1、Designation: D1509 95 (Reapproved 2012)Standard Test Methods forCarbon BlackHeating Loss1This standard is issued under the fixed designation D1509; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 in parentheses indicates the year of last reapproval. Asuperscript 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. Scope1.1 These test methods cover the determination of theheating los
3、s of carbon black at 125C. This heating lossconsists primarily of moisture, but other volatile materials mayalso be lost. These test methods are not applicable to treatedcarbon blacks that contain added volatile materials, if moistureloss is to be measured.1.2 The values stated in SI units are to be
4、 regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does 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 d
5、etermine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber
6、 and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 A carbon black sample is weighed before and afterheating for1hat125C. The observed difference in mass is theheating loss.4. Significance and Use4.1 In addition to determining the heating loss (primarilymoisture content) of carbon
7、black, these drying conditions areused to prepare samples prior to performing other carbon blacktests.4.2 When larger samples are prepared for other tests, use anopen vessel of suitable dimensions so that the depth of theblack is no more than 10 mm during conditioning.4.3 Carbon black is hygroscopic
8、. The amount of moistureabsorbed is related to the surface area of the black and to therelative humidity, ambient temperature, and time to which thematerial is exposed.Method AConvectionGravity Oven Method5. Apparatus5.1 Oven, gravity-convection type, capable of temperatureregulation of within 61C a
9、t 125C and temperature unifor-mity within 65C.5.2 Weighing Bottle, low-form, 30 mm in height and 60 mmin diameter, equipped with a ground-glass stopper.5.3 Analytical Balance, having a sensitivity of 0.1 mg.5.4 Desiccator.6. Sampling6.1 Samples shall be taken in accordance with PracticesD1799 or D19
10、00.6.1.1 Place the samples of carbon black in airtight samplecontainers. Allow the closed container to reach room tempera-ture before starting the test.7. Procedure7.1 Dry the weighing bottle and the stopper, with thestopper removed, in the specified oven set at 125C for 30 min.Place the bottle and
11、stopper in the desiccator and allow to coolto room temperature. Weigh the bottle with stopper to thenearest 0.1 mg.7.2 Weigh2gofcarbon black into the weighing bottle to thenearest 0.1 mg.1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct responsibi
12、lity of Subcommittee D24.31 onNon-Carbon Black Components of Carbon Black.Current edition approved June 1, 2012. Published November 2012. Originallyapproved in 1957. Last previous edition approved in 2007 as D1509 95 (2007).DOI: 10.1520/D1509-95R12.2For referenced ASTM standards, visit the ASTM webs
13、ite, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United State
14、s17.3 Place the weighing bottle, sample, and stopper in thespecified oven set at 125C for 1 h with the stopper removed.7.4 Replace the stopper and transfer the bottle and contentsto the desiccator. Remove the stopper and allow to cool toroom temperature. Replace the stopper on the weighing bottleand
15、 reweigh to the nearest 0.1 mg.NOTE 1Keep the stopper on the weighing bottle when transferring toand from the desiccator to prevent loss of carbon black due to air currents.7.5 Repeat the procedure on a second sample.8. Calculation8.1 Calculate the percent heating loss to the nearest 0.1 % asfollows
16、:H 5 B 2 C!/B 2 A!# 3100 (1)where:H = heating loss, %,A = mass of weighing bottle and stopper, g,B = mass of weighing bottle, stopper, and sample beforeheating, g, andC = mass of weighing bottle, stopper, and sample afterheating, g.9. Report9.1 Report the following information:9.1.1 Proper identific
17、ation of the sample, and9.1.2 Result reported to the nearest 0.1 %.10. Precision and Bias10.1 This precision and bias statement has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.10.2 PrecisionThe precision results in this precisi
18、on andbias section give an estimate of the precision of this testmethod with the materials (rubbers, carbon blacks, etc.) used inthe particular interlaboratory program described in 10.3-10.3.2.The precision parameters should not be used for acceptance orrejection testing of any group of materials wi
