1、Designation: D129 11Designation: 61/99British Standard 4454Standard 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 Department of Defense
3、.1. Scope*1.1 This test method covers the determination of sulfur inpetroleum products, including lubricating oils containing addi-tives, additive concentrates, and lubricating greases that cannotbe burned completely in a wick lamp. The test method isapplicable to any petroleum product sufficiently
4、low in vola-tility that it can be weighed accurately in an open sample boatand 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 in
5、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 metho
6、d 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 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standar
7、d 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 the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM
8、 Standards:2D1193 Specification for Reagent WaterD1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE144 Practice for Safe Use of Oxyge
9、n Combustion Bombs3. 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 gravimetrically as barium sulfate.3.2 (WarningStrict adh
10、erence 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 mechanical condition. It is desirable,however, that the high p
11、ressure decomposition device beenclosed in a shield of steel plate at least 13 mm thick, orequivalent protection be provided against unforeseeable con-tingencies.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of
12、 SubcommitteeD02.03 on Elemental Analysis.Current edition approved Oct. 1, 2011. Published October 2011. Originallyapproved in 1922. Last previous edition approved in 2005 as D12900(2005). DOI:10.1520/D0129-11.This test method was adopted as a joint ASTM-IP standard in 1964.In the IP, this test meth
13、od is under the jurisdiction of the StandardizationCommittee.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 Summary page onthe ASTM website.
14、1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Apparatus and Materials4.1 High Pressure Decomposition Device (see Note2),3having a capacity of not less than 300 mL
15、, so constructedthat it will not leak during the test and that quantitativerecovery of the liquids from the high pressure decompositiondevice may be achieved readily. The inner surface of the highpressure decomposition device may be made of stainless steelor any other material that will not be affec
16、ted by the combus-tion process 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 liquid in the hig
17、h pressure decompositiondevice.NOTE 2Criteria for judging the acceptability of new and used oxygencombustion high pressure decomposition devices are described in PracticeE144.4.2 Sample Cup, platinum, 24 mm in outside diameter at thebottom, 27 mm in outside diameter at the top, 12 mm in heightoutsid
18、e, and weighing 10 to 11 g.4.3 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 to monitoring the measurement process, the userof the tes
19、t method needs to determine the average value andcontrol limits of the QC sample (see Practice D6299 and MNL7).9X1.3 Record the QC results and analyze by control chartsor other statistically equivalent techniques to ascertain thestatistical control status of the total testing process (see PracticeD6
20、299 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 measured, the demonstratedstability of the testing process, and
21、customer requirements.Generally, 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 demonstrated that the testing is under statisticalcontrol, the QC testing frequency may be reduce
22、d. 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 materialroutinely analyzed. An ample supply of QC sample materialshould be available fo
23、r 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.8IP Standards for Petroleum and Its Products, Part I, Appendix E. Availablefrom Energy Institute, 61 New Ca
24、vendish St., London, WIG 7AR, U.K., http:/www.energyinst.org.9ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,6thed., ASTM International.D129 114SUMMARY OF CHANGESSubcommittee D02.03 has identified the location of selected changes to this standard since the last issue(D12900(2005)
25、that may impact the use of this standard.(1) Replaced the word “bomb” throughout the test methodwith the phrase “high pressure decomposition device.”ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
26、 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 responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every f
27、ive 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 ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
28、 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 shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
29、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 115
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