ASTM C1111-10(2015)

Standard Test Method for Determining Elements in Waste Streams by Inductively Coupled Plasma-Atomic Emission Spectroscopy

SIGNIFICANCE AND USE
5.1 This test method is useful for the determination of concentrations of metals in many waste streams from various nuclear and non-nuclear manufacturing processes. The test method is useful for characterizing liquid wastes and liquid wastes containing undissolved solids prior to treatment, storage, or stabilization. It has the capability for the simultaneous determination of up to 26 elements.  
5.2 The applicable concentration ranges of the elements analyzed by this procedure are listed in Table 1.
SCOPE
1.1 This test method covers the determination of trace, minor, and major elements in waste streams by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) following an acid digestion of the sample. Waste streams from manufacturing processes of nuclear and non-nuclear materials can be analyzed. This test method is applicable to the determination of total metals. Results from this test method can be used to characterize waste received by treatment facilities and to formulate appropriate treatment recipes. The results are also usable in process control within waste treatment facilities.  
1.2 This test method is applicable only to waste streams that contain radioactivity levels that do not require special personnel or environmental protection.  
1.3 A list of the elements determined in waste streams and the corresponding lower reporting limit is found in Table 1. (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.  
1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids. The composition of such samples is highly variable, both between waste stream types and within a single waste stream. As a result of this variability, a single acid digestion scheme may not be expected to succeed with all sample matrices. Certain elements may be recovered on a semi-quantitative basis, while most results will be highly quantitative.  
1.5 This test method should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and non-spectral interferences, and procedures for their correction.  
1.6 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.  
1.7 This test method contains notes that are explanatory and are not part of the mandatory requirements of the method.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.9 This standard does not purport to address all of the safety problems, 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-May-2015
• ICS: 13.030.30 - Special wastes
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

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: C1111 − 10 (Reapproved 2015)
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,
minor, and major elements in waste streams by inductively
1.7 This test method contains notes that are explanatory and
coupled plasma-atomic emission spectroscopy (ICP-AES) fol-
are not part of the mandatory requirements of the method.
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
used to characterize waste received by treatment facilities and
1.9 This standard does not purport to address all of the
to formulate appropriate treatment recipes. The results are also
safety problems, if any, associated with its use. It is the
usable in process control within waste treatment facilities.
responsibility of the user of this standard to establish appro-
1.2 This test method is applicable only to waste streams that
priate safety and health practices and determine the applica-
contain radioactivity levels that do not require special person-
bility of regulatory limitations prior to use.
nel or environmental protection.
2. Referenced Documents
1.3 A list of the elements determined in waste streams and
the corresponding lower reporting limit is found in Table 1.
2.1 ASTM Standards:
C859 Terminology Relating to Nuclear Materials
1.4 This test method has been used successfully for treat-
C1109 Practice for Analysis of Aqueous Leachates from
mentofalargevarietyofwastesolutionsandindustrialprocess
Nuclear Waste Materials Using Inductively Coupled
liquids. The composition of such samples is highly variable,
both between waste stream types and within a single waste Plasma-Atomic Emission Spectroscopy
stream. As a result of this variability, a single acid digestion C1234 Practice for Preparation of Oils and Oily Waste
scheme may not be expected to succeed with all sample
Samples by High-Pressure, High-Temperature Digestion
matrices. Certain elements may be recovered on a semi-
for Trace Element Determinations
quantitative basis, while most results will be highly quantita-
D1193 Specification for Reagent Water
tive.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
1.5 Thistestmethodshouldbeusedbyanalystsexperienced
E177 Practice for Use of the Terms Precision and Bias in
in the use of ICP-AES, the interpretation of spectral and
ASTM Test Methods
non-spectral interferences, and procedures for their correction.
