ASTM F1519-98(2014)
(Test Method)Standard Test Method for Qualitative Analysis of Volatile Extractables in Microwave Susceptors Used to Heat Food Products
Standard Test Method for Qualitative Analysis of Volatile Extractables in Microwave Susceptors Used to Heat Food Products
SIGNIFICANCE AND USE
5.1 This test method is intended to identify volatile extractables that may be emitted from microwave susceptor material during use. It may be a useful procedure to assist in minimizing the amount and type of volatile extractables produced. The susceptor design, materials used or manufacturing processes involved can be evaluated.
SCOPE
1.1 This test method is applicable to complete microwave susceptors.
1.2 This test method covers a procedure for identifying volatile extractables which are released when a microwave susceptor sample is tested under simulated end use conditions. The extractables are identified using gas chromatography/mass spectrometry (GC/MS).
1.3 This test method was evaluated for the identification of a variety of volatile extractables at a level of 0.010 μg/in.2 of susceptor surface. For extractables not evaluated, the analyst should perform studies to determine the level of extractable at which identification is achievable.
1.4 The analyst is encouraged to run known volatile extractables and/or incorporate techniques such as gas chromatography/high resolution mass spectrometry (GC/HRMS), gas chromatography/infrared spectroscopy (GC/IR) or other techniques to aid in verifying the identity of or identifying unknown volatile extractables. The analyst is referred to Practice E260 for additional guidance.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: F1519 − 98 (Reapproved 2014)
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 F874 Test Method for Temperature Measurement and Pro-
filing for Microwave Susceptors
1.1 This test method is applicable to complete microwave
F1308 Test Method for Quantitating Volatile Extractables in
susceptors.
Microwave Susceptors Used for Food Products
1.2 This test method covers a procedure for identifying
F1317 Test Method for Calibration of Microwave Ovens
volatile extractables which are released when a microwave
susceptor sample is tested under simulated end use conditions.
3. Terminology
The extractables are identified using gas chromatography/mass
3.1 Definitions:
spectrometry (GC/MS).
3.1.1 diffusion trapping—the collection of volatile extract-
1.3 This test method was evaluated for the identification of ables on an adsorbent by means of the mass diffusion of the
2 3
a variety of volatile extractables at a level of 0.010 µg/in. of volatile extractables (1).
susceptor surface. For extractables not evaluated, the analyst
3.1.2 microwave susceptors—packaging material which,
should perform studies to determine the level of extractable at
when placed in a microwave field interacts with the field and
which identification is achievable.
provides heating for the food products the package contains.
1.4 The analyst is encouraged to run known volatile extract-
3.1.3 volatile extractables—those compounds that give >
ables and/or incorporate techniques such as gas
50 % recovery in spike and recovery studies using the appli-
chromatography/high resolution mass spectrometry (GC/
cable volatile extractables method. Extractability does not
HRMS), gas chromatography/infrared spectroscopy (GC/IR)
necessarily imply migration of the extractable species to the
or other techniques to aid in verifying the identity of or
food product being heated on the susceptor.
identifying unknown volatile extractables. The analyst is re-
4. Summary of Test Method
ferred to Practice E260 for additional guidance.
4.1 The volatile extractables are released from the susceptor
1.5 The values stated in SI units are to be regarded as
when it has been heated to its end use heating conditions
standard. No other units of measurement are included in this
(temperature and heating time) using a thermostatically con-
standard.
trolled oil bath or calibrated microwave oven. The released
1.6 This standard does not purport to address all of the
volatile extractables are concentrated by diffusion trapping on
safety concerns, if any, associated with its use. It is the
an adsorbent. After adsorption is complete, the adsorbent is
responsibility of the user of this standard to establish appro-
heated to desorb the volatile extractables onto a gas chromato-
priate safety and health practices and determine the applica-
graphic column (Refs 1–2). The volatile extractables are then
bility of regulatory limitations prior to use.
separated using a gas chromatograph and detected by a mass
2. Referenced Documents
spectrometer. The volatile extractable identifications are con-
firmed by comparing their retention times and mass spectra to
2.1 ASTM Standards:
reference compounds under identical GC/MS conditions.
E260 Practice for Packed Column Gas Chromatography
5. Significance and Use
This test method is under the jurisdiction ofASTM Committee F02 on Flexible
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on
5.1 This test method is intended to identify volatile extract-
Chemical/Safety Properties.
ables that may be emitted from microwave susceptor material
Current edition approved April 1, 2014. Published April 2014. Originally
duringuse.Itmaybeausefulproceduretoassistinminimizing
approved in 1994. Last previous edition approved in 2008 as F1519 – 98(2008).
the amount and type of volatile extractables produced. The
DOI: 10.1520/F1519-98R14.
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 The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1519 − 98 (2014)
susceptor design, materials used or manufacturing processes 7.7 Thermometers—Capable of measuring up to 250°C.
involved can be evaluated. Calibrate thermometer with a NIST standardized thermometer
to ensure its accuracy.
