Acetone Extraction of Phenolic Molded or Laminated Products1 This standard is issued under the fixed designation D 494; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1.1 This test method covers the determination of the amount thickness of the section from which sample is taken, (6) nature of acetone-soluble matter in molded or laminated phenolic of molded piece, (7) technique used in molding, (8) distribution products. of fines in the material to be extracted, and (9) method of 1.2 The values stated in SI units are to be regarded as the grinding the specimen. These variations under some conditions standard. may cause a difference of 3 to 4 % in acetone-extractable 1.3 This standard does not purport to address all of the matter. For this reason, the test method should be used only as safety problems, if any, associated with its use. It is the a comparative test for measuring undercure. responsibility of the user of this standard to establish appro- 4.2 For laminated phenolic products, acetone extraction priate safety and health practices and determine the applica- indicates change in stage of cure, change in resin content, bility of regulatory limitations prior to use. change in type of resin used, presence of plasticizers or other acetone-extractable addition agents, and is affected in general 2. Referenced Documents by the same factors as stated in 6.1 2.1 ASTM Standards: 2 5. Apparatus D 618 Practice for Conditioning Plastics for Testing D 883 Terminology Relating to Plastics 5.1 SievesThe set of sieves used shall consist of sieves E 11 Specification for Wire Cloth and Sieves for Testing Nos. 40 (425-m) and 140 (106-m), with a cover and Purposes receiving pan, conforming to the requirements of Specification E 691 Practice for Conducting an Interlaboratory Study to E 11. Determine the Precision of a Test Method 5.2 Extraction ApparatusThe apparatus may be of the type shown in Fig. 1, or a Wiley-Richardson type, as shown in 3. Terminology Fig. 2. The former type is more suitable for use with small 3.1 All definitions are in accordance with Terminology electric hot plates, while the latter is more suitable for use with D 883. oil or water baths. In either case, it shall be possible to control the temperature so that the rate of extraction can be regulated 4. Significance and Use accurately. 4.1 For molded phenolic products, acetone extraction 5.3 Drying DishesThe drying dishes shall be lightweight should be considered solely as a quantitative expression of a dishes, approximately 63.5 mm [212 in.] in diameter and 38.1 property normally associated with degree of cure. There is no mm [112 in.] in height. demonstrably rigorous relation between the optimum mechani- 6. Preparation of Sample cal and electrical properties of a well-cured piece and the numerical value of the acetone test. The amount of acetone- 6.1 PrecautionsIt is of utmost importance that extreme soluble matter is affected by: (1) nature of resin and filler, (2) care shall be taken during the preparation of the sample for extraction. The sample shall be drillings if possible; however, if not possible, other suitable means of producing particles 1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics equivalent to drillings may be used. Drillings taken from a and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. large molded product shall be truly representative of all Current edition approved July 1, 2004. Published July 2004. Originally approved in 1946. Last previous edition approved in 1991 as D 494 - 91 which was withdrawn sections of the part in proper proportions. The drills for March 1998 and reinstated in July 2004. sampling shall be kept sharp and so operated that no undue 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or heating of the material shall occur which will tend to precure contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards volume information, refer to the standards Document Summary page on the material. the ASTM website.
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1 D 494 04
FIG. 2 Wiley-Richardson Type Extraction Apparatus
7. Conditioning 7.1 Condition the test specimens at 23 6 2C [73.4 6 3.6F] and 50 6 5 % relative humidity for not less than 40 h prior to test in accordance with Procedure A of Practice D 618 for those tests where conditioning is required. In cases of FIG. 1 Extraction Apparatus disagreement, the tolerances shall be 1C [1.8F] and 62 % relative humidity. 6.2 If it is impracticable to obtain samples by drilling, the 7.2 Test ConditionsConduct tests in the standard labora- parts may be broken up with a lathe, planer, milling machine, tory atmosphere of 23 6 2C [73.4 6 3.6F] and 50 6 5 % or a suitable grinder. A mortar and pestle or a pebble mill is relative humidity, unless otherwise specified in the test meth- considered suitable as a grinder, provided no perceptible ods or in this test method. In cases of disagreements, the heating occurs during the grinding procedure. A sharp file or tolerances shall be 1C [1.8F] and 62 % relative humidity. rasp may be used for procuring the sample where the size or shape of the part is such that no other method is suitable. 