ASTM D1266-2013 Standard Test Method for Sulfur in Petroleum Products (Lamp Method)《测定石油产品中硫的标准试验方法(燃灯法)》.pdf

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1、Designation: D1266 07D1266 13Designation: 107/86Standard Test Method forSulfur in Petroleum Products (Lamp Method)1This standard is issued under the fixed designation D1266; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year

2、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 This test method covers the deter

3、mination of total sulfur in liquid petroleum products in concentrations from 0.01 to 0.4mass % (Note 1). A special sulfate analysis procedure is described in Annex A1 that permits the determination of sulfur inconcentrations as low as 5 mg/kg.NOTE 1The comparable lamp method for the determination of

4、 sulfur in liquefied petroleum gas is described in Test Method D2784. For thedetermination of sulfur in heavier petroleum products that cannot be burned in a lamp, see the bomb high pressure decomposition device method (TestMethod D129) the quartz tube method (IP 63), or the high-temperature method

5、(Test Method D1552).1.2 The direct burning procedure (Section 9) is applicable to the analysis of such materials as gasoline, kerosine, naphtha, andother liquids that can be burned completely in a wick lamp. The blending procedure (Section 10) is applicable to the analysis ofgas oils and distillate

6、fuel oils, naphthenic acids, alkyl phenols, high sulfur content petroleum products, and many other materialsthat cannot be burned satisfactorily by the direct burning procedure.1.3 Phosphorus compounds normally present in commercial gasoline do not interfere.Acorrection is given for the small amount

7、of acid resulting from the combustion of the lead anti-knock fluids in gasolines. Appreciable concentrations of acid-forming orbase-forming elements from other sources interfere when the titration procedure is employed since no correction is provided inthese cases.1.4 The values stated in SI units a

8、re to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practi

9、ces and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D129 Test Method for Sulfur in Petroleum Products (General High Pressure Decomposition Device Method)D1193 Specification for Reagent WaterD1552 Test Method for Sulfur in Petroleum Pro

10、ducts (High-Temperature Method)D2784 Test Method for Sulfur in Liquefied Petroleum Gases (Oxy-Hydrogen Burner or Lamp)D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System PerformanceD6300 Practice for Determination of Pr

11、ecision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6792 Practice for Quality System in Petroleum Products and Lubricants Testing LaboratoriesE11 Specification for Woven Wire Test Sieve Cloth and Test Sieves2.2 Energy Institute Standard:3IP 63 Sulfur ContentThe Quartz

12、 Tube Method1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved Dec. 1, 2007June 15, 2013. Published January 2008August 2013. Originally approved

13、in 1969. Last previous edition approved in 20032007 asD126698(2003)D1266 07.1. DOI: 10.1520/D1266-07.10.1520/D1266-13.2 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

14、 the standards Document Summary page on the ASTM website.3 Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have b

15、een 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 official docume

16、nt.*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 States13. Summary of Test Method3.1 The sample is burned in a closed system, using a suitable lamp (Fig. 1) and an artificial

17、 atmosphere composed of 70 %carbon dioxide and 30 % oxygen to prevent formation of nitrogen oxides.The oxides of sulfur are absorbed and oxidized to sulfuricacid by means of hydrogen peroxide solution which is then flushed with air to remove dissolved carbon dioxide. Sulfur as sulfatein the absorben

18、t is determined acidimetrically by titration with standard sodium hydroxide solution, or gravimetrically byprecipitation as barium sulfate (see Annex A2).3.2 Alternatively, the sample may be burned in air, the sulfur as sulfate in the absorbent being determined by precipitation asbarium sulfate for

19、weighing (see Annex A2).NOTE 2In the absence of acid-forming or base-forming elements, other than sulfur, results by the volumetric and gravimetric finishes described areequivalent within the limits of precision of the method.3.3 For sulfur contents below 0.01 mass % it is necessary to determine the

20、 sulfate content in the absorber solutionturbidimetrically as barium sulfate (see Annex A1).4. Significance and Use4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. Thisknowledge can be used to predict performance, handling, or processi

