ASTM F1308-98(2008)
(Test Method)Standard Test Method for Quantitating Volatile Extractables in Microwave Susceptors Used for Food Products
Standard Test Method for Quantitating Volatile Extractables in Microwave Susceptors Used for Food Products
SIGNIFICANCE AND USE
This test method is intended to measure volatile extractables that may be emitted from a microwave susceptor material during use. It may be a useful procedure to assist in minimizing the amount of volatile extractables either through susceptor design or manufacturing processes.
Modification of this procedure by utilizing appropriate qualitative GC detection such as a mass spectrometer in place of the flame ionization detector may provide identification of volatile extractables of unknown identity.
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 E 260 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 μg/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 E 260 for procedures on determining sensitivity of chromatographic methods.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 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 warnings are given in 10.2, 11.1, and 11.6.
TABLE 1 Analyte Recovery Without Microwaving Compound(n)ARecovery Mean, %Within Laboratory Variability, %Overall Variability, %Note(s)B Benzene 5 97.7 7.8 9.0 2-Butoxy-ethanol4 98.7 6.7 8.41 Dibutyl Ether5109.716.5 23.7 Dodecane3101.110.7 10.71, 2 2-Furfural4 99.711.7 12.01 Furan-
2-Methanol3 100.014.116.41, 3 Isobutyl Alcohol4 96.0 7.1 7.94 Methylene
Chloride5 103.516.722.6 2-Propanol3 99.911.4 12.04 Styrene 5100.8 8.5 9.3 Toluene 4102.7 9.910.94 Overall101.1 11.614.4
A n = number of laboratories submitting data on compound.
B Notes: Collaborating laboratories provided the following reasons for not sub-
mitting data on a particular analyte:
1. The analyst felt interaction was occurring among various analytes and spent several days investigating. The laboratory manager refused to allow additional time for collaborative study.
2. The analyst questioned the solubility of the analyte and did not add to the spike mixture.
3. A fresh standard was not prepared fresh daily. This compound degrades measurably in water in 24 h.
4. The analyst experienced coelution of peaks under conditions of collaborative study on his/her particular system.
General Information
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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: F1308 − 98(Reapproved 2008)
Standard Test Method for
Quantitating Volatile Extractables in Microwave Susceptors
Used for Food Products
This standard is issued under the fixed designation F1308; 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 bility of regulatory limitations prior to use. Specific safety
hazards warnings are given in 10.2, 11.1, and 11.6.
1.1 This test method covers complete microwave suscep-
tors.
2. Referenced Documents
1.2 This test method covers a procedure for quantitating
2.1 ASTM Standards:
volatile compounds whose identity has been established and
E260 Practice for Packed Column Gas Chromatography
which are evolved when a microwave susceptor sample is
F1317 Test Method for Calibration of Microwave Ovens
tested under simulated use conditions.
2.2 TAPPI Standards:
1.3 This test method was collaboratively evaluated with a
T 402 Standard conditioning and testing atmospheres for
variety of volatile compounds (see statistical evaluation). For
paper, board, pulp handsheets, and related products
compounds other than those evaluated, the analyst should
TIS 808 Equilibrium relative humidities over saturated salt
determine the sensitivity and reproducibility of the method by
solutions
carrying out appropriate spike and recovery studies. The
analyst is referred to Practice E260 for guidance.
3. Terminology
1.4 For purposes of verifying the identity of or identifying
3.1 Definitions:
unknown volatile compounds, the analyst is encouraged to
3.1.1 microwave susceptors—a packaging material which,
incorporate techniques such as gas chromatography/mass
when placed in a microwave field, interacts with the field and
spectroscopy, gas chromatography/infrared spectroscopy, or
provides heating for the products the package contains.
other techniques in conjunction with this test method.
3.1.2 volatile extractables—those chemical species which
1.5 A sensitivity level of approximately 0.025 µg/in. is
are released from the microwave susceptor and can be detected
achievable for the compounds studied in Table 1. Where other
in the headspace under conditions simulating those under
compounds are being quantitated and uncertainty exists over
which the susceptor is used. Extractability does not necessarily
method sensitivity, the analyst is referred to Practice E260 for
mean migration of the extractable species to the product being
procedures on determining sensitivity of chromatographic
heated on the susceptors.
methods.
