ASTM F1519-98

Standard Test Method for Qualitative Analysis of Volatile Extractables in Microwave Susceptors Used to Heat Food Products

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 extractable identification with a variety of volatile extractables at a level of 0.010 [mu]g/in.  of susceptor. For extractables not evaluated, the analyst should perform studies to determine when extractable 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 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

• Status: Historical
• Publication Date: 09-Oct-1998
• ICS: 97.040.20 - Cooking ranges, working tables, ovens and similar appliances
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.30 - Mechanical Dispensers

Relations

• Replaced By: ASTM F1519-98(2003) - Standard Test Method for Qualitative Analysis of Volatile Extractables in Microwave Susceptors Used to Heat Food Products
• 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• Referred By: ASTM F1317-98(2019) - Standard Test Method for Calibration of Microwave Ovens (Withdrawn 2024)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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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 1519 – 98
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 F 1519; 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 in Microwave Susceptors Used for Food Products
F 1317 Test Method for Calibration of Microwave Ovens
1.1 This test method is applicable to complete microwave
susceptors.
3. Terminology
1.2 This test method covers a procedure for identifying
3.1 Definitions:
volatile extractables which are released when a microwave
3.1.1 diffusion trapping—the collection of volatile extract-
susceptor sample is tested under simulated end use conditions.
ables on an adsorbent by means of the mass diffusion of the
The extractables are identified using gas chromatography/mass
volatile extractables (1).
spectrometry (GC/MS).
3.1.2 microwave susceptors—packaging material which,
1.3 This test method was evaluated for the identification of
2 when placed in a microwave field interacts with the field and
a variety of volatile extractables at a level of 0.010 μg/in. of
provides heating for the food products the package contains.
susceptor surface. For extractables not evaluated, the analyst
3.1.3 volatile extractables—those compounds that give >
should perform studies to determine the level of extractable at
50 % recovery in spike and recovery studies using the appli-
which identification is achievable.
cable volatile extractables method. Extractability does not
1.4 The analyst is encouraged to run known volatile extract-
necessarily imply migration of the extractable species to the
ables and/or incorporate techniques such as gas
food product being heated on the susceptor.
chromatography/high resolution mass spectrometry (GC/
HRMS), gas chromatography/infrared spectroscopy (GC/IR)
4. Summary of Test Method
or other techniques to aid in verifying the identity of or
4.1 The volatile extractables are released from the susceptor
identifying unknown volatile extractables. The analyst is re-
when it has been heated to its end use heating conditions
ferred to Practice E 260 for additional guidance.
(temperature and heating time) using a thermostatically con-
1.5 This standard does not purport to address all of the
trolled oil bath or calibrated microwave oven. The released
safety concerns, if any, associated with its use. It is the
volatile extractables are concentrated by diffusion trapping on
responsibility of the user of this standard to establish appro-
an adsorbent. After adsorption is complete, the adsorbent is
priate safety and health practices and determine the applica-
heated to desorb the volatile extractables onto a gas chromato-
bility of regulatory limitations prior to use.
graphic column (Refs 1–7). The volatile extractables are then
2. Referenced Documents separated using a gas chromatograph and detected by a mass
spectrometer. The volatile extractable identifications are con-
2.1 ASTM Standards:
2 firmed by comparing their retention times and mass spectra to
E 260 Practice for Packed Column Gas Chromatography
reference compounds under identical GC/MS conditions.
F 874 Test Method for Temperature Measurement and Pro-
filing for Microwave Susceptors
5. Significance and Use
F 1308 Test Method for Quantitating Volatile Extractables
5.1 This test method is intended to identify volatile extract-
ables that may be emitted from microwave susceptor material
during use. It may be a useful procedure to assist in minimizing
This test method is under the jurisdiction of ASTM Committee F-2 on Flexible
the amount and type of volatile extractables produced. The
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
Methods.
Current edition approved Oct. 10, 1998. Published March 1999. Originally
published as F 1519–94. Last previous edition F 1519–94.
2 4
Annual Book of ASTM Standards, Vol 14.01. The boldface numbers in parentheses refer to a list of references at the end of
Annual Book of ASTM Standards, Vol 15.09. this test method.
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.
F1519–98
susceptor design, materials used or manufacturing processes vial with UHP helium or argon for 1 min and seal with a
involved can be evaluated. conditioned PTFE/silicon septa (PTFE surface toward adsor-
bent). Exercise care in handling the adsorbent.
6. Interferences
7.5.4 Blanks—The adsorbent should be tested for contami-
6.1 Gas Chromatography/Mass Spectrometry—The GC