2.2 ISO and European Standards:
1.6 No detailed operating instructions are provided because
ISO 1042 Laboratory Glassware—One-mark Volumetric
of differences among various makes and models of suitable
ICP-AES instruments. Instead, the analyst shall follow the Flasks
ISO 3585 Borosilicate Glass 3.3—Properties
instructions provided by the manufacturer of the particular
instrument. This test method does not address comparative ISO 8655 Piston-Operated Volumetric Instruments (6 parts)
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 [e-mail]. For Annual Book of ASTM
Test. Standardsvolume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2015. Published June 2015. Originally the ASTM website.
approved in 1988. Last previous edition approved in 2010 as C1111 – 10. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/C1111-10R15. 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 (2015)
TABLE 1 Analytical Wavelengths and Applicable Concentration
A
Ranges
Upper
Lower
B
Element Limit, Wavelength, nm
Limit,
mg/L
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.
2.3 US EPA Standard: nuclear and non-nuclear manufacturing processes. The test
Method 6010, Inductively Coupled Plasma Method, SW- method is useful for characterizing liquid wastes and liquid
846, Test Methods for Evaluating Solid Waste wastes containing undissolved solids prior to treatment,
storage, or stabilization. It has the capability for the simulta-
3. Terminology
neous determination of up to 26 elements.
3.1 Definitions—For definitions of terms used in this test
5.2 The applicable concentration ranges of the elements
method, refer to Terminology C859, Terminology E135, and
analyzed by this procedure are listed in Table 1.
Practice C1109.
6. Interferences
4. Summary of Test Method
6.1 Spectral interferences in ICP-AES, and ways to com-
4.1 The general principles of emission spectrometric analy-
pensate for them, include the following:
sis are given in Footnote 5. In this test method, elements are
6.1.1 Interelement Interferences—Interelement interfer-
determined, either sequentially or simultaneously, by ICP-AES
ences are characterized by spectral overlap of one element line
(Method 6010, SW-846).
over another. This interference can be compensated for by
correction of the raw data, which requires measurement of the
4.2 If the sample is a clear acidified solution, the elements
interfering element at the wavelength of interest. Table 2 lists
are determined with no further pretreatment. If the sample
some interference effects for the recommended wavelengths
contains undissolved solids, the elements are determined using
given in Table 1. The data in Table 2 are intended for use only
an aliquot of the thoroughly mixed sample after a nitric acid
as a rudimentary guide for indicating potential spectral inter-
digestion.
ferences. Various analytical systems may exhibit somewhat
5. Significance and Use different levels of interferences. Therefore, the interference
effects must be evaluated for each individual system.
5.1 This test method is useful for the determination of
6.1.2 Molecular Band Interference—Molecular band inter-
concentrations of metals in many waste streams from various
ference arising from overlap of molecular band spectra at the
wavelengthofinterestcanbeeliminatedbycarefulselectionof
AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
wavelength.
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
6.1.3 High Background—High background effects from
www.access.gpo.gov.
scattered light, etc., can be compensated for by background
ASTM Methods for Emission Spectrochemical Analysis, ASTM International,
1967. correction adjacent to the analyte line.
C1111 − 10 (2015)
TABLE 2 Analyte Concentration Equivalents Arising from Interferents at the 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
6.2 Non-Spectral Interferences—These include physical or 7.7 Inductively Coupled Plasma – Atomic Emission
chemical effects, such as high solids content or high acid Spectrometer, computer controlled, with a spectral bandpass of
concentration, that affect nebulization or the transport of the 0.05 nm or less.
sample to the plasma and its vaporization, atomization, or
NOTE 1—A bandpass of 0.05 nm or less is required to provide the
excitation in the plasma. Effects due to high solids content or
necessary spectral resolution.
high acid concentration can be reduced by a tenfold dilution of
NOTE 2—The spectrometer may be of the simultaneous multielement or
sequential scanning type. The spectrometer may be of the air path, inert
the sample and the use of a peristaltic pump in conjunction
gaspath,orvacuumtype,withspectrallinesselectedappropriatelyforuse
with a high-solids nebulizer.
with the specific instrument.
NOTE 3—An autosampler having a flowing rinse is recommended.
7. Apparatus
8. Reagents
7.1 Ordinary laboratory apparatus are not listed, but are
assumed to be present.
