ASTM F2013-10

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

SIGNIFICANCE AND USE
This test method is of particular use as a quality control tool for a molding or synthesis operation. Acetaldehyde is a volatile degradation product generated during melt processing of PET. Thus, it becomes trapped in the sidewalls of a molded article and desorbs slowly into the contents packaged therein. In some foods and beverages AA can impart an off-taste that is undesirable, thus, it is important to know its concentration in PET articles that are to be used in food contact applications.
The desorption conditions of 150 C for 60 min are such that no measurable AA is generated by the sample during the desorption process.
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, as opposed to the bottle test, Test Method D4509, an acetaldehyde test requiring 24 h of desorption time at 23°C into the bottle headspace and then the concentration of the headspace quantified by a similar GC method.
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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2010
• ICS: 55.100 - Bottles. Pots. Jars
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.15 - Chemical/Safety Properties

Relations

• Replaces: 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-Oct-2010

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 10
StandardTest 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 F2013; 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 a gas chromatographic proce- 3.1 The terms employed in this test method are commonly
dure for the determination of the ppm residual acetaldehyde used in normal laboratory practice and require no special
(AA) present in poly(ethylene terephthalate) (PET) homo- comment.
polymers and co-polymers which are used in the manufacture
4. Summary of Test Method
of beverage bottles. This includes sample types of both
4.1 A specified size (< 1000 µm) of granulated sample is
amorphous and solid-stated pellet and preform samples, as
weighed into a 20-mLhead-space vial, sealed, and then heated
opposedtothebottletest,TestMethodD4509,anacetaldehyde
at 150°C for 60 min. After heating, the gas above the sealed
test requiring 24 h of desorption time at 23°C into the bottle
sampleofPETpolymerisinjectedontoacapillaryGCcolumn.
headspace and then the concentration of the headspace quan-
The acetaldehyde is separated, and the ppm of acetaldehyde is
tified by a similar GC method.
calculated.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 5. Significance and Use
standard.
5.1 This test method is of particular use as a quality control
1.3 This standard does not purport to address all of the tool for a molding or synthesis operation. Acetaldehyde is a
safety concerns, if any, associated with its use. It is the
volatile degradation product generated during melt processing
responsibility of the user of this standard to establish appro- of PET. Thus, it becomes trapped in the sidewalls of a molded
priate safety and health practices and determine the applica-
article and desorbs slowly into the contents packaged therein.
bility of regulatory limitations prior to use.
In some foods and beveragesAAcan impart an off-taste that is
undesirable, thus, it is important to know its concentration in
2. Referenced Documents
PET articles that are to be used in food contact applications.
2
2.1 ASTM Standards: 5.2 The desorption conditions of 150 C for 60 min are such
D4509 Test Methods for Determining the 24-Hour Gas
that no measurable AA is generated by the sample during the
(AIR)SpaceAcetaldehydeContentofFreshlyBlownPET desorption process.
3
Bottles (Withdrawn 2004)
6. Sources of Error
E691 Practice for Conducting an Interlaboratory Study to
6.1 Abias is known to exist if the ratio of sample mass (mg)
Determine the Precision of a Test Method
to head-space vial volume (mL) exceeds a value of ten.
6.2 Acetaldehyde is very volatile and must be handled
1
This test method is under the jurisdiction ofASTM Committee F02 on Flexible carefullytoavoidsamplelossduringthecalibrationprocedure.
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
Storing the standard vials in a refrigerator (4 6 2°C) is a must
Chemical/Safety Properties.
to minimize the error due to volatility.
Current edition approved Oct. 1, 2010. Published October 2010. Originally
approved in 2000. Last previous edition published in 2005 as F2013 – 05. DOI:
6.3 Failuretoachieveatightsealonthehead-spacevialwill
10.1520/F2013-10.
result in the loss of acetaldehyde during storage and
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
desorption, producing a false low value.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
6.4 Failure to grind the sample to the appropriate particle
the ASTM website.
3
size may lead to a false low value for residual AA due to the
The last approved version of this historical standard is referenced on
www.astm.org. increased path length for desorption.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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F2013 − 10
6.5 Samples submitted for “residual AA measurement” 9.2 Using the syringe, fill it by placing the tip in the liquid
should be stored in a freezer (< –10°C) until they are tested. standard and quickly moving the plunger up and down several
Failure to do so can result in lower than expected results. time to evacuate any bubbl
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:F2013–05 Designation:F2013–10
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 F2013; 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
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, as opposed to the bottle test,
Test Method D4509, an acetaldehyde test requiring 24 h of desorption time at 23°C into the bottle headspace and then the
concentration of the headspace quantified by a similar GC method.
1.2
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D4509 Test Methods for Determining the 24-Hour Gas (AIR) Space Acetaldehyde Content of Freshly Blown PET Bottles
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 The terms employed in this test method are commonly used in normal laboratory practice and require no special comment.
4. Summary of Test Method
4.1 Aspecified size (800 to(< 1000 µm) of granulated sample is weighed into a 20-mLhead-space vial, sealed, and then heated
at 150°C for 60 min.After heating, the gas above the sealed sample of PET polymer is injected onto a capillary GC column. The
acetaldehyde is separated, and the ppm of acetaldehyde is calculated.
5. Significance and Use
5.1 This test method is of particular use as a quality control tool for a molding or synthesis operation.Acetaldehyde is a volatile
degradation product generated during melt processing of PET. Thus, it becomes trapped in the sidewalls of a molded article and
desorbsslowlyintothecontentspackagedtherein.InsomefoodsandbeveragesAAcanimpartanoff-tastethatisundesirable,thus,
it is important to know its concentration in PET articles that are to be used in food contact applications.
5.2 The desorption conditions of 150 C for 60 min are such that no measurable AA is generated by the sample during the
desorption process.
1
This test method is under the jurisdiction ofASTM Committee F02 on Flexible Barrier MaterialsPackaging and is the direct responsibility of Subcommittee F02.15 on
Chemical/Safety Properties.
Current edition approved April 1, 2005. Published September 2005. Originally approved in 2000 as published as F2013–00. Last previous edition approved in 2001 as
F2013–01. DOI: 10.1520/F2013-05.
Current edition approved Oct. 1, 2010. Published October 2010. Originally approved in 2000. Last previous edition published in 2005 as F2013 – 05. DOI:
10.1520/F2013-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
F2013–10
6. Sources of Error
6.1 A bias is known to exist if the ratio of sample mass (mg) to head-space vial volume (mL) exceeds a value of ten.
6.2 Acetaldehyde is very volatile and must be handled carefully to avoid sample loss during the calibration procedure. Storing
the standard vials in a refrigerator (4 6 2°C) is a must to minimize the error due to volatility.
6.3 Failure to achieve a tight seal on the head-space vial will result in the loss of acetaldehyde during storage and desorption,
producing a false low value.
6.4 Failure to grind the sample to the appropriate particle size may
...