1、Designation: D4122 10Standard Practice forCarbon BlackEvaluation of an Industry Reference Black1This standard is issued under the fixed designation D4122; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 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 practice covers guidelines for the production andtesting for uniformity of a lot of carbon black to be used as anIndustry Referen
3、ce 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 standard t
4、o establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D412 Test Methods for Vulcanized Rubber and Thermo-plastic ElastomersTensionD1506 Test Methods for Carbon BlackAsh ContentD1508 Test
5、 Method for Carbon Black, Pelleted Fines andAttritionD1509 Test Methods for Carbon BlackHeating LossD1510 Test Method for Carbon BlackIodine AdsorptionNumberD1513 Test Method for Carbon Black, PelletedPour Den-sityD1514 Test Method for Carbon BlackSieve ResidueD1618 Test Method for Carbon Black Extr
6、actablesTransmittance of Toluene ExtractD1765 Classification System for Carbon Blacks Used inRubber ProductsD2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized Sheets
7、D3191 Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber)Recipe and Evaluation ProceduresD3192 Test Methods for Carbon Black Evaluation in NR(Natural Rubber)D3265 Test Method for Carbon BlackTint StrengthD3493 Test Method for Carbon BlackOil AbsorptionNumber of Compressed Sample (COAN)D5
8、230 Test Method for Carbon BlackAutomated Indi-vidual Pellet HardnessD6556 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 guidelines are to be
9、 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 uniformitythroughout
10、 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 lot.4.2 The size o
11、f 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 in plastic to reduc
12、e 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 selected will be numbe
13、red 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 Feb. 1, 2010. Published March 2010. Originallyapproved in 1982. Last pre
14、vious edition approved in 2006 as D4122 06. DOI:10.1520/D4122-10.2For 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 webs
15、ite.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 correspon
16、ding 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 oneto
17、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 and 6.4.6.3 Rubber Physical Tests:6.3.1 Perform the following physical tests in rubber on boththe new and previous IRB. Test samples mixed in accordanc
18、ewith Test Methods D3191 and cure for 50 min at 145C as wellas samples mixed in accordance with Test Methods D3192,Test Method A, and cure for 30 min at 145C.6.3.1.1 In accordance with Test Methods D412, Test MethodA, test five dumbbells from each cured sheet and determine themedian values of tensil
19、e stress at 300 % elongation, tensilestrength, and ultimate elongation.6.3.1.2 Record data in absolute numbers (not as differencesfrom IRB) on Table 1, reporting tensile stress and tensilestrength to the nearest 0.1 MPa and ultimate elongation to thenearest 5 %.6.4 Informational Physicochemical Test
20、s:6.4.1 Perform the following physicochemical tests on thenew IRB:6.4.1.1 Iodine Adsorption Number (Test Method D1510)Report the result obtained from an individual determination ingrams of iodine per kilogram to the nearest 0.1 unit.6.4.1.2 Oil Absorption Number (Test Method D2414)Report the result
21、obtained from an individual determination in105m3kg (cm3/100 g) to the nearest 0.1 unit.6.4.2 Record data on Table 2 (or in a form that captures thesame information as in Table 2).7. Statistical Analysis7.1 For each test in Table 1, enter the results from eachlaboratory for each sample into the form
22、 shown in Table 3.Then calculate the statistics defined in Table 3.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
23、falls outside the intervaldefined by the upper and lower control limits shown in Table 3,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
24、average)falls outside the upper and lower control limits shown in Table3, then that laboratorys data for that test should be deleted andTable 3 should be recalculated excluding that laboratory. Suchdata indicates that the laboratory has a significant reproduc-ibility problem, which needs corrective
25、action.TABLE 1 Industry Reference Black Test DataLaboratory Number _Day ofMix-ing andDateSampleNo.Tensile Strength,MPa D3191TensileStress at300 %,MPaD3191Elonga-tion, %D3191Tensile Strength,MPaD3192300 %Modulus,MPaD3192Elonga-tion, %D3192Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _
26、 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 308Day No._ 508 308Date _ Prev. IRB 508 308Da
27、y No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308Day No._ 508 308Date _ Prev. IRB 508 308D4122 1027.4 After deleting data, the remaining data for each testmethod can be averaged to provide typical values for tabulationin Classification D1765 and average differences betwe
28、en thenew IRB and the previous one.7.5 For each test in Table 2, enter the results from eachlaboratory for each sample in the form shown in Table 3. Thencalculate the statistics defined in Table 3. The results are forinformation only and not to determine the uniformity of the lot.TABLE 2 Industry Re
