1、Designation: F 1500 98 (Reapproved 2008)Standard Test Method forQuantitating Non-UV-Absorbing Nonvolatile Extractablesfrom Microwave Susceptors Utilizing Solvents as FoodSimulants1This standard is issued under the fixed designation F 1500; the number immediately following the designation indicates t
2、he year oforiginal adoption or, in the case of revision, 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. Scope1.1 This test method is applicable to complete microw
3、avesusceptors.1.2 This test method covers a procedure for quantitatingnon-UV-absorbing nonvolatile compounds which are extract-able when the microwave susceptor is tested under simulateduse conditions for a particular food product.1.3 The values stated in SI units are to be regarded asstandard. No o
4、ther units of measurement are included in thisstandard.1.4 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 the applica-bility
5、 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 260 Practice for Packed Column Gas ChromatographyE 682 Practice for Liquid Chromatography Terms and Re-lationshipsE 685 Practice for Testing Fixed-Wavelength PhotometricDetectors Used in Liquid ChromatographyF 874 T
6、est Method for Temperature Measurement and Pro-filing for Microwave SusceptorsF 1317 Test Method for Calibration of Microwave OvensF 1349 Test Method for Nonvolatile Ultraviolet (UV) Ab-sorbing Extractables from Microwave Susceptors3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1
7、.1 microwave susceptorpackaging materials that,when placed in a microwave field, are designed to interact withthe field and provide substantial heat to the package contents.3.1.2 nonvolatile extractablesthose chemical specieswhich released from microwave food packaging under simu-lated use condition
8、s and are detected using an applicablenonvolatile extractables method.4. Summary of Test Method4.1 Nonvolatile extractables are determined by subjecting asample of the susceptor material to microwave heating undersimulated use conditions. The sample is washed with solventscovering a range of polarit
9、ies. The solvent washes are com-bined and the solvents evaporated just to dryness. The residueis redissolved in a measured quantity of chloroform and thesample split for gravimetric or other analyses, such as HPLC orIR. For the gravimetric determination, a measured portion ofthe sample is filtered a
10、nd evaporated and the residue weighed.For other analyses, the remainder of the sample is evaporatedand may be reconstituted in dimethylacetamide prior to injec-tion (see Test Method F 1349 for quantitation of UV-absorbingnonvolatiles by HPLC), or treated appropriately prior toexamination by other ch
11、romatographic or spectroscopic meth-ods.5. Significance and Use5.1 This test method was developed to measure non-UV-absorbing nonvolatile extractables that may be present andmigrate from a microwave susceptor material during use. Itmay be a useful procedure to assist in minimizing the amountof non-U
12、V-absorbing nonvolatile extractables either throughsusceptor design or manufacturing processes.5.2 Supplementation of this procedure with other analyticaltechnologies such as high-pressure liquid chromatography,supercritical fluid chromatography, or infrared or other formsof spectroscopy may provide
13、 the analyst with additionalinformation regarding the identification of the components ofthe non-UV-absorbing nonvolatile extractables in the suscep-tor.1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Packaging and is the direct responsibility of Subcommittee F02
14、.15 onChemical/Safety Properties.Current edition approved Oct. 1, 2008. Published November 2008. Originallyapproved in 1994. Last previous edition approved in 2003 as F 1500 98(2003).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.
