1、Designation: D482 12D482 13Designation: 4/96Standard Test Method forAsh from Petroleum Products1This standard is issued under the fixed designation D482; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、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.1. Scope*1.1 This test method covers the determination of ash in t
3、he range 0.0010.180 mass %, from distillate and residual fuels, gasturbine fuels, crude oils, lubricating oils, waxes, and other petroleum products, in which any ash-forming materials present arenormally considered to be undesirable impurities or contaminants (Note 1). The test method is limited to
4、petroleum products whichare free from added ash-forming additives, including certain phosphorus compounds (Note 2).NOTE 1In certain types of samples, all of the ash-forming metals are not retained quantitatively in the ash. This is particularly true of distillate oils,which require a special ash pro
5、cedure in order to retain metals quantitatively.NOTE 2This test method is not intended for the analysis of unused lubricating oils containing additives; for such samples use Test Method D874.Neither is it intended for the analysis of lubricating oils containing lead nor for used engine crankcase oil
6、s.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.The preferred expression of the property is mass %.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the res
7、ponsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D874 Test Method for Sulfated Ash from Lubricating Oils and AdditivesD4057 Practice for Manual
8、 Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum ProductsD4928 Test Method for Water in Crude Oils by Coulometric Karl Fischer TitrationD6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate A
9、nalytical Measure-ment System PerformanceD6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories3. Summary of Test Method3.1 The sample contained in a suitable vessel is ignited and allowed to burn until only ash and carbon remain. The carbonaceousresidue is reduc
10、ed to an ash by heating in a muffle furnace at 775C, cooled and weighed.4. Significance and Use4.1 Knowledge of the amount of ash-forming material present in a product can provide information as to whether or not theproduct is suitable for use in a given application. Ash can result from oil or water
11、-soluble metallic compounds or from extraneoussolids such as dirt and rust.1 This test method is under 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 Dec. 1, 2012June 15
12、, 2013. Published March 2013August 2013. Originally approved in 1938. Last previous edition approved in 20072012 asD482D482 12.07. DOI: 10.1520/D0482-12.10.1520/D0482-13.In the IP, this test method is under the jurisdiction of the Standardization Committee. This test method was adopted as a joint AS
13、TM-IP standard in 1965.2 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 Summary page on the ASTM website.This document is not an ASTM standard
14、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 recommends that users consult prior editions as appropriate. In all cases onl
15、y 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, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Evapo
16、rating Dish or Crucible , made of platinum, silica, or porcelain, of 90 mL minimum capacity to 120-mL maximumcapacity.a capacity of 50 to 150 mL.NOTE 3Alumina vessels may be used where appropriate. The use of vessels that are not made of platinum may contaminate the ash.5.2 Electric Muffle Furnace,
17、capable of maintaining a temperature of 775 6 25C and preferably having suitable apertures atthe front and rear so as to allow a slow natural draught of air to pass through.through or a programmable furnace controlling bothtemperature and air flow is suitable.5.3 Meeker Gas Burner, or equivalent.5.4
18、 Mechanical Shaker.5.5 Filter Paper.6. Reagents6.1 Propan-2-ol (WarningFlammable, can be explosive when evaporated to or near dryness.)6.2 Toluene(WarningFlammable, toxic.)6.3 Quality Control (QC) Samples , preferably are portions of one or more liquid petroleum materials that are stable andrepresen
19、tative of the samples of interest. These QC samples can be used to check the validity of the testing process as describedin Section 11.7. Sampling7.1 Obtain samples in accordance with the instructions in Practice D4057 or D4177. Before transferring the portion of thesample to be ashed to the evapora