29、ference Black Informational Test DataLaboratory Number_Day ofMixingand DateSample No.Iodine No.,g/kgD1510Oil AbsorptionNo.,105mg3/kg(cm3/100 g)D2414Day 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._
30、 _Date _Day No._ _Date _Day No._ _Date _TABLE 3 Statistical Analysis FormNOTEExperience so far has shown that neither a laboratorys test values nor a samples test values are random values about the grand average, buttend to reflect a persistent bias typified by the average value for the laboratory o
31、r the sample. Consequently, it is not appropriate to divide thereproducibility 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
32、 XR= (iX/LGrand average test value X5= (jXR/NUpper and lower control 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.D4122 1038. Acceptance8.1 All sublots tested as ho
33、mogeneous by this practice willbe considered acceptable by Committee D24 for use as the newIRB. The average values will be published in ClassificationD1765.9. Shelf Life9.1 The shelf life of the Industry Reference Black (IRB)carbon blacks is indefinite when properly stored in a mannerthat protects i
34、t from exposure to sources of moisture, such asprecipitation, other sources of liquid water, or high humidityenvironments. 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
35、 and other high surface area carbon blacks. Stepsare being taken within ASTM Committee D24 to developstandards 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 analysi
36、s form; table for IRB test data; uniformityguidelines for production and testingANNEX(Mandatory Information)A1. LISTING OF THE PROPERTIES OF INDUSTRY REFERENCE BLACKSA1.1 The listing of properties for Industry ReferenceBlacks (IRBs) is given in Table A1.1. The absolute values forI2number, OAN, COAN,
37、 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 an IRB is the elimination ofthe major part of laboratory-to-laboratory variation, it is usedas a reference mat
38、erial within each laboratory to correct actualmeasured property values in that laboratory.A1.1.1 The rubber properties of carbon black are typicallyreported as the difference between the values obtained for thetest and those obtained for the current IRB.NOTE A1.1IRB No. 73is an N330 type carbon blac
39、k prepared at onelocation, then evaluated by ASTM Committee D24 to ensure uniformity.A large 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.
40、6.4NOTE A1.2IRB No. 8 is an N330 type carbon black prepared at onelocation, then evaluated by ASTM Committee D24 to ensure uniformity.A large volume (115 910 kg (255 000 lb) of this carbon black wasprepared since it is used daily as a standard reference material by carbonblack producers. The carbon
41、black has an iodine number of 81.8 and OANof 103.0.5NOTE A1.3Previous Test Methods D3191 and Test Methods D3192testing was done following MethodA. No laboratory in the ITP to validateIRB#8 provided data for Method A. The more than two decade decline inthe use of IRBs probably can be attributed to an
42、 increase in the use of themore economical Methods B and C and a decline in the use of Method A.While no data was reported from Method A, it can be inferred from thedata and experience that the IRB#8 will be comparable to IRB#7 in thattest method, too. However, any laboratory using Method A should v
43、erifythis statement for their testing.NOTE A1.4With the exception of Test Methods D3191 Method BTensile Stress at 300 % Elongation, all the other reported difference fromIRB#7 values are less than the within laboratory test error reported forSRB B-4. This means that in a given laboratory testing bot
44、h IRB#7 andIRB#8, they would not be able to distinguish which sample was whichmaterial. The between laboratory testing error (9R9) for Test MethodsD3191 Method B Tensile Stress at 300 % Elongation is 1.41 (205) MPa(psi). This means that two different laboratories each testing IRB#7 andIRB#8 would no
45、t be able to agree between themselves as to which samplewas which material. Therefore, it can be concluded that, within testingerror, IRB#8 is a virtual drop-in replacement for IRB#7, negating the needto revise specifications.A1.2 The user of this table is cautioned against attemptingto add the diff
46、erences listed in the modulus and tensile strengthcolumns to determine the relationship of two carbon blacks notadjacent in time. Such an addition is likely to produce spuriousresults due to additive errors.A1.3 The listing of the properties of IRB No. 7 is given inTable A1.2. These values are the a
47、verage from the ITP toevaluate IRB No. 7.A1.4 The listing of the properties of IRB No. 8 is given inTable A1.3. These values are the average from the producerfrom their data to evaluate the uniformity of IRB No. 8.3Supporting data have been filed at ASTM International Headquarters and maybe obtained
48、 by requesting Research Report RR:D24-1005.4Available from Laboratory Standards, 227 Somerset, Borger, TX 79007.5Available from Continental Carbon Company, 16850 Park Row, Houston, TX77084, http:/ 104TABLE A1.1 Industry Reference BlacksIRB No. Producer LotSize, lbDate of ASTMAccept-anceIodineAbsorp-
49、tion No.,D1510,g/kgOAN,D2414,10-5m3/kgCOAN,D3493,10-5m3/kgTintStrength,D3265Difference from previous IRB, MPa (psi)D3192 D3191Modulus Tensile Modulus Tensile1 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
