Designation: D 2318 ~ 98 (Reapproved 2003) Quinoline-Insoluble (Ql) Content of Tar and Pitch’ ‘Thi stan ites nde he uo designation 12318 the mer meey flog he designation nie the ea of Standard Test Method for gia adept nin te Speedie epson od 1, Scope test method covers the determination of the soluble matter (Q) in tar and pitch. 1.2 Since this test method is empirical, stict adherence to all details of the procedure is necessary. 1.3 The values stated in ST units are to be regarded as the standard, 14 This standard does not purport to address all of the ‘safety concerns, If any, assoctated with Us use. It Ie the ‘esponsibility of the user ofthis standard to establish appro- priate safety and health practices and determine the applica- bility of regulatory limitations prior to use. See Section 7 2, Referenced Documents 21 ASTM Stondards: ® D171 Test Method for Relative Density of Solid Pitch and “Asphalt (Displacement Method) DIS Test Method for Water in Petroleum Products and Bituminous Materials by Distillation 1D 329 Specification for Aceto D 362 Specification for Industrial Grade Toluene! D830 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials 1D 4296 Practice for Sampling Pitch EL Specification for ASTM Thermometers EL Specification for Wite Cloth and Sieves for Testing Purposes, imary of Test Method 3.1 The sample is digested in hot quinoline and filtered. The insoluble material is washed, dried, and weighed. "This tet metod 6 wale the jaan of ASTAE Commitee OC co ‘eave Fut nd Lbs ad th dst posi o Sabcormits ‘0205 on Popes of Fuel, Psu Cok, snd Cuba Mate ‘Curent editor spose Ne I, 203, Pabishl Nanrbe 208. Oily snppoed io 1968, Lt rvoa dion sprord in 1998 ae 2318-9. "Terraced ASTM son, vst te ASTA web wneasn oro ontct ASTM Costner Senco at seen ar. Por dtl Book of AST ‘Stan vane fran teri he ann acer Sammy page oo “hao rvs th yer af lst vison Antara pene tse year nt reap el eng sue he seven rap 4, Significance and Use 4.1 This tost method is useful in evaluating and charaeter: taing tar and pitch, and as one element in establishing the ‘uniformity of shipments and sources of supply. 5. Apparatus 5.1 Fillering Cructbles, porcelain, with fine-porosity bot- tom, 25 to 40-ml. capacity, high-form, maximum pore diam- eter, 7. 52 Filler Apparatus—Filter lask and tube with erucible adapter. 53 Sieves—U. 8. Standard 600-pm (No. 30) and 250-ym (No. 60), conforming to Specification E 11. 54 Bleciric Hot Plate or Water Bath, maintrined at 75 5°C, 6. Reagents and Materials 6.1 Quinotine, Refined, meeting the following requirements: Gi. The quinoline shall distill from 5 t0 95% within a range of 2°C that shall include the temperature of 237.4°C after corrections for barometric pressure and emergent stem have shall be carried out in accordance ng a total immersion thermometer with a range from 195 to 305°C, graduated in 0.5°C, and conforming 10 the requirements for Thermometer 65C as described in Specification E 6.12 The quinoline shall have a specific gravity at 15.5/ 15.5°C of 1.092 to 1.098, as determined by Test Method D 71, or other method of equivalent accuracy. 6.1.3 The quinoline shall be clear and light in color and shall contain less than 0.5 volume % of water as determined by Test Method D 95. If not, redistill the quinoline in all-glass appa- ratus, discarding the frst 5% and collecting the next 90%. If the quinotine contains suspended matter but is clear, light in color, and conteins Tess than 0.5 % water, filter the quinoline through a erucible contsining Sg of Celite Filter. ‘6.14 Store the quinoline in a tightly closed, dark bottle, 6.2 Toluene, Industrial Pure, meeting Specification D 362. 63 Acetone, mesting Specification D 329, 64 Concentrated Hydrochlorie Acid. enter rest 0 Ba Ha Da FO So 7, et Conta A 26288, Ua St Copyright by AST Int (all ighs reserved) [Reprodicton authorized por Liense Agreement with DENISE BOOKER (VFT CANADA INC); Thu Feb 23 (4:40:43 BST 2006Aly p 2318 - 98 (2003) 65 Celte Analytical Filer did (CAPA) —Dry (0 co weight at 105°C, and store i tightly stoppered container 65.1 Do not vse any other grade of fills aid Because filtration characteristics may differ. CATA is manufactured only by Manville Co. and distributed through scientific supply houses tan 7. Hazards 7.1. Fumes of the solvents should be removed by means of | proper hoods from all working areas, The working area should be Kept free of sparks and flames. Quinoline fumes should not be inhaled, and prolonged contact with the skin should be avoided, Toluene is toxic and flammable. 