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)

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 Methods 200.7 and 200.9.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.
TABLE 1 Elements and Some Suggested WavelengthsA  Major ElementsICP Wavelength, nmAA Wavelength, nm Calcium317.933 (315.887)B422.7 Magnesium279.079 (285.213)285.2 Silicon251.611 (288.160)251.6 Aluminum308.215 (309.271)309.3 Iron259.940248.3 Manganese257.610279.5 Sodium588.995 (589.59)589.0 Potassium766.491766.5 Phosphorus214.914 (213.618)...C Strontium421.552460.7  Trace ElementsICP Wavelength, nmAA Wavelength, nm  Antimony206.833217.6 Arsenic193.696193.7 Barium455.403 (493.409)553.6 Beryllium313.042234.9 Boron249.773249.8 Cadmium226.502 (228.80)228.8 Chromium267.716 (205.552)357.9 Cobalt228.616240.7 (242.5) Copper324.754324.8 Lead220.353217.0 (283.3) Molybdenum202.030 (203.844)313.3 Nickel231.604 (221.647)232.0 Selenium196.090196.0 Silver328.068328.1 Sulfur180.731 (180.669)...C Thallium190.864276.8 Tin189.989235.5 (286.3) Vanadium292.402318.4 Zinc213.856 (202.551)213.9
A The suggested wavelengths may vary for your particular instrument.
B Numbers in parentheses are alternate wavelengths.
C Not recommended or not used.

General Information

• Status: Historical
• Publication Date: 31-May-2009
• 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(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-Jun-2009
• 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-Jun-2009
• Referred By: ASTM C1164-22 - Standard Practice for Evaluation of Limestone or Lime Uniformity From a Single Source
• Effective Date: 01-Jun-2009
• Referred By: ASTM C821-22 - Standard Specification for Lime for Use with Pozzolans
• Effective Date: 01-Jun-2009
• Referred By: ASTM C141/C141M-14(2022) - Standard Specification for Hydrated Hydraulic Lime for Structural Purposes
• Effective Date: 01-Jun-2009
• Referred By: ASTM C706-19 - Standard Specification for Limestone for Animal Feed Use
• Effective Date: 01-Jun-2009
• Referred By: ASTM C1489-15(2022) - Standard Specification for Lime Putty for Structural Purposes
• Effective Date: 01-Jun-2009
• Referred By: ASTM C1097-19 - Standard Specification for Hydrated Lime for Use in Asphalt Cement or Bituminous Paving Mixtures
• Effective Date: 01-Jun-2009
• Referred By: ASTM C602-20 - Standard Specification for Agricultural Liming Materials
• Effective Date: 01-Jun-2009
• Referred By: ASTM C50/C50M-13(2019) - Standard Practice for Sampling, Sample Preparation, Packaging, and Marking of Lime and Limestone Products
• Effective Date: 01-Jun-2009
• Referred By: ASTM C206-14(2022) - Standard Specification for Finishing Hydrated Lime
• Effective Date: 01-Jun-2009
• Referred By: ASTM C737-22 - Standard Specification for Limestone for Dusting of Coal Mines
• Effective Date: 01-Jun-2009

