ASTM D4218-96

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

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: 09-Jul-1996
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaced By: ASTM D4218-96(2001) - Standard Test Method for Determination of Carbon Black Content in Polyethylene Compounds By the Muffle-Furnace Technique
• Effective Date: 10-Jul-1996
• Referred By: ASTM D3350-21 - Standard Specification for Polyethylene Plastics Pipe and Fittings Materials
• Effective Date: 10-Jul-1996
• Referred By: ASTM F3123-22 - Standard Specification for Metric Outside Diameter Polyethylene (PE) Plastic Pipe (DR-PN)
• Effective Date: 10-Jul-1996
• Referred By: ASTM F3524/F3524M-23 - Standard Specification for Polyamide-12 (PA12) Line Pipe
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2306/F2306M-21 - Standard Specification for 300 mm to 1500 mm [12 in. to 60 in.] Annular Corrugated Profile-Wall Polyethylene (PE) Pipe and Fittings for Non-Pressure Gravity-Flow Storm Sewer and Subsurface Drainage Applications
• Effective Date: 10-Jul-1996
• Referred By: ASTM D2239-22 - Standard Specification for Polyethylene (PE) Plastic Pipe (SIDR-PR) Based on Controlled Inside Diameter
• Effective Date: 10-Jul-1996
• Referred By: ASTM D7273/D7273M-08(2020) - Standard Guide for Acceptance Testing Requirements for Geonets and Geonet Drainage Geocomposites
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2968/F2968M-21 - Standard Specification for Crosslinked Polyethylene (PEX) Pipe for Gas Distribution Applications
• Effective Date: 10-Jul-1996
• Referred By: ASTM F3034-21 - Standard Specification for Billets made by Winding Molten Extruded Stress-Rated High Density Polyethylene (HDPE)
• Effective Date: 10-Jul-1996
• Referred By: ASTM F3390-20 - Standard Specification for 3 through 24 in. Lined Flexible Corrugated Polyethylene Pipe for Land Drainage Applications
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2881/F2881M-21e1 - Standard Specification for 12 to 60 in. [300 to 1500 mm] Polypropylene (PP) Dual Wall Pipe and Fittings for Non-Pressure Storm Sewer Applications
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2905/F2905M-22 - Standard Specification for Crosslinked Polyethylene (PEX) Line Pipe For Oil and Gas Producing Applications
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2619/F2619M-20 - Standard Specification for High-Density Polyethylene (PE) Line Pipe
• Effective Date: 10-Jul-1996
• Referred By: ASTM D1603-20 - Standard Test Method for Carbon Black Content in Olefin Plastics
• Effective Date: 10-Jul-1996
• Referred By: ASTM F2763/F2763M-16(2021)e1 - Standard Specification for 12 to 60 in. [300 to 1500 mm] Dual and Triple Profile-Wall Polyethylene (PE) Pipe and Fittings for Sanitary Sewer Applications
• Effective Date: 10-Jul-1996

