1、Designation: D1510 11a D1510 12Standard 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 num
2、ber in parentheses 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 iodine a
3、dsorption number of carbon black.1.1.1 Method A is the original test method for this determination and Method B is an alternate test method using automatedsample processing and analysis.1.2 The iodine adsorption number of carbon black has been shown to decrease with sample aging. New SRB HT IodineSt
4、andards have been produced that exhibit stable iodine number upon aging. One or more of these SRB HT Iodine Standards arerecommended for daily monitoring (x-charts) to ensure that the results are within the control limits of the individual standard. Useall SRB HT Iodine Standards for standardization
5、 of iodine testing (see Section 8) when target values cannot be obtained.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its
6、 use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice fo
7、r Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD4821 Guide for Carbon BlackValidation of Test Method Precision and Bias3. Summary of Test Methods3.1 In Test Method A, a weighed sample of ca
8、rbon black is treated with a portion of standard iodine solution and the mixtureshaken and centrifuged. The excess iodine is then titrated with standard sodium thiosulfate solution, and the adsorbed iodine isexpressed as a fraction of the total mass of black.3.2 In Test Method B, a weighed sample of
9、 carbon black is treated with a portion of standard iodine solution using an automatedsample processor where the mixture is stirred, settled and aliquoted for automatic titration. The excess iodine is titrated withstandard sodium thiosulfate solution, and the adsorbed iodine is expressed as a fracti
10、on of the total mass of black.4. Significance and Use4.1 The iodine adsorption number is useful in characterizing carbon blacks. It is related to the surface area of carbon blacks andis generally in agreement with nitrogen surface area. The presence of volatiles, surface porosity, or extractables wi
11、ll influence theiodine adsorption number. Aging of carbon black can also influence the iodine number.5. Apparatus5.1 Vials, glass, optically clear type, with polyethylene stoppers, 45 cm3.5.2 Gravity Convection Drying Oven, capable of maintaining 125 6 5C.1 This test method is under the jurisdiction
12、 of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black SurfaceArea and Related Properties.Current edition approved May 1, 2011June 1, 2012. Published June 2011August 2012. Originally approved in 1957. Last previous edition approved in 2011 asD1
13、510 11.D1510 11a. DOI: 10.1520/D1510-11A.10.1520/D1510-12.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.
14、This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior edi
15、tions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Buret, either of the following may be used:5
16、.3.1 Digital Buret, 25-cm3 capacity, with 0.01-cm3 increment counter and zero reset control, or5.3.2 Buret, glass 25-cm3, Class A, side-arm filling, graduated in 0.05 cm3 and with automatic zero.5.4 Repetitive Dispenser, 25-cm3 capacity, 60.1% reproducibility and calibrated to within 60.03-cm3 accur
17、acy.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-cm3 with standard taper stopper.5.8 Funnel, large diameter, with standard taper joint to fit the 2000-cm3 flask.5.9 Glass Bottle, amber, 2000-cm3, with standar
18、d taper stopper.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 equipment necessary to carry out the test as written.5.15 Mechanical Shak
19、er, with at least 1 in. stroke length and a minimum of 240 strokes/min.5.16 Automatic Titrator.5.17 Redox Electrode, combined platinum ring electrode with an Ag/AgCl/KCl reference electrode and a ceramic frit.5.18 Volumetric Flask, 500 cm3 with standard taper stopper.5.19 Flask, 250 cm3 with ground
20、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 chemicals shall be of reagent grade.6.2 The preparation of the solutions listed below is described in Annex A1. Pre-mixe
21、d 0.04728 N iodine solution and 0.0394N sodium thiosulfate may be purchased from commercial sources. It is recommended that the normality of pre-mixed solutionsbe 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
22、 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 standard) per dm3. (WarningPotassium dichromate is carcinogenic
23、.)6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/dm3 (0.0394 N), containing 5 cm3 n-amyl alcohol per dm3.6.7 Sulfuric Acid, 10 %.6.8 Soluble Starch Solution, 1 %, containing 0.02 g salicylic acid per dm3.6.9 Deionized Water.7. Standardization of Solutions7.1 Sodium Thiosulfate, 0.0394 N (6