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
´1
Designation: C1301 − 95(Reapproved 2009)
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 C1301; 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.
´ NOTE—A units statement was added editorially as new paragraph 1.3 and subsequent paragraphs were renumbered in
June 2009.
1. Scope Coupled Plasma Atomic Emission Spectrometers
2.2 U.S. EPA Standards:
1.1 The following test method covers the use of inductively
Methods for the Determination of Metals in Environmental
coupled plasma-atomic emission spectroscopy (ICP) and
Samples; U.S. EPA Methods 200.2, 200.7, and
atomic absorption spectroscopy (AA) in the analysis of major
200.9; Smoley, C. K., 1992
and trace elements in limestone and lime (calcined limestone).
Method 6010, Inductively Coupled Plasma Method, SW-
1.2 Table 1 lists some of the elements that can be analyzed
846, Test Methods for Evaluating Solid Waste
by this test method and the preferred wavelengths. Also see
U.S. EPA Methods 200.7 and 200.9.
3. Terminology
1.3 The values stated in SI units are to be regarded as
3.1 Definitions—Definitions for terms used in this test
standard. No other units of measurement are included in this
method can be found in Terminologies C51 and E135.
standard.
3.2 Additional Definitions:
1.4 This standard does not purport to address all of the
3.2.1 total recoverable, n—trace element concentration in
safety concerns, if any, associated with its use. It is the
an unfiltered sample after heating in acid.
responsibility of the user of this standard to establish appro-
3.2.2 total digestion, n—complete digestion of a sample,
priate safety and health practices and determine the applica-
including silica and silicate minerals, using the fusion-flux
bility of regulatory limitations prior to use.
method.
2. Referenced Documents
4. Summary of Test Method
2.1 ASTM Standards:
4.1 Asample, digested by either fusion or acid, is atomized
C51 Terminology Relating to Lime and Limestone (as used
and passed into an excitation medium (a plasma in the case of
by the Industry)
ICP;aflameinthecaseofAA).Theresultingionsareanalyzed
D1193 Specification for Reagent Water
by atomic spectroscopy. Elemental concentrations are deter-
E135 Terminology Relating to Analytical Chemistry for
mined by graphically relating the emission/absorption at spe-
Metals, Ores, and Related Materials
cific wavelengths for an unknown sample to analytical curves
E863 Practice for Describing Atomic Absorption Spectro-
3 made from reference standards of known composition.
metric Equipment (Withdrawn 2004)
E1479 Practice for Describing and Specifying Inductively-
5. Significance and Use
5.1 The presence and concentration of elements in lime and
This test method is under the jurisdiction of ASTM Committee C07 on Lime
limestone is important in determining product quality and its
and is the direct responsibility of Subcommittee C07.05 on Chemical Tests
suitability for various uses. This test method provides a means
Current edition approved June 1, 2009. Published September 2009. Originally
ofmeasuringthemajorandtraceelementconcentrationinlime
approved in 1995. Last previous edition approved in 2001 as C1301 – 95(2001).
DOI: 10.1520/C1301-95R09E01.
and limestone.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL
The last approved version of this historical standard is referenced on 33431.
www.astm.org. 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
´1
C1301 − 95 (2009)
A
TABLE 1 Elements and Some Suggested Wavelengths
7. Apparatus
Major Elements ICP Wavelength, nm AA Wavelength, nm
7.1 Spectrometer.
B
Calcium 317.933 (315.887) 422.7
7.1.1 Inductively Coupled Plasma Emission Spectrometer
Magnesium 279.079 (285.213) 285.2
Silicon 251.611 (288.160) 251.6 (ICP)—Either a scanning sequential or multi-element simulta-
Aluminum 308.215 (309.271) 309.3
neous type ICP, with resolution appropriate for the elements to
Iron 259.940 248.3
be analyzed.The optical path may be in air, vacuum or an inert
Manganese 257.610 279.5
Sodium 588.995 (589.59) 589.0 gas. A detailed description of an ICP is given in Practice
Potassium 766.491 766.5
E1479.
C
Phosphorus 214.914 (213.618) .
7.1.2 Atomic Absorption Spectrometer (AA)—An atomic
Strontium 421.552 460.7
absorption spectrometer consisting of single or double beam
Trace Elements ICP Wavelength, nm AA Wavelength, nm
optics, a monochromator, photomultiplier detector, adjustable
slits, a wavelength range from 190 to 800 nm, and provisions
Antimony 206.833 217.6
Arsenic 193.696 193.7 for interfacing with either a strip chart recorder or a computer.
Barium 455.403 (493.409) 553.6
A simultaneous background correction system is also recom-
Beryllium 313.042 234.9
mended. A detailed description of an AA is given in Practice
Boron 249.773 249.8
Cadmium 226.502 (228.80) 228.8 E863.
Chromium 267.716 (205.552) 357.9
7.1.2.1 Hollow Cathode Lamps—Single hollow cathode
Cobalt 228.616 240.7 (242.5)
lamps, one for each element. Multi-element hollow cathode
Copper 324.754 324.8
Lead 220.353 217.0 (283.3)
lamps can be used but spectral interferences are possible.
Molybdenum 202.030 (203.844) 313.3
Nickel 231.604 (221.647) 232.0
8. Reagents
Selenium 196.090 196.0
Silver 328.068 328.1
8.1 Purity of Reagents—Reagents should conform to the
C
Sulfur 180.731 (180.669) .
specifications of the Committee on Analytical Reagents of the
Thallium 190.864 276.8
Tin 189.989 235.5 (286.3) American Chemical Society as a minimum when such speci-
Vanadium 292.402 318.4
fications are available. The high sensitivity of both the ICP
Zinc 213.856 (202.551) 213.9
andAAmayrequirereagentsofhighpurity.Itisrecommended
A
The suggested wavelengths may vary for your particular instrument.
that the reagents be of sufficiently high purity so as not to
B
Numbers in parentheses are alternate wavelengths.
C
lessen the accuracy of the determination.
Not recommended or not used.
8.2 Purity of Water—At minimum, water should conform to
Type II of Specification D1193.
6. Interferences
8.3 Stock Solutions—Standard stock solutions may be pur-
6.1 Chemical—Chemical interferences, most common in
chased or prepared from high purity metals or metal salts
AA, arise from the formation of molecular compounds that (Method 6010, SW-846; EPAMethods 200.7 and 200.9). Salts
cause absorbances at the wavelength of interest. This molecu-
should be dried at 105°C for 1 h, unless otherwise specified.
lar band spectral overlap can be minimized by buffering the
8.4 Multi-element Calibration Standards—ICP calibration
sample with matrix modifiers (a Lanthanum additive, for
is most often performed using multi-element calibration stan-
example), using standard additions techniques, matrix match-
dards prepared from single element stock solutions. Prior to
ing or by careful selection of operating conditions (for
preparing the mixed standards, each stock solution should be
example,usingahotternitrousoxide/acetyleneflame,selecting
analyzed separately to determine possible spectral interference
an alternate wavelength).
or the presence of impurities. Standards are combined in such
6.2 Physical—Physical interferences are the result of the a way that they are chemically compatible (no precipitation
inconsistencies in the introduction of the sample into the
occurs) and do not cause spectral interferences.An example of
instrument, namely the transport and atomization/nebulization
multi-element combinations is given in EPA Method 200.7.
ofthesample.Theseinconsistenciesareafunctionofchanging
8.5 Interference Check Sample—Interferencechecksamples
viscosity and surface tension, and are found primarily in
aremadefromsingleelementstocksolutionsataconcentration
samples of high-dissolved solids or high-acid concentrations.
level equal to that of the samples to be analyzed.
Physical interferences can be reduced by diluting the sample
8.6 Calibration Blank—A calibration blank is prepared at
and by the use of a peristaltic pump.
the same acid strength as that of the samples to be analyzed;
6.3 Spectral—Spectral interference, most common in ICP,
usually 5 or 10 %. To prepare a 10 % nitric acid calibration
consists of overlapping and unresolved peaks. Computer
blank, add one volume of nitric acid to nine volumes of water.
software, along with the analysis of the suspected interfering
element, can compensate for this effect. Using an alternate
wavelength is also a solution. Another spectral interference is
Reagent Chemicals, American Chemical Society Sp
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