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4218 – 96 An American National Standards
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 D 4218; 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.
1. Scope small diffusion flames burn in air and carbon is deposited on
cooled surfaces.
1.1 This test method covers the determination of black
3.2.2 furnace black—those carbon blacks produced using
polyethylene compounds containing channel or furnace black.
the principle of continuous oxidative combustion in closed
It is not applicable to thermal black.
systems.
1.2 This test method is not suitable for plastics that char on
3.2.3 thermal black—those carbon blacks based on a pro-
pyrolysis and should not be attempted for plastics that generate
cess that uses thermal decomposition in the absence of oxygen
corrosive fumes on pyrolysis.
and operates in a closed system. Particles grow very slowly and
1.3 The values stated in SI units are to be regarded as the
can become very large and filamentous structures.
standard.
3.3 Symbols:Symbols—Units and symbols used in this test
1.4 This standard does not purport to address all of the
method are those recommended in Practice E 380.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Black polyethylene compound contained in a disposable
bility of regulatory limitations prior to use. Specific hazard
aluminum weighing dish is pyrolyzed in a muffle furnace for a
statements are given in Section 7.
short period. During the pyrolysis of the polymer, the air in the
NOTE 1—There is no similar or equivalent ISO standard.
muffle furnace becomes oxygen-deficient to prevent the com-
bustion of the residual carbon black. Any soot, as defined in
2. Referenced Documents
Test Method D 2741, produced by the initial combustion of the
2.1 ASTM Standards:
gases is consumed before the carbon black itself.
D 883 Terminology Relating to Plastics
4.2 After cooling and weighing for residual carbon black,
D 1603 Test Method for Carbon Black in Olefin Plastics
the dish and contents may be reinserted into the muffle furnace
D 2741 Test Method for Susceptibility of Polyethylene
to determine ash content and the results used to determine true
Bottles to Soot Accumulation
carbon black content. This should be done only if the com-
E 380 Practice for Use of the International System of Units
pound is suspected of containing mineral fillers as well as
(SI) (The Modernized Metric System)
carbon black.
E 691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
5. Significance and Use
5.1 This test method is capable of yielding duplicate test
3. Terminology
data, in 20 min or less, for a simple carbon black content
3.1 Definitions: For definitions of plastics terms used in this
determination.
test method, see Terminology D 883.
5.2 This test method is suitable for manufacturing quality
3.2 Definitions of Terms Specific to This Standard:
control, technical service, and research work.
3.2.1 channel black—those carbon blacks produced by a
5.3 For referee requirements, the number of replicate mea-
process that operates in an open system in which a multitude of
surements is increased. Alternatively, a control sample of
known carbon black content is tested with the unknown
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics sample.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
5.4 Test Method D 1603 is available for referee testing
(Section D20.70.01).
should the involved parties so desire.
Current edition approved July 10, 1996. Published September 1996. Originally
published as D 4218 – 82. Last previous edition D 4218 – 91.
6. Apparatus
This revision includes the addition of an ISO equivalence statement and an
expanded terminology section.
6.1 Fume Hood or Vent Hood.
Annual Book of ASTM Standards, Vol 08.01
3 6.2 Muffle Furnace, approximately 100 mm in the three
Annual Book of ASTM Standards, Vol 08.02.
internal dimensions. Furnaces with larger internal dimensions
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4218
have been found to be unsuitable. The seal at the door must be 10.8 Place the weighed dish and contents into the muffle
free of gaping cracks or chips that will allow air into the furnace and set the interval timer for 3 min.
furnace. A muffle furnace with bare heating wires on the floor 10.9 After the elapsed time, remove the dish from the muffle
of the furnace must not be used without additional electrical furnace and place it in the desiccator to cool for at least 2 min.
safety precautions. Longer cooling periods do not affect the test.
6.3 Screen, 20-Mesh, approximately 120 by 100 mm. Fold 10.10 Reweigh the dish and remaining carbon black accu-
down approximately 10 mm of the long dimension to provide rately. Record the results as W .
a raised platform to fit inside the muffle furnace. 10.11 If ashable mineral fillers are suspected to be present in
6.4 Thermocouple-Probe Temperature Controller or the compound, replace the dish and contents into the muffle
Equivalent—This may be an integral part of newer muffle furnace for a period of 10 min or longer until only light-colored
furnaces or may be purchased separately to provide improved ash remains.
control on older furnaces. 10.12 Transfer the dish and contents from the muffle furnace
6.5 Desiccator (for example, 255 mm), with alumina or to the desiccator and let it cool for 2 min.
equivalent desiccant. 10.13 Reweigh the dish and ash accurately. Record the
6.6 Laboratory Interval Timer, with alarm. results as W .
6.7 Disposable Aluminum Weighing Dish—Dishes with 10.14 A minimum of two determinations is made for each
crimped sides and tabs on the rim are satisfactory. sample.
6.8 Long Tongs or Tweezers (250 to 300 mm).
11. Calculation
6.9 Analytical Balance, capable of measuring to 0.1 mg.
11.1 Calculate the percent carbon black content as follows:
7. Hazards
W – W
3 1
Carbon black, % 5 3 100 (1)
7.1 Do not use a muffle furnace with bare heating elements
W – W
2 1
on the floor of the furnace. Take steps to make the furnace
...