8. Procedure 6.3 In any case, the particles of the sample shall be of the 8.1 PrecautionsSince the method could otherwise expose smallest size practicable, so that they will pass through the No. the user to potentially unhealthy fumes of volatile organic 40 sieve with the minimum of reworking or grinding. It is chemicals, notably acetone, it is recommended that such important in preparing the sample that the smallest possible exposure be kept within strict conformity of applicable estab- volume shall be obtained for a unit weight of the material. lished OSHA Permissible Exposure Limits (PEL) and Time 6.4 The sample shall be sieved through a No. 40 sieve and Weighted Average (TWA) rules and other available guidance that part which will not pass through shall be reground and protocols for any of the organic solvents used. Exposure blended with the original material passing the sieve. After guidelines should be available in the Material Safety Data assembling the Nos. 40 and 140 sieves and the receiving pan, Sheet, Section 8, Exposure Control / Personal Protection. the sample shall be placed in the top sieve, the cover placed on, Typical safety measures include the use of engineering con- and the entire sample shall be resieved either by a mechanical trols, fully operating and properly adjusted ventilation and sieve shaker or hand sieving. If the hand-sieving method is personal protective equipment, such as hand, eye and breathing used, the sieve shall be rotated with slight tapping, the period protection, along with reliable monitoring and confirmation of of rotation being 5 min. compliance with designated OSHA and other applicable expo- 6.5 After sieving, the sample (that portion which has passed sure limits. through the No. 40 sieve and has been retained on the No. 140 8.2 ExtractionThe extraction procedure shall be carried sieve) shall be placed immediately in an airtight container to out in triplicate. Accurately weigh a 3.000-g portion of the prevent absorption of moisture by the powder and the conse- powdered sample into a tared, acid-hardened open-texture quent error in results. quantitative filter paper, 12.5 to 15 cm in diameter, or into a
2 D 494 04 standard, single-thickness extraction thimble, 80 by 22 mm, where: trimmed if necessary. After folding over the thimble or filter W = weight of the dish and extract, g, paper containing the sample so that none of the powder can D = weight of the dish, g, and float out, place it in a desiccator until ready to insert in the S = weight of original sample, g. siphon. 8.3 Press the filter paper or thimble containing the weighed 10. Report sample into the siphon in such a way that the outlet of the 10.1 Report the following information: bottom is not plugged. Place the condenser and the siphon in 10.1.1 Percentage of acetone-extractable matter for each the extraction tube and add 50 mL of cp acetone. Start the sample, and water through the condenser and adjust the heat (Note 1) so 10.1.2 Average percentage of acetone-extractable matter for that the siphon fills and empties between 15 and 20 times/h. the three samples. This rate shall be carefully maintained, and the sample shall be 11. Precision and Bias 3 extracted for 4 h. After the siphon empties, remove the flask and pour the contents into an individually weighed dish. Wash 11.1 Table 1 is based on an interlaboratory study in 1989 in the flask three times with the smallest possible quantity of accordance with Practice E 691, involving six materials tested acetone, using a wash bottle, and add the washings to the by six laboratories. extracted liquid in the dish. 11.2 Since no absolute method is available for comparison, no statement of bias can be presented for this test method. NOTE 1If an oil or water bath is used for heating, the height of the liquid in the bath should not come above 2.5 cm [1 in.] below the highest 12. Keywords level of the acetone in the siphon before the siphon starts to discharge. 12.1 acetone extraction; cure; laminated plastic; molded 8.4 DryingPlace the dish in a well-ventilated drying plastic; phenolic resin; plasticizers chamber, maintained at 50 6 2C and dry the sample to constant weight. Between dryings, all dishes containing the 3 Supporting data are available from ASTM International Headquarters. Request residue shall be kept in a desiccator to prevent the absorption RR:D20-1169. of moisture. 8.5 It is very important that the specified temperature shall TABLE 1 Precision Statistics be maintained, otherwise consistent results cannot be obtained Values in the Units of Extracted % between different laboratories. WarningAn electrically Material Average srA sRB rC RD heated oven should not be used unless it is exceedingly well A .3916 .08725 .2244 .24 .63 ventilated, as the acetone fumes are likely to come in contact B .5044 .0951 .2220 .27 .62 with the heated coils and cause an explosion. C .5406 .1590 .2223 .45 .62 D .5922 .2059 .2361 .58 .66 E 4.7628 .2142 1.2449 .60 3.49 9. Calculation F 4.6022 .2678 1.1051 .75 3.09 9.1 Calculate the percentage of acetone-extractable matter A sr is the within-laboratory standard deviation of the average. B in the specimen as follows: sR is the between-laboratories standard deviation of the average. C r = 2.8 sr. Acetone2extractable matter, % 5 [~W 2 D!/S] 3 100 (1) D R = 2.8 sR.
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