ASTM D1266-2018 Standard Test Method for Sulfur in Petroleum Products (Lamp Method)《石油产品中硫的标准试验方法(Lamp法)》.pdf

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1、Designation: D1266 18Designation: 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 of last

2、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 U.S. Department of Defense.1. Scope*1.1 This test method covers the determin

3、ation of total sulfurin liquid petroleum products in concentrations from 0.01 % to0.4 % by mass (Note 1). A special sulfate analysis procedure isdescribed in Annex A1 that permits the determination of sulfurin concentrations as low as 5 mg kg.NOTE 1The comparable lamp method for the determination of

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

5、ethod D1552).1.2 The direct burning procedure (Section 9) is applicable tothe analysis of such materials as gasoline, kerosine, naphtha,and other liquids that can be burned completely in a wick lamp.The blending procedure (Section 10) is applicable to theanalysis of gas oils and distillate fuel oils

6、, naphthenic acids,alkyl phenols, high sulfur content petroleum products, andmany other materials that cannot be burned satisfactorily by thedirect burning procedure.1.3 Phosphorus compounds normally present in commercialgasoline do not interfere. A correction is given for the smallamount of acid re

7、sulting from the combustion of the leadanti-knock fluids in gasolines. Appreciable concentrations ofacid-forming or base-forming elements from other sourcesinterfere when the titration procedure is employed since nocorrection is provided in these cases.1.4 The values stated in SI units are to be reg

8、arded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental prac

9、tices and deter-mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides an

10、d Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D129 Test Method for Sulfur in Petroleum Products (Gen-eral High Pressure Decomposition Device Method)D1193 Specification for Reagent WaterD1552 Test Method

11、 for Sulfur in Petroleum Products byHigh Temperature Combustion and Infrared (IR) Detec-tion or Thermal Conductivity Detection (TCD)D2784 Standard Test Method for Sulfur in Liquefied Petro-leum Gases (Oxy-Hydrogen Burner or Lamp) (Withdrawn2016)3D4057 Practice for Manual Sampling of Petroleum andPet

12、roleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Te

13、st Methods for Petroleum Products andLubricantsD6792 Practice for Quality Management Systems in Petro-leum Products, Liquid Fuels, and Lubricants TestingLaboratoriesE11 Specification for Woven Wire Test Sieve Cloth and TestSieves1This test method is under the jurisdiction of ASTM Committee D02 onPet

14、roleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved April 1, 2018. Published April 2018. Originallyapproved in 1969. Last previous edition approved in 2013 as D1266 13. DOI:10.1520/D1266-18.2For reference

15、d ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.

16、astm.org.*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 StatesThis international standard was developed in accordance with internationally recognized principles on standardiza

17、tion established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.12.2 Energy Institute Standard:4IP 63 Sulfur ContentThe Quartz Tube Method3. Summary of Test Met

18、hod3.1 The sample is burned in a closed system, using asuitable lamp (Fig. 1) and an artificial atmosphere composed of70 % carbon dioxide and 30 % oxygen to prevent formation ofnitrogen oxides. The oxides of sulfur are absorbed and oxi-dized to sulfuric acid by means of hydrogen peroxide solutionwhi

19、ch is then flushed with air to remove dissolved carbondioxide. Sulfur as sulfate in the absorbent is determinedacidimetrically by titration with standard sodium hydroxidesolution, or gravimetrically by precipitation as barium sulfate(see Annex A2).3.2 Alternatively, the sample may be burned in air,

20、thesulfur as sulfate in the absorbent being determined by precipi-tation as barium sulfate for weighing (see Annex A2).NOTE 2In the absence of acid-forming or base-forming elements,other than sulfur, results by the volumetric and gravimetric finishesdescribed are equivalent within the limits of prec

21、ision of the method.3.3 For sulfur contents below 0.01 % by mass, it is neces-sary to determine the 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 thesulfur level of various petrole

22、um products and additives. Thisknowledge can be used to predict performance, handling, orprocessing properties. In some cases the presence of sulfurcomponents is beneficial to the product and monitoring thedepletion of sulfur compounds provides useful information. Inother cases the presence of sulfu

23、r compounds is detrimental tothe processing or use of the product.5. Apparatus5.1 Absorbers, Chimneys, Lamps, and Spray Traps (Fig. 1),as required are described in detail in Annex A3. The standardflask and burner (Fig. A3.1) as shown is not suitable forburning highly aromatic mixtures without blendi

24、ng. The flaskand burner for aromatic samples (Fig. A3.1) permits burningthese samples directly without blending and may also be usedto burn nonaromatic samples; with this lamp, a second portwith control valve in the burner manifold is required.5.2 Cotton Wicking5,6Clean, unused, uniform, twistedwhit

25、e cotton yarn of good quality. For the burner to burnaromatic samples use long staple, fine-spun, commercial finegrade.6,75.3 Manifold System, consisting of a vacuum manifold withregulating device, valves, and so forth (Fig. 2) and a dualmanifold (burner and chimney) supplying a gas mixture ofapprox

26、imately 70 % carbon dioxide (CO2) and 30 % oxygen(O2) at regulated pressures. The vacuum manifold shall beconnected to a pump of sufficient capacity to permit a steadygas flow of about 3 L min through each absorber and tomaintain a constant manifold pressure of approximately 40 cmof water below atmo

27、spheric. The gas mixture in the chimneymanifold shall be maintained at a nearly constant pressure of1 cm to 2 cm of water and the burner manifold at approxi-mately 20 cm of water.Asuitable arrangement is shown in Fig.2 and described in Annex A3, but any other similar system canbe used. Modifications

28、 of the manifold and associated equip-ment for burning samples in air are shown in Fig. A2.1 anddescribed in Annex A2.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the spe

