1、Designation: D1552 08 (Reapproved 2014)1Standard Test Method forSulfur in Petroleum Products (High-Temperature Method)1This standard is issued under the fixed designation D1552; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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 U.S. Department of Defense.1NOTEFootnotes were updated editorial
3、ly in September 2014.1. Scope1.1 This test method covers three procedures for the deter-mination of total sulfur in petroleum products includinglubricating oils containing additives, and in additive concen-trates. This test method is applicable to samples boiling above177C (350F) and containing not
4、less than 0.06 mass % sulfur.Two of the three procedures use iodate detection; one employ-ing an induction furnace for pyrolysis, the other a resistancefurnace. The third procedure uses IR detection followingpyrolysis in a resistance furnace.1.2 Petroleum coke containing up to 8 mass % sulfur can be
5、analyzed.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 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 esta
6、blish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1266 Test Method for Sulfur in Petroleum Products (LampMethod)D4057 Practice for Manual Sampling of
7、Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3. Summary of Test Method3.1 Iodate De
8、tection SystemThe sample is burned in astream of oxygen at a sufficiently high temperature to convertabout 97 % of the sulfur to sulfur dioxide. A standardizationfactor is employed to obtain accurate results. The combustionproducts are passed into an absorber containing an acidsolution of potassium
9、iodide and starch indicator. A faint bluecolor is developed in the absorber solution by the addition ofstandard potassium iodate solution. As combustion proceeds,bleaching the blue color, more iodate is added. The amount ofstandard iodate consumed during the combustion is a measureof the sulfur cont
10、ent of the sample.3.2 IR Detection SystemThe sample is weighed into aspecial ceramic boat which is then placed into a combustionfurnace at 1371C (2500F) in an oxygen atmosphere. Mostsulfur present is combusted to SO2which is then measuredwith an infrared detector after moisture and dust are removedb
11、y traps. A microprocessor calculates the mass percent sulfurfrom the sample weight, the integrated detector signal and apredetermined calibration factor. Both the sample identificationnumber and mass percent sulfur are then printed out. Thecalibration factor is determined using standards approximati
12、ngthe material to be analyzed.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 sulfurcompounds is
13、beneficial to the product and monitoring thedepletion of sulfur can provide useful information. In othercases the presence of sulfur compounds is detrimental to theprocessing or use of the product.5. Interferences5.1 For the iodate systems, chlorine in concentrations lessthan 1 mass % does not inter
14、fere. The IR system can tolerate1This 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 Elemental Analysis.Current edition approved June 15, 2014. Published July 2014. Originallyapp
15、roved in 1958. Last previous edition approved in 2008 as D155208. DOI:10.1520/D1552-08R14E01.2For referenced 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
16、Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1somewhat higher concentrations. Nitrogen when present inexcess of 0.1 mass % may interfere with the iodate systems; theextent of such interference may be
17、dependent on the type ofnitrogen compound as well as the combustion conditions.Nitrogen does not interfere with the IR system. The alkali andalkaline earth metals, as well as zinc, phosphorus, and lead, donot interfere with either system.6. Apparatus6.1 Combustion and Iodate Detection System:6.1.1 F
18、urnacesTwo major types are available, the primarydifference being the manner in which the necessary hightemperatures are obtained. These two types are as follows:6.1.1.1 Induction Type, which depends upon the high-frequency electrical induction method of heating. This assem-bly shall be capable of a
19、ttaining a temperature of at least1482C (2700F) in the sample combustion zone, under theconditions set forth in 9.1 and shall be equipped with anadditional induction coil located above the combustion zone,substantially as shown in Fig. 1.6.1.1.2 The furnace work coil should have a minimumoutput of 5
