ASTM C1301-95

Standard Test Method for Major and Trace Elements in Limestone and Lime by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP) and Atomic Absorption (AA)

SCOPE
1.1 The following test method covers the use of inductively coupled plasma-atomic emission spectroscopy (ICP) and atomic absorption spectroscopy (AA) in the analysis of major and trace elements in limestone and lime (calcined limestone).  
1.2 Table 1 lists some of the elements that can be analyzed by this test method and the preferred wavelengths. Also see U.S. EPA Method 200.7 and 200.9.  
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: 31-Dec-2000
• Technical Committee: C07 - Lime and Limestone
• Drafting Committee: C07.05 - Chemical Tests

Relations

• Replaced By: ASTM C1301-95(2001) - Standard Test Method for Major and Trace Elements in Limestone and Lime by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP) and Atomic Absorption (AA)
• Effective Date: 01-Jan-2001
• Referred By: ASTM C821-22 - Standard Specification for Lime for Use with Pozzolans
• Effective Date: 01-Jan-2001
• Referred By: ASTM C1164-22 - Standard Practice for Evaluation of Limestone or Lime Uniformity From a Single Source
• Effective Date: 01-Jan-2001
• Referred By: ASTM C737-22 - Standard Specification for Limestone for Dusting of Coal Mines
• Effective Date: 01-Jan-2001
• Referred By: ASTM C1097-19 - Standard Specification for Hydrated Lime for Use in Asphalt Cement or Bituminous Paving Mixtures
• Effective Date: 01-Jan-2001
• Referred By: ASTM C50/C50M-13(2019) - Standard Practice for Sampling, Sample Preparation, Packaging, and Marking of Lime and Limestone Products
• Effective Date: 01-Jan-2001
• Referred By: ASTM C1489-15(2022) - Standard Specification for Lime Putty for Structural Purposes
• Effective Date: 01-Jan-2001
• Referred By: ASTM C706-19 - Standard Specification for Limestone for Animal Feed Use
• Effective Date: 01-Jan-2001
• Referred By: ASTM C1318-15a(2020) - Standard Test Method for Determination of Total Neutralizing Capability and Dissolved Calcium and Magnesium Oxide in Lime for Flue Gas Desulfurization (FGD)
• Effective Date: 01-Jan-2001
• Referred By: ASTM C602-20 - Standard Specification for Agricultural Liming Materials
• Effective Date: 01-Jan-2001
• Referred By: ASTM C206-14(2022) - Standard Specification for Finishing Hydrated Lime
• Effective Date: 01-Jan-2001
• Referred By: ASTM C141/C141M-14(2022) - Standard Specification for Hydrated Hydraulic Lime for Structural Purposes
• Effective Date: 01-Jan-2001

