1、Designation: D 482 03Designation: 4/96An American National StandardStandard Test Method forAsh from Petroleum Products1This standard is issued under the fixed designation D 482; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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 standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the
3、determination of ash in therange 0.0010.180 mass %, from distillate and residual fuels,gas turbine fuels, crude oils, lubricating oils, waxes, and otherpetroleum products, in which any ash-forming materialspresent are normally considered to be undesirable impurities orcontaminants (Note 1). The test
4、 method is limited to petroleumproducts which are free from added ash-forming additives,including certain phosphorus compounds (Note 2).NOTE 1In certain types of samples, all of the ash-forming metals arenot retained quantitatively in the ash. This is particularly true of distillateoils, which requi
5、re a special ash procedure in order to retain metalsquantitatively.NOTE 2This test method is not intended for the analysis of unusedlubricating oils containing additives; for such samples use Test MethodD 874. Neither is it intended for the analysis of lubricating oils containinglead nor for used en
6、gine crankcase oils.1.2 SI units are regarded as the standard. The preferredexpression of the property is mass %.1.3 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 sa
7、fety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 874 Test Method for Sulfated Ash from Lubricating Oilsand Additives2D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products3D 4177 Practice for
8、 Automatic Sampling of Petroleum andPetroleum Products3D 4928 Test Methods for Water in Crude Oils by Coulom-etric Karl Fischer Titration3D 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformance43. Summary of Test Method3.1 The sample
9、contained in a suitable vessel is ignited andallowed to burn until only ash and carbon remain. Thecarbonaceous residue is reduced to an ash by heating in amuffle furnace at 775C, cooled and weighed.4. Significance and Use4.1 Knowledge of the amount of ash-forming materialpresent in a product can pro
10、vide information as to whether ornot the product is suitable for use in a given application. Ashcan result from oil or water-soluble metallic compounds orfrom extraneous solids such as dirt and rust.5. Apparatus5.1 Evaporating Dish or Crucible, made of platinum, silica,or porcelain, of 90 mL minimum
11、 capacity to 120-mL maxi-mum capacity.5.2 Electric Muffle Furnace, capable of maintaining a tem-perature of 775 6 25C and preferably having suitableapertures at the front and rear so as to allow a slow naturaldraught of air to pass through.5.3 Meeker Gas Burner, or equivalent.5.4 Mechanical Shaker.5
12、6. Reagents6.1 Propan-2-ol(WarningFlammable, can be explo-sive when evaporated to or near dryness.)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approv
13、ed May 10, 2003. Published May 2003. Originallyapproved in 1938. Last previous edition approved in 2002 as D 48202.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was adopted as a joint ASTM-IP standard in 1965.2Annual Book of ASTM Standards, V
14、ol 05.01.3Annual Book of ASTM Standards, Vol 05.02.4Annual Book of ASTM Standards, Vol 05.03.5The sole source of supply of the mechanical shaker known to the committee atthis time is the Eberbach Corp., 505 S. Maple Rd., Ann Arbor, MI 48106-1024. Ifyou are aware of alternative suppliers, please prov
15、ide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO
16、 Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Toluene(WarningFlammable, toxic.)6.3 Quality Control (QC) Samples, preferably are portionsof one or more liquid petroleum materials that are stable andrepresentative of the samples of interest. These QC samplescan be used to check the va
17、lidity of the testing process asdescribed in Section 11.7. Sampling7.1 Obtain samples in accordance with the instructions inPractice D 4057 or D 4177. Before transferring the portion ofthe sample to be ashed to the evaporating dish or crucible, takeparticular care to ensure that the portion taken is
18、 trulyrepresentative of the larger portion. Vigorous shaking can benecessary.8. Procedure8.1 Heat the evaporating dish or crucible that is to be usedfor the test at 700 to 800C for a minimum of 10 min. Cool toroom temperature in a suitable container, and weigh to thenearest 0.1 mg.NOTE 3The containe
