ASTM D5016-98
(Test Method)Standard Test Method for Sulfur in Ash from Coal, Coke, and Residues from Coal Combustion Using High-Temperature Tube Furnace Combustion Method with Infrared Absorption
Standard Test Method for Sulfur in Ash from Coal, Coke, and Residues from Coal Combustion Using High-Temperature Tube Furnace Combustion Method with Infrared Absorption
SCOPE
1.1 This test method describes a procedure using a high-temperature tube furnace and infrared detection for the rapid determination of sulfur in ash from coal and coke.
1.2 This test method is an alternative for test methods described in Test Methods D1757.
1.3 The values stated in SI units (Practice E380) shall be regarded as the standard.
1.4 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.
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Designation: D 5016 – 98
Standard Test Method for
Sulfur in Ash from Coal, Coke, and Residues from Coal
Combustion Using High-Temperature Tube Furnace
Combustion Method with Infrared Absorption
This standard is issued under the fixed designation D 5016; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope ture of 1350°C in a stream of oxygen (see Note 1). The
combustible sulfur contained in the test portion is oxidized to
1.1 This test method describes a procedure using a high-
gaseous oxides of sulfur. Moisture and particulates are re-
temperature tube furnace and infrared detection for the rapid
moved by traps filled with anhydrous magnesium perchlorate.
determination of sulfur in ash from coal and coke.
The gas stream is passed through a cell in which sulfur dioxide
1.2 This test method is an alternative for test methods
is measured by an infrared absorption detector. Sulfur dioxide
described in Test Methods D 1757.
absorbs IR energy at a precise wavelength within the IR
1.3 The values stated in SI units (Practice E 380) shall be
spectrum. Energy is absorbed as the gas passes through the cell
regarded as the standard.
body in which the IR energy is being transmitted; thus, at the
1.4 This standard does not purport to address all of the
detector, less energy is received. All other IR energy is
safety concerns, if any, associated with its use. It is the
eliminated from reaching the detector by a precise wavelength
responsibility of the user of this standard to establish appro-
filter. The absorption of IR energy can be attributed only to
priate safety and health practices and determine the applica-
sulfur dioxide whose concentration is proportional to the
bility of regulatory limitations prior to use.
change in energy at the detector. One cell is used as both a
2. Referenced Documents reference and a measurement chamber. Total sulfur as sulfur
dioxide is detected on a continuous basis.
2.1 ASTM Standards:
D 1757 Test Methods for Sulfur in Ash from Coal and
NOTE 1—The promoter aids in the quantitative release of all sulfur
Coke
present in the test portion as SO . Refer to the instrument manufacturer’s
recommended procedure for using oxidizing agents or promoters com-
D 2795 Test Methods for Analysis of Coal and Coke Ash
monly referred to as “combustion accelerators.”
D 3174 Test Method for Ash in the Analysis Sample of Coal
and Coke from Coal
3.2 This test method is applicable for use with commercially
D 3682 Test Method for Major and Minor Elements in Coal
available sulfur analyzers equipped to carry out the operations
and Coke Ash by Atomic Absorption
in 3.1 automatically, and must be calibrated using certified
D 4326 Test Method for Major and Minor Elements in Coal
reference materials (CRM’s) covering the range of sulfur in the
and Coke Ash by X-Ray Fluorescence
ash samples being analyzed.
D 4621 Guide for Accountability and Quality Control in the
4. Significance and Use
Coal Analysis Laboratory
D 5142 Test Methods for Proximate Analysis of the Analy-
4.1 The purpose of this test method is to determine the
sis Sample of Coal and Coke by Instrumental Procedures
percent sulfur trioxide (SO ) portion of the major and minor
E 380 Practice for Use of the International System of Units
elements in coal ash.
(SI) (the Modernized Metric System)
4.2 This test method may be used to determine the percent
sulfur trioxide (SO ) portion of ash determined by Test
3. Summary of Test Method
Methods D 3174 or D 5142 for coals containing high amounts
3.1 A weighed test portion is mixed with a promoting agent
of calcium. The ash may then be reported on a sulfur trioxide
and ignited in a tube furnace at a minimum operating tempera-
free basis.
