm)
destructive to laboratory equipment and can also be a definite
No. 100 (150-μm)
safety hazard to laboratory personnel. Under no circumstances
No. 200 (75-μm)
shall the test be performed without proper and adequate
ventilation. Slowly add 1000 mL of 6 N hydrochloric acid
8. Procedure for Determining the Total Acid Insoluble
(HCl) allowing for excessive effervescence or foaming to
Residue Content
subside before further addition of solution. Agitate the con-
8.1 Perform the steps in 7.1 through 7.8.
tainer and contents gently by hand until excessive efferves-
8.2 Wash the diluted solution and residue from the aggre-
cence has subsided.
gate sample over pre-weighed nested sieve
...

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