1、Designation: D 1510 08aStandard Test Method forCarbon BlackIodine Adsorption Number1This standard is issued under the fixed designation D 1510; 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
2、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 iodineadsorptio
3、n number of carbon black.1.2 The iodine adsorption number of carbon black has beenshown to decrease with sample aging. New SRB HT IodineStandards have been produced that exhibit stable iodinenumber upon aging. These SRB HT Iodine Standards arerecommended for daily monitoring (x-charts) of testing an
4、d forstandardization of iodine testing (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, ass
5、ociated with its use. It is theresponsibility 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:2D 1799 Practice for Carbon BlackSampling PackagedShipmen
6、tsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 4821 Guide for Carbon BlackValidation of TestMethod Precision and Bias3. Summary of Test Method3.1 A weighed sample of c
7、arbon black is treated with aportion of standard iodine solution and the mixture shaken andcentrifuged. The excess iodine is then titrated with standardsodium thiosulfate solution, and the adsorbed iodine is ex-pressed as a fraction of the total mass of black.4. Significance and Use4.1 The iodine ad
8、sorption 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 adsorption number. Aging of carbon blackcan also
9、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-cm3capacity, with 0.01-cm3incre-ment counter a
10、nd 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, analytical, with 0.1-mg sensitivity.5.6 Centrifuge, wi
11、th minimum speed of 105 rad/s (1000 r/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, a
12、pproximately 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 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 A
13、utomatic Titrator.5.17 Redox Electrode, combined platinum ring electrodewith an Ag/AgCl/KCl reference electrode and a ceramic frit.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
14、Related Properties.Current edition approved Aug. 1, 2008. Published September 2008. Originallyapproved in 1957. Last previous edition approved in 2008 as D 1510 08.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
15、k 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.5.18 Volumetric Flask, 500 cm3with standard taper stopper.5.19 Flask, 250 cm3with
16、ground glass stopper.6. Reagents and 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 Annex A1. Pre-mixed 0.0473 N iodine solution and0.0394 N sodium thiosulfate may be purchased from c
17、ommer-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(0.0473 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 io
18、dide 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.)6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/dm3(0.0394 N), containing 5 cm3n
19、-amyl alcohol per dm3.6.7 Sulfuric Acid,10%.6.8 Soluble Starch Solution, 1 %, containing 0.02 g salicylicacid per dm3.6.9 Water.7. Standardization of Solutions7.1 Sodium Thiosulfate, 0.0394 N (60.00008):7.1.1 Use potassium dichromate solution as follows:7.1.2 Measure approximately 20 cm3of 10 % pota
20、ssiumiodide (see A1.4) solution into a small graduated cylinder andtransfer to a 250 cm3iodine flask with a ground glass stopper.7.1.3 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 shoul
21、d remaincolorless.NOTE 1If a yellow color should develop, discard this KI solution.7.1.4 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.7.1.5 Titrate the contents of
22、 the iodine flask against the newsodium thiosulfate solution following 7.2.6 and 7.2.7.7.2 Sodium Thiosulfate, 0.0394 N (60.00008):7.2.1 Use potassium iodate/iodide solution as follows:7.2.2 Pipet exactly 20 cm3of 0.0394 N potassium iodate/iodide solution into a 250-cm3iodine flask.7.2.3 Measure app
23、roximately 5 cm3of 10 % sulfuric acidinto a small graduated cylinder and add to the iodate/iodidesolution.7.2.4 Cap immediately and mix thoroughly.7.2.5 Titrate the contents of the iodine flask against the newsodium thiosulfate solution following 7.2.6 and 7.2.7.7.2.6 Digital Buret:7.2.6.1 Switch th
24、e digital buret to fill mode, fill the reservoirwith unstandardized sodium thiosulfate solution, and flush theinlet and delivery tubes.7.2.6.2 Change to the titrate mode and zero the counter.7.2.6.3 Add sodium thiosulfate until the contents of theiodine flask is a pale yellowish-green. Wash the bure
25、t tip andthe walls of the flask with water.7.2.6.4 Add 5 drops of starch solution to the flask.7.2.6.5 Continue adding sodium thiosulfate dropwise untilthe blue or blue-violet color almost disappears.7.2.6.6 Wash the tip and walls of the flask with water, thenadvance the counter in 0.01-cm3increment
26、s. Continue thissequence until the endpoint is reached, indicated by a colorless(potassium iodate) or sea-green (potassium dichromate) solu-tion.7.2.6.7 Record the titration value and repeat from 7.2.2 fora duplicate determination.7.2.6.8 Calculate the normality of the sodium thiosulfatesolutions as
27、 follows:N 5200.0394!T(1)where:N = normality, andT = titration volume, cm3.7.2.6.9 If N is not equal to 0.0394, adjust the solution in thefollowing manner: if the solution is too strong, add water (2.5cm3/dm3solution for each 0.0001 N over 0.0394); if thesolution is too weak, add solid sodium thiosu
28、lfate (0.025 g/dm3for each 0.0001 N under 0.0394).7.2.7 Glass Buret:7.2.7.1 Using a conventional glass buret, fill the buret withunstandardized sodium-thiosulfate solution and flush 2 to3cm3through the tip.7.2.7.2 Adjust to the mark and titrate to a pale yellowish-green endpoint.NOTE 2To achieve max
29、imum performance from a glass buret, it isnecessary to use a small magnifier and to read to the nearest 0.025 cm3.7.2.7.3 Wash the buret tip and the walls of the flask withwater.7.2.7.4 Add 5 drops of starch solution to the iodine flask.7.2.7.5 Continue adding sodium thiosulfate dropwise untilthe en
30、dpoint is reached, indicated by a colorless (potassiumiodate) or sea-green (potassium dichromate) solution.7.2.7.6 Record the titration value to the nearest 0.025 cm3and repeat from 7.2.7.1 for a duplicate determination.7.2.7.7 Calculate the normality of the sodium thiosulfatesolution as in 7.2.6.8.
