ASTM D3831-01(2006)
(Test Method)Standard Test Method for Manganese in Gasoline By Atomic Absorption Spectroscopy
Standard Test Method for Manganese in Gasoline By Atomic Absorption Spectroscopy
SIGNIFICANCE AND USE
Certain organo-manganese compounds act as antiknock agents when added to gasoline. This test method provides a means for determining the concentration of such a material in a gasoline sample.
SCOPE
1.1 This test method covers the determination of the total manganese content, present as methylcyclopentadienyl manganese tricarbonyl (MMT), of gasoline within the concentration range from 0.25 to 40 mg/L of manganese.
1.2 This test method is applicable to reformulated gasoline containing up to 12 % volume methyl tertiary butylether or up to 10 % volume ethanol. This test method may not be applicable to highly cracked materials containing greater than 18 volume % olefins as determined by Test Method D 1319 (nondepentanized).
1.3 This test method has been developed and tested specifically for the determination of MMT in gasoline over the recommended concentration range. Application of the method to other concentration ranges, to the determination of MMT in other materials, or to the determination of other manganese compounds in gasoline have not been tested
1.4 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mg/L manganese.
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 warning statements, see Sections 5 and 6.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3831 − 01(Reapproved 2006)
Standard Test Method for
Manganese in Gasoline By Atomic Absorption
Spectroscopy
This standard is issued under the fixed designation D3831; 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.
1. Scope* D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of the total
D4177 Practice for Automatic Sampling of Petroleum and
manganese content, present as methylcyclopentadienyl manga-
2 Petroleum Products
nese tricarbonyl (MMT), of gasoline within the concentration
D6299 Practice for Applying Statistical Quality Assurance
range from 0.25 to 40 mg/L of manganese.
and Control Charting Techniques to Evaluate Analytical
1.2 This test method is applicable to reformulated gasoline
Measurement System Performance
containing up to 12 % volume methyl tertiary butylether or up
D6300 Practice for Determination of Precision and Bias
to 10 % volume ethanol. This test method may not be appli-
Data for Use in Test Methods for Petroleum Products and
cable to highly cracked materials containing greater than 18
Lubricants
volume % olefins as determined by Test Method D1319
(nondepentanized).
3. Summary of Test Method
1.3 This test method has been developed and tested specifi-
3.1 The gasoline sample is treated with bromine solution
cally for the determination of MMT in gasoline over the
and diluted with methyl isobutyl ketone. The manganese
recommended concentration range. Application of the method
content of the sample is determined by atomic absorption
to other concentration ranges, to the determination of MMT in
spectrometry using an air-acetylene flame at 279.5 nm and
other materials, or to the determination of other manganese
standards prepared from an organo-manganese standard mate-
compounds in gasoline have not been tested
rial.
1.4 The values stated in SI units are to be regarded as the
4. Significance and Use
standard. The preferred concentration units are mg/L manga-
nese. 4.1 Certain organo-manganese compounds act as antiknock
agents when added to gasoline. This test method provides a
1.5 This standard does not purport to address all of the
means for determining the concentration of such a material in
safety concerns, if any, associated with its use. It is the
a gasoline sample.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use. For specific
warning statements, see Sections 5 and 6. 5.1 Atomic Absorption Spectrometer , capable of scale
expansion and equipped with a manganese hollow-cathode
2. Referenced Documents
lamp for monitoring manganese absorption at 279.5 nm, a
premix slot-type burner with rotatable burner head, and an
2.1 ASTM Standards:
D1319 Test Method for Hydrocarbon Types in Liquid Petro- adjustable nebulizer. (Warning—Hazardous. Potentially toxic
and explosive. Refer to the manufacturer’s instrument manual
leum Products by Fluorescent Indicator Adsorption
for associated safety hazards.)
5.2 Vials, up to 40-mL size with polyethylene or TFE-
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
fluorocarbon-lined caps or glass stoppers.
D02.03 on Elemental Analysis.
5.3 Pipet, Delivery, 1-mL size.
Current edition approved May 1, 2006. Published June 2006. Originally
approved in 1979. Last previous edition approved in 2001 as D3831 – 01. DOI:
5.4 Micropipet, 100-µL size, Eppendorf type or equivalent.
10.1520/D3831-01R06.
MMT is a registered trademark of Ethyl Corp.
5.5 Automatic Pipet,orequivalentdeliverypipet,capableof
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
delivering 9.0-mL quantities.
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. 6. Reagents
*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
D3831 − 01 (2006)
6.1 Purity of Reagents—Reagent grade chemicals shall be 8.2 Preparation of Instrument—Set the atomic absorption
used in all tests. Unless otherwise indicated, it is intended that spectrometer operating conditions to those recommended by
all reagents shall conform to the specifications of the Commit- the manufacturer for monitoring manganese absorption at
tee onAnalytical Reagents of theAmerican Chemical Society, 279.5 nm using an air-acetylene flame. This test method
where such specifications are available. Other grades may be assumes that good operating procedures are followed. Design
used, provided it is first ascertained that the reagent is of differences between spectrometers make it impractical to
sufficiently high purity to permit its use without lessening the exactly specify required instrument settings.
accuracy of the determination. 8.2.1 Nebulizemethylisobutylketoneintotheflame.Adjust
thenebulizer(sampleflowrate),acetylene,andairflowratesto
6.2 Bromine Solution— Add reagent grade bromine to an
give a lean, nonluminous flame.
equal volume of cyclohexane. (Warning—Bromine can cause
8.2.2 With methyl isobutyl ketone as a blank, nebulize, in
severe and painful burns when it contacts the skin. In addition
turn, the four working standards.
to other precautions, wear protective gloves in preparing the
solution and prepare, store, and use it in a well-ventilated
NOTE 1—Record the absorbances and check these data for linearity. If
nonlinear, readjust the sample or acetylene flow rates, or both, slightly to
hood.)
leaner conditions and repeat the calibrations until absorbances are linear.
6.3 Manganese Standard Solution 400 mg Mn/L—Dissolve
Rotation of the burner head to decrease the absorbance may aid in
the appropriate amount of organometallic manganese standard
achieving linearity.
NOTE 2—Three working standards may be used to cover the expected
inmethylisobutylketonetogiveastandardsolutionof400mg
concentration range of the samples. Fuel specification limits should be
Mn/L.
considered. For example, the use of the high 40 mg/Lstandard may not be
6.4 Manganese, Standard Solution 4.0, 10.0, 20.0, and 40.0 necessary.
mg Mn/L—Dilute the 400 mg/L standard manganese solution
9. Procedure
withmethylisobutylketoneusingvolumetricglasswaretogive
9.1 Deliver 100 µL of bromine solution into a vial.
the desired lower concentration manganese standard solutions.
9.2 Add 1.0 mL of the gasoline sample. Mix well.
6.5 Organometallic Manganese Standard —Pre-prepared
commercially available organometallic stock solutions have
9.3 Add 9.0 mL of methyl isobutyl ketone. Mix well.
been found to be satisfactory.
9.4 Aspirate the working standards and the sample into the
6.6 Methyl Isobutyl Ketone, reagent grade. (Warning—
flame and record the absorbances of each.
Flammable. Vapor harmful.) (Warning— Solutions of MMT
NOTE 3—Measure absorbances of the working standards and the
ingasolinearechemicallyunstablewhenexposedtolight.Low
samples promptly as the sample absorbances may change with time.
and erratic results may be obtained if the gasoline sample is
exposed to light prior to stabilization during analysis.)
10. Calculations
6.7 Quality Control (QC) Sample(s) , 10.1 The direct concentration read out of the instrument is
prefera
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