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 1301 – 95
Standard Test Method for
Major and Trace Elements in Limestone and Lime by
Inductively Coupled Plasma-Atomic Emission Spectroscopy
(ICP) and Atomic Absorption (AA)
This standard is issued under the fixed designation C 1301; 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.
A
TABLE 1 Elements and Some Suggested Wavelengths
1. Scope
Major Elements ICP Wavelength, nm AA Wavelength, nm
1.1 The following test method covers the use of inductively
B
Calcium 317.933 (315.887) 422.7
coupled plasma-atomic emission spectroscopy (ICP) and
Magnesium 279.079 (285.213) 285.2
atomic absorption spectroscopy (AA) in the analysis of major
Silicon 251.611 (288.160) 251.6
and trace elements in limestone and lime (calcined limestone).
Aluminum 308.215 (309.271) 309.3
Iron 259.940 248.3
1.2 Table 1 lists some of the elements that can be analyzed
Manganese 257.610 279.5
by this test method and the preferred wavelengths. Also see
Sodium 588.995 (589.59) 589.0
U.S. EPA Method 200.7 and 200.9.
Potassium 766.491 766.5
C
Phosphorus 214.914 (213.618) .
1.3 This standard does not purport to address all of the
Strontium 421.552 460.7
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
Trace Elements ICP Wavelength, nm AA Wavelength, nm
priate safety and health practices and determine the applica-
Antimony 206.833 217.6
bility of regulatory limitations prior to use.
Arsenic 193.696 193.7
Barium 455.403 (493.409) 553.6
2. Referenced Documents
Beryllium 313.042 234.9
Boron 249.773 249.8
2.1 ASTM Standards:
Cadmium 226.502 (228.80) 228.8
C 51 Terminology Relating to Lime and Limestone (As
Chromium 267.716 (205.552) 357.9
Cobalt 228.616 240.7 (242.5)
Used by the Industry)
Copper 324.754 324.8
D 1193 Specification for Reagent Water
Lead 220.353 217.0 (283.3)
E 135 Terminology Relating to Analytical Chemistry for
Molybdenum 202.030 (203.844) 313.3
Nickel 231.604 (221.647) 232.0
Metals, Ores, and Related Materials
Selenium 196.090 196.0
E 863 Practice for Describing Flame Atomic Absorption
Silver 328.068 328.1
C
Spectroscopy Equipment
Sulfur 180.731 (180.669) .
Thallium 190.864 276.8
E 1479 Practice for Describing and Specifying Inductively-
Tin 189.989 235.5 (286.3)
Coupled Plasma Optical Emission Spectrometers
Vanadium 292.402 318.4
2.2 U.S. EPA Standards: Zinc 213.856 (202.551) 213.9
A
Methods for the Determination of Metals in Environmental
The suggested wavelengths may vary for your particular instrument.
B
Numbers in parentheses are alternate wavelengths.
Samples; U.S. EPA Methods 200.2, 200.7 and 200.9;
C
6 Not recommended or not used.
Smoley, C. K., 1992
Method 6010, Inductively Coupled Plasma Method, SW-
846, Test Methods for Evaluating Solid Waste
method can be found in Terminologies C 51 and E 135.
3. Terminology
3.2 Additional Definitions:
3.2.1 total recoverable, n—trace element concentration in
3.1 Definitions—Definitions for terms used in this test
an unfiltered sample after heating in acid.
3.2.2 total digestion, n—complete digestion of a sample,
This test method is under the jurisdiction of ASTM Committee C-7 on Lime
and is the direct responsibility of Subcommittee C07.05 on Chemical Tests.
including silica and silicate minerals, using the fusion-flux
Current edition approved Aug. 15, 1995. Published October 1995.
method.
Annual Book of ASTM Standards, Vol 04.01.
Annual Book of ASTM Standards, Vol 11.01.
4. Summary of Test Method
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06.
4.1 A sample, digested by either fusion or acid, is atomized
Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL
and passed into an excitation medium (a plasma in the case of
33431.
7 ICP; a flame in the case of AA). The resulting ions are analyzed
Available from U.S. Government Printing Office, Washington, DC 20402.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
C 1301
by atomic spectroscopy. Elemental concentrations are deter- 8. Reagents
mined by graphically relating the emission/absorption at spe-
8.1 Purity of Reagents—Reagents should conform to the
cific wavelengths for an unknown sample to analytical curves
specifications of the Committee on Analytical Reagents of the
made from reference standards of known composition.
American Chemical Society as a minimum when such speci-
fications are available. The high sensitivity of both the ICP
5. Significance and Use
and AA may require reagents of high purity. It is recommended
5.1 The presence and concentration of elements in lime and
that the reagents be of sufficiently high purity so as not to
limestone is important in determining product quality and its
lessen the accuracy of the determination.
suitability for various uses. This test method provides a means
8.2 Purity of Water—At minimum, water should conform to
of measuring the major and trace element concentration in lime
Type II of Specification D 1193.
and limestone.
8.3 Stock Solutions—Standard stock solutions may be pur-
chased or prepared from high purity metals or metal salts
6. Interferences
(Method 6010, SW-846; EPA Method 200.7 and 200.9). Salts
6.1 Chemical—Chemical interferences, most common in
should be dried at 105°C for 1 h, unless otherwise specified.
AA, arise from the formation of molecular compounds that
8.4 Multielement Calibration Standards—ICP calibration is
cause absorbances at the wavelength of interest. This molecu-
most often performed using multielement calibration standards
lar band spectral overlap can be minimized by buffering the
prepared from single element stock solutions. Prior to prepar-
sample with matrix modifiers (a Lanthanum additive, for
ing the mixed standards, each stock solution should be ana-
example), using standard additions techniques, matrix match-
lyzed separately to determine possible spectral interference or
ing or by careful selection of operating conditions (for ex-
the presence of impurities. Standards are combined in such a
ample, using a hotter nitrous oxide/acetylene flame, selecting
way that they are chemically compatible (no precipitation
an alternate wavelength).
occurs) and do not cause spectral interferences. An example of
6.2 Physical—Physical interferences are the result of the
multielement combinations is given in EPA Method 200.7.
inconsistancies in the introduction of the sample into the
8.5 Interference Check Sample—Interference check
instrument, namely the transport and atomization/nebulization
samples are made from single element stock solutions at a
of the sample. These inconsistancies are a function of changing
concentration level equal to that of the samples to be analyzed.
viscosity and surface tension, and are found primarily in
8.6 Calibration Blank—A calibration blank is prepared at
samples of high-dissolved solids or high-acid concentrations.
the same acid strength as that of the samples to be analyzed;
Physical interferences can be reduced by diluting the sample
usually 5 or 10 %. To prepare a 10 % nitric acid calibration
and by the use of a peristaltic pump.
blank, add one volume of nitric acid to nine volumes of water.
6.3 Spectral—Spectral interference, most common in ICP,
This same blank can be used as the rinse solution for flushing
consists of overlapping and unresolved peaks. Computer soft-
the system between standards and samples.
ware, along with the analysis of the suspected interfering
8.7 Reagent Blank—The reagent blank contains all the
element, can compensate for this effect. Using an alternate
reagents in the same concentrations (including nitric acid) as
wavelength is also a solution. Another spectral interference is
the samples to be analyzed. The reagent blank is carried
caused by background, both stray light and continuous spec-
through the same processes as a sample for analysis.
trum (continuous argon spectrum, for example). Background
8.8 Nitric Acid—High purity nitric acid is recommended.
correction adjacent to the analyte line will correct background
8.9 Lithium Tetraborate (Li2B4O7) Powder or Lithium
spectral interference.
Metaborate (LiBO2)) Powder.
8.10 Non-Wetting Agent—Saturated solution of Hydrogen
7. Apparatus
Bromide (HBr), Potassium Bromide (KBr) or Potassium Iodide
7.1 Spectrometer.
(KI) as a non-wetting agent to prevent the flux from sticking to
7.1.1 Inductively Coupled Plasma Emission Spectrometer
the crucible.
(ICP)—Either a scanning sequential or multielement simulta-
8.11 Lanthanum Chloride (LaCl3) Powder—Lanthanum is
neous type ICP, with resolution appropriate for the elements to
added to samples for AA analysis as a releasing agent (for
be analyzed. The optical path may
...