4. Summary of Test Method
1.6 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 4.1 Volatile extractables are determined by subjecting a
standard. sample of the susceptor material to microwave heating, fol-
lowed by headspace sampling and gas chromatography. Quali-
1.7 This standard does not purport to address all of the
tative analysis may be carried out on a gas chromatograph
safety concerns, if any, associated with its use. It is the
(GC) coupled to an appropriate detector capable of compound
responsibility of the user of this standard to establish appro-
identification. Volatile extractables are quantitated by compari-
priate safety and health practices and determine the applica-
son with standards of known concentration.
This test method is under the jurisdiction ofASTM Committee F02 on Flexible
5. Significance and Use
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
5.1 This test method is intended to measure volatile extract-
Chemical/Safety Properties.
Current edition approved Oct. 1, 2008. Published November 2008. Originally
ablesthatmaybeemittedfromamicrowavesusceptormaterial
approved in 1990. Last previous edition approved in 2003 as F1308 – 98(2003).
duringuse.Itmaybeausefulproceduretoassistinminimizing
DOI: 10.1520/F1308-98R08.
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
Standards volume information, refer to the standard’s Document Summary page on Available from TechnicalAssociation of the Pulp and Paper Industry (TAPPI),
the ASTM website. 15 Technology Parkway South, Norcross, GA 30092, http://www.tappi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1308 − 98 (2008)
TABLE 1 Analyte Recovery Without Microwaving
Preparing apparatus properly and carrying out blank determi-
Within nations as specified in the procedure is essential to minimize
Recovery Overall
A B
Compound ( n) Laboratory Note(s)
this possibility.
Mean, % Variability, %
Variability, %
Benzene 5 97.7 7.8 9.0
7. Apparatus and Reagents
2-Butoxy-ethanol 4 98.7 6.7 8.4 1
Dibutyl Ether 5 109.7 16.5 23.7
7.1 Microwave Oven—Calibrated,700635W,noturntable.
Dodecane 3 101.1 10.7 10.7 1, 2
See Test Method F1317.
2-Furfural 4 99.7 11.7 12.0 1
Furan- 3 100.0 14.1 16.4 1, 3
7.2 Humidity Chambers, operated at 50 % RH and 23°C.
2-Methanol
Isobutyl Alcohol 4 96.0 7.1 7.9 4
7.2.1 Requirements for constant temperature-humidity
Methylene 5 103.5 16.7 22.6
chambers and equilibrium relative humidities over saturated
Chloride
2-Propanol 3 99.9 11.4 12.0 4 saltsolutionsareoutlinedinTAPPIMethodsT 402-om-88,and
Styrene 5 100.8 8.5 9.3
TIS 808-03.
Toluene 4 102.7 9.9 10.9 4
Overall 101.1 11.6 14.4
7.3 Vials, headspace, 20 mL (actual volume 21.5 mL). To
A
n = number of laboratories submitting data on compound.
ensure against extraneous peaks in the gas chromatographic
B
Notes: Collaborating laboratories provided the following reasons for not sub-
traces, wash vials thoroughly and dry in a 125°C air oven for
mitting data on a particular analyte:
a minimum of 4 h before using.
1. The analyst felt interaction was occurring among various analytes and spent
several days investigating. The laboratory manager refused to allow additional
7.4 Vial Crimp Caps.
time for collaborative study.
2. The analyst questioned the solubility of the analyte and did not add to the
7.5 Septa, Polytetrafluoroethylene (PTFE)/silicone. To en-
spike mixture.
3. A fresh standard was not prepared fresh daily. This compound degrades sure that the septa are free of volatiles, cover the bottom of a
measurably in water in 24 h.
15-cm petri dish with septa, PTFE-polymer side up. Micro-
4. The analyst experienced coelution of peaks under conditions of collaborative
wave at full power for 10 min. Place microwaved septa into a
study on his/her particular system.
vacuum (greater than 29 in.) oven at 130°C for 16 h.
