1、Designation: F 1308 98 (Reapproved 2003)Standard Test Method forQuantitating Volatile Extractables in Microwave SusceptorsUsed for Food Products1This standard is issued under the fixed designation F 1308; the number immediately following the designation indicates the year oforiginal adoption or, in
2、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 covers complete microwave suscep-tors.1.2 This test method covers
3、a procedure for quantitatingvolatile compounds whose identity has been established andwhich are evolved when a microwave susceptor sample istested under simulated use conditions.1.3 This test method was collaboratively evaluated with avariety of volatile compounds (see statistical evaluation). Forco
4、mpounds other than those evaluated, the analyst shoulddetermine the sensitivity and reproducibility of the method bycarrying out appropriate spike and recovery studies. Theanalyst is referred to Practice E 260 for guidance.1.4 For purposes of verifying the identity of or identifyingunknown volatile
5、compounds, the analyst is encouraged toincorporate techniques such as gas chromatography/mass spec-troscopy, gas chromatography/infrared spectroscopy, or othertechniques in conjunction with this test method.1.5 A sensitivity level of approximately 0.025 g/in.2isachievable for the compounds studied i
6、n Table 1. Where othercompounds are being quantitated and uncertainty exists overmethod sensitivity, the analyst is referred to Practice E 260 forprocedures on determining sensitivity of chromatographicmethods.1.6 This standard does not purport to address all of thesafety concerns, if any, associate
7、d 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. Specific safetyhazards warnings are given in 10.2, 11.1, and 11.6.2. Referenced Documents2.1 ASTM Standa
8、rds:2E 260 Practice for Packed Column Gas ChromatographyF 1317 Test Method for Calibration of Microwave Ovens2.2 TAPPI Standards:T 402 Standard conditioning and testing atmospheres forpaper, board, pulp handsheets, and related products3TIS 808 Equilibrium relative humidities over saturated saltsolut
9、ions33. Terminology3.1 Definitions:3.1.1 microwave susceptorsa packaging material which,when placed in a microwave field, interacts with the field andprovides heating for the products the package contains.3.1.2 volatile extractablesthose chemical species whichare released from the microwave suscepto
10、r and can be detectedin the headspace under conditions simulating those under1This test method is under the jurisdiction of ASTM Committee F02 on FlexibleBarrier Materials and is the direct responsibility of Subcommittee F02.15 onChemical/Safety Properties.Current edition approved Oct. 10, 1998. Pub
11、lished January 1999. Originallypublished as F 1308 90. Last previous edition F 1308 94.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summar
12、y page onthe ASTM website.3Available from the Technical Association of the Pulp and Paper Industry, P.O,Box 105113, Atlanta, GA 30348.TABLE 1 Analyte Recovery Without MicrowavingCompound (n)ARecoveryMean, %WithinLaboratoryVariability, %OverallVariability, %Note(s)BBenzene 5 97.7 7.8 9.02-Butoxy-etha
13、nol 4 98.7 6.7 8.4 1Dibutyl Ether 5 109.7 16.5 23.7Dodecane 3 101.1 10.7 10.7 1, 22-Furfural 4 99.7 11.7 12.0 1Furan-2-Methanol3 100.0 14.1 16.4 1, 3Isobutyl Alcohol 4 96.0 7.1 7.9 4MethyleneChloride5 103.5 16.7 22.62-Propanol 3 99.9 11.4 12.0 4Styrene 5 100.8 8.5 9.3Toluene 4 102.7 9.9 10.9 4Overal
14、l 101.1 11.6 14.4An = number of laboratories submitting data on compound.BNotes: Collaborating laboratories provided the following reasons for not sub-mitting data on a particular analyte:1. The analyst felt interaction was occurring among various analytes and spentseveral days investigating. The la
15、boratory manager refused to allow additionaltime for collaborative study.2. The analyst questioned the solubility of the analyte and did not add to thespike mixture.3. A fresh standard was not prepared fresh daily. This compound degradesmeasurably in water in 24 h.4. The analyst experienced coelutio
16、n of peaks under conditions of collaborativestudy on his/her particular system.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.which the susceptor is used. Extractability does not necessarilymean migration of the extractable species
17、to the product beingheated on the susceptors.4. Summary of Test Method4.1 Volatile extractables are determined by subjecting asample of the susceptor material to microwave heating, fol-lowed by headspace sampling and gas chromatography. Quali-tative analysis may be carried out on a gas chromatograph
18、(GC) coupled to an appropriate detector capable of compoundidentification. Volatile extractables are quantitated by compari-son with standards of known concentration.5. Significance and Use5.1 This test method is intended to measure volatile extract-ables that may be emitted from a microwave suscept
