1、Designation: D 1510 07Standard 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 p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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.1.1.1 Procedure A is the original procedure for this deter-mination.1.1.2 Procedure B specifies an increased sample mass ofcarbon black and volume of iodine solution (the ratio is thesame as in Procedure A) which results in a simplified formulafor the calculation of the iodi
4、ne number.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 and forstandardiz
5、ation of iodine testing (see Section 8) when targetvalues cannot be obtained.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with i
6、ts 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 PackagedShipmentsD 1900 Pract
7、ice 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 carbon black is
8、 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 adsorption numbe
9、r 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 influence the
10、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 and zero reset
11、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, with minimum spe
12、ed 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, approximately 3
13、00 by 300 mm for mixing.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 Related Properties.Current edition approved July 1, 2007. Published July 2007. Originally approvedin 1957.
14、Last previous edition approved in 2006 as D 1510 06a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyrig
15、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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, wit
16、h 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 Flask, 500 cm3with standard taper stopper.6. Reagents and Solutions6.1 Purity of Rea
17、gentsUnless 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 commer-cial sources. It is recommended that the normality of pre
18、-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 iodide per dm3.6.5 Potassium Dichromate Solution,c(K2Cr2O7)=0.006
19、567 (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-amyl alcohol per dm3.6.7 Sulfuric Acid,10%.6.8 Soluble Starch
20、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 % potassiumiodide (see A1.4) solution into a small graduated cylinder
21、 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 should remaincolorless.NOTE 1If a yellow color should develop, disca
22、rd 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 the iodine flask against the newsodium thiosulfate solution fo
23、llowing 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 approximately 5 cm3of 10 % sulfuric acidinto a small graduated cyl
24、inder 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 the digital buret to fill mode, fill the reservoirwith unstandard
25、ized 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 buret tip andthe walls of the flask with water.7.2.6.4 Add 5 drops
26、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-cm3increments. Continue thissequence until the endpoint is reached, indicat
27、ed 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 follows:N 5200.0394!T(1)where:N = normality, andT = titration
28、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 thiosulfate (0.025 g/dm3for each 0.0001 N under 0.0394).7.2.7 Glass B
29、uret: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 maximum performance from a glass buret, it isnecessary to use a sm
30、all 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 endpoint is reached, indicated by a colorless (potassiumiodate) o
31、r 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 7.2.6.8.7.3 Iodine Solution 0.0473 N (60.00003)This solutionmay be stan
32、dardized 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. Continue as in 7.2.6 or 7.2.7.D15100727.3.1.2 Calculate the normali
33、ty of the iodine solution asfollows:N 50.0394!T20(2)where:N = normality, andT =cm3of 0.0394 N sodium thiosulfate solution.7.3.1.3 If N is not equal to 0.0473 N, adjust solution in thefollowing manner: if the solution is too concentrated, add water(2.1 cm3/dm3for each 0.0001 N over 0.0473); if the so
34、lution 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. Standardization Using SRB HT Iodine Standards8.1 When a laboratory cannot obtain target values for allthree SRB HT Iodine Standards within esta
35、blished 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 all testresults.8.2 Test the three ASTM HT Iodine Standards in d
36、uplicateto 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 regression analysis using the standard valueof the standard (y
37、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 numbers may be generatedbased on the regression equation to find the
38、correspondencebetween a measured value and a normalized value.9. Sampling9.1 Samples shall be taken in accordance with PracticesD 1799 and D 1900.10. Procedure 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,
39、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.Iodine Number Sample Mass (g) Ratio I2: Sample Mass0130.9 0.5000 50
40、: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 using the sample massspecified in 10.2 for the range into which it has
41、 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 ofiodine solution and of sample masses are permissible only ifthe iodine
42、 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 vialwith proper capacity should be used in order to preserve theefficienc
43、y 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 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
44、 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 a 250-cm3Erlenmeyerflask and titrate with standard 0.039
45、4 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 reservoir withsolution, and flush the inlet and delivery tubes.10.7.1.2 Change to the titrate mode, zero the counter, andclean the tip with
46、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.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 wa
47、lls 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.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 2
48、5 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 multiplied 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 calcu
49、lations.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 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:D151007310.7.2.1 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 thiosulfat
