1、Designation:D109304 (Reapproved 2007) Designation: D1093 11Standard 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 t
2、he case of revision, 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 Department of Defense.1. Scope*1.1 Thi
3、s test method covers the qualitative determination of the acidity of hydrocarbon liquids and their distillation residues.(WarningMany hydrocarbon liquids are extremely flammable. Harmful if inhaled. Hydrocarbon liquid vapors can cause a flashfire.)1.2 If desired to determine the basicity of a hydroc
4、arbon liquid, proceed in accordance with 9.2 or 9.3, but substitute 3 dropsof phenolphthalein indicator solution for the methyl orange indicator. A pink or red color in the aqueous solution whenphenolphthalein is used indicates basicity.1.3 The results obtained by this test method are qualitative ex
5、pressions. However, for the preparation of reagents and in theprocedure, acceptable SI units are to be regarded as the standard.1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibilityof the user of this standard to establish
6、 appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products at Atmospheric PressureD91 Test Method for Precipitation Number of Lubricating OilsD850 Tes
7、t Method for Distillation of Industrial Aromatic Hydrocarbons and Related MaterialsD1078 Test Method for Distillation Range of Volatile Organic LiquidsD1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of P
8、etroleum and Petroleum 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 for acidity is a pink or red color when methyl orange indicator is used.3.1.2 basicity, nthe quality, state or degree of being
9、basic.3.1.2.1 DiscussionIn this test method, the criterion for basicity is a pink or red color when phenolphthalein indicator is used.3.1.3 distillation residue, nthat portion of the sample remaining after distillation using specified procedures.4. Summary of Test Method4.1 The sample of distillatio
10、n residue or hydrocarbon liquid is shaken with water and the aqueous layer tested for acidity tomethyl orange indicator.4.2 The aqueous layer can also be tested for basicity using phenolphthalein indicator.1This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lu
11、bricants and is the direct responsibility of Subcommittee D02.06 onAnalysis of Lubricants.Current edition approved MayDec. 1, 2007.2011. Published June 2007.January 2012. Originally approved in 1950. Last previous edition approved in 20042007 asD109304.D109304(2007). DOI: 10.1520/D1093-04R07.10.1520
12、/D1093-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is int
13、ended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the curr
14、ent versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Som
15、e petroleum products are treated with mineral acid as part of the refining procedure. Obviously, any residual mineralacid in a petroleum product is undesirable. The absence of a positive indication in the test for acidity of the distillation residue oraqueous extract of a hydrocarbon liquid is an as
16、surance of the care used in refining the fuel or solvent.6. Apparatus6.1 Centrifuge Tube, cone-shaped, 100-mL capacity; calibration not necessary.6.2 Centrifuge, capable of swinging two centrifuge tubes at 1500 rpm.NOTE 1Apparatus used for Test Method D91 is satisfactory.7. Reagents7.1 Purity of Rea
17、gentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3Other grades may be used, provide
18、d it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.7.1.1 Commercially prepared solutions may be used when they meet or exceed the specifications set in 7.1.7.2 Purity of WaterUnless otherwise indicated, refer
19、ences to water shall be understood to mean reagent water conforming toType IV Specifications D1193.7.3 Ethanol(95%) (WarningSee Note 2.)Either pure grain or denatured with 5% methanol.NOTE2Warning:Flammable, Vapor Harmful, if denatured it cannot be made non-toxic. (95 %) (WarningFlammable, Vapor Har
20、mful, if denaturedit cannot be made non-toxic. Either pure grain or denatured with 5 % methanol.7.4 Methyl Orange Indicator Solution (1 g/L)Prepare a methyl orange indicator aqueous solution equal to a concentration of1 g/L.7.4.1 One way to do this is to dissolve 1.0 6 0.1 g of methyl orange in wate
21、r and dilute to 1 L.7.5 Phenolphthalein Indicator Solution Dissolve 1.0 6 0.1 g of phenolphthalein in 100 mL of alcohol.Add sodium hydroxidesolution (NaOH, 0.8 g/L) dropwise to develop a very faint pink color.8. Sampling8.1 Using Practice D4057 (manual sampling) or Practice D4177 (automatic sampling
22、) as a guideline, ensure that a samplerepresentative of the material to be tested is obtained.9. Procedure9.1 All distillation flasks and glassware used in this test shall be clean and dry There shall be no contaminant present that couldaffect the acidic or basic nature of the material under test.9.
23、2 Distillation ResidueAfter measuring the percent residue collected from the distillation by Test Method D86, Test MethodD850, or Test Method D1078 as required, extract the residue with water as described below. Use either the graduated cylindercontaining the residue from the distillation procedure
24、directly or another appropriately sized container, such as a test tube,especially if the volume of water plus residue would make an extraction in the original graduated cylinder impractical. If analternate container is used, ensure the cooled residue is transferred with minimal delay.Add a volume of
25、 water equal to about threetimes the volume of residue, stopper, and shake the container vigorously for at least 30 s. Ensure there is ample head space in thestoppered container to allow adequate mixing. Allow the liquids to separate and pipet the clean aqueous layer into a second cleansmall contain
26、er, such as a test tube. Add 1 drop of methyl orange indicator solution to the container, disperse or mix the indicatorsolution with the aqueous layer, then observe the color of the aqueous layer.9.3 Hydrocarbon LiquidPlace 50 mLof the sample, 15 mLof water, and 3 drops of methyl orange indicator so
27、lution in a cleancentrifuge tube. Stopper the tube with a clean stopper (CautionDuring shaking, vent the centrifuge tube at frequent intervals,especially at the initial 5 s of shaking so that any build-up of vapors or pressure can be released), shake vigorously for 30 s, andcentrifuge at 1500 rpm fo
28、r 10 min. Remove the centrifuge tube and observe the color of the aqueous layer.9.4 For the determination of basicity use 3 drops of phenolphthalein indicator instead of methyl orange in either 9.2 or 9.3.10. Report10.1 If the methyl orange indicator is used, report the material as acidic if a pink
29、to red color is observed.10.2 If the phenolphthalein indicator is used, report the material 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.3Reagent Chemicals, American Chemical Society Specifications , America
30、n Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC
31、), Rockville, MD.D1093 11211. Precision and Bias11.1 In case of pass-fail data, or other qualitative tests, no generally accepted method for determining precision or bias iscurrently available.12. Keywords12.1distillation residue acidity; distillation residue basicity; hydrocarbon acidity; hydrocarb
32、on basicityD1093 11312.1 distillation residue acidity; distillation residue basicity; hydrocarbon acidity; hydrocarbon basicitySUMMARY OF CHANGESSubcommittee D02.06 has identified the location of selected changes to this standard since the last issue(D109304(2007) that may impact the use of this sta
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36、wn 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1093 114
