1、Designation: D 129 00 (Reapproved 2005)Designation: 61/99An American National StandardBritish Standard 4454Standard Test Method forSulfur in Petroleum Products (General Bomb Method)1This standard is issued under the fixed designation D 129; the number immediately following the designation indicates
2、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 (e) indicates an editorial change since the last revision or reapproval.This test method has been adopted for use by government age
3、ncies to replace Method 5202 of Federal Test Method No. 791b1. 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
4、 method isapplicable to any petroleum product sufficiently 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 i
5、nsolublein dilute hydrochloric acid and would interfere in 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, molybd
6、enumdisulfide, asbestos, mica, and so forth. The test method is not applicable toused oils containing wear metals, and lead or silicates from contamination.Samples that are excluded can be analyzed by Test Method D 1552.1.2 This standard does not purport to address all of thesafety concerns, if any,
7、 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. See 3.2 for specificprecautionary directions incorporated in the test method.2. Referenced Doc
8、uments2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceE 144 Practice for Safe Use of Oxygen C
9、ombustion Bombs3. Summary of Test Method3.1 The sample is oxidized by combustion in a bombcontaining oxygen under pressure. The sulfur, as sulfate in thebomb washings, is determined gravimetrically as barium sul-fate.3.2 WarningStrict adherence to all of the provisionsprescribed hereafter ensures ag
10、ainst explosive rupture of thebomb, or a blow-out, provided the bomb is of proper designand construction and in good mechanical condition. It isdesirable, however, that the bomb be enclosed in a shield ofsteel plate at least 13 mm thick, or equivalent protection beprovided against unforseeable conti
11、ngencies.4. Apparatus and Materials4.1 Bomb,3,4having a capacity of not less than 300 mL, soconstructed that it will not leak during the test and thatquantitative recovery of the liquids from the bomb may beachieved readily. The inner surface of the bomb may be madeof stainless steel or any other ma
12、terial that will not be affectedby the combustion process or products. Materials used in thebomb assembly, such as the head gasket and lead-wire insula-tion, shall be resistant to heat and chemical action, and shall notundergo any reaction that will affect the sulfur content of theliquid in the bomb
13、.4.2 Sample Cup, platinum, 24 mm in outside diameter at thebottom, 27 mm in outside diameter at the top, 12 mm in heightoutside, 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
14、 testprocedure by analyzing a quality control (QC) sample.X1.2 Prior to monitoring the measurement process, the userof the test method needs to determine the average value andcontrol limits of the QC sample (see Practice D 6299 and MNL7).11X1.3 Record the QC results and analyze by control chartsor o
15、ther statistically equivalent techniques to ascertain thestatistical control status of the total testing process (see PracticeD 6299 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 o
16、f QC testing is dependent on thecriticality of the quality being measured, the demonstratedstability of the testing process, and 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 routine
17、ly analyzed. However,when it is demonstrated 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
18、regularly tested be representative of the materialroutinely 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 D 6299 and MNL 7 for further guidance onQC and contr
19、ol charting techniquesSUMMARY OF CHANGESSub-Committee D02.03 has identified the location of selected changes to this standard since the last issue(D 129 - 95) that may impact the use of this standard.(1) Inserted QC statement in Section 5 and added section onQC (Section 10).ASTM International takes
20、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 such rights, are entirely their own respo
21、nsibility.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
22、 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 the ASTM Committee on Standards, at the a
23、ddress 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).11ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis, 6thed., available from ASTM Headquarters.D 129 00 (2005)4
