ASTM F1308-98

Standard Test Method for Quantitating Volatile Extractables in Microwave Susceptors Used for Food Products

SCOPE
1.1 This test method covers complete microwave susceptors.
1.2 This test method covers a procedure for quantitating volatile compounds whose identity has been established and which are evolved when a microwave susceptor sample is tested under simulated use conditions.
1.3 This test method was collaboratively evaluated with a variety of volatile compounds (see statistical evaluation). For compounds other than those evaluated, the analyst should determine the sensitivity and reproducibility of the method by carrying out appropriate spike and recovery studies. The analyst is referred to Practice E260 for guidance.
1.4 For purposes of verifying the identity of or identifying unknown volatile compounds, the analyst is encouraged to incorporate techniques such as gas chromatography/mass spectroscopy, gas chromatography/infrared spectroscopy, or other techniques in conjunction with this test method.
1.5 A sensitivity level of approximately 0.025 [mu]g/in.  is achievable for the compounds studied in Table 1. Where other compounds are being quantitated and uncertainty exists over method sensitivity, the analyst is referred to Practice E260 for procedures on determining sensitivity of chromatographic methods.
1.6 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 safety hazards statements are given in 9.1, 9.4, 11.1, and 11.7.

General Information

• Status: Historical
• Publication Date: 09-Oct-1998
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.30 - Mechanical Dispensers

Relations

• Replaced By: ASTM F1308-98(2003) - Standard Test Method for Quantitating Volatile Extractables in Microwave Susceptors Used for Food Products
• Effective Date: 10-Oct-1998
• Referred By: ASTM F1519-98(2019) - Standard Test Method for Qualitative Analysis of Volatile Extractables in Microwave Susceptors Used to Heat Food Products (Withdrawn 2024)
• Effective Date: 10-Oct-1998
• Referred By: ASTM F874-98(2019) - Standard Test Method for Temperature Measurement and Profiling for Microwave Susceptors (Withdrawn 2024)
• Effective Date: 10-Oct-1998
• Referred By: ASTM F1317-98(2019) - Standard Test Method for Calibration of Microwave Ovens (Withdrawn 2024)
• Effective Date: 10-Oct-1998

Standards Content (Sample)

