ASTM D1510-17 Standard Test Method for Carbon Black—Iodine Adsorption Number.pdf

1、Designation: D1510 17Standard Test Method forCarbon BlackIodine Adsorption Number1This standard is issued under the fixed designation D1510; 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 par

2、entheses 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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination of the iodineadsorpt

3、ion 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. Iodine Number refer-ence

4、materials have been produced that exhibit stable iodinenumber upon aging. One or more of these reference materialsare recommended for daily monitoring (x-charts) to ensure thatthe results are within the control limits of the individualreference material. Use all Iodine Number reference materialsfrom

5、 a set for standardization of iodine testing (see Section 8)when target values cannot be obtained.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if an

6、y, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internation

7、ally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Pract

8、ice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4821 Guide for Carbon BlackValidation of Test MethodPrecision and BiasE969 Spec

9、ification for Glass Volumetric (Transfer) Pipets2.2 European Standards:3ISO/EN/DIN 8655-3 Piston-operated volumetric apparatus -Part 3: Piston burettes3. 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

10、shaken and centrifuged. The excess iodine is thentitrated 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 anautomat

11、ed sample processor where the mixture is stirred,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

12、is useful in characterizingcarbon blacks. It is 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 io

13、dine number.5. Apparatus5.1 Vials, glass, optically clear type, with polyethylenestoppers, 45 cm3.1This test method is 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 editio

14、n approved Oct. 1, 2017. Published November 2017. Originallyapproved in 1957. Last previous edition approved in 2016 as D1510 16a. DOI:10.1520/D1510-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMSta

15、ndards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.Copyright ASTM International, 100 Barr Harbor Drive, PO B

16、ox C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by

17、the World Trade Organization Technical Barriers to Trade (TBT) Committee.119 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,

18、 glass 25-cm3, Class A, side-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

19、min).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-dm3.5.11 Stirrer, approximately 300 by 300 mm for mixing.

20、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 strokes/min.5.16 Automatic Titrator.5.17 Redox Electrode

21、, 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 Apparatus,equipped with disposable filter.46. Reagents and

22、 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 AnnexA1. Pre-mixed 0.04728 N iodine solution and0.0394 N sodium thiosulfate may be purchased from commer-cial sources. It is recommende

23、d that the normality of pre-mixedsolutions be verified before use.6.3 Iodine Solution, c(I2) = 0.02364 mol/dm3(0.04728 N),containing 57.0 g potassium iodide Kl per dm3.6.4 Potassium Iodate Solution, c(KIO3) = 0.00657 mol/dm3(0.0394 N ) containing 45.0 g potassium iodide per dm3.6.5 Potassium Dichrom

24、ate Solution, c(K2Cr2O7)=0.006567 mol/cm3(0.0394 N), containing 1.932 g potassiumdichromate (certified/traceable primary standard) per dm3.(WarningPotassium dichromate is carcinogenic.)6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/dm3(0.0394 N), containing 5 cm3n-amyl alcohol per dm3.6.7

25、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:7.1.1.1 Measure approximately 20 cm3of 10 % potassiumiodide

26、(see A1.4) solution into a small graduated cylinder andtransfer to a 250 cm3iodine flask with a ground glass stopper.7.1.1.2 Measure approximately 20 cm3of 10 % sulfuric acidsolution (see A1.5) into a small graduated cylinder and add tothe KI solution in the iodine flask. The mixture should remainco

27、lorless.NOTE 1If a yellow color should develop, discard this KI solution.7.1.1.3 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 min.7.1.1.4 Titrate the contents of the i

28、odine flask against thenew sodium thiosulfate solution following 7.1.3 or 7.1.4.7.1.2 Use potassium iodate/iodide solution as follows:7.1.2.1 Pipet exactly 20 cm3of 0.0394 N potassium iodate/iodide solution into a 250-cm3iodine flask.7.1.2.2 Measure approximately 5 cm3of 10 % sulfuric acidinto a sma

29、ll graduated cylinder and add to the iodate/iodidesolution.7.1.2.3 Cap immediately and mix thoroughly.7.1.2.4 Titrate the contents of the iodine flask against thenew sodium thiosulfate solution following 7.1.3 or 7.1.4.7.1.3 Digital Buret:7.1.3.1 Switch the digital buret to fill mode, fill the reser

30、voirwith unstandardized sodium thiosulfate solution, and flush theinlet and delivery tubes.7.1.3.2 Change to the titrate mode and zero the counter.7.1.3.3 Add sodium thiosulfate until the contents of theiodine flask are a pale yellowish (potassium iodate) or paleyellowish-green (potassium dichromate

31、). Wash the buret tipand the walls of the flask with water.7.1.3.4 Add 5 drops of starch solution to the flask.7.1.3.5 Continue adding sodium thiosulfate dropwise untilthe blue or blue-violet color almost disappears.7.1.3.6 Wash the tip and walls of the flask with water, thenadvance the counter in 0

32、.01-cm3increments. Continue thissequence until the endpoint is reached, indicated by a colorless(potassium iodate) or sea-green (potassium dichromate) solu-tion.4The sole source of supply of the apparatus known to the committee at this timeis Brinkmann Instruments, Inc., One Cantiague Rd., PO Box 10

