1、Designation: D1510 11aStandard 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 pa
2、rentheses 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 ha
4、ve 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 te
5、sting (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 there
6、sponsibility 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 BlackS
7、ampling 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 Bias3. Summary of Test Methods3.1 In Test Method A, a weighed sample of carbon black istrea
8、ted with a portion of standard iodine solution and themixture 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 istrea
9、ted with a portion of standard iodine solution using anautomated 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 of
10、black.4. Significance and Use4.1 The iodine adsorption number 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 ads
11、orption number. Aging of carbon blackcan also influence the iodine number.5. Apparatus5.1 Vials, glass, optically 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-
12、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 Dispenser, 25-cm3capacity, 60.1% repro-ducibility and calibrated to within 60.03-cm3accuracy.5.5 Balance, analytic
13、al, 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.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.21 on Carbon BlackS
14、urface Area and Related Properties.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 1957. Last previous edition approved in 2011 as D1510 11. DOI:10.1520/D1510-11A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
15、 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, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.8 Funnel, large diameter, with standard taper jo
16、int 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 Glassware, and
17、 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 Volumetric Flas
18、k, 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.36. Reagents and Solutions6.1 Purity of ReagentsUnless otherwise stated, all chemi-cals shall be of reagent grade.6.2 The prepara
19、tion of the solutions listed below is de-scribed in Annex A1. 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) = 0.02364 mol/dm3(0
20、.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/traceable primary
21、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 Water.7. Standa
22、rdization 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 stopper.7.1.1.
23、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, transfer 20 cm3of sta
24、ndard0.0394 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/iodide solution
25、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.7.1.2.4 Titrate the c
26、ontents 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 the titrate mo
27、de 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 flask.7.1.3.5 Cont
28、inue 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 iodate) or sea-g
29、reen (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 ismade to standardize the iodine solution as de
30、scribed 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 tip.7.1.4.2 Adjust to the mark and titrate to a
31、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 dropwise untilthe endpoint is reached, indicated by a
32、 colorless (potassiumiodate) or sea-green (potassium dichromate) solution.3The sole source of supply of 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
33、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 provide this information to ASTM Interna-tional Headquarters. Your comments will recei
34、ve careful consideration at a meetingof the responsible technical committee,1which you may attend.D1510 11a27.1.4.6 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, it isnecessary
35、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 solution as in 7.2.
36、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, add water (2.5c
37、m3/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 A1.3) standardi
38、zed 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 =cm3of 0.0394
39、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). (This iodine
40、 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 inGuide D4821. If a
41、ny 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 HT Iodine Stand
42、ards (y value) and the individualmeasured value (x value).8.4 Normalize the values of all subsequent test results usingthis regression equation:Normalized value 5measured value 3 slope!1 y2intercept (3)8.5 Alternatively, a table of numbers may be generatedbased on the regression equation to find the
43、 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 PracticesD1799 and D1900.1
44、0. Method A10.1 Dry an adequate sample of carbon black for 1 h, in agravity-convection oven set at 125C , in an open container ofsuitable dimensions, so that the depth of the black is no morethan 10 mm. Cool to room temperature in a desiccator beforeuse.10.2 Weigh a mass of the dried sample into a g
45、lass vial asshown by the following table.All masses must be to the nearest0.001 g in case of iodine numbers from 0 to 520.9 and to thenearest 0.0001 g in case of iodine numbers from 521.0 andabove.Iodine Number Sample Mass (g) Ratio I2: Sample Mass0130.9 0.500 50:1131.0280.9 0.250 100:1281.0520.9 0.
46、125 200:1521.0 and above 0.0625 400:110.2.1 Use the sample mass determined by the expectediodine number. If the result falls either above or below therange shown for that sample size, retest using the sample massspecified in 10.2 for the range into which it has fallen.NOTE 3Unagitated, unpelleted ca
47、rbon black may be densified, ifdesired, before drying, prior to weighing.10.2.2 The sample mass table given in 10.2 pertains to the25 cm3iodine solution as given in 10.3. Different volumes ofiodine solution and of sample masses are permissible only ifthe iodine solution to sample mass ratio is kept
48、the same as thatgiven by the table in 10.2. The sample mass must be kept to1.000 g maximum. Should the sample mass and correspondingvolume of iodine solution be increased, then a glass vial witha volume that is at least two times the amount of iodinesolution used for the test should be used in order
49、 to preserve theefficiency of the shaking.10.3 Pipet (or dispense from a calibrated repetitive dis-penser) 25 cm3of 0.04728 N I2solution into the glass vialcontaining the sample and cap immediately.10.4 Secure the vial in the mechanical shaker and shake for1 min at a minimum of 240 strokes/min.10.5 Centrifuge immediately for 1 min for pelleted blackand 3 min for loose black.10.6 Decant immediately. If more than one sample is beinganalyzed, the solution should be decanted into small flasks orclean, dry vials and capped immediately.10.7 Pipet 20 cm3of solution into
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