Designation: C 25 – 06
Standard Test Methods for
Chemical Analysis of Limestone, Quicklime, and Hydrated
Lime1
This standard is issued under the fixed designation C 25; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
1.1 These test methods cover the chemical analysis of
high-calcium and dolomitic limestone, quicklime, and hy-
drated lime. These test methods are classified as either standard
(preferred) or alternative (optional).
1.2 The standard test methods are those that employ classi-
cal gravimetric or volumetric analytical procedures and are
typically those required for referee analyses where chemical
specification requirements are an essential part of contractual
agreement between buyer and seller.
1.3 Alternative or optional test methods are provided for
those who wish to use procedures shorter or more convenient
than the standard methods for the routine determinations of
certain constituents. Optional test methods may sometimes be
preferred to the standard test methods, but frequently the use of
modern and expensive instrumentation is indicated which may
not be accessible to everyone. Therefore, the use of these test
methods must be left to the discretion of each laboratory.
1.4 The analytical procedures appear in the following order:
Section
Aluminum Oxide 15
Available Lime Index 28
Calcium and Magnesium Oxide:
Alternative EDTA Titration Method 31
Calcium Carbonate Equivalent 33
Calcium Oxide:
Gravimetric Method 16
Volumetric Method 17
Carbon Dioxide by Standard Method 22
Combined Oxides of Iron and Aluminum 12
Ferrous Iron Appendix X5
Free Calcium Oxide Appendix X6
Free Moisture in Hydrated Lime 21
Free Moisture in Limestone 20
Free Silica 29
Insoluble Matter Including Silicon Dioxide:
Standard Method 8
Optional Perchloric Acid Method 9
Insoluble Matter Other Than Silicon Diox-
ide
11
Loss on Ignition 19
Magnesium Oxide 18
Manganese:
Bismuthate Method Appendix X4
Periodate (Photometric) Method 27
pH Determination of Alkaline Earth Solu-
tions
34
Phosphorus:
Titrimetric Method Appendix X3
Molybdovanadate Method 26
Silicon Dioxide 10
Strontium Oxide Appendix X2
Sulfur Trioxide 23
Total Carbon:
Direct Combustion-Thermal Conductiv-
ity Cell Method
32
Total Carbon and Sulfur:
Combustion/Infrared Detection Method 35
Total Iron:
Standard Method, Potassium Dichro-
mate Titration
13
Potassium Permanganate Titration
Method
Appendix X1
Ortho-Phenanthroline, Photometric
Method
14
Total Sulfur:
Sodium Carbonate Fusion 24
Combustion-Iodate Titration Method 25
Unhydrated Oxides 30
1.5 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
precautionary statements, see 9.3, 10.2.1, 18.4.3, 31.6.4.2,
X2.3.1, and X5.4.1.1.
2. Referenced Documents
2.1 ASTM Standards: 2
C 50 Practice for Sampling, Sample Preparation, Packag-
ing, and Marking of Lime and Limestone Products
C 51 Terminology Relating to Lime and Limestone (as used
by the Industry)
C 911 Specification for Quicklime, Hydrated Lime, and
Limestone for Chemical and Industrial Uses
1 These test methods are under the jurisdiction of ASTM Committee C07 on
Lime and are the direct responsibility of Subcommittee C07.05 on Chemical Tests.
Current edition approved Feb. 15, 2006. Published March 2006. Originally
approved in 1919. Last previous edition approved in 1999 as C 25–99.
2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D 1193 Specification for Reagent Water
E 29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
E 50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
Related Materials
E 70 Test Method for pH of Aqueous Solutions With the
Glass Electrode
E 173 Practice for Conducting Interlaboratory Studies of
Methods for Chemical Analysis of Metals 3
E 200 Practice for Preparation, Standardization, and Stor-
age of Standard and Reagent Solutions for Chemical
Analysis
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
E 832 Specification for Laboratory Filter Papers
3. Terminology
3.1 Definitions—Unless otherwise specified, for definitions
of terms used in these test methods refer to Terminology C 51.
