Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors

SCOPE
1.1 This test method covers the determination of 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 polyethylene terephthalate (PET) susceptor. Adhesive and PET related compounds were quantitated using this test method.  
1.3 The values stated in SI units are to be regarded as the 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 precautionary statements are given in 4.3.2.3.

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Publication Date
09-Oct-1998
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ASTM F1349-98 - Standard Test Method for Nonvolatile Ultraviolet (UV) Absorbing Extractables from Microwave Susceptors
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: F 1349 – 98
Standard Test Method for
Nonvolatile Ultraviolet (UV) Absorbing Extractables from
Microwave Susceptors
This standard is issued under the fixed designation F 1349; 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 3.2.5 Detector-UV Absorbance, set for 254 nm. Adjust
sensitivity to give a 70 to 100 % of full scale peak for the 5-
1.1 This test method covers the determination of relatively
ppm dimethylterephthalate DMT standard.
polar ultraviolet (UV) absorbing components that may migrate
3.2.6 Gradient Program, 4 to 60 % Mobile Phase B in 8
from microwave susceptor packaging into food simulants, such
min; 60 to 70 % B in 9 min; 70 to 100 % B in 7 min; 100 % B
as corn oil and Miglyol 812.
for 11 min; 100 to 4 % B in 5 min; 4 % B for minimum of 5
1.2 This test method has been collaboratively studied using
min. Where Mobile Phase A ( v/v) is 85 + 15 + 0.25 %
bilaminate susceptors constructed of paperboard, adhesive, and
water:acetonitrile:acetic acid, and Mobile Phase B (v/v)is
a layer of polyethylene terephthalate polymer (PETE) suscep-
15 + 85 % water:acetonitrile.
tor. Adhesive and PETE related compounds were quantitated
3.2.7 Peak Area Integration System—Initialize data acqui-
using this test method.
sition or integration system, or both, from 5 to 35 min during
1.3 The values stated in SI units are to be regarded as the
the separation.
standard.
3.3 Hexane, LC/UV grade.
1.4 This standard does not purport to address all of the
3.4 Acetonitrile, LC/UV grade.
safety concerns, if any, associated with its use. It is the
3.5 Corn Oil—Obtain corn oil that is as pure and fresh as
responsibility of the user of this standard to establish appro-
possible to minimize peaks in nonvolatiles extractables chro-
priate safety and health practices and determine the applica-
matogram. Alternatively, Miglyol 812 (a fractionated coconut
bility of regulatory limitations prior to use. Specific precau-
oil) or synthetic fat simulant HB 307 can be used as a
tionary statements are given in 4.3.2.3.
substitute for corn oil.
2. Referenced Documents
3.6 Dimethylacetamide (DMAC), LC/UV grade.
3.7 Conical Bottom Test Tubes, 50 mL, graduated.
2.1 ASTM Standards:
3.8 Bishydroxyethyleneterephthalate (BHET).
F 874 Test Method for Temperature Measurement and Pro-
3.9 Diethylterephthalate (DET).
filing for Microwave Susceptors
3.10 Dimethylterephthalate (DMT).
F 1317 Test Method for Calibration of Microwave Ovens
3.11 Fluoroptic Thermometry System.
3. Apparatus and Reagents
3.12 Temperature Probes, four, high temperature
3.13 Glass Beads, 3 to 4 mm, clean thoroughly by rinsing
3.1 Microwave Oven, 700 6 35 W, calibrated. Refer to Test
with methylene chloride followed by soaking for 30 min in
Method F 1317.
acetonitrile. Dry thoroughly before using.
3.2 High-Pressure Liquid Chromatograph (HPLC), consist-
3.14 Recommended Microwave Nonvolatile Extraction
ing of:
Cell—Waldorf Polytetrafluoroethylene cell. (See Figs. 1-3).
3.2.1 Pump, capable of 1.5 mL/min with flow precision
62%.
3.2.2 Injector, loop-type, equipped with 20-μL loop.
3.2.3 Guard Column,C , 5 μm.
Fat simulant HB 307 is available from NATEC, Behringstrabe 154, Postfach
501568, 2000 Hamburg 50, West Germany.
3.2.4 Analytical Column,C , 5 μm, 250 by 4.6 mm.
Available from Polysciences, Inc., 400 Valley Rd., Warrington, PA 18976.
Request Catalog Number 18218.
Available from Fisher Scientific, 711 Forbes Ave., Pittsburgh, PA 15219.
This test method is under the jurisdiction of ASTM Committee F-2 on Flexible Request Catalog Number 1189984.
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test Available from Aldrich, 1001 W. St. Paul Ave., Milwaukee, WI 53233. Request
Methods. Catalog Number 18512-4.
Current edition approved Oct. 10, 1998. Published January 1999. Originally Luxtron Model 750, or equivalent, has been found suitable for this purpose.
