ASTM D1506-99(2013)
(Test Method)Standard Test Methods for Carbon Black—Ash Content
Standard Test Methods for Carbon Black—Ash Content
SIGNIFICANCE AND USE
4.1 The ash content of a carbon black is the amount of non-carbon components present after combustion. Primary contributants to ash are the manufacturing process water and the catalyst in the feedstock.
SCOPE
1.1 These test methods cover the determination of the ash content of carbon black.
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. For specific precautionary statements see Sections 6 and 13.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D1506 − 99(Reapproved 2013)
Standard Test Methods for
Carbon Black—Ash Content
This standard is issued under the fixed designation D1506; 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 contributants to ash are the manufacturing process water and
the catalyst in the feedstock.
1.1 These test methods cover the determination of the ash
content of carbon black.
Method A—Muffle Furnace Method
1.2 The values stated in SI units are to be regarded as
5. Apparatus
standard. No other units of measurement are included in this
standard.
5.1 Muffle Furnace, capable of temperature regulation of
1.3 This standard does not purport to address all of the 625°C at 550°C.
safety concerns, if any, associated with its use. It is the
5.2 Crucibles:
responsibility of the user of this standard to establish appro-
5.2.1 Porcelain Crucible, high-form, size O, rim 35 mm,
priate safety and health practices and determine the applica- 3
height 29 mm, capacity 15 cm , with cover size E.
bility of regulatory limitations prior to use. For specific
5.2.2 Porous Quartz Fiber Crucible, rim 47 mm, height 14
precautionary statements see Sections 6 and 13. 3
mm, with disk.
5.3 Analytical Balance, having a sensitivity of 0.1 mg.
2. Referenced Documents
5.4 Desiccator.
2.1 ASTM Standards:
D1799 Practice for Carbon Black—Sampling Packaged
5.5 Oven, gravity-convection type, capable of temperature
Shipments
regulation within 61°C at 125°C and temperature uniformity
D1900 Practice for Carbon Black—Sampling Bulk Ship-
within 65°C.
ments
D4483 Practice for Evaluating Precision for Test Method
6. Hazards
Standards in the Rubber and Carbon Black Manufacturing
6.1 Precautions:
Industries
6.1.1 Keep the door of the furnace open about 6 mm to
admit air to support the combustion of organic material.
3. Summary of Test Method
6.1.2 Exert care in removing ashed sample from furnace to
3.1 Apre-driedsample(1hat125°C)isweighedbeforeand
desiccator.
after combustion for 16 h at 550°C. The remaining ash is
6.1.3 Always keep the cover on the crucible when transfer-
weighed and calculated as a percent of the dried sample.
ring it to and from the desiccator to prevent the loss of ash due
to air currents.
4. Significance and Use
6.1.4 Afterthesamplehascooledinthedesiccator,admitair
slowly to avoid loss of ash from the crucible.
4.1 The ash content of a carbon black is the amount of
non-carbon components present after combustion. Primary
7. Sampling
7.1 Samples shall be taken in accordance with Practices
These test methods are under the jurisdiction of ASTM Committee D24 on D1799 or D1900.
Carbon Black and are the direct responsibility of Subcommittee D24.31 on
Non-Carbon Black Components of Carbon Black.
Current edition approved Nov. 1, 2013. Published January 2014. Originally
approved in 1957. Last previous edition approved in 2007 as D1506 – 99 (2007). The sole source of supply of the apparatus (quartz ashing dishes, Part Number
DOI: 10.1520/D1506-99R13. 303040) known to the committee at this time is CEM Corporation, P.O. Box 200,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Matthews, NC 28106. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
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the ASTM website. you may attend.
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D1506 − 99 (2013)
TABLE 1 Precision Parameters for D1506 Ash Content, (Type 1
8. Procedure
Precision)
8.1 Ignite the crucible with cover in the muffle furnace at
Units Percent Ash
550 6 25°C for 1 h. Place the crucible and cover in the
Material Mean Level Sr (r) SR (R)
desiccator. Cool to room temperature and weigh to nearest 0.1
IRB#6 (N330) 0.233 0.018 21.4 0.027 32.4
mg.
