ASTM D2415-1998(2003) Standard Test Method for Ash in Coal Tar and Pitch《测试煤焦油和硬沥青中灰分的标准试验方法》.pdf

1、Designation: D 2415 98 (Reapproved 2003)An American National StandardStandard Test Method forAsh in Coal Tar and Pitch1This standard is issued under the fixed designation D 2415; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the ashcontent of tar and pitch.1.2 The values stated in SI unit

3、s are to be regarded as thestandard.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 determine the applica-bility of regulatory limi

4、tations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 370 Test Method for Dehydration of Oil-Type Preserva-tivesD 4296 Practice for Sampling PitchE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Method3.1 The sample is carefully volatilized and burned in

5、amuffle furnace or by other suitable means, after which thecarbonaceous residue is completely oxidized and the remainingash stabilized at 900C in the muffle furnace.4. Significance and Use4.1 This test method determines the amount of inorganicmatter in the sample.5. Apparatus5.1 Muffle FurnaceA muff

6、le furnace with good air circu-lation and capable of having its temperature regulated at 900 610C.5.2 Dish or Crucible, porcelain, silica, or platinum, havinga capacity of 35 to 45 mL and a diameter at the top of 55 to 60mm.5.3 Sieve, U.S. Standard 600-m (No. 30), conforming toSpecification E11.6. B

7、ulk Sampling6.1 Samples from shipments shall be taken in accordancewith Practice D 4296 and shall be free of foreign substances.Thoroughly mix the sample immediately before removing arepresentative portion for the determination or for dehydration.7. Dehydration of Sample7.1 Hard PitchIf the solid bu

8、lk sample contains freewater, air-dry a representative portion in a forced draft oven at50C.7.2 Soft PitchIf the presence of water is indicated bysurface foam on heating, maintain a representative portion ofthe bulk sample at a temperature between 125 and 150C in anopen container until the surface i

9、s free of foam. Take care notto overheat, and remove heat source immediately when foamsubsides.7.3 TarDehydrate a representative portion of the bulksample in accordance with Test Method D 370, but stop thedistillation when the temperature reaches 170C. Separate anyoil from the water which has distil

10、led over (if crystals arepresent, warm sufficiently to ensure their solution), and thor-oughly mix the oil with the residual tar in the still after thelatter has cooled to a moderate temperature.8. Preparation of Working Sample8.1 Hard PitchIf the pitch can be crushed at roomtemperature, prepare a 2

11、0-g working sample by suitablecrushing, mixing, and quartering of a representative portion ofthe dry sample. The crushing can be done with a small jawcrusher and a mullite mortar and pestle. No particle in therepresentative sample shall be larger than 5 mm in anydimension. Crush this sample so that

12、all of it will pass the600-m (No. 30) sieve.8.2 Soft PitchIf the pitch is too soft to grind and too stickyto mix, heat a representative portion of the dry sample to thelowest temperature that will permit passage through the600-m (No. 30) sieve, taking care to avoid excessive loss of1This test method

13、 is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Nov. 1, 2003. Published November 2003. Originallyapproved in 1965. Last prev

14、ious edition approved in 1998 as D 241598.2For referenced ASTM standards, visit the ASTM website, 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.1Copyright ASTM Int

15、ernational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.volatile matter. Do not exceed 10 min for this melting period.Pass the heated sample through the 600-m sieve to removeforeign matter.8.3 TarHeat a representative portion of the dry tar to thelowest temper

16、ature that will permit passage through the600-m (No. 30) sieve, then filter through this sieve to removeforeign matter.8.4 Preservation of SamplesStore samples as large lumpsor as solidified melts in closed containers. Do not save crushedsamples for future analyses since changes in compositionsometi

17、mes occur in pulverized pitch.9. Procedure9.1 Ignite a clean dish or crucible for1hinthemufflefurnace at 900 6 10C. Cool slowly to about 100C, then placethe dish or crucible in a desiccator. When at room temperature,weigh to the nearest 0.1 mg.9.2 Transfer a 10-g portion of the representative, dehyd

18、ratedsample to the tared dish or crucible and weigh to the nearest 0.1mg. Place the container and the sample in the cold mufflefurnace and gradually heat to redness at a rate that avoidsmechanical loss from boil-over or spattering, due to too rapidan expulsion of volatile matter. Instead of the muff

19、le furnace, ahot plate or gas flame may be used to remove volatiles, as longas the same precautions against mechanical loss are taken.After the volatile matter has been driven off and a semi-cokeremains, complete the ignition in the muffle furnace at 900 610C. When all carbon appears to have burned

20、off, cool thedish or crucible to about 100C before placing it in adesiccator. When at room temperature weigh to the nearest 0.1mg. Repeat the ignition at 900 6 10C for 30-min intervalsuntil constant weight is obtained.10. Calculation10.1 Calculate the ash content of the sample as follows:Ash, % 5 10

21、0A/B (1)where:A = weight of ash, andB = weight of sample.11. Report11.1 Report the weight percent of ash to the nearest 0.01 %.12. Precision and Bias12.1 The following criteria shall be used for judging theacceptability of results (95 % probability):12.1.1 RepeatabilityDuplicate values by the same o

22、pera-tor shall not be considered suspect unless the determinedpercentages differ by more than 0.01.12.1.2 ReproducibilityThe values reported by each of twolaboratories, representing the arithmetic average of duplicatedeterminations, shall not be considered suspect unless thereported percentages diff

23、er by more than 0.03.12.2 BiasThis procedure has no bias because the value ofash is defined in terms of this test method.13. Keywords13.1 ash; inorganic matter; pitch; tarASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedi

24、n 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 responsible technical committee and mu

25、st 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 consideration at a meeting of th

26、eresponsible 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 Barr Harbor Drive, PO Box C70

27、0, 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).D 2415 98 (2003)2