ASTM F1519-98(2019)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: F1519 − 98 (Reapproved 2019)
Standard Test Method for
Qualitative Analysis of Volatile Extractables in Microwave
Susceptors Used to Heat Food Products
This standard is issued under the fixed designation F1519; 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 2. Referenced Documents
1.1 This test method is applicable to complete microwave 2.1 ASTM Standards:
susceptors. E260 Practice for Packed Column Gas Chromatography
F874 Test Method for Temperature Measurement and Pro-
1.2 This test method covers a procedure for identifying
filing for Microwave Susceptors
volatile extractables which are released when a microwave
F1308 Test Method for Quantitating Volatile Extractables in
susceptor sample is tested under simulated end use conditions.
Microwave Susceptors Used for Food Products
The extractables are identified using gas chromatography/mass
F1317 Test Method for Calibration of Microwave Ovens
spectrometry (GC/MS).
3. Terminology
1.3 This test method was evaluated for the identification of
a variety of volatile extractables at a level of 0.010 µg/in. of
3.1 Definitions:
susceptor surface. For extractables not evaluated, the analyst
3.1.1 diffusion trapping—the collection of volatile extract-
should perform studies to determine the level of extractable at
ables on an adsorbent by means of the mass diffusion of the
which identification is achievable.
volatile extractables (1).
1.4 The analyst is encouraged to run known volatile extract-
3.1.2 microwave susceptors—packaging material which,
ables and/or incorporate techniques such as gas
when placed in a microwave field interacts with the field and
chromatography/high resolution mass spectrometry (GC/
provides heating for the food products the package contains.
HRMS), gas chromatography/infrared spectroscopy (GC/IR)
3.1.3 volatile extractables—those compounds that give >
or other techniques to aid in verifying the identity of or
50 % recovery in spike and recovery studies using the appli-
identifying unknown volatile extractables. The analyst is re-
cable volatile extractables method. Extractability does not
ferred to Practice E260 for additional guidance.
necessarily imply migration of the extractable species to the
1.5 The values stated in SI units are to be regarded as
food product being heated on the susceptor.
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 The volatile extractables are released from the susceptor
1.6 This standard does not purport to address all of the
when it has been heated to its end use heating conditions
safety concerns, if any, associated with its use. It is the
(temperature and heating time) using a thermostatically con-
responsibility of the user of this standard to establish appro-
trolled oil bath or calibrated microwave oven. The released
priate safety, health, and environmental practices and deter-
volatile extractables are concentrated by diffusion trapping on
mine the applicability of regulatory limitations prior to use.
an adsorbent. After adsorption is complete, the adsorbent is
1.7 This international standard was developed in accor-
heated to desorb the volatile extractables onto a gas chromato-
dance with internationally recognized principles on standard-
graphic column (Refs 1–2). The volatile extractables are then
ization established in the Decision on Principles for the
separated using a gas chromatograph and detected by a mass
Development of International Standards, Guides and Recom-
spectrometer. The volatile extractable identifications are con-
mendations issued by the World Trade Organization Technical
firmed by comparing their retention times and mass spectra to
Barriers to Trade (TBT) Committee.
reference compounds under identical GC/MS conditions.
1 2
This test method is under the jurisdiction of ASTM Committee F02 on Primary For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Chemical/Safety Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2019. Published May 2019. Originally the ASTM website.
approved in 1994. Last previous edition approved in 2014 as F1519 – 98(2014). The boldface numbers in parentheses refer to a list of references at the end of
DOI: 10.1520/F1519-19. this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1519 − 98 (2019)
5. Significance and Use conditioned PTFE/silicon septa (PTFE surface toward adsor-
bent). Exercise care in handling the adsorbent.
5.1 This test method is intended to identify volatile extract-
7.5.4 Blanks—The adsorbent should be tested for contami-
ables that may be emitted from microwave susceptor material
nation prior to being used.
during use. It may be a useful procedure to assist in minimizing
the amount and type of volatile extractables produced. The 7.6 Oil Bath—Circulating bath capable of being heated to
susceptor design, materials used or manufacturing processes 250 6 1°C. Use silicone oil to heat vials.
involved can be evaluated.
7.7 Thermometers—Capable of measuring up to 250°C.
Calibrate thermometer with a NIST standardized thermometer
6. Interferences
to ensure its accuracy.
