1、Designation: D 1093 04 (Reapproved 2007)An American National StandardStandard Test Method forAcidity of Hydrocarbon Liquids and Their DistillationResidues1This standard is issued under the fixed designation D 1093; the number immediately following the designation indicates the year oforiginal adopti
2、on or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. S
3、cope1.1 This test method covers 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
4、of a hydrocarbonliquid, proceed 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 method are qualitativ
5、eexpressions. However, 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 establis
6、h appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD91 Test Method for Precipitation Number of LubricatingOilsD 850
7、Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsD 1193 Specification for Reagent WaterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling
8、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 degree of being
9、 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 of distillation
10、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 part of the ref
11、ining 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.6. Apparatus6.
12、1 Centrifuge Tube, cone-shaped, 100-mL capacity; cali-bration not necessary.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved May 1, 2007. Pub
13、lished June 2007. Originallyapproved in 1950. Last previous edition approved in 2004 as D 1093 04.2For 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 Docu
14、ment Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Centrifuge, capable of swinging two centrifuge tubes at1500 rpm.NOTE 1Apparatus used for Test Method D91is satisfactory.7. Reagents7.1 Purity of
15、 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 American Chemical Society,where such specifications are available.3Other grades may beused, prov
16、ided 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 or exceed the specifications set in 7.1.7.2 Purity of WaterUnless otherwise indicated, refe
17、rencesto water shall be understood to mean reagent water conformingto Type IV Specifications D 1193.7.3 Ethanol (95 %) (WarningSee Note 2.)Either puregrain or denatured with 5 % methanol.NOTE 2Warning: Flammable, Vapor Harmful, if denatured it cannotbe made non-toxic.7.4 Methyl Orange Indicator Solu
18、tion (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 6 0.1 g of methylorange in water and dilute to 1 L.7.5 Phenolphthalein Indicator Solution Dissolve 1.0 60.1 g of phenolphthalein in 100 mL of alcohol. Add sodi
19、umhydroxide solution (NaOH, 0.8 g/L) dropwise to develop avery faint pink color.8. Sampling8.1 Using Practice D 4057 (manual sampling) or PracticeD 4177 (automatic sampling) as a guideline, ensure that asample representative of the material to be tested is obtained.9. Procedure9.1 All distillation f
20、lasks 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 collected from the distillation by Test Method D86, TestMethod D 850, o
21、r Test Method D 1078 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 testtube, especially if the volume of water plus residue wouldmake a
22、n 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, and shakethe container vigorously for at least 30 s. Ensure ther
23、e 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 solution andobserve the color.9.3 Hydrocarbon LiquidPlace 50 mL of th
24、e sample, 15mL of water, and 3 drops of methyl orange indicator solutionin a clean centrifuge tube. Stopper the tube with a clean stopper(CautionDuring shaking, vent the centrifuge tube at fre-quent intervals, especially at the initial5sofshaking so thatany build-up of vapors or pressure can be rele
25、ased), shakevigorously for 30 s, and centrifuge at 1500 rpm for 10 min.Remove the centrifuge tube and observe the color of theaqueous 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
26、 indicator is used, report thematerial as acidic if a pink to red color is observed.10.2 If the phenolphthalein indicator is used, 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
27、 and Bias11.1 In case of pass-fail data, or other qualitative tests, nogenerally accepted method for determining precision or bias iscurrently available.12. Keywords12.1 distillation residue acidity; distillation residue basicity;hydrocarbon acidity; hydrocarbon basicity3Reagent Chemicals, American
28、Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.
29、S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D 1093 04 (2007)2ASTM International takes no position respecting 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
30、 any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard 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 ar
31、e invited either for revision of this standard or for additional standardsand should be addressed to ASTM International 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 rec
32、eived a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This 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 1093 04 (2007)3
