NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.

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Designation: D 1510 – 08

Standard Test Method for

Carbon Black—Iodine Adsorption Number1
This standard is issued under the fixed designation D 1510; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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. Scope sodium thiosulfate solution, and the adsorbed iodine is ex-

1.1 This test method covers the determination of the iodine pressed as a fraction of the total mass of black.
adsorption number of carbon black. 4. Significance and Use
1.2 The iodine adsorption number of carbon black has been
shown to decrease with sample aging. New SRB HT Iodine 4.1 The iodine adsorption number is useful in characterizing
Standards have been produced that exhibit stable iodine carbon blacks. It is related to the surface area of carbon blacks
number upon aging. These SRB HT Iodine Standards are and is generally in agreement with nitrogen surface area. The
recommended for daily monitoring (x-charts) of testing and for presence of volatiles, surface porosity, or extractables will
standardization of iodine testing (see Section 8) when target influence the iodine adsorption number. Aging of carbon black
values cannot be obtained. can also influence the iodine number.
1.3 5. Apparatus
1.4 This standard does not purport to address all of the
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safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 Vials, glass, optically clear type, with polyethylene
stoppers, 45 cm3.

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priate safety and health practices and determine the applica- 5.2 Gravity Convection Drying Oven, capable of maintain-
bility of regulatory limitations prior to use. ing 125 6 5°C.
5.3 Buret, either of the following may be used:
2. Referenced Documents
2.1 ASTM Standards: 2
Document Preview 5.3.1 Digital Buret, 25-cm3 capacity, with 0.01-cm3 incre-
ment counter and zero reset control, or
D 1799 Practice for Carbon Black—Sampling Packaged 5.3.2 Buret, glass 25-cm3, Class A, side-arm filling, gradu-
Shipments ated in 0.05 cm3 and with automatic zero.
ASTM D1510-08
D 1900 Practice for Carbon Black—Sampling Bulk Ship- 5.4 Repetitive Dispenser, 25-cm3 capacity, 60.1% repro-
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ducibility and calibrated to within 60.03-cm3 accuracy.
ments
D 4483 Practice for Evaluating Precision for Test Method 5.5 Balance, analytical, with 0.1-mg sensitivity.
Standards in the Rubber and Carbon Black Manufacturing 5.6 Centrifuge, with minimum speed of 105 rad/s (1000 r/
Industries min).
D 4821 Guide for Carbon Black—Validation of Test 5.7 Volumetric Flask, 2000-cm3 with standard taper stopper.
Method Precision and Bias 5.8 Funnel, large diameter, with standard taper joint to fit
the 2000-cm3 flask.
3. Summary of Test Method 5.9 Glass Bottle, amber, 2000-cm3, with standard taper
3.1 A weighed sample of carbon black is treated with a stopper.
portion of standard iodine solution and the mixture shaken and 5.10 Glass Jug, approximate capacity 20-dm3.
centrifuged. The excess iodine is then titrated with standard 5.11 Stirrer, approximately 300 by 300 mm for mixing.
5.12 Stirrer, approximately 100 by 100 mm for titrating.
5.13 Desiccator.
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon 5.14 Miscellaneous Class A Glassware, and equipment
Black and is the direct responsibility of Subcommittee D24.21 on Carbon Black
Surface Area and Related Properties.
necessary to carry out the test as written.
Current edition approved Jan. 15, 2008. Published February 2008. Originally 5.15 Mechanical Shaker, with at least 1 in. stroke length and
approved in 1957. Last previous edition approved in 2007 as D 1510 – 07a. a minimum of 240 strokes/min.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.16 Automatic Titrator.
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 5.17 Redox Electrode, combined platinum ring electrode
the ASTM website. with an Ag/AgCl/KCl reference electrode and a ceramic frit.

