1、Designation: D1618 17D1618 18Standard 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 year of la
2、st 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 extractables and is usefu
3、lin 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 This standard does no
4、t 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, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.4 This international sta
5、ndard 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 to Trade (TBT) Committee.2. Ref
6、erenced 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 Industries3. Terminology3.1 Definitions:
7、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-soluble discoloring residues present
8、 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 directions foroptimum performance.
9、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-type, 20 cm3, with a repeatabilit
10、y 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 Aug. 1, 2017June 1, 2018. Published August 2017July 2018. Originally approved in
11、 1965. Last previous edition approved in 20112017 asD1618 99 (2011).D1618 17. DOI: 10.1520/D1618-17.10.1520/D1618-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to
12、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 adequately depict all changes
13、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 Conshohocken, PA 19428-2959. United
14、 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.5.10 Wiping Paper, lint-free.5
15、.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 spectrophotometer and allow i
16、t 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 approximately 30 cm3 of toluene in
17、to 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. Discard this rinsingtoluene int
18、o 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 suitablelight source. The toluen
19、e 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 are cleaned.7.7 . Insert the cuv
20、et 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 samples, as it will vaporize some
21、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 the flask.NOTE 3If necessary, la
22、rger 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 possible into the glass funnel with
23、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 size for this particular sample.
24、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 a cuvet matched to the one in
25、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 information:9.1.1 Proper identification
26、of the sample, andD1618 1829.1.2 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.-99. Refer to this practice forterminology and other statistical details.10.2 It was det
27、ermined by a D24 task group formed to update the precision statement of this test method that the test precision,in particular the reproducibility, strongly depends on the level of transmittance. Therefore overall average or pooled values mightbe misleading. This is why the precision table has been
28、subdivided into three separate tables with defined ranges of percentage oftransmittance: high (100 to 95 %), medium (94.9 to 85 %) and low (below 85 %).10.3 The precision results in this precision and bias section give an estimate of the precision of this test method with thematerials used in the pa
29、rticular interlaboratory program described below. The precision parameters should not be used foracceptance or rejection testing of any group of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols of the test method. Any appropriat
30、e value may be used from Table 1Tables 1-3.10.4 A type 1 inter-laboratory precision program was conducted as detailed in Table 2Tables 1-3. Both repeatability andreproducibility represent short-term (daily) testing conditions. The testing was performed using two operators in each laboratoryperformin
31、g the test once on each of two days (total of four tests). A test result is the value obtained from a single determination.Acceptable difference values were not measured. The between-operator component of variation is included in the calculated valuesfor r and R.10.5 The results of the precision cal
32、culations for this test are given in Table 1Tables 1-3.The In each of these tables the materialsare arranged in ascendingdescending “mean level” order. The preferred precision is shown in bold text.10.6 RepeatabilityThe pooled relativeabsolute repeatability, (r,r), of this test has been established
33、as 1.60 %. 1.55 %transmittance for high transmittance values (100 to 95 %), 2.36 % transmittance for medium transmittance values (94.9 to 85 %)and 2.87 % transmittance for low transmittance values (below 85 % transmittance). Any other value in Table 1Tables 1-3 may beused as an estimate of repeatabi