29、cifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.8Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination

30、.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D1193.4Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,U.K., http:/www.energyinst.org.5The sole source of supply of co

31、tton wicking, yarn, white, 4-strand (2 mg cm-strand to 3 mg cm strand) known to the committee at this time is KoehlerInstrument Co., 1595 Sycamore Ave., Bohemia, NY 11716, or the type marketed byvarious suppliers in the United Kingdom as 13s/14 ends, scoured, and bleached.6If you are aware of altern

32、ative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.7The sole source of supply of fine grade known to the committee at this time isThomas Scient

33、ific, P.O. Box 99, Swedesboro, NJ 08085-0099.8Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, D

34、orset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Illustrative Sketch of the Assembled Lamp UnitD1266 1826.3 Carbon Dioxide and OxygenThe carbon dioxide(CO2) and the oxygen (O2) shall each be at least 99.5 % pure.Th

35、ese gases shall meet the requirements of 9.5.6.4 DiluentThe diluent used shall have a sulfur contentless than 0.001 mass %, be completely miscible with thesample to be analyzed, and permit burning at a moderate ratewithout smoking. Normal heptane, isooctane, and absoluteethyl alcohol have been found

36、 suitable (Note 9).6.5 Hydrochloric Acid (1 + 10)Mix 1 volume of concen-trated hydrochloric acid (HCl, relative density 1.19) with 10volumes of water.6.6 Hydrogen Peroxide Solution (1 + 19) Mix 1 volumeof concentrated hydrogen peroxide (H2O2, 30 %) with 19volumes of water. Store in a dark-colored gl

37、ass-stopperedbottle.6.7 Methyl Purple IndicatorAqueous solution containingapproximately 0.1 % active constituent.9(Not methyl violet.)6.8 Sodium Hydroxide Solution (100 g/L)Dissolve 100 gof sodium hydroxide (NaOH) in water and dilute to 1 L.6.9 Sodium Hydroxide, Standard Solution (0.05 M)Dilute2.8 m

38、L of saturated NaOH solution to 1 L (Note 3), using forthis purpose the clear saturated solution decanted after standinglong enough to permit any precipitate to settle out. Standardizeby titration against standard acid, using the methyl purpleindicator. Store in an alkali-resistant glass bottle and

39、protect tominimize contamination by CO2from the air. Use only puregum rubber tubing for connections between the storage bottlesand burets.NOTE 3The calculation of results can be simplified by adjusting themolarity of the NaOH solution to 0.0624 6 0.0001. Then 1 mL of theNaOH solution will be equival

40、ent to 0.0010 g of sulfur. In this case, thefactor 16.03M in the calculation (see 12.1) becomes 1.000.6.10 Quality Control (QC) Sample(s), preferably are por-tions of one or more liquid petroleum materials or productstandards of known sulfur content that were not used in thegeneration of the instrum

41、ent calibration curve. These (QC)samples are to be used to check the validity of the testingprocess as described in Section 12. An ample supply of QCsample material shall be available for the intended period ofuse, and must be homogeneous and stable under the anticipatedstorage conditions.7. Prepara

42、tion of Apparatus7.1 Take samples in accordance with the instructions inPractices D4057 or D4177.7.2 When the apparatus is first assembled, charge theabsorber with 30 mL 6 2 mL of water. Adjust the individualvalves between the vacuum manifold and spray traps so thatapproximately 3 Lof air per minute

43、 will be drawn through eachabsorber when the chimney outlets are open to the atmosphere,while maintaining the pressure in the vacuum manifold atapproximately 40 cm of water below atmospheric. When alladjustments have been made, remove the water from theabsorbers. The height of the liquids in the pre

44、ssure and vacuumregulators is indicated in Fig. 2, and during operation a slowleak of gas should be maintained through them.NOTE 4In use, place 300 mL to 400 mL of H2O2solution (1 + 19) inthe scrubber. Since the manifold manometer also serves as a scrubber atthe end of the test to remove CO2from the

45、 absorbent use H2O2solution(1 + 19) as the manometric liquid. Replace weekly or whenever thevolume becomes appreciably less than the original.7.3 Neutralize the H2O2solution (1 + 19) immediately be-fore use. As 30 mL of the solution is needed, transfer to abeaker multiples of 30 mL sufficient for th

46、e number of absorb-ers to be used simultaneously. Add 1 drop of methyl purpleindicator solution for each 100 mL of H2O2solution and thenadd 0.05 N NaOH solution dropwise until the color changesfrom purple to light green.7.4 Introduce 30 mL 6 2 mL of the freshly neutralizedH2O2solution (1 + 19) into

47、the larger bulb of each absorber. In9Fleisher Methyl Purple Indicator, U. S. Patent No. 2416619 may be obtainedfrom Harry Fleisher Chemical Co., Benjamin Franklin Station, Washington, DC20044, or from any chemical supply company handling Fleisher Methyl Purple.FIG. 2 Schematic Diagram of CO2-O2Suppl

48、y Manifold and Lamp SystemD1266 183addition, for each set of samples burned, prepare an extraabsorber for use as a control blank. Attach the spray traps andchimneys and connect them to their respective manifolds bymeans of sulfur-free rubber tubing. Close the chimney open-ings by means of corks.7.5

49、With the burner control valves closed, the valve to thevacuum regulator fully open, and the pressure in the vacuummanifold adjusted to approximately 40 cm of water belowatmospheric, turn on the CO2and O2supplies. (WarningAhazardous (explosive) condition can result if the CO2supply isinterrupted and the O2flow is continued while samples arebeing burned. The installation of suitable warning or controlequipment is recommended.) Adjust the chimney manifoldcontrol valve so that, at the required rate of flow through theabsorbers, only a small stream of CO2O2gas e