ASTM D3848-2003(2018) Standard Test Methods for Rubber&x2014 Evaluation of NBR (Acrylonitrile-Butadiene Copolymers) Mixed With Carbon Black.pdf

1、Designation: D3848 03 (Reapproved 2018)Standard Test Methods forRubberEvaluation of NBR (Acrylonitrile-ButadieneCopolymers) Mixed With Carbon Black1This standard is issued under the fixed designation D3848; the number immediately following the designation indicates the year oforiginal adoption or, i

2、n the case of revision, the 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.1. Scope1.1 These test methods specify the standard materials, testformula, mixing procedures,

3、 and test methods for the evalua-tion of acrylonitrile-butadiene rubber (NBR) mixed with car-bon black.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,

4、 if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with inter

5、nationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D412

6、Test Methods for Vulcanized Rubber and Thermoplas-tic ElastomersTensionD1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization Characteristics(Mooney Viscometer)D2084 Test Method for Rubber PropertyVulcanizationUsing Oscillating Disk Cure MeterD3182 Practice for RubberMateria

7、ls, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulcanized SheetsD3896 Practice for Rubber From Synthetic SourcesSamplingD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD5289 Test Method for Rub

8、ber PropertyVulcanizationUsing Rotorless Cure MetersD6204 Test Method for RubberMeasurement of Unvulca-nized Rheological Properties Using Rotorless Shear Rhe-ometers3. Significance and Use3.1 These test methods are mainly intended for refereepurposes but may be used for quality control of rubberprod

9、uction. They may also be used in research and develop-ment work and for comparison of different samples in astandard test formula.3.2 These test methods may also be used to obtain values forcustomer acceptance of rubber.4. Standard Test Formula4.1 Standard Formula:IRM/SRMSRM Quantity, PartsMaterial

10、No. By MassMasterbatch . 100.00 + XAZinc oxideB3.00Sulfur, coatedC. 1.50Stearic acidB1.00TBBSDB0.70 + XTotal mass 106.20 + XBatch factorsMillEMiniature internal mixerFAX = parts carbon black per 100 parts base polymer.BUse current IRM/SRM.CThe use of 2 % MgCO3coated sulfur is recommended. Standard 2

11、 % MgCO3coated sulfur Lot No. M266573-P is available from C. P. Hall Co., 4460 HudsonDrive, Stow, OH 44224.DN-tert-butyl-2-benzothiazolesulfenamide.EFor mill mixing, a batch factor should be selected to the nearest 0.5 to give aslarge as total mass as possible that will not exceed 525.0 g. Calculate

12、 all parts tothe nearest 0.01 part. Weigh the masterbatch to the nearest 1 g, the sulfur and theaccelerator to the nearest 0.02 g, and all the other compounding materials to thenearest 0.1 g.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and a

13、re the direct responsibility of SubcommitteeD11.23 on Synthetic Rubbers.Current edition approved June 1, 2018. Published August 2018. Originallyapproved in 1980. Last previous edition approved in 2013 as D3848 03 (2013).DOI: 10.1520/D3848-03R18.2For referenced ASTM standards, visit the ASTM website,

14、 www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThi

15、s international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (T

16、BT) Committee.1FFor MIM mix, select a batch factor to give a batch that will fill the mixing chambervolume to 75 % capacity. Calculate all parts to the nearest 0.1 g, the compoundingmaterial blend to the nearest 0.01 g, and the individual compounding materials, ifused, to the nearest 0.001 g.For the

17、 MIM procedure, it is recommended that a blend of compoundingmaterials be prepared to improve accuracy in the weighing of the materials. Thecompound material blend is prepared by blending a proportional mass of eachmaterial in a biconical or a vee blender. A mortar and pestle may be used forblending

18、 small quantities.5. Sample Preparation5.1 Obtain and prepare the test samples in accordance withPractice D3896.6. Mixing Procedures6.1 Three mixing procedures are provided as follows:6.1.1 Method AMill Mix (6.2) and6.1.2 Method BMiniature Internal Mixer Mix (6.3).6.1.3 Method CInternal MixerNOTE 1I

19、t is not implied that comparable results will be obtained bythese test methods.6.2 Method AMill Mix Procedure:6.2.1 For general mixing procedures, refer to PracticeD3182.6.2.2 Mixing CycleInitial Mix:Accu-Dura- mula-tion, tive,min min6.2.2.1With the mill roll temperature set at 50 5C(122 9F) and the

20、 mill opening set at 1.40mm (0.055 in.), band the masterbatch on theslow roll without cutting.226.2.2.2Add sulfur slowly and evenly across the millat a uniform rate.246.2.2.3Add stearic acid. Make one34 cut from eachside after the stearic acid has beenincorporated.266.2.2.4Add the zinc oxide and the

