ASTM C1301-95(2014)

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
5.1 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.

General Information

• Status: Historical
• Publication Date: 30-Jun-2014
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C07 - Lime and Limestone
• Drafting Committee: C07.05 - Chemical Tests

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2014)
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.
1. Scope 2.2 U.S. EPA Standards:
Methods for the Determination of Metals in Environmental
1.1 The following test method covers the use of inductively
Samples; U.S. EPA Methods 200.2, 200.7, and
coupled plasma-atomic emission spectroscopy (ICP) and
200.9; Smoley, C. K., 1992
atomic absorption spectroscopy (AA) in the analysis of major
Method 6010 InductivelyCoupledPlasmaMethod,SW-846,
and trace elements in limestone and lime (calcined limestone).
Test Methods for Evaluating Solid Waste
1.2 Table 1 lists some of the elements that can be analyzed
3. Terminology
by this test method and the preferred wavelengths. Also see
U.S. EPA Methods 200.7 and 200.9.
3.1 Definitions—Definitions for terms used in this test
method can be found in Terminologies C51 and E135.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3.2 Additional Definitions:
3.2.1 total recoverable, n—trace element concentration in
standard.
an unfiltered sample after heating in acid.
1.4 This standard does not purport to address all of the
3.2.2 total digestion, n—complete digestion of a sample,
safety concerns, if any, associated with its use. It is the
including silica and silicate minerals, using the fusion-flux
responsibility of the user of this standard to establish appro-
method.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
4.1 Asample, digested by either fusion or acid, is atomized
2. Referenced Documents
2 and passed into an excitation medium (a plasma in the case of
2.1 ASTM Standards:
ICP;aflameinthecaseofAA).Theresultingionsareanalyzed
C51 Terminology Relating to Lime and Limestone (as used
by atomic spectroscopy. Elemental concentrations are deter-
by the Industry)
mined by graphically relating the emission/absorption at spe-
D1193 Specification for Reagent Water
cific wavelengths for an unknown sample to analytical curves
E135 Terminology Relating to Analytical Chemistry for
made from reference standards of known composition.
Metals, Ores, and Related Materials
E863 Practice for Describing Atomic Absorption Spectro-
5. Significance and Use
metric Equipment (Withdrawn 2004)
5.1 The presence and concentration of elements in lime and
E1479 Practice for Describing and Specifying Inductively-
limestone is important in determining product quality and its
Coupled Plasma Atomic Emission Spectrometers
suitability for various uses. This test method provides a means
ofmeasuringthemajorandtraceelementconcentrationinlime
and limestone.
This test method is under the jurisdiction of ASTM Committee C07 on Lime
andLimestoneandisthedirectresponsibilityofSubcommitteeC07.05onChemical
6. Interferences
Tests.
6.1 Chemical—Chemical interferences, most common in
Current edition approved July 1, 2014. Published July 2014. Originally approved
ε
in 1995. Last previous edition approved in 2009 as C1301 – 95(2009) . DOI:
AA, arise from the formation of molecular compounds that
10.1520/C1301-95R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL
Standards volume information, refer to the standard’s Document Summary page on 33431.
the ASTM website. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
The last approved version of this historical standard is referenced on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.astm.org. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1301 − 95 (2014)
A
TABLE 1 Elements and Some Suggested Wavelengths
7.1.1 Inductively Coupled Plasma Emission Spectrometer
Major Elements ICP Wavelength, nm AA Wavelength, nm
(ICP)—Either a scanning sequential or multi-element simulta-
B
Calcium 317.933 (315.887) 422.7
neous type ICP, with resolution appropriate for the elements to
Magnesium 279.079 (285.213) 285.2
be analyzed.The optical path may be in air, vacuum or an inert
Silicon 251.611 (288.160) 251.6
gas. A detailed description of an ICP is given in Practice
Aluminum 308.215 (309.271) 309.3
Iron 259.940 248.3
E1479.
Manganese 257.610 279.5
7.1.2 Atomic Absorption Spectrometer (AA)—An atomic
Sodium 588.995 (589.59) 589.0
absorption spectrometer consisting of single or double beam
Potassium 766.491 766.5
C
Phosphorus 214.914 (213.618) .
optics, a monochromator, photomultiplier detector, adjustable
Strontium 421.552 460.7
slits, a wavelength range from 190 to 800 nm, and provisions
for interfacing with either a strip chart recorder or a computer.
Trace Elements ICP Wavelength, nm AA Wavelength, nm
A simultaneous background correction system is also recom-
Antimony 206.833 217.6
mended. A detailed description of an AA is given in Practice
Arsenic 193.696 193.7
Barium 455.403 (493.409) 553.6 E863.
Beryllium 313.042 234.9
7.1.2.1 Hollow Cathode Lamps—Single hollow cathode
Boron 249.773 249.8
lamps, one for each element. Multi-element hollow cathode
Cadmium 226.502 (228.80) 228.8
lamps can be used but spectral interferences are possible.
