ASTM F1349-08(2014)
(Test Method)Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors
Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 4.3.2.3.
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Standards Content (Sample)
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Designation:F1349 −08 (Reapproved 2014)
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 3.2 High-Pressure Liquid Chromatograph (HPLC), consist-
ing of:
1.1 This test method covers the determination of nonpolar
3.2.1 Pump, capable of 1.5 mL/min with flow precision
and relatively polar ultraviolet (UV) absorbing components
62%.
that may migrate from microwave susceptor packaging into
3.2.2 Injector, loop-type, equipped with 20-µL loop.
food simulants, such as corn oil and Miglyol 812.
3.2.3 Guard Column, C , 5 µm.
1.2 This test method has been collaboratively studied using
3.2.4 Analytical Column, C , 5 µm, 250 by 4.6 mm.
bilaminatesusceptorsconstructedofpaperboard,adhesive,and
3.2.5 Detector-UV Absorbance, set for 254 nm. Adjust
a layer of polyethylene terephthalate polymer (PETE) suscep-
sensitivity to give a 70 to 100 % of full scale peak for the 5-
tor. Adhesive and PETE related compounds were quantitated
ppm dimethylterephthalate DMT standard.
using this test method.
3.2.6 Gradient Program, 4 to 60 % Mobile Phase B in 8
min; 60 to 70 % B in 9 min; 70 to 100 % B in 7 min; 100 % B
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this for 11 min; 100 to 4 % B in 5 min; 4 % B for minimum of 5
min. Where Mobile Phase A (v/v) is 85 + 15 + 0.25 %
standard.
water:acetonitrile:acetic acid, and Mobile Phase B (v/v)is
1.4 This standard does not purport to address all of the
15 + 85 % water:acetonitrile.
safety concerns, if any, associated with its use. It is the
3.2.7 Peak Area Integration System—Initialize data acqui-
responsibility of the user of this standard to establish appro-
sition or integration system, or both, from 5 to 35 min during
priate safety and health practices and determine the applica-
the separation.
bility of regulatory limitations prior to use. Specific warning
statements are given in 4.3.2.3.
3.3 Hexane, LC/UV grade.
3.4 Acetonitrile, LC/UV grade.
2. Referenced Documents
3.5 Corn Oil—Obtain corn oil that is as pure and fresh as
2.1 ASTM Standards:
possible to minimize peaks in nonvolatiles extractables chro-
F874 Test Method for Temperature Measurement and Pro-
matogram. Alternatively, Miglyol 812 (a fractionated coconut
filing for Microwave Susceptors
oil)orsyntheticfatsimulantHB307canbeusedasasubstitute
F1317 Test Method for Calibration of Microwave Ovens
for corn oil.
3. Apparatus and Reagents
3.6 Dimethylacetamide (DMAC), LC/UV grade.
3.1 Microwave Oven, 700 6 35 W, calibrated. Refer to Test
3.7 Conical Bottom Test Tubes, 50 mL, graduated.
Method F1317.
3.8 Bishydroxyethyleneterephthalate (BHET).
3.9 Diethylterephthalate (DET).
This test method is under the jurisdiction ofASTM Committee F02 on Flexible
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
3.10 Dimethylterephthalate (DMT).
Chemical/Safety Properties.
Current edition approved April 1, 2014. Published April 2014. Originally 3.11 Fluoroptic Thermometry System.
approved in 1991. Last previous edition approved in 2008 as F1349 – 08. DOI:
3.12 Temperature Probes, four, high temperature.
10.1520/F1349-08R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.13 Glass Beads, 3 to 4 mm, clean thoroughly by rinsing
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
with methylene chloride followed by soaking for 30 min in
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. acetonitrile. Dry thoroughly before using.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1349−08 (2014)
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
NOTE 1—Relieve thread at bottom. Collar must seal to bottom of cap.
