1、Designation: D4122 10a (Reapproved 2015)Standard 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
2、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 This practice covers guidelines for the production andtesting for uniformity of a lot of carbon black to be used as
3、 anIndustry Reference 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
4、 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:2D412 Test Methods for Vulcanized Rubber and Thermoplas-tic ElastomersTensionD1506 Test Methods for Carbon BlackAs
5、h ContentD1508 Test 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 fo
6、r Carbon Black ExtractablesTransmittance 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 (Styre
7、ne-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)D5230 Test Method for Carbon BlackAutomated Indi-vi
8、dual 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 used to establish the averagephysicochemical and
9、 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 the entire production run. The production should
10、 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 of the lot is determined by historical records ont
11、he 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 reduce environmental expo-sure. The bagged black will
12、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 numbered from one throughn, where n is the total numbe
13、r of sublots, in order to representthe corresponding production lot.1This 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 Jan. 1, 2015. Published
14、February 2015. Originallyapproved in 1982. Last previous edition approved in 2010 as D4122 10a. DOI:10.1520/D4122-10AR15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refe
15、r 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 States15.2 n 4-dm3(1-gal) samples, numbered from one through n,and taken from the corresponding bags, will be sent to eachparticipant
16、 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 n days. These days shall be as near to con
17、secutive 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 accordancewith Test Methods D3191 and cure for 50 m
18、in 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 withTest Methods D412,Test MethodA, test five dumbbells from each cured sheet and determine themedian values of tensile stress at 300 % elongation, tensilestrengt
19、h, 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 Tests:6.4.1 Perform the following physicochemica
20、l 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 obtained from an individual determination in
21、105m3kg (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 shown in Table 3.Then calculate the statist
22、ics 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 falls outside the intervaldefined by the upp
23、er 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 average)falls outside the upper and lower co
24、ntrol 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 action.TABLE 1 Industry Reference Black Test
25、 DataLaboratory Number _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 5
26、0 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 30Date _ Prev. IRB 50 30Day No._
27、 50 30Date _ Prev. IRB 50 30D4122 10a (2015)27.4 After deleting data, the remaining data for each test canbe used to provide average differences between the new IRBand 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. T
28、hencalculate the statistics defined in Table 3. The results are forinformation only and not to determine the uniformity of the lot.TABLE 2 Industry Reference Black Informational Test DataLaboratory Number_Day of Mixingand DateSample No.Iodine No.,g/kgD1510Oil AbsorptionNo.,105mg3/kg (cm3/100 g)D2414
29、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 _Day No._ _Date _TABLE 3 Statistical Analysis FormNOTE 1Experience so far has shown that neither a laboratorys test values no
30、r 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 thereproducibility by the square root of L or N as might otherwise be the case when co
31、mparing 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 control limits for row averages 5X%6reproducibility of the test method.Column average X
32、C= jX/NUpper and lower control limits for column averages5X%6reproducibility of the test method.D4122 10a (2015)38. 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 of the Industry Ref
33、erence 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 extended period (years). T
34、his 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 reference blacks (IR
35、Bs); 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 properties for Indust
36、ry 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 of an IRB is the el
37、imination 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 values obtained for
38、 thetest and those obtained for the current IRB.NOTE A1.1IRB No. 73is an N330 type carbon black 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 m
39、aterial by carbonblack producers. The carbon black has an iodine number of 83.0 and OANof 101.6.4NOTE 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
40、 since it is used daily as a standard reference material by carbonblack producers. The carbon 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 ITPto validateIRB#8 provided data for
41、Method A. The more than two decade decline inthe use of IRBs probably can be attributed to an 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
42、 comparable to IRB#7 in thattest method, too. However, any laboratory using Method A should verifythis 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
43、 laboratory test error reported forSRB B-4. This means that in a given laboratory testing both IRB#7 andIRB#8, they would not be able to distinguish which sample was whichmaterial. The between laboratory testing error (“R“) for Test MethodsD3191 Method B Tensile Stress at 300 % Elongation is 1.41 (2
44、05) MPa(psi). This means that two different laboratories each testing IRB#7 andIRB#8 would not 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 rev
45、ise 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 in time. Such an addition is likely to produce spuriousresults due to additive errors.
46、A1.3 The listing of the properties of IRB No. 7 is given inTable A1.2. These values are the average 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
47、 No. 8.3Supporting data have been filed at ASTM International Headquarters and maybe obtained 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:/ 10a (2015)
48、4TABLE A1.1 Industry Reference BlacksIRB No. Producer LotSize, lbDate ofASTMAccept-anceIodineAbsorp-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
49、-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 82.1 97.1 86.5 107.1 15-min30-min+0.2 (+30)+0.5 (
