ANSI ASTM D1266-2013 Standard Test Method for Sulfur in Petroleum Products (Lamp Method).pdf

1、Designation: D1266 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 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 to 0.4mass % (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 sulf

4、urin 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 Method

5、 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, nap

6、hthenic 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 resulti

7、ng 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 regarded

8、 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 and health practices and determine t

9、he applica-bility of regulatory limitations prior to use.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 for Sulfur in Petroleum Products (High-Temp

10、erature Method)D2784 Test Method for Sulfur in Liquefied Petroleum Gases(Oxy-Hydrogen Burner or Lamp)D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData

11、 for Use in Test Methods for Petroleum Products andLubricantsD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesE11 Specification for Woven Wire Test Sieve Cloth and TestSieves2.2 Energy Institute Standard:3IP 63 Sulfur ContentThe Quartz Tube Method3. Summary o

12、f 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 to sulfuric acid by means of hydrogen peroxide s

13、olutionwhich is then flushed with air to remove dissolved carbondioxide. Sulfur as sulfate in the absorbent is determined1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elem

14、ental Analysis.Current edition approved June 15, 2013. Published August 2013. Originallyapproved in 1969. Last previous edition approved in 2007 as D1266 07. DOI:10.1520/D1266-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.

15、 For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A Summary of Changes section appears at the end of this standardCopyright A

16、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1acidimetrically 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, thesulfu

17、r 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 precision of

18、 the method.3.3 For sulfur contents below 0.01 mass % it is necessary todetermine the sulfate content in the absorber solution turbidi-metrically as barium sulfate (see Annex A1).4. Significance and Use4.1 This test method provides a means of monitoring thesulfur level of various petroleum products

19、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 sulfur compounds

20、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 blending. The flas

21、kand 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 Wicking4,5Clean, unused, uniform, twistedwhite cotton yar

22、n of good quality. For the burner to burnaromatic samples use long staple, fine-spun, commercial finegrade.5,65.3 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 ofapproximately 70 %

23、 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 atmospheric. The

24、 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 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 manifol

25、d and associated equipmentfor burning samples in air are shown in Fig.A2.1 and describedin 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 specifications of the

26、 Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.7Other 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 Wat

27、erUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D1193.6.3 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.

28、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 suitable (Note 9).6.5 Hydrochloric Acid (1

29、 + 10)Mix 1 volume of concen-trated hydrochloric acid (HCl, relative density 1.19) with 10volumes of water.4The sole source of supply of cotton wicking, yarn, white, 4strand (2 to 3mg/cm/strand) known to the committee at this time is Koehler Instrument Co., 1595Sycamore Ave., Bohemia, NY 11716, or t

30、he type marketed by various suppliers inthe United Kingdom as 13s/14 ends, scoured, and bleached.5If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical

31、committee,1which you may attend.6The sole source of supply of fine grade known to the committee at this time isThomas Scientific, P.O. Box 99, Swedesboro, NJ 08085-0099.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the test

32、ing of reagents notlisted by the American Chemical 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.FIG. 1 Illustrative Sketch of the Assembled Lamp

33、 UnitD1266 1326.6 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 solution containingapproximately 0.1 % active constituent.8(Not methyl violet.)6.

34、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 forthis purpose the clear saturated solution decanted after standinglong enough to p

35、ermit 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. Use only puregum rubber tubing for connections between the storage bottlesand buret

36、s.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 16.03M in the calculation (see 12.1) becomes 1.000.6.10 Quality Control (QC) Sample(s

37、), 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 used to check the validity of the testingprocess as described in Section 12. An ample

38、 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 assembled, charge theabsorber with 30 6 2 mL of water.Adjust the individual valvesbetwe

39、en 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 manifold atapproximately 40 cm of water below atmospheric. When alladjustments have

40、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 use, place 300 to 400 mL of H2O2solution (1 + 19) in thescrubber. Since the manifold

41、 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 original.7.2 Neutralize the H2O2solution (1 + 19) immediately be-fore use. As 30 mL of

42、the solution is needed, transfer to abeaker multiples of 30 mL sufficient for the number ofabsorbers to be used simultaneously. 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.

43、3 Introduce 30 6 2 mL of the freshly neutralized H2O2solution (1 + 19) into the larger bulb of each absorber. Inaddition, 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

44、sulfur-free rubber tubing. Close the chimney open-ings by means of corks.7.4 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. (WarningAh

45、azardous (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 theabso

46、rbers, only a small stream of CO2-O2gas escapes at the8Fleisher 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 Diag

47、ram of CO2-O2Supply Manifold and Lamp SystemD1266 133pressure regulator, a small stream of air enters at the vacuumregulator, 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 (Not

48、e 5).NOTE 5It is convenient to balance the gas flow system by regulatingthe pressure in the vacuum manifold. This is done 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 s

49、ample (see Section 8); fold the wickingonce to give a 15-cm long bundle for threading the burners.Thread the required number 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 for 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