ASTM D5513-99(2004)

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: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Relations

• Replaces: ASTM D5513-99 - Standard Practice for Microwave Digestion of Industrial Furnace Feedstreams and Waste for Trace Element Analysis
• Effective Date: 10-Mar-1999
• Replaced By: ASTM D5513-99(2009) - Standard Practice for Microwave Digestion of Industrial Furnace Feedstreams and Waste for Trace Element Analysis
• Effective Date: 01-Jul-2009
• Referred By: ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
• Effective Date: 10-Mar-1999

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5513–99(Reapproved2004)
Standard Practice for
Microwave Digestion of Industrial Furnace Feedstreams 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 (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
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
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
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 [e-mail]. 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
AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
vessels.
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.
D5513–99 (2004)
5.2 Analytical Balance—Capable of weighing to 0.001 g. 8. Sample
5.3 Labware—High-density volumetric polyethylene or
8.1 Although feedstream materials are generally pulverized
polypropylene flasks/sample containers are recommended for
powders or liquids, the homogeneity of some feedstream
this practice. The user should be mindful of the quality
materials can be uncertain. The laboratory sample should be
limitations associated with volumetric non-glass labware.
thoroughly mixed or homogenized prior to withdrawing a
portion for analysis. This practice assumes that non-liquid
6. Reagents and Materials
feedstreams are pulverized powders at the time of sample
6.1 Purity of Reagents—Reagent grade chemicals shall be
preparation.
used in all tests. Unless otherwise indicated, it is intended that
NOTE 2—If a non-liquid feedstream material is not in the form of a
all reagents conform to the specifications of the Committee on
pulverized powder, it may need to be reduced in particle size to pass
Analytical Reagents of theAmerican Chemical Society where
4 through a No. 100 sieve.
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
9. Calibration and Standardization
high purity to permit its use without lessening the accuracy of
9.1 Although equipment manufacturers specify general
the determination.
power output ratings for microwave digestion units, it is
6.2 Purity of Water—Unlessotherwiseindicated,references
importanttoverifytheactualpoweroutputofaspecificunit.It
to water shall be understood to mean meeting the numerical
is recommended that this microwave power check procedure
requirements of Type II water as defined by Specifications
be performed monthly.
D1193.
9.1.1 Power Check Procedure at 100 % Instrument Power:
6.3 Boric Acid Solution (20 g/L)—Dissolve 20 g of boric
9.1.1.1 Remove from the instrument cavity the turntable,
acid (H BO ) in water and dilute to 1 L. It may be necessary
3 3
to place solution on a combination hot plate/magnetic stirrer drive lug, and all vessels.
and with the aid of a stir bar, allow the solution to mix under 9.1.1.2 Adjusttheinstrumentcavityexhausttominimumair
gentle heat until boric acid is fully in solution.
flow (refer to the manufacturer’s instructions).
6.4 Hydrochloric Acid, 37%, (sp. gr. 1.200), HCl.
9.1.1.3 Program the instrument for 4-min time and 100%
6.5 Hydrofluoric Acid, 48%, (sp. gr. 1.150), HF.
power.
6.6 Nitric Acid, 70%, (sp. gr. 1.400), HNO .
3 9.1.1.4 Transfer 2000 6 2 mL of room temperature (19 to
25°C) water into a 2-L polypropylene beaker.
7. Hazards
9.1.1.5 Measureandrecordtheinitialwatertemperature(T)
i
7.1 It is recommended that all operations involving concen-
to the nearest 0.1°C.
trated acids be performed in a laboratory fume hood.
9.1.1.6 Place the beaker in the right front corner of the
7.2 Hydrochloric acid is a highly corrosive chemical that is
instrumentcavity(asyoufacethefrontoftheinstrument).This
reactive with metals and most alkaline chemicals. Impervious
positioncloselyapproximatesthepositionofadigestionvessel
gloves and chemical goggles are required for handling. See
during processing.
material safety data sheet (MSDS) for additional information.
9.1.1.7 Heat the water for the programmed time.
7.3 Hydrofluoric acid is a highly corrosive chemical that is
9.1.1.8 When the heating cycle is complete, immediately
reactive with metals and water or steam. Additionally, HF
removethebeakerfromthecavity,thoroughlystirthewaterto
specifically attacks silicate glass making certain fume hood
ensure even heat distribution, and measure the final tempera-
enclosures susceptible to damage. Impervious gloves and
ture (T) to the nearest 0.1°C.
f
chemical goggles are required for handling. See MSDS for
9.1.1.9 Calculate the delivered power in accordance with
additional information.
the following equations:
7.4 Nitricacidisahighlycorrosivechemicalthatisreactive
Power ~watts!5DT 3 ~35 W/°C! (1)
withmetalsandmostorganicmaterials.Imperviousglovesand
chemical goggles are required for handling. See MSDS for
where:
additional information.
DT = T − T.
f i
7.5 Some samples undergoing microwave digestion can
W/°C = K 3 Cp 3 M
exhibit a rapid pressure rise within the digestion vessel. The
t
potential exists for this type of sample to rupture the rupture
membrane and liberate corrosive gases. Because of this, the
microwave unit must be vented to a fume hood for proper
where:
evacuation of vapors.
W = watts,
K = 4.2, the factor for converting thermo-chemical
calories/s to joules to watts.
Reagent Chemicals, American Chemical Society Specifications, American
−1 −1
Cp = 1.0, the heat capacity for water, cal g degree ,
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
M = mass of water, g (1 mL H O=1 g), and
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
t = time, s.
and National Formulary,U.S.PharmacoepeialConvention,Inc.(USPC),Rockville,
9.1.1.10 If the calculated power is not within the specifica-
MD.
tions of the unit, do a second test beginning at 9.1.1.1 for
This information taken from the NIOSH Guide to Chemical Hazards, U.S.
Depart. of Health and Human Services, June 1990. confirmation before contacting the manufacturer.
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