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 D 1510 – 08
5.18 Volumetric Flask, 500 cm3 with standard taper stopper. 7.2.6.3 Add sodium thiosulfate until the contents of the
5.19 Flask, 250 cm3 with ground glass stopper. iodine flask is a pale yellowish-green. Wash the buret tip and
the walls of the flask with water.
6. Reagents and Solutions 7.2.6.4 Add 5 drops of starch solution to the flask.
6.1 Purity of Reagents—Unless otherwise stated, all chemi- 7.2.6.5 Continue adding sodium thiosulfate dropwise until
cals shall be of reagent grade. the blue or blue-violet color almost disappears.
6.2 The preparation of the solutions listed below is de- 7.2.6.6 Wash the tip and walls of the flask with water, then
scribed in Annex A1. Pre-mixed 0.0473 N iodine solution and advance the counter in 0.01-cm3 increments. Continue this
0.0394 N sodium thiosulfate may be purchased from commer- sequence until the endpoint is reached, indicated by a colorless
cial sources. It is recommended that the normality of pre-mixed (potassium iodate) or sea-green (potassium dichromate) solu-
solutions be verified before use. tion.
6.3 Iodine Solution, c(I2) = 0.02364 mol/dm3 (0.0473 N), 7.2.6.7 Record the titration value and repeat from 7.2.2 for
containing 57.0 g potassium iodide Kl per dm3. a duplicate determination.
6.4 Potassium Iodate Solution, c(KIO3) = 0.00657 mol/ 7.2.6.8 Calculate the normality of the sodium thiosulfate
dm3 (0.0394 N) containing 45.0 g potassium iodide per dm3. solutions as follows:
6.5 Potassium Dichromate Solution, c(K 2 Cr 2 O 7 ) = 20~0.0394!
0.006567 (0.0394 N), containing 1.932 g potassium dichromate N 5 T (1)
(certified/traceable primary standard) per dm3. (Warning—
Potassium dichromate is carcinogenic.) where:
6.6 Sodium Thiosulfate Solution, c(Na2S2O3) = 0.0394 mol/ N = normality, and
dm3 (0.0394 N), containing 5 cm3 n-amyl alcohol per dm3. T = titration volume, cm3.
6.7 Sulfuric Acid, 10 %. 7.2.6.9 If N is not equal to 0.0394, adjust the solution in the
6.8 Soluble Starch Solution, 1 %, containing 0.02 g salicylic following manner: if the solution is too strong, add water (2.5
acid per dm3. cm3/dm3 solution for each 0.0001 N over 0.0394); if the
solution is too weak, add solid sodium thiosulfate (0.025 g/dm3
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6.9 Water.
for each 0.0001 N under 0.0394).
7. Standardization of Solutions 7.2.7 Glass Buret:

