1、Designation: D 4122 06Standard Practice forCarbon BlackEvaluation of an Industry Reference Black1This standard is issued under the fixed designation D 4122; 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 practice covers guidelines for the production andtesting for uniformity of a lot of carbon black to be used as anIndustry Refe
3、rence Black (IRB).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 theresponsibility of the user of this standar
4、d 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 412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD 1506 Test Methods for Carbon BlackAsh ContentD 150
5、8 Test Method for Carbon Black, Pelleted Fines andAttritionD 1509 Test Methods for Carbon BlackHeating LossD 1510 Test Method for Carbon BlackIodine AdsorptionNumberD 1513 Test Method for Carbon Black, PelletedPourDensityD 1514 Test Method for Carbon BlackSieve ResidueD 1618 Test Method for Carbon B
6、lack ExtractablesTransmittance of Toluene ExtractD 1765 Classification System for Carbon Blacks Used inRubber ProductsD 2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulca
7、nized SheetsD 3191 Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber)Recipe and Evaluation ProceduresD 3192 Test Methods for Carbon Black Evaluation in NR(Natural Rubber)D 3265 Test Method for Carbon BlackTint StrengthD 3493 Test Method for Carbon BlackOil AbsorptionNumber of Compressed
8、 Sample (COAN)D 5230 Test Method for Carbon BlackAutomated Indi-vidual Pellet HardnessD 6556 Test Method for Carbon BlackTotal and ExternalSurface Area by Nitrogen Adsorption3. Significance and Use3.1 These guidelines are intended to ensure that IRBs areevaluated by a standard procedure.3.2 These gu
9、idelines are to be used to establish the averagephysicochemical and physical rubber properties of a lot ofcarbon black to be used as an IRB.4. Production, Quality Control, and Quality Assurance4.1 It is assumed that the manufacturer of the IRB will usestate-of-the-art techniques to ensure maximum un
10、iformitythroughout the entire production run. The production should bemade in one continuous production lot run. The testing calledfor in this practice is not intended to be a substitute forin-process quality control. This interlaboratory study is onlyadequate to verify the quality of a homogeneous
11、lot.4.2 The size of the lot is determined by historical records onthe rate of use. The lot should have an expected life of 8 to 10years at the most recent rate of use.4.3 The black should be bagged in 50-lb polyethylene bagsto reduce moisture incursion. Each pallet of bagged blackshould be wrapped i
12、n plastic to reduce environmental expo-sure. The bagged black will be segregated into at least twelveequal sized sublots for uniformity testing.5. Sampling5.1 After a suitable time to allow the black to stabilize, a bagwill be selected from the approximate middle of each of thesublots; the bags sele
13、cted will be numbered from one through1This practice is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.61 on Carbon BlackSampling and Statistical Analysis.Current edition approved Oct. 1, 2006. Published October 2006. Originallyapprov
14、ed in 1982. Last previous edition approved in 2005 as D 4122 05ae1.2For 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 Document Summary page onthe ASTM we
15、bsite.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.n, where n is the total number of sublots, in order to representthe corresponding production lot.5.2 n 4-dm3(1-gal) samples, numbered from one through n,and taken from the corresp
16、onding bags, will be sent to eachparticipant in the interlaboratory study to evaluate the newIRB.5.3 Additionally, a 4-dm3(1-gal) sample of the previousIRB taken from a common blended source will also be sent toeach participant.6. Procedure6.1 Test, in order, one of the n samples on each of the onet
17、o n days. These days shall be as near to consecutive aspossible.6.2 Each day a sample is tested, subject it to all of the testmethods described in 6.3-6.5.6.3 Physicochemical Tests:6.3.1 Perform the following physicochemical tests on boththe new and previous IRB:6.3.1.1 Iodine Adsorption Number (Tes
18、t Method D 1510)Report the result obtained from an individual determination ingrams of iodine per kilogram to the nearest 0.1 unit.6.3.1.2 Total and External NSA (Test Method D 6556)Report total and external NSA from a single determination in103m2/kg (m2/g) to the nearest 0.1 unit.6.3.1.3 Oil Absorp