21、ng properties. In some cases the presence of sulfurcomponents is beneficial to the product and monitoring the depletion of sulfur compounds provides useful information. In othercases the presence of sulfur compounds is detrimental to the processing or use of the product.5. Apparatus5.1 Absorbers, Ch

22、imneys, Lamps, and Spray Traps (Fig. 1), as required are described in detail in Annex A3. The standard flaskand burner (Fig. A3.1) as shown is not suitable for burning highly aromatic mixtures without blending. The flask and burner foraromatic samples (Fig. A3.1) permits burning these samples direct

23、ly without blending and may also be used to burn nonaromaticsamples; with this lamp, a second port with control valve in the burner manifold is required.5.2 Cotton Wicking4,5Clean, unused, uniform, twisted white cotton yarn of good quality. For the burner to burn aromaticsamples use long staple, fin

24、e-spun, commercial fine grade.5,65.3 Manifold System, consisting of a vacuum manifold with regulating device, valves, and so forth (Fig. 2) and a dual manifold(burner and chimney) supplying a gas mixture of approximately 70 % carbon dioxide (CO2) and 30 % oxygen (O2) at regulatedpressures. The vacuu

25、m manifold shall be connected to a pump of sufficient capacity to permit a steady gas flow of about 3 L/minthrough each absorber and to maintain a constant manifold pressure of approximately 40 cm of water below atmospheric. The gas4 The sole source of supply of cotton wicking, yarn, white, 4strand

26、(2 to 3 mg/cm/strand) known to the committee at this time is Koehler Instrument Co., 1595 SycamoreAve., Bohemia, NY 11716, or the type marketed by various suppliers in the United Kingdom as 13s/14 ends, scoured, and bleached.5 If you are aware of alternative suppliers, please provide this informatio

27、n to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.6 The sole source of supply of fine grade known to the committee at this time is Thomas Scientific, P.O. Box 99, Swedesboro, NJ 08085-0099.

28、FIG. 1 Illustrative Sketch of the Assembled Lamp UnitD1266 132mixture in the chimney manifold shall be maintained at a nearly constant pressure of 1 to 2 cm of water and the burner manifoldat approximately 20 cm of water. A suitable arrangement is shown in Fig. 2 and described in Annex A3, but any o

29、ther similarsystem can be used. Modifications of the manifold and associated equipment for burning samples in air are shown in Fig. A2.1and described in Annex A2.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is inten

30、ded that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.7 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use with

31、out lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType II or Type III of Specification D1193.6.3 Carbon Dioxide and OxygenThe carbon dioxide (CO2) and the oxygen (O2) shall each be

32、 at least 99.5 % pure. Thesegases shall meet the requirements of 9.5.6.4 DiluentThe diluent used shall have a sulfur content less than 0.001 mass %, be completely miscible with the sample tobe analyzed, and permit burning at a moderate rate without smoking. Normal heptane, isooctane, and absolute et

33、hyl alcohol havebeen found suitable (Note 9).6.5 Hydrochloric Acid (1 + 10)Mix 1 volume of concentrated hydrochloric acid (HCl, relative density 1.19) with 10 volumesof water.6.6 Hydrogen Peroxide Solution (1 + 19) Mix 1 volume of concentrated hydrogen peroxide (H2O2, 30 %) with 19 volumesof water.

34、Store in a dark-colored glass-stoppered bottle.6.7 Methyl Purple IndicatorAqueous solution containing approximately 0.1 % active constituent.8 (Not methyl violet.)6.8 Sodium Hydroxide Solution (100 g/L)Dissolve 100 g of sodium hydroxide (NaOH) in water and dilute to 1 L.6.9 Sodium Hydroxide, Standar

35、d Solution (0.05 M)Dilute 2.8 mL of saturated NaOH solution to 1 L (Note 3), using for thispurpose the clear saturated solution decanted after standing long enough to permit any precipitate to settle out. Standardize bytitration against standard acid, using the methyl purple indicator. Store in an a

