ASTM C1111-10(2020)

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.
Designation: C1111 − 10 (Reapproved 2020)
Standard Test Method for
Determining Elements in Waste Streams by Inductively
Coupled Plasma-Atomic Emission Spectroscopy
This standard is issued under the fixed designation C1111; 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 accuracy of different devices or the precision between instru-
ments of the same make and model.
1.1 This test method covers the determination of trace,
1.7 This test method contains notes that are explanatory and
minor, and major elements in waste streams by inductively
are not part of the mandatory requirements of the method.
coupled plasma-atomic emission spectroscopy (ICP-AES) fol-
lowing an acid digestion of the sample. Waste streams from
1.8 The values stated in SI units are to be regarded as
manufacturing processes of nuclear and non-nuclear materials
standard. No other units of measurement are included in this
can be analyzed. This test method is applicable to the deter-
standard.
mination of total metals. Results from this test method can be
1.9 This standard does not purport to address all of the
used to characterize waste received by treatment facilities and
safety concerns, if any, associated with its use. It is the
to formulate appropriate treatment recipes. The results are also
responsibility of the user of this standard to establish appro-
usable in process control within waste treatment facilities.
priate safety, health, and environmental practices and deter-
1.2 This test method is applicable only to waste streams that
mine the applicability of regulatory limitations prior to use.
contain radioactivity levels that do not require special person-
1.10 This international standard was developed in accor-
nel or environmental protection.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
1.3 A list of the elements determined in waste streams and
Development of International Standards, Guides and Recom-
the corresponding lower reporting limit is found in Table 1.
mendations issued by the World Trade Organization Technical
1.4 This test method has been used successfully for treat-
Barriers to Trade (TBT) Committee.
mentofalargevarietyofwastesolutionsandindustrialprocess
2. Referenced Documents
liquids. The composition of such samples is highly variable,
both between waste stream types and within a single waste
2.1 ASTM Standards:
stream. As a result of this variability, a single acid digestion
C859 Terminology Relating to Nuclear Materials
scheme may not be expected to succeed with all sample
C1109 Practice for Analysis of Aqueous Leachates from
matrices. Certain elements may be recovered on a semi-
Nuclear Waste Materials Using Inductively Coupled
quantitative basis, while most results will be highly quantita-
Plasma-Atomic Emission Spectroscopy
tive.
C1234 Practice for Preparation of Oils and Oily Waste
Samples by High-Pressure, High-Temperature Digestion
1.5 Thistestmethodshouldbeusedbyanalystsexperienced
for Trace Element Determinations
in the use of ICP-AES, the interpretation of spectral and
D1193 Specification for Reagent Water
non-spectral interferences, and procedures for their correction.
E135 Terminology Relating to Analytical Chemistry for
1.6 No detailed operating instructions are provided because
Metals, Ores, and Related Materials
of differences among various makes and models of suitable
E177 Practice for Use of the Terms Precision and Bias in
ICP-AES instruments. Instead, the analyst shall follow the
ASTM Test Methods
instructions provided by the manufacturer of the particular
2.2 ISO and European Standards:
instrument. This test method does not address comparative
ISO 1042 Laboratory Glassware—One-mark Volumetric
Flasks
1 2
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2020. Published January 2021. Originally the ASTM website.
approved in 1988. Last previous edition approved in 2015 as C1111 – 10 (2015). Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
DOI: 10.1520/C1111-10R20. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1111 − 10 (2020)
TABLE 1 Analytical Wavelengths and Applicable Concentration
A
Ranges
B
Lower Limit,
Element Upper Limit, mg/L Wavelength, nm
mg/L
Aluminum 0.02 5000 308.22, 237.01
Barium 0.001 100 493.41
Beryllium 0.0003 100 313.04
Boron 0.004 200 249.68
Cadmium 0.003 200 226.50
Calcium 0.004 1000 317.93, 393.37
Chromium 0.01 5000 267.72, 298.92
Cobalt 0.005 150 228.62
Copper 0.004 150 324.75
Iron 0.004 5000 271.44, 259.94
Lead 0.05 200 220.35
Lithium 0.004 150 670.78
Magnesium 0.0005 5000 293.65, 279.55
Manganese 0.001 150 257.61
Nickel 0.01 5000 231.60, 341.48
Phosphorus 0.2 250 178.29
Potassium 0.6 1000 766.49
Silver 0.006 150 328.07
Sodium 0.02 200 330.29, 588.99
Strontium 0.0004 100 421.55
Thorium 0.2 250 283.73
Titanium 0.003 150 334.94
Uranium 0.03 1000 409.01
Vanadium 0.005 250 292.40
Zinc 0.001 250 213.86
Zirconium 0.005 250 339.20
A
The estimated upper and lower concentration limits are to be used only as a
general guide. These values are instrument and sample dependent, and as the
sample matrix varies, these concentrations may be expected to vary also.
B
These limits obtained using a Jarrell-Ash ICAP-9000 ICP Spectrometer.
ISO 3585 Borosilicate Glass 3.3—Properties contains undissolved solids, the elements are determined using
ISO 8655 Piston-Operated Volumetric Instruments (6 parts) an aliquot of the thoroughly mixed sample after a nitric acid
digestion.