19、tion Number (Test Method D 2414)Report the result obtained from an individual determination in105m3kg (cm3/100 g) to the nearest 0.1 unit.6.3.1.4 Oil Absorption Number of Compressed Sam-ple (Test Method D 3493)Report the result obtained from anindividual determination in 105m3kg (cm3/100 g) to thene
20、arest 0.1 unit.6.3.1.5 Tint Strength (Test Method D 3265)Report theresult obtained from an individual determination in percent ofITRB to the nearest 0.1 unit.6.3.1.6 Pour Density (Test Method D 1513)Report theresult obtained from an individual determination in kg/m3(lb/ft3) to the nearest whole unit
21、.6.3.2 Record data on Table 1.6.4 Rubber Physical Tests:6.4.1 Perform the following physical tests in rubber on boththe new and previous IRB. Test samples mixed in accordancewith Test Methods D 3191 and cure for 50 min at 145C aswell as samples mixed in accordance with Test MethodsD 3192, Test Metho
22、d A, and cure for 30 min at 145C.6.4.1.1 In accordance with Test Methods D 412, TestMethod A, test five dumbbells from each cured sheet anddetermine the median values of tensile stress at 300 % elon-gation, tensile strength, and ultimate elongation.6.4.1.2 Record data in absolute numbers (not as dif
23、ferencesfrom IRB) on Table 1, reporting tensile stress and tensilestrength to the nearest 0.1 MPa and ultimate elongation to thenearest 5 %.6.5 Informational Physicochemical Tests:6.5.1 Perform the following physicochemical tests on thenew IRB:TABLE 1 Industry Reference Black Test DataLaboratory Num
24、ber _Day ofMix-ing andDateSampleNo.TensileStrength,MPa D 3191TensileStress at300 %,MPaD 3191Elonga-tion, %D 3191TensileStrength,MPaD 3192A300 %Modulus,MPaD 3192AElonga-tion, %D 3192AIodineNo., g/kgD 1510STSA103m2/kgD 6556NSAMulti-pointAdsorption103m2/kgD 6556Oil Ab-sorption,No., 105mg3/kg(cm3/100g)D
25、 2414Com-pressedOil No.,105mg3/kg(cm3/100g)D 3493TintStrength,D 3265PourDensity,kg/m3(lb/ft3)D 1513Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308D
26、ay No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308D41220626.5.1.1 Ash C
27、ontent (Test Methods D 1506)Report re-sults obtained from a single determination to the nearest0.01 %.6.5.1.2 Fines and Attrition (Test Method D 1508)Reportresults obtained from a single determination to the nearest0.1 %.6.5.1.3 Heating Loss (Test Methods D 1509)Report re-sults obtained from a singl
28、e determination to the nearest 0.1 %.6.5.1.4 Sieve Residue, 325 Mesh (Test Method D 1514)Report results obtained from a single determination to thenearest mg/kg (ppm).6.5.1.5 Transmittance of Toluene Extract (Test MethodD 1618)Report results obtained from a single determinationto the nearest 0.1 % t
29、ransmittance.6.5.1.6 Pellet Hardness (Test Method D 5230)Report re-sults obtained from a single determination to the nearest wholenumber for the maximum and average.7. Statistical Analysis7.1 For each test in Table 1, enter the results from eachlaboratory for each sample into the form shown in Table
30、 2.Then calculate the statistics defined in Table 2.NOTE 1Rubber physical test data are to be entered as differences fromthe previous IRB. For example:Difference 5 X12 X2(1)where:X1= measured value for new IRB, andX2= measured value for previous IRB.7.2 If any row average test result falls outside t
31、he intervaldefined by the upper and lower control limits shown in Table 2,this will indicate that the sublot of IRB represented by that rowaverage may be rejected by Committee D24 as being anonhomogeneous portion of the production lot.7.3 If any laboratory average test result (column average)falls o
32、utside the upper and lower control limits shown in Table2, then that laboratorys data for that test should be deleted andTable 2 should be recalculated excluding that laboratory. Suchdata indicates that the laboratory has a significant reproduc-ibility problem, which needs corrective action.7.4 Afte
33、r deleting data, the remaining data for each testmethod can be averaged to provide typical values for tabulationin Classification D 1765 and average differences between thenew IRB and the previous one.7.5 For each test in Table 3, enter the results from eachlaboratory for each sample in the form sho
34、wn in Table 2. Thencalculate the statistics defined in Table 2. The results are forinformation only and not to determine the uniformity of the lot.8. Acceptance8.1 All sublots tested as homogeneous by this practice willbe considered acceptable by Committee D24 for use as the newIRB. The average valu
