ASTM D4754-2018 Standard Test Method for Two-Sided Liquid Extraction of Plastic Materials Using FDA Migration Cell.pdf

1、Designation: D4754 11D4754 18Standard Test Method forTwo-Sided Liquid Extraction of Plastic Materials Using FDAMigration Cell1This standard is issued under the fixed designation D4754; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision

2、, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the use of the FDA migration cell in the extraction of components and permits q

3、uantitation ofindividual 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

4、 been applied to a variety of migrant/polymer systems in contact with numerous foods and foodsimulants.2 Though most of the migrants examined were radiolabeled, the use of the FDA cell has been validated for migrationstudies of unlabeled sytrene from polystyrene.31.4 This test method has been shown

5、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 plast

6、ics intended forsingle-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 somecases.NOTE 1For more information, see Practice D1898, the AOAC Methods of Analysis on Flexible Barrier Materials Exposed for Extr

7、action, and theGuidance for Industry: Preparation of Premarket Submissions for Food Contact Substances: Chemistry Recommendations, December 2007.1.7 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

8、 as the standard.1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.

9、 Specific hazards statements are given in Section 8.NOTE 2There is no known ISO equivalent to this test method.1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safe

10、ty, health, and environmental practices and determine the applicability ofregulatory limitations prior to use. Specific hazards statements are given in Section 8.NOTE 2There is no known ISO equivalent to this test method.1.10 This international standard was developed in accordance with international

11、ly recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:4D883 Terminolog

12、y Relating to Plastics1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Dec. 1, 2011May 1, 2018. Published December 2011May 2018. Originally approved in 1987. Last prev

13、ious edition approved in 20032011 asD4754 98D4754 11.(2003). DOI: 10.1520/D4754-11.10.1520/D4754-18.2 “A Study of Indirect Food Additive Migration,” Arthur D. Little, Inc., FDA Contract No. 223-77-2360.3 Supporting data have been filed at ASTM International Headquarters and may be obtained by reques

14、ting Research Report RR:D20-1141.4 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM

15、 standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all

16、 cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D1898 Pract

17、ice for Sampling of Plastics (Withdrawn 1998)5E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodIEEE/ASTM SI 10 Standard for Use of the International System of Units (SI): The Modernized Metric System2.2 Association of Offcial Analytical Chemists (AOAC)

18、 Methods of Analysis:Flexible Barrier Materials Exposed for Extraction62.3 Federal Document:Guidance for Industry: Preparation of Premarket Submissions for Food Contact Substances: Chemistry Recommendations,December 200773. Terminology3.1 GeneralThe units, symbols, and abbreviations used in this tes

19、t method are in accordance with Terminology D883 andPractice IEEE/ASTM SI 10.4. Summary of Test Method4.1 Specimens of plastic materials, formed in the shape of disks, are threaded onto a stainless steel wire with alternating glassbead spacers and placed in a glass vial. Solvent is added to the vial

20、 and the vial is capped and maintained at the desired extractiontemperature. Aliquots of the liquid are removed at various times and the migrant(s) in the liquid determined by suitable analyticalmethods.NOTE 3 Significant migration loss due to volatility may occur if migration is carried out at temp

21、eratures exceeding 50C for periods greater than 2weeks.5. Significance and Use5.1 Knowledge of migrants from plastic materials may serve many useful purposes, such as testing for compliance with foodadditive regulations. The procedure described in this test method is recommended as suitable for obta

22、ining such data on manymigrant(s)/plastic(s) combinations.6. Apparatus6.1 FDA Migration Cell (Fig. 1), consisting of:6.1.1 Glass Vials, 23-mL,6.1.2 Mininert Slide Valve Caps,6.1.3 Stainless Steel Wire (20-gage), and5 The last approved version of this historical standard is referenced on www.astm.org

23、.6 Available through the Association of Official Analytical Chemists, 481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-2417 USA.7 Available from Division of Food Contact Notifications, Office of Food Additive Safety, Center for Food Safety and Applied Nutrition, Food and Drug Admi

24、nistration,College Park, MD 20740, USA. https:/www.fda.gov/Food/GuidanceRegulation/GuidanceDocumentsRegulatoryInformation/IngredientsAdditivesGRASPackaging/ucm081818.htmFIG. 1 FDA Migration CellD4754 1826.1.4 Glass Bead (5-mm diameter), containing hole slightly larger than diameter of stainless stee

25、l wire.8 (Available at localhobby shops.)NOTE 4The apparatus, disk size, and number of disks are described for the 23-mL vial. Alternative vial sizes and corresponding test specimen sizesmay be substituted. (The volume-to-surface area ideally should be between 155 and 0.31 mL/cm2.) Note that validat

26、ion tests have only been conductedusing the 23-mL vials.NOTE 5Recommend one-time use of mininert valve (that is, discarding it at completion of study).6.2 Hot-Air Oven or Static Thermostatted Water Bath, with suitable safety provisions and capable of maintaining the desiredextraction temperature wit

27、hin 61C.6.3 Thermostatted Shaker Water Bath,Some migrant/plastic/liquid combinations may involve significant partitioning andwould benefit by having the cells shaken throughout the migration study.6.4 Liquid Syringes, for removing liquid aliquots from the cells and transferring them to the analytica

28、l instrumentation.6.5 Analytical Instrumentation, as required by the method chosen to determine the migrant(s).7. Reagents and Materials7.1 Purity of ReagentsAll solvents shall be HPLC or chromatographic grade and shown to be free of interferences in thedetection region of the migrant(s).8. Hazards8

29、.1 The usual safety precautions for handling flammable solvents are recommended when such solvents are used for extraction.9. Sampling9.1 Sample the plastic in accordance with Practice D1898.9.2 Select representative samples of the plastic to be tested from available stock on hand. Film, pellets, po

