1、Designation: D 6915 07Standard Practice forCarbon BlackEvaluation of Standard Reference Blacks1This standard is issued under the fixed designation D 6915; 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 (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 set of carbon blacks to be used asStandard Referenc
3、e Blacks (SRBs).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
4、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 1510 Test Method for Carbon BlackIodine AdsorptionNumberD 2414 Test Method for Carbon BlackOil AbsorptionNumber (OAN)D 3265 Test
5、Method for Carbon BlackTint StrengthD 3493 Test Method for Carbon BlackOil AbsorptionNumber of Compressed Sample (COAN)D 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 4821 Guide for Carbon BlackValidation of TestMethod Precisi
6、on and BiasD 6556 Test Method for Carbon BlackTotal and ExternalSurface Area by Nitrogen Adsorption3. Significance and Use3.1 This practice is intended to ensure that SRBs areproduced and evaluated by a standard procedure.3.2 This practice is to be used to establish the averagephysicochemical proper
7、ties of a set of carbon blacks to be usedas SRBs.3.3 The carbon black grades to be used as SRBs should beselected to give as much coverage of the typical usage rangefor each test and as nearly evenly spaced across the range aspossible. Typically, the carbon black grades selected consist ofthree trea
8、d (hard) type furnace grades (designatedA, B, and C),three carcass (soft) type furnace grades (designated D, E, andF), and one thermal type grade (designated G). SubcommitteeD24.61 may elect to carry one or more of the existing SRBsinto the next set provided there is enough remaining material atthe
9、rate of usage to last through the expected life of the nextset. Limiting the choice of grades to be used means that not alltests will have an SRB set that is evenly spaced across therange of interest. All the SRB candidates are produced atapproximately the same time by the various producers. Theyare
10、 used as a set once they are approved. The sets areconsecutively numbered. Values and identification for thecurrent set are given in Guide D 4821. Any SRBs carriedforward will be renumbered for the new set.4. Production, Quality Control, and Quality Assurance4.1 It is assumed that manufacturers of t
11、he SRBs will usestate-of-the-art techniques to ensure maximum uniformitythroughout the entire production run. The production should bemade in one continuous production and packaging lot run. Thetesting called for in this practice is not intended to be asubstitute for in-process quality control. This
12、 interlaboratorystudy is only adequate to verify the quality of a homogeneouslot.4.2 The size of the lot for each SRB is determined byhistorical records on the rate of use. The lot should have anexpected life of about five years at the most recent rate of use.Historically, the lot size has usually b
13、een 10 000 lb.5. Uniformity Sampling and Testing5.1 It is the producers responsibility to ensure the SRB isproduced under stable conditions using good statistical processcontrol techniques.5.2 The producer shall maintain all test equipment in propercalibration and be able to supply proof of calibrat
14、ion records,if requested.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 May 1, 2007. Published June 2007. Originallyapproved in 2003. Last
15、previous edition approved in 2005 as D 6915 05b.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 website.1Copyright AS
16、TM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 The producer of the SRB shall be responsible forperforming all testing to demonstrate lot uniformity, and theproducer must submit the uniformity data to subcommitteeD24.61. The tests to be perfo
17、rmed as a minimum are thoselisted in Section 6. All test results must be 62 repeatabilitystandard deviations as determined for each test using any oneof the following means of determining Sr:(1) Any appropriate SRB materials Srlisted in the preci-sion table for a given test.(2) The average pooled va
18、lue Srlisted in the precision tablefor a given test.(3) Determine a tests Srusing a linear regression fromexisting precision data for a given test as defined in Annex A1.5.4 The samples for determining lot uniformity shall betaken at the same time as when the SRB is packaged. Thenumber of samples ne
19、eded to demonstrate uniformity shall bedetermined by subcommittee D24.61 prior to the production ofthe SRB(s).5.5 The number of samples taken and the quantity collectedfor each sample shall be adequate to perform all uniformitytesting and have sufficient material, such that when all samplematerial i
20、s combined and blended, there will be enoughmaterial that all the laboratories participating in the determi-nation of the mean and control limit testing can perform the testprotocol and have material left if additional testing is subse-quently needed.6. Procedure6.1 Each laboratory will use the curr
