ASTM_D_3229_-_83_scan.pdf

9009276 0027877 22T Designation:D 3229-83 AMERICAN SOCIETY FOR TESTING AND MATERIALS H-24-/5 An Amencan National Standard 1916 Race St.,Philadelphia,Pa.49103 Reprinted from the Annual Book of ASTM Standards,Copyright ASTM If not listed in the current combined index.will appear in the next edition Standard Test Method for SPECTROMETRY LOW LEVELS OF LEAD IN GASOLINE BY X-RAY This standard is issued under the fixed designation D 3229;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.of total lead in gasoline in the range from 0.010 to 0.50 g Pb/U.S.gai.1.2 This standard may involve hazardous ma-terials,operations,and equipment.This standard does not purport to address all o f the safety prob-lems associated with its use.It is the responsibil-ity o f whoever uses this standard to consult and establish appropriate safetv and health practices and determine the applicability of regulatory limi-tations prior to use.For specific precautionary statements,see 6.3,6.4,6.5,and 6.7.2.Applicable Documents 2.1 ASTM Standards:D2599 Test Method for Lead in Gasoline by D3341 Test Method for Lead in Gasoline-,1 ,)C l x-by Spectromet$Iodine Monochloride Method3 3.Summary of Method 3.I Twenty millilitres of sample is mixed thor-oughly with 2 mL of bismuth internal standard solution.The mixture is placed in the X-ray beam of a spectrometer and the intensities of the lead La,radiation at 1.175 A,the bismuth Lal radiationat 1.144&andabackgroundat 1.194 A are determined.A blank,made w i t h Isooctane and bismuth internal standard,i s run ushg the same procedure.The lead concentration i s mea-sured by determining the ratio of the net counting rate at I.i75 A to the gross counting rate at i.144 A for the sample,subtracting the comparable ratio found for the blank,and comparing to a previously prepared calibration curve of concen-tration versus the same ratios.4.Significance and Use 4.1 This test method is used to ensure com-2003 5.Apparatus 5.I X-ray Spectrometer,capable of measuring radiations mentioned in 3.1 and of being Oper-ated under the following instrumental conditions or others giving equivalent results:Tube voltage-50 kV Tube current45 mA Analyzing crystal-lithium fluoride(LiF)Optical path-air,helium.or hydrogen Detector-proportional or scintillation NOTE 1:Caution-The X-ray spectrometer and manner of use should comply with the regulations covering the use of ionizing radiation or recommenda-tions of the International Commission on Radiological Protection,or both.Where hydrogen is used in the optical path,there is a potential explosion hazard.6.Reagents and Materials 6.1 Bismuth 2-Ethylhexoat8 6.2 Bismuth 2-Ethylhexoate internal Stand-ard Solution-Dilute the bismuth 2-ethylhexoate with heavy,odorless solvent or similar material to obtain a solution containing 3.00 g Bi/U.S.gal at 60F(I 5.6C).NOTE 2-Some stability difficulties have been ex-perienced with the bismuth internal standard solution.If the standard is blended to contain 5 56 2ethylhex-anoic acid the standard has been kund to iast dmos indefinitely.The 2ethylhexanoic acid stabilizes isooc-8 This tat method is under the juridiction of ASTM Com-mittee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee W2.03 on Elemental Analyses.Current edition approved Nov.28,1983.Published January 1984.Originally published as D 3229-73.Last prevous edition D 3229-73(1978).Annual Book of ASTM Standards,Vol 05.02.Annual Book oJASTM Srandards,Vol 05.03.Available from Angstrom,Inc.,P.O.Box 252,Belleville,MI48111.PROSLEM HARD COPY 1 0-8 NOTICE:This standard has either been superseded and replaced by a new version or discontinued.Contact ASTM International(www.astm.org)for the latest information.9009276 0027878 166 lane.toluene.and benzene solutions of the bismuth 2-ethylhexoate which arc otherwise stable for only a day or two.Nonna!octanoic acid does not stabilize this solution.6.3 Isooctane,lead free.(Danger-Extremely Flammable.Vapors harmful if inhaled.Vapor may cause flash fire.See Annex A 1.I.)6.4 Solvent,essentially paraffinic stock boiling from 380 to 460F(193 to 238C).(CautionCombustible.Vapor harmful.See Annex A 1.2.)6.5 Tetraethyllead(TEL)Solution,Standard(Note 3),in isooctane,toluene,(WarningAammable.Vapor harmful.See Annex Al.3.)or a mixture of these two solvents(Danger-Poison.Flammable.See Annex A 1.4.),containing approximately the following as determined in accordance with Test Method D 2599 or Test Method D 3341.5 g Pb/U.S.gal at 60F(15.6C)Keep the standard refrigerated when not in use.NOTE 3-A lead naphthenate solution of the same lead concentration has also proven satisfactory as a calibration standard.6.6 Tetraethyllead Solution,Standard(0.500g Pb/gal)-Dilute an aliquot of the standard prepar