1、Designation: D1618 99 (Reapproved 2011)D1618 17Standard 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 revisi
2、on, the 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 degree of toluene discoloration by carbon black extract
3、ables and is usefulin controlling the reaction processes for production of carbon black. This test method may not be applicable to carbon blacks withhigh extractables.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 Thi
4、s standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health and healthenvironmental practices and determine theapplicability of regulatory limitations prior to
5、use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers t
6、o Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries
7、3. Terminology3.1 Definitions:3.1.1 carbon black toluene discoloration, n the transmittance, at 425 nm, of the filtrate obtained from the toluene extract ofcarbon black, compared to that of pure toluene.4. Significance and Use4.1 The toluene discoloration value provides an estimate of toluene-solubl
8、e discoloring residues present on the carbon black.5. Apparatus and Reagent5.1 Spectrophotometer, with tungsten filament lamp, 20-nm maximum spectral bandpass, capable of measuring percenttransmittance at a 425-nm wavelength. The instrument is to be operated in accordance with the manufacturers dire
9、ctions foroptimum performance.5.2 Cuvets, rectangular, with an optical light path of 10 mm.5.3 Balance, analytical, with a sensitivity of 60.01 g.5.4 Oven, gravity-convection type, capable temperature regulation within 61C at 125C and temperature uniformity within65C.5.5 Pipet, automatic, bottle-typ
10、e, 20 cm3, with a repeatability of 60.1.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon BlackComponents of Carbon Black.Current edition approved May 1, 2011Aug. 1, 2017. Published July 2011August
11、 2017. Originally approved in 1965. Last previous edition approved in 20042011 asD1618 99 (2004).(2011). DOI: 10.1520/D1618-99R11.10.1520/D1618-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standard
12、svolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to
13、adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
14、ohocken, PA 19428-2959. United States15.6 Erlenmeyer Flasks, 125 cm3 with 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 the top.5.9 Beakers, 50 or 100 cm3, with pouring lips.
15、5.10 Wiping Paper, lint-free.5.11 Cotton Swabs.5.12 Fume Hood, fully 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 Practice D1799 or Practice D1900.7. Standardization of Apparatus7.1 Turn on the
16、 spectrophotometer and allow it to warm for the length of time specified by the manufacturer.7.2 Check the zero reading of the spectrophotometer in accordance with the manufacturers instructions, and adjust if necessary.7.3 Place the funnel with the filter paper into an Erlenmeyer flask. Filter appr
17、oximately 30 cm3 of toluene into the flask andstopper the flask.7.4 Pour a portion of the toluene into the beaker with the pouring lip for simplifying the transfer of the toluene to the cuvet.7.5 Rinse the cuvet with the filtered toluene three times, filling approximately one third full each time. D
18、iscard this rinsingtoluene into an approved safety container.NOTE 1The cuvet must be handled on the ground-glass sides only. Do not touch the smooth, clear sides with the fingers.7.6 Fill the cuvet and wipe the outside surfaces with the lint-free wiping paper while holding the cuvet in front of a su
19、itablelight source. The toluene must be free of any contaminants, such as lint particles, which might cause light scattering, thusinfluencing the test results. If necessary, rewipe the outside until perfectly clean, or clean the inside surfaces with a cotton swab.Repeat 7.5 if the inside surfaces ar
20、e cleaned.7.7 . Insert the cuvet into the spectrophotometer and adjust it to read 100 % transmittance at the 425-nm wavelength.8. Procedure8.1 Dry an adequate sample of carbon black at 125 6 1C for 60, +5, 0 min, using a gravity-convection oven.NOTE 2An infrared lamp must not be used for drying samp
21、les, as it will vaporize some of the extractable materials.8.2 Allow the sample to cool to room temperature in a desiccator.8.3 Weigh 2.00 6 0.01 g of the carbon black and transfer it to a 125-cm3 Erlenmeyer flask with ground-glass stopper.8.4 Add 20 cm3 of toluene to the sample flask and stopper th
22、e flask.NOTE 3If necessary, larger quantities of carbon black and toluene may be used, but the quantities must remain in this ratio of 1 g/10 cm3 of toluene.8.5 Without delay, shake the mixture vigorously either by hand or machine for 60, +5, 0 s.8.6 Immediately pour as much of the mixture as possib
23、le into the glass funnel with filter paper, which has previously beenprepared and inserted into an Erlenmeyer flask.8.7 The filtrate must be free of visible carbon black particles, otherwise the sample preparation shall be repeated (8.3). If theproblem persists, use filter paper with smaller pore si
