ASTM D1971-11
(Practice)Standard Practices for Digestion of Water Samples for Determination of Metals by Flame Atomic Absorption, Graphite Furnace Atomic Absorption, Plasma Emission Spectroscopy, or Plasma Mass Spectrometry
Standard Practices for Digestion of Water Samples for Determination of Metals by Flame Atomic Absorption, Graphite Furnace Atomic Absorption, Plasma Emission Spectroscopy, or Plasma Mass Spectrometry
SIGNIFICANCE AND USE
The determination of metals in water often requires the measurement of total (suspended and dissolved) metals as well as soluble (dissolved) metals. In such cases, consistent and dependable digestion procedures must be used so that data derived for the total metals content is reliable.
The practices given are applicable to a wide variety of sample types for the purpose of preparing a sample for metals analyses by atomic absorption spectrophotometry or plasma emission spectroscopy (see Test Methods D1976, D3919, D4691, and D4190) or plasma-mass spectrometry (See Test Method D5673) and have been shown to give good recovery in the following matrices: industrial effluents; waste water treatment plant influents, sludges, dewatered sludges, and effluents; river and lake waters; and plant and animal tissues. Elements which have shown good recovery include: copper, nickel, lead, zinc, cadmium, iron, manganese, magnesium, and calcium.
Good recovery for the indicated sample types and metals may not be achieved at all times due to each sample's unique characteristics. Users must always validate the practice for their particular samples.
The analytical results achieved after applying these practices cannot necessarily be deemed as a measure of bioavailable or environmentally available elements.
These three practices may not give the same recovery when applied to the same sample, nor will they necessarily give the same results as achieved using other digestion techniques. An alternate digestion technique is Practice D4309.
SCOPE
1.1 Most atomic absorption and plasma emission spectroscopy, and plasma-mass spectrometric test methods require that the metals of interest be dissolved in a liquid phase before being introduced into the spectrophotometer. These practices describe digestion or dissolution procedures whereby analyte metals associated with the solid fraction of a sample can be brought into solution for subsequent analysis. The following practices are included:
Sections Practice ADigestion with Mineral Acids and
Elevated Pressure 8 through 13 Practice BDigestion with Mineral Acids and
Heating at Atmospheric Pressure14 through 19 Practice CIn-bottle digestion with Mineral Acids20 through 25
1.2 These practices have been demonstrated to be applicable to a wide variety of sample types and sample matrices, and in many cases, will give complete dissolution of the analyte metals of interest. They are by no means the only digestion procedures available.
1.3 The user of these practices should be cautioned that these practices may not completely dissolve all portions of a sample's solid phase and may not give complete recovery of the desired analyte metals. In these cases, other digestion techniques are available that will effect complete dissolution of a sample. It is the user's responsibility to ensure the validity of these practices for use on their particular sample matrix, for their metals of interest.
1.4 This practice assumes that the criteria established in Guide D3856 can be met.
1.5 These digestion procedures have been selected for their wide application, low cost, and ease of use.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.7 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. Specific hazard statements are given in Section 6.
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Designation: D1971 − 11
StandardPractices for
Digestion of Water Samples for Determination of Metals by
Flame Atomic Absorption, Graphite Furnace Atomic
Absorption, Plasma Emission Spectroscopy, or Plasma
1
Mass Spectrometry
This standard is issued under the fixed designation D1971; 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* 1.6 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
1.1 Most atomic absorption and plasma emission
only.
spectroscopy, and plasma-mass spectrometric test methods
1.7 This standard does not purport to address all of the
require that the metals of interest be dissolved in a liquid phase
safety concerns, if any, associated with its use. It is the
before being introduced into the spectrophotometer. These
responsibility of the user of this standard to establish appro-
practices describe digestion or dissolution procedures whereby
priate safety and health practices and determine the applica-
analyte metals associated with the solid fraction of a sample
bility of regulatory limitations prior to use. Specific hazard
can be brought into solution for subsequent analysis. The
statements are given in Section 6.
following practices are included:
Sections
2. Referenced Documents
PracticeA—Digestion with MineralAcids and 8 through 13
2
Elevated Pressure
2.1 ASTM Standards:
Practice B—Digestion with MineralAcids and 14 through 19
D511 Test Methods for Calcium and Magnesium In Water
Heating atAtmospheric Pressure
Practice C—In-bottle digestion with MineralAcids 20 through 25 D857 Test Method for Aluminum in Water
D858 Test Methods for Manganese in Water
1.2 Thesepracticeshavebeendemonstratedtobeapplicable
D1068 Test Methods for Iron in Water
to a wide variety of sample types and sample matrices, and in
D1129 Terminology Relating to Water
many cases, will give complete dissolution of the analyte
D1193 Specification for Reagent Water
metals of interest. They are by no means the only digestion
D1687 Test Methods for Chromium in Water
procedures available.