Chromium 267.716 (205.552) 357.9
Cobalt 228.616 240.7 (242.5)
Copper 324.754 324.8
8. Reagents
Lead 220.353 217.0 (283.3)
Molybdenum 202.030 (203.844) 313.3
8.1 Purity of Reagents—Reagents should conform to the
Nickel 231.604 (221.647) 232.0
specifications of the Committee on Analytical Reagents of the
Selenium 196.090 196.0
Silver 328.068 328.1 American Chemical Society as a minimum when such speci-
C
Sulfur 180.731 (180.669) .
fications are available. The high sensitivity of both the ICP
Thallium 190.864 276.8
andAAmayrequirereagentsofhighpurity.Itisrecommended
Tin 189.989 235.5 (286.3)
Vanadium 292.402 318.4 that the reagents be of sufficiently high purity so as not to
Zinc 213.856 (202.551) 213.9
lessen the accuracy of the determination.
A
The suggested wavelengths may vary for your particular instrument.
8.2 Purity of Water—At minimum, water should conform to
B
Numbers in parentheses are alternate wavelengths.
C
Not recommended or not used. Type II of Specification D1193.
8.3 Stock Solutions—Standard stock solutions may be pur-
chased or prepared from high purity metals or metal salts
(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
sample with matrix modifiers (a Lanthanum additive, for
8.4 Multi-element Calibration Standards—ICP calibration
example), using standard additions techniques, matrix match-
is most often performed using multi-element calibration stan-
ing or by careful selection of operating conditions (for
dards prepared from single element stock solutions. Prior to
example,usingahotternitrousoxide/acetyleneflame,selecting
preparing the mixed standards, each stock solution should be
an alternate wavelength).
analyzed separately to determine possible spectral interference
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
viscosity and surface tension, and are found primarily in
8.5 Interference Check Sample—Interferencechecksamples
samples of high-dissolved solids or high-acid concentrations.
aremadefromsingleelementstocksolutionsataconcentration
Physical interferences can be reduced by diluting the sample
level equal to that of the samples to be analyzed.
and by the use of a peristaltic pump.
8.6 Calibration Blank—A calibration blank is prepared at
6.3 Spectral—Spectral interference, most common in ICP,
the same acid strength as that of the samples to be analyzed;
consists of overlapping and unresolved peaks. Computer
usually 5 or 10 %. To prepare a 10 % nitric acid calibration
software, along with the analysis of the suspected interfering
blank, add one volume of nitric acid to nine volumes of water.
element, can compensate for this effect. Using an alternate
This same blank can be used as the rinse solution for flushing
wavelength is also a solution. Another spectral interference is
the system between standards and samples.
caused by background, both stray l
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: C1301 − 95 (Reapproved 2009) C1301 − 95 (Reapproved 2014)
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.
ε NOTE—A units statement was added editorially as new paragraph 1.3 and subsequent paragraphs were renumbered in
June 2009.
1. 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.
2. Referenced Documents
2.1 ASTM Standards:
C51 Terminology Relating to Lime and Limestone (as used by the Industry)
D1193 Specification for Reagent Water
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E863 Practice for Describing Atomic Absorption Spectrometric Equipment (Withdrawn 2004)
E1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission Spectrometers
2.2 U.S. EPA Standards:
Methods for the Determination of Metals in Environmental Samples; U.S. EPA Methods 200.2, 200.7, and 200.9; Smoley, C.
K., 1992
Method 6010,Method 6010 Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid Waste
3. Terminology
3.1 Definitions—Definitions for terms used in this test method can be found in Terminologies C51 and E135.
3.2 Additional Definitions:
3.2.1 total recoverable, n—trace element concentration in an unfiltered sample after heating in acid.
3.2.2 total digestion, n—complete digestion of a sample, including silica and silicate minerals, using the fusion-flux method.
This test method is under the jurisdiction of ASTM Committee C07 on Lime and Limestone and is the direct responsibility of Subcommittee C07.05 on Chemical Tests.
Current edition approved June 1, 2009July 1, 2014. Published September 2009July 2014. Originally approved in 1995. Last previous edition approved in 20012009 as
ε
C1301 – 95(2001).(2009) . DOI: 10.1520/C1301-95R09E01.10.1520/C1301-95R14.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Available from CRC Press, 2000 Corporate Blvd., N. W., Boca Raton, FL 33431.
Available from U.S. Government Printing Office, Washington, DC 20402. Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington,
DC 20401, http://www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1301 − 95 (2014)
A
TABLE 1 Elements and Some Suggested Wavelengths
Major Elements ICP Wavelength, nm AA Wavelength, nm
B
Calcium 317.933 (315.887) 422.7
Magnesium 279.079 (285.213) 285.2
Silicon 251.611 (288.160) 251.6
Aluminum 308.215 (309.271) 309.3
Iron 259.940 248.3
Manganese 257.610 279.5
Sodium 588.995 (589.59) 589.0
Potassium 766.491 766.5
C
Phosphorus 214.914 (213.618) .