19、r in which the dish or crucible is cooled can bea desiccator not containing a desiccating agent. In addition, all weighingsof the crucibles should be performed as soon as the crucibles have cooled.If it should be necessary that the crucibles remain in the desiccator for alonger period, then all subs
20、equent weighings should be made afterallowing the crucibles and contents to remain in the desiccator for thesame length of time.8.2 When the sample is sufficiently mobile, mix thoroughlybefore weighing. The mixing is necessary to distribute catalystfines and other particulate material throughout the
21、 sample.Satisfactory mixing can usually be achieved by 10 min ofmanual shaking or 10 min using a mechanical shaker. Examinethe sample for homogeneity before proceeding with 8.3.Continue mixing the sample if it is not homogeneous.8.2.1 When it is evident that the sample is not homogenizedafter repeat
22、ed mixings, or there is a reasonable doubt, anon-aerating, high-speed shear mixer can be used. Such adevice is described in Annex A1 of Test Methods D 4928.8.2.2 When the sample cannot be satisfactorily homog-enized, reject the sample and acquire a new sample.8.2.3 When the sample is viscous or soli
23、d at room tempera-ture, heat the container carefully until the sample is entirelyliquid and mix carefully. An oven at an appropriate temperaturecan be used.8.2.4 The sample can contain water. After heating in anoven, the water can boil causing splattering or foaming. Theoperator shall proceed cautio
24、usly with the heating step, wear-ing appropriate personnel protective equipment, such as safetygoggles and gloves. Mixing this type of sample shall be donecarefully. Stirring, rather than shaking, is an option.8.3 The quantity of test specimen taken for testing willdepend upon the ash content expect
25、ed in the sample. Refer toTable 1. The weighing procedure will also depend uponwhether the sample requires heating or not, and whether morethan one portion has to be weighed.8.4 Using a top-loading balance, weigh into the dish orcrucible sufficient test specimen to the nearest 0.1 g to yield nomore
26、than 20 mg of ash. Determine the mass of the testspecimen used in the analysis at ambient temperature. One wayto do this is to take the difference between the initial and finalmasses of the sample container weighed at ambient tempera-tures. If one weighing is sufficient, as determined from Table 1,o
27、r experience, proceed with steps 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 thedish or crucible to cool to ambient temperature before addingmore sample as outlined in 8.4. Proceed with steps 8.6-8.11.8.6 Carefully hea
28、t the dish or crucible with a Meeker burneror equivalent until the contents can be ignited by the flame.Maintain the dish or crucible at such a temperature that thesample continues to burn at a uniform and moderate rateleaving only a carbonaceous residue when the burning ceases.A hot plate can be us
29、ed at this stage.8.6.1 The test sample may contain water that can causespattering. The operator shall heat the test portion cautiouslywhile wearing appropriate personnel protective equipment,such as safety goggles and gloves. If spattering is very severe,so that material escapes the confines of the
30、dish or the crucible,discard the test portion. If the first test portion is discarded, add2 6 1 mL of propan-2-ol (WarningFlammable) to a secondtest portion while stirring with a glass rod and warming the testportion gently to liquefy if it is solid or near solid. Proceed asdescribed in 8.6. If this
31、 is unsuccessful, repeat on a third testportion using a 10 6 1 mL mixture of 50 6 5 % by volumetoluene (WarningFlammable. Vapor harmful) and 50 6 5%by volume of propan-2-ol. In either case, any test specimen thatadheres to the glass rod can be returned to the dish using a stripof ashless filter pape
32、r. Continue burning as outlined in 8.6.8.7 Vigilance by the operator is mandatory; burning samplesshall never be left unattended.8.8 Some test specimens will require extra heating after theburning has ceased, particularly heavy samples such as marinefuels which form crusts over the unburned material
