ASTM D8213-18

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: D8213 − 18
Standard Test Method for
Determination of Boron in Coal
This standard is issued under the fixed designation D8213; 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 Emission Spectrometry, Inductively Coupled Plasma
Mass Spectrometry, and Graphite Furnace Atomic Ab
1.1 This test method describes a procedure for the analysis
E144 Practice for Safe Use of Oxygen Combustion Vessels
of total boron in coal.
E177 Practice for Use of the Terms Precision and Bias in
1.2 Units—The values stated in SI units are to be regarded
ASTM Test Methods
as standard. The values given in parentheses after SI units are
E691 Practice for Conducting an Interlaboratory Study to
provided for information only and are not considered standard.
Determine the Precision of a Test Method
1.3 This standard does not purport to address all of the
2.2 SAI Standard:
safety concerns, if any, associated with its use. It is the
AS 1038.10.3 Coal and Coke—Analysis and Testing, Part
responsibility of the user of this standard to establish appro-
10.3: Determination of Trace Elements—Coal and
priate safety, health, and environmental practices and deter-
Coke—Determination of Boron Content—ICP-AES
mine the applicability of regulatory limitations prior to use.
Method
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3. Terminology
ization established in the Decision on Principles for the
3.1 Definitions—Definitions applicable to these test meth-
Development of International Standards, Guides and Recom-
ods are listed in Terminology D121.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4. Summary of Test Method
4.1 Total boron is determined following one of five test
2. Referenced Documents
preparation procedures:
2.1 ASTM Standards:
4.1.1 Procedure A—The coal or coke to be analyzed is
D121 Terminology of Coal and Coke
combusted in a vessel with dilute nitric acid absorbing the
D1193 Specification for Reagent Water
boron vapors. The combustion vessel is rinsed into a vessel
D2013 Practice for Preparing Coal Samples for Analysis
with dilute nitric acid.
D3180 Practice for Calculating Coal and Coke Analyses
4.1.2 Procedure B—The coal or coke to be analyzed is
from As-Determined to Different Bases
ashed under controlled conditions. The residue is digested by
D5865 Test Method for Gross Calorific Value of Coal and
aqua-regia, and dissolved in 1 % nitric acid.
Coke
4.1.3 Procedure C—The coal or coke to be analyzed is
D6349 Test Method for Determination of Major and Minor
ashed under controlled conditions. The residue is digested in a
Elements in Coal, Coke, and Solid Residues from Com-
mixture of hydrofluoric, nitric, and hydrochloric acids.
bustion of Coal and Coke by Inductively Coupled
4.1.4 Procedure D—Following AS 1038.10.3, the coal or
Plasma—Atomic Emission Spectrometry
coke to be analyzed is ignited at 800 °C with Eschka mixture.
D6357 TestMethodsforDeterminationofTraceElementsin
The residue is dissolved in dilute hydrochloric acid.
Coal, Coke, and Combustion Residues from Coal Utiliza-
4.1.5 Procedure E—The coal or coke to be analyzed is
tion Processes by Inductively Coupled Plasma Atomic
digested using a microwave system following manufacturer’s
recommendation for temperatures, power, and time, using
either the acid mixtures specified in Test Methods D6357 or
This test method is under the jurisdiction of ASTM Committee D05 on Coal
Test Method D6349, depending upon instrument capabilities.
and Coke and is the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal. 4.1.6 Combustion residues are digested on an as-received
Current edition approved Dec. 1, 2018. Published February 2019. DOI: 10.1520/
basis.
D8213-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from SAI Global, Level 37, 680 George Street, Sydney NSW 2000,
the ASTM website. Australia, https://www.saiglobal.com/.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8213 − 18
4.1.7 The concentration of boron is determined by either 6.3.4 Teflon Beakers—Refer to 6.6 (Teflon Beakers) of Test
inductively coupled atomic emission spectrometry (ICPAES) Methods D6357.
or inductively coupled plasma mass spectrometry (ICPMS). 6.3.5 Hot Plate—Refer to 6.7 (Hot Plate) of Test Methods
Selected elements that occur at concentrations below the D6357.
detection limits of ICPAES can be quantitatively analyzed by 6.3.6 Volumetric Flasks—Refer to 6.8 (Volumetric Flasks)
graphite furnace atomic absorption spectrometry (GFAAS). of Test Methods D6357.
6.3.7 HDPE Bottles—Refer to 6.9 (HDPE Bottles) of Test
5. Significance and Use
Methods D6357.
5.1 The possible emission of boron that may be found in
6.3.8 Crucibles—Refer to 6.10 (Crucibles) of Test Methods
coal from coal combustion is an environmental concern.
D6357.
