ASTM F2013-01

Standard Test Method for Determination of Residual Acetaldehyde in Polyethylene Terephthalate Bottle Polymer Using an Automated Static Head-Space Sampling Device and a Capillary GC with a Flame Ionization Detector

SCOPE
1.1 This test method covers a gas chromatographic procedure for the determination of the ppm residual acetaldehyde (AA) present in poly(ethylene terephthalate) (PET) homo-polymers and co-polymers which are used in the manufacture of beverage bottles. This includes sample types of both amorphous and solid-stated pellet and preform samples.
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.

General Information

• Status: Historical
• Publication Date: 09-Apr-2001
• ICS: 55.100 - Bottles. Pots. Jars
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.30 - Mechanical Dispensers

Relations

• Replaces: ASTM F2013-00 - Standard Test Method for Determination of Residual Acetaldehyde in Polyethylene Terephthalate Bottle Polymer Using an Automated Static Head-Space Sampling Device and a Capillary GC with a Flame Ionization Detector
• Effective Date: 10-Apr-2001
• Replaced By: ASTM F2013-05 - Standard Test Method for Determination of Residual Acetaldehyde in Polyethylene Terephthalate Bottle Polymer Using an Automated Static Head-Space Sampling Device and a Capillary GC with a Flame Ionization Detector
• Effective Date: 01-Apr-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:F2013–01
Standard Test Method for
Determination of Residual Acetaldehyde in Polyethylene
Terephthalate Bottle Polymer Using an Automated Static
Head-Space Sampling Device and a Capillary GC with a
1
Flame Ionization Detector
This standard is issued under the fixed designation F 2013; 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 heated at 150°C for 60 min. After heating, the gas above the
sealed sample of PET polymer is injected onto a capillary GC
1.1 This test method covers a gas chromatographic proce-
column. The acetaldehyde is separated, and the ppm of
dure for the determination of the ppm residual acetaldehyde
acetaldehyde is calculated.
(AA) present in poly(ethylene terephthalate) (PET) homo-
polymers and co-polymers which are used in the manufacture
5. Significance and Use
of beverage bottles. This includes sample types of both
5.1 This test method is of particular use as a quality control
amorphous and solid-stated pellet and preform samples.
tool for a molding or synthesis operation. Acetaldehyde is a
1.2 This standard does not purport to address all of the
volatile degradation product generated during melt processing
safety concerns, if any, associated with its use. It is the
of PET. Thus, it becomes trapped in the sidewalls of a molded
responsibility of the user of this standard to establish appro-
article and desorbs slowly into the contents packaged therein.
priate safety and health practices and determine the applica-
In some foods and beveragesAAcan impart an off-taste that is
bility of regulatory limitations prior to use.
undesirable, thus, it is important to know its concentration in
2. Referenced Documents PET articles that are to be used in food contact applications.
5.2 The desorption conditions of 150 C for 60 min are such
2.1 ASTM Standards:
that no measurable AA is generated by the sample during the
D 4509 TestMethodforDeterminingthe24-HourGas(Air)
desorption process.
Space Acetaldehyde Content of Freshly Blown PET
2
Bottles
6. Sources of Error
E 691 Practice for Conducting an Interlaboratory Study to
3 6.1 Abiasisknowntoexistiftheratioofsamplemass(mg)
Determine the Precision of a Test Method
to head-space vial volume (mL) exceeds a value of ten.
3. Terminology 6.2 Acetaldehyde is very volatile and must be handled
carefullytoavoidsamplelossduringthecalibrationprocedure.
3.1 The terms employed in this test method are commonly
Storing the standard vials in a refrigerator is a must to
used in normal laboratory practice and require no special
minimize the error due to volatility.
comment.
6.3 Failuretoachieveatightsealonthehead-spacevialwill
4. Summary of Test Method result in the loss of acetaldehyde during storage and desorp-
tion, producing a false low value.
4.1 Aspecified size (800 to 1000 µm) of granulated sample
6.4 Failure to grind the sample to the appropriate particle
is weighed into a 20-mL head-space vial, sealed, and then
size may lead to a false low value for residual AA due to the
increased path length for desorption.
1 6.5 Samples submitted for 8residual AA measurement’
This test method is under the jurisdiction ofASTM Committee F02 on Flexible
should be stored in a freezer until they are tested. Failure to do
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
Methods.
so can result in lower than expected results.
Current edition approvedApril 2001. Published June 2001. Originally published
6.6 Excessive grinding of samples can cause residual AA
as F 2013 – 00. Last previous edition F 2013 – 00.
2
contained therein to be desorbed. Extensive excessive grinding
Annual Book of ASTM Standards, Vol 08.03.
3
Annual Book of ASTM Standards, Vol 14.02. can lead to actual melting of the polymer and AA generation.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
F2013
Samples which have been chilled in liquid nitrogen properly 8.2 Liquid Nitrogen, plant grade (R-3, S-3).
should only be in the grinder for ;30 s or less.
9. Calibration and Standardization
7. Apparatus
NOTE 1—The following procedure should be performed and recorded
4
7.1 Gas Chromatograph, Hewlett-Packard 6890 series
once every three months.
7.2 Integrator, Hewlett-Packard Model 6890 series, H-P
4
9.1 Break open a certified AA standard ampule (ampules
ChemStation, H-P LAN.
4 must be stored in a refrigerator) or prepareAAstandard by the
7.3 Head-Space Sampler, Hewlett-Packard 7694.
attached supplemental procedure. (See Appendix X5.)
7.
...