ASTM D1619-03(2008)

Standard Test Methods for Carbon Black<span class='unicode'>&#x2014;</span>Sulfur Content

SIGNIFICANCE AND USE
The total sulfur content of a carbon black is useful in calculations for reconstructing a rubber composition from analytical data.
SCOPE
1.1 These test methods cover the determination of the sulfur content of carbon black. The following test methods are included:
Sections Test Method AHigh-Temperature Combustion With In-
frared Absorption Detection Procedures6 to 13 Test Method BX-Ray Fluorescence14
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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: 30-Jun-2008
• ICS: 83.040.20 - Rubber compounding ingredients
• Technical Committee: D24 - Carbon Black
• Drafting Committee: D24.66 - Environment, Health, and Safety

Relations

• Replaces: ASTM D1619-03 - Standard Test Methods for Carbon Black&#8212;Sulfur Content
• Effective Date: 01-Jul-2008
• Replaced By: ASTM D1619-10 - Standard Test Methods for Carbon Black<span class='unicode'>&#x2014;</span>Sulfur Content
• Effective Date: 01-Nov-2010
• Referred By: ASTM D7679-16(2020) - Standard Test Method for Sulfur Content in Carbon Black Feedstock Oils
• Effective Date: 01-Jul-2008
• Referred By: ASTM D6602-13(2022)e1 - Standard Practice for Sampling and Testing of Possible Carbon Black Fugitive Emissions or Other Environmental Particulate, or Both
• Effective Date: 01-Jul-2008
• Referred By: ASTM D8466-22 - Standard Guide for Recovered Carbon Black—Carbon Black Test Methods for Testing rCB
• Effective Date: 01-Jul-2008
• Referred By: ASTM D5817-20 - Standard Practice for Carbon Black, Pelleted—Reduction, Blending, and Drying of Gross Samples for Testing
• Effective Date: 01-Jul-2008
• Referred By: ASTM D7849-23 - Standard Classification for Nomenclature of Reference Materials of Committee D24
• Effective Date: 01-Jul-2008