24、0.00008):7.1.1 Use potassium dichromate solution as follows:7.1.1.1 Measure approximately 20 cm3 of 10 % potassium iodide (see A1.4) solution into a small graduated cylinder andtransfer to a 250 cm3 iodine flask with a ground glass stopper.7.1.1.2 Measure approximately 20 cm3 of 10 % sulfuric acid s
25、olution (see A1.5) into a small graduated cylinder and add to theKI solution in the iodine flask. The mixture should remain colorless.NOTE 1If a yellow color should develop, discard this KI solution.7.1.1.3 Using a 20 cm3 pipet, transfer 20 cm3 of standard 0.0394 N potassium dichromate solution (see
26、 A1.8) into the 250 cm3iodine flask, replace stopper, swirl, and place in the dark for 15 min.3 The sole source of supply of the apparatus known to the committee at this time is Brinkmann Instruments, Inc., One Cantiague Rd., PO Box 1019, Westbury, NY11590-0207. The sole source of supply of the filt
27、er (disposable filter part #17594 K 5 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 are aware of alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Yo
28、ur comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.D1510 1227.1.1.4 Titrate the contents of the iodine flask against the new sodium thiosulfate solution following 7.1.3 or 7.1.4.7.1.2 Use potassium iodate/iodide solution as follo
29、ws:7.1.2.1 Pipet exactly 20 cm3 of 0.0394 N potassium iodate/iodide solution into a 250-cm3 iodine flask.7.1.2.2 Measure approximately 5 cm3 of 10 % sulfuric acid into a small graduated cylinder and add to the iodate/iodide solution.7.1.2.3 Cap immediately and mix thoroughly.7.1.2.4 Titrate the cont
30、ents of the iodine flask against the new 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 reservoir with unstandardized sodium thiosulfate solution, and flush the inletand delivery tubes.7.1.3.2 Change to the titrate mod
31、e and zero the counter.7.1.3.3 Add sodium thiosulfate until the contents of the iodine flask are a pale yellowish (potassium iodate) or paleyellowish-green (potassium dichromate). Wash the buret tip and the walls of the flask with water.7.1.3.4 Add 5 drops of starch solution to the flask.7.1.3.5 Con
32、tinue adding sodium thiosulfate dropwise until the blue or blue-violet color almost disappears.7.1.3.6 Wash the tip and walls of the flask with water, then advance the counter in 0.01-cm3 increments. Continue this sequenceuntil the endpoint is reached, indicated by a colorless (potassium iodate) or
33、sea-green (potassium dichromate) solution.7.1.3.7 Record the titration value and repeat from 7.1.1 or 7.1.2 for a duplicate determination.7.1.3.8 Calculate the normality of the sodium thiosulfate solution as in 7.1.5 and proceed as in 7.1.6. If the titration is made tostandardize the iodine solution
34、 as described in 7.2 calculate the normality of the iodine solution as in 7.2.1.2 and proceed as in7.2.1.3.7.1.4 Glass Buret:7.1.4.1 Using a conventional glass buret, fill the buret with unstandardized sodium-thiosulfate solution and flush 2 to 3 cm3through the tip.7.1.4.2 Adjust to the mark and tit
35、rate to a pale yellowish (potassium iodate) or pale yellowish-green (potassium dichromate).7.1.4.3 Wash the buret tip and the walls of the flask with water.7.1.4.4 Add 5 drops of starch solution to the iodine flask.7.1.4.5 Continue adding sodium thiosulfate dropwise until the endpoint is reached, in
36、dicated by a colorless (potassium iodate)or sea-green (potassium dichromate) solution.7.1.4.6 Record the titration value to the nearest 0.025 cm3 and repeat from 7.1.1 or 7.1.2 for a duplicate determination.NOTE 2To achieve maximum performance from a glass buret, it is necessary to use a small magni
37、fier and to read to the nearest 0.025 cm3.7.1.4.7 Calculate the normality of the sodium thiosulfate solution as in 7.1.5 and proceed as in 7.1.6. If the titration is made tostandardize the iodine solution as described in 7.2 calculate the normality of the iodine solution as in 7.2.1.2 and proceed as
38、 in7.2.1.3.7.1.5 Calculate the normality of the sodium thiosulfate solutions as follows:N 520 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 the following manner: if the solution is too strong, add water (2.5cm3/dm3 solution f
39、or each 0.0001 N over 0.0394); if the solution is too weak, add solid sodium thiosulfate (0.025 g/dm3 for each0.0001 N under 0.0394).7.2 Iodine Solution 0.04728 N (60.00003)This solution may be standardized against the secondary standard sodium-thiosulfate solution (see A1.3) standardized as in 7.1.