4. Significance and Use
4.1 These test methods provide accurate and reliable ana-
lytical procedures to determine the chemical constituents of
limestone, quicklime, and hydrated lime (See Note 1). The
percentages of specific constituents which determine a materi-
al’s quality or fitness for use are of significance depending
upon the purpose or end use of the material. Results obtained
may be used in relation to specification requirements.
4.2 Because quicklime and hydrated lime quickly absorb
water and carbon dioxide from the air, precision and bias are
extremely dependent upon precautions taken during sample
preparation and analysis to minimize excessive exposure to
ambient conditions.
NOTE 1—These test methods can be applied to other calcareous
materials if provisions are made to compensate for known interferences.
5. General Apparatus and Materials and Reagents
5.1 General Apparatus and Materials:
5.1.1 Balance—The balance shall be of an analytical type
with a capacity not to exceed 200 g. It may be of conventional
design or it may be a constant-load, direct-reading type. It shall
be capable of reproducing weighings within 0.0002 g with an
accuracy of 6 0.0002 g. Rapid weighing devices that may be
provided such as a chain, damper, or heavy riders shall not
increase the basic inaccuracy by more than 0.0001 g at any
reading and with any load within the rated capacity of the
balance.
5.1.2 Weights—Weights used for analysis shall conform to
Class S-1 requirements of the National Institute of Standards
and Technology as described in NIST Circular 547.4 They shall
be checked at least once a year or when questioned, and
adjusted to within allowable tolerances for Class S-1 weights.
All new sets of weights purchased shall have the weights of 1
g and larger made of stainless steel or other corrosion-resistant
alloy not requiring protective coating and shall meet the
density requirements for Class S.
5.1.3 Glassware and Laboratory Containers—Standard
volumetric flasks, burets, pipets, dispensers, etc., shall be
carefully selected precision grade or better and shall be
calibrated, if necessary, to meet the requirements of each
operation. Standard-type interchangeable ground glass or TFE-
fluorocarbon joints are recommended for all volumetric glass-
ware. Polyethylene containers are recommended for all aque-
ous solutions of alkalies and for standard solutions where the
presence of dissolved silica or alkali from the glass would be
objectionable.
5.1.4 Desiccators—Desiccators shall be provided with a
good desiccant such as anhydrous magnesium perchlorate,
activated alumina, sulfuric acid, or phosphoric anhydride.
Anhydrous calcium sulfate may also be used provided it has
been treated with a color-changing indicator to show when the
desiccant has lost its effectiveness. Calcium chloride and silica
gel are not satisfactory desiccants for this type of analysis.
5.1.5 Filter Paper—Filter paper shall conform to the re-
quirements of Specification E 832, Type II (quantitative). Class
E shall be used for coarse and gelatinous precipitates. When
medium-textured paper is required, Class F filter paper shall be
used. When a retentive paper is needed, Class G shall be used.
Recommendations:
Class
Filter Pore Size
(microns)
Filter Speed
E 20 to 25 fast speed
F 8 medium speed
G 2.5 slow speed
5.1.6 Crucibles—Platinum crucibles and tight fitting lids
should preferably be made of pure unalloyed platinum and be
of 25 to 35-mL capacity. Where alloyed platinum is used for
greater stiffness or to obviate sticking of fused material to
crucible or lid, the alloyed platinum should not decrease in
weight by more than 0.2 mg when heated at 1200 °C for 1 h.
5.1.7 Muffle Furnace—The electric muffle furnace should
be capable of continuous operation up to 1000 °C and be
capable of intermittent operation at higher temperatures if
required. It should have an indicating pyrometer accurate to
6 25 °C.
5.2 Reagents:
5.2.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society5
where such specifications are available. Other grades may be
used provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination. In addition to this, it is desirable
in many cases for the analyst to ensure the accuracy of his
results by running blanks or checking against a comparable
sample of known composition.
3 Withdrawn.
4 Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
5 Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeia Convention, Inc. (USPC), Rockville,
MD.
C 25 – 06
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5.2.2 Purity of Water—Unless otherwise indicated, refer-
ences to water are understood to mean distilled water or other
water of equivalent purity. Water conforming to Specification
D 1193 meets these requirements.