35、es will be published in ClassificationD 1765.9. Shelf Life9.1 The shelf life of the Industry Reference Black (IRB)carbon blacks is indefinite when properly stored in a mannerthat protects it from exposure to sources of moisture, such asprecipitation, other sources of liquid water, or high humidityen
36、vironments. Iodine number is the only property known tochange over an extended period (years). This is due to a slowincrease in the oxygen content and is primarily observed withtread blacks and other high surface area carbon blacks. Stepsare being taken within ASTM Committee D24 to developstandards
37、that are more stable over a long period.10. Keywords10.1 blending; industry reference blacks (IRBs); lot size;physical properties; physicochemical properties; shelf life;statistical analysis form; table for IRB test data; uniformityguidelines for production and testingTABLE 2 Statistical Analysis Fo
38、rmNOTE 1Experience so far has shown that neither a laboratorys test values nor a samples test values are random values about the grand average,but tend to reflect a persistent bias typified by the average value for the laboratory or the sample. Consequently, it is not appropriate to divide thereprod
39、ucibility by the square root of L or N as might otherwise be the case when comparing averages of L or N values to the grand average of L 3 Nvalues.Test Method: ASTM D _ _ _SampleNo.Laboratory No. 1 2 . i . LXR12.j.NXCX55Row average XR= (iX/LGrand average test value X5= (jXR/NUpper and lower control
40、limits for row averages = X56 reproducibility of the test method.Column average XC= (jX/NUpper and lower control limits for column averages = X56 reproducibility of the test method.D4122063ANNEX(Mandatory Information)A1. LISTING OF THE PROPERTIES OF INDUSTRY REFERENCE BLACKSA1.1 The listing of prope
41、rties for Industry ReferenceBlacks (IRBs) is given in Table A1.1. The absolute values forI2number, OAN, COAN, and tint strength are listed. Values fortensile stress at 300 % elongation or “modulus” and tensilestrength are given in relation to the previous IRB as a“difference.” Since the purpose of a
42、n IRB is the elimination ofthe major part of laboratory-to-laboratory variation, it is usedas a reference material within each laboratory to correct actualTABLE 3 Industry Reference Black Informational Test DataLaboratory Number_Day ofMixingand DateSample No.AshContentD 1506FinesContentD 1508Heating
43、LossD 1509SieveResidue,325 MeshD 1514Transmittanceof TolueneExtractD 1618PelletAttritionD 1508AveragePelletHardnessD 5230MaximumPelletHardnessD 5230Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._ _Date _Day No._
44、 _Date _Day No._ _Date _Day No._ _Date _TABLE A1.1 Industry Reference BlacksIRB No. Producer LotSize, lbDate of ASTMAccept-anceIodineAbsorp-tion No.,D 1510,g/kgOAN,D 2414,10-5m3/kgCOAN,D 3493,10-5m3/kgTintStrength,D 3265Difference from previous IRB, MPa (psi)D 3192 D 3191Modulus Tensile Modulus Tens
45、ile1 Phillips 150 000 12/59 81 97A. . 15-min30-min.35-min50-min.2 Continental 200 000 6/65 82 92 83 . 15-min30-min-0.3 (-50)-0.2 (-25)+1.9 (+275)+1.2 (+175)35-min50-min.3 Ashland 300 000 6/69 84.8 99.9 87.8 100.0 15-min30-min+0.7 (+100)+0.5 (+75)-0.5 (-75)-0.5 (-75)35-min50-min.4 Cabot 600 000 11/73
46、 82.1 97.1 86.5 107.1 15-min30-min+0.2 (+30)+0.5 (+70)+0.9 (+130)+0.8 (+110)35-min50-min.5 Columbian 500 000 12/79 81.9 102.1 89.6 101.5 15-min30-min+1.2 (+170)+0.9 (+130)0.0 (0.0)-0.6 (-90)35-min50-min+1.4 (+210)+1.2 (+180)+0.1 (+20)+0.2 (+30)6 Huber 900 000 6/85 80.0 100.0 87.2 99.2 15-min30-min-1
47、.7 (-245)-2.2 (-320)-0.9 (-130)-0.9 (-130)35-min50-min-2.6 (-375)-2.7 (-390)-1.5 (-220)-1.2 (-175)7 Sid Richardson 495 000 6/97 83.0 101.6 89.0 106.8 30-min +3.2 (+460) +1.5 (+220) 50-min +3.8 (+550 +1.6 (+230)AHand oil absorption.Editorially corrected.D4122064measured property values in that labora
48、tory.A1.1.1 The rubber properties of carbon black are typicallyreported as the difference between the values obtained for thetest and those obtained for IRB No. 7.NOTE A1.1IRB No. 73is an N330 type carbon black prepared at onelocation, then evaluated by ASTM Committee D24 to ensure uniformity.A larg
49、e volume (225 000 kg (495 000 lb) of this carbon black wasprepared since it is used daily as a standard reference material by carbonblack producers. The carbon black has an iodine number of 83.0 and OANof 101.6.4A1.2 The user of this table is cautioned against attemptingto add the differences listed in the modulus and tensile strengthcolumns to determine the relationship of t
