ap Designation: D 95 - 83 (Reapproved 1990)" Dp Designation MPMS Chapter 10.5 ®@ Designation 74/52 Standard Test Method for tillation “This nandard issued uoder the Sed designation D9S; the number iumedately folowing the designation indicates te year of a ance tian oy in tnt of evaion, te yea ofltTevson. A mumber in pcothoss inate the yar oat eappoval. A ‘Sinenpt ep (0 iadetes an eto change since the ast revision or reapproval “This st metho has een approved by de sponsoring comunltes and accepted by the cooperating organization i accordance wit cenublished procedures ‘his test method hasbeen approved for use by agencies ofthe Deparment of Defense and for listing in the DoD Index of Specifications and Standard {7 Neore= Poagraphs 13 and 112 were added enor in May 1990 1. Scope 1.1 This test method covers the determination of water in petroleum products, tars, and other bituminous materials by the distillation method. The specific products considered during the development of this test method are listed in Table 1. For bituminous emulsions refer to Test Method 1D 244, This test method, along with ASTM Test Method 14006 (API Chapter 10.2 and IP 358), supersedes the previous edition of ASTM Test Method D 95 (API Standard 2360, IP 74). Nore 1—With some types of ol, satisfactory results may be obtained from ASTM Test Method D4007 (API Chapter 10.3, 1P 358, and ASTM Method D 1796 API Chapter 10.) 1.2 This standard may involve hazardous materials, oper- cations, and equipment. This standard does not purport to ‘address all ofthe safety problems associated with its use. It is the responsibility of the user of this standard to establish ‘appropriate safety and health practices and determine the ‘applicability of regulatory limitations prior to use, For specific hazard statements, see 5.1.1.2 and 5.1.1.3. 1.3 The values stated in SI units are to be regarded as the standard, The values in parentheses are for information only. 2, Referenced Documents 2.1 ASTM Standards: 186 Method for Distillation of Petroleum Products? 1244 Test Methods for Emulsified Asphalts? “This est method is under the jurction of ASTM Commitee D2 oo ‘pazleum Produc ané Lulbicats and API Commitoe on Ptcoleum Measust- ‘pom ands the dee spony of Subcommitee D202 on Joint ASTM-APL Committe on Sint Peoieum Measurement. ‘Cane ison approved March 2, 1985, Publised January 1984, Oxginally published ws D9521. Las peeviows edition D 95 ~70 (1980). nme! Book of ASTM Standards, Vos 08.01 and 06.03. 2 mua Book af ASTM Standards, Vol 04.03, : 36 Water in Petroleum Products and Bituminous Materials by ng en rt ieee vot ea rises 1D 1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)* 14006 Test. Method for Water in Crude Oil by Distillation* 14007 Test Method for Water and Sediment in Crude Oil by the Centrifuge Method (Laboratory Procedure)® 14057 Practice for Manual Sampling of Petroleum and Petroleum Products* 14177 Method for Automatic Sampling of Petroleum and Petroleum Products* E 123 Specification. for, Apparatus for Determination of Water by Distillation* 2.2. API Manual of Petroleum Measurements Standards:* ‘Chapter 8.1 Manual Sampling of Petroleum and Petro- eum Products (ASTM Practice D 4057) Chapter 8.2 Automatic Sampling of Petroleum and Petro- eum Products (ASTM Test Method D 4177) Chapter 10.2 Determination of Water in Crude Oil by the Distillation Method (ASTM Test Method D 4006) Chapter 10.3 Determination of Water and Sediment in ‘Crude Oil by the Centrifuge Method (Laboratory Proce- duse) (ASTM Test Method D 4007) Chapter 10.6 Determination of Water and Sediment in Fuel Oil by the Centrifuge Method (ASTM Test Method D 1796) 23. British Standard:” 756 Dean and Stark Apparatus 3. Summary of ‘Test Method 3.1 ‘The material to be tested is heated under reflux with a * Annual Book of ASTM Standards, Vo 081 5 Amel Book of ASTM Standards. Wa 05.03. «Aula rom Amertan Povceum Fst 220 Lt, NW., Washington, be 20005, ~ avalae rom American National Standards Isis, 1430 Broadway. New ‘York, NY 10018.eae RS ipa ot Save Carrara Taio we bo Tens “eomatie ‘sphaltar, coe ter, wat gas ter, road tar, catback btm, Iqud esphet, tar 0s Petraum dtiate ‘oad ol, fe! ol, ubrestag o, petroleum ‘sonatas Vole splits iain ease water-immiscible solvent, which co-distills with the water in the sample, Condensed solvent and water ate continuously separated in a trap, the water settling in the graduated section of the trap and the solvent returning to the still. 4. Significance and Use 4.1 A knowledge of the water content of petroleum products is important in the refining, purchase, sale, and transfer of products, 4.2 The amount of water as determined by this method (to the nearest 0.05 volume %) shall be used to correct the volume involved in the custody transfer of oil. 5. Solvent-Carrier Liquid S.A solvent-carrier liquid appropriate to the material being tested (see Table 1) shall be used, 5.1.1 Aromatic Solvent—The following aromatic solvents are acceptable: 3.14.1 Industrial Grade Xylene. 