1、Designation: D1618 99 (Reapproved 2011)Standard Test Method forCarbon Black ExtractablesTransmittance of TolueneExtract1This standard is issued under the fixed designation D1618; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the measurement of the degreeof toluene discoloration by carbon black extractables and
3、 isuseful in controlling the reaction processes for production ofcarbon black. This test method may not be applicable to carbonblacks with high extractables.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard d
4、oes 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 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM St
5、andards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Terminology3.1 Definition:3.1.1 carbon black toluene disc
6、oloration, n the transmit-tance, at 425 nm, of the filtrate obtained from the tolueneextract of carbon black, compared to that of pure toluene.4. Significance and Use4.1 The toluene discoloration value provides an estimate oftoluene-soluble discoloring residues present on the carbonblack.5. Apparatu
7、s and Reagent5.1 Spectrophotometer, with tungsten filament lamp, 20-nmmaximum spectral bandpass, capable of measuring percenttransmittance at a 425-nm wavelength. The instrument is to beoperated in accordance with the manufacturers directions foroptimum performance.5.2 Cuvets, rectangular, with an o
8、ptical light path of 10 mm.5.3 Balance, analytical, with a sensitivity of 60.01 g.5.4 Oven, gravity-convection type, capable temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.5.5 Pipet, automatic, bottle-type, 20 cm3, with a repeatabil-ity of 60.1.5.6 Erlenmeyer Flasks, 1
9、25 cm3with ground-glass stopper.5.7 Filter Paper, qualitative grade, medium retention,medium-fast filter speed, 150-mm diameter.5.8 Glass Filtering Funnels, 75-mm inside diameter at thetop.5.9 Beakers,50or100cm3, with pouring lips.5.10 Wiping Paper, lint-free.5.11 Cotton Swabs.5.12 Fume Hood, fully
10、enclosed on three sides, with spark-proof fan and motor.5.13 Toluene, analytical reagent grade.6. Sampling6.1 Samples shall be taken in accordance with PracticeD1799 or Practice D1900.7. Standardization of Apparatus7.1 Turn on the spectrophotometer and allow it to warm forthe length of time specifie
11、d by the manufacturer.7.2 Check the zero reading of the spectrophotometer inaccordance with the manufacturers instructions, and adjust ifnecessary.1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.31 on Non-CarbonBla
12、ck Components of Carbon Black.Current edition approved May 1, 2011. Published July 2011. Originally approvedin 1965. Last previous edition approved in 2004 as D1618 99 (2004). DOI:10.1520/D1618-99R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
13、e 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 Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 Place the funnel with the filter paper int
14、o an Erlenmeyerflask. Filter approximately 30 cm3of toluene into the flask andstopper the flask.7.4 Pour a portion of the toluene into the beaker with thepouring lip for simplifying the transfer of the toluene to thecuvet.7.5 Rinse the cuvet with the filtered toluene three times,filling approximatel
15、y one third full each time. Discard thisrinsing toluene into an approved safety container.NOTE 1The cuvet must be handled on the ground-glass sides only. Donot touch the smooth, clear sides with the fingers.7.6 Fill the cuvet and wipe the outside surfaces with thelint-free wiping paper while holding
16、 the cuvet in front of asuitable light source. The toluene must be free of any contami-nants, such as lint particles, which might cause light scattering,thus influencing the test results. If necessary, rewipe the outsideuntil perfectly clean, or clean the inside surfaces with a cottonswab. Repeat 7.