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1619–03 (Reapproved 2008)
Standard Test Methods for
Carbon Black—Sulfur Content
This standard is issued under the fixed designation D1619; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 3. Significance and Use
1.1 These test methods cover the determination of the sulfur 3.1 The total sulfur content of a carbon black is useful in
content of carbon black. The following test methods are calculations for reconstructing a rubber composition from
included: analytical data.
Sections
4. Reagents
Test Method A High-Temperature Combustion With In- 6 to 13
frared Absorption Detection Procedures
4.1 Purity of Reagents—Reagent grade chemicals shall be
Test Method B X-Ray Fluorescence 14
used in all tests. Unless otherwise indicated, it is intended that
1.2 The values stated in SI units are to be regarded as
all reagents shall conform to the specifications of the Commit-
standard. No other units of measurement are included in this
tee onAnalytical Reagents of theAmerican Chemical Society,
standard. 3
where such specifications are available. Other grades may be
1.3 This standard does not purport to address all of the
used, provided it is first ascertained that the reagent is of
safety concerns, if any, associated with its use. It is the
sufficiently high purity to permit its use without lessening the
responsibility of the user of this standard to establish appro-
accuracy of the determination.
priate safety and health practices and determine the applica-
4.2 Purity of Water— Unless otherwise indicated, refer-
bility of regulatory limitations prior to use.
ences to water shall be understood to mean reagent water
conforming to Specification D1193.
2. Referenced Documents
2.1 ASTM Standards:
5. Sampling
D240 Test Method for Heat of Combustion of Liquid
5.1 Samples shall be taken in accordance with Practice
Hydrocarbon Fuels by Bomb Calorimeter
D1799 or Practice D1900.
D1193 Specification for Reagent Water
D1509 Test Methods for Carbon Black—Heating Loss TEST METHOD A HIGH-TEMPERATURE
COMBUSTION WITH INFRARED ABSORPTION
D1799 Practice for Carbon Black—Sampling Packaged
Shipments DETECTION PROCEDURES
D1900 Practice for Carbon Black—Sampling Bulk Ship-
6. Summary of Test Method
ments
6.1 The specimen is burned in a tube furnace at a minimum
D4483 Practice for Evaluating Precision for Test Method
operating temperature of 1350°C in a stream of oxygen to
Standards in the Rubber and Carbon Black Manufacturing
oxidize the sulfur. Moisture and particulates are removed from
Industries
the gas by traps filled with anhydrous magnesium perchlorate.
E1 Specification for ASTM Liquid-in-Glass Thermometers
The gas stream is passed through a cell in which sulfur dioxide
is measured by an infrared (IR) absorption detector. Sulfur
dioxide absorbs IR energy at a precise wavelength within the
These test methods are under the jurisdiction of ASTM Committee D24 on
IR spectrum. Energy is absorbed as the gas passes through the
Carbon Black and are the direct responsibility of Subcommittee D24.66 on
Environment, Health, and Safety.
Current edition approved July 1, 2008. Published September 2008. Originally
approved in 1958. Last previous edition approved in 2003 as D1619 – 03. DOI: Reagent Chemicals, American Chemical Society Specifications , American
10.1520/D1619-03R08. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1619–03 (2008)
cell body in which the IR energy is being transmitted. Thus, at allowable limits of the known value of the respective speci-
the detector, less energy is received. All other IR energy is men. If not, refer to the manufacturer’s instructions for
eliminated from reaching the detector by a precise wavelength checking linearity of the analyzer.
filter. Thus, the absorption of IR energy can be attributed only
11. Procedure
to sulfur dioxide whose concentration is proportional to the
11.1 Stabilize and calibrate the analyzer (see 10.1 through
change in energy at the detector. One cell is used as both a
10.3).
reference and a measurement chamber. Total sulfur as sulfur
11.2 Raise the furnace temperature as recommended by the
dioxide is detected on a continuous basis. This test method is
manufacturer to at least 1350°C. Weigh the specimen not to
empirical. Therefore, the apparatus must be calibrated by the
exceed more than 0.5 g of carbon black. Spread the specimen
use of standard reference materials (SRM).
evenly in a combustion boat and use a boat puller to position
6.2 This test method is for use with commercially available
the specimen in the hot zone of the furnace for at least 2 min,
sulfur analyzers equipped to carry out the preceding operations
or until completely combusted.
automatically and must be calibrated using standard reference
material (carbon black) of known sulfur content based on the
NOTE 1—The analytical cycle should begin automatically as soon as
range of sulfur in each carbon black specimen analyzed.
sulfur is detected.
11.3 When the analysis is complete, the instrument should
7. Apparatus
indicate the sulfur value. Refer to the manufacturer’s recom-
7.1 Measurement Apparatus—equipped to automatically
mended procedure.
combust the specimen.
7.2 Combustion Tube, made of mullite, porcelain, or zircon,
12. Report
approximately 40- to 45-mm inside diameter with a 3-mm
12.1 The percent sulfur value is obtained directly from the
thickwall,atleast450-mmlongwithprovisionsforroutingthe
apparatus.
gasses produced by combustion through the infrared cell.
7.3 Boat Puller—rod of a heat-resistant material with a bent
13. Precision and Bias
or disk end to insert and remove boats from the combustion
