ASTM D5198-09
(Practice)Standard Practice for Nitric Acid Digestion of Solid Waste
Standard Practice for Nitric Acid Digestion of Solid Waste
SIGNIFICANCE AND USE
A knowledge of the inorganic composition of a waste is often required for the selection of appropriate waste disposal practices. Solid waste may exist in a variety of forms and contain a range of organic and inorganic constituents. This practice describes a digestion procedure which dissolves many of the toxic inorganic constituents and produces a solution suitable for determination by such techniques as atomic absorption spectroscopy, atomic emission spectroscopy, and so forth. The relatively large sample size aids representative sampling of heterogenous wastes. The relatively small dilution factor allows lower detection limits than most other sample digestion methods. Volatile metals, such as lead and mercury, are not lost during this digestion procedure, however organo-lead and organo-mercury may not be completely digested. Hydride-forming elements, such as arsenic and selenium, may be partially lost. Samples with total metal contents greater than 5 % may give low results. The analyst is responsible for determining whether this practice is applicable to the solid waste being tested.
SCOPE
1.1 This practice describes the digestion of solid waste using nitric acid for the subsequent determination of inorganic constituents by plasma emission spectroscopy or atomic absorption spectroscopy.
1.2 The following elements may be solubilized by this practice:
aluminummanganese berylliummercury cadmiumnickel chromiumphosphorus coppervanadium ironzinc lead
1.3 This practice is to be used when the concentrations of total recoverable elements are to be determined from a waste sample. Total recoverable elements may or may not be equivalent to total elements, depending on the element sought and the sample matrix. Recovery from refractory sample matrices, such as soils, is usually significantly less than total concentrations of the elements present.
Note 1—This practice has been used successfully for oily sludges and a municipal digested sludge standard [Environmental Protection Agency (EPA) Sample No. 397]. The practice may be applicable to some elements not listed above, such as arsenic, barium, selenium, cobalt, magnesium, and calcium. Refractory elements such as silicon, silver, and titanium, as well as organo-mercury are not solubilized by this practice.
1.4 This practice has been divided into two methods, A and B, to account for the advent of digestion blocks. Method A utilizes an electric hot plate; Method B utilizes an electric digestion block.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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. For specific hazard statements, see Section 7.
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Designation: D5198 − 09
Standard Practice for
1
Nitric Acid Digestion of Solid Waste
This standard is issued under the fixed designation D5198; 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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
1.1 This practice describes the digestion of solid waste
statements, see Section 7.
using nitric acid for the subsequent determination of inorganic
constituents by plasma emission spectroscopy or atomic ab-
2. Referenced Documents
sorption spectroscopy.
2
2.1 ASTM Standards:
1.2 The following elements may be solubilized by this
D1193 Specification for Reagent Water
practice:
aluminum manganese 3. Summary of Practice
beryllium mercury
3.1 A weighed portion of the waste sample is mixed with
cadmium nickel
chromium phosphorus
1 + 1 nitric acid (HNO ) in an Erlenmeyer flask. The flask is
3
copper vanadium
heatedfor2hat90to95°Ctodissolvetheelementsofinterest.
iron zinc
After cooling, the contents of the flask are diluted with reagent
lead
water and filtered, and the filtrate is made up to appropriate
1.3 This practice is to be used when the concentrations of
volume for subsequent analysis.
total recoverable elements are to be determined from a waste
sample. Total recoverable elements may or may not be equiva-
4. Significance and Use
lent to total elements, depending on the element sought and the
4.1 Aknowledge of the inorganic composition of a waste is
sample matrix. Recovery from refractory sample matrices,
often required for the selection of appropriate waste disposal
such as soils, is usually significantly less than total concentra-
practices. Solid waste may exist in a variety of forms and
tions of the elements present.
contain a range of organic and inorganic constituents. This
NOTE 1—This practice has been used successfully for oily sludges and
practice describes a digestion procedure which dissolves many
a municipal digested sludge standard [Environmental Protection Agency
of the toxic inorganic constituents and produces a solution
(EPA) Sample No. 397].The practice may be applicable to some elements
suitable for determination by such techniques as atomic ab-
not listed above, such as arsenic, barium, selenium, cobalt, magnesium,
and calcium. Refractory elements such as silicon, silver, and titanium, as sorption spectroscopy, atomic emission spectroscopy, and so
well as organo-mercury are not solubilized by this practice.