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7.1 Sodium Thiosulfate, 0.0394 N (60.00008):
7.1.1 Use potassium dichromate solution as follows:
7.2.7.1 Using a conventional glass buret, fill the buret with
unstandardized sodium-thiosulfate solution and flush 2 to
3 cm3 through the tip.
Document Preview
7.1.2 Measure approximately 20 cm3 of 10 % potassium
iodide (see A1.4) solution into a small graduated cylinder and 7.2.7.2 Adjust to the mark and titrate to a pale yellowish-
green endpoint.
transfer to a 250 cm3 iodine flask with a ground glass stopper.
7.1.3 Measure approximately 20 cm3 of 10 % sulfuric acid NOTE 2—To achieve maximum performance from a glass buret, it is
solution (see A1.5) into a small graduated cylinder andASTM add to D1510-08
necessary to use a small magnifier and to read to the nearest 0.025 cm3.
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solution in the iodine flask. The mixture should remain
7.2.7.3 Wash the buret tip and the walls of the flask with
colorless.
water.
NOTE 1—If a yellow color should develop, discard this KI solution. 7.2.7.4 Add 5 drops of starch solution to the iodine flask.
7.1.4 Using a 20 cm3 pipet, transfer 20 cm3 of standard 7.2.7.5 Continue adding sodium thiosulfate dropwise until
0.0394 N potassium dichromate solution (see A1.8) into the the endpoint is reached, indicated by a colorless (potassium
250 cm3 iodine flask, replace stopper, swirl, and place in the iodate) or sea-green (potassium dichromate) solution.
dark for 15 min. 7.2.7.6 Record the titration value to the nearest 0.025 cm3
7.1.5 Titrate the contents of the iodine flask against the new and repeat from 7.2.7.1 for a duplicate determination.
sodium thiosulfate solution following 7.2.6 and 7.2.7. 7.2.7.7 Calculate the normality of the sodium thiosulfate
7.2 Sodium Thiosulfate, 0.0394 N (60.00008): solution as in 7.2.6.8.
7.2.1 Use potassium iodate/iodide solution as follows: 7.3 Iodine Solution 0.0473 N (60.00003)—This solution
7.2.2 Pipet exactly 20 cm3 of 0.0394 N potassium iodate/ may be standardized against the secondary standard sodium-
iodide solution into a 250-cm3 iodine flask. thiosulfate solution (see A1.3) standardized as in 7.2.
3
7.2.3 Measure approximately 5 cm of 10 % sulfuric acid 7.3.1 Use sodium thiosulfate solution as follows:
into a small graduated cylinder and add to the iodate/iodide 7.3.1.1 Pipet exactly 20 cm3 of iodine solution into a
solution. 250-cm3 iodine flask and cap. Continue as in 7.2.6 or 7.2.7.
7.2.4 Cap immediately and mix thoroughly. 7.3.1.2 Calculate the normality of the iodine solution as
7.2.5 Titrate the contents of the iodine flask against the new follows:
sodium thiosulfate solution following 7.2.6 and 7.2.7. ~0.0394!T
7.2.6 Digital Buret: N 5 20 (2)
7.2.6.1 Switch the digital buret to fill mode, fill the reservoir
with unstandardized sodium thiosulfate solution, and flush the where:
inlet and delivery tubes. N = normality, and
7.2.6.2 Change to the titrate mode and zero the counter. T = cm3 of 0.0394 N sodium thiosulfate solution.

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 D 1510 – 08
7.3.1.3 If N is not equal to 0.0473 N, adjust solution in the given by the table in 10.2. The sample mass must be kept to
following manner: if the solution is too concentrated, add water 1.0000 g maximum. Should the sample mass and correspond-
(2.1 cm3/dm3 for each 0.0001 N over 0.0473); if the solution is ing volume of iodine solution be increased, then a glass vial
too diluted, add iodine (12.7 mg/dm3 for each 0.0001 N under with a volume that is at least two times the amount of iodine
0.0473). (This iodine may be more conveniently dispensed solution used for the test should be used in order to preserve the
from a concentrated solution.) efficiency of the shaking.
10.3 Pipet (or dispense from a calibrated repetitive dis-
8. Normalization Using SRB HT Iodine Standards penser) 25 cm3 of 0.0473 N I2 solution into the glass vial
8.1 When a laboratory cannot obtain target values for all containing the sample and cap immediately.
three SRB HT Iodine Standards within established x-chart 10.4 Secure the vial in the mechanical shaker and shake for
tolerances, the user should review recommendations found in 1 min at a minimum of 240 strokes/min.
Guide D 4821. If any one of the three SRB HT Iodine 10.5 Centrifuge immediately for 1 min for pelleted black
Standards is still outside acceptable tolerances, the method and 3 min for loose black.
described in 8.2-8.5 should be used to standardize all test 10.6 Decant immediately. If more than one sample is being
results. analyzed, the solution should be decanted into small flasks or
8.2 Test the three ASTM HT Iodine Standards in duplicate clean, dry vials and capped immediately.
to establish the average measured value. Additional values are 10.7 Pipet 20 cm3 of solution into a 250-cm3 Erlenmeyer
added periodically, typically on a daily or weekly basis or flask and titrate with standard 0.0394 N sodium thiosulfate
when solutions are changed. A rolling average can be calcu- solution using either the digital or glass buret as follows:
lated from the latest four results. 10.7.1 Using a Digital Buret:
8.3 Perform a regression analysis using the standard value 10.7.1.1 Switch to the fill mode, fill the buret reservoir with
of the standard (y value) and the rolling average of the solution, and flush the inlet and delivery tubes.
measured value (x value). 10.7.1.2 Change to the titrate mode, zero the counter, and
8.4 Normalize the values of all subsequent samples using clean the tip with tissue.