13.1 These precision statements have been prepared in
tube.
accordance with Practice D4483. Refer to this practice for
terminology and other statistical details.
8. Reagents
13.2 The precision results in this precision and bias section
8.1 Purity of Reagents—see 4.1.
give an estimate of the precision of this test method with the
8.2 Magnesium Perchlorate.
materials used in the particular interlaboratory program de-
scribed below.The precision parameters should not be used for
9. Preparation of Apparatus
acce
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D1619–99 Designation:D1619–03 (Reapproved 2008)
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 (´) 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
1.1 These test methods cover the determination of the sulfur content of carbon black. The following test methods are included:
Sections
Test Method A High-Temperature Combustion With In- 6to13
frared Absorption Detection Procedures
Test Method B X-Ray Fluorescence 14
1.2The values stated in SI units are to be regarded as standard.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2.1 ASTM Standards:
D 240 Test Method for Heat of Combustion of Liquid Hydrocarbon Fuels by Bomb Calorimeter
D 1193 Specification for Reagent Water D1509Test Methods for Carbon Black—Heating Loss
D 1509 Test Methods for Carbon BlackHeating Loss
D 1799 Practice for Carbon Black—Sampling Packaged Shipments
D 1900 Practice for Carbon Black—Sampling Bulk Shipment Shipments
D 4483 Practice for DeterminingEvaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufac-
turing Industries
E 1 Specification for ASTM Liquid-in-Glass Thermometers
3. Significance and Use
3.1 The total sulfur content of a carbon black is useful in calculations for reconstructing a rubber composition from analytical
data.
4. Reagents
4.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
4.2 Purity of Water— Unless otherwise indicated, references to water shall be understood to mean reagent water conforming
to Specification D 1193.
5. Sampling
5.1 Samples shall be taken in accordance with Practice D 1799 or Practice D 1900.
These test methods are under the jurisdiction ofASTM Committee D-24D24 on 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.July 1, 2008. Published September 1999.2008. Originally published as D1619–58T.approved in 1958. Last previous edition
D1619–97. approved in 2003 as D 1619 – 03.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. ForAnnualBookofASTMStandards
, Vol 05.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 11.01.Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1619–03 (2008)
TEST METHOD A HIGH-TEMPERATURE COMBUSTION WITH INFRARED ABSORPTION DETECTION
PROCEDURES
6. Summary of Test Method
6.1 The specimen is burned in a tube furnace at a minimum operating temperature of 1350°C in a stream of oxygen to oxidize
the sulfur. Moisture and particulates are removed from the gas by traps filled with anhydrous magnesium perchlorate. The gas
stream is passed through a cell in which sulfur dioxide is measured by an infrared (IR) absorption detector. Sulfur dioxide absorbs
IR energy at a precise wavelength within the IR spectrum. Energy is absorbed as the gas passes through the cell body in which
the IR energy is being transmitted. Thus, at the detector, less energy is received. All other IR energy is eliminated from reaching
the detector by a precise wavelength 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 dioxide is detected on a continuous basis. This test method is empirical. Therefore, the apparatus
must be calibrated by the use of standard reference materials (SRM).
6.2 This test method is for use with commercially available sulfur analyzers equipped to carry out the preceding operations
automatically and must be calibrated using standard reference material (carbon black) of known sulfur content based on the range
of sulfur in each carbon black specimen analyzed.
7. Apparatus
7.1 Measurement Apparatus—equipped to automatically combust the specimen.
7.2 Combustion Tube, made of mullite, porcelain, or zircon, approximately 40- to 45-mm inside diameter with a 3-mm thick
wall, at least 450-mm long with provisions for routing the gasses produced by combustion through the infrared cell.
7.3 Boat Puller—rod of a heat-resistant material with a bent or disk end to insert and remove boats from the combustion tube.
8. Reagents
8.1 Purity of Reagents—see 4.1.
8.2 Magnesium Perchlorate.
9. Preparation of Apparatus
9.1 Assemble the apparatus according to the manufacturer’s instructions. Make a minimum of two determinations (see 10.3) to
condition the equipment prior to calibrating the system.
10. Calibration
10.1 Select black standard reference materials (SRM) containing known sulfur values of approximately 0.5, 1.0, and 1.5%
sulfur. Select standards having sulfur values of approximately 0.5, 1.0, and 1.5 % sulfur .
10.2 Adjustment of Response of Measurement System—Weigh out approximately 0.5 g of the 1.0 % sulfur standard. Analyze
the specimen (see Section 11). Repeat this procedure. Adjust instrument as recommended by the manufacturer until the absence
of drift is indicated.
10.3 Calibration Procedure—Weigh out four specimens of the 1.0 % sulfur standard. Follow the calibration procedure
recommended by the manufacturer. Confirm the calibration by analyzing the 1.0 % sulfur standard.The value should be within the
allowable limits of the known value. If not, repeat the procedure. Then weigh out and analyze two specimens, each of the other
calibration standards. Record the results after each analy
...