ASTM D5513-15

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

SIGNIFICANCE AND USE
4.1 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, flyash, 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 units of measurement are included in this standard.  
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.

General Information

• Status: Historical
• Publication Date: 31-Aug-2015
• ICS: 25.180.10 - Electric furnaces
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5513 − 15
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 3. Summary of Practice
1.1 This practice describes the multi-stage microwave di- 3.1 A weighed portion of the feed stream material is
gestionoftypicalindustrialfurnacefeedstreammaterialsusing combined with concentrated nitric acid in a
nitric, hydrofluoric, hydrochloric, and boric acids for the polytetrafluoroethylene-lined digestion vessel, and heated in a
subsequent determination of trace metals. microwave digestion unit. Following a programmed heating
cycle, the vessel is vented and specified quantities of hydro-
1.2 This practice has been used successfully on samples of
fluoric and hydrochloric acids are added, and the mixture
coal, coke, cement raw feed materials, and waste-derived fuels
undergoes further microwave heating. Following this heating
composed primarily of waste paint-related material in prepa-
cycle,thevesselisventedandaspecifiedquantityofboricacid
ration for measuring the following trace elements:Ag,As, Ba,
solutionisadded,andthemixtureundergoesafinalmicrowave
Be,Cd,Cr,Hg,Pb,Sb,andTl.Thispracticemaybeapplicable
heating.Followingthisfinalheatingcycle,thevesselisvented,
to elements not listed above.
the contents are quantitatively transferred to a volumetric flask
1.3 This practice is also effective for other waste materials
and brought to volume. Typically, the only undissolved mate-
(for example, flyash, foundry sand, alum process residue,
rial is particulate carbon. If particulate matter is observed,
cement kiln dust, etc.).
filtrationorcentrifugationmaybeneeded.Thedigestedsample
is ready for analysis.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.
4.1 The U.S. Environmental Protection Agency
1.5 This standard does not purport to address all of the
Regulations, 40 CFR 266, require that boilers, cement kilns,
safety concerns, if any, associated with its use. It is the
and other industrial furnaces utilizing waste-derived fuel ad-
responsibility of the user of this standard to establish appro-
here to specific guidelines in assessing potential metals emis-
priate safety and health practices and determine the applica-
sions. A common approach for estimating potential emissions
bility of regulatory limitations prior to use. Specific hazard
isperformingtotalmetalsanalysisonallfeedstreammaterials.
statements are given in Section 7.
This practice describes a multi-stage microwave-assisted di-
2. Referenced Documents gestion procedure that solubilizes trace elements for spectro-
2 scopic analyses.
2.1 ASTM Standards:
D1193Specification for Reagent Water
5. Apparatus
2.2 Other Document:
5.1 Microwave Digestion Unit—Equipped with an auto-
40 CFR 266Subpart H, HazardousWaste Burned in Boilers
3 matic turntable, pressure and/or temperature controller, and
and Industrial Furnaces, Latest Revision
closed perfluoroalkoxy (PFA)-lined digestion vessels equipped
with pressure relief/rupture membrane fittings or equivalent
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste
pressure relief device.The unit should comply with applicable
Management and is the direct responsibility of Subcommittee D34.01.06 on
regional, federal, or state standards for microwave leakage.
Analytical Methods.
The user must follow specific manufacturer’s instructions for
Current edition approved Sept. 1, 2015. Published September 2015. Originally
system installation.
approved in 1994. Last previous edition approved in 2009 as D5513–99 (2009).
DOI: 10.1520/D5513-15.
2 NOTE 1—The digestion unit used in developing this practice was
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
equipped with a pressure controller, automatic turntable, exhaust fan, and
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
programming capacity. The unit delivered 1000 W of power at 100%
Standards volume information, refer to the standard’s Document Summary page on
output.The lined digestion vessels consisted of a high-strength polymeric
the ASTM website.
3
AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700 vessel body and cap, inner PFAliner and rupture membrane housing, and
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. PFAvent stem.These vessels have a maximum operating pressure of 200
Copyright © ASTM International, 1
...

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 − 99 (Reapproved 2009) D5513 − 15
Standard Practice for
Microwave Digestion of Industrial Furnace Feedstreams
1
Feed Streams 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 feedstream 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 previously listed.listed above.
1.3 This practice is also effective for other waste materials (for example, flyash, 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 units of measurement are included in this standard.
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
2.2 Other Document:
3
40 CFR 266 , Subpart H, Hazardous Waste Burned in Boilers and Industrial Furnaces, Latest Revision
3. Summary of Practice
3.1 A weighed portion of the feedstream 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.
4. Significance and Use
4.1 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 feedstream feed stream materials. This
practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
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 July 1, 2009Sept. 1, 2015. Published August 2009September 2015. Originally approved in 1994. Last previous edition approved in 20042009
as D5513 – 99 (2004).(2009). DOI: 10.1520/D5513-99R09.10.1520/D5513-15.
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

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D5513 − 15
5. Apparatus
5.1 Microwave Digestion Unit—Equipped with an automatic turntable, pressure and/or temperature controller, and closed
perfluoroalkoxy (PFA)-lined digestion vessels equipped with pressure relief/rupture membr
...