Standard Test Methods for Lead in Gasoline by X-Ray Spectroscopy

SIGNIFICANCE AND USE
These test methods determine the concentration of lead (from alkyl addition) in gasoline. These alkyl additives improve the antiknock properties.
Test Method C is used to ensure compliance of trace lead as required by federal regulations for lead-free gasoline (40 CFR part 80).
SCOPE
1.1 These test methods cover the determination of the total lead content of a gasoline within the following concentration ranges: 0.010 to 5.0 g Pb/US gal 0.012 to 6.0 g Pb/UK gal 0.0026 to 1.32 g Pb/L
1.1.1 Test Methods A and B cover the range of 0.10 to 5.0 g Pb/US gal. Test Method C covers the range of 0.010 to 0.50 g Pb/US gal.
1.1.2 These test methods compensate for normal variation in gasoline composition and are independent of lead alkyl type.
1.2 Test Method A (formerly in withdrawn Test Method D 2599)—Sections 5-9.
Test Method B (formerly in withdrawn Test Method D 2599)—Sections 10-14.
Test Method C (formerly in withdrawn Test Method D 3229)—Sections 15-19.
1.3 The values stated in SI are to be regarded as the standard. For reporting purposes the values stated in grams per U.S. gallon are the preferred units in the United States. Note that in other countries, other units can be preferred.
1.4 This standard does not purport to address all of the safety concerns, if any, 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 of regulatory limitations prior to use. For specific hazard statements, see Sections 5, 6, 11, and 18.

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Publication Date
30-Nov-2007
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5059 − 07
StandardTest Methods for
1
Lead in Gasoline by X-Ray Spectroscopy
This standard is issued under the fixed designation D5059; 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 (´) 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* 2. Referenced Documents
2
1.1 These test methods cover the determination of the total 2.1 ASTM Standards:
D3341 Test Method for Lead in Gasoline—Iodine Mono-
lead content of a gasoline within the following concentration
ranges: chloride Method
D4057 Practice for Manual Sampling of Petroleum and
0.010 to 5.0 g Pb/US gal
0.012 to 6.0 g Pb/UK gal
Petroleum Products
0.0026 to 1.32 g Pb/L
D6299 Practice for Applying Statistical Quality Assurance
1.1.1 Test Methods A and B cover the range of 0.10 to 5.0
and Control Charting Techniques to Evaluate Analytical
g Pb/US gal. Test Method C covers the range of 0.010 to 0.50
Measurement System Performance
g Pb/US gal.
D6792 Practice for Quality System in Petroleum Products
1.1.2 These test methods compensate for normal variation
and Lubricants Testing Laboratories
ingasolinecompositionandareindependentofleadalkyltype.
3. Summary of Test Method
1.2 Test Method A (formerly in withdrawn Test Method
3.1 There are three alternative test methods, as follows.
D2599)—Sections 5-9.
3.1.1 Test Method A (Bismuth Internal Standard Method
Test Method B (formerly in withdrawn Test Method
High Concentration)—One volume of sample is mixed thor-
D2599)—Sections 10-14.
oughly with an equal volume of bismuth internal standard
Test Method C (formerly in withdrawn Test Method
solution. The mixture is placed in the X-ray beam and the
D3229)—Sections 15-19.
intensitiesofthelead L-α radiationat1.175 Åandthebismuth
1
1.3 The values stated in SI are to be regarded as the
L-α radiation at 1.144 Å are determined. The lead concentra-
1
standard. For reporting purposes the values stated in grams per
tion of the sample is measured by comparing the ratio of gross
U.S. gallon are the preferred units in the United States. Note
counting rate at 1.175 Å with the gross counting rate at 1.144
that in other countries, other units can be preferred.
Å to a previous prepared calibration curve of concentration
versus the same ratios.
1.4 This standard does not purport to address all of the
3.1.2 Test Method B (Scattered Tungsten Radiation
safety concerns, if any, associated with its use. It is the
Method)—The ratio of the net X-ray intensity of the lead L-α
responsibility of the user of this standard to establish appro-
1
radiation to the net intensity of the incoherently scattered
priate safety and health practices and determine the applica-
tungsten L-α radiation is obtained on a portion of the sample.
bility of regulatory limitations prior to use. For specific hazard
1
The lead content is determined by multiplying this ratio by a
statements, see Sections 5, 6, 11, and 18.
calibration factor obtained with a standard lead solution of
known concentration.
1
3.1.3 Test Method C (Bismuth Internal Standard Method,
These test methods are under the jurisdiction of Committee D02 on Petroleum
Products and Lubricants and are the direct responsibility of Subcommittee D02.03
Low Concentration)—Twenty millilitres of sample is mixed
on Elemental Analysis.
thoroughly with two milliliters of bismuth internal standard
Current edition approved Dec. 1, 2007. Published January 2008. Originally
ε1
approved in 1990. Last previous edition approved in 2003 as D5059–98(2003) .
2
Initially published as D2599 – 67T and D3229 – 73, now withdrawn. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
These test methods have been approved by the sponsoring committees and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
accepted by the cooperating organizations in accordance with established proce-
Standards volume information, refer to the standard’s Document Summary page on
dures. DOI: 10.1520/D5059-07.
the ASTM website.
*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 States
1