6.1 Gas Chromatography/Mass Spectrometry—The GC
7.8 GC/MS System:
conditions or column given may not exhibit sufficient resolu-
7.8.1 Gas Chromatograph—capable of temperature pro-
tion to identify all the volatile extractables. Alternate tech-
gramming. The inlet carrier gas line should be equipped with a
niques should be used to identify the unresolved volatile
valve capable of being completely opened and closed within
extractables such as alternate GC conditions, an alternate GC
1 s.
column, GC/HRMS, and/or GC/IR. The retention time and
7.8.2 The injector should have a removable glass liner or
mass spectrum or infrared spectrum of the volatile extractable
insert, having a volume of at least 300 µL or 40 mg of
should be verified with a reference standard.
adsorbent. The injector should have a closure that allows the
liner/insert to be inserted and the injector sealed within 5 s.
6.2 Apparatus and Materials—Method interferences may be
Modification of the injector may be required (3) through (4).
caused by contamination from vials, septa, syringes, etc.,
leading to misinterpretation of results at trace levels. All of the 7.8.3 GC Column—60M Stabilwax, 0.25 mm ID, 0.5 µm df.
materials must be routinely demonstrated to be free from 7.8.4 Mass Spectrometer, capable of scanning from 35 to
contamination under conditions of the analysis by running
300 amu every 2 s or less when mass spectral data are obtained
blanks. in the electron—impact ionization mode at a nominal electron
energy of 70 eV.
7. Apparatus and Reagents 7.8.5 Data System—An interfaced data system (DS) is
required to acquire, store, reduce and output mass spectral data.
7.1 Sample Cutter—No. 14 cork borer.
The computer software must allow searching of any GC/MS
7.2 Glassware—Wash all glassware thoroughly and dry in a
data file for ions of a specific nominal mass and plot its
125°C air oven for a minimum of 4 h prior to using. Use no
abundance versus time or scan number. This type of plot is
solvents.
defined as an extracted ion current profile (EICP).
7.2.1 Vials—40 mL.
7.9 Performance Volatile Standard for GC/MS System:
7.2.2 Culture Tubes—10 by 75 mm.
7.9.1 Stock Volatile Mixture—Pipet in accordance with
7.3 Vial Caps—Screw caps for 7.2.1 vials. Table 1 the appropriate volume into a 100 mL volumetric flask
which has been half filled with hexane. After all compounds
7.4 Vial Septa—Polytetrafluoroethylene PTFE faced silicon
have been added, fill to mark with hexane and mix well.
backed septa, 22 mm diameter. Place septa into a vacuum oven
Alternate compounds may be substituted. Refrigerate mixture
at 135°C for 16 h prior to using.
at 4°C until needed.
7.5 Volatile Adsorbent—Refer to manufacturer’s literature
regarding physical, chemical, absorptive and desorptive char-
acteristics of adsorbent.
7.5.1 Adsorbent—Tenax TA, 35/60 mesh.
TABLE 1 Stock Volatile Mixture—Preparation and Characteristic
7.5.2 Conditioning—Plug one end of a 14 cm long, 6.35 Ions, m/z, for Each Volatile
A
outside diameter by 5.3 mm inside diameter tube, premium
Compound Volume Pipetted, mL Characteristic Ions, m/z
grade 304 stainless steel with a plug of silanized glass wool.
2-Methyl furan 1.7 82, 81, 53
Benzene 1.7 78, 77, 52
Fill tube with adsorbent, and plug other end with silanized
n-Propyl acetate 1.7 73, 43
glass wool. Connect the tube to the injection port outlet of the
Trichloroethylene 1.0 130, 95
GC, set the UHP helium flow to 30 mL/min and condition
Hexanal 2.0 56, 72, 82
n-Butyl alcohol 2.0 43, 41, 56
adsorbent using the following program.
n-Butyl acrylate 1.7 55, 73, 85
Injection temperature 250°C
Dodecane 2.0 57, 71, 85
Temperature 1 70°C
Styrene 1.7 104, 103, 78
Time 1 30 min
1,4-Dichlorobutane 1.5 55, 90
Rate 10°C/min
N,N-Dimethylformamide 1.5 73, 44, 42
Temperature 2 250°C
Furfural 1.5 95, 96
Time 2 60 min
Benzaldehyde 1.5 106, 105, 77
Pentanoic acid 1.5 73, 60
7.5.3 Storage—Cap both ends of the tube after it cools,
2-(2-Butoxyethoxy)- 1.5 45, 57, 75
move to a chemical free area, uncap one end, remove glass
ethanol
wool, tap tube to transfer adsorbent to 40 mL glass vial, purge A
Pipet into 100 mL volumetric flask which has been half filled with hexane.
vial with UHP helium or argon for 1 min and seal with a
F1519 − 98 (2019)
7.9.2 Performance Volatile Standard—Dilute stock volatile
mixture in step 7.9.1 1:1000 with hexane. Alternate dilutions
may be made. Refr
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