20、ting dish or crucible, take particular care to ensure that the portion taken is truly representativeof the larger portion. Vigorous shaking can be necessary.8. Procedure8.1 Heat the evaporating dish or crucible that is to be used for the test at 700 to 800C for a minimum of 10 min. Cool to roomtempe
21、rature in a suitable container, and weigh to the nearest 0.1 mg.NOTE 4The container in which the dish or crucible is cooled can be a desiccator not containing a desiccating agent. In addition, all weighings of thecrucibles should be performed as soon as the crucibles have cooled. If it should be nec
22、essary that the crucibles remain in the desiccator for a longer period,then all subsequent weighings should be made after allowing the crucibles and contents to remain in the desiccator for the same length of time.8.2 When the sample is sufficiently mobile, mix thoroughly before weighing. The mixing
23、 is necessary to distribute catalyst finesand other particulate material throughout the sample. Satisfactory mixing can usually be achieved by 10 min of manual shakingor 10 min using a mechanical shaker. Examine the sample for homogeneity before proceeding with 8.3. Continue mixing thesample if it i
24、s not homogeneous.8.2.1 When it is evident that the sample is not homogenized after repeated mixings, or there is a reasonable doubt, anon-aerating, high-speed shear mixer can be used. Such a device is described in Annex A1 of Test Methods D4928.8.2.2 When the sample cannot be satisfactorily homogen
25、ized, reject the sample and acquire a new sample.8.2.3 When the sample is viscous or solid at room temperature, heat the container carefully until the sample is entirely liquidand mix carefully. An oven at an appropriate temperature can be used.8.2.4 The sample can contain water. After heating in an
26、 oven, the water can boil causing splattering or foaming. The operatorshall proceed cautiously with the heating step, wearing appropriate personnel protective equipment, such as safety goggles andgloves. Mixing this type of sample shall be done carefully. Stirring, rather than shaking, is an option.
27、8.3 The quantity of test specimen taken for testing will depend upon the ash content expected in the sample. Refer to Table 1.The weighing procedure will also depend upon whether the sample requires heating or not, and whether more than one portionhas to be weighed.TABLE 1 Test Specimen Mass versus
28、AshExpected Ash, mass % Test Specimen,mass, g Ash Mass, mg0.18 11 200.10 20 200.05 40 200.04 50 200.02 100 200.01 100 100.001 100 1D482 1328.4 Using a top-loading balance, weigh into the dish or crucible sufficient test specimen to the nearest 0.1 g to yield no morethan 20 mg of ash. Determine the m
29、ass of the test specimen used in the analysis at ambient temperature. One way to do this isto take the difference between the initial and final masses of the sample container weighed at ambient temperatures. If one weighingis sufficient, as determined from Table 1, or experience, proceed with steps
30、8.6-8.11.8.5 If more than one addition of test specimen is required, proceed only through 8.6 (noting 8.6.1 and 8.7) and allow the dishor crucible to cool to ambient temperature before adding more sample as outlined in 8.4. Proceed with steps 8.6-8.11.8.6 Carefully heat the dish or crucible with a M
31、eeker burner or equivalent until the contents can be ignited by the flame.Maintain the dish or crucible at such a temperature that the sample continues to burn at a uniform and moderate rate leaving onlya carbonaceous residue when the burning ceases. A hot plate can be used at this stage.8.6.1 The t
32、est sample may contain water that can cause spattering. The operator shall heat the test portion cautiously whilewearing appropriate personnel protective equipment, such as safety goggles and gloves. If spattering is very severe, so that materialescapes the confines of the dish or the crucible, disc
33、ard the test portion. If the first test portion is discarded, add 2 6 1 mL ofpropan-2-ol (WarningFlammable) to a second test portion while stirring with a glass rod and warming the test portion gentlyto liquefy if it is solid or near solid. Proceed as described in 8.6. If this is unsuccessful, repea
34、t on a third test portion using a 1061 mLmixture of 5065 % by volume toluene (WarningFlammable.Vapor harmful) and 5065 % by volume of propan-2-ol.In either case, any test specimen that adheres to the glass rod can be returned to the dish using a strip of ashless filter paper.Continue burning as outl
