1、Designation: D1552 15D1552 16Standard Test Method forSulfur in Petroleum Products by High TemperatureCombustion and IR DetectionInfrared (IR) Detection orThermal Conducitivity Detection (TCD)1This standard is issued under the fixed designation D1552; the number immediately following the designation
2、indicates the year oforiginal adoption or, in the case of revision, the year 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 agencie
3、s of the U.S. Department of Defense.1. Scope*1.1 This test method covers a procedure procedures for the determination of total sulfur in petroleum products includinglubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177 C(350
4、F) and containing a mass fraction of sulfur not less than 0.06 %. This procedure uses IR detection following pyrolysis in aresistance between 0.22 % and 24.2 %. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.These procedures use IR detection or TCD followi
5、ng combustion in a furnace.1.2 Petroleum coke containing up to 8 mass % sulfur can be analyzed.a mass fraction of sulfur between 2.53 % to 3.79 % sulfurmay be analyzed. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.NOTE 1The D155208 (2014) version of this
6、 standard contained two other procedures using iodate titrations. Since these procedures are no longerbeing used in the industry laboratories based on a survey of D02.SC 3 laboratories conducted in September 2014, they are being deleted. For earlierinformation on the deleted procedures, D155208 (201
7、4) may be perused.1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.4 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 stan
8、dard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1266D4057 Test Method for Sulfur in Petroleum Products (Lamp Method)Practice for Manual Sampling of Petroleum andPetroleum Produ
9、ctsD4057D4177 Practice for ManualAutomatic Sampling of Petroleum and Petroleum ProductsD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-ment System PerformanceD6300 Practice for Determination of Precision and Bias Data for Use i
10、n Test Methods for Petroleum Products and LubricantsD6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories3. Summary of Test Method3.1 The sample is weighed into a special ceramic boat which is then and placed into a combustion furnace at 1350 C (2460 F)in an oxy
11、gen atmosphere. furnace having an oxygen atmosphere sufficient to combust the entire sample and a temperature between1150 C and 1450 C for Procedure A or 1150 C for Procedure B. Most sulfur present is combusted to SO2, which is thenmeasured with an infrared a detector after moisture and dust are rem
12、oved by traps.AmicroprocessorThe instrument calculates themass percent sulfur from the sample weight,mass, the integrated detector signal, and a predetermined calibration factor. Thecalibration factor is determined using standards approximating the material to be analyzed.1 This test method is under
13、 the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved April 1, 2015July 1, 2016. Published May 2015August 2016. Originally approved in 1958. Last previous editio
14、n approved in 20142015 asD1552 08 (2014)D1552 15.1. DOI: 10.1520/D1552-15.10.1520/D1552-16.2 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 the standards Document Sum
15、mary page on the ASTM website.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 been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommend
16、s 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 document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, W
17、est Conshohocken, PA 19428-2959. United States13.1.1 Procedure AAfter combustion of the sample and subsequent moisture/dust removal, SO2 is measured using infrared (IR)detection.3.1.2 Procedure BAfter combustion of the sample and subsequent moisture/dust removal, SO2 is measured using thermalconduct
18、ivity detection. An apparatus utilizing TCD may require the sample gas to pass an oxygen scrubber and adsorption/desorption traps to allow passing of contaminants prior to measuring SO2.4. Significance and Use4.1 This test method provides a means of monitoring the sulfur level of various petroleum p
19、roducts and additives. Thisknowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compoundsis beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence ofsulfur compound
20、s is detrimental to the processing or use of the product.5. Apparatus5.1 Resistance Type Furnace, Combustion Furnace: capable of maintaining a temperature of at least 1350 C (2460 F).5.1.1 Procedure AFurnace capable of maintaining a constant temperature (between 1150 C minimum and 1450 Cmaximum) suf
21、ficient to ensure quantitative recovery of sulfur as its corresponding gas SO2.5.1.2 Procedure BFurnace capable of maintaining a temperature (1150 C) sufficient to ensure quantitative recovery of sulfuras its corresponding gas SO2.5.2 Absorber, as described in Test Method D1266.5.2 Combustion and IR
22、Sulfur Detection System, comprised of automatic balance, oxygengas flow controls, drying tubes,combustion furnace, infrared detector and microprocessor. The furnace shall be capable of maintaining a nominaloxygen scrubber,adsorption/desorption traps as required, combustion furnace, combustion boats
23、or tin (Sn) containers as required and either an IR(Procedure A) or TCD (Procedure B) SO2 operating temperature of 1350 C (2460 F).detector.5.3 Sieve, 60 mesh (250 m).6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
24、intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use
25、 without lessening the accuracy of the determination.6.2 Combustion PromoterMagnesium Oxide (Com-Aid) oxide (MgO), tungsten trioxode (WO3), or Alundum aluminumoxide (Al2O3). Alternatively, COM-CAT, a dual promoter that is both a fixing agent and oxidizing agent, may be used.46.3 Magnesium Perchlorat
26、e: Anhydrone. Drying Agent, Magnesium perchlorate: anhydrone(Mg(ClO4)2) or phosphorus pentoxide (P2O5). (WarningIn addition to other precautions, handle magnesium perchlorate withcare. Avoid contacting it with acid and organic materials. Reactions with fuel may be violent.)6.4 Oxygen (Extra Dry)The
27、oxygen shall be at least 99.5 % pure and show no detectable sulfur by blank determination.(WarningOxygen vigorously accelerates combustion.)6.5 Phosphorus PentoxideInert Gas(PHelium2O or5). argon, high purity grade, 99.995 % minimum purity, as required bymanufacturers recommendations.6.6 Ascarite, 8
