Designation: D2415 — 98 (Reapproved 2008) Standard Test Method for Ash in Coal Tar and Pitch? “Thi nda sv ni he aed digo D241 tte ember net folowing to designation indices the yes of vigil option aha case fev, he Yor fl reson A umber in pzethvessdcts the Jeo st reappova. A Ser epson (e)odetes an ella change see te ist evson or eapreval 1, Seope 1.1 This test method covers the determination of the ash content of tar and piteh, 12 The values stated standard. No other units of measurement are ineluded in this n ST units are (0 be regarded as standard 1.3 This standard does not purport to address all of the safety concems, if any, associated with iis use. It is the ‘responsibilty of the user of this standard to establish appro priate safety and health practices and determine the applica: bility of regulatory liitations prior to use. 2, Referenced Documents 2.1 ASTI Standards: D370 Practice for Dehydration of OilType Preservatives 1D4296 Practice for Sampling Pite’ ELL Specification for Woven Wire Test Sieve Cloth and Test 3. Summary of Test Method 3.1 The sample is carefully volailized and burned in a muffle furnace or by other suitsble means, after which the ‘carbonaceous residue is completely oxidized and the remaining ash stabilized st 900°C in the muffle furnace. 4, Significance and Use 4.1 This test method determines the amount of inorganic rmatter in the sample, 'S. Apparatus 5.1 Mufle Funace—A mute furnace with good air circu lation ancl capable of having its temperature rogulated at 900 == 10°C, "is wat method 6 vader the juts of ASTM Commitee DOD on ‘Pele Polls au Lbs od ithe diet repo o Sucon¥aee ‘DORIS on Paperten of Fs, Peel Coke aed Caron Neil Cunce dition sprored Oct. 15,2008, Pulsed Novem 208. Oily saproved a 1965. Law previous edilon approved in 2008 as D2NS-S8(200), OK: 101520215 98808, * Rr sefeeaed ASTM standands, vs the AST webs, woes, ot conic ASTA Customer Service at see gen Foe Se Mk of ASTD ‘Sundar vols inration, lero tnd’ Docent Samay age on the ASTM nsblte, Coppin OASIE nmoten, 1098 ‘Copyiht y ASTM it all cs essed); Wen 8 SRISEOT 2011 Dovelodedpitd by Denise ook (Rtepes¢Cannd) pursuant o Lice Agiectan No rer ped 52 Dish or Crucible, porcelain, silica, or platinum, Having a capacity of 35 10 45 mL and a diameter at the top of $5 10 60) 5.3 Sieve, U.S. Standard 600-1m (No. 30), conforming to Specification Et 6, Bulk Sampling G.I. Samples from shipments shall be taken in accordance with Practice D4296 and shall be free of foreign substances. ‘Thoroughly mix the sample immediately before removing a representative portion for the determination or for dehydration, 7. Dehydration of Sample 1A Hard PitchIf the solid bulk sample contains free ‘water, airy a representative portion ina forced draft oven at 50°C, 72 Soft Pitch the presence of water is indicated by surface foam on heating, maintain a representative portion of the bulk sample a a temperature between 125 and 150°C in an ‘open container until the surface is free of foam, Take care not (© overheat, snd remove heat source immediately when foam, subsides. 7.3 Tar-Deydrate a representative portion of the bulk sample in accordance with ‘Test Method 1370, but stop the distillation when the temperature reaches 170°C. Separate any cil from the water which has distilled over (if crystals are present, warm sulfciently to ensure their solution), and thor- ‘oughly mix the oil with the residual tar in the still after the latter his cooled to # moderate temperature 8. Preparation of Working Sample 8.1 Hand Pitch—If the pitch can be crushed at room temperature, prepare 9 20-3 working sample by suitable rushing, mixing, and quartering of a representative portion of the dry sample. The crushing can be done with a small jaw crusher and a mullite mortar and pestle, No particle in the tepresentative sample shall be larger than 5mm in any dimension. Crush this sample so that all of it will pass the 6600-um (No. 30) sieve, 8.2 Soft Piteh—If the pith is too soft to grind and loo sticky to mix, heat a representative portion of the dry sample to the lowest temperature that will permit passage through theAlly p2a15 - 98 (2008) 600m (No. 30) sieve, taking cate to avoid excessive Toss of| ‘olatile matter. Do not exceed 10 min for this melting perio. Pass the heated sample through the 600-ym sieve to remove forcign matter 8.3 Tar—Heat a representative portion of the dy tar tothe lowest temperature that will permit passage through the 600-2 (No, 30) sieve, then filter through this sieve to remove foreign matter. 84 Preservation of Samples—Store samples as large lamps or as solidified melts in closed containers. Do not save erushed samples for facure analyses since changes in composition sometimes occur in pulverized pitch 9, Procedure 9.1 Ignite a clean dish or crucible for 1 h in the muffle furnace at 900 2 10°C. Cool slowly to about 100°C, then place the dish or crucible in a desiceator. When at room temperature, ‘weigh to the nearest 0.1 mg, 9.2 Transfer a 10-g portion of the representative, dehydrated sample (othe tared dish or erucile and weigh to the nearest 0.1 mg. Place the container and the saunple in the cold muffle furnace and gradually heat to redness at a rate that avoids mechanical loss from boil-over or spattering, due (0 too rapid tan expulsion of volatile matier. Instead of the moiMle furnace, & hot plate or gas flame may be used to remove volatiles, as long as the same precautions against mechanical loss are taken After the volatile matter has been driven off and a semi-coke remains, complete the ignition in the muffle furnace at 900 = 10°C. When all carbon appears to have burned off, cool the. dish or crucible to about 100°C before placing it in a desiccator, When at room temperature weigh to the mg. Repeat the ignition at 900 * 10°C for 30-m ‘until constant weight is obtained. 10, Caleutation 10.1 Calculate the ash content of the sample as follows: = 1000/8 0 As where: A B weight of ash, and ‘weight of sample. IL, Report 11.1 Report the weight percent of ash to the nearest 0.01 %. 12, Precision and Bias 12.1 The following criteria shall be used for judging the acooplability of results (95 % probability): 12.1.1 Repeatabitiy—Duplicate values by the same opera- tor shall not be considered suspect unless the determined percentages differ by more than 0.01 12,12 Reproducibility —The values reported by each of (wo laboratories, representing the arithmetic average of duplicate deferminations, shall not be considered suspect unless the reported pereentages differ by more than 0.03. 12.2 Bias—This procedure has no bias because the value of ash is defined in terms of this test method, 13, Keywords 13.1 ash; inorganic matter; piteh; tar ASTI ixemationl takes no pasion rspectng ho vaya ary par gis asserted to connton wi any am mantoned ‘nin star Usors fis ladard are sxpressy advised at eterna otingement sich righs, are ontay fer oi fsponeay. ty fay su pant is adhe Tis stands subject fo verison a any tine by Ie responstie ecniacommitos and mus bo revowed vey feo yours and lroatraises, eter reeprovador than. Yur cnvment rent tha orrevson fh stance or reson saa ‘2d shout bo aarassed lo ASTH nora Heasqarers. You ceriment wl rcavo cereal contsoraon sa mtn a ‘eaponstie echnical commitoa. neh you ma trl ou fa thal your comments hav el rcalved a hearing you souls ‘rake you vis krogn Tot ASTM Commit on Sardar fe aaess shan Leon "Ths stands copyightd by ASTHletomaton, 10 Bar Haba’ Dv, PO x C700, Woe! Canahahocken, PA 19428.2050, nied Stato. indidl rps singe or mul cpl) of is stand aay bo oblanod By canactrg ASTI tho 2000 fabass or a Bf0-8320585 (prone), 8108328555 (aN), ar sordco@asinog lo fas og. Copyright by ASTM ltl sighs eserved; Wed Jan #143818 SDT2018 9 Dovmloedelpined by 1 oF tough the ASTHS webste enie Booker Riegeas¥Canss urinate Liens Arcee. Note eproduins ulin,