17、5 if the inside surfaces are cleaned.7.7 . Insert the cuvet into the spectrophotometer and adjustit to read 100 % transmittance at the 425-nm wavelength.8. Procedure8.1 Dry an adequate sample of carbon black at 125 6 1Cfor 60, +5, 0 min, using a gravity-convection oven.NOTE 2An infrared lamp must no
18、t be used for drying samples, as itwill vaporize some of the extractable materials.8.2 Allow the sample to cool to room temperature in adesiccator.8.3 Weigh 2.00 6 0.01 g of the carbon black and transfer itto a 125-cm3Erlenmeyer flask with ground-glass stopper.8.4 Add 20 cm3of toluene to the sample
19、flask and stopperthe flask.NOTE 3If necessary, larger quantities of carbon black and toluenemay be used, but the quantities must remain in this ratio of 1 g/10 cm3oftoluene.8.5 Without delay, shake the mixture vigorously either byhand or machine for 60, +5, 0 s.8.6 Immediately pour as much of the mi
20、xture as possibleinto the glass funnel with filter paper, which has previouslybeen prepared and inserted into an Erlenmeyer flask.8.7 As soon as filtration is complete, stopper the flask untilready to test.8.8 Check standardization of the spectrophotometer at 425nm in accordance with Section 7.8.9 P
21、our a portion of filtrate out of the stoppered flask intoa beaker with a pouring lip.8.10 Using a cuvet matched to the one in 7.5, or the samecuvet as used in 7.5, rinse and fill the cuvet in the same manneras in 7.5 and 7.6.8.11 Insert the cuvet into the spectrophotometer and recordthe percent tran
22、smittance obtained at 425 nm to the nearest0.1 %.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample, and9.1.2 Toluene discoloration value reported to the nearest0.1 % transmittance.10. Precision and Bias10.1 These precision statements have been prepared inaccorda
23、nce with Practice D4483. Refer to this practice forterminology and other statistical details.10.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials used in the particular interlaboratory program de-scribed below. The preci
24、sion parameters should not be used foracceptance or rejection testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 1.10.3 A type 1 inter-labora
25、tory precision program was con-ducted as detailed in Table 2. Both repeatability and reproduc-ibility represent short-term (daily) testing conditions. Thetesting was performed using two operators in each laboratoryperforming the test once on each of two days (total of fourtests). A test result is th
26、e value obtained from a singledetermination. Acceptable difference values were not mea-sured. The between-operator component of variation is in-cluded in the calculated values for r and R.10.4 The results of the precision calculations for this test aregiven in Table 1. The materials are arranged in
27、ascending“mean level” order.10.5 RepeatabilityThe pooled relative repeatability, (r),of this test has been established as 1.60 %. Any other value inTable 1 may be used as an estimate of repeatability, asappropriate. The difference between two single test results (ordeterminations) found on identical
28、 test material under therepeatability conditions prescribed for this test will exceed therepeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results that differ by more than the appropriate value fromTable 1 must be suspected
29、 of being from different populationsand some appropriate action taken.NOTE 4Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asignificant difference in the two materials, samples, etc., which generatedthe two test results.
30、10.6 ReproducibilityThe pooled relative reproducibility,(R), of this test has been established as 3.55 %.Any other valuein Table 1 may be used as an estimate of reproducibility, asappropriate. The difference between two single and indepen-dent test results found by two operators working under theTAB
31、LE 1 Precision Parameters for D1618 Extractables-TolueneDiscoloration, (Type 1 Precision)Units 105m3/kg (cm3/100 g)Material Mean Level Sr (r) SR (R)N550 96.91 0.68 1.93 1.87 5.28N650 97.41 0.65 1.83 1.34 3.79SRB N762 98.01 0.65 1.84 1.23 3.49SRB A5 (N135) 98.99 0.39 1.09 0.64 1.81IRB#6 (N330) 98.99
32、0.38 1.08 0.81 2.30Average 98.06Pooled Values 0.56 1.60 1.25 3.55D1618 99 (2011)2prescribed reproducibility conditions in different laboratorieson identical test material will exceed the reproducibility on anaverage of not more than once in 20 cases in the normal andcorrect operation of the method.
33、Two single test resultsproduced in different laboratories that differ by more than theappropriate value from Table 1 must be suspected of beingfrom different populations and some appropriate investigativeor technical/commercial action taken.10.7 BiasIn test method terminology, bias is the differ-enc
34、e between an average test value and the reference (true) testproperty value. Reference values do not exist for this testmethod since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.11. Keywords11.1 carbon black; extractables; tol
35、uene discolorationASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement o
36、f such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for
37、additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known t
38、o the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at
39、 the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Interlaboratory Precision ProgramNominal Test Period Material Number of LaboratoriesMarch 1996 N650 48October 1996 IRB#6 (N330) 40March 1997 SRB N762 44September 1997 SRB A5 (N135) 39March 1998 N550 45D1618 99 (2011)3