28、 mesh to 20 mesh.6.7 Vanadium Pentoxide, anhydrous, powdered V2O5.6.6 Quality Control (QC) Sample(s), preferably are portions of one or more petroleum products that are stable and representativeof the samples of interest. These QC samples can be used to check the validity of the testing process and
29、performance of theinstrument as described in Section 11.7. Sampling7.1 Take samples in accordance with the instructions in Practice D4057 or D4177.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
30、listed 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.4 The sole source of supply of COM-CAT known to the committee at t
31、his time is LECO Corporation, 3000 Lakeview Ave. St. Joseph, MI 49085 USA. If you are awareof alternative suppliers, please provide this information toASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1 which you may a
32、ttend.D1552 1628. Preparation of Apparatus8.1 ResistanceType FurnaceIR DetectionAssemble and adjust apparatus according to manufacturers instructions. Initializemicroprocessor,instrument, check power supplies, set oxygengas pressure and flows, and set furnace temperature to 1350 C(2460 F).temperatur
33、e.8.1.1 Condition a fresh anhydrone scrubber with four coal samples when analyzing petroleum coke samples, or with fourpetroleum product samples the instrument with samples that are representative or typical of the sample types to be analyzed.During the interlaboratory study, laboratories analyzed b
34、etween one and five conditioning samples.8.1.2 Calibrate the automatic balance according to manufacturers instructions.9. Standardization9.1 Determination of Standardization Factor:9.1.1 Because effects such as sample volatility can also affect the relative recovery as SO2 of the sulfur originally p
35、resent in thesample, it is necessary to determine a standardization factor. Proceed as described in Sections 9 through 12, using an oil sampleof similar type to the unknown sample and of accurately known sulfur content.59.1.2 Determine the calibration factor for the particular type of sample to be a
36、nalyzed (lubricating oil, petroleum coke, residualfuel) as recommended by the manufacturer.9.2 Quality ControlRun a suitable analytical quality control sample several times daily. When the observed value lies betweenacceptable limits on a quality control chart, proceed with sample determinations.10.
37、 Preparation of Coke10.1 It is assumed that a representative sample has been received for analysis. If the sample of coke received is not dry, it isrecommended that the sample be dried prior to grinding.10.2 Grind and sieve the sample received so as to pass a 60 mesh (250 m) sieve.10.3 Dry the sieve
38、d material to constant weight at 105 C to 110 C.11. Analysis of Quality Control Samples11.1 AQC sample shall be analyzed each day samples are analyzed to verify the testing procedure and instrument performance.Additional QC samples may be analyzed. The QC samples shall be treated as outlined in Sect
39、ion 12, depending upon the type offurnace set-up used by the lab.11.2 When QC/Quality Assurance (QA) protocols are already established in the testing facility, these may be used to confirmthe reliability of the test result.11.3 When there is no QC/QA protocol established in the testing facility, App
40、endix X1 can be used as the QC/QA system.12. Procedure with Resistance FurnaceIR Detection Procedures12.1 Allow the system to warm up and the furnace to reach operating temperature.12.2 After homogeneity of the sample is assured, select the appropriate sample size as recommended by the instrumentman
41、ufacturer.As an example, for liquid samples, take up to 0.13 g for analysis and for solid samples, take up to 0.4 g for analysis.12.3 Determine and store the system blank value.12.1 Weigh solid samples into combustion boats and record the net weights. For liquid samples, follow 12.4.1 12.4.4. It isp
42、ossible to weigh and store several weights in the microprocessor before beginning a series of burns.Procedure ACombustionwith Infrared (IR) Detection:12.1.1 Fill the combustion boat to one-third capacity with evenly spread MgO powder.Following instrument manufacturerrecommendations, allow the system
43、 to warm up and the furnace to reach an operating temperature between 1150 C minimum and1450 C maximum.12.1.2 Form a slight trench in the MgO powder with a scoop. Mix or swirl the test sample thoroughly to ensure homogeneity.Select the appropriate test specimen size as recommended by the instrument
44、manufacturer.As an example, for liquid samples, takeup to 0.13 g for analysis and for solid samples, take up to 0.4 g for analysis.12.1.3 Determine and store the system blank value.12.1.4 Place the combustion boat on the balance and weigh an appropriate amount of the sample into the trench in theMgO
45、Weigh solid samples into combustion boats or containers and record the net masses. For liquid samples, follow 12.1.4.1powder.to 12.1.4.4Record and enter the weight12.1.4.1 Following manufacturer recommendations; add combustion promoter, if used, to combustion boat or container usingscoop or spatula.
46、 Fill the combustion boat to one-third capacity with evenly spread MgO powder.5 Residual fuel oil Standard Reference Materials may be obtained from the National Institute of Standards and Technology or other sources.D1552 16312.1.4.2 Place combustion boat or container on the balance and tare.12.1.4.
47、3 Weigh an appropriate amount of the sample onto the combustion promoter. Record and enter the mass of sample. Ifusing combustion container, seal before recording sample mass.12.1.4.4 Remove the combustion boat or container from the balance. Additional combustion promoter can be added to opencombust
48、ion boat after weighing, if recommended by manufacturers guidance.12.1.5 Initiate gas flow and load sample into furnace.12.1.6 When the analysis is complete, read the result from the instrument.12.1.7 Remove the combustion boat from the balance and add MgO powder until the combustion boat is filled
49、to two-thirdscapacity. (Prepare furnace and instrument for next run according to manufacturers recommendation. Remove the expendedcombustion boat from the furnace, if used.WarningV2O5 can cause deterioration of the furnace ceramics so use it with care.)NOTE 2If unacceptable repeatability is encountered for particular oil samples, combustion promoter such as V2O5 or the LECO product Com-Aid canbe substituted for the MgO.12.1.8 Perform a second determination and average the two values for a single result.12.5 Initiate oxygen fl