7.2. Observe proper Inboratory procedures for handling hy. Arechlorie and diluting acid, shipments shall be taken in accordance swith Practice D 4296 and shall be free of foreign substances ‘Thoroughly mix the sample immediately before removing & representative portion forthe determination or for dehydration 9, Dehydration of Sample 9.1 Hard Pitch—I the solid bulk sample contains free water, aidry a representative portion ina forced draft oven st 50°C. 92 Soft Plich Xf the presence of water is indicated by surface foam on heating, maintain a representative portion of ‘he bul sample at «temperature between 125 and 180°C in an ‘open container uni the sueface is free of foam. Take cae not io overheat, and remove heat soure immediately when foam subsides. 9.3. Tar—A wet tar sample may ether be dehydrated or used a5 received as long as conditions steted in 9.3.1 and 9.3.2 ae ‘met 9.3.1 Dehydrate a representative portion ofthe bulk sample at atmospheric pressure using a simple sde-arm cision apparatus sila to the one in Test Method D 850 and sop the distillation when the temperature reaches 170°C. Separate any cil frm the water that has distilled over (if erystals are pres ‘warm suliciently to ensure their solution) and thoroughly mix the ol with the residual tr in the sil afer the later has cooled {oa moderate temperature. 9.32 As an alternative to dehydration, the water content of the tari determined by Test Method D9, and if tho water content is fess than 10 mass %, the Ql content is coreced to 4 dy-tr basis (se 13.2). This alternative test method applies ‘only to stable emulsions of water in tr, that i no. water separates when th tar sample is lft undisturbed for 24 hat zoom temperature, 10, Preparation of Working Sample 10.1 Hard Pitch the piteh can be crushed st room temperature, prepare a 20-g working sample by suitable crushing, mixing, and quartering of a representative portion of the dry sample. The crushing ean be dane with a small jaw crusher and a mullite mortar and pestle. No particle in’ che representative sample shall be larger than $ mm in any dimension, Crush this sample so thet all of it will pass the Copyright by ASTAC Tn (all sights reserved), 2 250-m (No, 60) sieve but will have a mini patticles. Store the sieved working sample in «tightly closed container and use within 24 h (see 10.4). 10.2 Soft Piich—I the pitch is too soft to grind and too sticky to mix, heat a representative portion ofthe dry sample to the lowest temperature thet will permit passage through the 600-um (No. 30) sieve, taking care to avoid excessive loss of volatile matter, Do not exceed 10 min far this meting perio. Pass the heated sample through the 600-ym sieve to remove foreign matter. 10.3. Tar—Heat a representative portion of the dey tar to the lowest temperature thet will permit passage through the £600 (No. 30) siove, then filter through this seve to remove foreign matter. 104 Preservation of Samples—Storo samples as large lumps or as solidified melis in closed containers. Discard ‘working samples 24 h after crushing and sioving as changes in ‘composition sometimes occar in pulverized pitch. 11, Crucible Preparations 11.1 Ifthe erucible, after thorough cleaning (Gee 11.2), has ‘been used for less than six determinations, clean ites follows: Remove the mat, wash the erucible with distilled wate, dry, and ignite in a mule furnace for Ih at about 800°C. Coat the crucible slowly by plscing it in a drying oven for 1 h after removal from the furnace fo prevent erscking and place it ina desiccator while still warm. 112 After the crucible has been used for sic determinations, remove any residual ash from pores in the filtering area by boiling in 1+1 hydrochloric acid, Add equal volume of concentrated hydrochloric acid to distilled water. Then bail the crucible in distilled wate, thoroughly back wash with distilled water, dry, and ignite as in 11.1. 12, Procedure 12.1 Make and record all weighings to the nearest In 122 Select a sample mass that will yield between 75 and 150 mig of matter insoluble in quinoline (Qt), unless this would requite ess than the minimum acceptable sample mass of 0.5, Bit! which ense O.5 g shall be used 123 Transfer 1 O.1 g of dry CAFA to a clean, dry, filtering crucible. Weigh immediately, end record the mass of crucible plus CARA. 124 Place the required amount of sansple in a tared beaker and weigh. Calculate and record the mass of the sample, ‘Transfer about half ofthe CAFA fiom the crucible othe beaker ‘with sample, Distribute the remaining CAFA evenly over the bottom of the emucible. 