forth. The relatively large sample size aids representative
sampling of heterogenous wastes. The relatively small dilution
1.4 This practice has been divided into two methods,Aand
B, to account for the advent of digestion blocks. Method A factor allows lower detection limits than most other sample
digestion methods. Volatile metals, such as lead and mercury,
utilizes an electric hot plate; Method B utilizes an electric
digestion block. are not lost during this digestion procedure, however organo-
lead and organo-mercury may not be completely digested.
1.5 The values stated in SI units are to be regarded as
Hydride-forming elements, such as arsenic and selenium, may
standard. No other units of measurement are included in this
be partially lost. Samples with total metal contents greater than
standard.
5 % may give low results. The analyst is responsible for
1.6 This standard does not purport to address all of the
determining whether this practice is applicable to the solid
safety concerns, if any, associated with its use. It is the
waste being tested.
responsibility of the user of this standard to establish appro-
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on
2
Analytical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2009. Published March 2009. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2003 as D5198 – 92 (2003). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5198-09. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5198 − 09
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D5198 − 09
METHOD A – HOT PLATE
5. Apparatus
5.1 Analytical Balance, capable of weighing to 0.01 g. 7. Hazards
7.1 Add the nitric acid mi
...
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:D5198–92(Reapproved 2003) Designation:D5198–09
Standard Practice for
1
Nitric Acid Digestion of Solid Waste
This standard is issued under the fixed designation D 5198; 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 practice describes the digestion of solid waste using nitric acid for the subsequent determination of inorganic
constituents by argon plasma emission spectroscopy or atomic absorption spectroscopy.
1.2 The following elements may be solubilized by this practice:
aluminum manganese
beryllium mercury
cadmium nickel
chromium phosphorus
copper vanadium
iron zinc
lead
1.3 This practice is to be used when the concentrations of total recoverable elements are to be determined from a waste sample.
Total recoverable elements may or may not be equivalent to total elements, depending on the element sought and the sample
matrix. Recovery from refractory sample matrices, such as soils, is usually significantly less than total concentrations of the
elements present.
NOTE1—This practice has been used successfully for oily sludges and a municipal digested sludge standard [Environmental ProtectionAgency (EPA)
Sample No. 397]. The practice may be applicable to some elements not listed above, such as arsenic, barium, selenium, cobalt, magnesium, and calcium.
Refractory elements such as silicon, silver, and titanium are not solubilized by this practice.
1.4 1—This practice has been used successfully for oily sludges and a municipal digested sludge standard [Environmental
Protection Agency (EPA) Sample No. 397]. The practice may be applicable to some elements not listed above, such as arsenic,
barium, selenium, cobalt, magnesium, and calcium. Refractory elements such as silicon, silver, and titanium, as well as
organo-mercury are not solubilized by this practice.
1.4 This practice has been divided into two methods,Aand B, to account for the advent of digestion blocks. MethodAutilizes
an electric hot plate; Method B utilizes an electric digestion block.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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. For specific hazard statements, see Section 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of Applicable Methods of Committee D19 on Water
D3223Test Method for Total Mercury in Water
D3682Test Method for Major and Minor Elements in Combustion Residues from Coal Utilization Processes
D3919Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
D4503Practice for Dissolution of Solid Waste by Lithium Metaborate Fusion
D4698Practice for Total Digestion of Sediment Samples for Chemical Analysis of Various Metals
E50Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related Materials
Specification for Reagent Water
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved Apr. 10, 2003. Published June 2003. Originally approved in 1992. Last previous edition approved in 1997 as D5198–92 (1997).
Current edition approved Feb. 1, 2009. Published March 2009. Originally approved in 1992. Last previous edition approved in 2003 as D 5198 – 92 (2003).
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D5198–09
3. Summary of Practice
3.1 Aweighed portion of the waste sample is mixed with 1 + 1 nitric acid (HNO ) in an Erlenmeyer flask. The flask is heated
3
for2hat90to 95°C to dissolve the eleme
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