19、or materialduring use. It may be a useful procedure to assist in minimizingthe amount of volatile extractables either through susceptordesign or manufacturing processes.5.2 Modification of this procedure by utilizing appropriatequalitative GC detection such as a mass spectrometer in placeof the flam
20、e ionization detector may provide identification ofvolatile extractables of unknown identity.6. Interferences6.1 Gas ChromatographyBecause of the potentially largenumber of chemical species that can be analyzed using thismethodology, not all species will be resolved from one anotheron a particular G
21、C column under a given set of conditions.Techniques available to the analyst to verify the identity of thespecies being quantitated include retention time comparisonsusing alternate GC conditions or using an alternate GC columnto verify identification. Good judgement of chromatographicresults is alw
22、ays important.4,5,6Refer to Practice E 260 forguidance.6.2 ApparatusBecause this test method is designed fortrace volatiles, and is highly sensitive, contaminants on vials,septa, syringes, etc. can lead to misinterpretation of results.Preparing apparatus properly and carrying out blank determi-natio
23、ns as specified in the procedure is essential to minimizethis possibility.7. Apparatus and Reagents7.1 Microwave OvenCalibrated, 7006 35 W, no turn-table. See Test Method F 1317.7.2 Humidity Chambers, operated at 50 % RH and 23C.7.2.1 Requirements for constant temperature-humiditychambers and equili
24、brium relative humidities over saturatedsalt solutions are outlined in TAPPI Methods T 402-om-88, andTIS 808-03.7.3 Vials,7headspace, 20 mL (actual volume 21.5 mL). Toensure against extraneous peaks in the gas chromatographictraces, wash vials thoroughly and dry in a 125C air oven fora minimum of 4
25、h before using.7.4 Vial Crimp Caps.87.5 Septa, Polytetrafluoroethylene (PTFE)/silicone.9To en-sure that the septa are free of volatiles, cover the bottom of a15-cm petri dish with septa, PTFE-polymer side up. Micro-wave at full power for 10 min. Place microwaved septa into avacuum (greater than 29 i
26、n.) oven at 130C for 16 h.7.6 Crimping Tool for vials.107.7 Syringe, 2 mL, gas-tight with valve.11Store syringe in90C oven between uses.7.8 Gas Chromatograph equipped as follows:7.8.1 FID Detector, compatible with capillary columns.7.8.2 Injector, split/splitless compatible with capillary col-umns.7
27、.8.3 Automated Headspace Sampler, Optional.127.8.4 Column, DB-5, 30 m, 0.25-mm inside diameter, 1-mfilm thickness,13or 0.32 mm.14(A short piece of deactivated0.25-mm fused silica column may be placed between theinjector and the column to serve as a guard column.)7.8.5 Peak-Area Integration System co
28、mpatible with GCsystem.Alternatively, a chart recorder and hand integration canbe used.7.9 Fluoroptic Thermometry System.157.10 Temperature Probes, high temperature.167.11 Beaker, 600 mL.7.12 Oven, hot air, set for 90C.7.13 Stopwatch.7.14 4-Heptanone.177.15 Standard SolutionsRegular Method:4McCown,
29、S. M., and Radenheimer, P., “An Equilibrium Headspace GasChromatographic Method for the Determination of Volatile Residues in VegetableOils and Fats,” LC/GC, Vol 7, No. 11, 1989, pp. 918924.5McNeal, T. P., and Breder, C. V., “Headspace Gas Chromatographic Determi-nation of Residual 1,3-Butadiene in
30、Rubber-Modified Plastics and Its Migrationfrom Plastic Containers Into Selected Foods,” Journal of the Association ofAnalytical Chemists, Vol 70, No. 1, 1987, pp. 1821.6McNeal, T. P., and Breder, C. V., “Headspace Sampling and Gas-SolidChromatographic Determination of Residual Acrylonitrile in Acryl
31、onitrile Copoly-mer Solutions,” Journal of the Association of Offcial Analytical Chemists, Vol 64,No. 2, 1981, pp. 270275.7Vials from Shamrock Glass Co., 200 N. Delaware Ave., Seaford, DE 302629-5500 (Catalog No. 667601) or from Chemical Research Supplies, P. O. Box888, Addison, IL 60101 or equivale
32、nt vials have been found suitable for thispurpose.8Vial crimp caps from Shamrock Glass Co., Catalog No. 778704 or fromHewlett Packard Computer Supplies Operation, PO Box 62124, San Francisco, CA94162, Catalog No. 07675-120625 or equivalent have been found suitable for thispurpose.9Septa from Shamroc
33、k Glass Co., Catalog No. 778173A or Hewlett-PackardComputer Supplies Operation, Catalog No. 5080-8726 or equivalent have beenfound suitable for this purpose.10Crimping tools from Supelco Inc., Belefonte, PA 16823, Catalog No. 33280.11Syringes from Alltech, 2051 Waukegan Rd., Deerfield, IL 60015, Cat
34、alog No.050034 or equivalent have been found suitable for this purpose.12The Hewlett-Packard Model No. 19395A or equivalent has been foundsuitable for this purpose.13Columns from J and W Scientific, 91 Blue Ravine Rd., Folsom, CA95630-4714, Catalog No. 122-5033 or equivalent has been found suitable