6. Interferences
7.8 GC/MS System:
6.1 Gas Chromatography/Mass Spectrometry—The GC 7.8.1 Gas Chromatograph—capable of temperature pro-
conditions or column given may not exhibit sufficient resolu-
gramming. The inlet carrier gas line should be equipped with a
tion to identify all the volatile extractables. Alternate tech- valve capable of being completely opened and closed within
niques should be used to identify the unresolved volatile
1s.
extractables such as alternate GC conditions, an alternate GC 7.8.2 The injector should have a removable glass liner or
column, GC/HRMS, and/or GC/IR. The retention time and
insert, having a volume of at least 300 µL or 40 mg of
mass spectrum or infrared spectrum of the volatile extractable adsorbent. The injector should have a closure that allows the
should be verified with a reference standard.
liner/insert to be inserted and the injector sealed within 5 s.
Modification of the injector may be required (3) through (4).
6.2 Apparatus and Materials—Methodinterferencesmaybe
7.8.3 GC Column—60M Stabilwax, 0.25 mm ID, 0.5 µm df.
caused by contamination from vials, septa, syringes, etc.,
7.8.4 Mass Spectrometer, capable of scanning from 35 to
leading to misinterpretation of results at trace levels.All of the
300 amu every2sor less when mass spectral data are obtained
materials must be routinely demonstrated to be free from
in the electron—impact ionization mode at a nominal electron
contamination under conditions of the analysis by running
energy of 70 eV.
blanks.
7.8.5 Data System—An interfaced data system (DS) is
requiredtoacquire,store,reduceandoutputmassspectraldata.
7. Apparatus and Reagents
The computer software must allow searching of any GC/MS
7.1 Sample Cutter—No. 14 cork borer.
data file for ions of a specific nominal mass and plot its
7.2 Glassware—Wash all glassware thoroughly and dry in a abundance versus time or scan number. This type of plot is
125°C air oven for a minimum of 4 h prior to using. Use no defined as an extracted ion current profile (EICP).
solvents.
7.9 Performance Volatile Standard for GC/MS System:
7.2.1 Vials—40 mL.
7.9.1 Stock Volatile Mixture—Pipet in accordance with
7.2.2 Culture Tubes—10 by 75 mm.
Table 1 the appropriate volume into a 100 mLvolumetric flask
7.3 Vial Caps—Screw caps for 7.2.1 vials. which has been half filled with hexane. After all compounds
have been added, fill to mark with hexane and mix well.
7.4 Vial Septa—Polytetrafluoroethylene PTFE faced silicon
Alternate compounds may be substituted. Refrigerate mixture
backed septa, 22 mm diameter. Place septa into a vacuum oven
at 4°C until needed.
at 135°C for 16 h prior to using.
7.9.2 Performance Volatile Standard—Dilute stock volatile
7.5 Volatile Adsorbent—Refer to manufacturer’s literature
mixture in step 7.9.1 1:1000 with hexane. Alternate dilutions
regarding physical, chemical, absorptive and desorptive char-
may be made. Refrigerate standard at 4°C until needed.
acteristics of adsorbent.
7.10 Susceptor Blank—Obtain a representative sample of
7.5.1 Adsorbent—Tenax TA, 35/60 mesh.
susceptor material to be tested. Bake in an air oven overnight
7.5.2 Conditioning—Plug one end of a 14 cm long, 6.35
at 105°C to remove any volatile extractables present. Store in
outside diameter by 5.3 mm inside diameter tube, premium
a clean, sealed glass container (for example, desiccator) until
grade 304 stainless steel with a plug of silanized glass wool.
needed.
Fill tube with adsorbent, and plug other end with silanized
glass wool. Connect the tube to the injection port outlet of the
GC, set the UHP helium flow to 30 mL/min and condition
TABLE 1 Stock Volatile Mixture—Preparation and Characteristic
adsorbent using the following program.
Ions, m/z, for Each Volatile
Injection temperature 250°C A
Compound Volume Pipetted, mL Characteristic Ions, m/z
Temperature 1 70°C
2-Methyl furan 1.7 82, 81, 53
Time 1 30 min
Benzene 1.7 78, 77, 52
Rate 10°C/min
n-Propyl acetate 1.7 73, 43
Temperature 2 250°C
Trichloroethylene 1.0 130, 95
Time 2 60 min
Hexanal 2.0 56, 72, 82
7.5.3 Storage—Cap both ends of the tube after it cools, n-Butyl alcohol 2.0 43, 41, 56
n-Butyl acrylate 1.7 55, 73, 85
move to a chemical free area, uncap one end, remove glass
Dodecane 2.0 57, 71, 85
wool, tap tube to transfer adsorbent to 40 mL glass vial, purge
Styrene 1.7 104, 103, 78
vial with UHP helium or argon for 1 min and seal with a
1,4-Dichlorobutane 1.5 55, 90
N,N-Dimethylformamide 1.5 73, 44, 42
conditioned PTFE/silicon septa (PTFE surface toward adsor-
Furfural 1.5 95, 96
bent). Exercise care in handling the adsorbent.
Benzaldehyde 1.5 106, 105, 77
7.5.4 Blanks—The adsorbent should be tested for contami- Pentanoic acid 1.5 73, 60
2-(2-Butoxyethoxy)- 1.5 45, 57, 75
nation prior to being used.
ethanol
7.6 Oil Bath—Circulating bath capable of being heated to A
Pipet into 100 mL volumetric flask which h
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.