1、Designation: D 1018 00 (Reapproved 2005)An American National StandardStandard Test Method forHydrogen In Petroleum Fractions1This standard is issued under the fixed designation D 1018; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, the year 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. Scope1.1 This test method cover
3、s the determination of hydrogenin petroleum fractions that can be burned completely withoutsmoking in a wick lamp.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theres
4、ponsibility 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 1266 Test Method for Sulfur in Petroleum Products(Lamp Method)D 4057 Practice for Manual
5、 Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformance3. Summary of Test Method3.1 The test specimen is burned from
6、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 performancecharacteristics.4.2 This te
7、st 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 shown in Fig. 1. The burner
8、 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 flask.NOTE 1The lamp and bu
9、rner are constructed in accordance withAppendix A3 of Test Method D 1266.5.2 ChimneyA chimney (see Note 2) conforming to thedimensions shown in Fig. 1.NOTE 2The chimney is constructed in accordance with Appendix A3of Test Method D 1266, except that the delivery tube is cut off and a shortlength of g
10、lass 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 manner: a 1-to 2-cm layer
11、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, uniform, two-strandtwisted
12、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 chamber packedwith gla
13、ss 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 May 1, 2005. Published May 2005. Originally
14、approved in 1949. Last previous edition approved in 2000 as D 1018 00.2For 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.3Turner-type absorption bulbs are satisfactory for this test method.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.anhydrous calcium sulfate4and phosphorus pentoxide in thatorder. A length of rubber tubing suitable for conn
16、ection 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 hold the two absorbersin tandem, immersed to a depth of approximately 5 cm.6. Reagents and Materials6.1 Purity of Re
17、agentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is f
18、irst 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, anhydrous (CaSO4).6.4 Phosphorous pentoxide (P2O5).6.5 Sulfuric acid (H2SO4), relative density 1.84.6.6 Quality Contr
19、ol (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 validity of the testing process, asdescribed in Section 10.7. Sampling7.1 Obtain samples in accordance with the instru
20、ctions inPractices D 4057 or D 4177. Ensure that test specimens arerepresentative of the test unit. Vigorous stirring or shaking maybe necessary.8. Procedure8.1 Connect the charged absorbers to each other and to thechimney delivery tube as shown in the complete assembly ofthe apparatus in Fig. 2.Att
21、ach 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 absorbers into the ice-water bath,connect the air flow system to the chimney, and purge thesystem with air for 15 min (War
22、ningsee 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 with a lint-free dry cloth,and place them beside the balance case for 30 min or more.Open the absorbers for a momen
23、t 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 (see Note 3) by drawing the strand through the burnertube with a small metal hook. Trim the wick as closely aspossibl
24、e 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, and insert the prepared burner into the flask. Capthe burner with its glass cap, and close the burner air inlet wit
25、ha 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, the volatility of the test specimen, thetightness of the wick in the burner tube, and the position of the wickrelati
26、ve 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 wick is required for highly volatile4The sole source of supply of the apparatus known to the committee at this ti
27、meis Drierite, available from Fisher Scientific, 711 Forbes Avenue, Pittsburgh, PA15219. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee
28、1, which you may attend.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, 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
29、United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.NOTE 1In the case of those dimensions for which no specifictolerances are designated above, the permissible variation is 610%tothenearest 1 mm, provided, however, that in no case shall the devi
30、ation begreater than 5 mm.FIG. 1 Lamp and ChimneyD 1018 00 (2005)2samples; also, the wick may have to be drawn down several millimetresbelow the top of the burner tube. Extremely volatile test specimens(WarningExtremely flammable.) may require immersion of the burnerflask in an ice-water bath during
31、 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 to the burner. In any case, the flame must burn smoothly andsymmetrically without jets in the inner cone o
32、r 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 nearest 1 mgand bring it immediately to the absorption train. Open theabsorbers in the train. Remove the ca
33、p 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. Immediatelyinsert the lamp in the chimney, using rubber bands or small coilsprings to hold the lamp in plac
34、e. 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 in rate of air flowafter it has been inserted in the chimney.8.5 After the desired amount (2 to 3 g) of test
35、 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 quickly as possible, connect the air line to a clean,thoroughly dry, assembled lamp and insert it in the chi
36、mney.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 tube,gently heat the tube with a microburner until all moisture hasbeen vaporized and swept into the absorber
37、s. 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, equilibrate,and weigh to the nearest 1 mg.9. Calculation9.1 Correct the mass of water formed for the lost
38、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 seconds.9.2 Calculate the hydrogen content of the sample as follows:Hydrogen, weight % 5 W 3 11.191!/S (2)where:
39、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/Quality Assurance (QA) protocols arealready established in the testing facility, these may be used toconfirm th
40、e 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. Precision and Bias611.1 The precision of this test method is not known to havebeen obtained in accordance with currently accepted guidelines(for
41、example, in Committee D02 Research Report RR:D02-1007).6There 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 AssemblyD 1018 00 (2005)311.2 The p
42、recision of this test method as obtained bystatistical examination of interlaboratory test results is asfollows:11.2.1 RepeatabilityThe difference between successivetest results obtained by the same operator with the sameapparatus under constant operating conditions on identical testmaterial would,
43、in the long run, in the normal and correctoperation of the test method, exceed the following value onlyin one case in twenty:Hydrogen Content,mass % Repeatability11 to 16 0.1111.2.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in di
44、fferent laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the following value only in one case in twenty:Hydrogen Content,mass % Reproducibility11 to 16 0.1811.3 BiasThe bias of this test method cannot be deter-mined since an
45、 appropriate standard reference material con-taining a known level of hydrogen in liquid petroleum hydro-carbon is not available.12. Keywords12.1 hydrogen; lampAPPENDIX(Nonmandatory Information)X1. QUALITY CONTROLX1.1 Confirm the performance of the instrument or the testprocedure by analyzing a qual
46、ity control (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 Practice D 6299).7,8X1.3 Record the QC results, and analyze by control chartsor other statistically equivalent techniques
47、to ascertain thestatistical control status of the total testing process (see PracticeD 6299).7,8Any out-of-control data should trigger investiga-tion 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
48、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 samples are routinely analyzed. However,when it is demonstrated th
49、at 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 QC sample materialshould be available for the intended period of use, and must behomogeneous and stable under the anticipated storageconditions.ASTM International takes no position respecting the validity of any pa
