ASTM D1619-22

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 − 20 D1619 − 22
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 U.S. 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- 6 to 13
frared Absorption Detection Procedures
Test Method B X-Ray Fluorescence 14 to 19
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:
D1509 Test Methods for Carbon Black—Heating Loss
D1799 Practice for Carbon Black—Sampling Packaged Shipments
D1900 Practice for Carbon Black—Sampling Bulk Shipments
D4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
3. Significance and Use
3.1 The total sulfur content of a carbon black is useful in determining whether a material meets a customer’s specifications,
providing data for performing a sulfur material balance around a process for environmental monitoring and reporting, and in
calculations for reconstructing a rubber composition from analytical data.
These test methods are under the jurisdiction of ASTM Committee D24 on Carbon Black and are the direct responsibility of Subcommittee D24.66 on Environment,
Health, and Safety.
Current edition approved Nov. 1, 2020Nov. 1, 2022. Published December 2020December 2022. Originally approved in 1958. Last previous edition approved in 20162020
as D1619 – 16a.D1619 – 20. DOI: 10.1520/D1619-20.10.1520/D1619-22.
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 the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1619 − 22
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.
5. Sampling
5.1 Samples of packaged materials shall be taken in accordance with Practice D1799 or Practice D1900.
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.
7.4 Gravity Convection Drying Oven, capable of maintaining 125 6 5°C.
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.
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.
D1619 − 22
10. Calibration
10.1 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 analysis. Compare the results obtained to the known sulfur values of the
specimens. They should be within the allowable limits of the known value of the respective specimen. If not, refer to the
manufacturer’s instructions for checking linearity of the analyzer.
11. Procedure
11.1 Sample Preparation—Dry an adequate sample of the carbon black for at least 1 h in a gravity-convection oven set at 125 6
5°C, in an open container of suitable dimensions, so that the depth of black is no more than 10 mm. Cool to room temperature
in a desiccator before use.
11.2 Stabilize and calibrate the analyzer (see 10.1 through 10.3).
11.3 Raise the furnace temperature as recommended by the manufacturer to at least 1350°C. Weigh the specimen not to exceed
more than 0.5 g of carbon black. Spread the specimen evenly in a combustion boat and use a boat puller to position the specimen
in the hot zone of the furnace for at least 2 min, or until completely combusted.
NOTE 1—The analytical cycle should begin automatically as soon as sulfur is detected.
11.4 When the analysis is complete, the instrument should indicate the sulfur value. Refer to the manufacturer’s recommended
procedure.
12. Report
12.1 The percent sulfur value is obtained directly from the apparatus.
12.2 Report results to the nearest 0.01 %.
13. Precision and Bias
13.1 These precision statements have been prepared in accordance with Practice D4483-99. Refer to this practice for terminology
and other statistical details.
13.2 The precision results in this precision and bias section give an estimate of the precision of this test method with the materials
used in the particular interlaboratory programs described in Table 1. The precision parameters should not be used for acceptance
or rejection testing of any group of materials without documentation that they are applicable to those particular materials and the
specific testing protocols of the test method. Any appropriate value may be used from Table 1.
13.3 Type 1 inter-laboratory precision programs were conducted as detailed in Table 1. Both repeatability and reproducibility
represent short term (daily) testing conditions. The testing was performed using two operators in each laboratory performing the
test once on each of two days (total of four tests). A test result is the value obtained from a single determination. Acceptable
difference values were not measured. The between operator component of variation is included in the calculated values for r, (r),
R, and (R).
Coal standards have been found to be suitable standards and are usually available from the instrument manufacturer or may be obtained from Alpha Products for Analysis,
3090 Johnson Road, Stevensville, MI 49127, www.alpha-resources.com.
D1619 − 22
A
TABLE 1 Precision Parameters for Test Methods D1619, Sulfur Content of Carbon Black (Type 1 Precision), Method A: Combustion
Units are percent
Number of
Material Period Laboratories Mean Level Sr r (r) SR R (R)
B
(M/H/L)
STRM-A (SRB-8G) Aug 2017 14(0/1/0) 0.022 0.002 0.007 29.791 0.021 0.060 269.841
STRM-A (SRB-8G) Aug 2017 14(0/1/0) 0.022 0.002 0.007 30 0.021 0.060 270
STRM-B (SRB-8F2) Mar 2015 11(0/2/0) 0.357 0.008 0.023 6.580 0.023 0.065 18.357
STRM-B (SRB-8F2) Mar 2015 11(0/2/0) 0.357 0.008 0.023 6.6 0.023 0.065 18
STRM-C (SRB-8B2) Mar/Apr 2014 12(1/0/1) 0.791 0.010 0.029 3.646 0.026 0.074 9.343
STRM-C (SRB-8B2) Mar/Apr 2014 12(1/0/1) 0.791 0.010 0.029 3.6 0.026 0.074 9.3
STRM-D (SRB-8E2) Aug 2016 17(0/1/0) 1.248 0.012 0.034 2.760 0.057 0.161 12.879
STRM-D (SRB-8E2) Aug 2016 17(0/1/0) 1.248 0.012 0.034 2.8 0.057 0.161 13
STRM-E (SRB-8D) Mar 2017 15(0/0/1) 1.850 0.020 0.056 3.009 0.133 0.376 20.298
STRM-E (SRB-8D) Mar 2017 15(0/0/1) 1.850 0.020 0.056 3.0 0.133 0.376 20
Average 0.854
Pooled Values 0.012 0.034 3.959 0.067 0.190 22.242
Pooled Values 0.012 0.034 4.0 0.067 0.190 22
A
Preferred precision shown in bold text. Statistically, relative precision is preferred. However, the increase in relative precision limits when dealing with a mean value near
zero, such as the SRB-8G material, makes the use of absolute precision more practical, so it is the preferred precision.
B
M = number of outliers for Laboratory Mean as identified by Mandel h-value; H = number of outliers for High Laboratory variation as identified by a 2-sided test using
the Mandel k-value; L = number of outliers for Low Laboratory variation as identified by a 2-sided test using the Mandel k-value. Low variation laboratories have variation
that is less than expected based on the statistical evaluation of the data set.
13.4 The res
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