ASTM D1018-2011 Standard Test Method for Hydrogen In Petroleum Fractions《石油馏分中氢含量的标准试验方法》.pdf

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1、Designation: D1018 11Standard Test Method forHydrogen In Petroleum Fractions1This standard is issued under the fixed designation D1018; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parenthe

2、ses 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 hydrogenin petroleum fract

3、ions that can be burned completely withoutsmoking in a wick lamp.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 standard does not purport to address all of thesafety concerns, if any, associated with its use. It is

4、 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:2D1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D4057 Practice for M

5、anual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3. Summary of Test Method3.1 The test

6、specimen is burned from a cotton wick in anatmosphere of purified air. The water formed is collected fromthe combustion gases by a desiccant and weighed.4. Significance and Use4.1 Knowledge of the hydrogen content of petroleum prod-ucts, particularly fuels, can be helpful in assessing performancecha

7、racteristics.4.2 This test method is suitable for most laboratory appli-cations requiring the determination of hydrogen in liquidpetroleum lubricants and products.5. Apparatus5.1 LampA lamp (see Note 1) consisting of a 25-mLErlenmeyer flask, a burner, and a burner cap conforming to thedimensions sho

8、wn in Fig. 1. The burner consists of twoconcentric glass tubes, the external one having an arm,provided with standard-taper glass joints for connection withthe flask, chimney, and burner cap. The burner has a smallopening near its base to allow equalization of the pressurebetween the chimney and fla

9、sk.NOTE 1The lamp and burner are constructed in accordance withAppendix A3 of Test Method D1266.5.2 ChimneyA chimney (see Note 2) conforming to thedimensions shown in Fig. 1.NOTE 2The chimney is constructed in accordance with Appendix A3of Test Method D1266, except that the delivery tube is cut off

10、and a shortlength of glass tubing is sealed on at right angles to the chimney. Thesecondary air inlet is not used and is sealed off.5.3 AbsorbersTwo absorption bulbs3suitable for collect-ing and weighing the water formed during combustion of thesample. The bulbs shall be filled in the following mann

11、er: a 1-to 2-cm layer of glass wool, a 5-cm layer of 6- to 10-mesh cpanhydrous calcium chloride, a 1-cm layer of glass wool, a 2-cmlayer of phosphorus pentoxide, and glass wool to the top of theabsorbers. One filling is sufficient for approximately 10 g ofwater.5.4 Cotton WickingClean, unused, unifo

12、rm, two-strandtwisted cotton wicking of good quality, weighing 0.5 to 0.6 g/mper strand.5.5 Air Purifying SystemThe compressed air (WarningCompressed gas under higher pressure) for the combustionshall be purified by passage through a scrubber containingsulfuric acid (relative density 1.84), a surge

13、chamber packedwith glass wool, and a drying tower filled with 10 to 20-mesh1This 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 approved June 1, 2011. Publish

14、ed July 2011. Originally approvedin 1949. Last previous edition approved in 2005 as D101800(2005). DOI:10.1520/D1018-11.2For 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

15、 to the standards Document Summary page onthe ASTM website.3Turner-type absorption bulbs are satisfactory for this test method.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

16、 States.anhydrous calcium sulfate4and phosphorus pentoxide in thatorder. A length of rubber tubing suitable for connection to theinlet tube of the burner shall be connected to the exit of thetower.5.6 Drying TubeA small U-tube containing anhydrouscalcium sulfate.45.7 Ice-Water Bath, large enough to

17、hold the two absorbersin tandem, immersed to a depth of approximately 5 cm.6. Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagent

18、s of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Calcium chloride (CaCl2).6.3 Calcium sulfate, a

19、nhydrous (CaSO4).6.4 Phosphorous pentoxide (P2O5).6.5 Sulfuric acid (H2SO4), relative density 1.84.6.6 Quality Control (QC) Samples, preferably, portions ofone or more liquid petroleum materials that are stable andrepresentative of the samples of interest. These QC samplescan be used to check the va

20、lidity of the testing process, asdescribed in Section 10.7. Sampling7.1 Obtain samples in accordance with the instructions inPractices D4057 or D4177. Ensure that test specimens arerepresentative of the test unit. Vigorous stirring or shaking maybe necessary.8. Procedure8.1 Connect the charged absor

21、bers to each other and to thechimney delivery tube as shown in the complete assembly ofthe apparatus in Fig. 2.Attach the U-tube containing anhydrouscalcium sulfate4to the exit end of the second absorber toeliminate diffusion of water vapor back into the system.Immerse the lower half of the absorber

22、s into the ice-water bath,connect the air flow system to the chimney, and purge thesystem with air for 15 min (Warningsee 5.5.) At the end ofthe purging period, turn off the air flow, close the absorbers,and remove them from the train. Allow the absorbers to reachroom temperature, gently wipe each w

23、ith a lint-free dry cloth,and place them beside the balance case for 30 min or more.Open the absorbers for a moment to equalize the pressure,close, and weigh to the nearest 1 mg.8.2 While the absorbers are standing, the lamp may beprepared. Thread the burner with the proper number of wickstrands (se

24、e Note 3) by drawing the strand through the burnertube with a small metal hook. Trim the wick as closely aspossible to the top of the burner, and draw the trimmed wickdown until it is flush with or slightly below the top of theburner. Pipet approximately 5 mL of test specimen into theburner flask, a

25、nd insert the prepared burner into the flask. Capthe burner with its glass cap, and close the burner air inlet witha rubber policeman. Allow the sample to rise by capillaryaction to the top of the wick.NOTE 3The burning characteristics of the flame are dependent uponthe flow of air to the burner, th

