1、Designation: D1025 10Standard Test Method forNonvolatile Residue of Polymerization-Grade Butadiene1, 2This standard is issued under the fixed designation D1025; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of nonvolatilematerial in polymerization-grade butadiene.1.2 WARNINGMercury has been d
3、esignated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable pro
4、duct Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.3 The values stated in SI units are to be
5、 regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and to
6、 determine theapplicability of regulatory limitations prior to use.2. Summary of Test Method2.1 A measured volume of liquid butadiene is allowed toevaporate at room temperature from a small glass evaporatingdish until only residue remains. The evaporation is thencompleted by heating the dish to a co
7、nstant weight.3. Significance and Use3.1 This test method is used to determine if there is anyheavy material in the butadiene. It is possible that thesematerials could be deleterious to a polymerization reaction.4. Apparatus4.1 Balance, Analytical, capable of weighing to the nearest0.1 mg.4.2 Evapor
8、ating Dish, glass, 80 mm in diameter and 45 mmin height.4.3 Graduated Cylinder, capacity of 25 mL, graduated in0.2-mL subdivisions.4.4 Oven, capable of maintaining a temperature of 105 65C.4.5 Cooling Vessel, tightly covered, such as a glass desic-cator, for cooling the evaporating dish before weigh
9、ing.4.6 Thermometer, range from 40 to 50C, graduated in1C intervals, mercury-filled. Temperature measuring devicesthat cover the temperature range of interest, such as the ASTM1C thermometer or liquid-in-glass thermometers, thermo-couples, or platinum resistance thermometers that provideequivalent o
10、r better accuracy and precision may be used.5. Preparation of Apparatus5.1 Clean the evaporating dishes with a chromic-acid solu-tion or other suitable cleaning agent before each test.(WarningCauses severe burns. A recognized carcinogen.Strong oxidizer. Contact with organic material may cause fire.)
11、Remove the dishes from the cleaning solution with stainless-steel forceps and handle only with forceps thereafter. Wash thedishes thoroughly, first with tap water, then with distilled water,and dry in the oven at 105C for about 1 h, or until constantweight is obtained. Before weighing, cool the dish
12、es for at least30 min in the cooling vessel.6. Procedure6.1 Weigh the evaporating dish to the nearest 0.1 mg on theanalytical balance.6.2 Chill the evaporating dish to ice temperature. Cool thebutadiene and the graduated cylinder to about 20C.(WarningExtremely flammable gas under pressure. Mayform e
13、xplosive peroxides upon exposure to air. Harmful ifinhaled. Irritating to eyes, skin, and mucous membranes.)Determine the sample temperature to the nearest 1C andtransfer 25 6 1 mL of sample to the evaporating dish. Recordthe sample volume and temperature.1This test method is under the jurisdiction
14、of Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.D0.04on C4 Hydrocarbons.Current edition approved May 1, 2010. Published June 2010. Originallyapproved in 1949. Last previous edition approved in 2004 as D102500(2004).DOI: 10.1520/D1025-10.2This
15、 test method is an adaptation of one developed and cooperatively tested bythe Butadiene Producers Committee on Specifications and Methods of Analysis ofthe Office of Rubber Reserve. It appears in the Butadiene Laboratory Manual, Officeof Rubber Reserve, as Method No. 2.1.56.2.1Copyright ASTM Interna
16、tional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Allow the sample to evaporate at room temperature in awell-ventilated hood. When evaporation is complete, place theevaporating dish in an oven at 105 6 5C until a weightconstant to 0.1 mg is obtained. Bef
17、ore each weighing, cool thedish for at least 30 min in the cooling vessel. Between each twoweighings, place the dish in the oven for at least 30 min.7. Calculation7.1 Calculate the amount of nonvolatile residue by means ofthe following equation:Nonvolatile residue, weight % 5 B 2 A!/ Sd 3 100where:A
18、 = weight of the evaporating dish, gB = weight of the evaporating dish plus residue, g,S = volume of the liquid butadiene sample, mL, andd = density of the sample at the temperature of measure-ment, g/mL, found by using Table 1.8. Precision and Bias8.1 PrecisionThe precision of this test method as d
19、eter-mined by statistical examination of interlaboratory results is asfollows:8.1.1 RepeatabilityThe difference between two test re-sults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and corre
20、ct operation ofthe test method, exceed the following values in only one casein twenty:0.02 %8.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in the normal
21、 and correct operation of the testmethod, exceed the following values in only one case intwenty:0.04 %8.1.3 BiasSince there is no accepted reference materialsuitable for determining the bias for the procedure in this testmethod for measuring non-volatile residue, no statement onbias is being made.9.
22、 Keywords9.1 butadiene; nonvolatile residueASTM 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
23、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 be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision
24、 of this 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 shou
25、ldmake 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 obtai
26、ned 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 1 Density of Butadiene at Various TemperaturesNOTEThese data may be used in a graphical manner for betterinterpolation between data points.Temperature, C Density, g/mL45 0.695840 0.690335 0.684830 0.679325 0.673720 0.668115 0.662510 0.65685 0.65100 0.6452D1025 102
