ASTM F1349-08(2019)
(Test Method)Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors (Withdrawn 2024)
Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors (Withdrawn 2024)
ABSTRACT
This test method establishes the apparatuses required, the standard procedures, and associated calculations involved in the determination of relatively polar nonvolatile ultraviolet (UV) absorbing extractable components that may migrate from microwave susceptor packaging into food simulants, such as corn oil and Miglyol 812. This test method has been collaboratively studied using bilaminate susceptors constructed of paperboard, adhesive, and a layer of polyethylene terephthalate polymer (PETE) susceptor.
SCOPE
1.1 This test method covers the determination of nonpolar and relatively polar ultraviolet (UV) absorbing components that may migrate from microwave susceptor packaging into food simulants, such as corn oil and Miglyol 812.
1.2 This test method has been collaboratively studied using bilaminate susceptors constructed of paperboard, adhesive, and a layer of polyethylene terephthalate polymer (PETE) susceptor. Adhesive and PETE related compounds were quantitated using this test method.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 4.3.2.3.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
WITHDRAWN RATIONALE
This test method covered the determination of nonpolar and relatively polar ultraviolet (UV) absorbing components that may migrate from microwave susceptor packaging into food simulants, such as corn oil and Miglyol 812.
Formerly under the jurisdiction of Committee F02 on Primary Barrier Packaging, this test method was withdrawn in April 2024. This standard is being withdrawn without replacement due to its limited use by industry.
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:F1349 −08 (Reapproved 2019)
Standard Test Method for
Nonvolatile Ultraviolet (UV) Absorbing Extractables from
Microwave Susceptors
This standard is issued under the fixed designation F1349; 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. Apparatus and Reagents
1.1 This test method covers the determination of nonpolar
3.1 Microwave Oven, 700 6 35 W, calibrated. Refer to Test
and relatively polar ultraviolet (UV) absorbing components
Method F1317.
that may migrate from microwave susceptor packaging into
3.2 High-Pressure Liquid Chromatograph (HPLC), consist-
food simulants, such as corn oil and Miglyol 812.
ing of:
1.2 This test method has been collaboratively studied using
3.2.1 Pump, capable of 1.5 mL/min with flow precision
bilaminatesusceptorsconstructedofpaperboard,adhesive,and
62%.
a layer of polyethylene terephthalate polymer (PETE) suscep-
3.2.2 Injector, loop-type, equipped with 20-µL loop.
tor. Adhesive and PETE related compounds were quantitated
3.2.3 Guard Column, C , 5 µm.
using this test method.
3.2.4 Analytical Column, C , 5 µm, 250 by 4.6 mm.
1.3 The values stated in SI units are to be regarded as
3.2.5 Detector-UV Absorbance, set for 254 nm. Adjust
standard. No other units of measurement are included in this
sensitivity to give a 70 to 100 % of full scale peak for the 5-
standard.
ppm dimethylterephthalate DMT standard.
1.4 This standard does not purport to address all of the
3.2.6 Gradient Program, 4 to 60 % Mobile Phase B in 8
safety concerns, if any, associated with its use. It is the
min; 60 to 70 % B in 9 min; 70 to 100 % B in 7 min; 100 % B
responsibility of the user of this standard to establish appro-
for 11 min; 100 to 4 % B in 5 min; 4 % B for minimum of 5
priate safety, health, and environmental practices and deter-
min. Where Mobile Phase A (v/v) is 85 + 15 + 0.25 %
mine the applicability of regulatory limitations prior to use.
water:acetonitrile:acetic acid, and Mobile Phase B (v/v)is
Specific warning statements are given in 4.3.2.3.
15 + 85 % water:acetonitrile.
1.5 This international standard was developed in accor-
3.2.7 Peak Area Integration System—Initialize data acqui-
dance with internationally recognized principles on standard-
sition or integration system, or both, from 5 to 35 min during
ization established in the Decision on Principles for the
the separation.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.3 Hexane, LC/UV grade.
Barriers to Trade (TBT) Committee.
3.4 Acetonitrile, LC/UV grade.
2. Referenced Documents
3.5 Corn Oil—Obtain corn oil that is as pure and fresh as
possible to minimize peaks in nonvolatiles extractables chro-
2.1 ASTM Standards:
matogram. Alternatively, Miglyol 812 (a fractionated coconut
F874 Test Method for Temperature Measurement and Pro-
oil)orsyntheticfatsimulantHB307canbeusedasasubstitute
filing for Microwave Susceptors
for corn oil.
