1、Designation: D 5227 01 (Reapproved 2008)1Standard Test Method forMeasurement of Hexane Extractable Content of Polyolefins1This standard is issued under the fixed designation D 5227; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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.1NOTEReapproved with editorial changes in November 2008.1. Scope1.1 This test method describes an extraction/gravimetri
3、cprocedure for determination of the amount of hexane solublelow molecular weight material present in polyethylene,polypropylene, ethylene-propylene copolymers, and ethylene-vinyl acetate copolymers. This test method is a modification ofthe Food and Drug Administration (FDA) procedure fordetermining
4、hexane extractables of polyolefins. This testmethod is based upon the presumption that the weight of theresidue extract present in the solvent is equal to the amountextracted from the film sample and could therefore be quanti-fied by measuring the weight loss of the extracted film,eliminating the co
5、mplex and time-consuming evaporationprocess described in 21 CFR 177.1520.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine
6、the applica-bility of regulatory limitations prior to use.1.3 The values stated in SI units are to be regarded as thestandard. Units used in 21 CFR 177.1520 are also used in thistest method. Units are in conformance with Federal Code 21CFR 177.1520, from which this test method is derived.NOTE 1There
7、 is no known ISO equivalent ISO to this test method.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1239 Test Method for Resistance of Plastic Films toExtraction by ChemicalsD 1600 Terminology for Abbreviated Terms Relating toPlasticsE 131 Terminology Relating to M
8、olecular SpectroscopyE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Federal Document:321 CFR 177.15203. Terminology3.1 The definitions given in Terminology D 883, D 1600,and E 131 are applicable to this test method.3.2 Abbreviations:Abbreviations
9、:3.2.1 EVAethylene-vinyl acetate copolymer.3.2.2 LDPElow-density polyethylene.3.2.3 HDPEhigh-density polyethylene.3.2.4 LLDPElinear low-density polyethylene.3.2.5 FDAFood and Drug Administration.3.2.6 PPpolypropylene.4. Summary of Test Method4.1 Film samples are extracted with hexane for 2 h at 49.5
10、6 0.5C, dried, and weighed.4.2 The loss in weight of the film is presumed to be equal tothe extractable content determined by solvent evaporation inthe FDA protocol.5. Significance and Use5.1 FDA requirements for maximum extractables are speci-fied for resin and uses. This test method provides a mea
11、ns todetermine the amount of hexane-soluble low molecular weightmaterial present in polyolefins. It is applicable to resinscontaining greater than 0.20 % extractables.6. Apparatus6.1 Water Bath, maintained at 49.5 6 0.5C.6.2 Resin Kettle, 1500-mL.41This test method is under the jurisdiction of ASTM
12、Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Nov. 1, 2008. Published March 2009. Originallyapproved in 1992. Last previous edition approved in 2001 as D 5227 - 01.2For referenced ASTM standards, visit the ASTM website
13、, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA
14、 19111-5098, http:/www.dodssp.daps.mil.4Ace Glass, Inc., Cat. No. 647615, or its equivalent, has been foundsatisfactory.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40female joint
15、s, and appropriate stoppers.56.4 Clamp.66.5 Allihn Condenser, Size C, with 45/50 male joint.76.6 Plastic Sleeves, tetrafluoroethylene (TFE), to fit Allihncondenser 45/50 male joint.6.7 Vacuum Oven, capable of maintaining 80 6 5C and aminimum of 25-in. Hg pressure.6.8 Magnetic Stirring Bar, egg-shape
16、d, TFE-coated, 112 by58 in.6.9 Submersible Magnetic Stirring Motor, with power sup-ply.86.10 Analytical Balance, capable of weighing to 0.1 mg.7. Reagents and Materials7.1 n-Hexane, aromatic free (1 mg/L), minimum 85 %n-Hexane-reagent grade or equivalent.9The solvent must befree of aromatic compound
17、s that would significantly increasethe solubility of the resin. The solvent grade specified repre-sents the minimum required purity.8. Materials8.1 Blown Film, compression molded films, or cast films aresuitable for testing.8.2 Film, approximately 2.5 g, with a thickness not exceed-ing 4 mil is requ
18、ired for a single determination.9. Procedure9.1 Assemble the resin kettle setup with glass stopper,clamp, and magnetic stirring bar. (See Fig. 1.)9.2 Add 1000 mL of n-Hexane to the kettle assembly.9.3 Stopper the kettle and clamp the assembly into the waterbath set at 49.5 6 0.5C.NOTE 2Temperature i
19、s a critical factor in this analysis and must notvary more than 1C. If the temperature exceeds these limits, the test mustbe discontinued and restarted. The FDA protocol also states the tempera-ture of the contents must be brought to 49.5 6 0.5C within 20 to 25 min.NOTE 3The level of water in the ba
20、th must be kept at least 2 cm abovethe level of the solvent in the kettle to ensure the temperature equilibrium.Position the kettle so that the center bottle of the kettle is sitting on asubmersible stirrer. Start stirring and allow the hexane to heat for 1 h.9.4 Using gloves and metal tweezers to a
21、void samplecontamination, cut about 2.7 g of the prepared film sample (4mil or less in thickness) into about 1-in. squares using cleansharp scissors.NOTE 4Care must be exercised when cutting the samples to avoidragged edges on the specimen. Small shards of film or contaminationpresent at initial wei
22、ghing can easily be lost during the test, adverselyaffecting the test results.9.5 Weigh 2.5 6 0.05 g of film squares and record the initialfilm weight to the nearest 0.1 mg. Also record the number offilm pieces.NOTE 5Forty or more squares will be obtained depending on the filmthickness. Some laborat
