Standard Test Method for Determination of Carbon Black Content in Polyethylene Compounds By the Muffle-Furnace Technique

SIGNIFICANCE AND USE
This test method is capable of yielding duplicate test data, in 20 min or less, for a simple carbon black content determination.
This test method is suitable for manufacturing quality control, technical service, and research work.
For referee requirements, the number of replicate measurements is increased. Alternatively, a control sample of known carbon black content is tested with the unknown sample.
Test Method D 1603 is available for referee testing should the involved parties so desire.
SCOPE
1.1 This test method covers the determination of black polyethylene compounds containing channel or furnace black. It is not applicable to thermal black.
1.2 This test method is not suitable for plastics that char on pyrolysis and should not be attempted for plastics that generate corrosive fumes on pyrolysis.
1.3 The values stated in SI units are to 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. Specific hazard statements are given in Section 7.  
Note 1—There is no similar or equivalent ISO standard.

General Information

Status
Historical
Publication Date
31-Oct-2008
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D4218-96(2008) - Standard Test Method for Determination of Carbon Black Content in Polyethylene Compounds By the Muffle-Furnace Technique
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4218 − 96(Reapproved 2008)
Standard Test Method for
Determination of Carbon Black Content in Polyethylene
Compounds By the Muffle-Furnace Technique
This standard is issued under the fixed designation D4218; 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.
1. Scope 3. Terminology
1.1 This test method covers the determination of black
3.1 Definitions—For definitions of plastics terms used in
polyethylene compounds containing channel or furnace black. this test method, see Terminology D883.
It is not applicable to thermal black.
3.2 Definitions of Terms Specific to This Standard:
1.2 This test method is not suitable for plastics that char on
3.2.1 channel black—those carbon blacks produced by a
pyrolysis and should not be attempted for plastics that generate
processthatoperatesinanopensysteminwhichamultitudeof
corrosive fumes on pyrolysis.
small diffusion flames burn in air and carbon is deposited on
cooled surfaces.
1.3 The values stated in SI units are to be regarded as the
3.2.2 furnace black—those carbon blacks produced using
standard.
the principle of continuous oxidative combustion in closed
1.4 This standard does not purport to address all of the
systems.
safety concerns, if any, associated with its use. It is the
3.2.3 thermal black—those carbon blacks based on a pro-
responsibility of the user of this standard to establish appro-
cess that uses thermal decomposition in the absence of oxygen
priate safety and health practices and determine the applica-
andoperatesinaclosedsystem.Particlesgrowveryslowlyand
bility of regulatory limitations prior to use. Specific hazard
can become very large and filamentous structures.
statements are given in Section 7.
3.3 Symbols—Units and symbols used in this test method
NOTE 1—There is no similar or equivalent ISO standard.
are those recommended in Practice IEEE/ASTM SI-10.
2. Referenced Documents
4. Summary of Test Method
2.1 ASTM Standards:
4.1 Black polyethylene compound contained in a disposable
D883 Terminology Relating to Plastics
aluminum weighing dish is pyrolyzed in a muffle furnace for a
D1603 Test Method for Carbon Black Content in Olefin
short period. During the pyrolysis of the polymer, the air in the
Plastics
muffle furnace becomes oxygen-deficient to prevent the com-
D2741 Test Method for Susceptibility of Polyethylene
bustion of the residual carbon black. Any soot, as defined in
Bottles to Soot Accumulation (Withdrawn 2011)
Test Method D2741, produced by the initial combustion of the
E691 Practice for Conducting an Interlaboratory Study to
gases is consumed before the carbon black itself.
Determine the Precision of a Test Method
4.2 After cooling and weighing for residual carbon black,
IEEE/ASTM SI-10 Standard for Use of the International
the dish and contents may be reinserted into the muffle furnace
System of Units (SI): The Modern Metric System
to determine ash content and the results used to determine true
carbon black content. This should be done only if the com-
pound is suspected of containing mineral fillers as well as
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
carbon black.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
(Section D20.70.01).
Current edition approved Nov. 1, 2008. Published December 2008. Originally
5. Significance and Use
approved in 1982. Last previous edition approved in 2001 as D4218 – 96(2001).
DOI: 10.1520/D4218-96R08.
5.1 This test method is capable of yielding duplicate test
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
data, in 20 min or less, for a simple carbon black content
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
determination.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
5.2 This test method is suitable for manufacturing quality
The last approved version of this historical standard is referenced on
www.astm.org. control, technical service, and research work.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4218 − 96 (2008)
5.3 For referee requirements, the number of replicate mea- 10. Procedure
surements is increased. Alternatively, a control sample of
10.1 Placethemufflefurnaceinafumehoodorunderavent
known carbon black content is tested with the unknown
hood.
sample.
10.2 Set the controller indicator to 600°C and let it stabilize
5.4 Test Method D1603 is available for referee testing
from 600 to 610°C.
should the involved parties so desire.
10.3 Mark an aluminum weighing dish with an identifying
impression on the tab.
6. Apparatus
6.1 Fume Hood or Vent Hood. 10.4 Place the dish on the screen in the muffle furnace and
burn off the surface oil for 2 min, as indicated by timer.
6.2 Muffle Furnace, approximately 100 mm in the three
internal dimensions. Furnaces with larger internal dimensions 10.5 Transfer the dish to the desiccator and let it cool for at
have been found to be unsuitable. The seal at the door must be least 2 min.
free of gaping cracks or chips that will allow air into the
10.6 Weigh the dish accurately on the analytical balance.
furnace. A muffle furnace with bare heating wires on the floor
Record the results as W .
of the furnace must not be used without additional electrical
10.7 Add about1gof specimen and reweigh the dish and
safety precautions.
contents accurately. Record the results as W .
6.3 Screen, 20-Mesh, approximately 120 by 100 mm. Fold
10.8 Place the weighed dish and contents into the muffle
down approximately 10 mm of the long dimension to provide
furnace and set the interval timer for 3 min.
a raised platform to fit inside the muffle furnace.
10.9 Aftertheelapsedtime,removethedishfromthemuffle
6.4 Thermocouple-Probe Temperature Controller or
furnace and place it in the desiccator to cool for at least 2 min.
Equivalent—This may be an integral part of newer muffle
Longer cooling periods do not affect the test.
furnaces or may be purchased separately to provide improved
control on older furnaces. 10.10 Reweigh the dish and remaining carbon black accu-
rately. Record the results as W .
6.5 Desiccator (for example, 255 mm), with alumina or
equivalent desiccant. 10.11 Ifashablemineralfillersaresuspectedtobepresentin
the compound, replace the dish and contents into the muffle
6.6 Laboratory Interval Timer, with alarm.
furnaceforaperiodof10minorlongeruntilonlylight-colored
6.7 Disposable Aluminum Weighing Dish—Dishes with
ash remai
...

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