1、Designation: D1510 16D1510 16aStandard 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 numb
2、er 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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination of the iodi
3、ne adsorption 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 Iodi
4、neStandards 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 standardiza
5、tion 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
6、 its 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 Practic
7、e for 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 BiasE969 Specification for Glass Volumetric (Transfer) Pipets2.2 Europ
8、ean 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 is treated with a portion of standard iodine solution and the mixtureshaken and centrifuged. The excess iodine is then titra
9、ted 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 carbon black is treated with a portion of standard iodine solution using an automatedsample processor where the mixture is stirred, se
10、ttled and aliquoted for automatic titration. The excess iodine is titrated withstandard sodium thiosulfate solution, and the adsorbed iodine is expressed as a fraction of the total mass of black.4. Significance and Use4.1 The iodine adsorption number is useful in characterizing carbon blacks. It is
11、related to the surface area of carbon blacks andis generally in agreement with nitrogen surface area. The presence of volatiles, surface porosity, or extractables will influence theiodine adsorption number. Aging of carbon black can also influence the iodine number.1 This test method is under the ju
12、risdiction 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 Jan. 1, 2016Nov. 1, 2016. Published February 2016November 2016. Originally approved in 1957. Last previous edition appr
13、oved in 20132016as D1510 13.D1510 16. DOI: 10.1520/D1510-16.10.1520/D1510-16A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on
14、the ASTM website.3 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes
15、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 editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official
16、document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Vials, glass, optically clear type, with polyethylene stoppers, 45 cm3.5.2 Gravity Convection Drying Oven, capable of maintaining 125 6 5C.5.3 Buret, either of t
17、he following may be used:5.3.1 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
18、 to within 60.03-cm3 accuracy.5.5 Balance, analytical, with 0.1-mg sensitivity.5.6 Centrifuge, with minimum speed of 105 rad/s (1000 rmin).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, ambe
19、r, 2000-cm3, with standard 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 wri
20、tten.5.15 Mechanical Shaker, 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 Fl
21、ask, 250 cm3 with 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 chemicals shall be of reagent grade.6.2 The preparation of the solutions listed below is descri
22、bed in Annex A1. Pre-mixed 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
23、 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 mol/cm3 (0.0394 N), containing 1.932 g potassium dichromate(certified/traceable primary standard) per dm3. (WarningPota
24、ssium dichromate is carcinogenic.)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
25、 Sodium Thiosulfate, 0.0394 N (60.00008):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.4 The sole source of supply
26、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 filter (disposable filter part #17594 K 5 m Minisart with luer lock outlet) known to the committee at this time is SartoriusSt
27、edim North America Inc., 131 Heartland Blvd., Edgewood, NY 11717. If you are aware of alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.
28、D1510 16a27.1.1.2 Measure approximately 20 cm3 of 10 % sulfuric acid solution (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, t
29、ransfer 20 cm3 of standard 0.0394 N potassium dichromate solution (see A1.8) into the 250 cm3iodine flask, replace stopper, swirl, and place in the dark for 15 min.7.1.1.4 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 potassiu
30、m iodate/iodide solution as follows: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 th
31、oroughly.7.1.2.4 Titrate the contents 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.
32、7.1.3.2 Change to the titrate mode 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
33、solution to the flask.7.1.3.5 Continue 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
34、 colorless (potassium iodate) or 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
35、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 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
36、.1.4.2 Adjust to the mark and titrate 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
37、until the endpoint is reached, indicated 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
38、is necessary to use a small magnifier 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 solu
39、tion as in 7.2.1.2 and proceed as 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,
40、 add water (2.5 cm3water per dm3 sodium thiosulfate solution for each 0.0001 N over 0.0394); if the solution is too weak, add solid sodium thiosulfate(0.025 g solid sodium thiosulfate per dm3 sodium thiosulfate solution for each 0.0001 N under 0.0394).7.2 Iodine Solution 0.04728 N (60.00003)This sol
41、ution may 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 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
42、 the normality of the iodine solution as follows:N 50.0394!T/20 (2)where:N = normality, andD1510 16a3T = cm3 of 0.0394 N sodium 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 water per dm3 i
43、odine solution for each 0.0001 N over 0.04728); if the solution is too diluted, add iodine (12.7 mg iodineper dm3 iodine solution for each 0.0001 N under 0.04728). (This iodine may be more conveniently dispensed from a concentratedsolution.)8. Normalization Using SRB HT Iodine Standards8.1 When a la
44、boratory cannot obtain target values for all three SRB HT Iodine Standards within established x-chart tolerances,the user should review recommendations found in Guide D4821. If any one of the three SRB HT Iodine Standards is still outsideacceptable tolerances, the method described in 8.2 8.5 should
45、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 Iodine Standards (y value) and the individual measuredvalue (x value).8.4 Normalize the values of all subsequent test results using
46、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 find the correspondence betweena measured value and a normalized value.8.6 Reevaluate the need for normalization whenever replace
47、ment 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 D1900.10. Blank Iodine Determination10.1 Method ABlank Iodine Determination:10.1.1 Make a blank iodine determination by pipeting
48、 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 11.10.1, 11.10.2, or 11.10.3.10.1.2 A 25-cm3 blank must be multiplied by 0.8 for use in the formula of 13.1.10.1.3 Make a duplicate blank determination and us
49、e 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 0.09 cm3. 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. See Table 1 for blank tolerance components.10.1.5 The blank tolerance for a 20 cm3 volume of iodine s