D1688 Test Methods for Copper in Water
1.3 The user of these practices should be cautioned that
D1691 Test Methods for Zinc in Water
these practices may not completely dissolve all portions of a
D1886 Test Methods for Nickel in Water
sample’s solid phase and may not give complete recovery of
D1976 Test Method for Elements in Water by Inductively-
the desired analyte metals. In these cases, other digestion
Coupled Argon Plasma Atomic Emission Spectroscopy
techniques are available that will effect complete dissolution of
D3370 Practices for Sampling Water from Closed Conduits
a sample. It is the user’s responsibility to ensure the validity of
D3372 Test Method for Molybdenum in Water
these practices for use on their particular sample matrix, for
D3557 Test Methods for Cadmium in Water
their metals of interest.
D3558 Test Methods for Cobalt in Water
D3559 Test Methods for Lead in Water
1.4 This practice assumes that the criteria established in
D3645 Test Methods for Beryllium in Water
Guide D3856 can be met.
D3856 Guide for Management Systems in Laboratories
1.5 These digestion procedures have been selected for their
Engaged in Analysis of Water
wide application, low cost, and ease of use.
D3866 Test Methods for Silver in Water
D3919 Practice for Measuring Trace Elements in Water by
Graphite Furnace Atomic Absorption Spectrophotometry
1
These practices are under the jurisdiction of ASTM Committee D19 on Water
and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
2
in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2011. Published April 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1991. Last previous edition approved in 2006 as D1971 – 02(2006). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D1971-11. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1
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D1971 − 11
D4190 TestMethodforElementsinWaterbyDirect-Current Method D5673) and have been shown to give good recovery in
Plasma Atomic Emission Spectroscopy the following matrices: industrial effluents; waste water treat-
D4191 Test Method for Sodium inWater byAtomicAbsorp- ment plant influents, sludges, dewatered sludges, an
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D1971–02 (Reapproved 2006) Designation:D1971–11
Standard Practices for
Digestion of Water Samples for Determination of Metals by
Flame Atomic Absorption, Graphite Furnace Atomic
Absorption, Plasma Emission Spectroscopy, or Plasma
1
Mass Spectrometry
This standard is issued under the fixed designation D1971; 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 Most atomic absorption and plasma emission spectroscopy, and plasma-mass spectrometric test methods require that the
metals of interest be dissolved in a liquid phase before being introduced into the spectrophotometer. These practices describe
digestion or dissolution procedures whereby analyte metals associated with the solid fraction of a sample can be brought into
solution for subsequent analysis. The following practices are included:
Sections
PracticeA—Digestion with MineralAcids and 8 through 13
Elevated Pressure
Practice B—Digestion with MineralAcids and 14 through 19
Heating atAtmospheric Pressure
Practice C—In-bottle digestion with MineralAcids 20 through 25
1.2 Thesepracticeshavebeendemonstratedtobeapplicabletoawidevarietyofsampletypesandsamplematrices,andinmany
cases, will give complete dissolution of the analyte metals of interest. They are by no means the only digestion procedures
available.
1.3 The user of these practices should be cautioned that these practices may not completely dissolve all portions of a sample’s
solid phase and may not give complete recovery of the desired analyte metals. In these cases, other digestion techniques are
available that will effect complete dissolution of a sample. It is the user’s responsibility to ensure the validity of these practices
for use on their particular sample matrix, for their metals of interest.
1.4 This practice assumes that the criteria established in Guide D3856 can be met.
1.5 These digestion procedures have been selected for their wide application, low cost, and ease of use.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.7 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. Specific hazard statements are given in Section 6.
2. Referenced Documents
2
2.1 ASTM Standards:
D511 Test Methods for Calcium and Magnesium In Water
D857 Test Method for Aluminum in Water
D858 Test Methods for Manganese in Water
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water D1192Guide for Equipment for Sampling Water and Steam in Closed Conduits
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
1
These practices are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in
Water.
Current edition approved Dec. 15, 2006. Published February 2007. Originally approved in 1991. Last previous edition approved in 2002 as D1971–02. DOI:
10.1520/D1971-02R06.
Current edition approved April 1, 2011. Published April 2011. Originally approved in 1991. Last previous edition approved in 2006 as D1971 – 02(2006). DOI:
10.1520/D1971-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D1971–11
D1691 Test Methods for Zinc in Water
D1886 Test Methods for Nickel in Water
D1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy
D3370 Practices for Sampling Water from Closed Conduits
D3372 Test Method for Molybdenum in Water
D3557 Test Methods for Cadmium in Water
D3558 Test Methods for Cobalt in Water
D3559 Test Methods for Lead in Water
D3645 Test Methods for Beryllium in Water
D3856
...
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