12.5 Add 25 mL of quinoline tothe beaker while sizing the mixture with a stirring rod of thermometer to break up lamps, then cover the beaker with a smell watch glass, Plaoo the beaker and a wash bottle containing quinoline on an electric hotplate or in a waterbath maintained at 75 + 5°C. (Asuitable ‘weight can be used to keep the beaker from being upset in the water bath.) Digest for at least 20 min, Occasionally sti the contents of the beaker to promote digestion. Check for com- pleteness of digestion by inspecting the bottom of the beaker for undigested pitch. Sepodacion authorized per Lietse Agreement with DENISE BOOKER (VET CANADA ING); Thu Feb 28 14:04 EST 2006{ly v 2318 ~ 98 (2003) 12.6 Insert the Alter tube with adapter in the Alte flask, and place the previously prepared and tared crucible in the adapter. Carefilly add suficient quinotine to the crucible to wet the elite thoroughly. Apply suction and form a mat of evenly iributed Celite. Maintain suetion until filtration and subse- ‘quent washing with quinotine are completed, 12.7 Pour the hot quinoline-pitch mixture into the erucible, ‘while the Celite inthe erucible is still wet, without disturbing the mat, Stir the mixture in the beaker immediately before ‘pouring successive portions into the enicible. Allow the eor= tents to drain completely, but not to the extent thatthe insoluble serial on the filter appears substantially dry. 12,8 Wash the besker, thermometer, or stitring rod, and crucible with small portions (2 to 3 mL. each) of quinoline at 75 2 5°C from the wash: bot, Pass all the washes through the filer. Allow each wash to pass almost completely through the filter before the next is added. Use a suitable policeman to sweep the insoluble particles into the crucible, Repeat the line washes until the filtrate is the seme color as the quinoline used for washing. Twelve washings are usually enough. passed through the toluene and wash with a total of 75 suction, Aer all the toluene hat passed through the filter, wash the contents of the erucibl the same manner with acetone, Maintain full suction for a minimum of S min after the acetone wash. Remove the crucible, and wipe the outside with a clean, soft eloth or tissue moistened with acetone. 12.9.1 During the quinoline and toluene washing do. not allow the CAPA mat to get completely dry as the filtration rate may decrease considerably. 12.10 Place the filtering crucible inthe drying oven at 105, to 110°C and dey to constant weight (1 mg). When the hot crucible is removed from the drying oven it shall have no odor (of quinoline, Transfer the crucible to the desiccator and cool for 25 min, thon weigh and record the weight of the filtering crucible and its contents (seo 12.1). 12.10.1 Insoluble matter on the filter, after wesbing with acetone, should have no ador of quinoline, which is evidence of insufficient washing. If odor of quinoline is detectable, repeat the entire determination 2.11 Ifthe mass of matter insoluble in quinoline is less than 75 mg or more than 150 mg, repeat the determination with fan adjusted sample mass of not less than 0.5 (see 12.2) 13, Calculation 13.1 Caleulate the QI content as follows: (i, mass % = (4 ~ ByC) x 100 0 where: A_ = {otal mass ofthe filtering crucible and CAPA added to the erucible, and matter insoluble in quinoline, tial mass of the filtering crucible containing dried CARA, and C_© mass of sample taken for the determination. 132 If the QL was determined on a wet tar sample (see 9.3.2), correct the QI value determined in 13.1 to dry-ar basis $ follows: nas 9 iy basis) Qt raes % (vet bis) ‘TOO wae omen a, ass) * 19 Bs o 14, Report 14.1 Report the QL content to the nearest 0.1 %, 15, Precision and Bias 15.1 The following criteria shall be used for judging the acceplability of results (95 % probability): 15.1.1 Repeatability Duplicate values by the same opera- tor shall not be considered suspect unless the determined potcentages differ by more than 0.2 when the QI content is 4% ot less, or by more than 0.3 when the QU content is more than 4%. 15.1.2. Reproducibility ~The values reported by cach of two laboratories, represeating the arithmetic average of duplicate determinations, shell not be considered suspect unless the reported peroentages differ by moro than 0.3 when the QF ‘content is 4 % or less, or by more than 0.6 when the Ql content is more than 4%. 15.2 Bias—This test method has no bias because the value ‘of quinoline-insouble is defined in terms of this test method, 16, Keywords 16.1 cosl-arinsolubles;piteh; Ql; quinoline insolubles; tar AST htematna kes no psion respecting te vasa sy patel dbs ase In connecton wth ay er menoned ‘nt star sor ts tana are axrasl avwed st Cotominton of he Vana of anys paler, ad th ak ‘otintingamont ef uch igh, a etry Dao eponeay is strands uot revise af ny ine by reper lca coneieand ns ered ov fv yrs at ‘arse eer roaaroved orien. Ya eommant ned ear atari sana brat concos ‘an shoul be cessed ASA imators Hassgsartors Your commenti rete catcnetorokon a aot eo ‘aspoosta technica! commit, ih you may ator ou fafa your commons havo ot rece wa hen yo had ‘mate yer views bron to th ASTA Conmitae on Slondor a th ase how ba Til sandr copyhed by ASTM rater 100 Bar Harbor Dive, PO Box C760, Hos Crahohocan PA 1928-268 ned Sates nia rps (geo mute epis) of the stnca may be obished by cantacng ASTM a the 30078 css or at 10-48z-%06 (phone) 6108329395 (a). er sarveegasimary {oma cr tough he ASTM net (ase on. Copyright by ASTM Ine (all rights reserved), 3 [Reproduction authorized per Hiconse Agreemtent with DENISE BOOKER (VFT CANADA INC); Th Feb 23 144063 BST 2006