ASTM D1093-11(2017) Standard Test Method for Acidity of Hydrocarbon Liquids and Their Distillation Residues.pdf

1、Designation: D1093 11 (Reapproved 2017)Standard Test Method forAcidity of Hydrocarbon Liquids and Their DistillationResidues1This standard is issued under the fixed designation D1093; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,

2、 the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method co

3、vers the qualitative determination ofthe acidity of hydrocarbon liquids and their distillation resi-dues. (WarningMany hydrocarbon liquids are extremelyflammable. Harmful if inhaled. Hydrocarbon liquid vapors cancause a flash fire.)1.2 If desired to determine the basicity of a hydrocarbonliquid, pro

4、ceed in accordance with 9.2 or 9.3, but substitute 3drops of phenolphthalein indicator solution for the methylorange indicator. A pink or red color in the aqueous solutionwhen phenolphthalein is used indicates basicity.1.3 The results obtained by this test method are qualitativeexpressions. However,

5、 for the preparation of reagents and inthe procedure, acceptable SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety

6、and health practices and determine the applica-bility of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Stand

7、ards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products andLiquid Fuels at Atmospheric PressureD91 Test Method for Precipitation Number of Lub

8、ricatingOilsD850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD1078 Test Method for Distillation Range of Volatile Or-ganic LiquidsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Auto

9、matic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definitions:3.1.1 acidity, nthe quality, state or degree of being acid.3.1.1.1 DiscussionIn this test method, the criterion foracidity is a pink or red color when methyl orange indicator isused.3.1.2 basicity, nthe quality, state or

10、degree of being basic.3.1.2.1 DiscussionIn this test method, the criterion forbasicity is a pink or red color when phenolphthalein indicatoris used.3.1.3 distillation residue, nthat portion of the sampleremaining after distillation using specified procedures.4. Summary of Test Method4.1 The sample o

11、f distillation residue or hydrocarbon liquidis shaken with water and the aqueous layer tested for acidity tomethyl orange indicator.4.2 The aqueous layer can also be tested for basicity usingphenolphthalein indicator.5. Significance and Use5.1 Some petroleum products are treated with mineral acidas

12、part of the refining procedure. Obviously, any residualmineral acid in a petroleum product is undesirable. Theabsence of a positive indication in the test for acidity of thedistillation residue or aqueous extract of a hydrocarbon liquidis an assurance of the care used in refining the fuel or solvent

13、.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved May 1, 2017. Published June 2017. Originallyapproved in 195

14、0. Last previous edition approved in 2011 as D1093 11. DOI:10.1520/D1093-11R17.2For 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 o

15、nthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDe

16、velopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16. Apparatus6.1 Centrifuge Tube, cone-shaped, 100 mL capacity; cali-bration not necessary.6.2 Centrifuge, capable of swinging two centrifuge tubes at15

17、00 r min.NOTE 1Apparatus used for Test Method D91 is satisfactory.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the Americ

18、an Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.1.1 Commercially prepared solutions may be used whenthey meet o

19、r exceed the specifications set in 7.1.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type IV Specifications D1193.7.3 Ethanol (95 %) (WarningFlammable, VaporHarmful, if denatured it cannot be made non-toxic. Either puregrain

20、or denatured with 5 % methanol.7.4 Methyl Orange Indicator Solution (1 g L)Prepare amethyl orange indicator aqueous solution equal to a concen-tration of 1 g L.7.4.1 One way to do this is to dissolve 1.0 g 6 0.1 g ofmethyl orange in water and dilute to 1 L.7.5 Phenolphthalein Indicator Solution Diss

21、olve 1.0 g 60.1 g of phenolphthalein in 100 mL of alcohol. Add sodiumhydroxide solution (NaOH, 0.8 g L) dropwise to develop avery faint pink color.8. Sampling8.1 Using Practice D4057 (manual sampling) or PracticeD4177 (automatic sampling) as a guideline, ensure that asample representative of the mat

22、erial to be tested is obtained.9. Procedure9.1 All distillation flasks and glassware used in this testshall be clean and dry There shall be no contaminant presentthat could affect the acidic or basic nature of the material undertest.9.2 Distillation ResidueAfter measuring the percent resi-due collec

23、ted from the distillation by Test Method D86, TestMethod D850, or Test Method D1078 as required, extract theresidue with water as described below. Use either the graduatedcylinder containing the residue from the distillation proceduredirectly or another appropriately sized container, such as a testt

24、ube, especially if the volume of water plus residue wouldmake an extraction in the original graduated cylinder imprac-tical. If an alternate container is used, ensure the cooled residueis transferred with minimal delay.Add a volume of water equalto about three times the volume of residue, stopper, a

25、nd shakethe container vigorously for at least 30 s. Ensure there is amplehead space in the stoppered container to allow adequatemixing. Allow the liquids to separate and pipet the cleanaqueous layer into a second clean small container, such as a testtube. Add 1 drop of methyl orange indicator soluti

26、on to thecontainer, disperse or mix the indicator solution with theaqueous layer, then observe the color of the aqueous layer.9.3 Hydrocarbon LiquidPlace 50 mL of the sample,15 mL of water, and 3 drops of methyl orange indicatorsolution in a clean centrifuge tube. Stopper the tube with aclean stoppe

27、r (WarningDuring shaking, vent the centrifugetube at frequent intervals, especially at the initial 5 s of shakingso that any build-up of vapors or pressure can be released),shake vigorously for 30 s, and centrifuge at 1500 r min for10 min. Remove the centrifuge tube and observe the color ofthe aqueo

28、us layer.9.4 For the determination of basicity use 3 drops of phenol-phthalein indicator instead of methyl orange in either 9.2 or9.3.10. Report10.1 If the methyl orange indicator is used, report thematerial as acidic if a pink to red color is observed.10.2 If the phenolphthalein indicator is used,

29、report thematerial as basic if a pink to red color appears.10.3 If neither indicator shows the color changes specified,the material can be reported neutral.11. Precision and Bias11.1 In case of pass-fail data, or other qualitative tests, nogenerally accepted method for determining precision or bias

30、iscurrently available.12. Keywords12.1 distillation residue acidity; distillation residue basicity;hydrocarbon acidity; hydrocarbon basicity3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by

31、 the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D1093 11 (2017)2ASTM International takes no position respecting the validity

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34、. 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.This standard is

35、 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 11 (2017)3