21、 accelerator. 3 96.2.2.5Make three34 cuts from each side and cutthe batch from the mill.2116.2.2.6Set the rolls at 0.8 mm (0.032 in.). Pass therolled batch endwise through the mill six times.2136.2.2.7Open the mill to give a minimum batchthickness of 6 mm (0.25 in.) and pass the stockthrough the mil

22、l four times, folding it back onitself each time.1146.2.2.8Check the batch mass and record. If it differsfrom the theoretical value by more than 0.5 %,discard the batch.6.2.2.9From this batch cut a sample for testing ofcompound viscosity in accordance with TestMethods D1646 or rheological properties

23、 in ac-cordance with Test Method D6204, vulcanizingcharacteristics in accordance with Test MethodD2084, or Test Method D5289, or both, if theseare desired. Condition the sample for 1 to 24 hat 23 2C (73.4 3.6F) before testing.6.2.2.10If tensile stress is required, sheet off thecompound from the mill

24、 at a setting to give afinished gage of approximately 2.2 mm (0.085in.) by passing the folded stock between therolls set at 50 5C (122 9F) four timesalways in the same direction to obtain theeffect of milling. Cool on a flat, dry metalsurface.6.2.2.11For routine laboratory testing, condition theshee

25、ted compound for 1 to 24 h at 23 2C(73.4 3.6F) and a relative humidity notgreater than 55 %. For maximum precision,condition for 1 to 24 h in a closed container toprevent absorption of moisture from the air orin an area controlled at 35 5 % relativehumidity.6.3 Method BMiniature Internal Mixer (MIM)

26、 Procedure:6.3.1For general mixing procedures, refer toPractice D3182. Mix with the MIM mixingchamber maintained at 60 3C (140 5F)and with an unloaded rotor speed of 6.3 to 6.6rad/s (60 to 63 rpm).6.3.2Prepare the masterbatch by passing itthrough a mill one time with the temperatureset at 50 5C (122

27、 9F) and an opening of0.5 mm (0.02 in.). Cut the sheet into strips thatare approximately 25 mm (1 in.) wide, ifdesired.6.3.3 Mixing Cycle:6.3.3.1Feed the rubber strips into the mixingchamber and, when all are in, start the timer.Break down the rubber.0.5 0.56.3.3.2Add all the zinc oxide, sulfur, ste

28、aric acid,and TBBS which have previously been blendedtogether, taking care to avoid any loss. Stopthe mixer briefly and sweep loose pigments intothe chamber with a brush.0.5 1.06.3.3.3Allow the compound to mix.6.3.3.4Turn off the motor, raise the ram, remove themixing chamber, and discharge the batc

29、h.Record the maximum batch temperature, ifdesired.8.0 9.06.3.3.5Pass the batch between the rolls of a millmaintained at 50 5C (122 9F) and 0.5mm (0.020 in.) opening once, then twice at 3.0mm (0.122 in.) opening.6.3.3.6Check the batch mass and record. If it differsfrom the theoretical value by more t

30、han 0.5 %,discard the batch.D3848 03 (2018)26.3.3.7Cut a sample for testing of compoundviscosity in accordance with Test MethodsD1646 or rheological properties in accordancewith Test Method D6204, or vulcanizing charac-teristics in accordance with Test MethodD2084, or Test Method D5289, if these are

31、 de-sired. Condition the sample 1 to 24 h at 23 2C (73.4 3.6F) before testing.6.3.3.8If stress strain testing is required, pass therolled stock end-wise through the mill six timeswith the mill temperature at 50 5C (1229F) and a roll separation of 0.8 mm (0.032in.).6.3.3.9If tensile stress is require

32、d, sheet off thecompound from the mill at a setting to give afinished gage of approximately 2.2 mm (0.085in.) by passing the folded stock between themill rolls set at 50 5C (122 9F) four timesalways in the same direction to obtain theeffect of milling. Cool on a flat, dry metalsurface.6.3.3.10For ro

33、utine laboratory testing, condition thesheeted compound for 1 to 24 h at 23 2C(73.4 3.6F) and a relative humidity notgreater than 55 %. For maximum precision,condition for 1 to 24 h in a closed container toprevent absorption of moisture from the air orin an area controlled at 35 5 % relativehumidity

34、.6.4 Internal Mixer Procedure:6.4.1 For general mixing procedure refer to Practice D3182.6.4.2 Mixing Cycle-Initial Mix:Accu-Dura- mula-tion, tive,min min6.4.2.1Adjust the internal mixer temperature toachieve the discharge conditions outlined in6.2.2. Close the discharge gate, start the rotorat 8.1

35、rad/s (77 rpm) and raise the ram.006.4.2.2Charge one half the rubber, all of the zincoxide, carbon black, stearic acid, and then theother one half of the rubber. Lower the ram.53.0.53.56.4.2.3Allow the batch to mix. .5 4.06.4.2.4Raise the ram and clean the mixer throat andthe top of the ram. Lower t