20、00 W; the minimum input rating of the furnace mustbe 1000 W. With the correct amount of iron chips, weighed to60.05 g, the maximum plate current will be between 350 and450 mA. (WarningThis type of furnace is capable ofinflicting high frequency burns and high-voltage shocks. Inaddition to other preca
21、utions, maintain all guards properly.)(WarningDisconnect the furnace from the power line when-ever electrical repairs or adjustments are made.)6.1.1.3 Resistance Type, capable of maintaining a tempera-ture of at least 1371C (2500F).6.1.2 Absorber, as described in Test Method D1266.NOTE 1Also suitabl
22、e for use with either type of furnace is anautomatic titrator, specifically designed for iodometry. This combines thefunctions of absorption and titration to a predetermined end point.6.1.3 Buret, standard 25-mL or automatic types availablefrom the manufacturers of the specific combustion units, are
23、suitable (Note 1).6.2 Combustion and IR Detection System, comprised ofautomatic balance, oxygen flow controls, drying tubes, com-bustion furnace, infrared detector and microprocessor. Thefurnace shall be capable of maintaining a nominal operatingtemperature of 1350C (2460F).6.3 Miscellaneous Apparat
24、usSpecific combustion assem-blies require additional equipment such as crucibles, combus-tion boats, crucible lids, boat pushers, separator disks, com-bustion tubes, sample inserters, oxygen flow indicator, andoxygen drying trains. The additional equipment required isdependent on the type of furnace
25、 used and is available from themanufacturer of the specific combustion unit. To attain thelower sulfur concentration given in Section 1, the ceramicsused with the induction furnace assembly shall be ignited in amuffle furnace at 1371C (2500F) for at least 4 h before use.6.4 Sieve, 60-mesh (250-mm).7
26、. Reagents and Materials7.1 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 Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are ava
27、ilable.3Other 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.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as defined
28、by Type II or III of Specification D1193.7.3 Alundum (Al2O3)orMagnesium Oxide (Com-Aid).7.4 Anhydrone (Magnesium Perchlorate). (WarningInaddition to other precautions, handle magnesium perchloratewith care. Avoid contacting it with acid and organic materials.Reactions with fuel may be violent.)7.5 H
29、ydrochloric Acid (3 + 197)Dilute 30 mL of concen-trated hydrochloric acid (HCl, relative density 1.19) to 2 L withwater. (WarningPoison. Corrosive. May be fatal if swal-lowed. Liquid and vapor cause severe burns.)7.6 Oxygen (Extra Dry)The oxygen shall be at least99.5 % pure and show no detectable su
30、lfur by blank determi-nation. (WarningOxygen vigorously accelerates combus-tion.)7.7 Phosphorus Pentoxide(P2O5).7.8 Potassium Alum (Aluminum Potassium Sulfate).7.9 Potassium Iodate, Standard Solution (0.06238 N), 1 mLof this solution is equivalent to 1 mg S)Dissolve 2.225 g ofpotassium iodate (KIO3)
31、 that has been dried at about 180C toconstant weight, in water and dilute to 1 L. Thoroughly mix thesolution.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society,
32、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 Combustion TubeD1552 08 (2014)127.10 Potassium Iodate, Standard Solution (0.006238 N),1 mL of this so
33、lution is equivalent to 0.1 mg S)Measureexactly 100 mL of KIO3solution (0.06238 N) into a 1Lvolumetric flask, and dilute to volume with water. Thoroughlymix the solution.7.11 Potassium Iodate, Standard Solution (0.01248 N),1 mL of this solution is equivalent to 0.2 mg S)Measureexactly 200 mL of KIO3
34、solution (0.06238 N) into a 1-Lvolumetric flask and dilute to volume with water. Thoroughlymix the solution.7.12 Ascarite, 8 to 20 mesh.7.13 Special Materials for Induction-Type Furnaces:7.13.1 Tin (20 to 30-mesh).7.13.2 Iron-Chip Accelerator having a sulfur content of notmore than 0.005 mass %.7.14
35、 Standard SamplePotassium alum (AlK(SO4)212H2O).7.15 Starch-Iodide SolutionMake a paste by adding9gofsoluble starch to 15 mL of water. Add this mixture, withstirring, to 500 mL of boiling water. Cool the mixture, add 15 gof potassium iodide (KI), and dilute to 1 L with water.7.16 Sulfuric Acid (rela