8.1 Purity of Reagents—Chemicals used in the preparation
of the standards must be of ultrahigh purity grade. Chemicals
7.2 Glassware, volumetric flasks complying with the re-
used in the preparation of the samples shall conform to the
quirements of ISO 1042, made of borosilicate glass complying
specifications of the Committee on Analytical Reagents of the
with the requirements of ISO 3585. Glassware should be
American Chemical Society, where such specifications are
cleaned before use by soaking in nitric acid and then rinsing
available.
thoroughly with water.
8.2 Purity of Water—Unless otherwise indicated, references
7.3 Filters, inert membrane, having pore size of 2.5 µm.
to water shall be understood to mean reagent water as defined
7.4 Piston-operated Volumetric Pipettors and Dispensers,
by Specification D1193, Type I, or water exceeding these
complying with the requirements of ISO 8655, for pipetting
specifications.
and dispensing of solutions, acids, and so forth.
7.5 Bottles, tetrafluoroethylene or polyethylene, for storage
Reagent Chemicals, American Chemical Society Specifications, American
of calibration and check solutions.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
7.6 Disposable Gloves, impermeable, for protection from
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
corrosive substances. Polyvinyl chloride (PVC) gloves are
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
suitable. MD.
C1111 − 10 (2015)
8.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid 8.9 Reagent Blank—The reagent blank must contain all of
(HNO ). the reagents and in the same volumes as used in the processing
of the samples. The reagent blank must be carried through the
8.4 Nitric Acid, 10 volume %—One volume of concentrated
complete procedure and contain the same acid concentration in
nitric acid (specific gravity 1.42) brought to ten volumes with
the final solution as the sample solution used for analysis.
water.
8.5 Stock Solutions—Standard stock solutions may be pur-
9. Calibration and Standardization
chased or prepared from ultrahigh purity grade metals or metal
9.1 After a warm-up time of at least 30 min, operate the
salts (Method 6010, SW-846).All salts must be dried for1hat
spectrometer according to the operation manual for the instru-
105°C unless otherwise specified. Stock solutions should
ment.
contain approximately 1000 to 10 000 mg/L of the element of
9.2 Calibrate the instrument by aspirating the blank and
interest to ensure long term stability in dilute nitric acid.
standards. A flush-out time of approximately 1 ⁄2 to 2 min
8.6 Multielement Working Calibration Standards—
should be allowed between standards, during which a calibra-
Multielement working calibration standards are prepared from
tion blank [10 volume % HNO ] is aspirated. The computer
the single element stock solutions at appropriate concentration
establishes the slope, intercept, and correlation statistics for
levelsforeachelement.Priortopreparingthemixedstandards,
each element. Suggested analytical wavelengths are listed in
each stock solution should be analyzed separately to determine
Table 1.
possible spectral interference or the presence of impurities.
9.3 To minimize physical interferences caused by changes
Care should be taken when preparing each multielement
in sample transport processes (due to variations in sample
calibration standard solution that the elements be compatible
viscosity and concentration), it may be necessary to use a
andstable.Anappropriateamountofconcentratednitricacidis
peristaltic pump in conjunction with certain nebulizers.
added to stock standard aliquots and final volume brought to
100 mL with water to ensure that the final nitric acid concen-
10. Sample Preparation
tration is 10 volume %. Transfer each multielement calibration
standard solution to a F
...

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.
Designation: C1111 − 10 C1111 − 10 (Reapproved 2015)
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
1.1 This test method covers the determination of trace, minor, and major elements in waste streams by inductively coupled
plasma-atomic emission spectroscopy (ICP-AES) following an acid digestion of the sample. Waste streams from manufacturing
processes of nuclear and non-nuclear materials can be analyzed. This test method is applicable to the determination of total metals.
Results from this test method can be used to characterize waste received by treatment facilities and to formulate appropriate
treatment recipes. The results are also usable in process control within waste treatment facilities.
