1、Designation: D 482 07Designation: 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 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly. The preferred expression of the property is mass %.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its us
7、e. 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 Standards:2D 874 Test Method for Sulfated Ash from Lubricating Oilsand AdditivesD 4057
8、 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 4928 Test Methods for Water in Crude Oils by Coulom-etric Karl Fischer TitrationD 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate
9、Analytical Measurement SystemPerformanceD 6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3. Summary of Test Method3.1 The sample contained in a suitable vessel is ignited andallowed to burn until only ash and carbon remain. Thecarbonaceous residue is reduced
10、 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 provide information as to whether ornot the product is suitable for use in a given application. Ashcan result from oil or water-solu
11、ble 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 capacity to 120-mL maxi-mum capacity.5.2 Electric Muffle Furnace, capable of maintaining a tem-perature of 775 6 25C and prefera
12、bly 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.31This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsib
13、ility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved Dec. 1, 2007. Published January 2008. Originallyapproved in 1938. Last previous edition approved in 2003 as D 48203.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was a
14、dopted as a joint ASTM-IP standard in 1965.2For 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.3The sole source o
15、f 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 provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ame
16、eting 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 Box C700, West Conshohocken, PA 19428-2959, United States.Copyright by ASTM Intl (all rights reserved); Mon Ap
17、r 21 02:17:39 EDT 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.6. Reagents6.1 Propan-2-ol(WarningFlammable, can be explo-sive when evaporated to or near dryness.)6.2 Toluene(WarningFlammable, toxic.)6.3 Quality Control (QC) Samples, pre
18、ferably 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 validity of the testing process asdescribed in Section 11.7. Sampling7.1 Obtain samples in accordance with the instructions inPractice
19、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 trulyrepresentative of the larger portion. Vigorous shaking can benecessary.8. Procedure8.1 Heat the evaporating dish or crucible th
20、at 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 container in which the dish or crucible is cooled can bea desiccator not containing a desiccating agent. In addition, all weighingsof the cru
21、cibles 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 subsequent weighings should be made afterallowing the crucibles and contents to remain in the desiccator for thesame length of time.8.2 W
22、hen the sample is sufficiently mobile, mix thoroughlybefore weighing. The mixing is necessary to distribute catalystfines and other particulate material throughout the sample.Satisfactory mixing can usually be achieved by 10 min ofmanual shaking or 10 min using a mechanical shaker. Examinethe sample
23、 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 repeated mixings, or there is a reasonable doubt, anon-aerating, high-speed shear mixer can be used. Such adevice is described in Annex A1
24、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 solid at room tempera-ture, heat the container carefully until the sample is entirelyliquid and mix carefully.An oven at an appropriate t
25、emperaturecan 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 cautiously with the heating step, wear-ing appropriate personnel protective equipment, such as safetygoggles and gloves. Mixing this type of
26、 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 expected in the sample. Refer toTable 1. The weighing procedure will also depend uponwhether the sample requires heating or not, and whether
27、 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 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 th
28、e 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,or 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
29、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 heat the dish or crucible with a Meeker burneror equivalent until the contents can be ignited by the flame.Maintain the dish or crucible
30、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 used at this stage.8.6.1 The test sample may contain water that can causespattering. The operator shall heat the test portion cautiously
31、while wearing appropriate personnel protective equipment,such as safety goggles and gloves. If spattering is very severe,so that material escapes the confines of the dish or the crucible,discard the test portion. If the first test portion is discarded, add2 6 1 mL of propan-2-ol (WarningFlammable) t
32、o 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 is unsuccessful, repeat on a third testportion using a 10 6 1 mL mixture of 50 6 5 % by volumetoluene (WarningFlammable. Vapor harmfu
33、l) 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 paper. Continue burning as outlined in 8.6.8.7 Vigilance by the operator is mandatory; burning samplesshall never be left unattended.8.8 S
34、ome test specimens will require extra heating after theburning has ceased, particularly heavy samples such as marinefuels which form crusts over the unburned material. 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 ashless
35、filter paper. Burn the remaining test specimen.8.9 The heavier material tends to foam, therefore the opera-tor shall exercise considerable care. Overheating shall beavoided so that neither the test specimen nor the dish are heatedto a red hot appearance, as this can result in loss of ash.Likewise, t
36、he 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.TABLE 1 Test Specimen Mass versus AshExpected Ash, mass %Test Specimen,mass, gAsh Mass, mg0.18 11 200.10 20 200.05 40 200.04 50 200.02 100 200.0
37、1 100 100.001 100 1D482072Copyright by ASTM Intl (all rights reserved); Mon Apr 21 02:17:39 EDT 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.8.10 Heat the residue in the muffle furnace at 775 6 25Cuntil all carbonaceous material has dis
38、appeared. Cool the dishto room temperature in a suitable container (Note 3), and weighto the nearest 0.1 mg.8.11 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
39、 not more than 0.5 mg.9. Calculation9.1 Calculate 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 place
40、s40.00 or more g 3 to 4 decimal places10.2 Record 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 Assur
41、ance (QA) protocols arealready established in 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 Bias412.1 The precision of this t
42、est method as obtained bystatistical examination 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,
43、 in the normal and correctoperation of the test 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 labo
44、ratories on identical test material would, in 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 a
45、n appropriate standard reference material con-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
46、 or the testprocedure by analyzing a 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 Practices D 6299 andD 6792 and MNL 7).5X1.3 Record the QC results and analyze by control chartsor o
47、ther statistically equivalent techniques, to ascertain thestatistical control status of the total testing process (seePractices D 6299 and D 6792 and MNL 7). Any out-of-controldata should trigger investigation for root cause(s).X1.4 In the absence of explicit requirements given in thetest method, th
48、e frequency of 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 sample
49、s are routinely 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 regularly tested be representative of the material4No ASTM Research Report is available for this standard.5ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,6thed., ASTM International, W. Conshohocken, PA.D482073Copyright by ASTM Intl (all
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