ASTM D5059-13
(Test Method)Standard Test Methods for Lead in Gasoline by X-Ray Spectroscopy
Standard Test Methods for Lead in Gasoline by X-Ray Spectroscopy
SIGNIFICANCE AND USE
4.1 These test methods determine the concentration of lead (from alkyl addition) in gasoline. These alkyl additives improve the antiknock properties.
4.2 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1.2 Test Method A (formerly in withdrawn Test Method D2599)—Sections 5-9.
Test Method B (formerly in withdrawn Test Method D2599)—Sections 10-14.
Test Method C (formerly in withdrawn Test Method D3229)—Sections 15-19.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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Designation: D5059 − 13
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* D3341 Test Method for Lead in Gasoline—Iodine Mono-
chloride Method
1.1 These test methods cover the determination of the total
D4057 Practice for Manual Sampling of Petroleum and
lead content of a gasoline within the following concentration
Petroleum Products
ranges:
D6299 Practice for Applying Statistical Quality Assurance
0.010 to 5.0 g Pb/US gal
and Control Charting Techniques to Evaluate Analytical
0.012 to 6.0 g Pb/UK gal
0.0026 to 1.32 g Pb/L Measurement System Performance
D6792 Practice for Quality System in Petroleum Products
1.1.1 Test Methods A and B cover the range of 0.10 to 5.0
and Lubricants Testing Laboratories
g Pb/US gal. Test Method C covers the range of 0.010 to 0.50
g Pb/US gal.
3. Summary of Test Method
1.1.2 These test methods compensate for normal variation
3.1 There are three alternative test methods, as follows.
ingasolinecompositionandareindependentofleadalkyltype.
3.1.1 Test Method A (Bismuth Internal Standard Method
1.2 Test Method A (formerly in withdrawn Test Method
High Concentration)—One volume of sample is mixed thor-
D2599)—Sections5–9.
oughly with an equal volume of bismuth internal standard
Test Method B (formerly in withdrawn Test Method
solution. The mixture is placed in the X-ray beam and the
D2599)—Sections10–14.
intensitiesofthelead L-α radiationat1.175 Åandthebismuth
1
Test Method C (formerly in withdrawn Test Method
L-α radiation at 1.144 Å are determined. The lead concentra-
1
D3229)—Sections15–19.
tion of the sample is measured by comparing the ratio of gross
1.3 The values stated in SI are to be regarded as the
counting rate at 1.175 Å with the gross counting rate at 1.144
standard. For reporting purposes the values stated in grams per
Å to a previous prepared calibration curve of concentration
U.S. gallon are the preferred units in the United States. Note
versus the same ratios.
that in other countries, other units can be preferred.
3.1.2 Test Method B (Scattered Tungsten Radiation
Method)—The ratio of the net X-ray intensity of the lead L-α
1.4 This standard does not purport to address all of the 1
radiation to the net intensity of the incoherently scattered
safety concerns, if any, associated with its use. It is the
tungsten L-α radiation is obtained on a portion of the sample.
responsibility of the user of this standard to establish appro- 1
The lead content is determined by multiplying this ratio by a
priate safety and health practices and determine the applica-
calibration factor obtained with a standard lead solution of
bility of regulatory limitations prior to use. For specific hazard
known concentration.
statements, see Sections 5, 6, 11, and 18.
3.1.3 Test Method C (Bismuth Internal Standard Method,
2. Referenced Documents
Low Concentration)—Twenty millilitres of sample is mixed
2 thoroughly with two milliliters of bismuth internal standard
2.1 ASTM Standards:
solution. The mixture is placed in the X-ray beam of a
spectrometer and the intensities of the lead L-α radiation at
1
1 1.175 Å, the bismuth L-α radiation at 1.144 Å, and a back-
These test methods are under the jurisdiction of Committee D02 on Petroleum
1
Products and Lubricants and are the direct responsibility of Subcommittee D02.03
ground at 1.194 Å are determined. A blank, made with
on Elemental Analysis.
iso-octane and bismuth internal standard, is run using the same
Current edition approved June 15, 2013. Published August 2013. Originally
procedure. The lead concentration is measured by determining
approved in 1990. Last previous edition approved in 2007 as D5059 – 07. DOI:
the ratio of the net counting rate at 1.175 Å to the gross
10.1520/D5059-13.
Initially published as D2599 – 67T and D3229 – 73, now withdrawn.
counting rate at 1.144 Å for the sample, subtracting the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
comparable ratio found for the blank, and comparing to a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
previously prepared calibration curve of concentration versus
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the same ratios.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
Designation: D5059 − 07 D5059 − 13
Standard Test 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*
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 D2599)—Sections 5-9.
Test Method B (formerly in withdrawn Test Method D2599)—Sections 10-14.
Test Method C (formerly in withdrawn Test Method D3229)—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:
D3341 Test Method for Lead in Gasoline—Iodine Monochloride Method
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6792 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.
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-α
1
radiation at 1.175 Å and the bismuth L-α radiation at 1.144 Å are determined. The lead concentration of the sample is measured
1
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 calibration
curve of concentration versus the same ratios.
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 Dec. 1, 2007June 15, 2013. Published January 2008August 2013. Originally approved in 1990. Last previous edition approved in 20032007 as
ε1
D5059–98(2003)D5059 – 07. . DOI: 10.1520/D5059-13.
Initially published as D2599 – 67T and D3229 – 73, now withdrawn.
These test methods have been approved by the sponsoring committees and accepted by the cooperating organizations in accordance with established procedures. DOI:
10.1520/D5059-07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
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 − 13
3.1.2 Test Method B (Scattered Tungsten Radiation Method)—The ratio of the net X-ray intensity of the lead L-α radiation to
1
the net intensity of the incoherently scattered tungsten L-α radiation is obtained on a portion of the sample. The lead content is
1
determined by multiplying this ratio by a calibration factor obtained with a standard lead solution of known concentration.
3.1.3 Test Method C (Bismuth Internal Standard Method, Low Concentration)—Twenty millilitres of sample is mixed
thoroughly with two milliliters of bismuth
...
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