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Designation: D95 − 13´1
Manual of Petroleum Measurement Standards (MPMS), Chapter 10.5
Standard Test Method for
Water in Petroleum Products and Bituminous Materials by Distillation1 This standard is issued under the fixed designation D95; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript 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.
ε1 NOTE—IP information was removed editorially in September 2013.
1. Scope* D244 Test Methods and Practices for Emulsified Asphalts
1.1 This test method covers the determination of water in D1796 Test Method for Water and Sediment in Fuel Oils by the range from 0 to 25 % volume in petroleum products, tars, the Centrifuge Method (Laboratory Procedure) (API and other bituminous materials by the distillation method. MPMS Chapter 10.6) D4006 Test Method for Water in Crude Oil by Distillation NOTE 1—Volatile water-soluble material, if present, may be measured (API MPMS Chapter 10.2) as water. D4057 Practice for Manual Sampling of Petroleum and
iTeh Standards 1.2 The specific products considered during the develop- ment of this test method are listed in Table 1. For bituminous emulsions refer to Test Method D244. For crude oils, refer to Petroleum Products (API MPMS Chapter 8.1) D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products (API MPMS Chapter 8.2) Test Method D4006 (API MPMS Chapter 10.2). (https://standards.iteh.ai) NOTE 2—With some types of oil, satisfactory results may be obtained D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products (API MPMS Chap- from Test Method D1796 (API MPMS Chapter 10.6). Document Preview 1.3 The values stated in SI units are to be regarded as the ter 8.3) E123 Specification for Apparatus for Determination of Water standard. The values in parentheses are for information only. by Distillation 2.2 API Standards:3 1.4 This standard does not purport to addressASTM D95-13e1 all of the MPMS Chapter 8.1 Manual Sampling of Petroleum and https://standards.iteh.ai/catalog/standards/sist/bef5595e-e33b-4334-971e-15da019822a6/astm-d95-13e1 safety concerns, if any, associated with its use. It is the Petroleum Products (ASTM Practice D4057) responsibility of the user of this standard to establish appro- MPMS Chapter 8.2 Automatic Sampling of Petroleum and priate safety and health practices and determine the applica- Petroleum Products (ASTM Practice D4177) bility of regulatory limitations prior to use. For specific hazard MPMS Chapter 8.3 Mixing and Handling of Liquid Samples statements, see Section 6. of Petroleum and Petroleum Products (ASTM Practice 2. Referenced Documents D5854) MPMS Chapter 10.2 Determination of Water in Crude Oil by 2.1 ASTM Standards:2 the Distillation Method (ASTM Test Method D4006) D235 Specification for Mineral Spirits (Petroleum Spirits) MPMS Chapter 10.6 Test Method for Water and Sediment in (Hydrocarbon Dry Cleaning Solvent) Fuel Oils by the Centrifuge Method (Laboratory Proce- dure) (ASTM Test Method D1796) 1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and the API Committee on Petroleum Measurement, and is the 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, 2013. Published July 2013. Originally approved in 1921. Last previous edition approved in 2010 as D95 – 05 (2010). DOI: 10.1520/D0095-13E01. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or 3 contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Published as Manual of Petroleum Measurement Standards. Available from Standards volume information, refer to the standard’s Document Summary page on American Petroleum Institute (API), 1220 L. St., NW, Washington, DC 20005-4070, the ASTM website. http://www.api.org..
*A Summary of Changes section appears at the end of this standard
1 D95 − 13´1 3. Terminology NOTE 4—It is recommended to use a wide boiling range solvent with 10% boiling below 100°C to help to ensure an even distillation rate. 3.1 Definitions: 3.1.1 bituminous material, n—in petroleum technology, a 6.1.3 Volatile Spirits Solvent—The following volatile spirits black or dark-colored very viscous liquid or semi-solid com- solvents are acceptable: posed principally of high molecular weight condensed 6.1.3.1 Petroleum Spirit, with a boiling range from 100 to aromatic, or naphthenic compounds, or both. 120°C (212 to 248°F). (Warning—Flammable. Vapor harm- ful.) 4. Summary of Test Method 6.1.3.2 Iso-octane, of 95% purity or better. (Warning— Extremely flammable. Harmful if inhaled. Vapors may cause 4.1 The material to be tested is heated under reflux with a fire.) water-immiscible solvent, which co-distills with the water in the sample. Condensed solvent and water are continuously 6.2 Solvent Blank—The water content of the solvent shall be separated in a trap, the water settling in the graduated section determined by distilling an equivalent amount of the same of the trap and the solvent returning to the still. solvent used for the test sample in the distillation apparatus and testing as outlined in Section 10. The blank shall be determined 5. Significance and Use to the nearest scale division and used to correct the volume of 5.1 A knowledge of the water content of petroleum products water in the trap in Section 11. is important in the refining, purchase, sale, and transfer of 7. Apparatus products. 7.1 General—The apparatus comprises a glass or metal still, 5.2 The amount of water as determined by this test method a heater, a reflux condenser, and a graduated glass trap. The (to the nearest 0.05 or 0.1 volume %, depending on the trap still, trap, and condenser may be connected by any suitable size used) may be used to correct the volume involved in the method that produces a leakproof joint. Preferred connections custody transfer of petroleum products and bituminous mate- are ground joints for glass and O-rings for metal to glass. rials. Typical assemblies are illustrated in Fig. 1, Fig. 2, and Fig. 3. 5.3 The allowable amount of water may be specified in iTeh Standards The stills and traps should be chosen to cover the range of contracts. materials and water contents expected. On assembly, care shall be taken to prevent the joints from freezing or sticking. Always 6. Solvent-Carrier Liquid (https://standards.iteh.ai) 6.1 A water-immiscible solvent-carrier liquid that is mis- apply a very thin film of stopcock grease to prevent the glassware joints from seizing.