---------------------- Page: 1 ----------------------
D5059 − 07
solution. The mixture is placed in the X-ray beam of a 6.3 Bismuth Internal Standard Solution —Dilute the
spectrometer and the intensities of the lead L-α radiation at hydrocarbon-soluble bismuth with a suitable solvent. If bis-
1
1.175 Å, the bismuth L-α radiation at 1.144 Å, and a back- muth 2-ethylhexoate is used, add 2-ethylhexanoic aci
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
e1
Designation:D5059–98 (Reapproved 2003) Designation:D5059–07
Designation: 228/79
Standard Test Methods for
1
Lead in Gasoline by X-Ray Spectroscopy
This standard is issued under the fixed designation D 5059; 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.
This standard has been approved for use by agencies of the Department of Defense.
1
e NOTE—Warning notes were editorially moved into the standard text in August 2003.
1. Scope*
1.1 Thesetestmethodscoverthedeterminationofthetotalleadcontentofagasolinewithinthefollowingconcentrationranges:
0.010 to 5.0 g Pb/US gal
0.012 to 6.0 g Pb/UK gal
0.0026 to 1.32 g Pb/L
1.1.1 TestMethodsAandBcovertherangeof0.10to5.0gPb/USgal.TestMethodCcoverstherangeof0.010to0.50gPb/US
gal.
1.1.2 These test methods compensate for normal variation in gasoline composition and are independent of lead alkyl type.
1.2 Test Method A (formerly in Test Method D2599)—Sections (formerly in withdrawn Test Method D 2599)—Sections 5-9.
Test Method B (formerly in Test Method D2599)—Sections (formerly in withdrawn Test Method D 2599)—Sections 10-14.
Test Method C (formerly in Test Method D3229)—Sections (formerly in withdrawn Test Method D 3229)—Sections 15-19.
1.3 The values stated in SI are to be regarded as the standard. For reporting purposes the values stated in grams per U.S. gallon
are the preferred units in the United States. Note that in other countries, other units can be preferred.
1.4 This standard does not purport to address all of the safety concerns, if any, 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 of regulatory
limitations prior to use. For specific hazard statements, see Sections 5, 6, 11, and 18.
2. Referenced Documents
2
2.1 ASTM Standards: D2599Test Method for Lead in Gasoline by X-Ray Spectrometry D3229Test Method for Low Levels of
Lead in Gasoline by Wavelength
Dispersive X-Ray Spectrometry
D 3341 Test Method for Lead in Gasoline-Iodine Monochloride Method
4
D 4057Practice for Manual Sampling of Petroleum and Petroleum Products Practice for Manual Sampling of Petroleum and
Petroleum Products
D 6299 Practice for Applying Statistical Quality Assurance Techniques to Evaluate Analytical Measurement System
Performance
D 6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
3. Summary of Test Method
3.1 There are three alternative test methods, as follows.
1
These test methods are under the jurisdiction of Committee D02 on Petroleum Products and Lubricants and are the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved May 10, 2003. Published August 2003. (Originally published as D2599 – 67T and D3229 – 73.) Originally approved in 1990. Last previous
edition approved in 1998 as D5059– 98.
e1
Current edition approved Dec. 1, 2007. Published January 2008. Originally approved in 1990. Last previous edition approved in 2003 as D 5059–98(2003) .
Initially published as D 2599 – 67T and D 3229 – 73, now withdrawn.
These test methods have been approved by the sponsoring committees and accepted by the cooperating organizations in accordance with established procedures.
2
Discontinued. See 1991
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 05.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
*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 States.
1

---------------------- Page: 1 ----------------------
D5059–07
3.1.1 Test Method A (Bismuth Internal Standard Method High Concentration)—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
L-a radiation at 1.175 Å and the bismuth L-a radiation at 1.144 Å are determined. The lead concentration of the sample is
1 1
measured by comparing the ratio of gross counting rate at 1.175 Å with the gross counting rate at 1.144 Å to a previous prepared
c
...

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