35、for thispurpose.14Catalog No. 123-5033 from J and W Scientific.15Luxtron Model 750 available from Luxtron Inc., 106 Terra Bella Ave.,Mountain View, CA 90403, or equivalent has been found suitable for this purpose.16Luxtron Model MIH or equivalent has been found suitable for this purpose.174-Heptanon
36、e from Aldrich, 940 West St. Paul Ave., Milwaukee, WI 53233,Catalog No. 10, 174-5 or equivalent has been found suitable for this purpose.F 1308 98 (2003)27.15.1 Internal Standard Solution (245 g/mL4-Heptanone)To approximately 950 mL of distilled water ina 1-L volumetric flask add 300 L of 4-heptanon
37、e. Mix welland dilute to volume with water.7.15.2 Standard Solution 1: (Prepare fresh daily.)To ap-proximately 475 mL of internal standard solution in a 500-mLvolumetric flask, add 50 L of each of the compounds to bequantitated. Mix well, and dilute to volume with internalstandard solution. If diffi
38、culty is experienced with dissolutionof analyte, alternate standard solution procedure may over-come this difficulty.7.15.3 Standard Solution 2Repeat 7.14.2 using 25 L ofeach compound.7.15.4 Standard Solution 3Repeat 7.14.2 using 10 L ofeach compound.7.16 Standard SolutionsAlternate Method:7.16.1 Al
39、ternate Internal Standard Solution (1225 g/mL4-Heptanone)To approximately 150 mL of helium-spargedorthodichlorobenzene (ODCB) in a 200-mL volumetric flaskadd 300 Lof 4-heptanone. Mix well and dilute to volume withODCB.7.16.2 Alternate Standard Solution 1 To approximately75 mL of alternate internal s
40、tandard solution in a 100-mLvolumetric flask, add 50 L of each of the compounds to bequantitated. Mix well, and dilute to volume with alternateinternal standard solution.7.16.3 Alternate Standard Solution 2 Repeat 7.15.2 using25 L of each compound.7.16.4 Alternate Standard Solution 3 Repeat 7.15.2 u
41、sing10 L of each compound.7.17 Susceptor BlankObtain a representative sample ofsusceptor material to be tested. Bake in an air oven overnightat 100C or higher to remove any volatile materials present.Store blank susceptor strips in humidity chamber 1 at 50 % RHand 23C until equilibrium moisture cont
42、ent is reached. Anexposure time of 24 h is generally adequate for most paper-based products. Strips should remain in the conditioningenvironment until needed for analysis.7.18 Syringe Needle, 13 gage.7.19 Variable Voltage Transformer, OptionalThis can oc-casionally be used for minor adjustments to l
43、ine voltage tobring power output of the microwave oven into the specifiedrange.8. Instrument Setup8.1 Determine sample test conditions as follows:8.1.1 Set up microwave susceptor in the configuration of itsintended use, that is, a popcorn bag filled with popcorn, a pizzadisk with pizza on top, etc.8
44、.1.2 Place temperature probes (7.10) on susceptor surface,disturbing the normal food load as little as possible. If thesusceptor has areas where the food does not normally contactthe surface, place the probes in these areas. Place the productin the center of the microwave oven.8.1.3 Cook the product
45、 in accordance with normal direc-tions, for the maximum cooking time. Record this time. Recordthe probe temperature(s), preferably at 5-s intervals, but atintervals not to exceed 15 s during cooking.8.1.4 Place 250 mL of room-temperature distilled water intoa 600-mL beaker. Place the beaker in the c
46、enter rear of themicrowave oven.8.1.5 Cut a 10 by 65-mm (6.5-cm2= 1-in.2) portion from thesusceptor sample to be tested. Insert carefully into the 20-mLheadspace vial.8.1.6 Using a 13-gage syringe needle, pierce a hole into aheadspace vial septum. Place the septum on the vial and crimp.8.1.7 Insert
47、one temperature probe (7.10) through the sep-tum hole into the vial and manipulate it until it is in contactwith the active face of the susceptor material. Place the vial onits side in the center of microwave oven, crimp end towardright of the oven, and susceptor with active face up.8.1.8 Microwave
48、at full power, recording the probe tem-perature, preferably at 5-s intervals, but at intervals not toexceed 15 s.8.1.9 Plot the temperatures from 8.1.3 and 8.1.8 on the samegraph.8.1.10 Compare the plots. If the trace from 8.1.8 closelyapproximates or is slightly higher than the plot from 8.1.3 then
49、the test time will be equal to the maximum product cook timeof the product in that oven. If the trace is substantially higheror lower than that of the susceptor with product, then adjust themass or surface area, or both, (by changing container size) ofthe water (using a fresh sample of room temperature distilledwater) as necessary to achieve a similar profile. Record themass of water and type of container that gives the bestagreement between the test sample and the product temperatureprofiles.8.2 Set up the gas chromatographic system to meet
