1、Designation: D 494 04Standard Test Method forAcetone Extraction of Phenolic Molded or LaminatedProducts1This standard is issued under the fixed designation D 494; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 the determination of the amountof acetone-soluble matter in molded or laminated phenolicproducts.1.2
3、The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of thesafety problems, 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 appli
4、ca-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 618 Practice for Conditioning Plastics for TestingD 883 Terminology Relating to PlasticsE 11 Specification for Wire Cloth and Sieves for TestingPurposesE 691 Practice for Conducting an Interlaboratory Study
5、 toDetermine the Precision of a Test Method3. Terminology3.1 All definitions are in accordance with TerminologyD 883.4. Significance and Use4.1 For molded phenolic products, acetone extractionshould be considered solely as a quantitative expression of aproperty normally associated with degree of cur
6、e. There is nodemonstrably rigorous relation between the optimum mechani-cal and electrical properties of a well-cured piece and thenumerical value of the acetone test. The amount of acetone-soluble matter is affected by: (1) nature of resin and filler, (2)lubricant, (3) molding temperature, (4) len
7、gth of cure, (5)thickness of the section from which sample is taken, (6) natureof molded piece, (7) technique used in molding, (8) distributionof fines in the material to be extracted, and (9) method ofgrinding the specimen. These variations under some conditionsmay cause a difference of 3 to 4 % in
8、 acetone-extractablematter. For this reason, the test method should be used only asa comparative test for measuring undercure.4.2 For laminated phenolic products, acetone extractionindicates change in stage of cure, change in resin content,change in type of resin used, presence of plasticizers or ot
9、heracetone-extractable addition agents, and is affected in generalby the same factors as stated in 6.15. Apparatus5.1 SievesThe set of sieves used shall consist of sievesNos. 40 (425-m) and 140 (106-m), with a cover andreceiving pan, conforming to the requirements of SpecificationE11.5.2 Extraction
10、ApparatusThe apparatus may be of thetype shown in Fig. 1, or a Wiley-Richardson type, as shown inFig. 2. The former type is more suitable for use with smallelectric hot plates, while the latter is more suitable for use withoil or water baths. In either case, it shall be possible to controlthe temper
11、ature so that the rate of extraction can be regulatedaccurately.5.3 Drying DishesThe drying dishes shall be lightweightdishes, approximately 63.5 mm 212 in. in diameter and 38.1mm 112 in. in height.6. Preparation of Sample6.1 PrecautionsIt is of utmost importance that extremecare shall be taken duri
12、ng the preparation of the sample forextraction. The sample shall be drillings if possible; however,if not possible, other suitable means of producing particlesequivalent to drillings may be used. Drillings taken from alarge molded product shall be truly representative of allsections of the part in p
13、roper proportions. The drills forsampling shall be kept sharp and so operated that no undueheating of the material shall occur which will tend to precurethe material.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 o
14、n Analytical Methods.Current edition approved July 1, 2004. Published July 2004. Originally approvedin 1946. Last previous edition approved in 1991 as D 494 - 91 which was withdrawnMarch 1998 and reinstated in July 2004.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
15、ASTM Customer Service at serviceastm.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.6.2 If it is impracticable
16、 to obtain samples by drilling, theparts may be broken up with a lathe, planer, milling machine,or a suitable grinder. A mortar and pestle or a pebble mill isconsidered suitable as a grinder, provided no perceptibleheating occurs during the grinding procedure. A sharp file orrasp may be used for pro
17、curing the sample where the size orshape of the part is such that no other method is suitable.6.3 In any case, the particles of the sample shall be of thesmallest size practicable, so that they will pass through the No.40 sieve with the minimum of reworking or grinding. It isimportant in preparing t
18、he sample that the smallest possiblevolume shall be obtained for a unit weight of the material.6.4 The sample shall be sieved through a No. 40 sieve andthat part which will not pass through shall be reground andblended with the original material passing the sieve. Afterassembling the Nos. 40 and 140
19、 sieves and the receiving pan,the sample shall be placed in the top sieve, the cover placed on,and the entire sample shall be resieved either by a mechanicalsieve shaker or hand sieving. If the hand-sieving method isused, the sieve shall be rotated with slight tapping, the periodof rotation being 5
20、min.6.5 After sieving, the sample (that portion which has passedthrough the No. 40 sieve and has been retained on the No. 140sieve) shall be placed immediately in an airtight container toprevent absorption of moisture by the powder and the conse-quent error in results.7. Conditioning7.1 Condition th