published as F 1349 – 91. Last previous edition F 1349 – 94. Available from Luxtron Co., 1060 Terra Bella Ave., Mountain View, CA 94043.
2 9
Miglyol 812 is a product of Dynamit Nobel Chemicals, available from HULS Luxtron Model MIW, or equivalent, has been found suitable for this purpose.
America, Inc., 80 Centennial Ave., PO Box 456, Piscataway, NJ 08855-0456. This and additional PTFE polymer materials are available from Read Plastics,
Annual Book of ASTM Standards, Vol 15.09. 12331 Wilkins Ave., Rockville, MD 20852.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
F1349–98
waving oil in the cell, the cell should be rinsed with methylene
chloride to remove residual oil and prevent carry-over.
3.15 Solvent Concentration Apparatus—Kuderna-Danish
evaporative concentrator, rotory evaporator; or Zymark Tur-
boVap at a nitrogen pressure of 30 psi and a water bath
temperature of 50°C.
4. Procedure
4.1 Temperature Measurement:
4.1.1 Refer to Test Method F 874 to determine the time and
water load specifications.
4.2 Sample Preparation and Microwave Heating:
NOTE 1—Always be sure the microwave oven is at ambient temperature
before starting any temperature measurement or heating procedure to
ensure consistency of output. Cooling of the microwave oven can be
expedited by using ice in beakers or crystallization dishes or by using cold
packs such as “blue ice.”
4.2.1 Select a representative piece of the susceptor sample
to be tested. If the susceptor is part of a package, trim excess
material from around susceptor. Determine the area of the
active susceptor material. The susceptor should be cut to fit into
a Waldorf PTFE Cell with the screw seal ring firmly seated
against the susceptor surface. Use of the Waldorf PTFE cell
reduces the risk of spilling hot oil and in addition, gives a
reproducible surface area (53.5 cm ) for extraction. Alterna-
NOTE 1—The ⁄16-in. (1.6-mm) diameter hole is for a Luxtron MIW
tively, cut a 13 by 18-cm rectangular piece of the active
temperature sensing probe. Number of holes and location may vary by
susceptor material, form an extraction boat with sides 1.5 cm
application.
FIG. 1 Collar Section of Waldorf Polytetrafluoroethylene high (boat configuration = 1.5 by 10 by 15 cm, approximately
Microwave Nonvolatile Extraction Cell
150 cm of surface area). Staple the corners of the boat
securely.
4.2.2 Add 53.2 g of Miglyol 812 of corn oil to the Waldorf
PTFE Cell. Alternatively, add 22.5 g oil and 75 g of glass
beads to the extraction boat.
4.2.3 Measure the mass of the room-temperature distilled
water load as determined in 4.1.1 into a 600-mL beaker and
add a boiling chip to this beaker.
4.2.4 Place Waldorf PTFE Cell or extraction boat contain-
ing the oil in the center of the microwave oven. Always
position cell/extraction boat in the same position for subse-
quent runs.
4.2.5 Insert the temperature sensing probes through pre-
formed holes in the walls in Waldorf PTFE Cells (shown in
Fig. 1 and in the lower center sketch of Fig. 2), or in the case
of the extraction boat, tape the probe to the wall of the oven
such that the probe tip maintains contact with the extraction
boat. Manipulate the probes until they make good firm contact
with the active face of the susceptor material.
4.2.6 Microwave the cell or alternate extraction boat using
the time specifications as determined in Test Method F 874.
Record the probe temperatures, preferably at 5-s intervals, but
at intervals not to exceed 15 s.
4.3 Quantitative Analysis:
4.3.1 Standard Curve:
NOTE 1—Relieve thread at bottom. Collar must seal to bottom of cap.
4.3.1.1 Prepare a standard mixture of 10 ppm ( w/v) each of
FIG. 2 Cap Section of Waldorf Polytetrafluorethylene Nonvolatile
BHET, DMT, DET, and any other identified UV components
Extraction Cell
This cell must be constructed by a machine shop experienced 11
Zymark Turbo Vap is a product of the Zymark Corp., Zymark Ctr., Hopkinton,
in working with polytetrafluoroethylene (PTFE). After micro- MA 01748.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
F1349–98
FIG. 3 Suggested Modifications to Waldorf Cell
(see appendix) of the susceptor in DMAC. Proceed to generate into a 50-mL conical test tube or into a Kuderna-Danish
chromatograms using high pressure liquid chromatography in evaporative concentrator with a 10-mL receiver or other
accordance with 3.2.5, 3.2.6, and 4.3.2.8. Retention times for solvent concentration apparatus. Rinse the
...

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