24、ze for this particular sample.8.8 As soon as filtration is complete, stopper the flask until ready to test.8.9 Check standardization of the spectrophotometer at 425 nm in accordance with Section 7.8.10 Pour a portion of filtrate out of the stoppered flask into a beaker with a pouring lip.8.11 Using
25、a cuvet matched to the one in 7.5, or the same cuvet as used in 7.5, rinse and fill the cuvet in the same manner asin 7.5 and 7.6.8.12 Insert the cuvet into the spectrophotometer and record the percent transmittance obtained at 425 nm to the nearest 0.1 %.9. Report9.1 Report the following informatio
26、n:9.1.1 Proper identification of the sample, andD1618 1729.1.2 Toluene discoloration value reported to the nearest 0.1 % transmittance.10. Precision and Bias10.1 These precision statements have been prepared in accordance with Practice D4483. Refer to this practice for terminologyand other statistic
27、al details.10.2 The precision results in this precision and bias section give an estimate of the precision of this test method with thematerials used in the particular interlaboratory program described below. The precision parameters should not be used foracceptance or rejection testing of any group
28、 of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols of the test method. Any appropriate value may be used from Table 1.10.3 A type 1 inter-laboratory precision program was conducted as detailed in Table 2. Both repeatability an
29、d reproducibilityrepresent short-term (daily) testing conditions. The testing was performed using two operators in each laboratory performing thetest once on each of two days (total of four tests). A test result is the value obtained from a single determination. Acceptabledifference values were not
30、measured. The between-operator component of variation is included in the calculated values for r andR.10.4 The results of the precision calculations for this test are given in Table 1. The materials are arranged in ascending “meanlevel” order.10.5 RepeatabilityThe pooled relative repeatability, (r),
31、 of this test has been established as 1.60 %. Any other value in Table1 may be used as an estimate of repeatability, as appropriate. The difference between two single test results (or determinations)found on identical test material under the repeatability conditions prescribed for this test will exc
32、eed the repeatability on an averageof not more than once in 20 cases in the normal and correct operation of the method. Two single test results that differ by morethan the appropriate value from Table 1 must be suspected of being from different populations and some appropriate action taken.NOTE 4App
33、ropriate action may be an investigation of the test method procedure or apparatus for faulty operation or the declaration of a significantdifference in the two materials, samples, etc., which generated the two test results.10.6 ReproducibilityThe pooled relative reproducibility, (R), of this test ha
34、s been established as 3.55 %. Any other value inTable 1 may be used as an estimate of reproducibility, as appropriate. The difference between two single and independent testresults found by two operators working under the prescribed reproducibility conditions in different laboratories on identical t
35、estmaterial will exceed the reproducibility on an average of not more than once in 20 cases in the normal and correct operation ofthe method. Two single test results produced in different laboratories that differ by more than the appropriate value from Table 1must be suspected of being from differen
36、t populations and some appropriate investigative or technical/commercial action taken.10.7 BiasIn test method terminology, bias is the difference between an average test value and the reference (true) test propertyvalue. Reference values do not exist for this test method since the value or level of
37、the test property is exclusively defined by thetest method. Bias, therefore, cannot be determined.11. Keywords11.1 carbon black; extractables; toluene discolorationTABLE 1 Precision Parameters for D1618 Extractables-TolueneDiscoloration, (Type 1 Precision)Units 105 m3/kg (cm3/100 g)Material Mean Lev
38、el 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 0.38 1.08 0.81 2.30Average 98.06Pooled Values 0.56 1.60 1.25 3.55D1618 173ASTM International takes no position respecting the validi
39、ty 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 of such rights, are entirely their own responsibility.This standard is subjec
40、t 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 additional standardsand should be addressed to ASTM International Headquarter
41、s. 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 to the ASTM Committee on Standards, at the address shown below.This standard i
42、s 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 the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or servicea
43、stm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 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 174