5. Apparatus
This test method is under the jurisdiction of ASTM Committee D-5 on Coal and
5.1 Tube Furnace, electrically heated, capable of heating
Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements in
Ash and Trace Elements of Coal.
150 to 165-mm length of the hot zone area of the combustion
Current edition approved Sept. 10, 1998. Published December 1998. Originally
tube (see 5.2) to at least 1350°C. Specific dimensions can vary
published as D 5016 – 89. Last previous edition D 5016 – 95.
2 with manufacturer’s design.
Annual Book of ASTM Standards. Vol 05.05.
5.2 Combustion Tube, made of mullite, porcelain, or zircon,
Annual Book of ASTM Standards. Vol 14.02.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5016
approximately 23-mm inside diameter with a 3-mm thick wall, 7.3 Certified Reference Materials (CRMs):
at least 450 mm long with means to route the gases produced NIST Coal Fly Ash—SRM 1633b, 2689, 2690, 2691
by combustion through the infrared cell. NIST Cements—SRM 1880, 1881M, 1884, 1885, 1886,
5.3 Sample Combustion Boats, made of iron-free material 1887, 1888, 1889
and of a convenient size suitable for the instrument being used.
8. Procedure
5.4 Boat Puller, rod of a heat resistant material with a bent
8.1 Instrument Preparation—All instrument preparation is
or disk end used to insert and remove boats from the combus-
to be done in accordance with the manufacturer’s instructions.
tion tube.
8.2 Calibration of the Infrared Detection System—Select
6. Reagents
Certified Reference Materials (CRM’s) with known dry-basis
6.1 Purity of Reagents—Reagent grade chemicals shall be
sulfur values in the range of the samples to be analyzed. For the
used unless otherwise specified. All reagents shall conform to
initial calibration and periodic verification of instrument lin-
the specifications of the Committee on Analytical Reagents of
earity, at least three such CRM’s are recommended for each
the American Chemical Society, where such specifications
range of sulfur values to be determined. Two of the CRM’s
exist. Other grades may be used, provided it is first ascertained
should bracket the range of sulfur values to be tested and the
that the reagent is of sufficiently high purity to permit its use
third should be near the mid-point of the expected range. When
without affecting the accuracy of the determination.
performing a single point calibration use a CRM that has a
6.2 Magnesium Perchlorate (Mg(ClO ) )—Warning: Mag-
sulfur value higher than the expected range of the samples to be
4 2
nesium perchlorate is a strong oxidizing agent. Do not attempt
analyzed. Records for all calibrations will be maintained in
to regenerate the absorbent. Do not permit contact with organic
accordance with Guide D 4621.
materials or reducing agents.
8.2.1 Calibration Procedure—Make a minimum of two
6.3 Promotor—Refer to the instrument manufacturer’s rec-
determinations to condition the equipment prior to beginning
ommended combustion accelerator. Suitable combustion accel-
the calibration procedure. The as-determined sulfur value of
erators include vanadium pentoxide, iron powder, and char-
the CRM shall be used for calibration of the system. This value
coal.
must have been previously calculated from the certified dry-
basis sulfur value and residual moisture determined using
NOTE 2—Caution: Some promoters may contain sulfur. The user shall
either Test Methods D 3173, D 5142, or the procedure recom-
determine the sulfur content of the promoter by analyzing it as a sample
and make appropriate corrections in 9.1 based on the mass of the promoter mended by the vendor of the CRM. Alternatively, a quantity of
and its sulfur content.
the CRM can be dried using the previously mentioned proce-
dures for determining moisture, in which case the dry basis
6.4 Oxygen, 99.5 % Pure—Compressed gas contained in a
sulfur value can be used. That quantity of CRM dried for
cylinder equipped with a suitable pressure regu
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