5.2 When test portions are burned according to this
6.4 Procedure C:
procedure, the total boron is quantitatively retained and is
6.4.1 Spectrometer—Refer to 6.1 (Inductively Coupled
representative of concentrations in the whole coal.
Plasma Atomic Emission Spectrometer (ICPAES)) or 6.2 (In-
ductively Coupled Plasma Mass Spectrometer (ICPMS))of
6. Apparatus
Test Methods D6357.
6.1 Balance—capable of weighing the analysis sample to
6.4.2 Argon Gas Supply, high purity (99.99 %).
the nearest 0.1 mg.
6.4.3 Muffle Furnace—Refer to 6.4 (Muffle Furnace) ofTest
Methods D6357.
6.2 Procedure A:
6.4.4 Crucibles—Refer to 6.10 (Crucibles) of Test Methods
6.2.1 Combustion Vessel, constructed of materials that are
D6357.
not affected by the combustion process or products. The vessel
6.4.5 Stirring Hotplate and Bars—Refer to 7.5 (Stirring
must be designed so that all liquid combustion products can be
Hotplate and Bars) of Test Method D6349.
quantitatively recovered by washing the inner surfaces. There
6.4.6 Polycarbonate Bottles—Refer to 7.6 (Polycarbonate
must be no gas leakage during the test. The vessel must be
Bottles) of Test Method D6349.
capable of withstanding a hydrostatic-pressure test to approxi-
mately 20 MPa at room temperature without stressing any part
6.5 Procedure D:
beyond its elastic limit.
6.5.1 Refer to Section 7 (Apparatus) of AS 1038.10.3.
6.2.2 Water Bath—A container large enough to hold the
6.6 Procedure E:
combustion vessel and enough cooling water to dissipate the
6.6.1 Spectrometer—Refer to 6.1 (Inductively Coupled
heat generated during the combustion process. The container
Plasma Atomic Emission Spectrometer (ICPAES)) or 6.2 (In-
shall be designed to allow a constant flow of water around the
ductively Coupled Plasma Mass Spectrometer (ICPMS))of
combustion vessel.
Test Methods D6357.
6.2.3 Combustion Crucibles—Samplesshallbeburnedinan
6.6.2 Argon Gas Supply, high purity (99.99 %).
open crucible of platinum, quartz, or acceptable base-metal
6.6.3 Microwave Sample Preparation System—Capable of
alloy.
rapid heating of the sample at high pressures.
6.2.4 Firing Wire,100 mm,nickel-chromiumalloy,No.34B
6.6.4 High Pressure Digestion Vessel—Closed vessel, ca-
& S gauge, or platinum, No. 34 or No. 38B & S gauge.
pable of withstanding the temperatures and pressures selected,
6.2.5 Firing Circuit—A 6 V to 16 V alternating or direct
and suitable for use with the acid mixture selected.
current is required for ignition purposes with an ammeter or
pilot light in the circuit to indicate when current is flowing. A
7. Reagents
step-down transformer connected to an alternating-current
7.1 Purity of Reagents—Allacidsusedinthesetestmethods
lighting circuit or batteries can be used. (Warning—The
must be trace metal purity grade or equivalent. Redistilled
ignition circuit switch shall be of the momentary double-
acids are acceptable.
contact type, normally open, except when held closed by the
7.2 Purity of Water—The purity of the water used in these
operator. The switch should be depressed only long enough to
test methods shall be equivalent to ASTM Type II reagent
fire the charge.)
water of Specification D1193.
6.2.6 Spectrometer—Refer to 6.1 (Inductively Coupled
Plasma Atomic Emission Spectrometer (ICPAES)) or 6.2 (In-
7.3 Calibration Standards—Aqueous single-element solu-
ductively Coupled Plasma Mass Spectrometer (ICPMS))of
tions made up in 10 % HNO are used for calibration of
Test Methods D6357.
ICPAES and ICPMS systems.The standards may be purchased
6.2.7 Argon Gas Supply, high purity (99.99 %).
or prepared from high-purity grade chemicals or metals.
6.3 Procedure B:
7.4 Boron Stock Standard Solution (1000 ppm)—Single-
6.3.1 Spectrometer—Refer to 6.1 (Inductively Coupled
element standards either purchased or prepared from high
Plasma Atomic Emission Spectrometer (ICPAES)) or 6.2 (In-
purity grade chemicals or metals.
ductively Coupled Plasma Mass Spectrometer (ICPMS))of
7.5 Nitric Acid (1+9)—Dilute 100 mLof concentrated nitric
Test Methods D6357.
acid (HNO , sp gr 1.42) to 1 L with water.