1.2 This test method is applicable only to waste streams that contain radioactivity levels that do not require special personnel
or environmental protection.
1.3 A list of the elements determined in waste streams and the corresponding lower reporting limit is found in Table 1.
1.4 This test method has been used successfully for treatment of a large variety of waste solutions and industrial process liquids.
The composition of such samples is highly variable, both between waste stream types and within a single waste stream. As a result
of this variability, a single acid digestion scheme may not be expected to succeed with all sample matrices. Certain elements may
be recovered on a semi-quantitative basis, while most results will be highly quantitative.
1.5 This test method should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and
non-spectral interferences, and procedures for their correction.
1.6 No detailed operating instructions are provided because of differences among various makes and models of suitable
ICP-AES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument.
This test method does not address comparative accuracy of different devices or the precision between instruments of the same make
and model.
1.7 This test method contains notes that are explanatory and are not part of the mandatory requirements of the method.
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.9 This standard does not purport to address all of the safety problems, 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:
C859 Terminology Relating to Nuclear Materials
C1109 Practice for Analysis of Aqueous Leachates from Nuclear Waste Materials Using Inductively Coupled Plasma-Atomic
Emission Spectroscopy
C1234 Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace
Element Determinations
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
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Oct. 1, 2010June 1, 2015. Published October 2010June 2015. Originally approved in 1988. Last previous edition approved in 20042010 as
C1111 – 04.C1111 – 10. DOI: 10.1520/C1111-10.10.1520/C1111-10R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standardsvolume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1111 − 10 (2015)
TABLE 1 Analytical Wavelengths and Applicable Concentration
A
Ranges
Upper
Lower
B
Element Limit, Wavelength, nm
Limit,
mg/L
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.
2.2 ISO and European Standards:
ISO 1042 Laboratory Glassware—One-mark Volumetric Flasks
ISO 3585 Borosilicate Glass 3.3—Properties
ISO 8655 Piston-Operated Volumetric Instruments (6 parts)
2.3 US EPA Standard:
Method 6010, Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid Waste
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology C859, Terminology E135, and Practice
C1109.
4. Summary of Test Method
4.1 The general principles of emission spectrometric analysis are given in Ref.Footnote (5.1). In this test method, elements are
determined, either sequentially or simultaneously, by ICP-AES (Method 6010, SW-846).
4.2 If the sample is a clear acidified solution, the elements are determined with no further pretreatment. If the sample contains
undissolved solids, the elements are determined using an aliquot of the thoroughly mixed sample after a nitric acid digestion.
5. Significance and Use
5.1 This test method is useful for the determination of concentrations of metals in many waste streams from various nuclear and
non-nuclear manufacturing processes. The test method is useful for characterizing liquid wastes and liquid wastes containing
undissolved solids prior to treatment, storage, or stabilization. It has the capability for the simultaneous determination of up to 26
elements.
5.2 The applicable concentration ranges of the elements analyzed by this procedure are listed in Table 1.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
The boldface numbers in parentheses refer to a list of references at the end of this standard.ASTM Methods for Emission Spectrochemical Analysis, ASTM International,
1967.
C1111 − 10 (2015)
6. Interferences
6.1 Spectral interferences in ICP-AES, and ways to compensate for them, include the following:
6.1.1 Interelement Interferences—Interelement interferences are characterized by spectral overlap of one element line over
another. This interference can be compensated for by correction of the raw data, which requires measurement of the interfering
element at the wavelength of interest. Table 2 lists some interference effects for the recommended wavelengths given in Table 1.
The data in Table 2 are intended for use only as a rudimentary guide for indicating potential spectral interferences. Various
analytical systems may exhibit somewhat different levels of interferences. Therefore, the interference effects must be evaluated for
each individual system.
6.1.2 Molecular Band Interference—Molecular band interference arising from overlap of molecular band spectra at the
wavelength of interest can be eliminated by careful selection of wavelength.
6.1.3 High Background—High background effects from scattered light, etc., can be compensated for by background correction
adjacent to the analyte line.