34、lity, as appropriate. The difference between two single test results (or determinations) found onidentical test material under the repeatability conditions prescribed for this test will exceed the repeatability on an average of notmore than once in 20 cases in the normal and correct operation of the
35、 method. Two single test results that differ by more than theappropriate value from Table 1Tables 1-3 must be suspected of being from different populations and some appropriate action taken.NOTE 4Appropriate action may be an investigation of the test method procedure or apparatus for faulty operatio
36、n or the declaration of a significantdifference in the two materials, samples, etc., which generated the two test results.10.7 ReproducibilityThe pooled relativeabsolute reproducibility, (R,R), of this test has been established as 3.55 %. 4.12 %transmittance for high transmittance values (100 to 95
37、%), 7.73 % transmittance for medium transmittance values (94.9 to 85 %)and 11.15 % transmittance for low transmittance values (below 85 % transmittance). Any other value in Table 1Tables 1-3 maybe used as an estimate of reproducibility, as appropriate. The difference between two single and independe
38、nt test results found bytwo operators working under the prescribed reproducibility conditions in different laboratories on identical test material will exceedthe reproducibility on an average of not more than once in 20 cases in the normal and correct operation of the method. Two singletest results
39、produced in different laboratories that differ by more than the appropriate value from Table 1Tables 1-3 must besuspected of being from different populations and some appropriate investigative or technical/commercial action taken.TABLE 1 Precision Parameters for D1618, Carbon Black Extractables - Tr
40、ansmittance of Toluene Extract, (Type 1 Precision), 95 to 100TransmittanceUnits Percent transmittanceMaterial PeriodNumber ofLaboratories(M/H/L)AMean Level Sr r (r) SR R (R)SRB-8C (HS Tread) Sep 2010 67(1/2/9) 99.0 0.39 1.12 1.1 0.99 2.80 2.8SRB-8F2 (N683) Mar 2015 69(1/2/6) 98.2 0.57 1.60 1.6 1.54
41、4.35 4.4N550 Sep 2013 66(2/3/6) 98.1 0.47 1.33 1.4 1.50 4.24 4.3SRB-8A (N326) Sep 2011 60(1/2/5) 98.1 0.58 1.63 1.7 1.18 3.35 3.4SRB-8A2 (N326) Mar 2013 68(1/1/2) 98.0 0.62 1.74 1.8 1.48 4.19 4.3ITRB2 (N330) Mar 2011 56(2/2/9) 98.0 0.65 1.83 1.9 1.35 3.81 3.9SRB-8D (LS Carcass) Mar 2017 67(1/2/6) 97
42、.9 0.42 1.20 1.2 1.49 4.22 4.3N650 Sep 2012 52(0/2/3) 97.7 0.62 1.74 1.8 1.51 4.27 4.4SRB-8B2 (N134) Mar/Apr 2014 66(2/1/3) 97.2 0.63 1.77 1.8 1.35 3.82 3.9N234 Mar 2012 62(1/3/2) 96.9 0.49 1.40 1.4 1.30 3.67 3.8N120 Aug 2015 67(0/3/1) 95.8 0.53 1.50 1.6 1.67 4.73 4.9IRB9 (N330) Mar 2016 73(0/4/1) 9
43、5.0 0.53 1.51 1.6 1.90 5.39 5.7Average 97.5Pooled Values 0.55 1.55 1.6 1.46 4.12 4.2A M = number of outliers for Mean; H = number of outliers for High variation; L = number of outliers for Low variation.D1618 18310.8 BiasIn test method terminology, bias Bias is the difference between an average a te
44、st value and the reference (true) testproperty value. Reference values do not exist a reference value. However, for this test method since the value or level of the testproperty is exclusively defined by the test method. Bias, therefore, cannot be method, bias has not been determined.TABLE 1 Precisi
45、on Parameters for D1618 Extractables-Toluene Discoloration, (Type 1 Precision)Units 105 m3/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 0.38 1.08
46、0.81 2.30Average 98.06Pooled Values 0.56 1.60 1.25 3.55TABLE 2 Precision Parameters for D1618, Carbon Black Extractables - Transmittance of Toluene Extract, (Type 1 Precision), 85 to 94.9TransmittanceUnits Percent transmittanceMaterial PeriodNumber ofLaboratories(M/H/L)AMean Level Sr r (r) SR R (R)S
47、RB-8B (N134) Jun 2009 63(1/4/4) 91.9 0.67 1.91 2.1 2.29 6.49 7.1SRB-8E2 (N660) Aug 2016 69(2/0/1) 89.6 0.67 1.89 2.1 2.02 5.72 6.4N772 Mar 2005 43(0/2/2) 89.6 0.99 2.81 3.1 2.84 8.05 9.0SRB-8E (N660) Sep 2008 51(1/2/6) 85.3 0.95 2.69 3.1 3.52 9.96 11.7Average 89.1Pooled Values 0.84 2.36 2.7 2.73 7.7
48、3 8.7A M = number of outliers for Mean; H = number of outliers for High variation; L = number of outliers for Low variation.TABLE 2 Interlaboratory Precision ProgramNominal Test Period MaterialNumber ofLaboratoriesMarch 1996 N650 48October 1996 IRB#6 (N330) 40March 1997 SRB N762 44September 1997 SRB
49、 A5 (N135) 39March 1998 N550 45TABLE 3 Precision Parameters for D1618, Carbon Black Extractables - Transmittance of Toluene Extract, (Type 1 Precision), 85 Trans-mittanceUnits Percent transmittanceMaterial PeriodNumber ofLaboratories(M/H/L)AMean Level Sr r (r) SR R (R)N762 Aug 2014 65(1/3/1) 73.4 0.84 2.38 3.2 4.41 12.48 17.0SRB-8F (N683) Mar 2010 66(1/2/4) 70.5 1.10 3.13 4.4 2.82 7.99 11.3SRB-8G (N990) Aug 2017 65(1/1/2) 24.7 1.08 3.05 12.3 4.38 12.39 50.1Average 56.2Pooled Values 1.01 2.87 5.1 3.94 11.15 19.8A M = number of outliers for Mean; H = number o
