1、Designation: D 5439 95 (Reapproved 2006)Standard Test Method forDetermination of Sediment in Moellon1This standard is issued under the fixed designation D 5439; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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 tolueneinsoluble sediment contained in Moellon. This test method wasderived fr
3、om Test Method D 473.1.2 The values stated in SI units 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 practice
4、s and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 473 Test Method for Sediment in Crude Oils and FuelOils by the Extraction MethodD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic S
5、ampling 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. Apparatus4.1 Extraction Apparatus (see Fig. 1 and Fig.
6、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 the ends projecting through a lid ofsufficient diam
7、eter 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 copper or brass, the tin coating shallhave a minim
8、um 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 not less than 15 gand not more than 17 g. The thi
9、mble 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-resistant, shall be made of platinum, stainless steel,ni
10、ckel-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 be approxi-mately 20 mm in diameter and 25 mm de
11、ep, 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 Fig. 1aby1This test method is under the jurisdict
12、ion 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 Chemists Assn.(Method H 231957).Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 199
13、3. Last previous edition approved in 2001 as D 5439 95(2001).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.
14、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 Extraction Apparatus for Determination of Sediment1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1
15、9428-2959, United States.means of the corrosion-resistant wire looped over the bottom ofthe condenser coil and attached to the basket supports or as inFig. 1b where the wire supports of the basket are attached tohooks soldered to the underside of the condenser lid.4.1.6 Source of Heat, a source of h
16、eat, 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 to dry point)A2.0CResidue after evaporation 0.001 %Substances darkened by
17、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 any pipe, tank, or other system and toplace the sample into the laboratory
18、test container.6.2 Only representative samples obtained as specified inPractices D 4057 and D 4177 shall be used for this test method.7. Procedure7.1 For referee tests, use a new extraction thimble. Forroutine tests, thimbles may be reused. Before reusing athimble, it must be heated to a dull red he
19、at (preferably in anelectric furnace) to remove the combustible portion of theaccumulated sediment. Subject the thimble to a preliminaryextraction as described in 7.2 before being used for anotherdetermination.NOTE 1Silver solder should be used on all joints.FIG. 2 Basket Thimble SupportD 5439 95 (2
20、006)27.2 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 thimble for atleast 1 h. Then dry the thimble for1hatatemperature of 11
21、5to 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 estimated 10-g test portion of the sample in thethimble immediately after
22、 the sample has been mixed asdescribed in Practices D 4057 and D 4177. 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, and extract with the hot toluene for 30min after the solvent droppin
23、g 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 water content, usethe assembly shown in Fig. 1b. In this procedure, a
24、ny 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 apparatus to cool and emptythe cup.7.5 After the extraction is completed, dr
25、y 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; dry, cool,and weigh the thimble as described in 7.5. Repeat thisex
26、traction 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 of thatof the original sample as follows:Mass % 5MS 9.6!OSM 9.3!3 1
27、00 (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 procedure used.NOTE 1Since water and sediment values are commonly reporte
28、d 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 naturally occurring materials (with a specific gravitylower than th
29、at 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 gravity, if unknown) by 2.Volume % 5 MPS/2.0! 3 CSP or 0.85 if unknown# (
30、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 described in 10.1.1 and 10.1.2.10.1.1 RepeatabilityThe difference bet
31、ween 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 the following value inonly one case in twenty:0.017 1 0.255 S (3)wher
32、e: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 normal and correct operation ofthe test method, exceed the following
33、value in only one case intwenty:0.033 1 0.255 S (4)where:S = average result, %.11. Keywords11.1 leather; Moellon; sediment; toluene insolubleD 5439 95 (2006)3ANNEX(Mandatory Information)A1. PRECAUTIONARY INFORMATIONA1.1 Toluene Precaution:A1.1.1 Keep away from heat, sparks, and open flame.A1.1.2 Vap
34、or 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 contact with the skin.ASTM International takes no position respectin
35、g the validity of any patent rights asserted in connection with 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 standa
36、rd is subject to revision at any time by the responsible technical committee and must 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 Internationa
37、l Headquarters. Your comments will receive careful consideration at a meeting of theresponsible 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.Th
38、is standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, 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 5439 95 (2006)4