5.2.3 Concentration of Reagents:
5.2.3.1 Concentrated Acids and Ammonium Hydroxide—
When acids and ammonium hydroxide are specified by name
or chemical formula only, it shall be understood that concen-
trated reagents approximating the following specific gravities
or concentrations are intended:
Acetic acid (HC2H3O2) 99.5 %
Hydrochloric acid (HCl) sp gr 1.19
Hydrofluoric acid (HF) 48 %
Nitric acid (HNO3) sp gr 1.42
Perchloric acid (HClO4) 70 %
Phosphoric acid (H3PO4) 85 %
Sulfuric acid (H2SO4) sp gr 1.84
Ammonium hydroxide (NH4OH) sp gr 0.90
5.2.3.2 Dilute Reagents—The concentration of dilute acids
and NH4OH except when standardized, are specified as a ratio
stating the number of measured volumes of the concentrated
reagent to be diluted with a given number of measured volumes
of water. In conformance with international practice, new and
revised methods will use the “plus” designation instead of the
ratio (:) symbol as the specified designation of dilution; for
example, H2SO4(5 + 95) means 5 volumes of concentrated
H2SO4(sp gr 1.84) diluted with 95 volumes of water.
5.2.3.3 Standard Solutions—Concentrations of standard so-
lutions shall be expressed as normalities (N) or as equivalents
in grams per millilitre of the component to be determined, for
example: 0.1 N K2Cr2O7 solution (1 mL = 0.004 g Fe2O3). The
average of at least three determinations shall be used for all
standardizations. The standardization used to determine the
strength of the standard solutions is described in the text under
each of the appropriate procedures.
6. General Procedures
6.1 Sampling—Samples of lime and limestone for chemical
analysis shall be taken and prepared in accordance with the
requirements of Practice C 50 applicable to the material to be
tested.
6.2 Tared or Weighed Crucibles—The tare weight of cru-
cibles shall be determined by preheating the empty crucible to
constant weight at the same temperature and under the same
conditions as shall be used for the final ignition of a residue and
cooling in a desiccator for the same period of time used for the
crucible containing the residue.
6.3 Constancy of Weight of Ignited Residue—To definitely
establish the constancy of weight of the ignited residue, the
residue and container shall be ignited at the specified tempera-
ture and time, cooled to room temperature in a desiccator, and
weighed. The residue and container shall then be reheated for
at least 30 min at the same temperature, cooled in a desiccator
for the same period of time, and reweighed. Additional ignition
periods may be required until two consecutive weights do not
differ by more than 0.2 mg, at which time it shall be considered
that constant weight has been attained. For ignition loss, each
reheating period shall be 5 min.
6.4 Calculation:
6.4.1 The calculations included in the individual procedures
sometimes assume that the exact weight specified has been
used. Accurately weighed samples which are approximately
but not exactly equal to the weight specified may be used
provided appropriate corrections are made in the calculation.
Unless otherwise stated, weights of all samples and residues
should be recorded to the nearest 0.0001 g.
6.4.2 In all mathematical operations on a set of observed
values, the equivalent of two more places of figures than in the
single observed values shall be retained. For example, if
observed values are read or determined to the nearest 0.1 mg,
carry numbers to the nearest 0.001 mg in calculation.
6.5 Rounding Figures—Rounding figures to the nearest
significant place required in the report should be done after the
calculations are completed, in order to keep the final results
free from calculation errors. The rounding procedure should
follow the principle outlined in Practice E 29.
7. Performance Requirements for Test Methods
7.1 Referee Analyses—The reference test methods that ap-
pear in Sections 8 through 32, or any other test methods
qualified in accordance with 7.3, are required for referee
analysis in those cases where conformance to the requirements
of a chemical specification are questioned. In these cases a
limestone, quicklime, or hydrated lime shall not be rejected for
failure to conform to chemical requirements unless all sample
preparation and analysis of any one constituent is made entirely
by reference test methods prescribed in the appropriate sections
of this test method or by other qualified test methods. Excep-
tion can be made when specific test methods are prescribed in
the standard specification for the limestone, quicklime, or
hydrated lime in question. The test methods actually used for
the analysis shall be designated.
