ASTM D4754-98

Standard Test Method for Two-Sided Liquid Extraction of Plastic Materials Using FDA Migration Cell

SCOPE
1.1 This test method covers the use of the FDA migration cell in the extraction of components and permits quantitation of individual migrants from plastic materials by suitable extracting liquids, including liquid foods and food-stimulating solvents.
1.2 This test method provides a two-sided, liquid extraction test for plastic materials that can be formed into film, sheet, or disks.
1.3 This test method has been applied to a variety of migrant/polymer systems in contact with numerous foods and food simulants.  Though most of the migrants examined were radiolabeled, the use of the FDA cell has been validated for migration studies of unlabeled sytrene from polystyrene.  
1.4 This test method has been shown to yield reproducible results under the conditions for migration tests requested by the FDA. However, if the data is to be submitted to the FDA, it is suggested that their guidelines be consulted.
1.5 Because it employs two-sided extraction, this test method may not be suitable for multi-layered plastics intended for single-sided food contact use.
1.6 The size of the FDA migration cell as described may preclude its use in determining total nonvolatile extractives in some cases. Note 1-For more information, see Practice D1898, the AOAC Methods of Analysis on Flexible Barrier Materials Exposed for Extraction, and the 1988 FDA Guidelines for Chemistry and Technology.
1.7 Analytical procedures must be available to quantitate the migrant(s) generated by this test method.
1.8 The values stated in SI units are to be regarded as the standard.
1.9 This standard does not purport to address all of the safety problems, 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 hazards statements are given in Section 8. Note 2-There is no similar or equivalent ISO standard.