6.2 Non-Spectral Interferences—These include physical or chemical effects, such as high solids content or high acid
concentration, that affect nebulization or the transport of the sample to the plasma and its vaporization, atomization, or excitation
in the plasma. Effects due to high solids content or high acid concentration can be reduced by a tenfold dilution of the sample and
the use of a peristaltic pump in conjunction with a high-solids nebulizer.
7. Apparatus
7.1 Ordinary laboratory apparatus are not listed, but are assumed to be present.
7.2 Glassware, volumetric flasks complying with the requirements of ISO 1042, made of borosilicate glass complying with the
requirements of ISO 3585. Glassware should be cleaned before use by soaking in nitric acid and then rinsing thoroughly with
water.
7.3 Filters, inert membrane, having pore size of 2.5 μm.
7.4 Piston-operated Volumetric Pipettors and Dispensers, complying with the requirements of ISO 8655, for pipetting and
dispensing of solutions, acids, and so forth.
7.5 Bottles, tetrafluoroethylene or polyethylene, for storage of calibration and check solutions.
TABLE 2 Analyte Concentration Equivalents Arising from Interferents at the 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
C1111 − 10 (2015)
7.6 Disposable Gloves, impermeable, for protection from corrosive substances. Polyvinyl chloride (PVC) gloves are suitable.
7.7 Inductively Coupled Plasma – Atomic Emission Spectrometer, computer controlled, with a spectral bandpass of 0.05 nm or
less.
NOTE 1—A bandpass of 0.05 nm or less is required to provide the necessary spectral resolution.
NOTE 2—The spectrometer may be of the simultaneous multielement or sequential scanning type. The spectrometer may be of the air path, inert gas
path, or vacuum type, with spectral lines selected appropriately for use with the specific instrument.
NOTE 3—An autosampler having a flowing rinse is recommended.
8. Reagents
8.1 Purity of Reagents—Chemicals used in the preparation of the standards must be of ultrahigh purity grade. Chemicals used
in the preparation of the samples shall conform to the specifications of the Committee on Analytical Reagents of the American
Chemical Society, where such specifications are available.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Specification D1193, Type I, or water exceeding these specifications.
8.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
8.4 Nitric Acid, 10 volume %—One volume of concentrated nitric acid (specific gravity 1.42) brought to ten volumes with water.
8.5 Stock Solutions—Standard stock solutions may be purchased or prepared from ultrahigh purity grade metals or metal salts
(Method 6010, SW-846). All salts must be dried for 1 h at 105°C unless otherwise specified. Stock solutions should contain
approximately 1 0001000 to 10 000 10 000 mg/L of the element of interest to ensure long term stability in dilute nitric acid.acid.
8.6 Multielement Working Calibration Standards—Multielement working calibration standards are prepared from the single
element stock solutions at appropriate concentration levels for each element. Prior to preparing the mixed standards, each stock
solution should be analyzed separately to determine possible spectral interference or the presence of impurities. Care should be
taken when preparing each multielement calibration standard solution that the elements be compatible and stable. An appropriate
amount of concentrated nitric acid is added to stock standard aliquots and final volume brought to 100 mL with water to ensure
that the final nitric acid concentration is 10 volume %. Transfer each multielement calibration standard solution to a FEP
fluorocarbon or new polyethylene bottle for storage. Fresh calibration standards should be prepared as needed with the realization
that concentration can change with time; the recommended maximum shelf-life for these solutions is one month. Calibration
standards must be initially verified using a quality control sample monitored weekly for stability. The actual number of calibration
standards needed will be a function of both chemical compatibility and the restrictions of the computer system used to control the
spectrometer. Additional calibration standards may be needed if a second, less sensitive emission line is used to extend the linear
range of one or more elements. Although not specifically required, some typical standard combinations are given below when using
the specific analytical wavelengths listed in Table 1.
8.6.1 Mixed Standard Solution I—Aluminum, barium, chromium, copper, iron, potassium, magnesium, manganese, nickel, and
sodium.
8.6.2 Mixed Standard S
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