FIG. 2Cap Section of Waldorf Polytetrafluorethylene Nonvolatile
Extraction Cell
F1349−08 (2014)
FIG. 3 Suggested Modifications to Waldorf Cell
3.14 Recommended Microwave Nonvolatile Extraction activesusceptormaterial.Thesusceptorshouldbecuttofitinto
Cell—Waldorf Polytetrafluoroethylene cell. (See Figs. 1-3). a Waldorf PTFE Cell with the screw seal ring firmly seated
This cell must be constructed by a machine shop experienced against the susceptor surface. Use of the Waldorf PTFE cell
in working with polytetrafluoroethylene (PTFE). After micro- reduces the risk of spilling hot oil and in addition, gives a
waving oil in the cell, the cell should be rinsed with methylene reproducible surface area (53.5 cm ) for extraction.
chloride to remove residual oil and prevent carry-over. Alternatively, cut a 13 by 18-cm rectangular piece of the active
susceptor material, form an extraction boat with sides 1.5 cm
3.15 Solvent Concentration Apparatus—Kuderna-Danish
high (boat configuration = 1.5 by 10 by 15 cm, approximately
evaporative concentrator, rotory evaporator; or Zymark Tur-
150 cm of surface area). Staple the corners of the boat
boVap at a nitrogen pressure of 30 psi and a water bath
securely.
temperature of 50°C.
4.2.2 Add 53.2 g of Miglyol 812 of corn oil to the Waldorf
4. Procedure PTFECell.Alternatively,add22.5goiland75gofglassbeads
to the extraction boat.
4.1 Temperature Measurement:
4.2.3 Measure the mass of the room-temperature distilled
4.1.1 Refer to Test Method F874 to determine the time and
water load as determined in 4.1.1 into a 600-mL beaker and
water load specifications.
add a boiling chip to this beaker.
4.2 Sample Preparation and Microwave Heating:
4.2.4 PlaceWaldorfPTFECellorextractionboatcontaining
NOTE1—Alwaysbesurethemicrowaveovenisatambienttemperature
the oil in the center of the microwave oven. Always position
before starting any temperature measurement or heating procedure to
cell/extraction boat in the same position for subsequent runs.
ensure consistency of output. Cooling of the microwave oven can be
4.2.5 Insert the temperature sensing probes through pre-
expeditedbyusingiceinbeakersorcrystallizationdishesorbyusingcold
formed holes in the walls in Waldorf PTFE Cells (shown in
packs such as “blue ice.”
Fig. 1 and in the lower center sketch of Fig. 2), or in the case
4.2.1 Select a representative piece of the susceptor sample
of the extraction boat, tape the probe to the wall of the oven
to be tested. If the susceptor is part of a package, trim excess
such that the probe tip maintains contact with the extraction
material from around susceptor. Determine the area of the
boat. Manipulate the probes until they make good firm contact
with the active face of the susceptor material.
The sole source of supply of the apparatus known to the committee at this time
4.2.6 Microwave the cell or alternate extraction boat using
is Read Plastics, 12331 Wilkins Ave., Rockville, MD 20852. If you are aware of
the time specifications as determined in Test Method F874.
alternative suppliers, please provide this information to ASTM International
Record the probe temperatures, preferably at 5-s intervals, but
Headquarters.Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. at intervals not to exceed 15 s.
F1349−08 (2014)
4.3 Quantitative Analysis:
cyclic trimer = 2.8
tetramer = 5.2
4.3.1 Standard Curve:
pentamer = 6.8
hexamer = 7.8
4.3.1.1 Prepare a standard mixture of 10 ppm (w/v) each of
heptamer = 8.8
BHET, DMT, DET, and any other identified UV components
octamer = 9.8
(see appendix) of the susceptor in DMAC. Proceed to generate
nonamer = 10.2
chromatograms using high pressure liquid chromatography in
4.3.2.11 Subtract blank oil peak contributions from the
accordance with 3.2.5, 3.2.6, and 4.3.2.8. Retention times for
sample chromatograms. Sum all the remaining peak areas in
BHET, DMT, and DET will be approximately 7.6, 16.6, and
the sample chromatogram.
21.5 min respectively.
4.3.
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