23、ories have found that a basket assembly, as shownin Appendix X1, eliminates the need to count the film pieces before andafter the solvent extraction step.9.6 Add the film sample to the hexane making sure allsquares become immersed in the solvent. (Use tweezers.)Replace the kettle head with condenser
24、 column. Extract for 2 h.9.7 After the extraction period:9.7.1 Filter the contents of the resin kettle through the frittedporcelain funnel.9.7.2 Transfer the film squares, using tweezers, to a 200-mLBerzelius beaker and recount the film pieces to verify that nonewere lost during transfer.9.7.3 Cover
25、 the beaker with a watchglass and place it in avacuum oven at 80 6 5C for 2 h.9.7.4 After 2 h, remove the covered beaker from the vacuumoven and place it in a desiccator to cool to room temperature(about 1 h).9.8 Remove the film squares using tweezers and weigh themto the nearest 0.1 mg.9.9 Repeat 9
26、.7.3 and 9.7.4 until a constant weight isobtained.10. Calculation10.1 Calculate the weight percent of extractables present inthe original sample as follows:hexane extractables, % 5A 2 B! 3 100 3 0.935A(1)where:A = weight of original sample film, g,B = weight of the film after extraction, g, and5Ace
27、Glass, Inc., Cat. No. 648640, or its equivalent, has been foundsatisfactory.6Ace Glass, Inc., Cat. No. 649610, or its equivalent, has been foundsatisfactory.7Ace Glass, Inc., Cat. No. 674006, or its equivalent, has been foundsatisfactory.8VWR Scientific Co., Cat. No. 58947-409, or its equivalent, ha
28、s been foundsatisfactory.9EM Science, Omnisolv reagent grade, or its equivalent, has been foundsatisfactory.FIG. 1 Resin Kettle SetupD 5227 01 (2008)120.935 = correlation factor to eliminate the bias between theoriginal FDA technique and this alternate testmethod.11. Report11.1 Report the hexane ext
29、ractables to the nearest 0.01 % ascalculated in 10.1.12. Precision and Bias1012.1 Hexane Extractable Content of Polyolefins:12.1.1 Table 1 is based on a round robin conducted in 1990in accordance with Practice E 691, involving five materialstested by ten laboratories. The materials were supplied by
30、onelaboratory. Each test result was an individual determination.Each laboratory obtained six test results for each of the fivematerials. Each laboratory obtained two test results for eachmaterial tested each day for three days.NOTE 6Caution: The following explanations of r and R (12.1.2-12.1.2.3) ar
31、e only intended to present a meaningful way of considering theapproximate precision of this test method. The data in Table 1 should notbe rigorously applied to acceptance or rejection of material, as those dataare specific to the round robin and may not be representative of other lots,conditions, ma
32、terials, or laboratories. Users of this test method shouldapply the principles outlined in Practice E 691 to generate data specific totheir laboratory and materials, or between specific laboratories. Theprinciples of 12.1.2-12.1.2.3 would then be valid for such data.12.1.2 Concept of r and RIf Sr an
33、d SR have beencalculated from a large enough body of data, and for test resultsthat were averages from testing five specimens.12.1.2.1 Repeatability Limit, r(Comparing two test re-sults for the same material, obtained by the same operatorusing the same equipment on the same day.) The two testresults
34、 should be judged not equivalent if they differ by morethan the r value for that material.12.1.2.2 Reproducibility Limit, R(Comparing two testresults for the same material, obtained by different operatorsusing different equipment in different laboratories.) The twotest results should be judged not e
35、quivalent if they differ bymore than the R value for that material.12.1.2.3 Any judgment in accordance with 12.1.2.1 or12.1.2.2 would have an approximate 95 % (0.95) probability ofbeing correct.12.1.3 BiasThere are no recognized standards by whichto estimate bias of this test method.13. Keywords13.1
36、 ethylene-propylene copolymers; ethylene-vinyl acetatecopolymers; extractables; FDA; hexane; plastics; polyethyl-ene; solvent extractionAPPENDIX(Nonmandatory Information)X1. BASKET ASSEMBLY FOR n-HEXANE EXTRACTABLESX1.1 If one uses the basket assembly shown in Fig. X1.1,the following steps should be
37、 performed after the 2-h hexaneextraction (9.6):X1.1.1 Rinse the basket and contents by immersing severaltimes in fresh n-hexane contained in a small beaker, allowingthe basket to drain between rinsings.X1.1.2 Remove the excess solvent by briefly blowing thebasket with a stream of nitrogen or dry ai
38、r.X1.1.3 Place the basket in a vacuum oven for 2 h at 8065C, then cool to ambient temperature in a desiccator (about 1h).X1.1.4 Reweigh the basket and its contents to the nearest0.1 mg.10Supporting data are available from ASTM Headquarters. Request RR: D20-1173.TABLE 1 Hexane Extractable Content of
39、Polyolefins, WeightMaterial Average Sr SR r RHDPE 0.26 0.03 0.05 0.09 0.15LLDPE 0.88 0.11 0.16 0.31 0.46LDPE 1.74 0.08 0.15 0.21 0.42EVA 3.54 0.28 0.33 0.78 0.93PP 3.80 0.29 0.35 0.81 0.98D 5227 01 (2008)13ASTM International takes no position respecting the validity of any patent rights asserted in
40、connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the res
41、ponsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive caref
42、ul consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International
43、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).FIG. X1.1 Basket for n-Hexane ExtractablesD 5227 01 (2008)14