F1317 Test Method for Calibration of Microwave Ovens
3.6 Dimethylacetamide (DMAC), LC/UV grade.
3.7 Conical Bottom Test Tubes, 50 mL, graduated.
This test method is under the jurisdiction ofASTM Committee F02 on Primary
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
3.8 Bishydroxyethyleneterephthalate (BHET).
Chemical/Safety Properties.
Current edition approved March 1, 2019. Published May 2019. Originally
3.9 Diethylterephthalate (DET).
approved in 1991. Last previous edition approved in 2014 as F1349 – 08(2014).
DOI: 10.1520/F1349-19.
3.10 Dimethylterephthalate (DMT).
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
3.11 Fluoroptic Thermometry System.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 3.12 Temperature Probes, four, high temperature.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1349−08 (2019)
expeditedbyusingiceinbeakersorcrystallizationdishesorbyusingcold
3.13 Glass Beads, 3 to 4 mm, clean thoroughly by rinsing
packs such as “blue ice.”
with methylene chloride followed by soaking for 30 min in
acetonitrile. Dry thoroughly before using.
4.2.1 Select a representative piece of the susceptor sample
to be tested. If the susceptor is part of a package, trim excess
3.14 Recommended Microwave Nonvolatile Extraction
material from around susceptor. Determine the area of the
Cell—Waldorf Polytetrafluoroethylene cell. (See Figs. 1-3).
activesusceptormaterial.Thesusceptorshouldbecuttofitinto
This cell must be constructed by a machine shop experienced
a Waldorf PTFE Cell with the screw seal ring firmly seated
in working with polytetrafluoroethylene (PTFE). After micro-
against the susceptor surface. Use of the Waldorf PTFE cell
waving oil in the cell, the cell should be rinsed with methylene
reduces the risk of spilling hot oil and in addition, gives a
chloride to remove residual oil and prevent carry-over.
reproducible surface area (53.5 cm ) for extraction.
3.15 Solvent Concentration Apparatus—Kuderna-Danish
Alternatively, cut a 13 by 18-cm rectangular piece of the active
evaporative concentrator, rotory evaporator; or Zymark Tur-
susceptor material, form an extraction boat with sides 1.5 cm
boVap at a nitrogen pressure of 30 psi and a water bath
high (boat configuration = 1.5 by 10 by 15 cm, approximately
temperature of 50°C.
150 cm of surface area). Staple the corners of the boat
securely.
4. Procedure
4.2.2 Add 53.2 g of Miglyol 812 of corn oil to the Waldorf
4.1 Temperature Measurement:
PTFECell.Alternatively,add22.5goiland75gofglassbeads
4.1.1 Refer to Test Method F874 to determine the time and
to the extraction boat.
water load specifications.
4.2.3 Measure the mass of the room-temperature distilled
4.2 Sample Preparation and Microwave Heating:
water load as determined in 4.1.1 into a 600-mL beaker and
add a boiling chip to this beaker.
NOTE1—Alwaysbesurethemicrowaveovenisatambienttemperature
before starting any temperature measurement or heating procedure to
4.2.4 PlaceWaldorfPTFECellorextractionboatcontaining
ensure consistency of output. Cooling of the microwave oven can be
the oil in the center of the microwave oven. Always position
cell/extraction boat in the same position for subsequent runs.
The sole source of supply of the apparatus known to the committee at this time
4.2.5 Insert the temperature sensing probes through pre-
is Read Plastics, 12331 Wilkins Ave., Rockville, MD 20852. If you are aware of
formed holes in the walls in Waldorf PTFE Cells (shown in
alternative suppliers, please provide this information to ASTM International
Fig. 1 and in the lower center sketch of Fig. 2), or in the case
Headquarters.Your comments will receive careful consideration at a meeting of the
of the extraction boat, tape the probe to the wall of the oven
responsible technical committee, which you may attend.
NOTE 1—The ⁄16-in. (1.6-mm) diameter hole is for a Luxtron MIW
temperature sensing probe. Number of holes and location may vary by
application.
FIG. 1Collar Section of Waldorf Polytetrafluoroethylene Micro-
wave Nonvolatile Extraction Cell
F1349−08 (2019)
NOTE 1—Relieve thread at bottom. Collar must seal to bottom of cap.
