1、Designation: D 5805 00 (Reapproved 2004)e1Standard Test Methods forRubberDetermination of Carbon Black in Masterbatches1This standard is issued under the fixed designation D 5805; 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 (e) indicates an editorial change since the last revision or reapproval.e1NOTEThe title, keywords, and footnotes were revised editorially in December 2004.1. Scope1.1 These test methods cover
3、the determination of theamount of carbon black in a masterbatch and cover emulsionSBR-carbon black mixtures, but may be applicable to otherpolymers. Three test methods are included:SectionsInert Atmosphere Pyrolysis 3-10Vacuum Pyrolysis 11-17Thermogravimetric Analyzer 18-24NOTE 1The nomenclature use
4、d in these test methods is in accordancewith Practice D 1418.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is th
5、eresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1418 Practice for Rubber and Rubber LaticesNomenclatureD 6370 Test Method for Rubber
6、Compositional Analysisby Thermogravimetry (TGA)TEST METHOD ACARBON BLACKInert Atmosphere Pyrolysis Test Method3. Summary of Test Method3.1 The prepared dried sample and a sample of standardSBR black determinate are tested in triplicate. The samples areweighed accurately into tared crucibles and then
7、 placed in acombustion tube at 550C, which is continuously flushed withCO2until the rubber hydrocarbon is distilled. The crucibles andcontents are cooled in a desiccator, weighed, then inserted intoa muffle furnace at 550C until all carbonaceous material isburned. The crucible and contents are again
8、 cooled in adesiccator and weighed. The percentage of carbon black iscalculated from the weights.4. Significance and Use4.1 The carbon black content of an unvulcanized black oroil-black SBR masterbatch may be determined by this testmethod if an inert (CO2) atmosphere and a determinate (seeNote 2) of
9、 known carbon black content are available.NOTE 2Determinate black masterbatch may be prepared by carefuladdition of exact amounts of rubber and carbon black on a mill. Analternative would be a thorough blending of a quantity of black master-batch and determination of the carbon black by use of a pre
10、viouslyestablished determinate.5. Apparatus5.1 Drying Oven.5.2 Porcelain Crucibles, No. 00000, tared.5.3 Weighing Bottles, tared.5.4 Fused Alumina Combustion Boats.35.5 Combustion Tubes.45.6 Combustion Furnace.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless
11、 otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee on1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and is the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Dec. 1, 2004. Publ
12、ished December 2004. Originallyapproved in 2000. Last previous edition approved in 2000 as D 5805 - 00.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards
13、 Document Summary page onthe ASTM website.3Alundum No. 3 combustion boats have been found satisfactory for this purpose.4The sole source of supply of the combustion tube known to the committee atthis time is the McDaniel high-temperature combustion tube, 30 in. (762 mm) longby 1 in. (25.4 mm) in dia
14、meter available from Dunlap and Co., 623 Staring Lane,Baton Rouge, LA 70810. This tube will accommodate a maximum of twocombustion boats containing six samples each within the heated area of the furnace.If you are aware of alternative suppliers, please provide this information to ASTMInternational H
15、eadquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Analytical Reagents of the American Chemical Socie
16、ty, wheresuch specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7. Preparation of Sample7.1 Blend 200 g of dried sample obtained in accordancewith
17、 4.1 or 9.1 by passing it five times between the rolls of alaboratory mill. Maintain the roll temperature at 50 6 5C (1226 9F) and a distance between the rolls of 0.5 6 0.13 mm(0.020 6 0.005 in.). After blending, sheet the sample from themill with the distance between the rolls set at 0.25 6 0.05 mm
18、(0.010 6 0.002 in.). Dry approximately2goftheblended,thinly sheeted material for1hintheoven at 100 6 5C (2126 9F). Keep the dried sheet in a desiccator until ready toweigh the samples.8. Procedure8.1 Into the tared porcelain crucibles accurately weigh three0.3 to 0.5-g samples from the sheet of mate