19、thout documen-tation that they are applicable to those particular materials andthe specific testing protocols of the test method.10.3 Convection-Gravity OvenTest Method AA Type 1interlaboratory precision program was conducted in 1994. Bothrepeatability and reproducibility represent short-term testin
20、gconditions. Eight laboratories tested three carbon blacks (Ma-terials A, B, and C) twice on each of two different days. A testresult is the value obtained from a single determination.Acceptable difference values were not measured. (See Table 1for the individual precision results for these three car
21、bonblacks, which span a broad range for heat loss.)10.3.1 RepeatabilityThe pooled absolute repeatability, r,of Method A heat loss has been established as 0.070 %. Twosingle test results (or determinations) that differ by more than0.070 % must be considered suspect, that is, to have come fromdifferen
22、t sample populations. Such a decision dictates thatsome appropriate action be taken.10.3.2 ReproducibilityThe pooled absolutereproducibility, R, of Method A heat loss has been establishedas 0.356 %. Two single test results (or determinations) pro-duced in separate laboratories that differ by more th
23、an 0.356 %must be considered suspect, that is, that they represent differentsample populations. Such a decision dictates that appropriateinvestigative or technical or commercial actions, or both, betaken.10.4 BiasIn test method terminology, bias is the differencebetween an average test value and the
24、 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.Method BMoisture Balance Method11. Apparatus11.1 Moisture Balance, having a sensitivity
25、 of 0.1 mg andpreferably an indirect heating source.NOTE 2An indirect heating source is preferred due to the ability of acarbon black to absorb infrared radiation and elevate the temperature ofthe carbon black higher than the surrounding atmosphere.11.2 Desiccator.TABLE 1 Test Methods D1509 Test Met
26、hod PrecisionType 1 (Convection-Gravity OvenMethod A)AMaterialMean Level,% Mass LossWithin LaboratoriesBBetween LaboratoriesBSrr (r) SRR (R)B 0.03 0.012 0.033 95.4 0.033 0.093 271A 0.24 0.011 0.032 12.9 0.051 0.145 59.0C 0.40 0.039 0.112 28.2 0.210 0.593 149Average 0.23Pooled values 0.025 0.070 30.9
27、 0.126 0.356 158AThis is short-term precision (days) with outliers removed from the data set.BSymbols are defined as follows:Sr= within-laboratory standard deviation,r = repeatability (in measurement units),(r) = repeatability (in relative percent),SR= between-laboratory standard deviation,R = repro
28、ducibility (in measurement units), and(R) = reproducibility (in relative percent).D1509 95 (2012)212. Sampling12.1 Samples shall be taken in accordance with PracticesD1799 or D1900.12.1.1 Place the samples of carbon black in air-tight con-tainers. Allow the closed container to reach room temperature
29、before starting the test.13. Procedure13.1 Set up the moisture balance according to the manufac-turers instructions. The temperature should not exceed 125C.13.2 Place approximately2gofcarbon black into themoisture balance and determine its mass to the nearest 0.1 mg.13.3 Close the lid and start the
30、machine.13.4 Once the mass loss, under these drying conditions, isless than 1 mg over 30 s the test portion is considered dry andthe percent mass loss should be recorded to the nearest 0.1 %.14. Calculation14.1 Calculate the percent heating loss to the nearest 0.1 %as follows:H 5 A 2 B!/A# 3100 (2)w
31、here:H = heating loss, %,A = mass of test portion before heating, g, andB = mass of test portion after heating, g.15. Report15.1 Report the following information:15.1.1 Proper identification of the sample, and15.1.2 Result obtained from an individual determination,reported to the nearest 0.1 %.16. P
32、recision and Bias16.1 No precision and bias statement has been developed onthis procedure; however, it is anticipated that it will bedeveloped (see Practice D4483).17. Keywords17.1 carbon black; heating loss; moisture; volatile materialsASTM International takes no position respecting the validity of
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35、our 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 is co
36、pyrighted 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 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/).D1509 95 (2012)3