30、wders, sheet, and, insome cases, actual end-use articles are suitable. Protect the samples from exposure to liquids or contamination by migration fromcontact with other materials.NOTE 6See RR:D20-1141 for details regarding sample test specimens.10. Test Specimen10.1 Test specimens in the form of rou

31、nd disks (11 by 1 mm) are prepared from the plastic to be tested. Disks can be stampedout of sheets of actual end-use articles of non-brittle plastic by means of the appropriate sized cork borer. Alternatively, disks canbe formed by using a heated press and an appropriate shim or mold containing hol

32、es the size of the disk. Holes can be put in thecenter of the disk by means of a drill or a heated wire.NOTE 7Whenever possible, plastic from actual end-use articles should be tested.NOTE 8When actual end-use articles are tested, the cut edges of the disks may have a different structure than the sur

33、faces, and henceforth themigration 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. Ifa significant edge effect is suspected, however, tests can be run comparing disks formed by using a heated press with disk

34、s cut from a sheet formed undersimilar conditions.11. Preparation of Apparatus11.1 Alternately thread glass beads and 14 plastic disks onto the stainless steel wire (see Fig. 1). Prepare at least 4 sets for eachliquid extractant used. Place resulting stacks of disks into 23 mL glass vials.Add 22 mL

35、of extraction liquid and screw Mininertcaps 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 theabove prepared vials at the extr

36、action temperature for 2 h. Discard the liquid in the vials and replenish with fresh extracting liquid.NOTE 9Depending upon the conditions under which the test specimens were prepared, removal of any migrant surface bloom might not be warranted.Under these conditions, simply omit the wash step for r

37、emoving migrant surface bloom.12. Procedure12.1 Place properly prepared vials in thermostatted oven or bath.12.2 To prepare standards for quantitating the migration, place extraction solvent(s) and known quantities of the migrant(s) tobe studied in a vial containing the support stand with glass bead

38、 spacers. Place these standard vials in the same thermostatted ovenor bath.8 Glass beads sold at hobby shops have been found satisfactory for this purpose.D4754 18312.3 To prepare the blank, place only the extraction solvent(s) in a vial containing the support stand with glass bead spacers.Place the

39、se blank vials in the same thermostatted oven or bath.12.4 At pre-selected times, typically 5 to 8 samplings over a 2-week period, withdraw L aliquots from each sample, standard,and blank vial and analyze using selected methodology.NOTE 10At each sampling, check to see if cell caps are tight.NOTE 11

40、Volume withdraw is dictated by analytical procedure being utilized. If aliquots of more than 1 % by volume are removed during samplings,separate vials should be used for each test period.12.5 Use response of standards on each day of analysis to quantitate the migrant(s).13. Calculation13.1 The test

41、results can be calculated in a number of ways depending upon the application of the data.13.2 One simple way to express the test results is to calculate the concentration of the migrant(s) in the liquid at a given timein some unit such as parts per million (ppm) or parts per billion (ppb).13.3 A sec

42、ond way to express the test results is in milligrams of migrant(s) per square metremeter of sample exposed, E, asfollows:E 5W 2B!/2piR21CT!N#where:W = total weight of migrant(s) in the liquid, mg,B = weight of migrant(s) in the blank, mg,R = radius of the disk, m,C = circumference of disk, m,T = thi

43、ckness of disk, m, andN = number of disks per cell.13.4 A third and more rigorous way to express the test results is to calculate diffusion and partition coefficients for theplastic/migrant(s)/liquid system used. These calculations, however, are beyond the scope of this test method. A brief descript

44、ionis contained in Appendix X1Appendix X1. .14. Report14.1 Report the test results, either as concentration of migrant(s) per unit volume of liquid, or concentration of migrant(s) persquare metre of disk area.15. Precision and Bias315.1 TableTable 1 1 is based on a round-robin conducted in 1984 in a

45、ccordance with Practice E691. Twelve laboratoriesreported results (ppm) for styrene migration from polystyrene disks into 50/50 ethanol/water at 49C. The disks were prepared atone source. Five replicate sample cells were then setup by each laboratory which conducted the studies. One aliquot was take

46、nfrom each cell at six times over 2 weeks. A test result was obtained from the analysis of each aliquot. Each laboratory reported30 test results.NOTE 12 The following explanations of Ir and IR (see 15.2) are only intended to present a meaningful way of considering the approximate precisionof this te

47、st method. The data in Table 1 should not be rigorously applied to acceptance or rejection of material, as those data are specific to the round-robinand may not be representative of other lots, conditions, materials, or laboratories. Users of this test method should apply the principles outlined in

48、PracticeTABLE 1 Precision for Migration of Residual Styrene fromPolystyreneTime, h Values in ppmAvg SrA SRB rC RD4 0.222 0.022 0.11 0.062 0.3124 0.979 0.080 0.12 0.226 0.3472 2.282 0.153 0.27 0.433 0.76168 3.875 0.198 0.46 0.560 1.30240 4.790 0.197 0.62 0.558 1.75336 5.711 0.276 0.82 0.781 2.32A Sr

49、= within-laboratory standard deviation of the average,B SR = between-laboratories standard deviation of the average,C r = 2.83Sr, andD R = 2.83SR.D4754 184E691 to generate data specific to their laboratory and materials, or between specific laboratories. The principles of 15.2 through 15.2.3 would then bevalid for such data.15.2 Concept ofr and RSince Srr and SRR have been calculated from data produced by 12 laboratories, and for test results thatwere averages from testing 5 sample cells:15.2.1 Repeatability,rSr (Comparing two test results for th