ASTM D5577-94(2010)e1
(Guide)Standard Guide for Techniques to Separate and Identify Contaminants in Recycled Plastics (Withdrawn 2019)
Standard Guide for Techniques to Separate and Identify Contaminants in Recycled Plastics (Withdrawn 2019)
SIGNIFICANCE AND USE
Recycled plastic materials may contain incompatible plastic or other undesirable contaminants that could affect the processing or quality, or both, of the plastic prepared for reuse. Techniques to separate and identify incompatible plastics, moisture, chemicals, or original product residues, and solid contaminants such as metals, paper, glass, and wood are essential to the processing of recycled plastic materials.
This guide lists existing ASTM and ISO methods plus currently practiced industrial techniques for identification and classification of contaminants in recycled plastics flake or pellets.
SCOPE
1.1 This guide is intended to provide information on available methods for the separation and classification of contaminants such as moisture, incompatible polymers, metals, adhesives, glass, paper, wood, chemicals, and original-product residues in recycled plastic flakes or pellets. Although no specific methods for identification or characterization of foam products are included, foam products are not excluded from this guide. The methods presented apply to post-consumer plastics.
1.2 For specific procedures existing as ASTM test methods, this guide only lists the appropriate reference. Where no current ASTM standard exists, however, this guide gives procedures for the separation or identification, or both, of specific contaminants. Appendix X1 lists the tests and the specific contaminant addressed by each procedure.
1.3 This guide does not include procedures to quantify the contaminants unless this information is available in referenced ASTM standards.
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.
Note 1—There is no known ISO equivalent to this standard.
WITHDRAWN RATIONALE
This guide is intended to provide information on available methods for the separation and classification of contaminants such as moisture, incompatible polymers, metals, adhesives, glass, paper, wood, chemicals, and original-product residues in recycled plastic flakes or pellets. Although no specific methods for identification or characterization of foam products are included, foam products are not excluded from this guide. The methods presented apply to post-consumer plastics.
Formerly under the jurisdiction of Committee D20 on Plastics, this guide was withdrawn in January 2019 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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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
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Designation: D5577 − 94 (Reapproved 2010)
Standard Guide for
Techniques to Separate and Identify Contaminants in
Recycled Plastics
This standard is issued under the fixed designation D5577; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Reapproved with editorial change to Note 1 in January 2010.
1. Scope D792Test Methods for Density and Specific Gravity (Rela-
tive Density) of Plastics by Displacement
1.1 This guide is intended to provide information on avail-
D883Terminology Relating to Plastics
able methods for the separation and classification of contami-
D1003Test Method for Haze and Luminous Transmittance
nants such as moisture, incompatible polymers, metals,
of Transparent Plastics
adhesives, glass, paper, wood, chemicals, and original-product
D1193Specification for Reagent Water
residues in recycled plastic flakes or pellets. Although no
D1238Test Method for Melt Flow Rates of Thermoplastics
specific methods for identification or characterization of foam
by Extrusion Plastometer
products are included, foam products are not excluded from
D1457 Specification for Polytetrafluoroethylene (Ptfe)
this guide. The methods presented apply to post-consumer
Molding and Extrusion Materials (Withdrawn 1996)
plastics.
D1505Test Method for Density of Plastics by the Density-
1.2 For specific procedures existing asASTM test methods,
Gradient Technique
this guide only lists the appropriate reference. Where no
D1898Practice for Sampling of Plastics (Withdrawn 1998)
current ASTM standard exists, however, this guide gives
D1925Test Method forYellowness Index of Plastics (With-
procedures for the separation or identification, or both, of
drawn 1995)
specific contaminants. Appendix X1 lists the tests and the
D3418Test Method for Transition Temperatures and En-
specific contaminant addressed by each procedure.
thalpies of Fusion and Crystallization of Polymers by
Differential Scanning Calorimetry
1.3 This guide does not include procedures to quantify the
contaminants unless this information is available in referenced D4019Test Method for Moisture in Plastics by Coulometric
ASTM standards. Regeneration of Phosphorus Pentoxide (Withdrawn
2002)
1.4 This standard does not purport to address all of the
D5033GuideforDevelopmentofASTMStandardsRelating
safety concerns, if any, associated with its use. It is the
to Recycling and Use of Recycled Plastics (Withdrawn
responsibility of the user of this standard to establish appro-
2007)
priate safety and health practices and determine the applica-
D5227TestMethodforMeasurementofHexaneExtractable
bility of regulatory limitations prior to use.