35、ined in 8.6.8.7 Vigilance by the operator is mandatory; burning samples shall never be left unattended.8.8 Some test specimens will require extra heating after the burning has ceased, particularly heavy samples such as marine fuelswhich form crusts over the unburned material. The crust can be broken
36、 with a glass rod. Any crust that adheres to the glass rodcan be returned to the dish using a strip of ashless filter paper. Burn the remaining test specimen.8.9 The heavier material tends to foam, therefore the operator shall exercise considerable care. Overheating shall be avoidedso that neither t
37、he test specimen nor the dish are heated to a red hot appearance, as this can result in loss of ash. Likewise, theflame shall never be higher than the rim of the dish to avoid superheating the crust, thereby producing sparks that can result inconsiderable loss of ash.8.10 Heat the residue in the muf
38、fle furnace at 775625C until all carbonaceous material has disappeared. Cool the dish to roomtemperature in a suitable container (Note 34), and weigh to the nearest 0.1 mg.8.11 Reheat the dish at 775 6 25 C for at least 20 min, cool in a suitable container (Note 34), and reweigh. Repeat the heating,
39、cooling, and weighing process until consecutive weighings differ by not more than 0.5 mg.9. Calculation9.1 Calculate the mass of the ash as a percentage of the original samples as follows:Ash,mass %5w/W! 3100 (1)where:w = mass of ash, g, andW = mass of sample, g.10. Report10.1 Report the results as
40、follows:Test Specimen Mass Report9.00 to 39.99 g 3 decimal places40.00 or more g 3 to 4 decimal places10.2 Record the value reported as ash in accordance with Test Method D482, stating the mass of the sample taken.11. Quality Control:11.1 Confirm the performance of the instrument or the test procedu
41、re by analyzing a QC sample (see 6.3).11.1.1 When QC/Quality Assurance (QA) protocols are already established in the testing facility, these may be used to confirmthe reliability of the test result.11.1.2 When there is no QC/QA protocol established in the testing facility, Appendix X1 can be used as
42、 the QC/QA system.12. Precision and Bias312.1 The precision of this test method as obtained by statistical examination of interlaboratory test results is as follows:3 No ASTM Research Report is available for this standard.D482 13312.1.1 RepeatabilityThe difference between successive tests results, o
43、btained by the same operator with the same apparatusunder constant operating conditions on identical test material would, in the long run, in the normal and correct operation of thetest method, exceed the following values only in one case in twenty:Ash, mass % Repeatability0.001 to 0.079 0.0030.080
44、to 0.180 0.00712.1.2 ReproducibilityThe difference between two single and independent results obtained by different operators in differentlaboratories on identical test material would, in the long run, in the normal and correct operation of the test method, exceed thefollowing values only in one cas
45、e in twenty:Ash, mass % Reproducibility0.001 to 0.079 0.0050.080 to 0.180 0.02412.2 BiasThe bias of this test method cannot be determined since an appropriate standard reference material containing aknown level of ash in liquid petroleum hydrocarbon is not available.13. Keywords13.1 ash; crude oils;
46、 distillate oils; fuel oils; lubricating oilsAPPENDIX(Nonmandatory Information)X1. QUALITY CONTROLX1.1 Confirm the performance of the instrument or the test procedure by analyzing a QC sample.X1.2 Prior to monitoring the measurement process, the user of the test method needs to determine the average
47、 value and controllimits of the QC sample (see Practices D6299 and D6792 and MNL 7).4X1.3 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 Practices D6299 and D6792 and MNL 7
48、). Any out-of-control data should triggerinvestigation for 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 process, and customer re
49、quirements. Generally, a QCsample is analyzed each testing day with routine samples. The QC frequency should be increased if a large number of samples areroutinely analyzed. However, when it is demonstrated that the testing is under statistical control, the QC testing frequency maybe reduced. The QC sample 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