SRB D5 (N762) 0.258 0.015 16.0 0.030 32.6
N650 0.289 0.019 18.7 0.031 30.4
8.2 Dry an adequate sample of carbon black for1hinthe
N550 0.436 0.025 16.1 0.037 23.7
gravity-convection oven set at 125°C in an open container of
SRB A5 (N135) 0.565 0.023 11.5 0.056 27.9
Average 0.356
suitable dimensions, so that the depth of the black is no more
Pooled Values 0.020 16.0 0.037 29.7
than 10 mm. Cool and store the sample in a desiccator.
8.3 Weigh 2 60.1 g of the dried carbon black into the
ignited crucible and weigh to the nearest 0.1 mg. Place the
TABLE 2 Interlaboratory Precision Program
uncovered crucible and its cover into the furnace (Note 1)at
Nominal Test Period Material Number of Laboratories
550°C for 16 h (porcelain crucible) or 1.5 h (porous quartz
March 1996 N650 45
fibercrucible–see6.1.1).Coverthecruciblecontainingtheash, October 1996 IRB#6 (N330) 37
March 1997 SRB N762 48
remove from the furnace to the desiccator, and allow to cool to
September 1997 SRB A5 (N135) 43
room temperature. Weigh the covered crucible to the nearest
March 1998 N550 46
0.1 mg. Put the covered crucible back into the desiccator for
additional 0.5 h. Reweigh to the nearest 0.1 mg. Repeat this
weighing process until constant mass is obtained.
performing the test once on each of two days (total of four
NOTE 1—For carbon blacks with very low ash content (such as high
tests). A test result is the value obtained from a single
purityblacks)largersamplemassandlongerashingtimemayberequired.
determination. Acceptable difference values were not mea-
NOTE 2—If control testing is done at temperatures exceeding 550°C,
sured. The between operator component of variation is in-
some volatile salts may be lost from inorganic ash.
cluded in the calculated values for r and R.
9. Calculation
11.4 The results of the precision calculations for this test are
given in Table 1. The materials are arranged in ascending
9.1 Calculate the percent ash to the nearest 0.01 % as
follows: “mean level” order.
11.5 Repeatability—The pooled relative repeatability, (r), of
A 5 @~D 2 B!/~C 2 B!# 3100 (1)
this test has been established as 16.0 %. Any other value in
where:
Table 1 may be used as an estimate of repeatability, as
A = ash, %,
appropriate. The difference between two single test results (or
B = mass of crucible, g,
determinations) found on identical test material under the
C = mass of crucible plus the sample, g, and
repeatability conditions prescribed for this test will exceed the
D = mass of crucible plus the ash, g.
repeatability on an average of not more than once in 20 cases
in the normal and correct operation of the method. Two single
10. Report
test results that differ by more than the appropriate value from
10.1 Report the following information:
Table 1 must be suspected of being from different populations
10.1.1 Proper identification of the sample, and
and some appropriate action taken.
10.1.2 A result obtained from an individual determination
NOTE 3—Appropriate action may be an investigation of the test method
reported to the nearest 0.01 %.
procedure or apparatus for faulty operation or the declaration of a
significant difference in the two materials, samples, etc., which generated
11. Precision and Bias
the two test results.
11.1 These precision statements have been prepared in
11.6 Reproducibility—The pooled relative reproducibility,
accordance with Practice D4483. Refer to this practice for
(R),ofthistesthasbeenestablishedas29.7 %.Anyothervalue
terminology and other statistical details.
in Table 1 may be used as an estimate of reproducibility, as
11.2 The precision results in this precision and bias section appropriate. The difference between two single and indepen-
give an estimate of the precision of this test method with the dent test results found by two operators working under the
materials used in the particular interlaboratory program de- prescribed reproducibility conditions in different laboratories
scribed below.The precision parameters should not be used for on identical test material will exceed the reproducibility on an
acceptance or rejection te
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