1、Designation: D129 11D129 13 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 ofo
2、riginal 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 Department of
3、 Defense.1. Scope*1.1 This test method covers the determination of sulfur in petroleum products, including lubricating oils containing additives,additive concentrates, and lubricating greases that cannot be burned completely in a wick lamp. The test method is applicable toany petroleum product suffi
4、ciently low in volatility that it can be weighed accurately in an open sample boat and containing at least0.1 % sulfur.NOTE 1This test method is not applicable to samples containing elements that give residues, other than barium sulfate, which are insoluble in dilutehydrochloric acid and would inter
5、fere in the precipitation step. These interfering elements include iron, aluminum, calcium, silicon, and lead which aresometimes present in greases, lube oil additives, or additive oils. Other acid insoluble materials that interfere are silica, molybdenum disulfide, asbestos,mica, and so forth. The
6、test method is not applicable to used oils containing wear metals, and lead or silicates from contamination. Samples that areexcluded can be analyzed by Test Method D1552.1.2 This test method is applicable to samples with the sulfur in the range 0.09 to 5.5 mass %.1.3 The values stated in SI units a
7、re to be regarded as standard. No other units of measurement are included in this standard.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 standard to establish appropriate safety and health practi
8、ces and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)D6299 Practice for Applying Statistical Quality Assurance and Control
9、Charting Techniques to Evaluate Analytical Measure-ment System PerformanceE144 Practice for Safe Use of Oxygen Combustion Bombs3. Summary of Test Method3.1 The sample is oxidized by combustion in a high pressure decomposition device containing oxygen under pressure. Thesulfur, as sulfate in the high
10、 pressure decomposition device washings, is determined gravimetrically as barium sulfate.3.2 (WarningStrict adherence to all of the provisions prescribed hereafter ensures against explosive rupture of the highpressure decomposition device, or a blow-out, provided the high pressure decomposition devi
11、ce is of proper design andconstruction and in good mechanical condition. It is desirable, however, that the high pressure decomposition device be enclosedin a shield of steel plate at least 13 mm thick, or equivalent protection be provided against unforeseeable contingencies.)1 This test method is u
12、nder the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 onElemental Analysis.Current edition approved Oct. 1, 2011June 15, 2013. Published October 2011August 2013. Originally approved in 1922. Last previous edition appr
13、oved in 20052011 asD12900(2005).D129 11. DOI: 10.1520/D0129-11.10.1520/D0129-13.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 Standardization Committee.2 For referencedASTM standards, visit theASTM website, www.astm.org,
14、 or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary 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
15、have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends 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
16、document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3 (WarningInitial testing and periodic examination of the pressure vessel is essential to ensure its fitness f
17、or service. Thisis particularly important if the pressure vessel has been dropped and has any obvious signs of physical damage.)4. Apparatus and Materials4.1 High Pressure Decomposition Device (see Note 2),3having a capacity of not less than 300 mL, so constructed that it willnot leak during the tes
18、t and that quantitative recovery of the liquids from the high pressure decomposition device may be achievedreadily. The inner surface of the high pressure decomposition device may be made of stainless steel or any other material that willnot be affected by the combustion process or products. Materia
19、ls used in the high pressure decomposition device assembly, suchas the head gasket and lead-wire insulation, shall be resistant to heat and chemical action, and shall not undergo any reaction thatwill affect the sulfur content of the liquid in the high pressure decomposition device.NOTE 2Criteria fo
20、r judging the acceptability of new and used oxygen combustion high pressure decomposition devices are described in PracticeE144.4.2 Oxygen Charging EquipmentThe valves, gauges, filling tube, and fittings used in the oxygen charging system shall meetindustry safety codes and be rated for use at input
21、 pressure up to 20 875 kPa and discharge pressure up to 5575 kPa. Separategauges shall be provided to show the supply pressure and the pressure vessel pressure. The pressure vessel gauge shall not be lessthan 75 mm in diameter and preferably graduated from 0 kPa to 5575 kPa in 100 kPa subdivisions.
22、Both gauges shall be absolutelyoil-free and shall never be tested in a hydraulic system containing oil. The charging equipment shall include either a pressurereducing valve which will limit the discharge pressure to a maximum of 4055 kPa or a relief valve set to discharge at 4055 kPain case the pres
23、sure vessel should accidentally be overcharged. Means shall also be provided for releasing the residual pressurein the filling tube after the pressure valve has been closed.4.3 Sample Cup, platinum, 24 mm in outside diameter at the bottom, 27 mm in outside diameter at the top, 12 mm in heightoutside
24、, and weighing 10 to 11 g.4.4 Firing Wire, platinum, No. 26 B sulfurAPPENDIX(Nonmandatory Information)X1. QUALITY CONTROLX1.1 Confirm the performance of the instrument or the test procedure by analyzing a quality control (QC) sample.X1.2 Prior to monitoring the measurement process, the user of the t
25、est method needs to determine the average value and controllimits of the QC sample (see Practice D6299 and MNL 7).9X1.3 Record the QC results and analyze by control charts or other statistically equivalent techniques to ascertain the statisticalcontrol status of the total testing process (see Practi
26、ce D6299 and MNL 7). Any out-of-control data should trigger investigationfor root cause(s).X1.4 In the absence of explicit requirements given in the test method, the frequency of QC testing is dependent on the criticalityof the quality being measured, the demonstrated stability of the testing proces
27、s, and customer requirements. Generally, a QCsample is analyzed each testing day with routine samples. The QC frequency should be increased if a large number of samples are8 IP Standards for Petroleum and Its Products, Part I, Appendix E. Available from Energy Institute, 61 New Cavendish St., London
28、, WIG 7AR, U.K.,http:/www.energyinst.org.9 ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6th ed., ASTM International.D129 135routinely analyzed. However, when it is demonstrated that the testing is under statistical control, the QC testing frequency maybe reduced. The QC sample
29、precision should be checked against the ASTM method precision to ensure data quality.X1.5 It is recommended that, if possible, the type of QC sample that is regularly tested be representative of the material routinelyanalyzed. An ample supply of QC sample material should be available for the intende
30、d period of use, and must be homogenousand stable under the anticipated storage conditions. See Practice D6299 and MNL 7 for further guidance on QC and controlcharting techniques.SUMMARY OF CHANGESSubcommittee D02.03 has identified the location of selected changes to this standard since the last iss
31、ue(D12900(2005)D129 11) that may impact the use of this standard.(1) Replaced the word “bomb”Added information in sections 1.2throughout, 3.3the, 4.2test, 4.5method, 4.7with the phrase, and 4.8“high pressure decomposition device.”in Scope and Apparatus sections to keep consistent with equivalent tes
32、t method IP 61.ASTM International takes no position 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 s
33、uch rights, are entirely their own responsibility.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 addi
34、tional standardsand should be addressed to ASTM 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 th
35、e ASTM Committee on Standards, at the address 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 ASTM website (www.astm.org/COPYRIGHT/).D129 136