33、19, Westbury, NY11590-0207. The sole source of supply of the filter (disposable filter part #17594 K5 m Minisart with luer lock outlet) known to the committee at this time is SartoriusStedim North America Inc., 131 Heartland Blvd., Edgewood, NY 11717. If you areaware of alternative suppliers, please

34、 provide this information to ASTM Interna-tional Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.D1510 17219 7.1.3.7 Record the titration value and repeat from 7.1.1 or7.1.2 for a duplicate determination.7.1.3.8

35、Calculate the normality of the sodium thiosulfatesolution as in 7.1.5 and proceed as in 7.1.6. If the titration ismade to standardize the iodine solution as described in 7.2calculate the normality of the iodine solution as in 7.2.1.2 andproceed as in 7.2.1.3.7.1.4 Glass Buret:7.1.4.1 Using a convent

36、ional glass buret, fill the buret withunstandardized sodium-thiosulfate solution and flush 2 to3cm3through the tip.7.1.4.2 Adjust to the mark and titrate to a pale yellowish(potassium iodate) or pale yellowish-green (potassium dichro-mate).7.1.4.3 Wash the buret tip and the walls of the flask withwa

37、ter.7.1.4.4 Add 5 drops of starch solution to the iodine flask.7.1.4.5 Continue adding sodium thiosulfate dropwise untilthe endpoint is reached, indicated by a colorless (potassiumiodate) or sea-green (potassium dichromate) solution.7.1.4.6 Record the titration value to the nearest 0.025 cm3and repe

38、at from 7.1.1 or 7.1.2 for a duplicate determination.NOTE 2To achieve maximum performance from a glass buret, it isnecessary to use a small magnifier and to read to the nearest 0.025 cm3.7.1.4.7 Calculate the normality of the sodium thiosulfatesolution as in 7.1.5 and proceed as in 7.1.6. If the tit

39、ration ismade to standardize the iodine solution as described in 7.2calculate the normality of the iodine solution as in 7.2.1.2 andproceed as in 7.2.1.3.7.1.5 Calculate the normality of the sodium thiosulfatesolutions as follows:N 5 20 0.0394!/T (1)where:N = normality, andT = titration volume, cm3.

40、7.1.6 If N is not equal to 0.0394, adjust the solution in thefollowing manner: if the solution is too strong, add water (2.5cm3water per dm3sodium thiosulfate solution for each 0.0001N over 0.0394); if the solution is too weak, add solid sodiumthiosulfate (0.025 g solid sodium thiosulfate per dm3sod

41、iumthiosulfate solution for each 0.0001 N under 0.0394).7.2 Iodine Solution 0.04728 N (60.00003)This solutionmay be standardized against the secondary standard sodium-thiosulfate solution (see A1.3) standardized as in 7.1.7.2.1 Use sodium thiosulfate solution as follows:7.2.1.1 Pipet exactly 20 cm3o

42、f iodine solution into a250-cm3iodine flask and cap. Continue as in 7.1.3 or 7.1.4.7.2.1.2 Calculate the normality of the iodine solution asfollows:N 5 0.0394! T/20 (2)where:N = normality, andT =cm3of 0.0394 N sodium thiosulfate solution.7.2.1.3 If N is not equal to 0.04728 N, adjust solution in the

43、following manner: if the solution is too concentrated, add water(2.1 cm3water per dm3iodine solution for each 0.0001 N over0.04728); if the solution is too diluted, add iodine (12.7 mgiodine per dm3iodine solution for each 0.0001 N under0.04728). (This iodine may be more conveniently dispensedfrom a

44、 concentrated solution.)8. Normalization Using Iodine Number ReferenceMaterials8.1 The SRB HT reference materials (previously known asSRB HT Iodine Standards) are no longer commercially avail-able but may still be in use in some laboratories. A new lot wasprepared by the same process as the SBR HT r

45、eferencematerials and was designated as Iodine Number Reference(INR) to be consistent with D24s naming protocol for refer-ence materials. The SRB HT and INR reference materials areeach a set of three materials with different reference values.The three materials from either SRB HT or INR referencemat

46、erials should be used together for normalization. Do notnormalize using some materials from both sets.8.2 When a laboratory cannot obtain target values for allthree SRB HT or INR reference materials within establishedcontrol limits, the user should review recommendations foundin Guide D4821. If any

47、one of the three SRB HT or INRreference materials is still outside acceptable control limits, themethod described in 8.3 8.6 should be used to normalize alltest results.8.3 Test the three SRB HT or INR reference materials fourtimes each.8.4 Perform a regression analysis using the target value ofthe

48、SRB HT or INR reference materials (y value) and theindividual measured value (x value).8.5 Normalize the values of all subsequent test results usingthis regression equation:Normalized value 5 measured value 3slope!1y 2 intercept (3)8.6 Alternatively, a table of numbers may be generatedbased on the r

49、egression equation to find the correspondencebetween a measured value and a normalized value.8.7 Reevaluate the need for normalization whenever re-placement apparatus or new lots of iodine or sodium thiosulfatesolutions, or both, are put into use.9. Sampling9.1 Samples shall be taken in accordance with PracticesD1799 and D1900.10. Blank Iodine Determination10.1 Method ABlank Iodine Determination:10.1.1 Make a blank iodine determination by pipeting 20cm3or dispensing 25 cm3of 0.04728 N iodine solution into a125-cm3Erlenmeyer flask and titrating with 0.03