21、ent SRBs to verify thatall test methods are in calibration.6.2 Each sample is tested once on each of two days by twodifferent technicians (total of four test results).6.3 Physicochemical Tests:6.3.1 Perform the following physicochemical tests on thenew SRB (this does not apply to the testing of the
22、Heat Treated(HT) SRBs):6.3.1.1 Iodine Adsorption Number (Test 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 Multipoint B.E.T. NSA (Test Method D 6556)Report a single determination in 103m2/kg (m2/g) to thenear
23、est 0.1 unit.6.3.1.3 Oil Absorption Number (Test Method D 2414)Report the result obtained from an individual determination in10-5m3/kg (cm3/100 g) to the nearest 0.1 unit.NOTE 1Each participating laboratory must ensure that the absorptom-eter has been properly calibrated. Reported OAN values must be
24、 regressedto the previous SRB set.6.3.1.4 Oil Absorption Number of Compressed Sample (TestMethod D 3493)Report the result obtained from an indi-vidual determination in 10-5m3/kg (cm3/100 g) to the nearest0.1 unit.NOTE 2Each participating laboratory must ensure that the absorptom-eter has been proper
25、ly calibrated. Reported COAN values must beregressed to the previous SRB set.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 Statistical Thickness Surface Area (STSA) (TestMethod D 6556)Report sing
26、le determination in 103m2/kg(m2/g) to the nearest 0.1 unit.6.4 For the HT SRBs, perform the Iodine AdsorptionNumber Test (Test Method D 1510). Report the result obtainedfrom an individual determination in grams of iodine perkilogram to the nearest 0.1 unit.7. Statistical Analysis7.1 The uniformity s
27、ample material collected by the pro-ducer shall be blended, apportioned, and sent to each partici-pant in the interlaboratory study to evaluate the new SRB.7.2 To achieve statistical validity and allow for the removalof outliers, at least 20 laboratories should participate in theevaluation for each
28、test method.7.3 Each participating laboratory shall maintain all testequipment in proper calibration and be able to supply proof ofcalibration and calibration records, if requested.7.4 The interlaboratory study protocol shall be determinedby subcommittee D24.61 prior to the production of the SRB(s).
29、7.5 The mean and control limit values of the SRBs for eachtest shall be determined using the methodology of PracticeD 4483, including the removal of outlier values.7.6 When calibration data is collected along with the testresults for a new SRB and an analysis of the calibration datashows that any gi
30、ven laboratory is not in a state of calibration,the data from that laboratory may be removed from the data seteven though the data is not flagged as being an outlier by thetechniques of Practice D 4483.7.7 After eliminating the outliers and any laboratories not ina state of calibration, the remainin
31、g data for each test methodwill be used to provide mean and control limit values fortabulation in Guide D 4821. This information may also beplaced in each test method, if desired. The analysis could beused to develop new precision and bias values for each testmethod.8. Acceptance8.1 Subcommittee D24
32、.61 may reject all or part of acandidate SRB lot as not uniform. All SRB lots tested ashomogeneous by this practice will be considered acceptable byCommittee D24 for use as a new SRB. The mean values andcontrol limits will be published in Guide D 4821.9. Shelf Life9.1 The shelf life of the Standard
33、Reference Black (SRB)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)
34、. 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; lot size; physical propert
35、ies; physicochemi-cal properties; shelf life; standard reference blacks (SRBs)D6915072ANNEXA1. DETERMINATION OF SrUSING LINEAR REGRESSIONA1.1 An appropriate Srlevel can be determined using aregression analysis of mean level and Srvalues found in theprecision table for a given test. The regression ma
36、y beperformed using all six furnace SRBs, or, if more appropriate,using the three tread (hard) blacks or three carcass (soft) blacksas demonstrated in Fig.A1.1. The regression coefficients (slopeand intercept) are then used to estimate an Srfor a materialsmean level as shown in Fig.A1.2 and TableA1.
37、1. The exampleis a tread or hard black with an STSA mean level of 160 m2/gand an estimated Srof 1.65 m2/g.FIG. A1.1 SRB-6 Series STSA Repeatability Standard DeviationFIG. A1.2 Estimation of STSA Srfor Tread Product Using SRB-6TABLE A1.1 Precision Data for SRB-6 Tread StandardsSRB STSA Mean SrA-6 135
38、.7 1.37B-6 105.4 0.96C-6 79.2 0.69Regression CoefficientsASlope 0.0121Intercept 0.2824AModel: Sr= 0.0121x 0.2824Estimate for x = 160Sr= 1.65D6915073ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
39、of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every fi
40、ve years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
41、committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D6915074