19、rial being tested andthree 0.3 to 0.5-g samples from a similarly prepared sheet ofstandard SBR black determinate (see Note 2). Due to thehygroscopic nature of the samples and the carbon black, weighthe crucibles and contents in the tared weighing bottles.8.2 Place the six crucibles in a fused alumin
20、a combustionboat, or boats, alternating the samples of determinate and thetest samples. Insert the combustion boat, or boats, into thecombustion tube. Pass a stream of oxygen-free CO2throughthe tube at a flow rate of 150 to 240 cm3(atmosphericpressure)/min. After the tube has been swept free of oxyg
21、en(approximately 5 min is sufficient time), place it in thecombustion furnace maintained at a temperature of 550 625C, and distill off the rubber hydrocarbon. Continue to passCO2through the tube, while allowing the tube to remain in thefurnace for 30 min. At the end of this period, remove thecombust
22、ion tube from the furnace and allow it to cool,meanwhile continuing the flow of CO2through it. When it iscool, remove the boat, or boats, and place the crucibles in adesiccator until they cool to room temperature and are ready tobe weighed. Accurately weigh the crucibles and contents.8.3 After weigh
23、ing the crucibles containing the carbonblack residues, ignite the samples by either of the followingmethods:8.3.1 Place the crucibles and contents in a combustion boat,or boats, and insert them into a second combustion tube. Placethe tube in a combustion furnace maintained at 550 6 25Cand pass a str
24、eam of oxygen or air through the tube.8.3.2 Alternately, place the crucibles and contents in amuffle furnace maintained at 550 6 25C. After the carbon hasbeen completely burned, remove the boat, or boats, from themuffle furnace and place the crucibles in a desiccator. When thecrucibles have cooled t
25、o room temperature, weigh them.9. Calculation9.1 Calculate the percentage of ash, R, in the dry sample asfollows:R 5 F 2 E!/D 2 E!# 3 100 (1)where:F = mass of crucible plus ash after ignition of the carbonblack, g,E = mass of crucible, g, andD = mass of original dry sample plus crucible, g.9.2 Calcu
26、late the individual values, c1, c2, and c3, for carbonblack content of the material being tested on the dry, ash-freebasis as follows:c 5 100Q 2 F!/D 2 E!1 2 0.01R! (2)where:Q = mass of crucible and residue after distillation ofhydrocarbon, g, and F, D, E, and R are defined in 9.1.9.3 Calculate the
27、individual values, c18, c28, and c38, forcarbon black content of the standard SBR carbon blackdeterminate (see Note 2) on the dry, ash-free basis in accor-dance with 3.1.2, using the appropriate values obtained on thesamples of the determinate.9.4 Calculate the corrected percentage of carbon black i
28、nthe material being tested as follows:Carbon black, % 5 C 1 A 2 C8 (3)where:C = average of the three values of percentage carbon black(c1, c2, and c3) on the dry, ash-free basis, obtained onthe material being tested,A = percentage of carbon black assigned as the standardvalue for the standard SBR ca
29、rbon black determinate(see Note 2), andC8 = average of the three values of percentage carbonblack, c18, c28, and c38, on the dry, ash-free basis,obtained on the standard carbon black determinate.10. Precision and Bias10.1 Precision and bias have not been determined.TEST METHOD BVacuum Pyrolysis Test
30、 Method11. Summary of Test Method11.1 The prepared dried sample is tested in triplicate. Thesamples accurately are weighed into tared crucibles and placedin a combustion tube and maintained under very low pressureat 600C until the rubber is distilled. The samples are cooledand returned to atmospheri
31、c pressure. The crucibles andcontents are then further cooled in a desiccator and weighed.The percentage of carbon black is calculated on an ash-freebasis.12. Significance and Use12.1 Carbon black in unvulcanized carbon black or oil-carbon black SBR masterbatch may be determined by this testmethod w
32、ithout the use of a determinate sample.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset,
33、 U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 5805 00 (2004)e1213. Apparatus13.1 Porcelain Crucible, No. 00000.13.2 Combustion Boats, sized to accommodate crucibles.13.3 Combustion Tube, high-silica (see Fig. 1).413.4 Comb
34、ustion Furnace, capable of controlling tempera-ture at 600 6 25C.13.5 Vacuum Pump.13.6 Vacuum Seal Lubricant for ground-glass joint.13.7 Muffle Furnace, capable of controlling at 550 6 25C.13.8 Drying Oven, capable of controlling at 105 6 5C.13.9 Insertion Rod.13.10 Trap, to condense vapors coming f
