1、Designation: D5439 95 (Reapproved 2012)Standard Test Method forDetermination of Sediment in Moellon1This standard is issued under the fixed designation D5439; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the tolueneinsoluble sediment contained in Moellon. This test method wasderived from
3、Test Method D473.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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
4、to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D473 Test Method for Sediment in Crude Oils and Fuel Oilsby the Extraction MethodD4057 Practice for Manual Sampling of Petroleum an
5、dPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 ISO Standard:3ISO 5272 Toluene for Industrial Use - Specifications3. Significance and Use3.1 This test method is intended for use in determining thetoluene insoluble sediment contained in Moellon.4. Appara
6、tus4.1 Extraction Apparatus (see Fig. 1 and Fig. 2), consistingof the parts described in 4.1.1-4.1.6.4.1.1 Extraction Flask, a wide-neck Erlenmeyer flask of 1-Lcapacity.4.1.2 Condenser, a condenser in the form of a metal coilapproximately 25 mm in diameter and 50 mm in lengthattached to, and with th
7、e ends projecting through a lid ofsufficient diameter to cover the neck of the flask as shown inFig. 1. The coil should be made from stainless steel, tin,tin-plated copper, or tin-plated brass tubing having an outsidediameter of 5 to 8 mm and a wall thickness of 1.5 mm. Ifconstructed of tin-plated c
8、opper or brass, the tin coating shallhave a minimum thickness of 0.075 mm. The exposed surfaceof the coil for cooling purposes is about 115 cm2.4.1.3 Extraction ThimbleThe extraction thimble shouldbe of a refractory porous material, pore size index P15, 25 mmin diameter by 70 mm in height, weighing
9、not less than 15 gand not more than 17 g. The thimble shall be suspended fromthe condenser coil by means of a basket so that it hangsapproximately midway between the surface of the extractingsolvent and the bottom of the condenser coil.4.1.4 Thimble BasketThe thimble basket shall becorrosion-resista
10、nt, shall be made of platinum, stainless steel,nickel-chromium alloy, or similar material, and shall meet therequirements of Fig. 2.4.1.5 Water CupA water cup shall be used when testing asample having a high-water content (see Fig. 1b). The cup shallbe made of glass, shall be conical in shape, shall
11、 be approxi-mately 20 mm in diameter and 25 mm deep, and shall have acapacity of approximately 3 mL. A glass hook fused on the rimat one side is so shaped that when hung on the condenser thecup hangs with its rim reasonably level. In this procedure, thethimble basket is suspended either as shown in
12、Fig. 1abymeans of the corrosion-resistant wire looped over the bottom of1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This testmethod was developed in cooperation with the American Leather Chemist
13、s Assn.(Method H 231957).Current edition approved April 1, 2012. Published April 2012. Originallyapproved in 1993. Last previous edition approved in 2006 as D5439 95(2006).DOI: 10.1520/D5439-95R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service a
14、t serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute, 11 West 42nd St., 13thFloor, New York, NY 10036.NOTE 1Apparatus B shows the water cup in position.FIG. 1 Extr
15、action Apparatus for Determination of Sediment1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the condenser coil and attached to the basket supports or as inFig. 1b where the wire supports of the basket are attached tohooks soldered
16、to the underside of the condenser lid.4.1.6 Source of Heat, a source of heat, preferably a hot plate,suitable for vaporizing toluene.5. Solvent5.1 Toluene, conforming to ISO 5272, Grade 2.(WarningFlammable.)5.1.1 The typical characteristics for the reagent are:Color (APHA) 10Boiling range (initial t
17、o dry point)A2.0CResidue after evaporation 0.001 %Substances darkened by H2SO4passes ACS testSulfur compounds (as S) 0.003 %Water (H2O) (by Karl Fischer titration) 0.03 %_ARecorded boiling point 110.6C.6. Sampling6.1 Sampling is defined as all steps required to obtain analiquot of the contents of an
18、y pipe, tank, or other system and toplace the sample into the laboratory test container.6.2 Only representative samples obtained as specified inPractices D4057 and D4177 shall be used for this test method.7. Procedure7.1 For referee tests, use a new extraction thimble. Forroutine tests, thimbles may
19、 be reused. Before reusing athimble, it must be heated to a dull red heat (preferably in anelectric furnace) to remove the combustible portion of theNOTE 1Silver solder should be used on all joints.FIG. 2 Basket Thimble SupportD5439 95 (2012)2accumulated sediment. Subject the thimble to a preliminar
