1、Designation: D 1266 98 (Reapproved 2003)e1Designation: 107/86An American National StandardStandard Test Method forSulfur in Petroleum Products (Lamp Method)1This standard is issued under the fixed designation D 1266; the number immediately following the designation indicates the year oforiginal adop
2、tion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.e1
3、NOTEWarning notes were editorially moved into the standard text in July 2003.1. Scope1.1 This test method covers the determination of total sulfurin liquid petroleum products in concentrations from 0.01 to 0.4mass % (Note 1). A special sulfate analysis procedure isdescribed in Annex A1 that permits
4、the determination of sulfurin concentrations as low as 5 mg/kg.NOTE 1The comparable lamp method for the determination of sulfurin liquefied petroleum gas is described in Test Method D 2784. For thedetermination of sulfur in heavier petroleum products that cannot beburned in a lamp, see the bomb meth
5、od (Test Method D 129) the quartztube method (IP 63), or the high-temperature method (Test MethodD 1552).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 blend
6、ing procedure (Section 10) is applicable to theanalysis of gas oils and distillate fuel oils, 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
7、in commercialgasoline do not interfere. A correction is given for the smallamount of acid resulting 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 s
8、ince nocorrection is provided in these cases.1.4 The values stated in SI units are to be regarded as thestandard.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 sa
9、fety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 129 Test Method for Sulfur in Petroleum Products (Gen-eral Bomb Method)2D 1193 Specification for Reagent Water3D 1229 Test Method for Rubber PropertyCompressi
10、onSet at Low Temperatures4D 1552 Test Method for Sulfur in Petroleum Products (HighTemperature Method)2D 2784 Test Method for Sulfur in Liquefied PetroleumGases (Oxy-Hydrogen Burner or Lamp)2E 11 Specification for Wire Cloth and Sieves for TestingPurposes52.2 Institute of Petroleum Standard:6IP 63 S
11、ulfur ContentThe Quartz Tube Method3. Summary of Test Method3.1 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 t
12、o sulfuric acid by means of hydrogen peroxide solutionwhich 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
13、 A2).1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved May 10, 2003. Published July 2003. Originallyapproved in 1969. Last previous edition approv
14、ed in 1998 as D 126698.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 09.01.5Annual Book of ASTM Standards, Vol 14.02.6Available from Institute of Petroleum (IP), 61 New Cavendish St., London,WIG 7AR, U.K.1Copyright ASTM Intern
15、ational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 Alternatively, the sample may be burned in air, 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
16、 or base-forming elements,other than sulfur, results by the volumetric and gravimetric finishesdescribed are equivalent within the limits of precision of the method.3.3 For sulfur contents below 0.01 mass % it is necessary todetermine the sulfate content in the absorber solution turbidi-metrically a
17、s barium sulfate (see Annex A1).4. Significance and Use4.1 This test method provides a means of monitoring thesulfur level of various petroleum products and additives. Thisknowledge can be used to predict performance, handling, orprocessing properties. In some cases the presence of sulfurcomponents
18、is beneficial to the product and monitoring thedepletion of sulfur compounds provides useful information. Inother cases the presence of sulfur compounds is detrimental tothe processing or use of the product.5. Apparatus5.1 Absorbers, Chimneys, Lamps, and Spray Traps (Fig. 1),as required are describe
19、d in detail in Annex A3. The standardflask and burner (Fig. A3.1) as shown is not suitable forburning highly aromatic mixtures without blending. The flaskand burner for aromatic samples (Fig. A3.1) permits burningthese samples directly without blending and may also be usedto burn nonaromatic samples
20、; with this lamp, a second portwith control valve in the burner manifold is required.5.2 Cotton Wicking7,8Clean, unused, uniform, twistedwhite cotton yarn of good quality. For the burner to burnaromatic samples use long staple, fine-spun, commercial finegrade.8,95.3 Manifold System, consisting of a
21、vacuum manifold withregulating device, valves, and so forth (Fig. 2) and a dualmanifold (burner and chimney) supplying a gas mixture ofapproximately 70 % carbon dioxide (CO2) and 30 % oxygen(O2) at regulated pressures. The vacuum manifold shall beconnected to a pump of sufficient capacity to permit
22、a steadygas flow of about 3 L/min through each absorber and tomaintain a constant manifold pressure of approximately 40 cmof water below atmospheric. The gas mixture in the chimneymanifold shall be maintained at a nearly constant pressure of 1to 2 cm of water and the burner manifold at approximately
23、 20cm of water. A suitable arrangement is shown in Fig. 2 anddescribed in Annex A3, but any other similar system can beused. Modifications of the manifold and associated equipmentfor burning samples in air are shown in Fig. A2.1 and describedin Annex A2.6. Reagents and Materials6.1 Purity of Reagent
24、sReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,7The sole source of supply of cotton wicking, yarn, white, 4strand (2 to 3mg/c
25、m/strand) known to the committee at this time is Koehler Instrument Co., 1595Sycamore Ave., Bohemia, NY 11716, or the type marketed by various suppliers inthe United Kingdom as 13s/14 ends, scoured, and bleached.8If you are aware of alternative suppliers, please provide this information toASTM Inter
26、national Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.9The sole source of supply of fine grade known to the committee at this time isThomas Scientific, P.O. Box 99, Swedesboro, NJ 08085-0099.FIG. 1 Illustrat
27、ive Sketch of the Assembled Lamp UnitD 1266 98 (2003)e12where such specifications are available.10Other 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.6.2 Purity of WaterUnless ot
28、herwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D 1193.6.3 Carbon Dioxide and OxygenThe carbon dioxide(CO2) and the oxygen (O2) shall each be at least 99.5 % pure.These gases shall meet the requirements of 9.5.6.4 Dilu
29、entThe 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 suitable (Note 9).6.5 Hydrochloric Acid (1 + 10)Mix
30、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 glass-stopperedbottle.6.7 Methyl Purple IndicatorAqueous
31、 solution containingapproximately 0.1 % active constituent.11(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 mL of saturated NaOH solution to 1 L (Note 3), using f
32、orthis 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 protect tominimize contamination by CO2from the air.
