1、Designation: D4122 17Standard 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 Thermoplas-tic 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 ExtractD2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D3182 Practice for RubberMaterials, Equipment, and Pro-cedures for Mixing Standard Compounds and PreparingStandard Vulcanized SheetsD3191 Test Methods for Carbon Black in SBR (Styrene-Butadiene Rubber
7、)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)D5230 Test Method for Carbon BlackAutomated Indi-vidual Pellet Hardnes
8、sD6556 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 used to establish the averagephysicochemical and physical rubber pr
9、operties 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 the entire production run. The production should bemade in one cont
10、inuous 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 of the lot is determined by historical records onthe rate of use. The
11、 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 reduce environmental expo-sure. Depending on the size of the lot, the bag
12、ged black will besegregated into equal sized sublots, typically ten to twenty,representing some logical subdivision, such as a truck load.5. Sampling5.1 To avoid having to break down stacked and wrappedbags on a pallet, the bags to be used as samples for uniformityand property determination testing
13、are typically removed atappropriate times from the bagging stream.At least one sampleper sublot will be collected for uniformity testing. If more than1This practice is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.61 on Carbon BlackS
14、ampling and Statistical Analysis.Current edition approved Jan. 1, 2017. Published January 2017. Originallyapproved in 1982. Last previous edition approved in 2015 as D4122 10a (2015).DOI: 10.1520/D4122-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer S
15、ervice 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 StatesThis international standard was developed i
16、n 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 (TBT) Committee.1one sample point is ident
17、ified for each sublot, they should bespaced to represent approximately equal quantities. Typically,two bags are taken at each sampling point. One is retained bythe producer for in-house uniformity testing and one is used forsamples to be distributed to participants in the rubber testingand uniformit
18、y ITP. The bags selected will be numbered fromone through n, where n is the total number of sublots, in orderto represent the corresponding production lot or labeled toidentify the sublot and its position relative to the whole of thecorresponding production lot.5.2 n 4-dm3(1-gal) samples, numbered f
19、rom one through n,or marked with the labels from 5.1 as taken from the corre-sponding bags, will be sent to each participant in the interlabo-ratory study to evaluate the new IRB.5.3 Additionally, a 4-dm3(1-gal) sample of the previousIRB taken from a common blended source will also be sent toeach pa
20、rticipant.6. Procedure6.1 It is preferred that all of the samples be tested on thesame day for any of the test methods described in 6.2 and 6.3.If the testing cannot be completed in the same day, it should becompleted in consecutive days.6.2 Rubber Physical Tests:6.2.1 Perform the following physical
21、 tests in rubber on boththe new and previous IRB. Test samples mixed in accordancewith Test Methods D3191, Test Method A, Test Method B, orTest Method C and cure for 50 min at 145C as well as samplesmixed in accordance with Test Methods D3192, Test MethodA, Test Method B, or Test Method C and cure f
22、or 30 min at145C. It is preferred that participating laboratories be found sothat data from all test methods can be included for evaluation.6.2.1.1 In accordance withTest Methods D412,Test MethodA, test five dumbbells from each cured sheet and determine themean values of tensile stress at 300 % elon
23、gation, tensilestrength, and ultimate elongation.6.2.1.2 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 %.6.3 Informational Physicochemical Tests:6.3.1 Perform the fo
24、llowing physicochemical tests on thenew IRB:6.3.1.1 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.6.3.1.2 Oil Absorption Number (Test Method D2414)Report the result obtained from an indiv
25、idual determination in105m3kg (cm3/100 g) to the nearest 0.1 unit.6.3.2 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 shown in Table 3.Then
26、 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.TABLE 1 Industry Reference Black Test DataLaboratory Numb
27、er _ Test Method _Day of Mix-ing and DateSampleNo.Tensile Strength,MPa D3191TensileStress at300 %,MPaD3191Elonga-tion, %D3191Tensile Strength,MPaD3192300 %Modulus,MPaD3192Elonga-tion, %D3192Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Da
