ASTM D2415-2015 Standard Test Method for Ash in Coal Tar and Pitch《煤焦油和硬沥青中灰分的标准试验方法》.pdf

1、Designation: D2415 98 (Reapproved 2012)D2415 15Standard Test Method forAsh in Coal Tar and Pitch1This standard is issued under the fixed designation D2415; 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.1. Scope Scope*1.1 This test method covers the determination of the ash content of tar and pitch.1.2 The values stated in SI units are to be rega

3、rded as standard. No other units of measurement are included in this standard.1.3 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 practices and deter

4、mine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D370D850 PracticeTest Method for Dehydration of Oil-Type PreservativesDistillation of IndustrialAromatic Hydrocarbons andRelated MaterialsD4296 Practice for Sampling PitchE11 Specification for Wov

5、en Wire Test Sieve Cloth and Test Sieves3. Summary of Test Method3.1 The sample is carefully volatilized and burned in a muffle furnace or by other suitable means, after which the carbonaceousresidue is completely oxidized and the remaining ash stabilized at 900C900 C in the muffle furnace.4. Signif

6、icance and Use4.1 This test method determines the amount of inorganic matter in the sample.5. Apparatus5.1 Muffle FurnaceA muffle furnace with good air circulation and capable of having its temperature regulated at 900900 C6 10C.10 C.5.2 Dish or Crucible, porcelain, silica, or platinum, having a cap

7、acity of 3535 mL to 45 mL 45 mL and a diameter at the topof 5555 mm to 60 mm.60 mm.5.3 Sieve, U.S. Standard 600-mStandard 600 m (No. 30), conforming to Specification E11.6. Bulk Sampling6.1 Samples from shipments shall be taken in accordance with Practice D4296 and shall be free of foreign substance

8、s.Thoroughly mix the sample immediately before removing a representative portion for the determination or for dehydration.7. Dehydration of Sample7.1 Hard PitchIf the solid bulk sample contains free water, air-dry a representative portion in a forced draft oven at50C.50 C.1 This test method is under

9、 the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved Nov. 1, 2012Dec. 1, 2015. Published November 2012December 201

10、5. Originally approved in 1965. Last previous edition approved in 20082012as D241598(2008).D2415 98 (2012). DOI: 10.1520/D2415-98R12.10.1520/D2415-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Stand

11、ardsvolume 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

12、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.*A Summary of Changes section appears at the end of this standardCopyrigh

13、t ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17.2 Soft PitchIf the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulksample at a temperature between 125125 C and 150C150 C in an open con

14、tainer until the surface is free of foam. Take care notto overheat, and remove heat source immediately when foam subsides.7.3 TarDehydrate a representative portion of the bulk sample in accordance with Test Method D370D850, but stop thedistillation when the temperature reaches 170C.170 C. Separate a

15、ny oil from the water which has distilled over (if crystals arepresent, warm sufficiently to ensure their solution), and thoroughly mix the oil with the residual tar in the still after the latter hascooled to a moderate temperature.8. Preparation of Working Sample8.1 Hard PitchIf the pitch can be cr

16、ushed at room temperature, prepare a 20-g20 g working sample by suitable crushing,mixing, and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crusher and amullite mortar and pestle. No particle in the representative sample shall be larger than 5 mm

17、 5 mm in any dimension. Crush thissample so that all of it will pass the 600-m600 m (No. 30) sieve.8.2 Soft PitchIf the pitch is too soft to grind and too sticky to mix, heat a representative portion of the dry sample to the lowesttemperature that will permit passage through the 600-m600 m (No. 30)

18、sieve, taking care to avoid excessive loss of volatilematter. Do not exceed 10 min 10 min for this melting period. Pass the heated sample through the 600-m600 m sieve to removeforeign matter.8.3 TarHeat a representative portion of the dry tar to the lowest temperature that will permit passage throug

19、h the600-m600 m (No. 30) sieve, then filter through this sieve to remove foreign matter.8.4 Preservation of SamplesStore samples as large lumps or as solidified melts in closed containers. Do not save crushedsamples for future analyses since changes in composition sometimes occur in pulverized pitch

20、.9. Procedure9.1 Ignite a clean dish or crucible for 1 h in the muffle furnace at 900900 C610C.10 C. Cool slowly to about 100C,100 C,then place the dish or crucible in a desiccator. When at room temperature, weigh to the nearest 0.1 mg.0.1 mg.9.2 Transfer a 10-g10 g portion of the representative, de

21、hydrated sample to the tared dish or crucible and weigh to the nearest0.1 mg. 0.1 mg. Place the container and the sample in the cold muffle furnace and gradually heat to redness at a rate that avoidsmechanical loss from boil-over or spattering, due to too rapid an expulsion of volatile matter. Inste

22、ad of the muffle furnace, a hotplate or gas flame may be used to remove volatiles, as long as the same precautions against mechanical loss are taken. After thevolatile matter has been driven off and a semi-coke remains, complete the ignition in the muffle furnace at 900900 C 610C.10 C. When all carb

23、on appears to have burned off, cool the dish or crucible to about 100C100 C before placing it in adesiccator. When at room temperature weigh to the nearest 0.1 mg. 0.1 mg. Repeat the ignition at 900900 C 6 10C10 C for30-min30 min intervals until constant weight is obtained.10. Calculation10.1 Calcul

24、ate the ash content of the sample as follows:Ash,%5100A/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 the acceptability of results (95 % probabili

25、ty):12.1.1 RepeatabilityDuplicate values by the same operator shall not be considered suspect unless the determined percentagesdiffer by more than 0.01.12.1.2 ReproducibilityThe values reported by each of two laboratories, representing the arithmetic average of duplicatedeterminations, shall not be

26、considered suspect unless the reported percentages differ by more than 0.03.12.2 BiasThis procedure has no bias because the value of ash is defined in terms of this test method.13. Keywords13.1 ash; inorganic matter; pitch; tarD2415 152SUMMARY OF CHANGESSubcommittee D02.05 has identified the locatio

27、n of selected changes to this standard since the last issue(D2415 98 (2012) that may impact the use of this standard. (Approved Dec. 1, 2015.)(1) Replaced Practice D370 with Test Method D850.ASTM International takes no position respecting the validity of any patent rights asserted in connection with

28、 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 responsible techni

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