26、e volatility of the test specimen, thetightness of the wick in the burner tube, and the position of the wickrelative to the top of the burner. The latter two factors can be establishedbefore an actual determination is made so that the flame can be controlledby the rate of air flow. A tightly fitting

27、 wick is required for highly volatile4The sole source of supply of the apparatus known to the committee at this timeis Drierite, available from Fisher Scientific, 711 Forbes Avenue, Pittsburgh, PA15219. If you are aware of alternative suppliers, please provide this information toASTM International H

28、eadquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by th

29、e American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.NOTEIn the case of those dimensions for which no specific tolerancesare designa

30、ted above, the permissible variation is 610 % to the nearest 1mm, provided, however, that in no case shall the deviation be greater than5 mm.FIG. 1 Lamp and ChimneyD1018 112samples; also, the wick may have to be drawn down several millimetresbelow the top of the burner tube. Extremely volatile test

31、specimens(WarningExtremely flammable.) may require immersion of the burnerflask in an ice-water bath during the burning period.Amore loosely fittingwick is required for less volatile test specimens, and in some instances theburner flask may require warming to ensure an even flow of test specimenfuel

32、 to the burner. In any case, the flame must burn smoothly andsymmetrically without jets in the inner cone or smoke on the outer fringes.8.3 Connect the weighed absorbers to the chimney tube,attach the U-tube,4and immerse the absorbers in the ice-waterbath.8.4 Weigh the assembled lamp quickly to the

33、nearest 1 mgand bring it immediately to the absorption train. Open theabsorbers in the train. Remove the cap and rubber policemanfrom the lamp, and connect the air flow to the burner. Ignite thelamp with a microburner, and rapidly adjust the air flow untila symmetrical nonsmoking flame is obtained.

34、Immediatelyinsert the lamp in the chimney, using rubber bands or small coilsprings to hold the lamp in place. Record to the nearest secondthe time that elapsed between ignition of the burner andinsertion of the lamp in the chimney as lost burning time. Theflame may require further minor adjustment i

35、n rate of air flowafter it has been inserted in the chimney.8.5 After the desired amount (2 to 3 g) of test specimen hasbeen burned, interrupt the air flow, immediately remove theburner from the chimney, cap it, and replace the rubberpoliceman. Note and record the time for the complete analysis.As q

36、uickly as possible, connect the air line to a clean,thoroughly dry, assembled lamp and insert it in the chimney.8.6 Weigh the lamp containing the test specimen to thenearest 1 mg.8.7 Purge the system with purified air for a period of 5 min.If any condensed water is visible in the chimney delivery tu

37、be,gently heat the tube with a microburner until all moisture hasbeen vaporized and swept into the absorbers. At the end of thepurging period, turn off the air flow, close the absorbers, andremove them from the train.Allow the absorbers to reach roomtemperature, wipe each with a lint-free dry cloth,

38、 equilibrate,and weigh to the nearest 1 mg.9. Calculation9.1 Correct the mass of water formed for the lost burningtime as follows:W 5 w 3 t/t 2 s!# (1)where:W = corrected grams of water collected,w = grams of water absorbed,t = time in seconds for complete analysis, ands = lost burning time in secon

39、ds.9.2 Calculate the hydrogen content of the sample as follows:Hydrogen, weight % 5 W 3 11.191!/S (2)where:W = corrected grams of water collected, andS = grams of sample burned.10. Quality Control10.1 Confirm the performance of the test procedure byanalyzing a QC sample (see 6.6).10.1.1 When QC/Qual

40、ity Assurance (QA) protocols arealready established in the testing facility, these may be used toconfirm the reliability of the test result.10.1.2 When there is no QC/QA protocol established in thetesting facility, Appendix X1 can be used as the QC/QAsystem.11. Reporting11.1 Report the results to th

41、e nearest 0.1 m%, and indicatethat they were obtained using Test Method D1018.12. Precision and Bias612.1 The precision of this test method is not known to havebeen obtained in accordance with currently accepted guidelines(for example, in Committee D02 Research Report RR:D02-1007).12.2 The precision

42、 of this test method as obtained bystatistical examination of interlaboratory test results is asfollows:12.2.1 RepeatabilityThe difference between successivetest results obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial would, in the l

43、ong run, in the normal and correct6There is no extant ASTM Research Report for this test method.ASulfuric acid scrubber. DLamp and chimney.BSurge chamber. EAbsorption bulbs.CDrierite, phosphorus pentoxide tower. FDrierite tube.FIG. 2 Apparatus AssemblyD1018 113operation of the test method, exceed th

44、e following value onlyin one case in twenty:Hydrogen Content,mass % Repeatability11 to 16 0.1112.2.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in the nor

45、mal and correct operation of the testmethod, exceed the following value only in one case in twenty:Hydrogen Content,mass % Reproducibility11 to 16 0.1812.3 BiasThe bias of this test method cannot be deter-mined since an appropriate standard reference material con-taining a known level of hydrogen in

46、 liquid petroleum hydro-carbon is not available.13. Keywords13.1 hydrogen; lampAPPENDIX(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 use

47、rof the test method needs to determine the average value andcontrol limits of the QC sample (see Practice D6299).7,8X1.3 Record the QC results, and analyze by control chartsor other statistically equivalent techniques to ascertain thestatistical control status of the total testing process (see Pract

48、iceD6299).7,8Any out-of-control data should trigger investigationfor 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 cus

49、tomer 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 reduced. The QCsample precision should be checked against the ASTM testmethod precision to ensure data quality.8X1.5 It is recommended that, if possible, the type of QCsample that is regularly tested be representative of the materialroutinely analyzed. An ample supply of