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 1308 – 98
Standard Test Method for
Quantitating Volatile Extractables in Microwave Susceptors
Used for Food Products
This standard is issued under the fixed designation F 1308; 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.
TABLE 1 Analyte Recovery Without Microwaving
1. Scope
Within
1.1 This test method covers complete microwave suscep-
Recovery Overall
A B
Compound (n) Laboratory Note(s)
Mean, % Variability, %
tors.
Variability, %
1.2 This test method covers a procedure for quantitating
Benzene 5 97.7 7.8 9.0
volatile compounds whose identity has been established and
2-Butoxy-ethanol 4 98.7 6.7 8.4 1
Dibutyl Ether 5 109.7 16.5 23.7
which are evolved when a microwave susceptor sample is
Dodecane 3 101.1 10.7 10.7 1, 2
tested under simulated use conditions.
2-Furfural 4 99.7 11.7 12.0 1
1.3 This test method was collaboratively evaluated with a
Furan- 3 100.0 14.1 16.4 1, 3
2-Methanol
variety of volatile compounds (see statistical evaluation). For
Isobutyl Alcohol 4 96.0 7.1 7.9 4
compounds other than those evaluated, the analyst should
Methylene 5 103.5 16.7 22.6
determine the sensitivity and reproducibility of the method by
Chloride
2-Propanol 3 99.9 11.4 12.0 4
carrying out appropriate spike and recovery studies. The
Styrene 5 100.8 8.5 9.3
analyst is referred to Practice E 260 for guidance.
Toluene 4 102.7 9.9 10.9 4
1.4 For purposes of verifying the identity of or identifying Overall 101.1 11.6 14.4
A
unknown volatile compounds, the analyst is encouraged to
n = number of laboratories submitting data on compound.
B
Notes: Collaborating laboratories provided the following reasons for not sub-
incorporate techniques such as gas chromatography/mass spec-
mitting data on a particular analyte:
troscopy, gas chromatography/infrared spectroscopy, or other
1. The analyst felt interaction was occurring among various analytes and spent
techniques in conjunction with this test method.
several days investigating. The laboratory manager refused to allow additional
time for collaborative study.
1.5 A sensitivity level of approximately 0.025 μg/in. is
2. The analyst questioned the solubility of the analyte and did not add to the
achievable for the compounds studied in Table 1. Where other
spike mixture.
compounds are being quantitated and uncertainty exists over
3. A fresh standard was not prepared fresh daily. This compound degrades
measurably in water in 24 h.
method sensitivity, the analyst is referred to Practice E 260 for
4. The analyst experienced coelution of peaks under conditions of collaborative
procedures on determining sensitivity of chromatographic
study on his/her particular system.
methods.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
T 402 Standard conditioning and testing atmospheres for
responsibility of the user of this standard to establish appro-
paper, board, pulp handsheets, and related products
priate safety and health practices and determine the applica-
TIS 808 Equilibrium relative humidities over saturated salt
bility of regulatory limitations prior to use. Specific safety
solutions
hazards statements are given in Notes 1, 3, and 4.
3. Terminology
2. Referenced Documents
3.1 Definitions:
2.1 ASTM Standards:
3.1.1 microwave susceptors—a packaging material which,
E 260 Practice for Packed Column Gas Chromatography
when placed in a microwave field, interacts with the field and
F 1317 Test Method for Calibration of Microwave Ovens
provides heating for the products the package contains.
2.2 TAPPI Standards:
3.1.2 volatile extractables—those chemical species which
are released from the microwave susceptor and can be detected
in the headspace under conditions simulating those under
This test method is under the jurisdiction of ASTM Committee F-2 on Flexible
which the susceptor is used. Extractability does not necessarily
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
Methods.
Current edition approved Oct. 10, 1998. Published January 1999. Originally
published as F 1308 – 90. Last previous edition F 1308 – 94.
2 4
Annual Book of ASTM Standards, Vol 14.02. Available from the Technical Association of the Pulp and Paper Industry, P.O,
Annual Book of ASTM Standards, Vol 15.09. Box 105113, Atlanta, GA 30348.
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.
F1308–98
mean migration of the extractable species to the product being 7.3 Vials, headspace, 20 mL (actual volume 21.5 mL). To
heated on the susceptors. ensure against extraneous peaks in the gas chromatographic
traces, wash vials thoroughly and dry in a 125°C air oven for
4. Summary of Test Method
a minimum of 4 h before using.