nation prior to being used.
conditions or column given may not exhibit sufficient resolu- 7.6 Oil Bath—Circulating bath capable of being heated to
13 14
tion to identify all the volatile extractables. Alternate tech-
250 6 1°C. Use silicone oil to heat vials.
niques should be used to identify the unresolved volatile 7.7 Thermometers—Capable of measuring up to 250°C.
extractables such as alternate GC conditions, an alternate GC
Calibrate thermometer with a NIST standardized thermom-
column, GC/HRMS, and/or GC/IR. The retention time and eter to ensure its accuracy.
mass spectrum or infrared spectrum of the volatile extractable
7.8 GC/MS System:
should be verified with a reference standard. 7.8.1 Gas Chromatograph— , capable of temperature pro-
6.2 Apparatus and Materials—Method interferences may
gramming. The inlet carrier gas line should be equipped with a
be caused by contamination from vials, septa, syringes, etc., valve capable of being completely opened and closed within
leading to misinterpretation of results at trace levels. All of the
1s.
materials must be routinely demonstrated to be free from 7.8.2 The injector should have a removable glass liner or
contamination under conditions of the analysis by running
insert, having a volume of at least 300 μL or 40 mg of
blanks. adsorbent. The injector should have a closure that allows the
liner/insert to be inserted and the injector sealed within 5 s.
7. Apparatus and Reagents
Modification of the injector may be required (2) through (6).
7.1 Sample Cutter—No. 14 cork borer.
7.8.3 GC Column—60M Stabilwax, 0.25 mm ID, 0.5 μm
7.2 Glassware—Wash all glassware thoroughly and dry in a
df.
125°C air oven for a minimum of 4 h prior to using. Use no
7.8.4 Mass Spectrometer, capable of scanning from 35 to
solvents.
300 amu every2sor less when mass spectral data are obtained
7.2.1 Vials—40 mL.
in the electron—impact ionization mode at a nominal electron
7.2.2 Culture Tubes—10 by 75 mm.
energy of 70 eV.
7.3 Vial Caps—Screw caps for 7.2.1 vials.
7.8.5 Data System—An interfaced data system (DS) is
7.4 Vial Septa—Polytetrafluoroethylene PTFE faced silicon
required to acquire, store, reduce and output mass spectral data.
backed septa, 22 mm diameter. Place septa into a vacuum
The computer software must allow searching of any GC/MS
oven at 135°C for 16 h prior to using.
data file for ions of a specific nominal mass and plot its
7.5 Volatile Adsorbent—Refer to manufacturer’s literature
abundance versus time or scan number. This type of plot is
regarding physical, chemical, absorptive and desorptive char-
defined as an extracted ion current profile (EICP).
acteristics of adsorbent.
7.9 Performance Volatile Standard for GC/MS System:
7.5.1 Adsorbent—Tenax TA, 35/60 mesh.
7.9.1 Stock Volatile Mixture—Pipet in accordance with
7.5.2 Conditioning—Plug one end of a 14 cm long, 6.35
Table 1 the appropriate volume into a 100 mL volumetric flask
outside diameter by 5.3 mm inside diameter tube, premium
which has been half filled with hexane. After all compounds
grade 304 stainless steel with a plug of silanized glass
have been added, fill to mark with hexane and mix well.
wool. Fill tube with adsorbent, and plug other end with
Alternate compounds may be substituted. Refrigerate mixture
silanized glass wool. Connect the tube to the injection port
at 4°C until needed.
outlet of the GC, set the UHP helium flow to 30 mL/min and
7.9.2 Performance Volatile Standard—Dilute stock volatile
condition adsorbent using the following program.
mixture in step 7.9.1 1:1000 with hexane. Alternate dilutions
Injection temperature 250°C may be made. Refrigerate standard at 4°C until needed.
Temperature 1 70°C
7.10 Susceptor Blank—Obtain a representative sample of
Time 1 30 min
susceptor material to be tested. Bake in an air oven overnight
Rate 10°C/min
Temperature 2 250°C at 105°C to remove any volatile extractables present. Store in
Time 2 60 min
a clean, sealed glass container (for example, desiccator) until
needed.
7.5.3 Storage—Cap both ends of the tube after it cools,
move to a chemical free area, uncap one end, remove glass
wool, tap tube to transfer adsorbent to 40 mL glass vial, purge
Catalog No. L-01268-52, Cole Palmer Instrument Company, 7425 North Oak
Park Ave., Chicago, IL 60648, or equivalent.
5 14
Catalog No. 07-845E, Fisher Scientific, P.O. Box 4060, Plano, TX 75074, or Catalog No. L-01294-00, Cole Palmer Instrument Co., or equivalent.
equivalent. Catalog No. 14-995-5#, Fisher Scientific, or equivalent.
6 16
Catalog No. 9534, Alltech Associates, Inc., 2051 Waukegan Rd., Deerfield, IL Catalog No. 15041D, Fisher Scientific, or equivalent.
60015, or equivalent. 5890 Gas Chromatograph, Hewlett Packard Company, 3000 Hanover St., Palo
Catalog No. 14-962-10A, Fisher Scientific, or equivalent. Alto, CA 94304, or equivalent.
8 18
Catalog No. 95321, Alltech Associates, Inc., or equivalent. Catalog No. 2328, Alltech Associates, Inc., or equivalent.
9 19
Catalog No. 95322, Alltech Associates, Inc., or equivalent. Catalog No. 10641, Restek Corp., Penn Eagle Industrial Park, 100 Benner
Catalog No. 04915 and 049151, Alltech Associates, Inc., or equivalent. Circle, Bellefonte, PA 16823-8812, or equivalent.
11 20
Catalog No. 303010ST, Alltech Associates, Inc., or equivalent. 5971A Mass Selective Detector, Hewlett Packard Company, 3000 Hanover
Catalog No. 4038, Alltech Associates, Inc., or equivalent. Street, Palo Alto, CA 94304, or equivalent.
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.
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