1、Designation: D1509 95 (Reapproved 2012)D1509 15Standard 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.
2、A number 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 U.S. Department of Defense.1. Scope1.1 These test methods cover the determination of t
3、he heating loss of carbon black at 125C. This heating loss consists primarilyof moisture, but other volatile materials may also be lost.These test methods are not applicable to treated carbon blacks that containadded volatile materials, if moisture loss is to be measured.1.2 These test methods may a
4、lso be used for the determination of the heating loss of recovered carbon fillers (rCF/rCB) at125C. However, these materials were not included in the precision studies and therefore, the precision statements contained inthis standard may not be valid for these materials.1.3 The values stated in SI u
5、nits are to be regarded as the standard. The values given in parentheses are for information only.1.4 This 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 and health
6、 practices and determine the applicability of regulatorylimitations prior to use.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 Standard
7、s in the Rubber and Carbon Black Manufacturing Industries3. Summary of Test Method3.1 A carbon black sample is weighed before and after heating for 1 h at 125C. The observed difference in mass is the heatingloss.4. Significance and Use4.1 In addition to determining the heating loss (primarily moistu
8、re content) of carbon black, these drying conditions are usedto prepare samples prior to performing other carbon black tests.4.2 When larger samples are prepared for other tests, use an open vessel of suitable dimensions so that the depth of the blackis no more than 10 mm during conditioning.4.3 Car
9、bon black is hygroscopic. The amount of moisture absorbed is related to the surface area of the black and to the relativehumidity, ambient temperature, and time to which the material is exposed.Method AConvectionGravity Oven Method5. Apparatus5.1 Oven, gravity-convection type, capable of temperature
10、 regulation of within 61C at 125C and temperature uniformitywithin 65C.1 These test methods are under the jurisdiction ofASTM Committee D24 on Carbon Black and are the direct responsibility of Subcommittee D24.31 on Non-Carbon BlackComponents of Carbon Black.Current edition approved June 1, 2012Nov.
11、 1, 2015. Published November 2012December 2015. Originally approved in 1957. Last previous edition approved in 20072012as D1509 95 (2007).(2012). DOI: 10.1520/D1509-95R12.10.1520/D1509-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at servicea
12、stm.org. For Annual Book of ASTM Standardsvolume 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. Beca
13、useit may not be technically possible to 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 B
14、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2 Weighing Bottle, low-form, 30 mm in height and 60 mm in 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 acc
15、ordance with Practices D1799 or D1900.6.1.1 Place the samples of carbon black in airtight sample containers. Allow the closed container to reach room temperaturebefore starting the test.7. Procedure7.1 Dry the weighing bottle and the stopper, with the stopper removed, in the specified oven set at 12
16、5C for 30 min. Place thebottle and stopper in the desiccator and allow to cool to room temperature. Weigh the bottle with stopper to the nearest 0.1 mg.7.2 Weigh 2 g of carbon black into the weighing bottle to the nearest 0.1 mg.7.3 Place the weighing bottle, sample, and stopper in the specified ove
17、n set at 125C for 1 h with the stopper removed.7.4 Replace the stopper and transfer the bottle and contents to the desiccator. Remove the stopper and allow to cool to roomtemperature. Replace the stopper on the weighing bottle and reweigh to the nearest 0.1 mg.NOTE 1Keep the stopper on the weighing
18、bottle when transferring to and 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 % as follows:H 5B 2C!/B 2A!# 3100 (1)where:H = heating loss, %,A = mass of weigh
19、ing bottle and stopper, g,B = mass of weighing bottle, stopper, and sample before heating, g, andC = mass of weighing bottle, stopper, and sample after heating, g.9. Report9.1 Report the following information:9.1.1 Proper identification of the sample, and9.1.2 Result reported to the nearest 0.1 %.10
20、. Precision and Bias10.1 This precision and bias statement has been prepared in accordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.10.2 PrecisionThe precision results in this precision and bias section give an estimate of the precision of this test m