15、org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus and Reagents6.1 Microwave Oven, 700 6 35 W, no tur
16、ntable, calibratedin accordance with Test Method F 1317.6.2 Extraction Cell, Waldorf, described in Test MethodF 1349.NOTE 1If the cell is not equipped with a PTFE gasket, cut a gasketring to match the size of the sleeve from a116-in. PTFE sheet. Use of thegasket between the sleeve and the sample red
17、uces damage to the sample.6.3 Microwave Temperature Measurement System.6.4 Temperature Probe, high temperature.6.5 Beaker, 400-mL borosilicate glass.6.6 Hexane, analytical reagent grade or better.6.7 Acetonitrile, analytical reagent grade or better.6.8 Methylene Chloride, analytical reagent grade or
18、 better.6.9 Chloroform, analytical reagent grade or better.6.10 Dimethylacetamide, HPLC grade or better.6.11 Methanol, analytical reagent grade or better, dried overanhydrous sodium sulfate.6.12 Distilled Water.6.13 Nitrogen, grade suitable for solvent evaporation pur-poses.6.14 Rotary Evaporator, o
19、r equivalent.6.15 Weighing Boat, aluminum, formed by shaping alumi-num foil into a round boat approximately 1.5 cm in diameter.6.16 Filter, 0.45 m, compatible with chloroform.6.17 Round-Bottom Flask, 250 mL, with neck to fit rotaryevaporator.6.18 Vial,20mL.6.19 Heat Lamp, 125 W, or equivalent.6.20 B
20、oiling Stones.6.21 Watchglass, 8.5 or 9.0-cm diameter.7. Sampling7.1 The sample of microwave susceptor selected for extrac-tion should be representative of the entire susceptor.7.2 The sample should be undamaged, that is, laminationintact, uncreased (unless this is the normal configuration) andunalt
21、ered.7.3 Carefully cut a circular portion of the susceptor largeenough to fit the Waldorf cell with the top threaded sleeveremoved. Be sure the sample is cut large enough to fill theentire bottom of the cell. Carefully trim away any frayed edgesbefore testing.7.4 Preclean the susceptor to remove dus
22、t and fibers byblowing a stream of nitrogen over the surface for a fewseconds, or by gently brushing the surface with a camel hairbrush.8. Procedure8.1 Calibrate the microwave oven in accordance with TestMethod F 1317 to ensure that it is 700 6 35 W.8.2 Determine the sample test conditions by using
23、themethod for temperature profiling of microwave susceptors inuse in accordance with Test Method F 874.8.3 Place the precut susceptor sample into the bottomsection of the Waldorf cell. Carefully place the polytetrafluo-roethylene polymer (PTFE) gasket on top of the susceptor toprevent tearing when t
24、he cell sleeve is threaded in. Thread thetop sleeve of the cell into the bottom section of the cell,trapping the susceptor sample securely between the gasket andthe bottom of the cell.8.4 Carefully insert a temperature probe (6.4) through thesmall temperature probe port opening of the cell and ensur
25、ethat it maintains good contact with the susceptor surface. Inserta second probe onto a different area of the susceptor in thesame way.8.5 Place 50 mL of distilled water and a boiling chip into a400-mL beaker and place the beaker in the center rear of theoven. Place a watchglass over the opening of
26、the Waldorf cell.8.6 Place the Waldorf cell in the center of the microwaveoven, and microwave the sample on high power for the timedetermined during the temperature profiling procedure.8.7 Compare the temperature profiles obtained in 8.6 withthose obtained from the susceptor in contact with product.
27、 Ifthe two profiles are in reasonable agreement, proceed to 8.8,otherwise repeat 8.3 through 8.6, using more or less water inthe beaker to adjust the profile appropriately.8.8 Without removing the sample, watchglass, or fiber opticprobes from the cell, allow the sample to cool for 5 min.8.9 Remove t
28、he temperature probe(s) from the cell. Rinsethe bottom of the watchglass covering the Waldorf cell with 20mL of hexane, pouring the solvent into the cell. Swirl thesolvent in the cell for 10 s, then pour it into a 250-mLroundbottom flask. Repeat using a second 20-mL aliquot ofhexane.8.10 Repeat 8.9
29、using two 20-mL aliquots of methylenechloride.8.11 Repeat 8.9 using two 20-mL aliquots of acetonitrile.8.12 Repeat 8.9 using two 20-mL aliquots of methanol.8.13 Using a rotary evaporator with a water bath tempera-ture of 50C, reduce the volume of the combined solvents inthe round-bottom flask to app
30、roximately 10 mL. Transfer theremaining solvent to a 20-mL vial. Rinse the roundbottom flaskwith two 1 mL portions of acetonitrile and combine with thecontents of the vial.8.14 Apply a gentle stream of nitrogen to the solvent in thevial. Apply gentle heat as necessary to expedite evaporation.Evapora