35、rom combustiontube (see Fig. 1).14. Preparation of Sample14.1 Blend 200 g of the dried sample obtained in accor-dance with 4.1 or 9.1 by passing it five times between the rollsof a laboratory mill. Maintain the roll temperature at 50 6 5C(122 6 9F) and a distance between the rolls of 0.5 6 0.13 mm(0
36、.20 6 0.005 in.). After blending, sheet the sample from themill with the distance between the rolls set at 0.25 6 0.05 mm(0.010 6 0.002 in.). Dry approximately2goftheblended,thinly sheeted material for1hintheoven at 105 6 5C. Keepthe dried sheet in a desiccator until ready to weigh the samples.15. P
37、rocedure15.1 Place into a tared crucible 0.3 to 0.5 g (to the nearest0.1 mg) from the sheet of material being tested. Using theinsertion rod, insert the boat containing the crucibles into thetube to maximum depth. Insert the ground-glass stopper coatedproperly with vacuum seal lubricant, turn on the
38、 vacuum pump,and evacuate the tube to less than 1.3 kPa.15.2 Introduce the combustion tube into the combustionfurnace maintained at 600 6 25C, using care not to rotate thetube or otherwise cause sample disturbance. Allow the tube toremain in the furnace for 10 min, maintaining maximumpressure of 1.3
39、 kPa (10 mm Hg) during combustion. Removethe tube from the furnace, allow the tube and contents to coolfor 7 min, and slowly allow pressure to increase to preventblowing residue out of crucible.15.3 Remove the boat and place it in a desiccator to cool toroom temperature. Weigh each crucible and resi
40、due to thenearest 0.1 mg. Determine the ash content on a portion ofsample.16. Calculation16.1 Calculate the percentage of carbon black as follows:Carbon black, % 5 A 2 B! 2 0.01 CD!/C 2 0.01 CD!# 3 100(4)where:A = mass of crucible and residue after distilling, g,B = mass of crucible, g,C = mass of o
41、riginal sample, g, andD = percentage of ash.17. Precision and Bias17.1 Precision and bias have not been determined.TEST METHOD CThermogravimetric Analyzer18. Summary of Test Method18.1 The prepared, dried sample is placed in a calibratedthermogravimetric analyzer (TGA) where it is weighed usingthe i
42、ntegral balance (See Test Method D 6370). The sample isheated to 575C in an inert atmosphere to pyrolyze the rubberand other softeners. The atmosphere is then switched to air,combusting the carbon black. The difference in mass beforeand after the switch of gases is the mass of the carbon blackcontai
43、ned in the sample.FIG. 1 Vacuum Combustion Tube and Trap ArrangementD 5805 00 (2004)e1319. Significance and Use19.1 The carbon black content of any vulcanized or unvul-canized compound may be determined by this method withoutuse of a determinate sample.19.2 Expertise in thermogravimetric analysis (T
44、GA) is nec-essary to the successful application of this test method.20. Apparatus20.1 Thermogravimetric Analyzer, maintained and operatedin accordance with manufacturers instructions.21. Preparation of Sample21.1 Blend 200 g of dried sample obtained in accordancewith 4.1 or 9.1 by passing it five ti
45、mes between the rolls of alaboratory mill. Maintain the roll temperature at 50 6 5C (1226 9F) and a distance between the rolls of 0.5 6 0.13 mm(0.020 6 0.005 in.). After blending, sheet the sample from themill with the distance between the rolls set at 0.25 6 0.05 mm(0.010 6 0.002 in.). Dry approxim
46、ately2goftheblended,thinly sheeted material for1hintheoven at 100 6 5C (2126 9F). Keep the dried sheet in a desiccator until ready toweigh the samples.22. Procedure22.1 Set zero on the analyzer following manufacturersinstructions.22.2 Place in the instrument pan 10 6 3 mg of the preparedsample. Weig
47、h accurately using integral instrument balance.22.3 Under inert atmosphere heat the sample to 575 6 50Cand hold until constant mass.22.4 Switch atmosphere to air and hold until constant mass.23. Calculation23.1 Calculate the percentage of carbon black in thesamples as follows:C 5 A 2 B!100!/I (5)whe
48、re:C = % carbon black in the sample,A = constant mass of sample at 575C under inert gas,B = constant mass of sample at 575C under air, andI = initial mass of sample.23.2 Alternatively, the instrument may perform this calcu-lation automatically.24. Precision and Bias24.1 Precision and bias have not b
49、een determined.25. Keywords25.1 carbon black; masterbatch; thermogravimetric analysis(TGA)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 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