31、7.3 Iodine Solution 0.0473 N (60.00003)This solutionmay be standardized against the secondary standard sodium-thiosulfate solution (see A1.3) standardized as in 7.2.7.3.1 Use sodium thiosulfate solution as follows:7.3.1.1 Pipet exactly 20 cm3of iodine solution into a250-cm3iodine flask and cap. Cont
32、inue as in 7.2.6 or 7.2.7.7.3.1.2 Calculate the normality of the iodine solution asfollows:N 50.0394!T20(2)where:N = normality, andT =cm3of 0.0394 N sodium thiosulfate solution.D 1510 08a27.3.1.3 If N is not equal to 0.0473 N, adjust solution in thefollowing manner: if the solution is too concentrat
33、ed, add water(2.1 cm3/dm3for each 0.0001 N over 0.0473); if the solution istoo diluted, add iodine (12.7 mg/dm3for each 0.0001 N under0.0473). (This iodine may be more conveniently dispensedfrom a concentrated solution.)8. Normalization Using SRB HT Iodine Standards8.1 When a laboratory cannot obtai
34、n target values for allthree SRB HT Iodine Standards within established x-charttolerances, the user should review recommendations found inGuide D 4821. If any one of the three SRB HT IodineStandards is still outside acceptable tolerances, the methoddescribed in 8.2-8.5 should be used to standardize
35、all testresults.8.2 Test the three ASTM HT Iodine Standards in duplicateto establish the average measured value. Additional values areadded periodically, typically on a daily or weekly basis orwhen solutions are changed. A rolling average can be calcu-lated from the latest four results.8.3 Perform a
36、 regression analysis using the standard valueof the standard (y value) and the rolling average of themeasured value (x value).8.4 Normalize the values of all subsequent samples usingthis regression equation:Normalized value 5measured value 3 slope!1 y2intercept (3)8.5 Alternatively, a table of numbe
37、rs may be generatedbased on the regression equation to find the correspondencebetween a measured value and a normalized value.9. Sampling9.1 Samples shall be taken in accordance with PracticesD 1799 and D 1900.10. Test Procedure10.1 Dry an adequate sample of carbon black for 1 h, in agravity-convect
38、ion 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 glass vial asshown by the following table.All masses must be to the nearest0.0001 g.
39、Iodine Number Sample Mass (g) Ratio I2: Sample Mass0130.9 0.5000 50:1131.0280.9 0.2500 100:1281.0520.9 0.1250 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 usi
40、ng the sample massspecified in 10.2 for the range into which it has fallen.NOTE 3Unagitated, unpelleted carbon 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 ofiod
41、ine solution and of sample masses are permissible only ifthe iodine solution to sample mass ratio is kept the same as thatgiven by the table in 10.2. The sample mass must be kept to1.0000 g maximum. Should the sample mass and correspond-ing volume of iodine solution be increased, then a glass vialwi
42、th a volume that is at least two times the amount of iodinesolution used for the test should be used in order to preserve theefficiency of the shaking.10.3 Pipet (or dispense from a calibrated repetitive dis-penser) 25 cm3of 0.0473 N I2solution into the glass vialcontaining the sample and cap immedi
43、ately.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 flask
44、s orclean, dry vials and capped immediately.10.7 Pipet 20 cm3of solution into a 250-cm3Erlenmeyerflask and titrate with standard 0.0394 N sodium thiosulfatesolution using either the digital or glass buret as follows:10.7.1 Using a Digital Buret:10.7.1.1 Switch to the fill mode, fill the buret reserv
45、oir withsolution, and flush the inlet and delivery tubes.10.7.1.2 Change to the titrate mode, zero the counter, andclean the tip with tissue.10.7.1.3 Add sodium thiosulfate until the solution is paleyellow. Wash the buret tip and walls of the flask with water.10.7.1.4 Add 5 drops of starch solution.
46、10.7.1.5 Continue adding sodium thiosulfate dropwise untilthe blue or blue-violet color almost disappears.10.7.1.6 Wash the tip and walls of the flask with water andthen advance the counter in 0.01-cm3increments. Continue thissequence until the endpoint is reached as indicated by acolorless solution
47、.10.7.1.7 Record the buret reading to the nearest 0.01 cm3.10.7.1.8 Make a blank iodine determination by pipeting20 cm3or dispensing 25 cm3of 0.0473 N iodine solution intoa 125-cm3Erlenmeyer flask and titrating with 0.0394 N sodiumthiosulfate as in 10.7.1 or 10.7.2.10.7.1.9 A 25-cm3blank must be mul
48、tiplied by 0.8 for usein the formula of 11.1.10.7.1.10 Make a duplicate blank determination and use theaverage of the two in the calculations.NOTE 4A duplicate blank determination need be run only once eachday, unless new solutions are introduced during the day.10.7.1.11 If both solutions are within
49、 acceptable limits, theblank will measure 24.00 6 0.05 cm3. If not, the normalities ofone or both solutions should be rechecked.10.7.2 Using a Conventional Glass Buret:10.7.2.1 Clean the tip with a tissue. Add sodium thiosulfateuntil the solution is pale yellow. Wash the buret tip and wallsof the flask with water.10.7.2.2 Add 5 drops of starch solution.10.7.2.3 Continue adding sodium thiosulfate dropwise untilthe endpoint is reached as indicated by a colorless solution.10.7.2.4 Record the titration volume to the nearest 0.25 cm3.10.7.2.5 Make blank determinations