21、ethod withthe materials (rubbers, carbon blacks, etc.) used in the particular interlaboratory program described in 10.3 10.3.2. The precisionparameters should not be used for acceptance or rejection testing of any group of materials without documentation that they areapplicable to those particular m
22、aterials and the specific testing protocols of the test method.10.3 Convection-Gravity OvenTest Method AA Type 1 interlaboratory precision program was conducted in 1994. Bothrepeatability and reproducibility represent short-term testing conditions. Eight laboratories tested three carbon blacks (Mate
23、rialsA, B, and C) twice on each of two different days. A test result is the value obtained from a single determination. Acceptabledifference values were not measured. (See Table 1 for the individual precision results for these three carbon blacks, which spana broad range for heat loss.)10.3.1 Repeat
24、abilityThe pooled absolute repeatability, r, of Method A heat loss has been established as 0.070 %. Two singletest results (or determinations) that differ by more than 0.070 % must be considered suspect, that is, to have come from differentsample populations. Such a decision dictates that some appro
25、priate action be taken.10.3.2 ReproducibilityThe pooled absolute reproducibility, R, of Method A heat loss has been established as 0.356 %. Twosingle test results (or determinations) produced in separate laboratories that differ by more than 0.356 % must be consideredsuspect, that is, that they repr
26、esent different sample populations. Such a decision dictates that appropriate investigative or technicalor commercial actions, or both, be taken.10.4 BiasIn test method terminology, bias is the difference between an average test value and the reference (true) test propertyvalue. Reference values do
27、not exist for this test method since the value or level of the test property is exclusively defined by thetest method. Bias, therefore, cannot be determined.D1509 152Method BMoisture Balance Method11. Apparatus11.1 Moisture Balance, having a sensitivity of 0.1 mg and preferably an indirect heating s
28、ource.NOTE 2An indirect heating source is preferred due to the ability of a carbon black to absorb infrared radiation and elevate the temperature of thecarbon black higher than the surrounding atmosphere.11.2 Desiccator.12. Sampling12.1 Samples shall be taken in accordance with Practices D1799 or D1
29、900.12.1.1 Place the samples of carbon black in air-tight containers. Allow the closed container to reach room temperature beforestarting the test.13. Procedure13.1 Set up the moisture balance according to the manufacturers instructions. The temperature should not exceed 125C.13.2 Place approximatel
30、y 2 g of carbon black into the moisture balance and determine its mass to the nearest 0.1 mg.13.3 Close the lid and start the machine.13.4 Once the mass loss, under these drying conditions, is less than 1 mg over 30 s the test portion is considered dry and thepercent mass loss should be recorded to
31、the nearest 0.1 %.14. Calculation14.1 Calculate the percent heating loss to the nearest 0.1 % as follows:H 5A 2B!/A# 3100 (2)where: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 Prope
32、r identification of the sample, and15.1.2 Result obtained from an individual determination, reported to the nearest 0.1 %.16. Precision and Bias16.1 No precision and bias statement has been developed on this procedure; however, it is anticipated that it will be developed(see Practice D4483).TABLE 1
33、Test Methods D1509 Test Method PrecisionType 1 (Convection-Gravity OvenMethod A)AMaterial Mean Level,% Mass Loss Within LaboratoriesB Between LaboratoriesBSr r (r) SR R (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.
34、23Pooled values 0.025 0.070 30.9 0.126 0.356 158A This is short-term precision (days) with outliers removed from the data set.B Symbols are defined as follows:Sr = within-laboratory standard deviation,r = repeatability (in measurement units),(r) = repeatability (in relative percent),SR = between-lab
35、oratory standard deviation,R = reproducibility (in measurement units), and(R) = reproducibility (in relative percent).D1509 15317. Keywords17.1 carbon black; heating loss; moisture; volatile materialsASTM International takes no position respecting the validity of any patent rights asserted in connec
36、tion 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 subject to revision at any time by the responsib
37、le 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 Headquarters. Your comments will receive careful cons
38、ideration 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 copyrighted by ASTM International, 100 B
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