ASTM D5513-99(2009)

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 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 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 feedstream 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.
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: 30-Jun-2009
• ICS: 25.180.10 - Electric furnaces
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Relations

• Replaces: ASTM D5513-99(2004) - 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: 01-Jul-2009

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 (Reapproved2009)
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 (´) 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 feedstream material is com-
gestionoftypicalindustrialfurnacefeedstreammaterialsusing bined 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 previously listed.
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
is performing total metals analysis on all feedstream materials.
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-
40CFR266,SubpartH,HazardousWasteBurnedinBoilers
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
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
federal or state standards, or both, for microwave leakage.The
Analytical Methods.
user must follow specific manufacturer’s instructions for sys-
Current edition approved July 1, 2009. Published August 2009. Originally
tem installation.
approved in 1994. Last previous edition approved in 2004 as D5513–99 (2004).
DOI: 10.1520/D5513-99R09.
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 delivers 1000 W of power at 100%
Standards volume information, refer to the standard’s Document Summary page on
output. The lined digestion vessels consist of a high-strength polymeric
the ASTM website.
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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5513 − 99 (2009)
psig. There are a number of suitable lab grade microwave systems
chemical goggles are required for handling. See MSDS for
available to the user that meet these minimum specifications. The user
additional information.
must follow specific manufacturer’s instructions for using digestion
7.5 Some samples undergoing microwave digestion can
vessels.
exhibit a rapid pressure rise within the digestion vessel. The
5.2 Analytical Balance—Capable of weighing to 0.001 g.
potential exists for this type of sample to rupture the rupture
5.3 Labware—High-density volumetric polyethylene or
membrane and liberate corrosive gases. Because of this, the
polypropylene flasks/sample containers are recommended for
microwave unit must be vented to a fume hood for proper
this practice. The user should be mindful of the quality
evacuation of vapors.
limitations associated with volumetric non-glass labware.
8. Sample
6. Reagents and Materials
8.1 Although feedstream materials are generally pulverized
6.1 Purity of Reagents—Reagent grade chemicals shall be
powders or liquids, the homogeneity of some feedstream
used in all tests. Unless otherwise indicated, it is intended that
materials can be uncertain. The laboratory sample should be
all reagents conform to the specifications of the Committee on
thoroughly mixed or homogenized prior to withdrawing a
Analytical Reagents of theAmerican Chemical Society where
portion for analysis. This practice assumes that non-liquid
such specifications are available. Other grades may be used,
feedstreams are pulverized powders at the time of sample
provided it is first ascertained that the reagent is of sufficiently
preparation.
high purity to permit its use without lessening the accuracy of
NOTE 2—If a non-liquid feedstream material is not in the form of a
the determination.
pulverized powder, it may need to be reduced in particle size to pass
through a No. 100 sieve.
6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean meeting the numerical
9. Calibration and Standardization
requirements of Type II water as defined by Specifications
9.1 Although equipment manufacturers specify general
D1193.
power output ratings for microwave digestion units, it is
6.3 Boric Acid Solution (20 g/L)—Dissolve 20 g of boric
importanttoverifytheactualpoweroutputofaspecificunit.It
acid (H BO ) in water and dilute to 1 L. It may be necessary
3 3
is recommended that this microwave power check procedure
to place solution on a combination hot plate/magnetic stirrer
be performed monthly.
and with the aid of a stir bar, allow the solution to mix under
9.1.1 Power Check Procedure at 100 % Instrument Power:
gentle heat until boric acid is fully in solution.
9.1.1.1 Remove from the instrument cavity the turntable,
6.4 Hydrochloric Acid, 37%, (sp. gr. 1.200), HCl.
drive lug, and all vessels.
9.1.1.2 Adjusttheinstrumentcavityexhausttominimumair
6.5 Hydrofluoric Acid, 48%, (sp. gr. 1.150), HF.
flow (refer to the manufacturer’s instructions).
6.6 Nitric Acid, 70%, (sp. gr. 1.400), HNO .
9.1.1.3 Program the instrument for 4-min time and 100%
power.
7. Hazards
9.1.1.4 Transfer 2000 6 2 mL of room temperature (19 to
7.1 It is recommended that all operations involving concen-
25°C) water into a 2-L polypropylene beaker.
trated acids be performed in a laboratory fume hood.
9.1.1.5 Measureandrecordtheinitialwatertemperature(T)
i
to the nearest 0.1°C.
7.2 Hydrochloric acid is a highly corrosive chemical that is
9.1.1.6 Place the beaker in the right front corner of the
reactive with metals and most alkaline chemicals. Impervious
instrumentcavity(asyoufacethefrontoftheinstrument).This
gloves and chemical goggles are required for handling. See
positioncloselyapproximatesthepositionofadigestionvessel
material safety data sheet (MSDS) for additional information.
during processing.
7.3 Hydrofluoric acid is a highly corrosive chemical that is
9.1.1.7 Heat the water for the programmed time.
reactive with metals and water or steam. Additionally, HF
9.1.1.8 When the heating cycle is complete, immediately
specifically attacks silicate glass making certain fume hood
removethebeakerfromthecavity,thoroughlystirthewaterto
enclosures susceptible to damage. Impervious gloves and
ensure even heat distribution, and measure the final tempera-
chemical goggles are required for handling. See MSDS for
ture (T) to the nearest 0.1°C.
f
additional information.
9.1.1.9 Calculate the delivered power in accordance with
7.4 Nitricacidisahighlycorrosivechemicalthatisreactive
the following equations:
withmetalsandmostorganicmaterials.Imperviousglovesand
Power watts 5 ∆T 3 35 W/°C (1)
~ ! ~ !
where:
Reagent Chemicals, American Chemical Society Specifications, American
∆T = T − T.
f i
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
W/°C =
K 3 Cp 3 M
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia t
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. where:
This information taken from the NIOSH Guide to Chemical Hazards, U.S.
W = watts,
Depart. of Health and Human Services, June 1990.
D5513 − 99 (2009)
10.1.9 Following the cooling step (0 power) in Stage 1, the
K = 4.2, the factor for converting thermo-chemical
vessels should be cool to the touch. Additional cooling time
calories/s to joules to watts.
−1 −1
may be necessary if vessels remain hot. Vent the vessels in a
Cp = 1.0, the heat capacity for water, cal g de
...