1、Designation: D129 18 British Standard 4454Designation: 61/99Standard Test Method forSulfur in Petroleum Products (General High PressureDecomposition Device Method)1This standard is issued under the fixed designation D129; the number immediately following the designation indicates the year oforiginal
2、 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 agencies of the U.S. Department of D
3、efense.1. Scope*1.1 This test method covers the determination of sulfur inpetroleum products, including lubricating oils containingadditives, additive concentrates, and lubricating greases thatcannot be burned completely in a wick lamp. The test methodis applicable to any petroleum product sufficien
4、tly low involatility that it can be weighed accurately in an open sampleboat and containing at least 0.1 % sulfur.NOTE 1This test method is not applicable to samples containingelements that give residues, other than barium sulfate, which are insolublein dilute hydrochloric acid and would interfere i
5、n the precipitation step.These interfering elements include iron, aluminum, calcium, silicon, andlead which are sometimes present in greases, lube oil additives, or additiveoils. Other acid insoluble materials that interfere are silica, molybdenumdisulfide, asbestos, mica, and so forth. The test met
6、hod is not applicable toused oils containing wear metals, and lead or silicates from contamination.Samples that are excluded can be analyzed by Test Method D1552.1.2 This test method is applicable to samples with the sulfurin the range 0.09 % to 5.5 % by mass.1.3 The values stated in SI units are to
7、 be regarded asstandard. No other units of measurement are included in thisstandard.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 establish appro-priate safety, health, and environment
8、al practices and deter-mine the applicability of regulatory limitations prior to use.1.5 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, Gu
9、ides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1552 Test Method for Sulfur in Petroleum Products byHigh Temperature Combustion and Infrared (IR) Detec-tion or
10、 Thermal Conductivity Detection (TCD)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement
11、 System PerformanceE144 Practice for Safe Use of Oxygen Combustion Vessels3. Summary of Test Method3.1 The sample is oxidized by combustion in a high pressuredecomposition device containing oxygen under pressure. Thesulfur, as sulfate in the high pressure decomposition devicewashings, is determined
12、gravimetrically as barium sulfate.3.2 (WarningStrict adherence to all of the provisionsprescribed hereafter ensures against explosive rupture of thehigh pressure decomposition device, or a blow-out, providedthe high pressure decomposition device is of proper design andconstruction and in good mechan
13、ical condition. It is desirable,however, that the high pressure decomposition device beenclosed in a shield of steel plate at least 13 mm thick, orequivalent protection be provided against unforeseeable con-tingencies.)3.3 (WarningInitial testing and periodic examination ofthe pressure vessel is ess
14、ential to ensure its fitness for service.1This 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 April 1, 2018. Published April 2018. Ori
15、ginallyapproved in 1922. Last previous edition approved in 2013 as D129 13. DOI:10.1520/D0129-18.This test method was adopted as a joint ASTM-IP standard in 1964.In the IP, this test method is under the jurisdiction of the StandardizationCommittee.2For referenced ASTM standards, visit the ASTM websi
16、te, 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Dr
17、ive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations i
18、ssued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1This is particularly important if the pressure vessel has beendropped and has any obvious signs of physical damage.)4. Apparatus and Materials4.1 High Pressure Decomposition Device (see Note 2),3having a capacity of n
19、ot less than 300 mL, so constructed thatit will not leak during the test and that quantitative recovery ofthe liquids from the high pressure decomposition device maybe achieved readily. The inner surface of the high pressuredecomposition device may be made of stainless steel or anyother material tha
20、t will not be affected by the combustionprocess or products. Materials used in the high pressuredecomposition device assembly, such as the head gasket andlead-wire insulation, shall be resistant to heat and chemicalaction, and shall not undergo any reaction that will affect thesulfur content of the
21、liquid in the high pressure decompositiondevice.NOTE 2Criteria for judging the acceptability of new and used oxygencombustion high pressure decomposition devices are described in PracticeE144.4.2 Oxygen Charging EquipmentThe valves, gauges, fill-ing tube, and fittings used in the oxygen charging sys
22、tem shallmeet industry safety codes and be rated for use at inputpressure up to 20 875 kPa and discharge pressure up to5575 kPa. Separate gauges shall be provided to show thesupply pressure and the pressure vessel pressure. The pressurevessel gauge shall not be less than 75 mm in diameter andprefera
23、bly graduated from 0 kPa to 5575 kPa in 100 kPasubdivisions. Both gauges shall be absolutely oil-free and shallnever be tested in a hydraulic system containing oil. Thecharging equipment shall include either a pressure reducingvalve which will limit the discharge pressure to a maximum of4055 kPa or
24、a relief valve set to discharge at 4055 kPa in casethe pressure vessel should accidentally be overcharged. Meansshall also be provided for releasing the residual pressure in thefilling tube after the pressure valve has been closed.4.3 Sample Cup, platinum, 24 mm in outside diameter at thebottom, 27
25、mm in outside diameter at the top, 12 mm in heightoutside, and weighing 10 g to 11 g.4.4 Firing Wire, platinum, No. 26B sulfurAPPENDIX(Nonmandatory Information)X1. QUALITY CONTROLX1.1 Confirm the performance of the instrument or the testprocedure by analyzing a quality control (QC) sample.X1.2 Prior
26、 to monitoring the measurement process, the userof the test method needs to determine the average value andcontrol limits of the QC sample (see Practice D6299 and MNL7).10X1.3 Record the QC results and analyze by control charts orother statistically equivalent techniques to ascertain the statis-tica
27、l control status of the total testing process (see PracticeD6299 and MNL 7). Any out-of-control data should triggerinvestigation for root cause(s).X1.4 In the absence of explicit requirements given in thetest method, the frequency of QC testing is dependent on thecriticality of the quality being mea
28、sured, the demonstratedstability of the testing process, and customer requirements.7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1278. ContactASTM CustomerService at serviceastm.org.8Supporting data have been filed at ASTM
29、 International Headquarters and maybe obtained by requesting Research Report RR:D02-1007. ContactASTM CustomerService at serviceastm.org.9IP Standards for Petroleum and Its Products, Part I, Appendix E. Availablefrom Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http:/www.energyinst
30、.org.10ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,6thed., ASTM International.D129 184Generally, a QC sample is analyzed each testing day withroutine samples. The QC frequency should be increased if alarge number of samples are routinely analyzed. However,when it is demonstrate
31、d that the testing is under statisticalcontrol, the QC testing frequency may be reduced. The QCsample precision should be checked against the ASTM methodprecision to ensure data quality.X1.5 It is recommended that, if possible, the type of QCsample that is regularly tested be representative of the m
32、aterialroutinely analyzed. An ample supply of QC sample materialshould be available for the intended period of use, and must behomogenous and stable under the anticipated storage condi-tions. See Practice D6299 and MNL 7 for further guidance onQC and control charting techniques.SUMMARY OF CHANGESSub
33、committee D02.03 has identified the location of selected changes to this standard since the last issue(D129 13) that may impact the use of this standard. (Approved April 1, 2018.)(1) Added Practices D4057 and D4177 to Referenced Docu-ments.(2) Added new subsection 6.1.ASTM International takes no pos
34、ition respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibil
35、ity.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to AS
36、TM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address
37、 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 185