Strontium 421.552 460.7
Trace Elements ICP Wavelength, nm AA Wavelength, nm
Antimony 206.833 217.6
Arsenic 193.696 193.7
Barium 455.403 (493.409) 553.6
Beryllium 313.042 234.9
Boron 249.773 249.8
Cadmium 226.502 (228.80) 228.8
Chromium 267.716 (205.552) 357.9
Cobalt 228.616 240.7 (242.5)
Copper 324.754 324.8
Lead 220.353 217.0 (283.3)
Molybdenum 202.030 (203.844) 313.3
Nickel 231.604 (221.647) 232.0
Selenium 196.090 196.0
Silver 328.068 328.1
C
Sulfur 180.731 (180.669) .
Thallium 190.864 276.8
Tin 189.989 235.5 (286.3)
Vanadium 292.402 318.4
Zinc 213.856 (202.551) 213.9
A
TABLE 1 Elements and Some Suggested Wavelengths
Major Elements ICP Wavelength, nm AA Wavelength, nm
B
Calcium 317.933 (315.887) 422.7
Magnesium 279.079 (285.213) 285.2
Silicon 251.611 (288.160) 251.6
Aluminum 308.215 (309.271) 309.3
Iron 259.940 248.3
Manganese 257.610 279.5
Sodium 588.995 (589.59) 589.0
Potassium 766.491 766.5
C
Phosphorus 214.914 (213.618) .
Strontium 421.552 460.7
Trace Elements ICP Wavelength, nm AA Wavelength, nm
Antimony 206.833 217.6
Arsenic 193.696 193.7
Barium 455.403 (493.409) 553.6
Beryllium 313.042 234.9
Boron 249.773 249.8
Cadmium 226.502 (228.80) 228.8
Chromium 267.716 (205.552) 357.9
Cobalt 228.616 240.7 (242.5)
Copper 324.754 324.8
Lead 220.353 217.0 (283.3)
Molybdenum 202.030 (203.844) 313.3
Nickel 231.604 (221.647) 232.0
Selenium 196.090 196.0
Silver 328.068 328.1
C
Sulfur 180.731 (180.669) .
Thallium 190.864 276.8
Tin 189.989 235.5 (286.3)
Vanadium 292.402 318.4
Zinc 213.856 (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.
C1301 − 95 (2014)
4. Summary of Test Method
4.1 A sample, digested by either fusion or acid, is atomized and passed into an excitation medium (a plasma in the case of ICP;
a flame in the case of AA). The resulting ions are analyzed by atomic spectroscopy. Elemental concentrations are determined by
graphically relating the emission/absorption at specific wavelengths for an unknown sample to analytical curves made from
reference standards of known composition.
5. Significance and Use
5.1 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.
6. Interferences
6.1 Chemical—Chemical interferences, most common in AA, arise from the formation of molecular compounds that cause
absorbances at the wavelength of interest. This molecular band spectral overlap can be minimized by buffering the sample with
matrix modifiers (a Lanthanum additive, for example), using standard additions techniques, matrix matching or by careful selection
of operating conditions (for example, using a hotter nitrous oxide/acetylene flame, selecting an alternate wavelength).
6.2 Physical—Physical interferences are the result of the inconsistencies in the introduction of the sample into the instrument,
namely the transport and atomization/nebulization of the sample. These inconsistencies are a function of changing viscosity and
surface tension, and are found primarily in samples of high-dissolved solids or high-acid concentrations. Physical interferences can
be reduced by diluting the sample and by the use of a peristaltic pump.
6.3 Spectral—Spectral interference, most common in ICP, consists of overlapping and unresolved peaks. Computer 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 caused by background, both stray light and continuous spectrum (continuous argon
spectrum, for example). Background correction adjacent to the analyte line will correct background spectral interference.
7. Apparatus
7.1 Spectrometer.
7.1.1 Inductively Coupled Plasma Emission Spectrometer (ICP)—Either a scanning sequential or multi-element simultaneous
type ICP, with resolution appropriate for the elements to be analyzed. The optical path may be in air, vacuum or an inert gas. A
detailed description of an ICP is given in Practice E1479.
7.1.2 Atomic Absorption Spectrometer (AA)—An atomic absorption spectrometer consisting of single or double beam optics, a
monochromator, photomultiplier detector, adjustable slits, a wavelength range from 190 to 800 nm, and provisions for interfacing
with either a strip chart recorder or a computer. A simultaneous background correction system is also recommended. A detailed
description of an AA is given in Practice E863.
7.1.2.1 Hollow Cathode Lamps—Single hollow cathode lamps, one for each element. Multi-element hollow cathode lamps can
be used but spectral interferences are possible.
8. Reagents
8.1 Purity of Reagents—Reagents should conform to the specifications of the Committee on Analytical Reagents of the
American Chemical Society as a minimum when such specifications are available. The high sensitivity of both the ICP and AA
may require reagents of high purity. It is recommended that the reagents be of sufficiently high purity so as not to lessen the
accuracy of the determination.
8.2 Purity of Water—At minimum, water should conform to Type II of Specification D1193.
8.3 Stock Solutions—Standard stock solutions may be purchased or prepared from high purity metals or metal salts (Method
6010, SW-846; EPA Methods 200.7 and 200.9). Salts should be dried at 105°C for 1 h, unless otherwise specified.
8.4 Multi-element Calibration Standards—ICP calibration is most often perfor
...