36、he ram.2.0 6.06.4.2.5Allow the batch to mix until a temperature of170C (338F) or a total mixing time of 6 min isreached, whichever occurs first. Discharge thebatch.2.0 6.06.4.2.6Determine and record the batch mass; if themass differs by more than 0.5 % of thetheoretical mass, discard the batch.6.4.2

37、.7Pass the batch immediately through thestandard laboratory mill three times, set at 6.0mm (0.25 in.) and 40 5C (104 9F).6.4.2.8Allow the batch to rest for 1 to 24 h.6.4.3 Final Mix:6.4.3.1 Adjust the internal mixer temperature to 40 6 5C(104 6 9F), turn off steam and turn on full cooling water toth

38、e rotors, at 8.1 rad/s (77 rpm), and raise the ram.Accu-Dura- mula-tion, tive,min min6.4.3.2Charge12 the batch, with all the sulfur andaccelerator rolled into this portion of the batchbefore feeding to the mixer. Add the remainingportion of the batch. Lower the ram.556.4.3.3Allow the batch to mix un

39、til a temperature of110 5C (230 9F) or a total mixing time of3 min is reached, whichever occurs first.Discharge the batch.2.5 3.06.4.3.4Determine the record the batch mass; if themass differs by more than 0.5 % of thetheoretical mass, discard it.6.4.3.5With the rolls of a standard laboratory millmai

40、ntained at 40 5C (104 9F) and set at0.8 mm (0.0032 in.) opening, pass the rolledbatch endwise through the rolls six times.2.0 5.06.4.3.6Open the rolls to give a minimum thicknessof 6 mm (0.25 in.) and pass the compoundthrough four times, folding it back itself eachtime.1.0 6.06.4.3.7Cut enough sampl

41、es for testing of compoundviscosity in accordance with Test MethodsD1646, or rheological properties in accordancewith Test Method D6204, or vulcanizing charac-teristics in accordance with Test MethodD2084, or Test Method D5289, if these are de-sired. Condition the sample for 1 to 24 h at 23 3C (73.4

42、 5.4F) before testing.6.4.3.8If tensile stress is required, sheet off thecompound from the mill at a setting to give afinished of approximately 2.2 mm (0.085 in.) bypassing the folded stock between the rolls setat 50 5C (122 9F) four times always in thesame direction to obtain the effects of milldir

43、ection. Cool on a flat, dry metal surface.6.4.3.9Four routine laboratory testing, condition thesheeted compound for 1 to 24 h at 23 3C(73.4 5.4F) and a relative humidity notgreater than 55 %. For maximum precision,condition for 1 to 24 h in a closed container toprevent absorption of moisture from th

44、e air orin an area controlled at 35 5 % relativehumidity.D3848 03 (2018)37. Test for Cure Characteristics Using the Cure Meter7.1 Measure vulcanization characteristics with an Oscillat-ing Disk cure meter in accordance with Test Method D2084 ora Rotorless Cure Meter in accordance with Test MethodD52

45、89.7.2 The recommended standard Oscillating Disk test condi-tions are: 1.7 Hz oscillation frequency; 61 amplitude ofoscillation, 160C die temperature, 30-min test time, and nopreheating. The recommended test conditions for the RotorlessCure Meter are: 1.7 Hz oscillation frequency, 60.5 of arc fortor

46、sional shear cure meters and 60.05mm for linear shear curemeters, 160 C die temperature, 30 min test time, and nopreheating. Tolerances for the listed conditions are included inthe specified test methods.7.3 The recommended standard test parameters are: ML,MH, tsl, t50 and t90.8. Preparation and Tes

47、ting of Vulcanizates8.1 An alternative to measuring vulcanization parameters isthe measurement of stress-strain properties of vulcanizates inaccordance with Test Methods D412. Prepare test sheets andvulcanize them in accordance with Practice D3182.8.1.1 The recommended standard vulcanization times f

48、orthe mill mixed compound are 20, 40, and 60 min at 150C(302F). The recommended standard vulcanization time for theminiature internal mixer compounds is 40 min at 150C.NOTE 2Vulcanization times of 25, 50, and 75 min at 145C (293F)for the mill-mixed compounds and 50 min at 145C for the MIM-mixedcompo

49、unds may also be used, but will not necessarily give the sameresults as the recommended standard vulcanization conditions.8.1.2 Condition all vulcanizates for 16 to 96 h at a tempera-ture of 23 6 2C (73.4 6 3.6F) prior to making stress-straintests.NOTE 3Quality control of rubber production may require testingwithin 1 to6htoprovide close surveillance of plant operations; however,slightly different results may be obtained.8.1.3 Prepare test spec