6.3.2 Argon Gas Supply, high purity (99.99 %).
6.3.3 Muffle Furnace—Refer to 6.4 (Muffle Furnace) ofTest 7.6 Blank Solutions—Allofthetestmethodsinthisstandard
Methods D6357. require two types of blank solutions.Acalibration blank that is
D8213 − 18
used to establish the analytical calibration curve and a method recommended for safe operations in the use of the oxygen
blank which is used to evaluate possible contamination and combustion vessel. Additional precautions are given in Rec-
assess spectral background. ommended Practice E144, for use of oxygen combustion
7.6.1 Calibration Blank—A 1 % nitric acid solution. vessels.)
7.6.2 Method Blank—Consists of all the reagents in the
10.1.4.1 The mass of coal sample and the pressure of the
same volumes as used in preparing the samples. The method
oxygen admitted to the vessel must not exceed the vessel
blank shall be processed through the entire sample digestion
manufacturer’s recommendation.
scheme.
10.1.4.2 Inspect the vessel parts carefully after each use.
Frequently check the threads on the main closure for wear.
7.7 Procedure A:
Replace the cracked or significantly worn parts. Return the
7.7.1 Oxygen—Manufactured from liquid air, guaranteed to
vessel to the manufacturer occasionally for inspection and
be greater than 99.5 % pure, and free of combustible matter.
possibly proof testing.
Oxygen made by the electrolytic process contains small
10.1.4.3 The oxygen supply cylinder should be equipped
amounts of hydrogen rendering it unfit unless purified by
with an approved type of safety device, such as a reducing
passage over copper oxide at 500 °C.
valve, in addition to the needle valve and pressure gauge used
7.8 Procedure B:
in regulating the oxygen feed to the vessel.Valves, gauges, and
7.8.1 Aqua Regia Solution—Refer to 7.3 (Aqua Regia So-
gaskets must meet industry safety code. Suitable reducing
lution) of Test Methods D6357.
valves and adaptors for approximately 3.0 MPa to 5.0 MPa
7.9 Procedure C:
discharge pressure are obtainable from commercial sources of
7.9.1 Mixed Acid Solution, 70/30 HCl/HF—Refer to 8.5.5
compressed-gas equipment. Check the pressure gauge periodi-
(Mixed Acid Solution, 70/30 HCl/HF) of Test Method D6349.
cally for accuracy.
10.1.4.4 During ignition of a sample, the operator must not
7.10 Procedure D:
permit any portion of his body to extend over the combustion
7.10.1 Refer to Section 6 (Reagents) of AS 1038.10.3.
vessel or its container.
7.11 Procedure E:
10.1.4.5 Exercise extreme caution when combustion aids
7.11.1 Hydrochloric Acid
are employed so as not to exceed the vessel manufacturer’s
7.11.2 Hydrofluoric Acid
recommendations and to avoid damage to the vessel.
7.11.3 Nitric Acid
10.1.4.6 Admit oxygen slowly into the vessel to avoid
blowing powdered material from the crucible.
8. Hazards
10.1.4.7 Do not fire the vessel if it has been filled to greater
8.1 Procedure A: Refer to Section 8 (Hazards) of Test
3.0 MPa pressure with oxygen, if the vessel has been dropped
Method D5865.
orturnedoverafterloading,orifthereisevidenceofagasleak
when the vessel is submerged in the water bath.
9. Sample
10.1.5 Place the vessel in a cooling water bath, with water
9.1 The analysis sample is the material pulverized to pass
moving. Attach the ignition wires from the firing circuits, and
250 µm (No. 60) sieve, prepared in accordance with Practice
ignite the sample. Allow the vessel to remain in the cooling
D2013.
water for 15 min to allow cooling and absorption of soluble
vapors within the vessel.
10. Test Solution Preparation
10.1.6 Remove the vessel and release the pressure at a
uniform rate, such that the operation will require not less than
10.1 Procedure A: Vessel Combustion
2 min. Examine the vessel interior and discard the test if
10.1.1 Thoroughly mix the analysis sample of coal. Care-
unburned or sooty deposits are found.
fullyweighapproximately1 g 60.2 gintoapreviouslyignited
10.1.7 Quantitatively rinse the vessel, electrodes, and cru-
crucible in which it is to be combusted.
cible into the vessel with several small portions of HNO
10.1.2 For samples in excess of 5 % sulfur, the mass of coal
(1+9). Dilute the contents of the vessel with HNO (1+9) to a
must be reduced to 0.5 g 6 0.1 g to ensure that all the acidic
total volume of 50 mL or 100 mL.
vapors produced in the combustion process are quantitatively
retained in solution. 10.1.8 Prepare a method blank with each batch of samples
10.1.3 Transfer 10 mL of HNO (1+9) to the combustion to be analyzed.
vessel. Attach the fuse wire to the vessel electrodes. Place the
10.2 Procedure B: D6357 (Ashing) and Modified D6357
crucible with the sample into the electrode support of the
(Diss
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