Document aromatic solvents Preview cible in the material being tested (see Table 1) shall be used. 7.2 Still—A glass or metal vessel with a short neck and 6.1.1 Aromatic Solvent—The following suitable joint for accommodating the reflux tube of the trap are acceptable: shall be used. Vessels of 500, 1000, and 2000-mL nominal 6.1.1.1 Industrial Grade Xylene—(Warning—Flammable. capacity have proved satisfactory. Vapor harmful.) ASTM D95-13e1 7.3 Heater—A suitable gas burner or electric heater may be https://standards.iteh.ai/catalog/standards/sist/bef5595e-e33b-4334-971e-15da019822a6/astm-d95-13e1 6.1.1.2 A blend of 20 volume % industrial grade toluene and used with the glass still. A gas ring burner with ports on the 80 volume % industrial grade xylene. (Warning—Flammable. Vapor harmful.) inside circumference shall be used with the metal still. The gas 6.1.1.3 Petroleum Naphtha or Coal Tar Naphtha, free of ring burner shall be of such dimensions that it may be moved water, yielding not more than 5% distillates at 125°C (257°F) and not less than 20% at 160°C (320°F) and with a relative density (specific gravity) not lower than 0.8545 at 15.56/ 15.56°C (60/60°F). (Warning—Extremely flammable. Harm- ful if inhaled. Vapors may cause fire.) 6.1.2 Petroleum Distillate Solvent—A petroleum distillate solvent containing at least 2% (V/V) aromatics and with an initial boiling point (IBP) greater than 80°C (176°F); and a final boiling point (FBP) below 250°C (482°F) shall be used. NOTE 3—Examples of suitable solvents include Types I and IV and Classes A and B of Specification D235.
TABLE 1 Type of Solvent-Carrier Liquid to Use Versus Material to
Be Tested Type of Solvent-Carrier Liquid Material to be Tested Aromatic asphalt, bitumen, tar, and related products
2 D95 − 13´1 ogy (NIST)4 traceable equipment. Verification shall be with a traceable 5 mL Micro Burette or Micro Pipette, readable to the nearest 0.01 mL. 9.1.1 In styles A, B, C, and D, as specified in Table 2 (Table 1 in Specification E123), each subdivision (that is, 0.1 mL through 1.0 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. 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 the case 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 and 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 into the apparatus and test in accordance with Section 10. When complete, discard the contents of the trap and add the FIG. 2 Two-millilitre Receiver Showing Alternative Connections to volume of water as specified as first test in Table 3 directly to Glass Still 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 the apparatus is satisfactory only if the trap readings are within up and down the vessel when testing materials that are likely to the tolerances specified in Table 3. foam or solidify in the still. iTeh Standards 9.3 A reading outside the permissible limits suggests a malfunction resulting from vapor leaks, too rapid boiling, glassware for use in this test(https://standards.iteh.ai) 7.4 Glassware—Dimensions and descriptions of typical method are provided in Specifi- inaccuracies in calibration of the trap, or ingress of extraneous cation E123. moisture. Eliminate these factors before repeating the verifica-
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NOTE 5—Instead of standardizing on a particular apparatus specifica- 10. Procedure tion with respect to dimensions and style, a given apparatus will be deemed satisfactory when accurate results are obtained by the standard NOTE 6—The precision of this test method will be affected by water addition technique described in Section 9. ASTM D95-13e1droplets adhering to surfaces in the apparatus and therefore not settling into the water trap to be measured. To minimize the problem, all apparatus 8.https://standards.iteh.ai/catalog/standards/sist/bef5595e-e33b-4334-971e-15da019822a6/astm-d95-13e1 Sampling must be cleaned chemically at least daily to remove surface films and debris, which hinder free drainage of water in the test apparatus. More 8.1 Sampling is defined as all steps required to obtain an frequent cleaning is recommended if the nature of samples being run aliquot of the contents of any pipe, tank, or other system and to causes persistent contamination. place the sample into the laboratory test container. Only 10.1 Measure a suitable amount of sample to an accuracy of representative samples obtained as specified in Practices 6 1% and transfer it to the still. D4057 (API MPMS Chapter 8.1) and D4177 (API MPMS 10.2 Measure ordinary liquid samples in a graduated cylin- Chapter 8.2) shall be used for this test method. der of an appropriate size. Rinse the material adhering to the 8.2 The size of the test portion should be based on the cylinder with one 50-mL and two 25-mL portions of the expected water content of the sample, such that the water yield solvent-carrier liquid (see Section 6 and Table 1). Drain the does not exceed the capacity of the trap (unless a trap with a cylinder thoroughly after the sample transfer and each rinsing. stopcock is used permitting excess water to be withdrawn into 10.3 Weigh solid or viscous materials directly into the still a graduated cylinder). and add 100 mL of the selected solvent-carrier liquid. In cases 8.3 Practice D5854 (API MPMS Chapter 8.3) contains of material with a low-water content when large samples must information on sampling and homogenization efficiency of be used, a solvent-carrier liquid volume in excess of 100 mL unknown mixers. This test method should not be followed may be necessary. without strict adherence to Practice D5854 (API MPMS 10.4 Glass beads or other boiling aids may be added, if Chapter 8.3). necessary, to reduce bumping. 10.5 Assemble the components of the apparatus, as illus- 9. Verification trated in Fig. 1, Fig. 2, and Fig. 3, choosing the trap in 9.1 The accuracy of the graduation marks on the trap shall be certified or verified, using only national or international 4 National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop standards, such as National Institute of Standards and Technol- 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.