28、y No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30Date _ Prev. IRB 50 30Day No._ 50 30
29、Date _ Prev. IRB 50 30D4122 1727.2 If any row average test result 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
30、 production lot.7.3 If any laboratory average test result (column 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 h
31、as a significant reproduc-ibility problem, which needs corrective action.7.4 After deleting data, the remaining data for each test canbe used to provide average differences between the new IRBand the previous one.TABLE 2 Industry Reference Black Informational Test DataLaboratory Number_Day of Mixing
32、and 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._ _Date _Day No._ _Date _Day No._ _Date _TABLE 3 Statistical Analys
33、is FormNOTE 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 ther
34、eproducibility 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 Nvalues.Test Method: ASTM D _ _ _SampleNo.Laboratory No. 1 2 . i . LXR12.j.NXC X%5Row average XR= iX/LGrand average test value X%5( jXR/NUpper and lower contr
35、ol limits for row averages 5X%6reproducibility of the test method.Column average XC= jX/NUpper and lower control limits for column averages5X%6reproducibility of the test method.D4122 1737.5 For each test in Table 2, enter the results from eachlaboratory for each sample in the form shown in Table 3.
36、 Thencalculate the statistics defined in Table 3. 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.9. Shelf Life9.1 The shelf life
37、 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 humidityenvironments. Iodine number is the only property known tochange over an extend
38、ed 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 that are more stable over a long period.10. Keywords10.1 blending; industry
39、reference blacks (IRBs); lot size;physical properties; physicochemical properties; shelf life;statistical analysis 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 p
40、roperties for Industry Reference Blacks(IRBs) is given in Table A1.1. The absolute values for I2number, 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
41、 of an IRB is the elimination ofthe major part of laboratory-to-laboratory variation, it is usedas a reference material 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
42、 values obtained for thetest and those obtained for the current IRB.NOTE A1.1IRB No. 83is 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
43、standard reference material by carbonblack producers. The carbon black has an iodine number of 81.8 and OANof 103.0.NOTE A1.2IRB No. 93is an N330 type carbon black prepared at onelocation, then evaluated by ASTM Committee D24 to ensure uniformity.A large volume (181 818 kg (400 000 lb) of this carbo
44、n black wasprepared since it is used daily as a standard reference material by carbonblack producers. The carbon black has an iodine number of 82.1 and OANvalue of 98.9.NOTE A1.3Prior to the introduction of IRB8, all rubber testing wasdone following Method A of Test Methods D3191 and Test MethodsD31
45、92. No laboratory in the ITP to validate IRB8 provided data forMethod A for either Test Methods D3191 or Test Methods D3192.Therefore, data from Methods B and C were included in the table. In theITP to validate IRB9, data was provided for all three methods of TestMethods D3191 and Test Methods D3192
46、. The difference from IRB8 toIRB9 data for all three methods has been included in Table A1.1.NOTE A1.4All the reported “difference from IRB8 to IRB9” valuesfor all three test methods of Test Methods D3191 and Test Methods D3192are less than the within laboratory test error reported in the applicable
47、precision statement sections of those two Test Methods. This means thatin a given laboratory using these test methods for testing both IRB8 andIRB9, they would not be able to distinguish which sample was whichmaterial based on their test results. Therefore, it can be concluded that,within testing er
48、ror, IRB9 is a virtual drop-in replacement for IRB8,negating the need to revise industry specifications.A1.2 The user of this table is cautioned against attemptingto add the differences listed in the modulus and tensile strengthcolumns to determine the relationship of two carbon blacks notadjacent i
49、n time. Such an addition is likely to produce spuriousresults due to additive errors.A1.3 The listing of the properties of IRB No. 8 is given inTable A1.2. These values are the average from the producerfrom their data to evaluate the uniformity of IRB No. 8.A1.4 The listing of the properties of IRB9 is given in TableA1.3. These values are the
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