40、7.2.1 Use sodium thiosulfate solution as follows:7.2.1.1 Pipet exactly 20 cm3 of iodine solution into a 250-cm3 iodine flask and cap. Continue as in 7.1.3 or 7.1.4.7.2.1.2 Calculate the normality of the iodine solution as follows:N 50.0394! T/20 (2)where:N = normality, andT = cm3 of 0.0394 N sodium
41、thiosulfate solution.7.2.1.3 If N is not equal to 0.04728 N, adjust solution in the following manner: if the solution is too concentrated, add water(2.1 cm3/dm3 for each 0.0001 N over 0.04728); if the solution is too diluted, add iodine (12.7 mg/dm3 for each 0.0001 N under0.04728). (This iodine may
42、be more conveniently dispensed from a concentrated solution.)D1510 1238. Normalization Using SRB HT Iodine Standards8.1 When a laboratory cannot obtain target values for all three SRB HT Iodine Standards within established x-chart tolerances,the user should review recommendations found in Guide D482
43、1. If any one of the three SRB HT Iodine Standards is still outsideacceptable tolerances, the method described in 8.2-8.5 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 of the SRB HT Iod
44、ine Standards (y value) and the individual measuredvalue (x value).8.4 Normalize the values of all subsequent test results using this regression equation:Normalized value5measured value3slope!1y 2intercept (3)8.5 Alternatively, a table of numbers may be generated based on the regression equation to
45、find the correspondence betweena measured value and a normalized value.8.6 Reevaluate the need for normalization whenever replacement 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 Practices D1799 and
46、 D1900.10. Method A10.1 Dry an adequate sample of carbon black for 1 h, in a gravity-convection oven set at 125C , in an open container of suitabledimensions, so that the depth of the black is no more than 10 mm. Cool to room temperature in a desiccator before use.Blank IodineDetermination:10.1.1 Ma
47、ke a blank iodine determination by pipeting 20 cm3 or dispensing 25 cm3 of 0.04728 N iodine solution into a 125-cm3Erlenmeyer flask and titrating with 0.0394 N sodium thiosulfate as in 10.3.1, 10.3.2, or 10.3.3.10.1.2 A 25-cm3 blank must be multiplied by 0.8 for use in the formula of 12.1.10.1.3 Mak
48、e a duplicate blank determination and use the average of the two in the calculations.NOTE 3A duplicate blank determination need be run only once each day, unless new solutions are introduced during the day.10.1.4 If both solutions are within acceptable limits, the blank will measure 24.00 6 0.06 cm3
49、. If not, the normalities of oneor both solutions should be rechecked. If, after the recheck of solutions, normalities are still outside the acceptable limits refer to7.2.1.3 to adjust iodine solution.10.2 Weigh a mass of the dried sample into a glass vial as shown by the following table. All masses must be to the nearest 0.001g in case of iodine numbers from 0 to 520.9 and to the nearest 0.0001 g in case of iodine numbers from 521.0 and above.SamplePreparation and Iodine Determination:Iodine Number Sample Mass (g) Ratio I2: Sample Mass0130.9 0.500 50:1131.02