31、te just to dryness, avoiding any heating after all thesolvent is evaporated.8.15 Pipet 10 mL of chloroform into the vial. Swirl withgentle heating to dissolve the residue in the vial.8.16 Dry a clean aluminum weigh boat by placing under aheat lamp for 5 min. Allow to cool and weigh, recording thiswe
32、ight as “tare.” Filter 8 mL of the chloroform solutionthrough the 0.45-m filter into the tared weigh boat and rinsethe filter with a further 1 mL of chloroform.8.17 Place the weigh boat under the heat lamp and evapo-rate the solvent to a constant weight (60.5 mg). Record thisweight in milligrams as
33、“A.”8.18 Repeat 8.9 to 8.17 using solvents which have not beenexposed to a susceptor. Record the final weight in milligramsafter evaporation as“ B.”8.19 Evaporate the remaining 2 mL of chloroform solutionfrom 8.15 to dryness. At this point the residue may beredissolved in 2 mL of dimethylacetamide w
34、ith gentle heating,filtered through a 0.45-m filter and injected onto an HPLCF 1500 98 (2008)2system operated in accordance with Test Method F 1349. (SeePractices E 260, E 682, and E 685 for further informationregarding HPLC set-up and use.) Other sample preparationschemes can be developed for speci
35、fic applications involvingother chromatographic or spectroscopic techniques. The ana-lyst should take the steps necessary to ensure that a represen-tative sample of the residue is obtained, and that the analyteshave not been degraded by the sample preparation schemechosen.9. Calculation9.1 Calculate
36、 total nonvolatile extractable as follows:Total nonvolatile extractable mg/in.2!5 A 2 tare 2 B! 3 108.3 3 8where:A = weight from 8.17,B = weight from 8.18,tare = weight from 8.16,8.3 = square inches of susceptor exposed in Waldorf cell,8 = volume of solvent evaporated, and10 = total volume of sample
37、.10. Precision and Bias10.1 Six laboratories participated in a collaborative study ofnonvolatiles recovered from a bilaminate PETE/adhesive/paperboard susceptor construction obtained from a singlesource. Duplicate analyses were performed at heating times of2 and 5 min using water loads specific to t
38、he individualmicrowave ovens. Participants were asked to evaluate threeextraction procedures: Test Method F 1349 using Miglyol 812in place of corn oil; Test Method F 1349 on extracts from adough similar to a pizza crust consisting of 10:40:50 (w/w/w)Miglyol 812 + water + low-protein flour; and this
39、procedure.Each laboratory was supplied with bilaminate susceptors,Miglyol 812 and flour from single lots, and appropriatestandard materials for HPLC quantitation. Table 1 lists thestatistical results for the determination of diethyleneglycoldibenzoate (DEGDB) and polyethylene terephthalate trimer(PE
40、TE) migrating from the susceptors, normalized to correctfor the various sample areas used by individual collaborators.NOTE 2UV quantitation was used to establish the test methodsvalidity because of the lack of other widely available detection methods.Precision for non-UV-absorbing compounds is expec
41、ted to be similar forthis procedure.10.2 Since no absolute method is available for comparison,no statement regarding bias can be made for this test method.11. Keywords11.1 extractables, nonvolatile; extractables, non-UV absorb-ing; extraction cell, Waldorf; food simulant, corn oil; foodsimulant, dou
42、gh; food simulant, Myglyol; food simulant,solvents; HPLC; microwave; microwave susceptors; Myglyol;nonvolatiles; susceptor; susceptors, microwave; temperaturemeasurement, microwaveASTM International takes no position respecting the validity of any patent rights asserted in connection with any item m
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46、O 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).T
47、ABLE 1 Statistical Results for Determination of DEGDBand PETE Migrating From SusceptorsAnalyte/MatrixAmount Extracted, g/in.2Average SlabSrSrCoV,%SRSRCoV,%DEGDB, 2 minDough 13.88 3.82 2.93 21 4.81 35Miglyol 812 42.20 12.79 22.46 53 25.85 61Test MethodF 150043.25 4.57 14.09 32 14.81 34DEGDB, 5 minDou
48、gh 24.15 7.27 8.17 34 10.93 45Miglyol 812 86.26 21.82 24.54 28 32.84 38Test MethodF 150085.10 8.70 32.08 38 33.24 39PETE, 2 minDough 1.70 0.56 1.38 81 1.49 87Miglyol 812 54.33 7.46 16.06 30 17.71 33Test MethodF 15008.29 1.35 3.14 38 3.42 41PETE, 5 minDough 3.31 1.82 2.04 62 2.73 82Miglyol 812 88.56 2.93 13.90 16 14.20 16Test MethodF 150015.65 1.89 6.10 39 6.39 41Gravimetric2min5min254729711869059435811146224585F 1500 98 (2008)3