FIG. 2Cap Section of Waldorf Polytetrafluorethylene Nonvolatile
Extraction Cell
FIG. 3 Suggested Modifications to Waldorf Cell
such that the probe tip maintains contact with the extraction
F1349−08 (2019)
boat. Manipulate the probes until they make good firm contact 4.3.2.10 For reference, various oligomers of polyethylene
with the active face of the susceptor material. terephthalate (PETE) will have the following retention times
relative to DET:
4.2.6 Microwave the cell or alternate extraction boat using
the time specifications as determined in Test Method F874.
cyclic trimer = 2.8
tetramer = 5.2
Record the probe temperatures, preferably at 5-s intervals, but
pentamer = 6.8
at intervals not to exceed 15 s.
hexamer = 7.8
heptamer = 8.8
4.3 Quantitative Analysis:
octamer = 9.8
4.3.1 Standard Curve:
nonamer = 10.2
4.3.1.1 Prepare a standard mixture of 10 ppm (w/v) each of
4.3.2.11 Subtract blank oil peak contributions from the
BHET, DMT, DET, and any other identified UV components
...
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: F1349 − 08 (Reapproved 2019)
Standard Test Method for
Nonvolatile Ultraviolet (UV) Absorbing Extractables from
Microwave Susceptors
This standard is issued under the fixed designation F1349; 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. Apparatus and Reagents
1.1 This test method covers the determination of nonpolar
3.1 Microwave Oven, 700 6 35 W, calibrated. Refer to Test
and relatively polar ultraviolet (UV) absorbing components
Method F1317.
that may migrate from microwave susceptor packaging into
3.2 High-Pressure Liquid Chromatograph (HPLC), consist-
food simulants, such as corn oil and Miglyol 812.
ing of:
1.2 This test method has been collaboratively studied using
3.2.1 Pump, capable of 1.5 mL/min with flow precision
bilaminate susceptors constructed of paperboard, adhesive, and
62 %.
a layer of polyethylene terephthalate polymer (PETE) suscep-
3.2.2 Injector, loop-type, equipped with 20-µL loop.
tor. Adhesive and PETE related compounds were quantitated
3.2.3 Guard Column, C , 5 µm.
using this test method.
3.2.4 Analytical Column, C , 5 µm, 250 by 4.6 mm.
1.3 The values stated in SI units are to be regarded as
3.2.5 Detector-UV Absorbance, set for 254 nm. Adjust
standard. No other units of measurement are included in this
sensitivity to give a 70 to 100 % of full scale peak for the 5-
standard.
ppm dimethylterephthalate DMT standard.
1.4 This standard does not purport to address all of the
3.2.6 Gradient Program, 4 to 60 % Mobile Phase B in 8
safety concerns, if any, associated with its use. It is the
min; 60 to 70 % B in 9 min; 70 to 100 % B in 7 min; 100 % B
responsibility of the user of this standard to establish appro-
for 11 min; 100 to 4 % B in 5 min; 4 % B for minimum of 5
priate safety, health, and environmental practices and deter-
min. Where Mobile Phase A (v/v) is 85 + 15 + 0.25 %
mine the applicability of regulatory limitations prior to use.
water:acetonitrile:acetic acid, and Mobile Phase B (v/v) is
Specific warning statements are given in 4.3.2.3.
15 + 85 % water:acetonitrile.
1.5 This international standard was developed in accor-
3.2.7 Peak Area Integration System—Initialize data acqui-
dance with internationally recognized principles on standard-
sition or integration system, or both, from 5 to 35 min during
ization established in the Decision on Principles for the
the separation.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.3 Hexane, LC/UV grade.
Barriers to Trade (TBT) Committee.
3.4 Acetonitrile, LC/UV grade.
2. Referenced Documents
3.5 Corn Oil—Obtain corn oil that is as pure and fresh as
possible to minimize peaks in nonvolatiles extractables chro-
2.1 ASTM Standards:
matogram. Alternatively, Miglyol 812 (a fractionated coconut
F874 Test Method for Temperature Measurement and Pro-
oil) or synthetic fat simulant HB 307 can be used as a substitute
filing for Microwave Susceptors
for corn oil.
F1317 Test Method for Calibration of Microwave Ovens
3.6 Dimethylacetamide (DMAC), LC/UV grade.
3.7 Conical Bottom Test Tubes, 50 mL, graduated.
This test method is under the jurisdiction of ASTM Committee F02 on Primary
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
3.8 Bishydroxyethyleneterephthalate (BHET).
Chemical/Safety Properties.
Current edition approved March 1, 2019. Published May 2019. Originally
3.9 Diethylterephthalate (DET).
approved in 1991. Last previous edition approved in 2014 as F1349 – 08(2014).
DOI: 10.1520/F1349-19.
3.10 Dimethylterephthalate (DMT).
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
3.11 Fluoroptic Thermometry System.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 3.12 Temperature Probes, four, high temperature.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1349 − 08 (2019)
expedited by using ice in beakers or crystallization dishes or by using cold
3.13 Glass Beads, 3 to 4 mm, clean thoroughly by rinsing
packs such as “blue ice.”
with methylene chloride followed by soaking for 30 min in
acetonitrile. Dry thoroughly before using.