20、yextraction as described in 7.2 before being used for anotherdetermination.7.2 Before using a new thimble, rub the outside surface withfine sandpaper and remove all loosened material with a stiffbrush. Give the thimble a preliminary extraction with thetoluene, allowing the solvent to drip from the t
21、himble for atleast 1 h. Then dry the thimble for1hatatemperature of 115to 120C; cool in a desiccator, without desiccant, for 1 h, andweigh to the nearest 0.1 mg. Repeat this extraction until themasses of the thimble, after two successive extractions, do notdiffer by more than 0.2 mg.7.3 Place an est
22、imated 10-g test portion of the sample in thethimble immediately after the sample has been mixed asdescribed in Practices D4057 and D4177. Do not attempt toadjust this estimated 10-g portion to any exact predeterminedamount. Weigh to the nearest 0.01 g. Place the thimble in theextraction apparatus,
23、and extract with the hot toluene for 30min after the solvent dropping from the thimble is colorless.Ensure that the rate of extraction is such that the surface of themixture of oil and toluene in the thimble does not rise higherthan to within 20 mm of the top.7.4 When testing samples having a high w
24、ater content, usethe assembly shown in Fig. 1b. In this procedure, any water inthe test portion is removed as its toluene azeotrope and iscollected in the water cup, where it separates as a bottom layer.The toluene layer overflows into the thimble. If the cupbecomes full of water, allow the apparatu
25、s to cool and emptythe cup.7.5 After the extraction is completed, dry the thimble for 1h at 115 to 120C; cool in a desiccator, without desiccant, for1 h and weigh to the nearest 0.2 mg.7.6 Repeat the extraction, allowing the solvent to drip fromthe thimble for at least 1 h but not longer than 1.25 h
26、; dry, cool,and weigh the thimble as described in 7.5. Repeat thisextraction for further 1-h periods, if necessary, until the massesof the dried thimble plus sediment, after two successiveextractions, do not differ by more than 0.2 mg.8. Calculation8.1 Calculate the mass of the sediment as a percent
27、 of thatof the original sample as follows:Mass % 5MS 9.6!OSM 9.3!3 100 (1)where:M = mass,S = sediment, andO = original sample mass.9. Report9.1 Report the results to the nearest 0.01 % as the masspercent of sediment by extraction (Note 1). The test report shallreference this test method as the proce
28、dure used.NOTE 1Since water and sediment values are commonly reported asvolume percent, calculate the volume of the sediment as a percent of theoriginal sample. As a major portion of the sediment probably would besand (silicon dioxide, which has a specific gravity of 2.32) and a smallamount of other
29、 naturally occurring materials (with a specific gravitylower than that of sand), use an arbitrary specific gravity of 2.0 for theresulting sediment. Then, to obtain volume percent sediment, divide themass percent sediment multiplied by the specific gravity of the crude at15C (use 0.85 specific gravi
30、ty, if unknown) by 2.Volume % 5 MPS/2.0! 3 CSP or 0.85 if unknown# (2)where:M = mass,P = percent,S = sediment, andCSP = crude specific gravity.10. Precision10.1 The precision of this test method, as based on masspercent and examination of interlaboratory test results in therange from 0 to 0.4 % is d
31、escribed in 10.1.1 and 10.1.2.10.1.1 RepeatabilityThe difference between successivetest results, obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial, would, in the long run, in the normal and correctoperation of the test method, exceed t
32、he following value inonly one case in twenty:0.017 1 0.255 S (3)where:S = average result, %.10.1.2 ReproducibilityThe difference between two singleand independent test results obtained by different operatorsworking in different laboratories on identical test material,would, in the long run, in the n
33、ormal and correct operation ofthe test method, exceed the following value in only one case intwenty:0.033 1 0.255 S (4)where:S = average result, %.11. Keywords11.1 leather; Moellon; sediment; toluene insolubleD5439 95 (2012)3ANNEX(Mandatory Information)A1. PRECAUTIONARY INFORMATIONA1.1 Toluene Preca
34、ution:A1.1.1 Keep away from heat, sparks, and open flame.A1.1.2 Vapor is harmful.A1.1.3 Toluene is toxic.A1.1.4 Particular care must be taken to avoid breathing thevapor and to protect the eyes.A1.1.5 Keep the container closed.A1.1.6 Use with adequate ventilation.A1.1.7 Avoid prolonged or repeated c
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