1、Designation: D1510 13Standard 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 Department of Defense.1. Scope1.1 This test method covers the determination of the iodineadsorption n
3、umber 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 hav
4、e been produced that exhibit stable iodinenumber upon aging. One or more of these SRB HT IodineStandards are recommended for daily monitoring (x-charts) toensure that the results are within the control limits of theindividual standard. Use all SRB HT Iodine Standards forstandardization of iodine tes
5、ting (see Section 8) when targetvalues 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 any, associated with its use. It is theres
6、ponsibility of the user 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:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSa
7、mpling 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 Specification for Glass Volumetric (Transfer) Pipets2.2 European Standards:3ISO/EN/
8、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 shaken and centrifuged. The excess iodine is thentitrated with standard sodium
9、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,settled and aliquoted for auto
10、matic 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 related to the surface area of
11、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, optically clear type, with polyethyle
12、nestoppers, 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: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
13、and Related Properties.Current edition approved July 1, 2013. Published August 2013. Originallyapproved in 1957. Last previous edition approved in 2012 as D1510 12. DOI:10.1520/D1510-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceas
14、tm.org. For Annual Book of ASTMStandards 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 Internat
15、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3.1 Digital Buret, 25-cm3capacity, with 0.01-cm3incre-ment counter and zero reset control, or5.3.2 Buret, glass 25-cm3, Class A, side-arm filling, gradu-ated in 0.05 cm3and with automatic zero.5.4 Repetitive
16、 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).5.7 Volumetric Flask, 2000-cm3with standard taper stopper.5.8 Funnel, large diameter, with stand
17、ard 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.5.12 Stirrer, approximately 100 by 100 mm for titrating.5.13 Desiccator.5.14 Miscellaneous Class A Gl
18、assware, 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, combined platinum ring electrodewith an Ag/AgCl/KCl reference electrode and a ceramic frit.5.18 Vol
19、umetric 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 Solutions6.1 Purity of ReagentsUnless otherwise stated, all chemi-cals shall be of reagent grade.6.2
20、 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 recommended that the normality of pre-mixedsolutions be verified before use.6.3 Iodine Solution, c(I2) = 0.0236
21、4 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 Dichromate Solution, c(K2Cr2O7)=0.006567 (0.0394 N), containing 1.932 g potassium dichromate(certified/trace
22、able 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 Sulfuric Acid, 10 %.6.8 Soluble Starch Solution, 1 %, containing 0.02 g salicylicacid per dm3.6.9 Deionized
23、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 (see A1.4) solution into a small graduated cylinder andtransfer to a 250 cm3iodine flask with a ground glass
24、 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 remaincolorless.NOTE 1If a yellow color should develop, discard this KI solution.7.1.1.3 Using a 20 cm3pipet, transf
25、er 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 iodine flask against thenew sodium thiosulfate solution following 7.1.3 or 7.1.4.7.1.2 Use potassium iodate/i
26、odide 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 small graduated cylinder and add to the iodate/iodidesolution.7.1.2.3 Cap immediately and mix thoroughly.7.1.2.