33、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 equivalent to 0.0010 g of sulfur. In this case, thefactor 16
34、.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 instrument calibration curve. These (QC)samples are to be us
35、ed 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. Preparation of Apparatus7.1 When the apparatus is first asse
36、mbled, charge theabsorber with 30 6 2 mL of water. Adjust the individual valvesbetween the vacuum manifold and spray traps so that approxi-mately 3 L of air per minute will be drawn through eachabsorber when the chimney outlets are open to the atmosphere,while maintaining the pressure in the vacuum
37、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 pressure and vacuumregulators is indicated in Fig. 2, and during operation a slowleak of gas should be maintained through them.NOTE 4In
38、use, place 300 to 400 mL of H2O2solution (1 + 19) in thescrubber. Since the manifold manometer also serves as a scrubber at theend of the test to remove CO2from the absorbent use H2O2solution(1 + 19) as the manometric liquid. Replace weekly or whenever thevolume becomes appreciably less than the ori
39、ginal.7.2 Neutralize the H2O2solution (1 + 19) immediately be-fore use. As 30 mL of the solution is needed, transfer to a10Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemi
40、cal Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.11Fleisher Methyl Purple Indicator, U. S. Patent No. 2416619 may be obtainedfrom Harry Fleisher
41、 Chemical Co., Benjamin Franklin Station, Washington, DC20044, or from any chemical supply company handling Fleisher Methyl Purple.FIG. 2 Schematic Diagram of CO2-O2Supply Manifold and Lamp SystemD 1266 98 (2003)e13beaker multiples of 30 mL sufficient for the number ofabsorbers to be used simultaneo
42、usly. Add 1 drop of methylpurple indicator solution for each 100 mL of H2O2solution andthen add 0.05 N NaOH solution dropwise until the colorchanges from purple to light green.7.3 Introduce 30 6 2 mL of the freshly neutralized H2O2solution (1 + 19) into the larger bulb of each absorber. Inaddition,
43、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.7.4 With the burner control valves closed, the va
44、lve 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 arebein
45、g 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 CO2-O2gas escapes at thepressure regulator, a small stream of air enters at the vacuumregula
46、tor, and the pressure in the chimney manifold is 1 to 2 cmof water. Minor adjustment of the vacuum regulator andvacuum control valve may be necessary to achieve thiscondition (Note 5).NOTE 5It is convenient to balance the gas flow system by regulatingthe pressure in the vacuum manifold. This is done
47、 by raising or loweringthe air inlet tube in the vacuum regulator by sliding it in a rubber sleeve.7.5 Cut the wicking to 30-cm lengths. Use the number oflengths dictated by the sample (see Section 8); fold the wickingonce to give a 15-cm long bundle for threading the burners.Thread the required num
48、ber of burners by inserting the loopedends into the top of the inner tube of the burner. Draw thewicking through by means of a metal hook. Trim the wick asclose as possible to the top of the burner with a pair of sharpscissors. It is essential that thoroughly cleaned burners and newwicking be used f
49、or each test.8. Control of Combustion8.1 Most types of liquid samples burn with a luminousyellow flame, the size and shape of which is dependent on thegas flow to the burner, the volatility of the material, thetightness of the fit of the wick in the burner tube, and theposition of the top of the wick relative to the top of the burner.It is preferable that the latter two variables be fixed withrelation to the first before burning is started so that the flamecan be controlled by variation in the rate of CO2-O2flow.8.2 Highly volatile samples require a tight-fitting w