7.1.1 When there is a question regarding acceptance, referee
analyses shall be made in duplicate. If the two results do not
agree within the permissible variation given in Table 1, the
determination including sample preparation shall be repeated
TABLE 1 Maximum Permissible Variations in ResultsA
(Column 1)
Constituent
(Column 2)
Maximum Difference
Between Duplicates
(Column 3)
Maximum Difference of
the Average of Duplicates
from SRM Certificate
ValuesB
Al as Al2O3 0.20 6 0.30
Ca as CaO 0.20 6 0.30
Mg as MgO 0.20 6 0.30
C (lime and hydrated lime) 0.20 6 0.30
C (limestone) 0.60 6 0.60
Fe as Fe2O3 0.10 6 0.15
Si as SiO2 0.15 6 0.30
Mn 0.05 6 0.10
P 0.02 6 0.05
Sr as SrO 0.05 C
S 0.03 6 0.05
A For demonstrating the performance of rapid test methods the SRM closest in
overall composition to the limestone shall be used (See Table 2). In the case of
quicklime or hydrated lime, the SRM closest in overall composition, after heating
at 1000 °C for 1 h, to the product composition shall be used, except for C and S
determinations (See Note 3).
B Interelement corrections may be used for any standardization provided
improved accuracy can be demonstrated.
C No SRM currently available.
C 25 – 06
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in duplicate until the results agree within the permissible
variation. When the results agree within the permissible
variation, their average shall be accepted as the correct value.
For the purpose of comparing results, the percentages shall be
calculated to one more significant figure than reported as
indicated in the test methods. When a blank determination is
specified, one shall be made with each individual analysis or
with each group of two or more samples analyzed on the same
day for a given constituent.
7.1.2 Test results from Referee methods intended for use as
a basis for product acceptance or rejection, or for manufactur-
er’s certification, can be used only after demonstration of
precise and accurate analyses by meeting the requirements of
7.1.3, or except when demonstrated under 7.3.2.1. Such dem-
onstrations may be made concurrently with analysis of the
limestone, quicklime, or hydrated lime product being tested.
The demonstration is required only for those constituents being
used as a basis for acceptance, rejection, or certification of a
limestone, quicklime, or hydrated lime, but may be made for
any constituent of limestone, quicklime, or hydrated lime
product for which a standard exists. Such demonstrations must
be made annually.
7.1.3 Demonstrations shall be made by analysis of each
constituent of concern in a SRM limestone, quicklime, or
hydrated lime (See Notes 2 and 3). Duplicate samples shall be
run on different days. The same test methods to be used for
analysis of the limestone, quicklime, or hydrated lime being
tested shall be used for analysis of the SRM. If the duplicate
results do not agree within the permissible variation given in
Table 1, the determinations shall be repeated, following iden-
tification and correction of problems or errors, until a set of
duplicate results do agree within the permissible variation.
NOTE 2—The term SRM refers to approved Standard Reference Mate-
rials listed in Table 2.
NOTE 3—There are no SRMs that are quicklime or hydrated lime as
supplied. When analyzing a quicklime or hydrated lime the SRM in
carbonate form needs to be converted to closely resemble the matrix of the
product being tested. To accomplish this conversion, heat the chosen SRM
for 1 h at 1000 °C, immediately prior to analysis and protect it from
hydration or carbonation with sealed containers and desiccation during
cooling. Carbon and sulfur may be driven off during heating, rendering the
converted SRM unsuitable as a standard for carbon and sulfur determi-
nations. For carbon and sulfur determinations use the appropriate SRM in
its normal matrix.
7.1.4 The average of the results of acceptable duplicate
determinations for each constituent may differ from the SRM
certificate value by no more than the value shown in Column
3 of Table 1. When no SRM certificate value is given, a
generally accepted accuracy standard for that constituent has
not been identified. In such cases, only the differences between
duplicate values as specified in 7.1.3 sh