ASTM D494-2004(2010)e1 Standard Test Method for Acetone Extraction of Phenolic Molded or Laminated Products《酚醛模压或层压产品的丙酮萃取标准试验方法》.pdf

1、Designation: D494 04 (Reapproved 2010)1Standard Test Method forAcetone Extraction of Phenolic Molded or LaminatedProducts1This standard is issued under the fixed designation D494; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the

2、 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 July 2010.1. Scope*1.1 This test method covers the determination of the amounto

3、f acetone-soluble matter in molded or laminated phenolicproducts.1.2 The values stated in SI units are to be regarded asstandard.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

4、 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1This test method is similar to ISO 308.2. Referenced Documents2.1 ASTM Standards:2D618 Practice for Conditioning Plastics for TestingD883 Terminology Relating to PlasticsE11 Specif

5、ication for Woven Wire Test Sieve Cloth and TestSievesE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standards:ISO 308 PlasticsPhenolic moulding materialsDetermination of acetone-soluble matter (apparent resincontent of material in the unmould

6、ed state)3. Terminology3.1 All definitions are in accordance with TerminologyD883.4. Significance and Use4.1 For molded phenolic products, acetone extraction shallbe considered solely as a quantitative expression of a propertynormally associated with degree of cure. There is no demon-strably rigorou

7、s relation between the optimum mechanical andelectrical properties of a well-cured piece and the numericalvalue of the acetone test. The amount of acetone-soluble matteris affected by: (1) nature of resin and filler, (2) lubricant, (3)molding temperature, (4) length of cure, (5) thickness of thesect

8、ion from which sample is taken, (6) nature of molded piece,(7) technique used in molding, (8) distribution of fines in thematerial to be extracted, and (9) method of grinding thespecimen. These variations under some conditions will cause adifference of 3 to 4 % in acetone-extractable matter. For thi

9、sreason, the test method shall be used only as a comparative testfor 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 otheracetone-extractable addition agent

10、s, 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 ApparatusThe apparatus may be of thet

11、ype 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 with1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of S

12、ubcommittee D20.70 on Analytical Methods.Current edition approved July 1, 2010. Published October 2010. Originallyapproved in 1946. Last previous edition approved in 2004 as D494 - 04. DOI:10.1520/D0494-04R10E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cus

13、tomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke

14、n, PA 19428-2959, United States.oil or water baths. In either case, it shall be possible to controlthe temperature 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

15、height.6. Preparation of Sample6.1 PrecautionsIt is of utmost importance that extremecare shall be taken during 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 shall be

16、 used. Drillings taken from alarge molded product shall be truly representative of allsections of the part in proper 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.NOTE 2If it is impracti

17、cable to obtain samples by drilling, the partsmay be broken up with a lathe, planer, milling machine, or a suitablegrinder. A mortar and pestle or a pebble mill is considered suitable as agrinder, provided no perceptible heating occurs during the grindingprocedure. A sharp file or rasp may be used f

18、or procuring the samplewhere the size or shape of the part is such that no other method is suitable.6.2 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 prepa

19、ring the sample that the smallest possiblevolume shall be obtained for a unit weight of the material.6.3 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 a

20、nd 140 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 be

21、ing 5 min.6.4 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 Condit

22、ion the 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 D618for those tests where conditioning is required. In cases ofdisagreement, the tolerances shall be 1C 1.8F and 62%relative humidity.7.2 Test Co

23、nditionsConduct 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.FIG. 1 Extraction ApparatusFI

24、G. 2 Wiley-Richardson Type Extraction ApparatusD494 04 (2010)128. Procedure8.1 PrecautionsSince the method is capable of exposingthe user to potentially unhealthy fumes of volatile organicchemicals, notably acetone, such exposure shall be kept withinstrict conformity of applicable established OSHA P

25、ermissibleExposure Limits (PEL) and Time Weighted Average (TWA)rules and other available guidance protocols for any of theorganic solvents used. Exposure guidelines should be availablein the Material Safety Data Sheet, Section 8, Exposure Control/ Personal Protection. Typical safety measures include

26、 the useof engineering controls, fully operating and properly adjustedventilation and personal protective equipment, such as hand,eye and breathing protection, along with reliable monitoringand confirmation of compliance with designated OSHA andother applicable exposure limits.8.2 ExtractionThe extr

27、action procedure shall be carriedout in triplicate. Accurately weigh a 3.000-g portion of thepowdered sample into a tared, acid-hardened open-texturequantitative filter paper, 12.5 to 15 cm in diameter, or into astandard, single-thickness extraction thimble, 80 by 22 mm,trimmed if necessary. After f

28、olding 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 not plugg

29、ed. 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 3)sothat the siphon fills and empties between 15 and 20 times/h.This rate shall be carefully maintained, and the sample shall beextracted for 4 h.

30、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 3If an oil or water bath is used for heating,

31、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 dryings, a

32、ll 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.NOTE 4An electrically heated oven should not be

33、 used unless it isexceedingly well ventilated, as the acetone fumes are likely to come incontact with 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)where:W =

34、 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.11. Precis

35、ion and Bias311.1 Table 1 is based on an interlaboratory study in 1989 inaccordance with Practice E691, 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 acetone extr

36、action; cure; laminated plastic; moldedplastic; phenolic resin; plasticizers3Supporting data are available from ASTM International Headquarters. RequestRR:D20-1169.D494 04 (2010)13SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D

37、494 - 04)that may impact the use of this standard. (July 1, 2010)(1) Added the ISO equivalency statement as Note 1.(2) Removed non-mandatory language in sections 4.1, 5.2,6.1, and 8.1.(3) Changed Section 6.2 to Note 2.(4) Renumbered Notes in text and renumbered text outline.(5) Changed text immediat

38、ely following section 8.5 to Note 4.ASTM 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 of any such patent rights, and the ris

39、kof 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 are invited either for revision of thi

40、s 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 received a fair hearing you shouldmake

41、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) of this standard may be obtained by

42、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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 1 Precision StatisticsValu

43、es 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 =2.8sr.DR =2.8sR.D494 04 (2010)14