1、Designation: F 1500 98 (Reapproved 2003)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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is applicable to complete micro
3、wavesusceptors.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 This standard does not purport to address all of thesafety conce
4、rns, 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 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E 260 Practice for Packed Column Gas Chr
5、omatographyE 682 Practice for Liquid Chromatography Terms and Re-lationshipsE 685 Practice for Testing Fixed-Wavelength PhotometricDetectors Used in Liquid ChromatographyF 874 Test Method for Temperature Measurement and Pro-filing for Microwave SusceptorsF 1317 Test Method for Calibration of Microwa
6、ve OvensF 1349 Test Method for Nonvolatile Ultraviolet (UV) Ab-sorbing Extractables from Microwave Susceptors3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 microwave susceptorpackaging materials that,when placed in a microwave field, are designed to interact withthe field and
7、 provide substantial heat to the package contents.3.1.2 nonvolatile extractablesthose chemical specieswhich released from microwave food packaging under simu-lated use conditions and are detected using an applicablenonvolatile extractables method.4. Summary of Test Method4.1 Nonvolatile extractables
8、 are determined by subjecting asample of the susceptor material to microwave heating undersimulated use conditions. The sample is washed with solventscovering a range of polarities. The solvent washes are com-bined and the solvents evaporated just to dryness. The residueis redissolved in a measured
9、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 and evaporated and the residue weighed.For other analyses, the remainder of the sample is evaporatedand may be reconstituted
10、 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 chromatographic or spectroscopic meth-ods.5. Significance and Use5.1 This test method was developed to measure non-UV-absorbi
11、ng 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-UV-absorbing nonvolatile extractables either throughsusceptor design or manufacturing processes.5.2 Supplementation of this
12、procedure with other analyticaltechnologies such as high-pressure liquid chromatography,supercritical fluid chromatography, or infrared or other formsof spectroscopy may provide the analyst with additionalinformation regarding the identification of the components ofthe non-UV-absorbing nonvolatile e
13、xtractables in the suscep-tor.6. Apparatus and Reagents6.1 Microwave Oven, 700 6 35 W, no turntable, calibratedin accordance with Test Method F 1317.1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Materials and is the direct responsibility of Subcommittee F02.15
14、onChemical/Safety Properties.Current edition approved Oct. 10, 1998. Published January 1999. Originallypublished as F 1500 - 94. Last previous edition F 1500 94.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book o
15、f 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.6.2 Extraction Cell, Waldorf, described in Test MethodF 1349.36.3 Microwave Temperatu
16、re Measurement System.46.4 Temperature Probe, high temperature.56.5 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 better.6.9 Chloroform, analytical reagent grad
17、e 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, or equivalent.6.15 Weighing Boat, aluminum, form
18、ed by shaping alumi-num foil into a round boat approximately 1.5 cm in diameter.6.16 Filter, 0.45 m,6compatible 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 Boiling Stones.6.21 Watchglass, 8.5 or 9.0-cm di
19、ameter.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) andunaltered.7.3 Carefully cut a circular portion of th
20、e 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 dust and fibers byblowing a stream of nitrogen ove
21、r 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 themethod for temperature profiling of microwav
22、e 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 the cell sleeve is threaded in. Thread thetop sl
23、eeve 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 ensurethat it maintains good contact with the suscep
24、tor 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 the Waldorf cell.8.6 Place the Waldorf cell in
25、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. Ifthe two profiles are in reasonable agreement
26、, 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 the temperature probe(s) from the cell. Rinsethe
27、 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 using two 20-mL aliquots of methylenechloride.8
28、.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 approximately 10 mL. Transfer theremaining solvent
29、 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.Evaporate just to dryness, avoiding any heating after
30、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 thisweight as “tare.” Filter 8 mL of the chloroform s
31、olutionthrough 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 “A.”8.18 Repeat 8.9 to 8.17 using solvents whic
32、h 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 be3If the cell is not equipped with a PTFE gasket, cut a gasket ring to match thesize of th
33、e sleeve from a116-in. PTFE sheet. Use of the gasket between the sleeveand the sample reduces damage to the sample.4Model 750 Fluoroptic Thermometry System of Luxtron, Inc., 1060 Terra BellaAve., Mountain View, CA 90403, has been found satisfactory for this purpose.5Model MIW of Luxtron, Inc., has b
34、een found satisfactory.6Acrodisc filters from Gelman Sciences, Inc., 600 S. Wagner Road, Ann Arbor,MI 48106 313/665-0651, have been found satisfactory.F 1500 98 (2003)2redissolved in 2 mL of dimethylacetamide with gentle heating,filtered through a 0.45-m filter and injected onto an HPLCsystem operat
35、ed 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 specific applications involvingother chromatographic or spectroscopic techniques. The ana-lyst should take the s
36、teps 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 total nonvolatile extractable as follows:Total nonvolatile extractable mg/in.2!5 A 2 tare 2 B! 3 108.3 3 8
37、where: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.10. Precision and Bias10.1 Six laboratories participated in a collaborative study ofnonvolatiles recovered
38、 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 the individualmicrowave ovens. Participants were asked to evaluate threeextraction procedures: Test Method F
39、 1349 using Miglyol 8127in 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 procedure.Each laboratory was supplied with bilaminate susceptors,Miglyol 812 and flour from single lots,
40、and appropriatestandard materials for HPLC quantitation. Table 1 lists thestatistical results for the determination of diethyleneglycoldibenzoate (DEGDB) and polyethylene terephthalate trimer(PETE) migrating from the susceptors, normalized to correctfor the various sample areas used by individual co
41、llaborators.NOTE 1UV 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 expected to be similar forthis procedure.10.2 Since no absolute method is available for comparison,no statement
42、 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, dough; food simulant, Myglyol; food simulant,solvents; HPLC; microwave; microwave susceptors; Myglyol;nonvola
43、tiles; susceptor; susceptors, microwave; temperaturemeasurement, microwaveASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity
44、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 responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments
45、are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not r
46、eceived 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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies
47、) 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).7Available from HULS America, Inc., 80 Centennial Ave., Piscataway, NJ08855.TABLE 1 Statistical Results for
48、 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 minDough 24.15 7.27 8.17 34 10.93 45
49、Miglyol 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 (2003)3
