ASTM D1618-99

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Designation: D 1618 – 99
Standard Test Method for
Carbon Black Extractables—Transmittance of Toluene
Extract
This standard is issued under the fixed designation D 1618; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope transmittance at a 425-nm wavelength. The instrument is to be
operated in accordance with the manufacturer’s directions for
1.1 This test method covers the measurement of the degree
optimum performance.
of toluene discoloration by carbon black extractables and is
5.2 Cuvets, rectangular, with an optical light path of 10 mm.
useful in controlling the reaction processes for production of
5.3 Balance, analytical, with a sensitivity of 60.01 g.
carbon black. This test method may not be applicable to carbon
5.4 Oven, gravity-convection type, capable temperature
blacks with high extractables.
regulation within 61°C at 125°C and temperature uniformity
1.2 The values stated in SI units are to be regarded as
within 65°C.
standard.
5.5 Pipet, automatic, bottle-type, 20 cm , with a repeatabil-
1.3 This standard does not purport to address all of the
ity of 60.1.
safety concerns, if any, associated with its use. It is the
5.6 Erlenmeyer Flasks, 125 cm with ground-glass stopper.
responsibility of the user of this standard to establish appro-
5.7 Filter Paper, qualitative grade, medium retention,
priate safety and health practices and determine the applica-
medium-fast filter speed, 150-mm diameter.
bility of regulatory limitations prior to use.
5.8 Glass Filtering Funnels, 75-mm inside diameter at the
2. Referenced Documents
top.
5.9 Beakers,50or100 cm , with pouring lips.
2.1 ASTM Standards:
5.10 Wiping Paper, lint-free.
D 1799 Practice for Carbon Black—Sampling Packaged
5.11 Cotton Swabs.
Shipments
5.12 Fume Hood, fully enclosed on three sides, with spark-
D 1900 Practice for Carbon Black—Sampling Bulk Ship-
proof fan and motor.
ments
5.13 Toluene, analytical reagent grade.
D 4483 Practice for Determining Precision for Test Method
Standards in the Rubber and Carbon Black Industries
6. Sampling
3. Terminology
6.1 Samples shall be taken in accordance with Practice
D 1799 or Practice D 1900.
3.1 Definition:
3.1.1 carbon black toluene discoloration, n— the transmit-
7. Standardization of Apparatus
tance, at 425 nm, of the filtrate obtained from the toluene
7.1 Turn on the spectrophotometer and allow it to warm for
extract of carbon black, compared to that of pure toluene.
the length of time specified by the manufacturer.
4. Significance and Use 7.2 Check the zero reading of the spectrophotometer in
accordance with the manufacturer’s instructions, and adjust if
4.1 The toluene discoloration value provides an estimate of
necessary.
toluene-soluble discoloring residues present on the carbon
7.3 Place the funnel with the filter paper into an Erlenmeyer
black.
flask. Filter approximately 30 cm of toluene into the flask and
5. Apparatus and Reagent
stopper the flask.
7.4 Pour a portion of the toluene into the beaker with the
5.1 Spectrophotometer, with tungsten filament lamp, 20-nm
pouring lip for simplifying the transfer of the toluene to the
maximum spectral bandpass, capable of measuring percent
cuvet.
7.5 Rinse the cuvet with the filtered toluene three times,
This test method is under the jurisdiction of ASTM Committee D-24 on Carbon
filling approximately one third full each time. Discard this
Black and is the direct responsibility of Subcommittee D 24.31 on Non-Carbon
rinsing toluene into an approved safety container.
Black Components of Carbon Black.
Current edition approved Aug. 10, 1999. Published September 1999. Originally
NOTE 1—The cuvet must be handled on the ground-glass sides only. Do
published as D 1618 – 65 T. Last previous edition D 1618 – 97.
not touch the smooth, clear sides with the fingers.
Annual Book of ASTM Standards, Vol. 09.01.
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D 1618
7.6 Fill the cuvet and wipe the outside surfaces with the without documentation that they are applicable to those par-
lint-free wiping paper while holding the cuvet in front of a ticular materials and the specific testing protocols of the test
suitable light source. The toluene must be free of any contami- method. Any appropriate value may be used from Table 1.
nants, such as lint particles, which might cause light scattering, 10.3 A type 1 inter-laboratory precision program was con-
thus influencing the test results. If necessary, rewipe the outside ducted as detailed in Table 2. Both repeatability and reproduc-
until perfectly clean, or clean the inside surfaces with a cotton ibility represent short term (daily) testing conditions. The
swab. Repeat 7.5 if the inside surfaces are cleaned. testing was performed using two operators in each laboratory
7.7 . Insert the cuvet into the spectrophotometer and adjust performing the test once on each of two days (total of four
it to read 100 % transmittance at the 425-nm wavelength. tests). A test result is the value obtained from a single
determination. Acceptable difference values were not mea-
8. Procedure sured. The between operator component of variation is in-
cluded in the calculated values for r and R.
8.1 Dry an adequate sample of carbon black at 125 6 1°C
10.4 The results of the precision calculations for this test are
for 60, + 5, − 0 min, using a gravity-convection oven.
given in Table 1. The materials are arranged in ascending
NOTE 2—An infrared lamp must not be used for drying samples, as it
“mean level” order
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