ASTM D1018-2011(2016) Standard Test Method for Hydrogen In Petroleum Fractions《石油馏分中的氢的标准试验方法 》.pdf

1、Designation: D1018 11 (Reapproved 2016)Standard 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

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 U.S. Department of Defense.1. Scope1.1 This test method covers the determination of hydr

3、ogenin petroleum fractions 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, associat

4、ed 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.2. Referenced Documents2.1 ASTM Standards:2D1266 Test Method for Sulfur in Petroleum Products (LampMetho

5、d)D4057 Practice for Manual 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 Te

6、st Method3.1 The test 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 petroleumproducts, particularly fuels, can be helpful in asse

7、ssing perfor-mance characteristics.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 conformin

8、g to thedimensions shown 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 pressurebetwe

9、en the chimney and flask.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 del

10、ivery tube is cut off 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 bulbs (see Note 3) suitablefor collecting and weighing the water formed during combus-tion of the sample. The bulbs sh

11、all be filled in the followingmanner: a 1 cm to 2 cm layer of glass wool, a 5 cm layer of6 mesh to 10 mesh cp anhydrous calcium chloride, a 1 cm layerof glass wool, a 2 cm layer of phosphorus pentoxide, and glasswool to the top of the absorbers. One filling is sufficient forapproximately 10 g of wat

12、er.NOTE 3Turner-type absorption bulbs are satisfactory for this testmethod.5.4 Cotton WickingClean, unused, uniform, two-strandtwisted cotton wicking of good quality, weighing 0.5 g m to0.6 g m per strand.5.5 Air Purifying SystemThe compressed air (WarningCompressed gas under higher pressure) for th

13、e combustion1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved April 1, 2016. Published May 2016. Originallyapproved in 1949. Last p

14、revious edition approved in 2011 as D1018 11. DOI:10.1520/D1018-11R16.2For 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

15、 website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1shall be purified by passage through a scrubber containingsulfuric acid (relative density 1.84), a surge chamber packedwith glass wool, and a drying tower filled with 10 mesh to

16、20 mesh anhydrous calcium sulfate3and phosphorus pentoxidein that order. A length of rubber tubing suitable for connectionto the inlet tube of the burner shall be connected to the exit ofthe tower.5.6 Drying TubeA small U-tube containing anhydrouscalcium sulfate.35.7 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.4Other 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 sulfate3to 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 4) 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 with3The 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

26、 alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Socie

27、ty, Washington, DC. For suggestions on the testing of reagents notlisted by the 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.N

28、OTE 1In the case of those dimensions for which no specifictolerances are designated above, the permissible variation is 610 % to thenearest 1 mm, provided, however, that in no case shall the deviation begreater than 5 mm.FIG. 1 Lamp and ChimneyD1018 11 (2016)2a rubber policeman. Allow the sample to

29、rise by capillaryaction to the top of the wick.NOTE 4The burning characteristics of the flame are dependent uponthe flow of air to the burner, the 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 t

30、wo factors can be establishedbefore an actual determination is made so that the flame can be controlledby the rate of air flow. A tightly fitting wick is required for highly volatilesamples; also, the wick may have to be drawn down several millimetresbelow the top of the burner tube. Extremely volat

31、ile test 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 spe

32、cimenfuel 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,3and immerse the absorbers in the ice-waterbath.8.4 Weigh the assembled lamp quickl

33、y to the 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 o

34、btained. 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 adj

35、ustment in rate of air flowafter it has been inserted in the chimney.8.5 After the desired amount (2 g to 3 g) of test specimenhas been 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 an

36、alysis.As quickly 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

37、delivery tube,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

38、 dry cloth, 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 ti

39、me in seconds.9.2 Calculate the hydrogen content of the sample as follows:Hydrogen, weight % 5 W 311.191!/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 Wh

40、en QC/Quality 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 res

41、ults to the nearest 0.1 m%, and indicatethat they were obtained using Test Method D1018.ASulfuric acid scrubber. DLamp and chimney.BSurge chamber. EAbsorption bulbs.CDrierite, phosphorus pentoxide tower. FDrierite tube.FIG. 2 Apparatus AssemblyD1018 11 (2016)312. Precision and Bias512.1 The precisio

42、n 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 of this test method as obtained bystatistical examination of interlaboratory test results is asfollows:12.2.1 Repeata

43、bilityThe difference between successivetest 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 test method, exceed the following value onlyin one case in twenty:H

44、ydrogen 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 normal and correct operation of the testmethod,

45、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 liquid petroleum hydro-carbon is not availab

46、le.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 userof the test method needs to determine the av

47、erage value andcontrol limits of the QC sample (see Practice D6299).6,7X1.3 Record the QC results, and analyze by control chartsor other statistically equivalent techniques to ascertain thestatistical control status of the total testing process (see PracticeD6299).6,7Any out-of-control data should t

48、rigger 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 customer requirements.Generally, a QC sample is

49、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.7X1.5 It is recommended that, if possible, the type of QCsample that is regularly tested be representative of the materialroutinely analyzed. An ample supply of QC sample materialshould be available fo