Content of Polyolefins
NOTE 1—There is no known ISO equivalent to this standard.
E169PracticesforGeneralTechniquesofUltraviolet-Visible
Quantitative Analysis
2. Referenced Documents
E355PracticeforGasChromatographyTermsandRelation-
2.1 ASTM Standards:
ships
D789Test Methods for Determination of Solution Viscosi-
E682Practice for Liquid Chromatography Terms and Rela-
ties of Polyamide (PA)
tionships
E794TestMethodforMeltingAndCrystallizationTempera-
tures By Thermal Analysis
This guide is under the jurisdiction ofASTM Committee D20 on Plastics and
E1252Practice for General Techniques for Obtaining Infra-
is the direct responsibility of Subcommittee D20.95 on Recycled Plastics.
red Spectra for Qualitative Analysis
Current edition approved Jan. 1, 2010. Published February 2010. Originally
approved in 1994. Last previous edition approved in 2003 as D5577-94(2003).
DOI: 10.1520/D5577-94R10E01.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5577 − 94 (2010)
2.2 ISO Standards: 5.2 This guide lists existing ASTM and ISO methods plus
ISO 3451/1-1981Plastics—Determination of Ash; Part 1: currently practiced industrial techniques for identification and
General Methods classification of contaminants in recycled plastics flake or
ISO 1183-1987Methods for Determining the Density and pellets.
Relative Density of Noncellular Plastics
6. Sampling
3. Terminology
6.1 Unless otherwise stated, materials should be sampled in
3.1 This terminology used in this guide is in accordance accordance with the procedures described in Practice D1898.
with Terminology D883 and Guide D5033. Adequate statistical sampling should be considered as an
acceptable alternative.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 chemicals—nonhazardous or hazardous materials (for
7. Existing ASTM or ISO Procedures
example,insecticidesorherbicides)potentiallyusedincontact
with plastic materials. 7.1 Moisture:
7.1.1 A coulometric method (Test Method D4019), the
3.2.2 glue—adhesives used for labels or joining bottle parts
standard test method for haze (Test Method D1003), Karl
(for example, ethylene-vinyl acetate).
Fisher titration (Test Method D789), or a gravimetric proce-
3.2.3 heavy metals—metals heavier than sodium on the
dure (13.6.1 of Specification D1457) can be used to estimate
periodic table (for example, lead, arsenic, cadmium,
the moisture content of recycled plastic materials.
chromium, or copper).
7.2 Visual Inspection and Product Uniformity:
3.2.4 heavy plastic—unfilled polymers such as polystyrene,
7.2.1 Color:
poly(ethylene terephthalate), and poly(vinyl chloride) and
7.2.1.1 Test Method D1925 measures the yellowness index
filled materials with densities greater than 1.00g/cm .
of clear acrylic plastics and the haze and the luminous
3.2.5 light plastic—polymers such as polyethylene and
transmittance procedure (Test Method D1003) characterizes
polypropylene with densities less than 1.00 g/cm .
the color of transparent unpigmented recycled plastic materi-
als. These tests are not readily applied to pigmented plastic
3.2.6 original-product residues—residues from any
original-product contents of a plastic package (for example, samples.
milk, juice, or detergent).
NOTE 2—Test Method D1925 is currently being revised by ASTM
Subcommittee D20.40 to address reproducibility and bias problems.
3.2.7 particles—piece of metal, glass, wood, paper, or other
discreetly shaped material equal to or larger than 0.1 mm .