4.1 Volatile extractables are determined by subjecting a
7.4 Vial Crimp Caps.
sample of the susceptor material to microwave heating, fol-
7.5 Septa, Polytetrafluoroethylene (PTFE)/silicone. To en-
lowed by headspace sampling and gas chromatography. Quali-
sure that the septa are free of volatiles, cover the bottom of a
tative analysis may be carried out on a gas chromatograph
15-cm petri dish with septa, PTFE-polymer side up. Micro-
(GC) coupled to an appropriate detector capable of compound
wave at full power for 10 min. Place microwaved septa into a
identification. Volatile extractables are quantitated by compari-
vacuum (greater than 29 in.) oven at 130°C for 16 h.
son with standards of known concentration.
7.6 Crimping Tool for vials.
7.7 Syringe, 2 mL, gas-tight with valve. Store syringe in
5. Significance and Use
90°C oven between uses.
5.1 This test method is intended to measure volatile extract-
7.8 Gas Chromatograph equipped as follows:
ables that may be emitted from a microwave susceptor material
7.8.1 FID Detector, compatible with capillary columns.
during use. It may be a useful procedure to assist in minimizing
7.8.2 Injector, split/splitless compatible with capillary col-
the amount of volatile extractables either through susceptor
umns.
design or manufacturing processes.
7.8.3 Automated Headspace Sampler, Optional.
5.2 Modification of this procedure by utilizing appropriate
7.8.4 Column, DB-5, 30 m, 0.25-mm inside diameter, 1-μm
qualitative GC detection such as a mass spectrometer in place
14 15
film thickness, or 0.32 mm. (A short piece of deactivated
of the flame ionization detector may provide identification of
0.25-mm fused silica column may be placed between the
volatile extractables of unknown identity.
injector and the column to serve as a guard column.)
7.8.5 Peak-Area Integration System compatible with GC
6. Interferences
system. Alternatively, a chart recorder and hand integration can
6.1 Gas Chromatography—Because of the potentially large
be used.
number of chemical species that can be analyzed using this
7.9 Fluoroptic Thermometry System.
methodology, not all species will be resolved from one another
7.10 Temperature Probes, high temperature.
on a particular GC column under a given set of conditions.
7.11 Beaker, 600 mL.
Techniques available to the analyst to verify the identity of the
7.12 Oven, hot air, set for 90°C.
species being quantitated include retention time comparisons
7.13 Stopwatch.
using alternate GC conditions or using an alternate GC column
7.14 4-Heptanone.
to verify identification. Good judgement of chromatographic
5,6,7 7.15 Standard Solutions—Regular Method:
results is always important. Refer to Practice E 260 for
7.15.1 Internal Standard Solution (245 μg/mL
guidance.
4-Heptanone)—To approximately 950 mL of distilled water in
6.2 Apparatus—Because this test method is designed for
a 1-L volumetric flask add 300 μL of 4-heptanone. Mix well
trace volatiles, and is highly sensitive, contaminants on vials,
and dilute to volume with water.
septa, syringes, etc. can lead to misinterpretation of results.
Preparing apparatus properly and carrying out blank determi-
nations as specified in the procedure is essential to minimize
this possibility.
Vials from Shamrock Glass Co., 200 N. Delaware Ave., Seaford, DE 302
629-5500 (Catalog No. 667601) or from Chemical Research Supplies, P. O. Box
7. Apparatus and Reagents
888, Addison, IL 60101 or equivalent vials have been found suitable for this
purpose.
7.1 Microwave Oven—Calibrated, 7006 35 W, no turn-
Vial crimp caps from Shamrock Glass Co., Catalog No. 778704 or from
table. See Test Method F 1317.
Hewlett Packard Computer Supplies Operation, PO Box 62124, San Francisco, CA
7.2 Humidity Chambers, operated at 50 % RH and 23°C.
94162, Catalog No. 07675-120625 or equivalent have been found suitable for this
7.2.1 Requirements for constant temperature-humidity purpose.
Septa from Shamrock Glass Co., Catalog No. 778173A or Hewlett-Packard
chambers and equilibrium relative humidities over saturated
Computer Supplies Operation, Catalog No. 5080-8726 or equivalent have been
salt solutions are outlined in TAPPI Methods T 402-om-88, and
found suitable for this purpose.
TIS 808-03.
Crimping tools from Supelco Inc., Belefonte, PA 16823, Catalog No. 33280.
Syringes from Alltech, 2051 Waukegan Rd., Deerfield, IL 60015, Catalog No.
050034 or equivalent have been found suitable for this purpose.
5 13
McCown, S. M., and Radenheimer, P., “An Equilibrium Headspace Gas The Hewlett-Packard Model No. 19395A or equivalent has been found
Chromatographic Method for the Determination of Volatile Residues in Vegetable suitable for this purpose.
