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TM_D_2599_
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.ASTM D2579?111 0757510 00262Y1 9:-AMERICAN SOCIETY FORTESTING AND MATERIALS 1916 Race St.,Philadelphia,Pa.19103 Reprinted from the Annual Book o f ASTM Standards,Copyright ASTM If not listed in the current combined index,will appear in the next edition.Designation:D 2599-87 Designation:228/79 Standard Test Method for Lead In Gasoline by X-Ray Spectrometry This standard is issued under the fixed designation D 2599;the number immediately following the designation indicates the year of or&al adoption or,i n the case of revision,the year of last revision.A number in parentheses indicates the year of l a s t reapproval.A superscript epsilon(e)indicates an editorial change since the last revision or reapproval.This is also a standard of the Institute of Petroleum issued under the fKed designation IP 228/72.The final number indicates the year of last revision.These methods were issued as a joint ASTM-IP tentative in 1968.1.Scope 3.1.2 Test Method B(Scattered Tungsten Radiation 1.1 These test methods cover the determination of the Method)-The ratio Of the net x-ray intensity Of the lead total lead content of a gasoline within the following concen-radiation to the net intensity of the incoherently tration ranges:scattered tungsten Gal radiation is obtained on a portion of the sample.The lead content is determined by multiplying this ratio by a calibration factor obtained with a standard lead solution of tetraethyllead in isooctane.0.10 to 5.00 g Pb/US gal 0.12 to 6.00 g Pb/UK gal 0.026 to 1.32 g Pb/L These test methods compensate for normal variation in gasoline composition and are independent of lead alkyl type.1.2 This standard may involve hazardous materials,oper-ations,and equipment.This standard does not purport to address all of the safety problems associated with its use.It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability-ofregulatory limitations prior to use.For specific hazard statements,see 5.I,6.3,6.5,10.1,11.1,and 12.2.1.3 The values stated in g Pb/US gal are the preferred units in the United States.Note that in other countries,other units may be preferred.2.Referenced Documents 2.1 ASTM Standards:D3341 Test Method for Lead in Gasoline-Iodine Monochloride Method 3.Summary of Test Methods 3.1 There are two alternative methods,as follows.3.1.1 Test Method A(Bismuth Internal Standard Method)-One volume of sample is mixed thoroughly with an equal volume of bismuth internal standard solution.The mixture is placed in the X-ray beam and the intensities of the lead Gal radiation at 1.175 A and the bismuth L w I radiation at 1.144 A are determined.The lead concentration of the sample is measured by comparing the ratio of gross counting rate at 1,175 A with the gross countiag rate at 1.144 A to a previous prepared calibration curve of concentration versus the same ratios.*This test method is under the jurisdiction of Committee D.2 on Petroleum and Petroleum Products and is the direct responsibility of Subcommittee W2.03 on Elemental Analysis.Current edition approved Oct.30,1987.Published December 1987.OriginaUy published as D 2599-67 T.Last previous edition D 2599-81.Annual Book o f ASTM Standards,Vol 05.02.4.Significance and Use 4.1 These methods determine the concentration of lead(from alkyl addition)in gasoline.These alkyl additives improve the antiknock properties.TEST METHOD A(BISMUTH INTERNAL STANDARD)5.Apparatus 5.1 X-ray Spectrometer,capable of measunng radiations mentioned in 3.1.1 and of being operated under the fol-lowing instrumental conditions or other giving equivalent results:T u b e voltage 50 kV T u b e current Analyzing crystal lithium fluoride(LiF)Optical path air,helium Detector proportional or scintiiiation 20 to 45 mA 5.1.1 Caution-The X-ray spectrometer and manner of use should comply with the regulations governing the use of ionizing radiation or recommendations of the International Commission of Radiological Protection,or both.6.Reagents and Materiais 6.1 Bismuth 2-Ethylhexoate.6.2 Bismuth 2-Ethylhexoate Internal Standard Solution-Dilute the bismuth 2-ethylhexoate with heavy,odorless solvent or similar material to obtain a solution containing the following:3.00 g Bi/US gai at 15.5C(60F)3.60 g Bi/UK gai at 155C(60F)0.793 g Bi/L at 15C 6.3 Isooctane NOTE 1:Vaming-Extremely flammable.6.4 Solven-A heavy,odorless solvent of an essentially paraEnic stock boiling from 380 to 460F(193 to 238C).6.5 Tetraethyllead(TEL)(Warning-see Note 2),Stan-dard Solution(Note 3),in isooctane,toluene,or a mixture of 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.ASTM D2577 87 ei 07575LO 0026242 O m-/d m D2599 these two solvents containing approximately the foilowing as determined in accordance with Test Method D 3341:NOTE 2:Warning-Toxic by ingestion.5 g Pb/S gal at 15.5C(600 6 g PbWK gal at 15.5C(60F)1.3 g Pb/L at