7.2.2 Melt Flow for Product Uniformity—Uniformity of
some recycled plastic flakes or pellets can be estimated by
3.2.8 specks—any material equal to or less than 0.1 mm .
measuring the flow rate of the material using an extrusion
plastometer (Test Method D1238).
4. Summary of Guide
7.3 Density or Specific Gravity—The displacement method
4.1 Thisguideprovidesdetailsofseveralproceduresusedto
for specific gravity or relative density (Test Method D792)or
separate and classify contaminants including, but not limited
the density-gradient procedure for density (Test Method
to, moisture, original product residues, incompatible plastic,
D1505) are useful techniques to determine contamination of
metal, paper, glass, adhesives, and wood in recycled plastic
recycledplasticflakesorpelletsampleswithoneormoreother
flakes or pellets. This guide lists existing ASTM and ISO
polymers.
methods that can be used to characterize solid and some liquid
contaminants. In addition, this guide presents details of some
NOTE3—TestMethodD1505usesrelativelysmalltestspecimens,soit
industry procedures for identification of contaminants. Appen-
may not be applicable for analysis of nonhomogeneous recycled plastic
materials.
dixX1providesinformationonquantitativeaspectsofsomeof
these industry standards that can also be used to estimate the
7.4 Inorganic Contaminants:
concentration of various contaminants.
7.4.1 Anashtest,suchasISO3451/1,orthemuffle-furnace
techniques currently being evaluated within ASTM Subcom-
5. Significance and Use
mittee D20.70 (project designation X70-8702) can be used to
estimate the inorganic filler content of recycled plastic flake or
5.1 Recycled plastic materials may contain incompatible
pellets.
plastic or other undesirable contaminants that could affect the
processingorquality,orboth,oftheplasticpreparedforreuse.
NOTE 4—Some volatile metals may be lost using the test indicated in
Techniques to separate and identify incompatible plastics, 7.4.1.ASTMSubcommitteeD20.70iscurrentlydevelopingatestmethod
(project X70-9201) for metals, including heavy metals, that will include
moisture, chemicals, or original product residues, and solid
sample-preparation techniques to minimize the loss of volatile metals
contaminants such as metals, paper, glass, and wood are
prior to analysis by X-ray fluorescence or spectroscopic techniques.
essential to the processing of recycled plastic materials.
7.4.2 Ferrous (iron) contaminants can be removed with a
magnet and aluminum contaminants are separated from plastic
materials using density procedures in accordance with 8.3.
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. 7.5 Thermal Analysis:
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D5577 − 94 (2010)
7.5.1 Since most polymers exhibit unique temperatures for 8.3.1 and 8.3.2 with a portion of virgin resin representing the
melting or other phase transitions, measurement of these bulkofthetestmaterial(forexample,poly(ethyleneterephtha-
transition temperatures (Test Method D3418) or the melting late) (PET) if you are interested in contaminants in recycled
and crystallization temperatures (Test Method E794)ofa PET).
sample may provide useful information regarding the identity
NOTE6—Thepresenceofgluecontaminationisindicatedbybondingof
ofpolymericcomponentspresentinarecycledplasticmaterial.
theplastictothepolyestersheetusedasareleasematerialduringmolding
7.5.2 Both Test Methods D3418 and E794 involve thermal
of the plaque.
NOTE 7—An alternative procedure for poly(ethylene terephthalate)
gravimetric analysis (TGA) or differential scanning calorim-
involves melting pellets for 10 min at 275°C in an aluminum pan. This
etry (DSC). These techniques utilize small samples (5 to 15
melt is rapidly quenched in ice water to prevent crystallization and the
mg),sotheymaynotbepracticalforuseincharacterizationof
resulting disk or plaque is visually inspected for contaminants and black
potentially nonhomogeneous recycled plastic materials.
specks by comparison with a control disk or plaque prepared from virgin
PET.Inthiscase,blackspecksareattributedtodegradedpaper,adhesives,
7.6 Infrared Analysis—Qualitative infrared analysis using
poly(vinylchloride),orothercontaminantsinthepoly(ethyleneterephtha-
the techniques of Practice E1252 can be used to identify
late).
polymeric, chemical, and, in some cases, inorganic compo-
8.3 Separations Based on Density:
nents of recycled plastic materials. Sample size considerations
8.3.1 Water-Density Separation:
indicatedin7.5.2mayalsoapplytopreparationofsamplesfor
8.3.1.1 Fillacleanplasticcontainerwith2Lofcleanwater.
infrared analysis.