General Information

• Status: Historical
• Publication Date: 09-Jul-1998
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaced By: ASTM D4754-98(2003) - Standard Test Method for Two-Sided Liquid Extraction of Plastic Materials Using FDA Migration Cell
• Effective Date: 10-Mar-2003
• Referred By: ASTM F34-13(2023) - Standard Practice for Construction of Test Cell for Liquid Extraction of Flexible Barrier Materials
• Effective Date: 10-Jul-1998
• Referred By: ASTM F2097-20 - Standard Guide for Design and Evaluation of Primary Flexible Packaging for Medical Products
• Effective Date: 10-Jul-1998
• Referred By: ASTM F561-19 - Standard Practice for Retrieval and Analysis of Medical Devices, and Associated Tissues and Fluids
• Effective Date: 10-Jul-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: D 4754 – 98
Standard Test Method for
Two-Sided Liquid Extraction of Plastic Materials Using FDA
Migration Cell
This standard is issued under the fixed designation D 4754; 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 * responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This test method covers the use of the FDA migration
bility of regulatory limitations prior to use. Specific hazards
cell in the extraction of components and permits quantitation of
statements are given in Section 8.
individual migrants from plastic materials by suitable extract-
ing liquids, including liquid foods and food-stimulating sol-
NOTE 2—There is no similar or equivalent ISO standard.
vents.
2. Referenced Documents
1.2 This test method provides a two-sided, liquid extraction
test for plastic materials that can be formed into film, sheet, or
2.1 ASTM Standards:
disks.
D 883 Terminology Relating to Plastics
1.3 This test method has been applied to a variety of
D 1898 Practice for Sampling of Plastics
migrant/polymer systems in contact with numerous foods and
E 380 Practice for Use of the International System of Units
food simulants. Though most of the migrants examined were
(SI) (the Modernized Metric System)
radiolabeled, the use of the FDA cell has been validated for
E 691 Practice for Conducting an Interlaboratory Study to
migration studies of unlabeled sytrene from polystyrene.
Determine the Precision of a Test Method
1.4 This test method has been shown to yield reproducible
2.2 Association of Offıcial Analytical Chemists (AOAC)
results under the conditions for migration tests requested by the
Methods of Analysis:
FDA. However, if the data is to be submitted to the FDA, it is
Flexible Barrier Materials Exposed for Extraction
suggested that their guidelines be consulted.
2.3 Federal Document:
1.5 Because it employs two-sided extraction, this test
1995 Recommendations for Chemistry Data for Indirect
method may not be suitable for multi-layered plastics intended
Food Additive Petitions
for single-sided food contact use.
3. Terminology
1.6 The size of the FDA migration cell as described may
preclude its use in determining total nonvolatile extractives in
3.1 General—The units, symbols, and abbreviations used in
some cases. this test method are in accordance with Terminology D 883 and
Practice E 380.
NOTE 1—For more information, see Practice D 1898, the AOAC
Methods of Analysis on Flexible Barrier Materials Exposed for Extrac-
4. Summary of Test Method
tion, and the 1995 Recommendations for Chemistry Data for Indirect
4.1 Specimens of plastic materials, formed in the shape of
Food Additive Petitions.
disks, are threaded onto a stainless steel wire with alternating
1.7 Analytical procedures must be available to quantitate
glass bead spacers and placed in a glass vial. Solvent is added
the migrant(s) generated by this test method.
to the vial and the vial is capped and maintained at the desired
1.8 The values stated in SI units are to be regarded as the
extraction temperature. Aliquots of the liquid are removed at
standard.
various times and the migrant(s) in the liquid determined by
1.9 This standard does not purport to address all of the
suitable analytical methods.
safety concerns, if any, associated with its use. It is the
NOTE 3—Caution: Significant migration loss due to volatility may
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Annual Book of ASTM Standards, Vol 08.02.
Current edition approved July 10, 1998. Published January 1999. Originally Annual Book of ASTM Standards, Vol 14.02.
published as D 4754 – 87. Last previous edition D 4754 – 93. Available through the Association of Official Analytical Chemists, Washington,
“A Study of Indirect Food Additive Migration,” Arthur D. Little, Inc., FDA DC.
Contract No. 223-77-2360. Available from Chemistry Review Branch, Office of Premarket Approval,
Supporting data are available from ASTM Headquarters. Request RR: D20- Center for Food Safety and Applied Nutrition, Food and Drug Administration,
1141. Washington, DC 20204.
*A Summary of Changes section appears at the end of this standard.
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.
D 4754 – 98
occur if migration is carried out at temperatures exceeding 50°C for
6.4 Liquid Syringes, for removing liquid aliquots from the
periods greater than 2 weeks.
cells and transferring them to the analytical instrumentation.
6.5 Analytical Instrumentation, as required by the method
5. Significance and Use
chosen to determine the migrant(s).
5.1 Knowledge of migrants from plastic materials may
serve many useful purposes, such as testing for compliance 7. Reagents and Materials
with food additive regulations. The procedure described in this
7.1 Purity of Reagents—All solvents shall be HPLC or
test method is recommended as suitable for obtaining such data
chromatographic grade and shown to be free of interferences in
on many migrant(s)/plastic(s) combinations.
the detection region of the migrant(s).
6. Apparatus
8. Hazards
6.1 FDA Migration Cell (Fig. 1), consisting of:
8.1 The usual safety precautions for handling flammable
6.1.1 Glass Vials, 23-mL,
solvents are recommended when such solvents are used for
6.1.2 Mininertt Slide Valve Caps,
extraction.
6.1.3 Stainless Steel Wire (20-gage), and
9. Sampling
6.1.4 Glass Bead (5-mm diameter), containing hole slightly
larger than diameter of stainless steel wire. (Available at local
9.1 Sample the plastic in accordance with Practice D 1898.
hobby shops.)
9.2 Select representative samples of the plastic to be tested
from available stock on hand. Film, pellets, powders, sheet,
NOTE 4—The apparatus, disk size, and number of disks are described
and, in some cases, actual end-use articles are suitable. Protect
for the 23-mL vial. Alternative vial sizes and corresponding test specimen
sizes may be substituted. (The volume-to-surface area ideally should be the samples from exposure to liquids or contamination by
between 155 and 0.31 mL/cm .) Note that validation tests have only been
migration from contact with other materials.
conducted using the 23-mL vials.
NOTE 6—See RR: D 20-1141 for details regarding sample test speci-
NOTE 5—Recommend one-time use of mininert valve (that is, discard-
mens.
ing it at completion of study).
6.2 Hot-Air Oven or Static Thermostatted Water Bath, with
10. Test Specimen
suitable safety provisions and capable of maintaining the
10.1 Test specimens in the form of round disks (11 by 1
desired extraction temperature within 61°C.
mm) are prepared from the plastic to be tested. Disks can be
6.3 Thermostatted Shaker Water Bath —Some migrant/
stamped out of sheets of actual end-use articles of non-brittle
plastic/liquid combinations may involve significant partition-
plastic by means of the appropriate sized cork borer. Alterna-
ing and would benefit by having the cells shaken throughout
tively, disks can be formed by using a heated press and an
the migration study.
appropriate shim or mold containing holes the size of the disk.
Holes can be put in the center of the disk by means of a drill
or a heated wire.
NOTE 7—Whenever possible, plastic from actual end-use articles
FDA Migration Cell components are available from Supelco, Inc., P.O. Box
should be tested.
628, 146 S. Water St., Bellefonte, PA 16823.
9 NOTE 8—When actual end-use articles are tested, the cut edges of the
Glass beads sold at hobby shops have been found satisfactory for this purpose.
disks may have a different structure than the surfaces, and henceforth the
Available from Precision Scientific, 3737 W. Cortland St., Chicago, IL 60647.
migration rates may be altered. Because the area of the surfaces is much
greater than that of the cut edges, the effect of the edges would be limited.
If a significant edge effect is suspected, however, tests can be run
comparing disks formed by using a heated press with disks cut from a
sheet formed under similar conditions.
11. Preparation of Apparatus
11.1 Alternately thread glass beads and 14 plastic disks onto
the stainless steel wire (see Fig. 1). Prepare at least 4 sets for
each liquid extractant used. Place resulting stacks of disks into
23 mL glass vials. Add 22 mL of extraction liquid and screw
Mininertt caps tightly onto the vials.
11.2 Use the above prepared vials to determine the total
amount of migrant(s).
11.3 To calculate migration rates, the samples should be
washed to remove any surface bloom of the migrant(s).
Maintain the above prepared vials at the extraction temperature
for 2 h. Discard the liquid in the vials and replenish with fresh
extracting liquid.
NOTE 9—Depending upon the conditions under which th
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