21、e test specimens at 23 6 2C 73.4 63.6F and 50 6 5 % relative humidity for not less than 40 hprior to test in accordance with Procedure A of Practice D 618for those tests where conditioning is required. In cases ofdisagreement, the tolerances shall be 1C 1.8F and 62%relative humidity.7.2 Test Conditi
22、onsConduct tests in the standard labora-tory atmosphere of 23 6 2C 73.4 6 3.6F and 50 6 5%relative humidity, unless otherwise specified in the test meth-ods or in this test method. In cases of disagreements, thetolerances shall be 1C 1.8F and 62 % relative humidity.8. Procedure8.1 PrecautionsSince t
23、he method could otherwise exposethe user to potentially unhealthy fumes of volatile organicchemicals, notably acetone, it is recommended that suchexposure be kept within strict conformity of applicable estab-lished OSHA Permissible Exposure Limits (PEL) and TimeWeighted Average (TWA) rules and other
24、 available guidanceprotocols for any of the organic solvents used. Exposureguidelines should be available in the Material Safety DataSheet, Section 8, Exposure Control / Personal Protection.Typical safety measures include the use of engineering con-trols, fully operating and properly adjusted ventil
25、ation andpersonal protective equipment, such as hand, eye and breathingprotection, along with reliable monitoring and confirmation ofcompliance with designated OSHA and other applicable expo-sure limits.8.2 ExtractionThe extraction procedure shall be carriedout in triplicate. Accurately weigh a 3.00
26、0-g portion of thepowdered sample into a tared, acid-hardened open-texturequantitative filter paper, 12.5 to 15 cm in diameter, or into aFIG. 1 Extraction ApparatusFIG. 2 Wiley-Richardson Type Extraction ApparatusD494042standard, single-thickness extraction thimble, 80 by 22 mm,trimmed if necessary.
27、 After folding over the thimble or filterpaper containing the sample so that none of the powder canfloat out, place it in a desiccator until ready to insert in thesiphon.8.3 Press the filter paper or thimble containing the weighedsample into the siphon in such a way that the outlet of thebottom is n
28、ot plugged. Place the condenser and the siphon inthe extraction tube and add 50 mL of cp acetone. Start thewater through the condenser and adjust the heat (Note 1) sothat the siphon fills and empties between 15 and 20 times/h.This rate shall be carefully maintained, and the sample shall beextracted
29、for 4 h. After the siphon empties, remove the flaskand pour the contents into an individually weighed dish. Washthe flask three times with the smallest possible quantity ofacetone, using a wash bottle, and add the washings to theextracted liquid in the dish.NOTE 1If an oil or water bath is used for
30、heating, the height of theliquid in the bath should not come above 2.5 cm 1 in. below the highestlevel of the acetone in the siphon before the siphon starts to discharge.8.4 DryingPlace the dish in a well-ventilated dryingchamber, maintained at 50 6 2C and dry the sample toconstant weight. Between d
31、ryings, all dishes containing theresidue shall be kept in a desiccator to prevent the absorptionof moisture.8.5 It is very important that the specified temperature shallbe maintained, otherwise consistent results cannot be obtainedbetween different laboratories. WarningAn electricallyheated oven sho
32、uld not be used unless it is exceedingly wellventilated, as the acetone fumes are likely to come in contactwith the heated coils and cause an explosion.9. Calculation9.1 Calculate the percentage of acetone-extractable matterin the specimen as follows:Acetone2extractable matter, % 5 W 2 D!/S 3 100 (1
33、)where:W = weight of the dish and extract, g,D = weight of the dish, g, andS = weight of original sample, g.10. Report10.1 Report the following information:10.1.1 Percentage of acetone-extractable matter for eachsample, and10.1.2 Average percentage of acetone-extractable matter forthe three samples.
34、11. Precision and Bias311.1 Table 1 is based on an interlaboratory study in 1989 inaccordance with Practice E 691, involving six materials testedby six laboratories.11.2 Since no absolute method is available for comparison,no statement of bias can be presented for this test method.12. Keywords12.1 a
35、cetone extraction; cure; laminated plastic; moldedplastic; phenolic resin; plasticizersASTM 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
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38、ts 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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or mu
39、ltiple 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).3Supporting data are available from ASTM International Headquarters. RequestRR:D20-1169.TABLE
40、1 Precision StatisticsValues in the Units of Extracted %Material Average srAsRBrCRDA .3916 .08725 .2244 .24 .63B .5044 .0951 .2220 .27 .62C .5406 .1590 .2223 .45 .62D .5922 .2059 .2361 .58 .66E 4.7628 .2142 1.2449 .60 3.49F 4.6022 .2678 1.1051 .75 3.09Asris the within-laboratory standard deviation of the average.BsRis the between-laboratories standard deviation of the average.Cr = 2.8 sr.DR = 2.8 sR.D494043