7.6 Crimping Tool for vials.
7.7 Syringe, 2 mL, gas-tight with valve. Store syringe in
the amount of volatile extractables either through susceptor
90°C oven between uses.
design or manufacturing processes.
7.8 Gas Chromatograph equipped as follows:
5.2 Modification of this procedure by utilizing appropriate
7.8.1 FID Detector, compatible with capillary columns.
qualitative GC detection such as a mass spectrometer in place
7.8.2 Injector, split/splitless compatible with capillary col-
of the flame ionization detector may provide identification of
volatile extractables of unknown identity. umns.
7.8.3 Automated Headspace Sampler, Optional.
6. Interferences
7.8.4 Column, DB-5, 30 m, 0.25-mm inside diameter, 1-µm
film thickness, or 0.32 mm. (A short piece of deactivated
6.1 Gas Chromatography—Because of the potentially large
0.25-mm fused silica column may be placed between the
number of chemical species that can be analyzed using this
injector and the column to serve as a guard column.)
methodology, not all species will be resolved from one another
on a particular GC column under a given set of conditions. 7.8.5 Peak-Area Integration System compatible with GC
system.Alternatively,achartrecorderandhandintegrationcan
Techniques available to the analyst to verify the identity of the
species being quantitated include retention time comparisons be used.
using alternate GC conditions or using an alternate GC column
7.9 Fluoroptic Thermometry System .
to verify identification. Good judgement of chromatographic
4,5,6
7.10 Temperature Probes, high temperature.
results is always important. Refer to Practice E260 for
guidance.
7.11 Beaker, 600 mL.
6.2 Apparatus—Because this test method is designed for
7.12 Oven, hot air, set for 90°C.
trace volatiles, and is highly sensitive, contaminants on vials,
7.13 Stopwatch.
septa, syringes, etc. can lead to misinterpretation of results.
7.14 4-Heptanone.
7.15 Standard Solutions—Regular Method:
McCown, S. M., and Radenheimer, P., “An Equilibrium Headspace Gas
Chromatographic Method for the Determination of Volatile Residues in Vegetable 7.15.1 Internal Standard Solution (245 µg/mL
Oils and Fats,” LC/GC, Vol 7, No. 11, 1989, pp. 918–924.
4-Heptanone)—To approximately 950 mL of distilled water in
McNeal, T. P., and Breder, C. V., “Headspace Gas Chromatographic Determi-
a 1-L volumetric flask add 300 µL of 4-heptanone. Mix well
nation of Residual 1,3-Butadiene in Rubber-Modified Plastics and Its Migration
and dilute to volume with water.
from Plastic Containers Into Selected Foods,” Journal of the Association of
Analytical Chemists, Vol 70, No. 1, 1987, pp. 18–21.
7.15.2 Standard Solution 1: (Prepare fresh daily.)—To ap-
McNeal, T. P., and Breder, C. V., “Headspace Sampling and Gas-Solid
proximately 475 mL of internal standard solution in a 500-mL
Chromatographic Determination of Residual Acrylonitrile in Acrylonitrile Copoly-
volumetric flask, add 50 µL of each of the compounds to be
mer Solutions,” Journal of the Association of Offıcial Analytical Chemists, Vol 64,
No. 2, 1981, pp. 270–275. quantitated. Mix well, and dilute to volume with internal
F1308 − 98 (2008)
standard solution. If difficulty is experienced with dissolution 8.1.6 Using a 13-gage syringe needle, pierce a hole into a
of analyte, alternate standard solution procedure may over- headspace vial septum. Place the septum on the vial and crimp.
come this difficulty.
8.1.7 Insert one temperature probe (7.10) through the sep-
7.15.3 Standard Solution 2—Repeat 7.14.2 using 25 µL of
tum hole into the vial and manipulate it until it is in contact
each compound.
with the active face of the susceptor material. Place the vial on
7.15.4 Standard Solution 3—Repeat 7.14.2 using 10 µL of its side in the center of microwave oven, crimp end toward
each compound. right of the oven, and susceptor with active face up.