36、lkali-resistant glass bottle and protect to minimizecontamination by CO2 from the air. Use only pure gum rubber tubing for connections between the storage bottles and burets.NOTE 3The calculation of results can be simplified by adjusting the molarity of the NaOH solution to 0.0624 6 0.0001. Then 1 m

37、L of the NaOHsolution will be equivalent to 0.0010 g of sulfur. In this case, the factor 16.03M in the calculation (see 12.1) becomes 1.000.7 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed

38、bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.8 Fleisher Methyl Purple Indicator, U. S. Patent No. 2416619 may be obtai

39、ned from Harry Fleisher Chemical Co., Benjamin Franklin Station, Washington, DC 20044, orfrom any chemical supply company handling Fleisher Methyl Purple.FIG. 2 Schematic Diagram of CO2-O2 Supply Manifold and Lamp SystemD1266 1336.10 Quality Control (QC) Sample(s), preferably are portions of one or

40、more liquid petroleum materials or product standardsof known sulfur content that were not used in the generation of the instrument calibration curve. These (QC) samples are to beused to check the validity of the testing process as described in Section 12. An ample supply of QC sample material shall

41、beavailable for the intended period of use, and must be homogeneous and stable under the anticipated storage conditions.7. Preparation of Apparatus7.1 When the apparatus is first assembled, charge the absorber with 30 6 2 mL of water. Adjust the individual valves betweenthe vacuum manifold and spray

42、 traps so that approximately 3 L of air per minute will be drawn through each absorber when thechimney outlets are open to the atmosphere, while maintaining the pressure in the vacuum manifold at approximately 40 cm ofwater below atmospheric. When all adjustments have been made, remove the water fro

43、m the absorbers. The height of the liquidsin the pressure and vacuum regulators is indicated in Fig. 2, and during operation a slow leak of gas should be maintained throughthem.NOTE 4In use, place 300 to 400 mL of H2O2 solution (1 + 19) in the scrubber. Since the manifold manometer also serves as a

44、scrubber at the endof the test to remove CO2 from the absorbent use H2O2 solution (1 + 19) as the manometric liquid. Replace weekly or whenever the volume becomesappreciably less than the original.7.2 Neutralize the H2O2 solution (1 + 19) immediately before use. As 30 mL of the solution is needed, t

45、ransfer to a beakermultiples of 30 mLsufficient for the number of absorbers to be used simultaneously.Add 1 drop of methyl purple indicator solutionfor each 100 mL of H2O2 solution and then add 0.05 N NaOH solution dropwise until the color changes from purple to light green.7.3 Introduce 30 6 2 mL o

46、f the freshly neutralized H2O2 solution (1 + 19) into the larger bulb of each absorber. In addition,for each set of samples burned, prepare an extra absorber for use as a control blank. Attach the spray traps and chimneys andconnect them to their respective manifolds by means of sulfur-free rubber t

47、ubing. Close the chimney openings by means of corks.7.4 With the burner control valves closed, the valve to the vacuum regulator fully open, and the pressure in the vacuum manifoldadjusted to approximately 40 cm of water below atmospheric, turn on the CO2 and O2 supplies. (WarningA hazardous(explosi

48、ve) condition can result if the CO2 supply is interrupted and the O2 flow is continued while samples are being burned. Theinstallation of suitable warning or control equipment is recommended.) Adjust the chimney manifold control valve so that, at therequired rate of flow through the absorbers, only

49、a small stream of CO2-O2 gas escapes at the pressure regulator, a small streamof air enters at the vacuum regulator, and the pressure in the chimney manifold is 1 to 2 cm of water. Minor adjustment of thevacuum regulator and vacuum control valve may be necessary to achieve this condition (Note 5).NOTE 5It is convenient to balance the gas flow system by regulating the pressure in the vacuum manifold. This is done by raising or lowering theair inlet tube in the vacuum regulator by sliding it in a rubber sleeve.7.5 Cut the wicking to 30-cm lengths. Use the numb