4.2.1 Select a representative piece of the susceptor sample
to be tested. If the susceptor is part of a package, trim excess
3.14 Recommended Microwave Nonvolatile Extraction
material from around susceptor. Determine the area of the
Cell—Waldorf Polytetrafluoroethylene cell. (See Figs. 1-3).
active susceptor material. The susceptor should be cut to fit into
This cell must be constructed by a machine shop experienced
a Waldorf PTFE Cell with the screw seal ring firmly seated
in working with polytetrafluoroethylene (PTFE). After micro-
against the susceptor surface. Use of the Waldorf PTFE cell
waving oil in the cell, the cell should be rinsed with methylene
reduces the risk of spilling hot oil and in addition, gives a
chloride to remove residual oil and prevent carry-over.
reproducible surface area (53.5 cm ) for extraction.
3.15 Solvent Concentration Apparatus—Kuderna-Danish
Alternatively, cut a 13 by 18-cm rectangular piece of the active
evaporative concentrator, rotory evaporator; or Zymark Tur-
susceptor material, form an extraction boat with sides 1.5 cm
boVap at a nitrogen pressure of 30 psi and a water bath
high (boat configuration = 1.5 by 10 by 15 cm, approximately
temperature of 50°C. 2
150 cm of surface area). Staple the corners of the boat
securely.
4. Procedure
4.2.2 Add 53.2 g of Miglyol 812 of corn oil to the Waldorf
4.1 Temperature Measurement:
PTFE Cell. Alternatively, add 22.5 g oil and 75 g of glass beads
4.1.1 Refer to Test Method F874 to determine the time and
to the extraction boat.
water load specifications.
4.2.3 Measure the mass of the room-temperature distilled
4.2 Sample Preparation and Microwave Heating:
water load as determined in 4.1.1 into a 600-mL beaker and
add a boiling chip to this beaker.
NOTE 1—Always be sure the microwave oven is at ambient temperature
before starting any temperature measurement or heating procedure to
4.2.4 Place Waldorf PTFE Cell or extraction boat containing
ensure consistency of output. Cooling of the microwave oven can be
the oil in the center of the microwave oven. Always position
cell/extraction boat in the same position for subsequent runs.
The sole source of supply of the apparatus known to the committee at this time
4.2.5 Insert the temperature sensing probes through pre-
is Read Plastics, 12331 Wilkins Ave., Rockville, MD 20852. If you are aware of
formed holes in the walls in Waldorf PTFE Cells (shown in
alternative suppliers, please provide this information to ASTM International
Fig. 1 and in the lower center sketch of Fig. 2), or in the case
Headquarters. Your comments will receive careful consideration at a meeting of the
of the extraction boat, tape the probe to the wall of the oven
responsible technical committee, which you may attend.
NOTE 1—The ⁄16-in. (1.6-mm) diameter hole is for a Luxtron MIW
temperature sensing probe. Number of holes and location may vary by
application.
FIG. 1 Collar Section of Waldorf Polytetrafluoroethylene Micro-
wave Nonvolatile Extraction Cell
F1349 − 08 (2019)
NOTE 1—Relieve thread at bottom. Collar must seal to bottom of cap.
FIG. 2 Cap Section of Waldorf Polytetrafluorethylene Nonvolatile
Extraction Cell
FIG. 3 Suggested Modifications to Waldorf Cell
such that the probe tip maintains contact with the extraction
F1349 − 08 (2019)
boat. Manipulate the probes until they make good firm contact 4.3.2.10 For reference, various oligomers of polyethylene
with the active face of the susceptor material. terephthalate (PETE) will have the following retention times
4.2.6 Microwave the cell or alternate extraction boat using relative to DET:
the time specifications as determined in Test Method F874.
cyclic trimer = 2.8
tetramer = 5.2
Record the probe temperatures, preferably at 5-s intervals, but
pentamer = 6.8
at intervals not to exceed 15 s.
hexamer = 7.8
heptamer = 8.8
4.3 Quantitative Analysis:
octamer = 9.8
4.3.1 Standard Curve:
nonamer = 10.2
4.3.1.1 Prepare a standard mixture of 10 ppm (w/v) each of
4.3.2.11 Subtract blank oil peak contributions from the
BHET, DMT, DET, and any other identified UV components
sample chromatograms. Sum all the remaining peak areas in
(see appendix) of the susceptor i
...
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