ASTM D95-2013 Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation《蒸馏法测定石油产品和沥青材料中含水量的标准试验方法》.pdf

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1、Designation: D95 05 (Reapproved 2010)D95 13 Highway Transportation StandardAASHTO No. T55Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5Designation: 74/82 (88)Standard Test Method forWater in Petroleum Products and Bituminous Materials byDistillation1This standard is issued under the

2、fixed designation D95; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revis

3、ion or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope Scope*1.1 This test method covers the determination of water in the range from 0 to 25 % volume in petroleum products, tars, and otherbituminous materials by the distillation method.NOTE 1Vola

4、tile water-soluble material, if present, may be measured as water.1.2 The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsionsrefer to Test Method D244. For crude oils, refer to Test Method D4006 (API MPMS Chapter 10.2).NOTE 2With so

5、me types of oil, satisfactory results may be obtained from Test Method D1796 (API MPMS Chapter 10.6).1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.1.4 This standard does not purport to address all of the safety concerns, if a

6、ny, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Section 6.1 This test method is under the jurisdiction of

7、ASTM Committee D02 on Petroleum Products and Lubricants and the API Committee on Petroleum Measurement, and isthe direct responsibility of Subcommittee D02.02 /COMQ, the joint ASTM-API Committee on Hydrocarbon Measurement for Custody Transfer (Joint ASTM-API).Current edition approved May 1, 2010May

8、1, 2013. Published May 2010July 2013. Originally approved in 1921. Last previous edition approved in 20052010 asD95D95 05 (2010).05. DOI: 10.1520/D0095-05R10.10.1520/D0095-13.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what chan

9、ges 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 current versionof the standard as published by ASTM is to be considered the offic

10、ial document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:2D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydro

11、carbon Dry Cleaning Solvent)D244 Test Methods and Practices for Emulsified AsphaltsD1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure) (API MPMS Chapter10.6)D4006 Test Method for Water in Crude Oil by Distillation (API MPMS Chapter 10.2)D4057 Practic

12、e for Manual Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.1)D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2)D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (API MPMS Chapter 8.3)E123 Spec

13、ification for Apparatus for Determination of Water by Distillation2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum and Petroleum Products (ASTM Practice D4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum and Petroleum Products (ASTM Practice D4177)MPMS Chapter 8.3 Mixing and Hand

14、ling of Liquid Samples of Petroleum and Petroleum Products (ASTM Practice D5854)MPMS Chapter 10.2 Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D4006)MPMS Chapter 10.6 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)(A

15、STM Test Method D1796)3. Terminology3.1 Definitions:3.1.1 bituminous material, nin petroleum technology, a black or dark-colored very viscous liquid or semi-solid composedprincipally of high molecular weight condensed aromatic, or naphthenic compounds, or both.4. Summary of Test Method4.1 The materi

16、al to be tested is heated under reflux with a water-immiscible solvent, which co-distills with the water in thesample. Condensed solvent and water are continuously separated in a trap, the water settling in the graduated section of the trapand the solvent returning to the still.5. Significance and U

17、se5.1 Aknowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products.5.2 The amount of water as determined by this test method (to the nearest 0.05 or 0.1 volume %, depending on the trap sizeused) may be used to correct the volume involve

18、d in the custody transfer of petroleum products and bituminous materials.5.3 The allowable amount of water may be specified in contracts.6. Solvent-Carrier Liquid6.1 A water-immiscible solvent-carrier liquid appropriate to that is miscible in the material being tested (see Table 1) shall beused.6.1.

19、1 Aromatic SolventThe following aromatic solvents are acceptable:6.1.1.1 Industrial Grade Xylene(WarningFlammable. Vapor harmful.)6.1.1.2 A blend of 20 volume % industrial grade toluene and 80 volume % industrial grade xylene. (WarningFlammable.Vapor harmful.)6.1.1.3 Petroleum Naphtha or Coal Tar Na

20、phtha, free of water, yielding not more than 5% distillates at 125C (257F) and notless than 20% at 160C (320F) and with a relative density (specific gravity) not lower than 0.8545 at 15.56/15.56C (60/60F).(WarningExtremely flammable. Harmful if inhaled. Vapors may cause fire.)6.1.2 Petroleum Distill

21、ate SolventApetroleum distillate solvent, 5% boiling between 90 and 100C (194 and 212F) and 90%distilling below 210C (410F),solvent containing at least 2% (V/V) aromatics and with an initial boiling point (IBP) greater than80C (176F); and a final boiling point (FBP) below 250C (482F) shall be used.

