1、Designation: D 4559 99 (Reapproved 2004)Standard Test Method forVolatile Matter in Silicone Fluid1This standard is issued under the fixed designation D 4559; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. 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 describes a procedure for determiningthe volatile matter in silicone fluids used for electrical insula-tion.1.2 T
3、his standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of whoever uses this standard to consult andestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.2. Refere
4、nced Documents2.1 ASTM Standards:2D 923 Test Method for Sampling Electrical Insulating Liq-uidsD 2225 Test Methods for Silicone Fluids Used for ElectricalInsulationD 4652 Specification for Silicone Fluid Used for ElectricalInsulationD 5423 Specification for Forced-Convection LaboratoryOvens for Eval
5、uation of Electrical Insulation3. Summary of Test Method3.1 Specimens are weighed before and after heating for aspecific time in a forced air oven to determine weight loss.4. Significance and Use4.1 High values may indicate contamination of the siliconewith other materials, inadequate removal of vol
6、atile compo-nents by the producer, or the presence of a depolymerizationcatalyst.4.2 The outcome will be affected directly by the presence ofany high vapor pressure material in the sample, such assolvents or low molecular weight silicones.4.3 A high volatile content could also indicate the presenceo
7、f a depolymerization catalyst in the fluid. The time andtemperature specified in this test method are ideal for detectingthe effect of such a material, as the depolymerization takesplace at a highly accelerated rate and the low molecular weightcomponents are rapidly evaporated. The result is a verys
8、ignificant weight loss during the test period. The exact amountdepends on the type and amount of catalyst present. Theconditions specified in the method should not cause measure-able depolymerization of silicone if such a catalyst is notpresent.5. Apparatus5.1 Air-circulating Oven, capable of meetin
9、g the require-ments of Specification D 5423.5.2 Griffn Pyrex Beakers, 50-mL, with the following di-mensions:5.2.1 Outside Diameter42 6 0.6 mm.5.2.2 Wall Thickness0.14 to 0.165 mm.5.3 Analytical Balance, capable of measuring to 1 mg.6. Sampling6.1 Obtain a sample of the silicone fluid to be tested us
10、ingappropriate ASTM sampling apparatus in accordance with TestMethods D 923.7. Procedure7.1 Clean two 50-mL beakers by washing in toluene,followed by a rinse in acetone or other appropriate cleaningmethod.7.2 Bake two 50-mL beakers at 150 6 5C for a minimumof 1 h, transfer to a desiccator using clea
11、n, dry gloves orcrucible tongs and cool the beakers to ambient temperatures.Use clean, dry gloves or crucible tongs to handle beakers fromthis point forward. Weigh each beaker to the nearest mg (T).7.3 Weigh a 2.0 6 0.2 g sample to the nearest mg in eachbeaker (W1).7.4 Heat at 150 6 5C in an air cir
12、culating oven for 24 60.25 h, cool in a desiccator, and reweigh (W2).8. Calculation and Report8.1 Calculate the volatile matter in silicone fluid as follows:Volatile Matter, % 5W12 W2W12 T3 1001This test method is under the jurisdiction of ASTM Committee D27 onElectrical Insulating Liquids and Gases
13、 and is the direct responsibility of Subcom-mittee D27.07 on Physical Test.Current edition approved Oct. 1, 2004. Published November 2004. Originallyapproved in 1986. Last previous edition approved in 1999 as D 4559 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact A
14、STM 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.where:W1= weight of silicon
15、e fluid and beaker,W2= weight of silicone fluid and beaker after heating, andT = weight of beaker.8.2 Calculate the volatile matter, as the simple averagepercentage of the two tests.8.3 Report the simple average of the two tests, rounded tothe nearest 0.1 % as the volatile matter, %.9. Precision and
16、 Bias39.1 RepeatabilityThe difference between results obtainedby the same operator with the same apparatus under constantoperating conditions on identical test material would, in thelong run, exceed the value of 0.243 only one case in twenty.9.2 ReproducibilityThe difference between two single andin
17、dependent results obtained by different operators working indifferent laboratories on identical test material would, in thelong run, exceed the value of 0.565 only one case in twenty.9.3 BiasAn estimate of bias of -0.032 was obtained forthis test method using the spiked values and the measuredvalue
18、of the base oil.9.4 Limit of DetectabilityThe limit of detectability wasnot calculated due to insufficient data.10. Keywords10.1 insulating liquid; silicone; volaticityASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin t
19、his standard. Users of this standard are expressly advised that determination of the validity 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
20、be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments 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 there
21、sponsible technical committee, which you may attend. If you feel that your comments 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,
22、West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple 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).3A research report is available from ASTM International. RequestRR:D271010.D 4559 99 (2004)2