Oils and Fats,” LC/GC, Vol 7, No. 11, 1989, pp. 918–924. Columns from J and W Scientific, 91 Blue Ravine Rd., Folsom, CA
McNeal, T. P., and Breder, C. V., “Headspace Gas Chromatographic Determi- 95630-4714, Catalog No. 122-5033 or equivalent has been found suitable for this
nation of Residual 1,3-Butadiene in Rubber-Modified Plastics and Its Migration purpose.
from Plastic Containers Into Selected Foods,” Journal of the Association of Catalog No. 123-5033 from J and W Scientific.
Analytical Chemists, Vol 70, No. 1, 1987, pp. 18–21. Luxtron Model 750 available from Luxtron Inc., 106 Terra Bella Ave.,
McNeal, T. P., and Breder, C. V., “Headspace Sampling and Gas-Solid Mountain View, CA 90403, or equivalent has been found suitable for this purpose.
Chromatographic Determination of Residual Acrylonitrile in Acrylonitrile Copoly- Luxtron Model MIH or equivalent has been found suitable for this purpose.
mer Solutions,” Journal of the Association of Offıcial Analytical Chemists, Vol 64, 4-Heptanone from Aldrich, 940 West St. Paul Ave., Milwaukee, WI 53233,
No. 2, 1981, pp. 270–275. Catalog No. 10, 174-5 or equivalent has been found suitable for this purpose.
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.
F1308–98
2 2
7.15.2 Standard Solution 1: (Prepare fresh daily.)—To ap- 8.1.5 Cut a 10 by 65-mm (6.5-cm = 1-in. ) portion from the
proximately 475 mL of internal standard solution in a 500-mL susceptor sample to be tested. Insert carefully into the 20-mL
volumetric flask, add 50 μL of each of the compounds to be headspace vial.
quantitated. Mix well, and dilute to volume with internal
8.1.6 Using a 13-gage syringe needle, pierce a hole into a
standard solution. If difficulty is experienced with dissolution headspace vial septum. Place the septum on the vial and crimp.
of analyte, alternate standard solution procedure may over-
8.1.7 Insert one temperature probe (7.10) through the sep-
come this difficulty. tum hole into the vial and manipulate it until it is in contact
7.15.3 Standard Solution 2—Repeat 7.14.2 using 25 μL of with the active face of the susceptor material. Place the vial on
its side in the center of microwave oven, crimp end toward
each compound.
right of the oven, and susceptor with active face up.
7.15.4 Standard Solution 3—Repeat 7.14.2 using 10 μL of
8.1.8 Microwave at full power, recording the probe tem-
each compound.
perature, preferably at 5-s intervals, but at intervals not to
7.16 Standard Solutions—Alternate Method:
exceed 15 s.
7.16.1 Alternate Internal Standard Solution (1225 μg/mL
8.1.9 Plot the temperatures from 8.1.3 and 8.1.8 on the same
4-Heptanone)—To approximately 150 mL of helium-sparged
graph.
orthodichlorobenzene (ODCB) in a 200-mL volumetric flask
8.1.10 Compare the plots. If the trace from 8.1.8 closely
add 300 μL of 4-heptanone. Mix well and dilute to volume with
approximates or is slightly higher than the plot from 8.1.3 then
ODCB.
the test time will be equal to the maximum product cook time
7.16.2 Alternate Standard Solution 1— To approximately
of the product in that oven. If the trace is substantially higher
75 mL of alternate internal standard solution in a 100-mL
or lower than that of the susceptor with product, then adjust the
volumetric flask, add 50 μL of each of the compounds to be
mass or surface area, or both, (by changing container size) of
quantitated. Mix well, and dilute to volume with alternate
the water (using a fresh sample of room temperature distilled
internal standard solution.
water) as necessary to achieve a similar profile. Record the
7.16.3 Alternate Standard Solution 2— Repeat 7.15.2 using
mass of water and type of container that gives the best
25 μL of each compound.
agreement between the test sample and the product temperature
7.16.4 Alternate Standard Solution 3— Repeat 7.15.2 using
profiles.
10 μL of each compound.
8.2 Set up the gas chromatographic system to meet the
7.17 Susceptor Blank—Obtain a representative sample of
following criteria.
susceptor material to be tested. Bake in an air oven overnight
8.2.1 Injector Temperature—250°C.
at 100°C or higher to remove any volatile materials present.
8.2.2 Detector Temperature—250°C.
Store blank susceptor strips in humidity chamber 1 at 50 % RH
8.2.3 Column Temperature:
and 23°C until equilibrium moisture content is reached. An
8.2.3.1 Initial—40°C for 4 min.
exposure time of 24 h is generally adequate for most paper-
8.2.3.2 Program—Adjust to give a retention window of:
based products. Strips should remain in the conditioning
(1) At least 15 min for volatile compounds bracketed by
environment until needed for analysis.
2-propanol and dichlorobenzene, retention time for 2-prop
...