5.1.1.2 A blend of 20 volume % industrial grade toluene and 80 volume % industrial grade xylene (Warning—Flam- ‘mable. Vapor harmful. See Annex Al.1.) 5.1.1.3 Petroleum or Coal Tar Naphtha (Warning—Ex- tremely flammable. Harmful if inhaled. Vapors may cause fire. See Annex), free of water, yielding not more than 5% distillates at 125°C (257°F) and not less than 20% at 160°C (320°F) when tested by Method D 86 and with a relative density (specific gravity) not lower than 0.8545 at 15.56/ 15.56°C (60/60°F).. 5.1.2 Petroleum Distillate Solvent—A petroleum distillate XS pees S) settee RECEIVER, ae RK (GPrIONAL) \--Stass C Po sent Fig. 1 ‘Typical Assembly with Glass Stil (Deen and Stark) TT 100 maa ‘SCALE (APPROX | Gnapuation (=| itenvacs eos me Fuoinr: PLAIN om I FIG. 2 Two-militre Receiver Showing Alternative Connections ‘to Glass Stil solvent, $% boiling between 90° and 100°C (194° and 212°F) and 90% distilling below 210°C (410°F), shall be used. 5.1.3 Volatile Spirits Solveni—The following volatile spirits solvents are acceptable: 5.1.3.1 Petroleum Spirit, with a boiling range of 100° to 120°C (212 to 248°F). 3.1.3.2 Isooctane, of 95% purity or better. 6. Apparatus 6.1 General—The apparatus comprises a glass or metal still, a heater, a reflux condenser, and a graduated glass trap. ‘The stil, ap, and condenser may be connected by any suitable method that produces a leakproof joint, Preferred connections are ground joints for glass and O-rings for metal to glass. Typical assembiies are illustrated in Figs. 1, 2, and 3, ‘The stills and traps should be chosen to cover the range of materials and water contents expected. 6.2 Still—A glass or metal vessel with a short neck and suitable joint for accommodating the reflux tube of the trap shall be used. Vessels of $00, 1000, and 2000-mL nominal ‘capacity have proved satisfactory. 6.3 Heater—A suitable gas burner or electric heater may be used with the glass still. A gas ring burner with ports on the inside circumference shall be used with the metal still. ‘The gas ring burner shall be of such dimensions that it may bbe moved up and down the vesse! when testing materials that are likely to form or solidify in the stil. 6.4 Glassware—Dimensions and descriptions of typical sglassware for use in this method are provided in Specification E123 and British Standard 756, A straight water-cooled ‘condenser with a length of 400 mL is recommended in place of the length of 300 mL specified in British Standard 756. Nore 2—Instead of standardizing on a particular apparatus speciti- cation with respect to dimensions and style, a given apparatus will be ‘deemed satisfactory when accurate results are obtained by the standard ‘dition technique described in Section 7. 7. Standardization 7.1 A given assembly of apparatus will be considered100 MM ‘SEALE (APPROX) METAL sTiLL—— satisfactory when accurate readings are obtained from the ‘addition of known amounts of water from a calibrated buret or pipet to a clear hydrocarbon oil and tested in accordance with Section 9. 7.2. The readings shall be judged accurate if the permis. ‘TABLE 2 Permissible Limits in Mites Capecly of Volume of Water Perris Lins for Recewer at Aéed to Fas ‘Recover ster 20°C mare 20°C 2 7 7208 10 1 ear 10 5 5x02 2 2 12802 RING BURNER. Note—Trap shal be 1520 16 me n inside cametor FIG. 3 Typleal Assomblies with Metal Stil sible limits given in Table 2 for the various sized graduated ‘raps are not exceeded. 73 A reading outside the permissible limits suggests @ maifunetion resulting from vapor leaks, too rapid boiling, inaccuracies in calibration of the trap, or ingress of extra- neous moisture, Eliminate these factors before repeating the standardization. 8, Sampling 8.1 Sampling is defined as all steps required to obtain an aliquot of the contents of any pipe, tank, or other system and ‘o place the sampleinto the laboratory test container. Only representative samples obtained as specified in Practice 1D 4037 (API Chapter 8,1) and Method D 4177 (API Chapterih 0 95 ANNEX (Mandatory Information) Al. PRECAUTIONARY STATEMENTS AL. Xylene/Toluene ‘Vapors may cause flash fre. ‘Warning—Flammable. Vapor harmful Keep away from heat, sparks, and open flame. Keep away from heat, sparks, and open flame. Keep container closed. Keep container closed. Use with adequate ventilation. Use with adequate ventilation, Avoid a build-up of vapors and eliminate all sources of Avoid breathing of vapor or spray mist. ignition, especially nonexplosion proof electrical apparatus Avoid prolonged or repeated contact with skin and heaters. Avoid prolonged breathing of vapors or spray mist. Al2 Naphthe Avoid prolonged or repeated skin contact ‘Warning—Extremely flammable. Harmfl if inhaled, The American Sooty for Testing nd Materials tates no postin respecting the vay of any patent rights asserted in conection wih any tem menaned inthis standard. Users otis starard aro expressly advised tat ceeamiatono te vay of ery such Patert rights, andthe rk of nsngamar of euch rights, are ena the ow respons. 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