36、tive density 1.84)Concentratedsulfuric acid (H2SO4). (WarningPoison. Corrosive. Strongoxidizer.)7.17 Vanadium Pentoxide, anhydrous, powdered V2O5.7.18 Quality Control (QC) Sample(s) , preferably are por-tions of one or more petroleum products that are stable andrepresentative of the samples of inter
37、est. These QC samplescan be used to check the validity of the testing process andperformance of the instrument as described in Section 12.8. Sampling8.1 Take samples in accordance with the instructions inPractice D4057.9. Preparation of Apparatus9.1 Induction-Type FurnaceAssemble the apparatus ac-co
38、rding to the instructions furnished by the manufacturer.Purify the oxygen by passing it through (1)H2SO4(relativedensity 1.84), ( 2) Ascarite, and (3) magnesium perchlorate(Mg(ClO4)2) or phosphorus pentoxide (P2O5)(Warningsee7.4). Connect a rotameter between the purifying train and thefurnace. Inser
39、t a small glass-wool plug in the upper end of theglass tubing connecting the furnace with the absorber to catchoxides of tin. Connect the exit end of the combustion tube tothe absorber with glass tubing, using gum rubber tubing tomake connections. Position the absorber so as to make thisdelivery lin
40、e as short as possible. Fig. 2 illustrates schemati-cally the assembled apparatus. Adjust the oxygen flow to 1 60.05 L/min. Add 65 mL of HCl (3 + 197) and 2 mL ofstarch-iodide solution to the absorber. Add a sufficient amountof the appropriate standard KIO3solution (Table 1) to producea faint blue c
41、olor. This color will serve as the end point for thetitration. Adjust the buret to zero. Turn on the furnace filamentswitch and allow at least 1 min warm-up before runningsamples (Warningsee 7.4).9.2 ResistanceType FurnaceAssemble the apparatus ac-cording to the instructions furnished by the manufac
42、turer.Purify the oxygen by passing it through (1)H2SO4(relativedensity 1.84), (2) Ascarite, and (3) Mg(ClO4)2or P2O5(Warningsee 7.4). Connect a rotameter between the purify-ing train and the furnace. Fig. 3 illustrates schematically theassembled apparatus. Turn on the current and adjust thefurnace c
43、ontrol to maintain a constant temperature of1316 6 14C (2400 6 25F). Adjust the oxygen flow rate to2 6 0.1 L/min. Add 65 mL of HCl (3 6 197) and 2 mL ofstarch-iodide solution to the absorber. Add a few drops of theappropriate standard KIO3solution (Table 2) to produce a faintblue color. Adjust the b
44、uret to zero.9.3 ResistanceType FurnaceIR DetectionAssemble andadjust apparatus according to manufacturers instructions.Initialize microprocessor, check power supplies, set oxygenpressure and flows and set furnace temperature to 1371C(2500F).9.3.1 Condition a fresh anhydrone scrubber with four coals
45、amples when analyzing petroleum coke samples, or with fourpetroleum product samples that are representative or typical ofthe sample types to be analyzed.9.3.2 Calibrate the automatic balance according to manu-facturers instructions.10. Standardization10.1 For Iodate Methods:10.1.1 Determination of A
46、lum Factor:10.1.1.1 Because these rapid combustion methods involvethe reversible reaction 2SO2+O2= 2SO3, it is not possible toevolve all the sulfur as SO2. The equilibrium of the reaction istemperature dependent and, in an oxygen atmosphere above1316C, about 97 % of the sulfur is present as SO2. To
47、assurethat the furnace is in proper adjustment and that its operationproduces acceptably high temperature, potassium alum isemployed for standardizing the apparatus. Depending on thetype of combustion equipment used, proceed as described inSections 10 to 14 to determine the alum factor. Use 15 mgwei
48、ghed to 60.1 mg of potassium alum for this determination.FIG. 2 Schematic Illustration of Induction-Type FurnaceTABLE 1 Sample Weight for Induction FurnaceSulfur Content, %Weight of Sampleto be Taken, mgNormality of StandardKIO3solution for Titration0to2 90A0.0062382 to 4 50 to 90 0.0062384 to 10 50
49、 to 90 0.01248Over 10 12.1.1 (Note 2)AApproximate.D1552 08 (2014)13Use the same materials in the determination of the alum andstandardization factors as for the unknown samples. Forexample, V2O5has a definite effect and should be included ifused for unknowns as recommended in the procedure with theresistance-type furnace.10.1.1.2 Calculate the alum factor as follows:Alum factor AF! 5 SA3 WA!/100Va2 Vb! 3 C1! (1)where:SA= mass percent sulfur in potassium alum used,WA= milligrams of potassium alum used,Va= millilitres of s
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