8.1.8 Microwave at full power, recording the probe tem-
7.16 Standard Solutions—Alternate Method:
perature, preferably at 5-s intervals, but at intervals not to
7.16.1 Alternate Internal Standard Solution (1225 µg/mL
exceed 15 s.
4-Heptanone)—To approximately 150 mL of helium-sparged
8.1.9 Plotthetemperaturesfrom8.1.3and8.1.8onthesame
orthodichlorobenzene (ODCB) in a 200-mL volumetric flask
graph.
add300µLof4-heptanone.Mixwellanddilutetovolumewith
ODCB. 8.1.10 Compare the plots. If the trace from 8.1.8 closely
approximates or is slightly higher than the plot from 8.1.3 then
7.16.2 Alternate Standard Solution 1—Toapproximately75
mL of alternate internal standard solution in a 100-mL volu- the test time will be equal to the maximum product cook time
of the product in that oven. If the trace is substantially higher
metric flask, add 50 µL of each of the compounds to be
quantitated. Mix well, and dilute to volume with alternate or lower than that of the susceptor with product, then adjust the
mass or surface area, or both, (by changing container size) of
internal standard solution.
the water (using a fresh sample of room temperature distilled
7.16.3 Alternate Standard Solution 2— Repeat 7.15.2 using
water) as necessary to achieve a similar profile. Record the
25 µL of each compound.
mass of water and type of container that gives the best
7.16.4 Alternate Standard Solution 3— Repeat 7.15.2 using
agreementbetweenthetestsampleandtheproducttemperature
10 µL of each compound.
profiles.
7.17 Susceptor Blank—Obtain a representative sample of
8.2 Set up the gas chromatographic system to meet the
susceptor material to be tested. Bake in an air oven overnight
following criteria.
at 100°C or higher to remove any volatile materials present.
Store blank susceptor strips in humidity chamber 1 at 50 % RH 8.2.1 Injector Temperature—250°C.
and 23°C until equilibrium moisture content is reached. An
8.2.2 Detector Temperature—250°C.
exposure time of 24 h is generally adequate for most paper-
8.2.3 Column Temperature:
based products. Strips should remain in the conditioning
8.2.3.1 Initial—40°C for 4 min.
environment until needed for analysis.
8.2.3.2 Program—Adjust to give a retention window of:
7.18 Syringe Needle, 13 gage.
(1) At least 15 min for volatile compounds bracketed by
7.19 Variable Voltage Transformer, Optional—This can oc- 2-propanol and dichlorobenzene, retention time for 2-propanol
of approximately 3 min and retention time for dichlorobenzene
casionally be used for minor adjustments to line voltage to
bring power output of the microwave oven into the specified of approximately 20 min.
range.
(2) ProvidingaseparationofDi-n-butyletherandstyreneof
R = 0.5 or greater. For a 30-m by 0.25-mm column this is
8. Instrument Setup
approximately 4°C/min with a nominal carrier flow of 1.5
mL/min.
8.1 Determine sample test conditions as follows:
8.2.4 Attenuation or sensitivity, or both, set to give an
8.1.1 Set up microwave susceptor in the configuration of its
internal standard peak height of 60 to 90% of full scale on
intended use, that is, a popcorn bag filled with popcorn, a pizza
recorder or integrator.
disk with pizza on top, etc.
8.1.2 Place temperature probes (7.10) on susceptor surface,
9. Sampling
disturbing the normal food load as little as possible. If the
susceptor has areas where the food does not normally contact
9.1 The sample of microwave susceptor selected for extrac-
the surface, place the probes in these areas. Place the product
tion should be representative of the entire susceptor.
in the center of the microwave oven.
9.2 The sample should be undamaged, that is, lamination
8.1.3 Cook the product in accordance with normal direc-
intact, uncreased (unless this is normal configuration) and
tions,forthemaximumcookingtime.Recordthistime.Record
unaltered.
the probe temperature(s), preferably at 5-s intervals, but at
2 2
intervals not to exceed 15 s during cooking.
9.3 Carefully cut a 10 by 65-mm (6.5 cm = 1 in. ) portion
8.1.4 Place 250 mLof room-temperature distilled water into
from the susce
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