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this regression equation: 10.7.1.3 Add sodium thiosulfate until the solution is pale
Normalized value 5 ~measured value 3 slope! 1 y2intercept (3) yellow. Wash the buret tip and walls of the flask with water.
10.7.1.4 Add 5 drops of starch solution.
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8.5 Alternatively, a table of numbers may be generated
based on the regression equation to find the correspondence
10.7.1.5 Continue adding sodium thiosulfate dropwise until
the blue or blue-violet color almost disappears.
between a measured value and a normalized value.

9. Sampling
Document Preview 10.7.1.6 Wash the tip and walls of the flask with water and
then advance the counter in 0.01-cm3 increments. Continue this
sequence until the endpoint is reached as indicated by a
9.1 Samples shall be taken in accordance with Practices colorless solution.
D 1799 and D 1900. ASTM D1510-08
10.7.1.7 Record the buret reading to the nearest 0.01 cm3.
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10. Test Procedure
10.7.1.8 Make a blank iodine determination by pipeting
20 cm3 or dispensing 25 cm3 of 0.0473 N iodine solution into
10.1 Dry an adequate sample of carbon black for 1 h, in a a 125-cm3 Erlenmeyer flask and titrating with 0.0394 N sodium
gravity-convection oven set at 125°C , in an open container of thiosulfate as in 10.7.1 or 10.7.2.
suitable dimensions, so that the depth of the black is no more 10.7.1.9 A 25-cm3 blank must be multiplied by 0.8 for use
than 10 mm. Cool to room temperature in a desiccator before in the formula of 11.1.
use. 10.7.1.10 Make a duplicate blank determination and use the
10.2 Weigh a mass of the dried sample into a glass vial as average of the two in the calculations.
shown by the following table. All masses must be to the nearest
0.0001 g. NOTE 4—A duplicate blank determination need be run only once each
day, unless new solutions are introduced during the day.
Iodine Number Sample Mass (g) Ratio I2: Sample Mass
0–130.9 0.5000 50:1 10.7.1.11 If both solutions are within acceptable limits, the
131.0–280.9 0.2500 100:1
281.0–520.9 0.1250 200:1
blank will measure 24.00 6 0.05 cm3. If not, the normalities of
521.0 and above 0.0625 400:1 one or both solutions should be rechecked.
10.7.2 Using a Conventional Glass Buret:
10.2.1 Use the sample mass determined by the expected
10.7.2.1 Clean the tip with a tissue. Add sodium thiosulfate
iodine number. If the result falls either above or below the
until the solution is pale yellow. Wash the buret tip and walls
range shown for that sample size, retest using the sample mass
of the flask with water.
specified in 10.2 for the range into which it has fallen.
10.7.2.2 Add 5 drops of starch solution.
NOTE 3—Unagitated, unpelleted carbon black may be densified, if 10.7.2.3 Continue adding sodium thiosulfate dropwise until
desired, before drying, prior to weighing. the endpoint is reached as indicated by a colorless solution.
10.2.2 The sample mass table given in 10.2 pertains to the 10.7.2.4 Record the titration volume to the nearest 0.25 cm3.
25 cm3 iodine solution as given in 10.3. Different volumes of 10.7.2.5 Make blank determinations as in 10.7.1.8,
iodine solution and of sample masses are permissible only if 10.7.1.10, and 10.7.1.11.
the iodine solution to sample mass ratio is kept the same as that 10.7.3 Using an Auto-titrator: