ASTM C1301-22

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Designation: C1301 − 95 (Reapproved 2014) C1301 − 22
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
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E863 Practice for Describing Atomic Absorption Spectrometric Equipment (Withdrawn 2004)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
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 July 1, 2014Dec. 1, 2022. Published July 2014December 2022. Originally approved in 1995. Last previous edition approved in 20092014 as
ε
C1301 – 95 (2014).(2009) . DOI: 10.1520/C1301-95R14.10.1520/C1301-22.
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volume information, refer to the standard’s Document Summary page on the ASTM website.
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C1301 − 22
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.
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.
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.
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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°C105 °C for 1 h, unless otherwise specified.
8.4 Multi-element Calibration Standards—ICP calibration is most often performed using multi-element calibration standards
prepared from single element stock solutions. Prior to preparing the mixed standards, each stock solution should be analyzed
separately to determine possible spectral interference or the presence of impurities. Standards are combined in such a way that they
are chemically compatible (no precipitation occurs) and do not cause spectral interferences. An example of multi-element
combinations is given in EPA Method 200.7.
8.5 Interference Check Sample—Interference check samples are made from single element stock solutions at a concentration level
equal to that of the samples to be analyzed.
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. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
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8.6 Calibration Blank—A calibration blank is prepared at the same acid strength as that of the samples to be analyzed; usually
5 or 10 %. To prepare a 10 % nitric acid calibration blank, add one volume of nitric acid to nine volumes of water. This same blank
can be used as the rinse solution for flushing the system between standards and samples.
8.7 Reagent Blank—The reagent blank contains all the reagents in the same concentrations (including nitric acid) as the samples
to be analyzed. The reagent blank is carried through the same processes as a sample for analysis.
8.8 Nitric Acid—High purity nitric acid is recommended.
8.9 Lithium Tetraborate (Li2B4O7) Powder or Lithium Metaborate (LiBO2)) Powder.
8.10 Non-Wetting Agent—Saturated solution of Hydrogen Bromide (HBr), Potassium Bromide (KBr) or Potassium Iodide (KI) as
a non-wetting agent to prevent the flux from sticking to the crucible.
8.11 Lanthanum Chloride (LaCl3) Powder—Lanthanum is added to samples for AA analysis as a releasing agent (for Calcium)
and ionization suppressant (for Aluminum). When added to the sample solution, Lanthanum will preferentially react with potential
interferents and “release” the analyte. In addition, the Lanthanum will preferentially ionize relative to Aluminum, aiding in the
number of ground state Aluminum atoms. A typical Lanthanum additive is prepared by dissolving 175 g LaCl3 in 1 L of water
(equivalent to 100 g/L Lanthanum).
9. Preparation of Apparatus
9.1 Prepare and operate the spectrometer in accordance with the manufacturer’s instructions. The present method assumes that
good operating procedures are followed. Design differences between spectrometers make it impractical to specify the required
steps in detail here.
10. Calibration and Standardization
10.1 Allow a warm-up time of at least 30 min. Operate the spectrometer according to the operation manual for the instrument.
10.2 Calibrate the instrument by aspirating the blank and standards. A10 % by volume HNO rinse solution is aspirated for a
minimum of 60 s between each standard. Most new systems are controlled by computer. The computer will establish the slope,
intercept and correlation coefficients for each element. Some suggested wavelengths are given in Table 1 and EPA Methods 200.2,
200.7, and 200.9.
10.3 A peristaltic pump is recommended for aspirating standards and samples. The peristaltic pump will reduce physical
interferences caused by changes in specimen viscosity and concentration (transport processes).
11. Sample Preparation
11.1 Major Elements—Samples for major element analysis are prepared for total digestion using lithium tetraborate or lithium
metaborate as a flux. Major elements include Calcium, Magnesium, Silicon, Aluminum, Iron, Manganese, Sodium and Potassium.
Trace elements such as Lead, Arsenic, Selenium and Antimony will partially volatilize using this fusion method and it is therefore
not recommended for trace element analysis.
11.1.1 Take a representative minus 100 mesh sample split and dry at 105°C105 °C for 2 h.
11.1.2 Weigh 0.25 g of dried sample in a graphite or platinum crucible. Then weigh 1.00 g of lithium metaborate in the crucible.
Add a few drops of non-wetting agent if needed. Mix the sample and lithium metaborate (the flux) well. Cover the mixed
sample-lithium metaborate with an additional 0.50 g of lithium metaborate. This will give a total sample-flux ratio of 1:6.
11.1.3 Place a lid (optional) on the crucible prepared in 11.1.2 and place in a muffle furnace at 1000°C1000 °C for 30 min. Gently
agitate the molten contents of the crucible at least once during the 30° min heating.
11.1.4 Add 12.5 mL of concentrated nitric acid and 40 mL of water to a clean 250 mL wide-mouth plastic bottle.
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11.1.5 When the 30 min heating in 11.1.3 is complete, quickly pour molten contents of the crucible into the plastic bottle described
in 11.1.4. The water will bubble and sizzle. Quickly put the lid on the plastic bottle and shake. To aid in digestion place the bottle
in a warm ultrasonic bath.
11.1.6 The contents of the plastic bottle can either be quantitatively transferred to a 250 mL volumetric flask and diluted to volume
or diluted to volume by weight (th
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