1、Designation: D1025 10 (Reapproved 2015)1Standard 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
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.1NOTESubsection 5.6 was revised editorially in May 2015.1. Scope1.1 This test method covers the determination of nonvolati
3、lematerial in polymerization-grade butadiene.1.2 WARNINGMercury has been designated 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 wh
4、en handling mercury andmercury containing products. See the applicable product 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 c
5、ountrymay be prohibited by law.1.3 The values stated in SI units are to be 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
6、this standard to establish appro-priate safety and health practices and to determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:E1 Specification for ASTM Liquid-in-Glass Thermometers3. Summary of Test Method3.1 A measured volume of liquid butadi
7、ene 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 constant weight.4. Significance and Use4.1 This test method is used to determine if there is anyheavy material in the butadiene. It
8、is possible that thesematerials could be deleterious to a polymerization reaction.5. Apparatus5.1 Balance, Analytical, capable of weighing to the nearest0.1 mg.5.2 Evaporating Dish, glass, 80 mm in diameter and 45 mmin height.5.3 Graduated Cylinder, capacity of 25 mL, graduated in0.2 mL subdivisions
9、.5.4 Oven, capable of maintaining a temperature of 105 C 65 C.5.5 Cooling Vessel, tightly covered, such as a glassdesiccator, for cooling the evaporating dish before weighing.5.6 Thermometer, range from 40 C to 50 C, graduated in1 C intervals, conforming to the requirements for ASTMThermometer 1C as
10、 prescribed in Specification E1 is satisfac-tory. Temperature measuring devices that cover the tempera-ture range of interest, such as the ASTM 1C thermometer, orliquid-in-glass thermometers, thermocouples, or platinum re-sistance thermometers that provide equivalent or better accu-racy and precisio
11、n may be used.6. Preparation of Apparatus6.1 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.)Remove the dishes from the cle
12、aning 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 105 C for about 1 h, or until constantweight is obtained. Before weighing, cool the dishes for at least30 min in the
13、cooling vessel.1This test method is under the jurisdiction of Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.D0.04 on C4 Hydrocarbons.Current edition approved April 1, 2015. Published May 2015. Originallyapproved in 1949. Last p
14、revious edition approved in 2010 as D1025 10. DOI:10.1520/D1025-10R15E01.2This 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 M
15、anual, Officeof Rubber Reserve, as Method No. 2.1.56.2.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Procedure7.1 Weigh the evaporating dish to the nearest 0.1 mg on theanalytical balance.7.2 Chill the evaporating dish to ice tem
16、perature. Cool thebutadiene and the graduated cylinder to about 20 C.(WarningExtremely flammable gas under pressure. Mayform explosive peroxides upon exposure to air. Harmful ifinhaled. Irritating to eyes, skin, and mucous membranes.)Determine the sample temperature to the nearest 1 C andtransfer 25
17、 mL 6 1 mL of sample to the evaporating dish.Record the sample volume and temperature.7.3 Allow the sample to evaporate at room temperature in awell-ventilated hood. When evaporation is complete, place theevaporating dish in an oven at 105 C 6 5 C until a weightconstant to 0.1 mg is obtained. Before
18、 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.8. Calculation8.1 Calculate the amount of nonvolatile residue by means ofthe following equation:Nonvolatile residue, weight % 5 B 2 A!/Sd# 3100where:A = w
19、eight 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 ofmeasurement, g/mL, found by using Table 1.9. Precision and Bias9.1 PrecisionThe precision of this test method as deter-m
20、ined by statistical examination of interlaboratory results is asfollows:9.1.1 RepeatabilityThe difference between two test resultsobtained by the same operator with the same apparatus underconstant operating conditions on identical test material would,in the long run, in the normal and correct opera
21、tion of the testmethod, exceed the following values in only one case intwenty:0.02%9.1.2 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 and corr
22、ect operation of the testmethod, exceed the following values in only one case intwenty:0.04%9.1.3 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.10. Keywords
23、10.1 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 the risk
24、of 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 this
25、 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 y
26、our 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 c
27、ontacting 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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1 Density of Butadiene at Various TemperaturesNOTE 1These 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 10 (2015)12
