ASTM D5513-22

Standard Practice for Microwave Digestion of Industrial Furnace Feed Streams and Waste for Trace Element Analysis

SIGNIFICANCE AND USE
5.1 The U.S. Environmental Protection Agency Regulations, 40 CFR 266, require that boilers, cement kilns, and other industrial furnaces utilizing waste-derived fuel adhere to specific guidelines in assessing potential metals emissions. A common approach for estimating potential emissions is performing total metals analysis on all feed stream materials. This practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
SCOPE
1.1 This practice describes the multi-stage microwave digestion of typical industrial furnace feed stream materials using nitric, hydrofluoric, hydrochloric, and boric acids for the subsequent determination of trace metals.  
1.2 This practice has been used successfully on samples of coal, coke, cement raw feed materials, and waste-derived fuels composed primarily of waste paint-related material in preparation for measuring the following trace elements: Ag, As, Ba, Be, Cd, Cr, Hg, Pb, Sb, and Tl. This practice may be applicable to elements not listed above.  
1.3 This practice is also effective for other waste materials (for example, fly ash, foundry sand, alum process residue, cement kiln dust, etc.).  
1.4 The values stated in SI units are to be regarded as standard. Other units of measurement in parentheses in this standard are informational.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 8.  
1.6 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.

General Information

• Status: Published
• Publication Date: 30-Sep-2022
• ICS: 25.180.10 - Electric furnaces
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

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: D5513 − 22
Standard Practice for
Microwave Digestion of Industrial Furnace Feed Streams
1
and Waste for Trace Element Analysis
This standard is issued under the fixed designation D5513; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This practice describes the multi-stage microwave di-
D1193Specification for Reagent Water
gestionoftypicalindustrialfurnacefeedstreammaterialsusing
D5681Terminology for Waste and Waste Management
nitric, hydrofluoric, hydrochloric, and boric acids for the
2.2 Other Document:
subsequent determination of trace metals.
40 CFR 266Subpart H, HazardousWaste Burned in Boilers
3
1.2 This practice has been used successfully on samples of
and Industrial Furnaces, Latest Revision
coal, coke, cement raw feed materials, and waste-derived fuels
3. Terminology
composed primarily of waste paint-related material in prepa-
ration for measuring the following trace elements:Ag,As, Ba,
3.1 For definitions of terms used in this practice, refer to
Be,Cd,Cr,Hg,Pb,Sb,andTl.Thispracticemaybeapplicable
Terminology D5681.
to elements not listed above.
4. Summary of Practice
1.3 This practice is also effective for other waste materials
4.1 A weighed portion of the feed stream material is
(for example, fly ash, foundry sand, alum process residue,
combined with concentrated nitric acid in a
cement kiln dust, etc.).
polytetrafluoroethylene-lined digestion vessel, and heated in a
microwave digestion unit. Following a programmed heating
1.4 The values stated in SI units are to be regarded as
standard. Other units of measurement in parentheses in this cycle, the vessel is vented and specified quantities of hydro-
fluoric and hydrochloric acids are added, and the mixture
standard are informational.
undergoes further microwave heating. Following this heating
1.5 This standard does not purport to address all of the
cycle,thevesselisventedandaspecifiedquantityofboricacid
safety concerns, if any, associated with its use. It is the
solutionisadded,andthemixtureundergoesafinalmicrowave
responsibility of the user of this standard to establish appro-
heating.Followingthisfinalheatingcycle,thevesselisvented,
priate safety, health, and environmental practices and deter-
thecontentsarequantitativelytransferredtoavolumetricflask,
mine the applicability of regulatory limitations prior to use.
and brought to volume. Typically, the only undissolved mate-
Specific hazard statements are given in Section 8.
rial is particulate carbon. If particulate matter is observed,
1.6 This international standard was developed in accor-
filtrationorcentrifugationmaybeneeded.Thedigestedsample
dance with internationally recognized principles on standard-
is ready for analysis.
ization established in the Decision on Principles for the
5. Significance and Use
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5.1 The U.S. Environmental Protection Agency
Barriers to Trade (TBT) Committee.
Regulations, 40 CFR 266, require that boilers, cement kilns,
and other industrial furnaces utilizing waste-derived fuel ad-
here to specific guidelines in assessing potential metals emis-
sions. A common approach for estimating potential emissions
isperformingtotalmetalsanalysisonallfeedstreammaterials.
1 2
This practice is under the jurisdiction of ASTM Committee D34 on Waste For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Management and is the direct responsibility of Subcommittee D34.01.06 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Analytical Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2022. Published October 2022. Originally the ASTM website.
3
approved in 1994. Last previous edition approved in 2015 as D5513–15. DOI: AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
10.1520/D5513-22. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5513 − 22
5
This practice describes a multi-stage microwave-assisted di- 8. Hazards
gestion procedure that solubilizes trace elements for spectro-
8.1 It is recommended that all operations involving concen-
scopic analy
...

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: D5513 − 15 D5513 − 22
Standard Practice for
Microwave Digestion of Industrial Furnace Feed Streams
1
and Waste for Trace Element Analysis
This standard is issued under the fixed designation D5513; 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 multi-stage microwave digestion of typical industrial furnace feed stream materials using nitric,
hydrofluoric, hydrochloric, and boric acids for the subsequent determination of trace metals.
1.2 This practice has been used successfully on samples of coal, coke, cement raw feed materials, and waste-derived fuels
composed primarily of waste paint-related material in preparation for measuring the following trace elements: Ag, As, Ba, Be, Cd,
Cr, Hg, Pb, Sb, and Tl. This practice may be applicable to elements not listed above.
1.3 This practice is also effective for other waste materials (for example, flyash, fly ash, foundry sand, alum process residue,
cement kiln dust, etc.).
1.4 The values stated in SI units are to be regarded as standard. No other Other units of measurement are includedin parentheses
in this standard.standard are informational.
1.5 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. Specific hazard statements are given in Section 78.
1.6 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
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D5681 Terminology for Waste and Waste Management
2.2 Other Document:
3
40 CFR 266 Subpart H, Hazardous Waste Burned in Boilers and Industrial Furnaces, Latest Revision
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 Sept. 1, 2015Oct. 1, 2022. Published September 2015October 2022. Originally approved in 1994. Last previous edition approved in 20092015
as D5513 – 99 (2009).D5513 – 15. DOI: 10.1520/D5513-15.10.1520/D5513-22.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5513 − 22
3. Terminology
3.1 For definitions of terms used in this practice, refer to Terminology D5681.
4. Summary of Practice
4.1 A weighed portion of the feed stream material is combined with concentrated nitric acid in a polytetrafluoroethylene-lined
digestion vessel, and heated in a microwave digestion unit. Following a programmed heating cycle, the vessel is vented and
specified quantities of hydrofluoric and hydrochloric acids are added, and the mixture undergoes further microwave heating.
Following this heating cycle, the vessel is vented and a specified quantity of boric acid solution is added, and the mixture undergoes
a final microwave heating. Following this final heating cycle, the vessel is vented, the contents are quantitatively transferred to a
volumetric flask, and brought to volume. Typically, the only undissolved material is particulate carbon. If particulate matter is
observed, filtration or centrifugation may be needed. The digested sample is ready for analysis.
5. Significance and Use
5.1 The U.S. Environmental Protection Agency Regulations, 40 CFR 266, require that boilers, cement kilns, and other industrial
furnaces utilizing waste-derived fuel adhere to specific guidelines in assessing potential metals emissions. A com
...