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)

SIGNIFICANCE AND USE
The presence and concentration of elements in lime and limestone is important in determining product quality and its suitability for various uses. This test method provides a means of measuring the major and trace element concentration in lime and limestone.
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
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C07 - Lime and Limestone
• Drafting Committee: C07.05 - Chemical Tests

Relations

• Replaces: 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)
• Effective Date: 01-Jan-2001
• Replaced By: ASTM C1301-95(2009)e1 - 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-Jun-2009
• 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
• Referred By: ASTM C821-22 - Standard Specification for Lime for Use with Pozzolans
• Effective Date: 01-Jan-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C1301–95 (Reapproved 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)
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 (´) 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
C51 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 Atomic Absorption Spectro-
Silver 328.068 328.1
C
metric 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 Atomic 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
5 Not recommended or not used.
Smoley, C. K., 1992
Method 6010, Inductively Coupled Plasma Method, SW-
846, Test Methods for Evaluating Solid Waste
1 3. Terminology
This test method is under the jurisdiction of ASTM Committee C07 on Lime
and is the direct responsibility of Subcommittee C07.05 on Chemical Tests
3.1 Definitions—Definitions for terms used in this test
Current edition approved May 10, 2001. Published October 1995.
method can be found in TerminologiesC51 and E 135.
Annual Book of ASTM Standards, Vol 04.01.
3.2 Additional Definitions:
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 03.05.
Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL
33431. Available from U.S. Government Printing Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1301–95 (2001)
3.2.1 total recoverable, n—trace element concentration in 7.1.2 Atomic Absorption Spectrometer (AA)—An atomic
an unfiltered sample after heating in acid. absorption spectrometer consisting of single or double beam
3.2.2 total digestion, n—complete digestion of a sample, optics, a monochromator, photomultiplier detector, adjustable
including silica and silicate minerals, using the fusion-flux slits, a wavelength range from 190 to 800 nm, and provisions
method. for interfacing with either a strip chart recorder or a computer.
A simultaneous background correction system is also recom-
4. Summary of Test Method mended. A detailed description of an AA is given in Practice
E 863.
4.1 Asample, digested by either fusion or acid, is atomized
7.1.2.1 Hollow Cathode Lamps—Single hollow cathode
and passed into an excitation medium (a plasma in the case of
lamps, one for each element. Multi-element hollow cathode
ICP;aflameinthecaseofAA).Theresultingionsareanalyzed
lamps can be used but spectral interferences are possible.
by atomic spectroscopy. Elemental concentrations are deter-
mined by graphically relating the emission/absorption at spe-
8. Reagents
cific wavelengths for an unknown sample to analytical curves
made from reference standards of known composition.
8.1 Purity of Reagents—Reagents should conform to the
specifications of the Committee on Analytical Reagents of the
5. Significance and Use
American Chemical Society as a minimum when such speci-
fications are available. The high sensitivity of both the ICP
5.1 The presence and concentration of elements in lime and
andAAmay require reagents of high purity. It is recommended
limestone is important in determining product quality and its
that the reagents be of sufficiently high purity so as not to
suitability for various uses. This test method provides a means
lessen the accuracy of the determination.
ofmeasuringthemajorandtraceelementconcentrationinlime
8.2 Purity of Water—At minimum, water should conform to
and limestone.
Type II of Specification D 1193.
8.3 Stock Solutions—Standard stock solutions may be pur-
6. Interferences
chased or prepared from high purity metals or metal salts
6.1 Chemical—Chemical interferences, most common in
(Method 6010, SW-846; EPA Method 200.7 and 200.9). Salts
AA, arise from the formation of molecular compounds that
should be dried at 105°C for 1 h, unless otherwise specified.
cause absorbances at the wavelength of interest. This molecu-
8.4 Multi-element Calibration Standards—ICP calibration
lar band spectral overlap can be minimized by buffering the
is most often performed using multi-element calibration stan-
sample with matrix modifiers (a Lanthanum additive, for
dards prepared from single element stock solutions. Prior to
example), using standard additions techniques, matrix match-
preparing the mixed standards, each stock solution should be
ing or by careful selection of operating conditions (for ex-
analyzed separately to determine possible spectral interference
ample, using a hotter nitrous oxide/acetylene flame, selecting
or the presence of impurities. Standards are combined in such
an alternate wavelength).
a way that they are chemically compatible (no precipitation
6.2 Physical—Physical interferences are the result of the
occurs) and do not cause spectral interferences.An example of
inconsistencies in the introduction of the sample into the
multi-element combinations is given in EPA Method 200.7.
instrument, namely the transport and atomization/nebulization
8.5 Interference Check Sample—Interference check
ofthesample.Theseinconsistenciesareafunctionofchanging
samples are made from single element stock solutions at a
viscosity and surface tension, and are found primarily in
concentration level equal to that of the samples to be analyzed.
samples of high-dissolved solids or high-acid concentrations.
8.6 Calibration Blank—A calibration blank is prepared at
Physical interferences can be reduced by diluting the sample
the same acid strength as that of the samples to be analyzed;
and by the use of a peristaltic pump.
usually 5 or 10 %. To prepare a 10 % nitric acid calibration
6.3 Spectral—Spectral interference, most common in ICP,
blank, add one volume of nitric acid to nine volumes of water.
consists of overlapping and unresolved peaks. Computer soft-
This same blank can be used as the rinse solution for flushing
ware, along with the analysis of the suspected interfering
the system between standards and samples.
element, can compensate for this effect. Using an alternate
8.7 Reagent Blank—The reagent blank contains all the
wavelength is also a solution. Another spectral interference is
reagents in the same concentrations (including nitric acid) as
caused by background, both stray light and continuous spec-
the samples to be analyzed. The reagent blank is carried
trum (continuous argon spectrum, for example). Background
through the same processes as a sample for analysis.
correction adjacent to the analyte line will correct background
8.8 Nitric Acid—High purity nitric acid is recommended.
spectral interference.
8.9 Lithium Tetr
...