ASTM D1619-99

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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.
Designation: D 1619 – 99
Standard Test Methods for
Carbon Black—Sulfur Content
This standard is issued under the fixed designation D 1619; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 4. Reagents
1.1 These test methods cover the determination of the sulfur 4.1 Purity of Reagents—Reagent grade chemicals shall be
content of carbon black. The following test methods are used in all tests. Unless otherwise indicated, it is intended that
included: all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
Sections
Test Method A High-Temperature Combustion With In- 6to13
where such specifications are available. Other grades may be
frared Absorption Detection Procedures
used, provided it is first ascertained that the reagent is of
Test Method B X-Ray Fluorescence 14
sufficiently high purity to permit its use without lessening the
1.2 The values stated in SI units are to be regarded as
accuracy of the determination.
standard.
4.2 Purity of Water— Unless otherwise indicated, refer-
1.3 This standard does not purport to address all of the
ences to water shall be understood to mean reagent water
safety concerns, if any, associated with its use. It is the
conforming to Specification D 1193.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5. Sampling
bility of regulatory limitations prior to use.
5.1 Samples shall be taken in accordance with Practice
D 1799 or Practice D 1900.
2. Referenced Documents
2.1 ASTM Standards: TEST METHOD A HIGH-TEMPERATURE
D 240 Test Method for Heat of Combustion of Liquid COMBUSTION WITH INFRARED ABSORPTION
Hydrocarbon Fuels by Bomb Calorimeter DETECTION PROCEDURES
D 1193 Specification for Reagent Water
6. Summary of Test Method
D 1509 Test Methods for Carbon Black—Heating Loss
6.1 The specimen is burned in a tube furnace at a minimum
D 1799 Practice for Carbon Black—Sampling Packaged
Shipments operating temperature of 1350°C in a stream of oxygen to
D 1900 Practice for Carbon Black—Sampling Bulk Ship- oxidize the sulfur. Moisture and particulates are removed from
ment the gas by traps filled with anhydrous magnesium perchlorate.
D 4483 Practice for Determining Precision for Test Method The gas stream is passed through a cell in which sulfur dioxide
Standards in the Rubber and Carbon Black Industries is measured by an infrared (IR) absorption detector. Sulfur
E 1 Specification for ASTM Thermometers dioxide absorbs IR energy at a precise wavelength within the
IR spectrum. Energy is absorbed as the gas passes through the
3. Significance and Use
cell body in which the IR energy is being transmitted. Thus, at
3.1 The total sulfur content of a carbon black is useful in the detector, less energy is received. All other IR energy is
calculations for reconstructing a rubber composition from eliminated from reaching the detector by a precise wavelength
analytical data. filter. Thus, the absorption of IR energy can be attributed only
to sulfur dioxide whose concentration is proportional to the
change in energy at the detector. One cell is used as both a
reference and a measurement chamber. Total sulfur as sulfur
These test methods are under the jurisdiction of ASTM Committee D-24 on
dioxide is detected on a continuous basis. This test method is
Carbon Black and are the direct responsibility of Subcommittee D24.31 on
Non-Carbon-Black Components of Carbon Black.
Current edition approved Aug. 10, 1999. Published September 1999. Originally
Reagent Chemicals, American Chemical Society Specifications, American
published as D 1619 – 58 T. Last previous edition D 1619–97.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 05.01.
listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 09.01.
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 14.03.
MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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 1619
NOTE 1—The analytical cycle should begin automatically as soon as
empirical. Therefore, the apparatus must be calibrated by the
sulfur is detected.
use of standard reference materials (SRM).
6.2 This test method is for use with commercially available
11.3 When the analysis is complete, the instrument should
sulfur analyzers equipped to carry out the preceding operations
indicate the sulfur value. Refer to the manufacturer’s recom-
automatically and must be calibrated using standard reference
mended procedure.
material (carbon black) of known sulfur content based on the
12. Report
range of sulfur in each carbon black specimen analyzed.
12.1 The percent sulfur value is obtained directly from the
7. Apparatus
apparatus.
7.1 Measurement Apparatus—equipped to automatically
13. Precision and Bias
combust the specimen.
7.2 Combustion Tube, made of mullite, porcelain, or zircon,
13.1 These precision statements have been prepared in
approximately 40- to 45-mm inside diameter with a 3-mm
accordance with Practice D 4483. Refer to this practice for
thick wall, at least 450-mm long with provisions for routing the
terminology and other statistical details.
gasses produced by combustion through the infrared cell.
13.2 The precision results in this precision and bias section
7.3 Boat Puller—rod of a heat-resistant material with a bent
give an estimate of the precision of this test method with the
or disk end to insert and remove boats from the combustion
materials used in the particular interlaboratory program de-
tube.
scribed below. The precision parameters should not be used for
acceptance or rejection testing of any group of materials
8. Reagents
without documentation that they are applicable to those par-
8.1 Purity of Reagents—see 4.1.
ticular materials and the specific testing protocols of the test
8.2 Magnesium Perchlorate.
method. Any appropriate value may be used from Table 1
13.3 A type 1 inter-laboratory precision program was con-
9. Preparation of Apparatus
ducted as detailed in Table 2. Both repeatability and reproduc-
9.1 Assemble the apparatus according to the manufacturer’s
ibility represent short term (daily) testing conditions. The
instructions. Make a minimum of two determinations (see
testing was performed u
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