2.3 US EPA Standard:
Method 6010, Inductively Coupled Plasma Method, SW-
5. Significance and Use
846, Test Methods for Evaluating Solid Waste
5.1 This test method is useful for the determination of
3. Terminology
concentrations of metals in many waste streams from various
3.1 Definitions: nuclear and non-nuclear manufacturing processes. The test
method is useful for characterizing liquid wastes and liquid
3.1.1 For definitions of terms used in this test method, refer
to Terminology C859, Terminology E135, and Practice C1109. wastes containing undissolved solids prior to treatment,
storage, or stabilization. It has the capability for the simulta-
4. Summary of Test Method neous determination of up to 26 elements.
4.1 The general principles of emission spectrometric analy- 5.2 The applicable concentration ranges of the elements
sis are given in ASTM Methods for Emission Spectrochemical
analyzed by this procedure are listed in Table 1.
Analysis. In this test method, elements are determined, either
sequentially or simultaneously, by ICP-AES (Method 6010,
6. Interferences
SW-846).
6.1 Spectral interferences in ICP-AES, and ways to com-
4.2 If the sample is a clear acidified solution, the elements
pensate for them, include the following:
are determined with no further pretreatment. If the sample
6.1.1 Interelement Interferences—Interelement interfer-
ences are characterized by spectral overlap of one element line
over another. This interference can be compensated for by
Available from U.S. Government Printing Office, Superintendent of
correction of the raw data, which requires measurement of the
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
interfering element at the wavelength of interest. Table 2 lists
www.access.gpo.gov.
5 some interference effects for the recommended wavelengths
ASTM Methods for Emission Spectrochemical Analysis, ASTM International,
1967. given in Table 1. The data in Table 2 are intended for use only
C1111 − 10 (2020)
TABLE 2 Analyte Concentration Equivalents Arising from Interferents at 1000 mg/L Level
Wave-
Interferent, mg/L
Analyte lengths,
Aluminum Chromium Copper Iron Nickel Antimony Silicon Tin Uranium Vanadium
nm
Aluminum 308.22 0.0020 0.0044 0.0199
Aluminum 237.21 −0.0022 −0.0084 0.0350
Barium 493.41
Beryllium 313.04 0.0013
Boron 249.68 0.0015
Cadmium 226.50 0.0002 −0.0004
Calcium 317.93 −0.0018
Calcium 393.37 0.0002
Chromium 267.72 0.0025 0.0018
Chromium 298.92 0.0560
Cobalt 228.62 0.0001 0.0001
Copper 324.75
Iron 259.94 0.0001 −0.0001 −0.0002
Iron 271.44 0.0039 −0.0015 0.0220
Lead 220.35 −0.0012 −0.0028 0.0002 0.0006 0.0016
Lithium 670.78 0.0003
Magnesium 279.55
Magnesium 293.65 −0.0270 −0.1390 0.0350
Manganese 257.61 0.0002
Nickel 231.60 −0.0002 0.0003 0.0001 0.0003
Nickel 341.48 0.0027
Phosphorus 178.29 0.0002 −0.0079 0.0120 0.0004 0.0044
Potassium 766.49 0.0010 −0.0005 0.0014
Silver 328.07 0.0003
Sodium 330.29 0.0035 −0.0220 −0.0145 −0.1580
Sodium 588.99 0.0006 0.0017 0.0002
Strontium 421.55
Thorium 283.73 0.0007 0.0005 0.0049 0.0500
Titanium 334.94 0.0003
Vanadium 292.40 −0.0029 −0.0014
Zinc 213.85 0.0034 0.0001 0.0038
Zirconium 339.20 −0.0003 −0.0002 −0.0005
as a rudimentary guide for indicating potential spectral inter- cleaned before use by soaking in nitric acid and then rinsing
ferences. Various analytical systems may exhibit somewhat thoroughly with water.
different levels of interferences. Therefore, the interference
7.3 Filters, inert membrane, having pore size of 2.5 µm.
effects must be evaluated for each individual system.
7.4 Piston-operated Volumetric Pipettors and Dispensers,
6.1.2 Molecular Band Interference—Molecular band inter-
complying with the requirements of ISO 8655, for pipetting
ference arising from overlap of molecular band spectra at the
and dispensing of solutions, acids, and so forth.
wavelengthofinterestcanbeeliminatedbycarefulselectionof
wavelength.
7.5 Bottles, tetrafluoroethylene or polyethylene, for storage
6.1.3 High Background—High background effects from
of calibration and check solutions.
scattered light, etc., can be compensated for by background
7.6 Disposable Gloves, impermeable, for protection from
correction adjacent to the analyte line.
corrosive substances. Polyvinyl chloride (PVC) gloves are
6.2 Non-spectral Interferences—These include physical or
suitable.
chemical effects, such as high solids content or high acid
7.7 Inductively Coupled Plasma—Atomic Emission
concentration, that affect nebulization or the transport of the
Spectrometer, computer controlled, with a spectral bandpass of
sample to the plasma and its vaporization, atomization, or
0.05 nm or less.
excitation in the plasma. Effects due to high solids content or
high acid concentration can be reduced by a tenfold dilution of
NOTE 1—A bandpass of 0.05 nm or less is required to provide the
necessary spectral resolution.
the sample and the use of a peristaltic pump in conjunction
NOTE 2—The spectrometer may be of the simultaneous multielement or
with a high-solids nebulizer.
sequential scanning type. The spectrometer may be of the air path, inert
gaspath,orvacuumtype,withspectrallinesselectedappropriatelyforuse
7. Apparatus
with the specific instrument.
7.1 Ordinary laboratory apparatus are not listed, but are NOTE 3—An autosampler having a flowing rinse is recommended.
assumed to be present.
8. Reagents
7.2 Glassware, volumetric flasks comp
...