22、Percent may be determined by mass or byvolume. (Warning Flammable. Vapor harmful.)NOTE 3Examples of suitable solvents include Types I and IV and Classes A and B of Specification D235.NOTE 4It is recommended to use a wide boiling range solvent with 10% boiling below 100C to help to ensure an even dis

23、tillation rate.6.1.3 Volatile Spirits SolventThe following volatile spirits solvents are acceptable:2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Doc

24、ument Summary page on the ASTM website.3 Published as Manual of Petroleum Measurement Standards. Available from American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070,http:/www.api.orgD95 1326.1.3.1 Petroleum Spirit, with a boiling range from 100 to 120C (212 to 248F). (Warni

25、ngFlammable. Vapor harmful.)6.1.3.2 Iso-octane, of 95% purity or better. (WarningExtremely flammable. Harmful if inhaled. Vapors may cause fire.)6.2 Solvent BlankThe water content of the solvent shall be determined by distilling an equivalent amount of the same solventused for the test sample in the

26、 distillation apparatus and testing as outlined in Section 10. The blank shall be determined to thenearest scale division and used to correct the volume of water in the trap in Section 11.7. Apparatus7.1 GeneralThe apparatus comprises a glass or metal still, a heater, a reflux condenser, and a gradu

27、ated glass trap. The still,trap, and condenser may be connected by any suitable method that produces a leakproof joint. Preferred connections are groundjoints for glass and O-rings for metal to glass. Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3. The stills and trapsshould be cho

28、sen to cover the range of materials and water contents expected. On assembly, care shall be taken to prevent the jointsfrom freezing or sticking. Always apply a very thin film of stopcock grease to prevent the glassware joints from seizing.7.2 StillAglass or metal vessel with a short neck and suitab

29、le joint for accommodating the reflux tube of the trap shall be used.Vessels of 500, 1000, and 2000-mL nominal capacity have proved satisfactory.7.3 HeaterA suitable gas burner or electric heater may be used with the glass still. A gas ring burner with ports on the insidecircumference shall be used

30、with the metal still. The gas ring burner shall be of such dimensions that it may be moved up and downthe vessel when testing materials that are likely to foam or solidify in the still.7.4 GlasswareDimensions and descriptions of typical glassware for use in this test method are provided in Specifica

31、tion E123.TABLE 1 Type of Solvent-Carrier Liquid Versus Material to BeTestedType of Solvent-Carrier Liquid Material to be TestedAromatic asphalt, tar, coal tar, water gas tar, roadtar, cut-back bitumin, liquid asphalt, taracidPetroleum distillate road oil, fuel oil, lubricating oil, petroleumsulfona

32、tesVolatile spirits lubricating greaseTABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material toBe TestedType of Solvent-Carrier Liquid Material to be TestedAromatic asphalt, bitumen, tar, and related productsPetroleum distillate fuel oil, lubricating oil, lubricatingoil additivesVolatile spir

33、its greasesFIG. 1 Typical Assembly with Glass StillD95 133NOTE 5Instead of standardizing on a particular apparatus specification with respect to dimensions and style, a given apparatus will be deemedsatisfactory when accurate results are obtained by the standard addition technique described in Secti

34、on 9.8. Sampling8.1 Sampling is defined as all steps required to obtain an aliquot of the contents of any pipe, tank, or other system and to placethe sample into the laboratory test container. Only representative samples obtained as specified in Practices D4057 (API MPMSChapter 8.1) and D4177 (API M

35、PMS Chapter 8.2) shall be used for this test method.8.2 The size of the test portion should be based on the expected water content of the sample, such that the water yield does notexceed the capacity of the trap (unless a trap with a stopcock is used permitting excess water to be withdrawn into a gr