33、. The crustcan be broken with a glass rod. Any crust that adheres to theglass rod can be returned to the dish using a strip of ashlessfilter paper. Burn the remaining test specimen.8.9 The heavier material tends to foam, therefore the opera-tor shall exercise considerable care. Overheating shall bea
34、voided so that neither the test specimen nor the dish are heatedto a red hot appearance, as this can result in loss of ash.Likewise, the flame shall never be higher than the rim of thedish to avoid superheating the crust, thereby producing sparksthat can result in considerable loss of ash.8.10 Heat
35、the residue in the muffle furnace at 775 6 25Cuntil all carbonaceous material has disappeared. Cool the dishto room temperature in a suitable container (Note 3), and weighto the nearest 0.1 mg.TABLE 1 Test Specimen Mass versus AshExpected Ash, mass %Test Specimen,mass, gAsh Mass, mg0.18 11 200.10 20
36、 200.05 40 200.04 50 200.02 100 200.01 100 100.001 100 1D4820328.11 Reheat the dish at 775 6 25 C for at least 20 min, coolin a suitable container (Note 3), and reweigh. Repeat theheating, cooling, and weighing process until consecutiveweighings differ by not more than 0.5 mg.9. Calculation9.1 Calcu
37、late the mass of the ash as a percentage of theoriginal samples as follows:Ash, mass % 5 w/W! 3 100 (1)where:w = mass of ash, g, andW = mass of sample, g.10. Report10.1 Report the results as follows:Test Specimen Mass Report9.00 to 39.99 g 3 decimal places40.00 or more g 3 to 4 decimal places10.2 Re
38、cord the value reported as ash in accordance withTest Method D 482, stating the mass of the sample taken.11. Quality Control11.1 Confirm the performance of the instrument or the testprocedure by analyzing a QC sample (see 6.3).11.1.1 When QC/Quality Assurance (QA) protocols arealready established in
39、 the testing facility, these may be used toconfirm the reliability of the test result.11.1.2 When there is no QC/QA protocol established in thetesting facility, Appendix X1 can be used as the QC/QAsystem.12. Precision and Bias612.1 The precision of this test method as obtained bystatistical examinat
40、ion of interlaboratory test results is asfollows:12.1.1 RepeatabilityThe difference between successivetests results, obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial would, in the long run, in the normal and correctoperation of the te
41、st method, exceed the following values onlyin one case in twenty:Ash, mass % Repeatability0.001 to 0.0790.080 to 0.1800.0030.00712.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators indifferent laboratories on identical test material would, in
42、 thelong run, in the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:Ash, mass % Reproducibility0.001 to 0.0790.080 to 0.1800.0050.02412.2 BiasThe bias of this test method cannot be deter-mined since an appropriate standard reference material con
43、-taining a known level of ash in liquid petroleum hydrocarbonis not available.13. Keywords13.1 ash; crude oils; distillate oils; fuel oils; lubricating oilsAPPENDIX(Nonmandatory Information)X1. QUALITY CONTROLX1.1 Confirm the performance of the instrument or the testprocedure by analyzing a QC sampl
44、e.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).7X1.3 Record the QC results and analyze by control chartsor other statistically equivalent techniques, to ascertain th
45、estatistical 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 of QC testing is dependent on thecriticality of the quali
46、ty 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 routinely analyzed. However,when it is demonstrated that the te
47、sting 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 materialroutin
48、ely 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 Control Charting techniques.6No ASTM Research Report is avail
49、able for this standard.7ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,6thed., ASTM International, W. Conshohocken, PA.D482033SUMMARY OF CHANGESSubcommittee D02.03 has identified the location of selected changes to this standard since the last issue(D 48202) that may impact the use of this standard.(1) Updated Table 1 to correct the “Test Specimen, mass, g”value from “9” to “11” for an “Expected Ash, mass %” valueof 0.18 to align with the calculated value determined by Eq 1.ASTM International takes no position respecting the validity of any patent