27、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 reservoirwith unstandardized sodium thiosulfate solution, and flush theinlet and delivery tubes.7.1.3.2 Change to
28、 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). Wash the buret tipand the walls of the flask with water.7.1.3.4 Add 5 drops of starch solution to the fla
29、sk.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 0.01-cm3increments. Continue thissequence until the endpoint is reached, indicated by a colorless(potassium i
30、odate) or sea-green (potassium dichromate) solu-tion.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 Calculate the normality of the sodium thiosulfatesolution as in 7.1.5 and proceed as in 7.1.6. If the titration is4The sole source of supply of
31、the apparatus known to the committee at this timeis Brinkmann Instruments, Inc., One Cantiague Rd., PO Box 1019, 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
32、North America Inc., 131 Heartland Blvd., Edgewood, NY 11717. If you areaware of alternative suppliers, please 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
33、132made 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 conventional glass buret, fill the buret withunstandardized sodium-thiosulfate solution and flush 2 to3cm3through the
34、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 withwater.7.1.4.4 Add 5 drops of starch solution to the iodine flask.7.1.4.5 Continue adding sodium thiosulfate dropw
35、ise 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 repeat from 7.1.1 or 7.1.2 for a duplicate determination.NOTE 2To achieve maximum performance from a glass buret, i
36、t 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 titration ismade to standardize the iodine solution as described in 7.2calculate the normality of the iodine solut
37、ion 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, cm3.7.1.6 If N is not equal to 0.0394, adjust the solution in thefollowing manner: if the solution is too strong, a
38、dd water (2.5cm3/dm3solution for each 0.0001 N over 0.0394); if thesolution is too weak, add solid sodium thiosulfate (0.025 g/dm3for 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 A
39、1.3) standardized as in 7.1.7.2.1 Use sodium thiosulfate solution as follows:7.2.1.1 Pipet exactly 20 cm3of 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
40、=cm3of 0.0394 N sodium thiosulfate solution.7.2.1.3 If N is not equal to 0.04728 N, adjust solution in thefollowing manner: if the solution is too concentrated, add water(2.1 cm3/dm3for each 0.0001 N over 0.04728); if the solutionis too diluted, add iodine (12.7 mg/dm3for each 0.0001 Nunder 0.04728)
41、. (This iodine may be more convenientlydispensed from a concentrated solution.)8. Normalization Using SRB HT Iodine Standards8.1 When a laboratory cannot obtain target values for allthree SRB HT Iodine Standards within established x-charttolerances, the user should review recommendations found inGui
42、de D4821. If any one of the three SRB HT Iodine Standardsis still outside acceptable tolerances, the method described in8.2-8.5 should be used to normalize all test results.8.2 Test the three SRB HT Iodine Standards four times each.8.3 Perform a regression analysis using the target value ofthe SRB H
43、T Iodine Standards (y value) and the individualmeasured value (x value).8.4 Normalize the values of all subsequent test results usingthis regression equation:Normalized value 5 measured value 3slope!1y 2 intercept (3)8.5 Alternatively, a table of numbers may be generatedbased on the regression equat
44、ion to find the correspondencebetween a measured value and a normalized value.8.6 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 PracticesD1
45、799 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 0.0394 N sodiumthiosulfate as in 11.10.1, 11.10.2,or11.10.3.
46、10.1.2 A 25-cm3blank must be multiplied by 0.8 for use inthe formula of 13.1.10.1.3 Make a duplicate blank determination and use theaverage of the two in the calculations.NOTE 3A duplicate blank determination need be run only once eachday, unless new solutions are introduced during the day.10.1.4 If
47、 both solutions are within acceptable limits, theblank will measure 24.00 6 0.09 cm3. If not, the normalities ofone or both solutions should be rechecked. If, after the recheckof solutions, normalities are still outside the acceptable limitsrefer to 7.2.1.3 to adjust iodine solution. See Table 1 for
48、 blanktolerance components.10.1.5 The blank tolerance for a 20 cm3volume of iodinesolution is defined as the sum of (1) titration volume deviationfor acceptable variation in both iodine and sodium thiosulfatesolution concentrations, and (2) dispenser tolerance for ClassA20 mL pipet.TABLE 1 Blank Tol
49、erance ComponentsBlankVolume cm3A. SolutionDeviations cm3B. DispenserTolerance cm3BlankTolerance cm320.00 0.06 0.03 0.09D1510 13310.1.6 The solution deviation is based on the maximumvariation in solution concentrations defined in 7.1 and 7.2.Tolerances for ClassAvolumetric pipets are from SpecificationE969.10.2 Method BBlank Iodine Determination:10.2.1 Make a blank iodine determination by placing amagnetic stir bar into an empty beaker and place the beakerinto the automated sample processor.10.2.2 Initiate the automatic sample processor and titrationapparatus.
