1、Designation: D 1510 09bStandard 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.1.1.1 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
4、have been produced that exhibit stable iodinenumber upon aging. These SRB HT Iodine Standards arerecommended for daily monitoring (x-charts) of testing and forstandardization of iodine testing (see Section 8) when targetvalues cannot be obtained.1.3 The values stated in SI units are to be regarded a
5、sstandard. 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 theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the
6、 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carb
7、on Black ManufacturingIndustriesD 4821 Guide for Carbon BlackValidation of TestMethod Precision and Bias3. Summary of Test Methods3.1 In Test Method A, a weighed sample of carbon black istreated with a portion of standard iodine solution and themixture shaken and centrifuged. The excess iodine is th
8、entitrated 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 istreated with a portion of standard iodine solution using anautomated sample processor where the mixture is stirre
9、d,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 ofblack.4. Significance and Use4.1 The iodine adsorption number is useful in characterizingcarbon blacks. It is
10、 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 iodine number.5. Apparatus5.1 Vials, glass, optic
11、ally 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 control, or5.3.2 Buret, glass 25-cm3, Class A, si
12、de-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 speed of 105 rad/s (1000 r/min).1This test method is
13、 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 Sept. 1, 2009. Published September 2009. Originallyapproved in 1957. Last previous edition approved in 2009
14、 as D 1510 09a.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.1Copyright ASTM International, 100 Barr Harbor
15、 Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 capac
16、ity 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 equipmentnecessary to carry out the test as written.5.15 Mechanical Shaker, with at least 1 in. stroke length anda minimum
17、 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.5.19 Flask, 250 cm3with ground glass stopper.5.20 Automatic Sample Processor and Titr
18、ation 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 preparation of the solutions listed below is de-scribed in Annex A1. Pre-mixed 0.04728 N iodine solution and0.0394 N sodium thiosu
19、lfate 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(0.04728 N),containing 57.0 g potassium iodide Kl per dm3.6.4 Potassium Iodate Solution, c(KIO3) = 0.00657 mol/dm3(0.0394 N)
20、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.)6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/dm
21、3(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. Standardization of Solutions7.1 Sodium Thiosulfate, 0.0394 N (60.00008):7.1.1 Use potassium dichromate solution as follows:7.1.1.
22、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.7.1.1.2 Measure approximately 20 cm3of 10 % sulfuric acidsolution (see A1.5) into a small graduated cylinder and add tothe KI sol
23、ution 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 standard0.0394 N potassium dichromate solution (see A1.8) into the250 cm3iodine flask, replace stopper, swirl, and place in th
24、edark 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 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 Meas
25、ure 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 contents 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
26、 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 mode and zero the counter.7.1.3.3 Add sodium thiosulfate until the contents of theiodine flask are a pale yellowish (potassiu
27、m 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 Continue adding sodium thiosulfate dropwise untilthe blue or blue-violet color almost disappears.7.1.3.6 Wash the tip and walls
28、 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-green (potassium dichromate) solu-tion.7.1.3.7 Record the titration value and repeat from 7.1.1 or7.1.2 for a duplicate dete
29、rmination.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 described 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
30、.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 pale yellowish(potassium iodate) or pale yellowish-green (potassium dichro-mate).7.1.4.3 Wash the buret tip and the walls o
31、f 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 colorless (potassiumiodate) or sea-green (potassium dichromate) solution.3The sole source of supply of the apparatus known
32、 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 part #17594 K5 m Minisart with luer lock outlet) known to the committee at this time is SartoriusStedim North America Inc.,
33、 131 Heartland Blvd., Edgewood, NY 11717. If you areaware of alternative suppliers, please provide this information to ASTM Interna-tional Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.D 1510 09b27.1.4.6 Record
34、 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 to use a small magnifier and to read to the nearest 0.025 cm3.7.1.4.7 Calculate the normality of the sodium thiosulfatesol
35、ution 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 7.2.1.2 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
36、(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 (2.5cm3/dm3solution for each 0.0001 N over 0.0394); if thesolution is too weak, add solid sodium thiosulfate (0.025 g/dm3for ea
37、ch 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) standardized 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-cm
38、3iodine 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 N sodium thiosulfate solution.7.2.1.3 If N is not equal to 0.04728 N, adjust solution in thefollowing manner: if the solut
39、ion 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 may be more convenientlydispensed from a concentrated solution.)8. Normalization Using SRB HT Iodine Standards8.1 When a
40、laboratory cannot obtain 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
41、be used to normalize all test results.8.2 Test the three SRB HT Iodine Standards in duplicate toestablish 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
42、results.8.3 Perform a regression analysis using the target value ofthe SRB HT Iodine Standards (y value) and the rolling averageof the measured value (x value).8.4 Normalize the values of all subsequent test results usingthis regression equation:Normalized value 5measured value 3 slope!1 y2intercept
43、 (3)8.5 Alternatively, a table of numbers 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. Method A10.1 Dry an adequate sample of carbon b
44、lack 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 glass vial asshown by the following table.All masse
45、s 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 0.125 200:1521.0 and above 0.0625 400:110.2.1 Use th
46、e 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 carbon black may be densified, ifdesired, before dry
47、ing, 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 the same as thatgiven by the table in 10.2. The sa
48、mple 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 to preserve theefficiency of the shaking.10.3 Pip
49、et (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 a 250-cm3Erlenmeyerflask and titrate with standard
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