36、aduatedcylinder).8.3 Practice D5854 (API MPMS Chapter 8.3) contains information on sampling and homogenization efficiency of unknownmixers. This test method should not be followed without strict adherence to Practice D5854 (API MPMS Chapter 8.3).9. Verification9.1 The accuracy of the graduation mark

37、s on the trap shall be certified or verified, using only national or international standards,such as National Institute of Standards and Technology (NIST)4 traceable equipment. Verification shall be with a traceable 5 mLMicro Burette or Micro Pipette, readable to the nearest 0.01 mL.9.1.1 In stylesA

38、, B, C, and D, as specified in Table 2 (Table 1 in Specification E123), each subdivision (that is, 0.1 mL through1.0 mL) in the conical portion of the tube shall be verified. Thereafter, each major subdivision (that is, 2.0 mL, 3.0 mL, 4.0 mL,and up to the total volume of the trap) shall be verified

39、.9.1.2 In styles E and F, as specified in Table 2, each major subdivision (0.1 mL, 1.0 mL, 2.0 mL, 4.0 mL, and 5.0 mL in thecase of Style E; 0.05 mL, 0.5 mL, 1.0 mL, 1.5 mL, and 2.0 mL in the case of Style F) shall be verified.9.2 The entire glassware assembly shall be verified prior to first use an

40、d at a regular frequency thereafter as follows.9.2.1 Put 400 mL of dry (0.02 % water maximum) xylene or the solvent to be utilized in the analysis of unknown samples intothe apparatus and test in accordance with Section 10. When complete, discard the contents of the trap and add the volume of watera

41、s specified as first test in Table 3 directly to the distillation flask and test in accordance with Section 10.9.2.2 Repeat the test in 9.2.1, and add the volume specified as second test in Table 3 directly to the flask. The assembly of theapparatus is satisfactory only if the trap readings are with

42、in the tolerances specified in Table 3.9.3 A reading outside the permissible limits suggests a malfunction resulting from vapor leaks, too rapid boiling, inaccuraciesin calibration of the trap, or ingress of extraneous moisture. Eliminate these factors before repeating the verification.10. Procedure

43、NOTE 6The precision of this test method will be affected by water droplets adhering to surfaces in the apparatus and therefore not settling into thewater trap to be measured. To minimize the problem, all apparatus must be cleaned chemically at least daily to remove surface films and debris, which4 N

44、ational Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.FIG. 2 Two-millilitre Receiver Showing Alternative Connections to Glass StillD95 134NOTE 1Trap shall be 15 to 16 mm in inside diameter.FIG. 3 Typical Assemblies with Metal

45、 StillD95 135hinder free drainage of water in the test apparatus. More frequent cleaning is recommended if the nature of samples being run causes persistentcontamination.10.1 Measure a suitable amount of sample to an accuracy of 6 1% and transfer it to the still.10.2 Measure ordinary liquid samples

46、in a graduated cylinder of an appropriate size. Rinse the material adhering to the cylinderwith one 50-mL and two 25-mL portions of the solvent-carrier liquid (see Section 6 and Table 1). Drain the cylinder thoroughlyafter the sample transfer and each rinsing.10.3 Weigh solid or viscous materials di

47、rectly into the still and add 100 mL of the selected solvent-carrier liquid. In cases ofmaterial with a low-water content when large samples must be used, a solvent-carrier liquid volume in excess of 100 mL may benecessary.10.4 Glass beads or other boiling aids may be added, if necessary, to reduce

48、bumping.10.5 Assemble the components of the apparatus, as illustrated in Fig. 1, Fig. 2, and Fig. 3, choosing the trap in accordance withthe expected water content of the sample and making all connections vapor and liquid tight. If a metal still with a removable coveris used, insert a gasket of heav

49、y paper, moistened with solvent, between the still body and the cover. The condenser tube and trapmust be chemically clean to ensure free drainage of water into the bottom of the trap. Insert a loose cotton plug in the top of thecondenser to prevent condensation of atmospheric moisture inside it. Circulate cold water through the jacket of the condenser.TABLE 2 Specifications and Sizes of TrapsDescriptionStyleTop ofGraduatedTubeBottom ofGraduatedTubeBottom ofVapor TubeSize of TrapmLRangemLSmallestScaleDivision,mLScale ErrorMaximum,mL