ASTM D1510-2009 Standard Test Method for Carbon Black&x2014 Iodine Adsorption Number.pdf
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1、Designation: D 1510 09Standard Test Method forCarbon BlackIodine Adsorption Number1This standard is issued under the fixed designation D 1510; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the determination of the iodineadsorption
3、 number of carbon black.1.1.1 Method A is the original test method for this determi-nation and Method B is an alternate test method usingautomated sample processing and analysis.1.2 The iodine adsorption number of carbon black has beenshown to decrease with sample aging. New SRB HT IodineStandards h
4、ave been produced that exhibit stable iodinenumber upon aging. These SRB HT Iodine Standards arerecommended for daily monitoring (x-charts) of testing and forstandardization of iodine testing (see Section 8) when targetvalues cannot be obtained.1.3 The values stated in SI units are to be regarded as
5、standard. No other units of measurement are included in thisstandard.1.4 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 to establish appro-priate safety and health practices and determine the
6、applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbo
7、n Black ManufacturingIndustriesD 4821 Guide for Carbon BlackValidation of TestMethod Precision and Bias3. Summary of Test Methods3.1 In Test Method A, a weighed sample of carbon black istreated with a portion of standard iodine solution and themixture shaken and centrifuged. The excess iodine is the
8、ntitrated with standard sodium thiosulfate solution, and theadsorbed iodine is expressed as a fraction of the total mass ofblack.3.2 In Test Method B, a weighed sample of carbon black istreated with a portion of standard iodine solution using anautomated sample processor where the mixture is stirred
9、,settled and aliquoted for automatic titration. The excess iodineis titrated with standard sodium thiosulfate solution, and theadsorbed iodine is expressed as a fraction of the total mass ofblack.4. Significance and Use4.1 The iodine adsorption number is useful in characterizingcarbon blacks. It is
10、related to the surface area of carbon blacksand is generally in agreement with nitrogen surface area. Thepresence of volatiles, surface porosity, or extractables willinfluence the iodine adsorption number. Aging of carbon blackcan also influence the iodine number.5. Apparatus5.1 Vials, glass, optica
11、lly clear type, with polyethylenestoppers, 45 cm3.5.2 Gravity Convection Drying Oven, capable of maintain-ing 125 6 5C.5.3 Buret, either of the following may be used:5.3.1 Digital Buret, 25-cm3capacity, with 0.01-cm3incre-ment counter and zero reset control, or5.3.2 Buret, glass 25-cm3, Class A, sid
12、e-arm filling, gradu-ated in 0.05 cm3and with automatic zero.5.4 Repetitive Dispenser, 25-cm3capacity, 60.1% repro-ducibility and calibrated to within 60.03-cm3accuracy.5.5 Balance, analytical, with 0.1-mg sensitivity.5.6 Centrifuge, with minimum speed of 105 rad/s (1000 r/min).1This test method is
13、under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.21 on Carbon BlackSurface Area and Related Properties.Current edition approved May 15, 2009. Published June 2009. Originallyapproved in 1957. Last previous edition approved in 2008 as D 1
14、510 08c.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 ASTM International, 100 Barr Harbor Drive,
15、 PO Box C700, West Conshohocken, PA 19428-2959, United States.5.7 Volumetric Flask, 2000-cm3with standard taper stopper.5.8 Funnel, large diameter, with standard taper joint to fitthe 2000-cm3flask.5.9 Glass Bottle, amber, 2000-cm3, with standard taperstopper.5.10 Glass Jug, approximate capacity 20-
16、dm3.5.11 Stirrer, approximately 300 by 300 mm for mixing.5.12 Stirrer, approximately 100 by 100 mm for titrating.5.13 Desiccator.5.14 Miscellaneous Class A Glassware, and equipmentnecessary to carry out the test as written.5.15 Mechanical Shaker, with at least 1 in. stroke length anda minimum of 240
17、 strokes/min.5.16 Automatic Titrator.5.17 Redox Electrode, combined platinum ring electrodewith an Ag/AgCl/KCl reference electrode and a ceramic frit.5.18 Volumetric Flask, 500 cm3with standard taper stopper.5.19 Flask, 250 cm3with ground glass stopper.5.20 Automatic Sample Processor and Titration A
18、pparatus,equipped with disposable filter.36. Reagents and Solutions6.1 Purity of ReagentsUnless otherwise stated, all chemi-cals shall be of reagent grade.6.2 The preparation of the solutions listed below is de-scribed in Annex A1. Pre-mixed 0.0473 N iodine solution and0.0394 N sodium thiosulfate ma
19、y be purchased from commer-cial sources. It is recommended that the normality of pre-mixedsolutions be verified before use.6.3 Iodine Solution, c(I2) = 0.02364 mol/dm3(0.0473 N),containing 57.0 g potassium iodide Kl per dm3.6.4 Potassium Iodate Solution, c(KIO3) = 0.00657 mol/dm3(0.0394 N) containin
20、g 45.0 g potassium iodide per dm3.6.5 Potassium Dichromate Solution,c(K2Cr2O7)=0.006567 (0.0394 N), containing 1.932 g potassium dichromate(certified/traceable primary standard) per dm3.(WarningPotassium dichromate is carcinogenic.)6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/dm3(0.0394
21、N), containing 5 cm3n-amyl alcohol per dm3.6.7 Sulfuric Acid,10%.6.8 Soluble Starch Solution, 1 %, containing 0.02 g salicylicacid per dm3.6.9 Deionized Water.7. Standardization of Solutions7.1 Sodium Thiosulfate, 0.0394 N (60.00008):7.1.1 Use potassium dichromate solution as follows:7.1.2 Measure a
22、pproximately 20 cm3of 10 % potassiumiodide (see A1.4) solution into a small graduated cylinder andtransfer to a 250 cm3iodine flask with a ground glass stopper.7.1.3 Measure approximately 20 cm3of 10 % sulfuric acidsolution (see A1.5) into a small graduated cylinder and add tothe KI solution in the
23、iodine flask. The mixture should remaincolorless.NOTE 1If a yellow color should develop, discard this KI solution.7.1.4 Using a 20 cm3pipet, transfer 20 cm3of standard0.0394 N potassium dichromate solution (see A1.8) into the250 cm3iodine flask, replace stopper, swirl, and place in thedark for 15 mi
24、n.7.1.5 Titrate the contents of the iodine flask against the newsodium thiosulfate solution following 7.2.6 or 7.2.7.7.2 Sodium Thiosulfate, 0.0394 N (60.00008):7.2.1 Use potassium iodate/iodide solution as follows:7.2.2 Pipet exactly 20 cm3of 0.0394 N potassium iodate/iodide solution into a 250-cm3
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