Add sufficient nonionic surfactant to make a 2% (weight/
7.7 Chromatographic Analysis—The principles of gas
volume) solution and mix thoroughly.
chromatography, described in Practice E355, and liquid
NOTE 8—Acknowledging that water quality varies from one part of the
chromatography, described in Practice E682, are useful for
countrytoanother,minimumwaterqualityforthistestincludesproperties
separation and classification of chemical contaminants or
of Type III grade reagent water as defined in Specification D1193.
residues from original-use contents of plastic packages.
NOTE 9—Air pockets within flake material may cause the material to
fold back on itself. The surfactant (for example, Triton X-100 ) helps
eliminate this problem with plastic flakes.
8. Additional Industrial Procedures
8.3.1.2 Obtain a representative sample of recycled plastic
8.1 Specimen Preparation:
flakes (see 6.1) and weigh 100 6 10 g into a clean, dry plastic
8.1.1 Using standard injection molding equipment, prepare
container.
homogenized sample plaques.
8.1.2 Plaques, or slices from plaques prepared in 8.1.1, can
NOTE 10—The sample should be free of particles identified by a
procedure such as that described in 8.1.
be used for differential scanning calorimetry (DSC), infrared
analysis, and other test procedures requiring small, homoge-
8.3.1.3 Add the surfactant solution from 8.3.1.1 to the
neous specimens.
sample container and mix well with a spatula.Allow solids to
settle for at least 5 min.
8.2 Visible Inspection Procedures:
8.3.1.4 Skim light plastic and any contaminants (for
8.2.1 Inspection Table for Large, Visible Contaminants:
example,paper)fromthetopofthewaterusingasmallkitchen
8.2.1.1 Using a laboratory spatula, spread 450 620gof
strainer. Transfer these materials to a larger strainer and rinse
recycled plastic flakes or pellets on a clean, white inspection
with water to remove residual surfactant.
table.
8.3.1.5 Pour the remaining contents from the sample con-
8.2.1.2 Without the benefit of magnification, describe the
tainer (see 8.3.1.4) through another large strainer and wash
types of individual contaminant “particles” as defined in 3.2.7,
these heavier materials with water to remove residual surfac-
thenusing10×magnification,describethe“specks”asdefined
tant.
in 3.2.8.
8.3.1.6 If desired, these collected heavy materials are dried
8.2.1.3 Thermal techniques (see 7.5) and infrared analysis
and characterized by thermal (see 7.5) or infrared (see 7.6)
(see 7.6) can be used to identify some of the isolated contami-
techniques.
nants.
8.3.2 Propanol/Water Density Separation:
NOTE 5—To obtain a quantitative estimate of the contaminants, these
8.3.2.1 Add 1840 mL of 2-propanol and 1660 mL of water
contaminants can be removed and weighed, but there is not existing
(drinking, distilled, or deionized) to a 4-L plastic bottle. Mix
precision and bias data related to this estimated contaminant concentra-
well to provide a solution containing 52% (volume:volume)
tions in recycled plastics.
2-propanol in water.
8.2.2 Inspection of Molded Specimens or Plaques:
8.3.2.2 Pour 200 mL of the solution from 8.3.2.1 into a
8.2.2.1 Weigh 4 to5gofdry plastic flake on to a polyester
500-mLgraduatedcylinderandmeasurethespecificgravityof
sheet or aluminum foil in a 15.2 by 15.2 by 0.013-cm mold.
this solution with a hydrometer.The specific gravity should b
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