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

SIGNIFICANCE AND USE
The U.S. Environmental Protection Agency Regulations, 40 CFR, 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 materials. This practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
SCOPE
1.1 This test method covers the biodegradation properties of a material by reproducibly exposing materials to conditions typical of municipal solid waste (MSW) composting. A material is composted under controlled conditions using a synthetic compost matrix and determining the acclimation time, cumulative oxygen uptake, cumulative carbon dioxide production, and percent of theoretical biodegradation over the period of the test. This test method does not establish the suitability of the composted product for any use.
1.2 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
1.3 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.

General Information

Status
Historical
Publication Date
09-Mar-1999
Technical Committee
Current Stage
Ref Project

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ASTM D5513-99(2004) - Standard Practice for Microwave Digestion of Industrial Furnace Feedstreams and Waste for Trace Element Analysis
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5513–99(Reapproved2004)
Standard Practice for
Microwave Digestion of Industrial Furnace Feedstreams and
1
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope microwave digestion unit. Following a programmed heating
cycle, the vessel is vented and specified quantities of hydrof-
1.1 This practice describes the multi-stage microwave di-
luoric and hydrochloric acids are added, and the mixture
gestionoftypicalindustrialfurnacefeedstreammaterialsusing
undergoes further microwave heating. Following this heating
nitric, hydrofluoric, hydrochloric, and boric acids for the
cycle,thevesselisventedandaspecifiedquantityofboricacid
subsequent determination of trace metals.
solutionisadded,andthemixtureundergoesafinalmicrowave
1.2 This practice has been used successfully on samples of
heating.Followingthisfinalheatingcycle,thevesselisvented,
coal, coke, cement raw feed materials, and waste-derived fuels
the contents are quantitatively transferred to a volumetric flask
composed primarily of waste paint-related material in prepa-
and brought to volume. Typically, the only undissolved mate-
ration for measuring the following trace elements:Ag,As, Ba,
rial is particulate carbon. If particulate matter is observed,
Be,Cd,Cr,Hg,Pb,Sb,andTl.Thispracticemaybeapplicable
filtrationorcentrifugationmaybeneeded.Thedigestedsample
to elements not previously listed.
is ready for analysis.
1.3 This practice is also effective for other waste materials
(for example, flyash, foundry sand, alum process residue,
4. Significance and Use
cement kiln dust, etc.).
4.1 The U.S. Environmental Protection Agency Regula-
1.4 This standard does not purport to address all of the
tions, 40 CFR, require that boilers, cement kilns, and other
safety concerns, if any, associated with its use. It is the
industrial furnaces utilizing waste-derived fuel adhere to spe-
responsibility of the user of this standard to establish appro-
cific guidelines in assessing potential metals emissions. A
priate safety and health practices and determine the applica-
common approach for estimating potential emissions is per-
bility of regulatory limitations prior to use. Specific hazard
forming total metals analysis on all feedstream materials. This
statements are given in Section 7.
practice describes a multi-stage microwave-assisted digestion
2. Referenced Documents procedure that solubilizes trace elements for spectroscopic
2
analyses.
2.1 ASTM Standards:
D1193 Specifications for Reagent Water
5. Apparatus
2.2 Other Document:
5.1 Microwave Digestion Unit—Equipped with an auto-
40 CFR 266, Subpart H, Hazardous Waste Burned in
3 matic turntable, pressure and/or temperature controller, and
Boilers and Industrial Furnaces, Latest Revision
closed perfluoroalkoxy (PFA)-lined digestion vessels equipped
3. Summary of Practice with pressure relief/rupture membrane fittings or equivalent
pressure relief device.The unit should comply with applicable
3.1 A weighed portion of the feedstream material is com-
federal or state standards, or both, for microwave leakage.The
bined with concentrated nitric acid in a
user must follow specific manufacturer’s instructions for sys-
polytetrafluoroethylene-lined digestion vessel, and heated in a
tem installation.
NOTE 1—The digestion unit used in developing this practice was
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste
equipped with a pressure controller, automatic turntable, exhaust fan, and
Management and is the direct responsibility of Subcommittee D34.01.06 on
programming capacity. The unit delivers 1000 W of power at 100%
Analytical Methods.
output. The lined digestion vessels consist of a high-strength polymeric
Current edition approved March 10, 1999. Published May 1999. Originally
published as D5513–94. Last previous edition D5513–94 (1998). vessel body and cap, inner PFAliner and rupture membrane housing, and
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
PFAvent stem.These vessels have a maximum operating pressure of 200
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
psig. There are a number of suitable lab grade microwave systems
Standards volume information, refer to the standard’s Document Summary page on
available to the user that meet these minimum specifications. The user
the ASTM website.
must follow specific manufacturer’s instructions for using digestion
3
AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
vessels.
Robbins Ave., Philadelp
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