ASTM D4046-14
(Test Method)Standard Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry
Standard Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry
SIGNIFICANCE AND USE
4.1 In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate causes a higher residue value than observed in untreated fuel, which can lead to erroneous conclusions as to the coke forming propensity of the fuel. The presence of such alkyl nitrate in the fuel can be determined using this test method. This test method can be used to determine the amount of alkyl nitrate that has been added to diesel fuel to improve Cetane Number. The test method is applicable as a basis for judging compliance with specifications covering any alkyl nitrate.
SCOPE
1.1 This test method covers a procedure for the determination of 0.03 to 0.30 volume % of alkyl nitrate in diesel fuels.
1.2 This test method can be used for the determination of any alkyl nitrate in diesel fuel provided that standards used for calibration contain the same alkyl nitrate ester as the test specimens to be analyzed.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 Section 7.
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Designation: D4046 − 14
Standard Test Method for
1
Alkyl Nitrate in Diesel Fuels by Spectrophotometry
This standard is issued under the fixed designation D4046; 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* value than observed in untreated fuel, which can lead to
erroneous conclusions as to the coke forming propensity of the
1.1 This test method covers a procedure for the determina-
fuel. The presence of such alkyl nitrate in the fuel can be
tion of 0.03 to 0.30 volume % of alkyl nitrate in diesel fuels.
determined using this test method. This test method can be
1.2 This test method can be used for the determination of
used to determine the amount of alkyl nitrate that has been
any alkyl nitrate in diesel fuel provided that standards used for
added to diesel fuel to improve Cetane Number. The test
calibration contain the same alkyl nitrate ester as the test
method is applicable as a basis for judging compliance with
specimens to be analyzed.
specifications covering any alkyl nitrate.
1.3 The values stated in SI units are to be regarded as
5. Interferences
standard. No other units of measurement are included in this
standard.
5.1 Other nitrate esters, inorganic nitrate ions, and nitrogen
oxides will interfere.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Apparatus
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6.1 Absorption Cells, matched, having a 1.000 6 0.002-cm
bility of regulatory limitations prior to use. For specific hazard path length.
statements, see Section 7.
6.2 Separatory Funnel, Squibb-type glass stoppered with
TFE-fluorocarbon stopcock, 125-mL capacity.
2. Referenced Documents
2
6.3 Shaking Machine, automatic, capable of multiple
2.1 ASTM Standards:
samples and 250 oscillations/min.
D1193 Specification for Reagent Water
6.4 Spectrophotometer, capable of measuring absorption in
3. Summary of Test Method
the region of 452 6 5 nm.
3.1 The determination is based on the simultaneous hydro-
6.5 Volumetric Flask, 10- and 100-mL capacity.
lysis of the ester in 65 % sulfuric acid solution and nitration of
6.6 Measuring Pipet, 1-mL, 3-mL, 4-mL, and 10-mL.
m-xylenol by the nitric acid liberated. The nitroxylenol is
extracted from the reaction mixture and reacted with sodium
6.7 Buret, 10-mL capacity.
hydroxide to form the yellow salt. The color is measured
spectrophotometrically at 452 nm, and the concentration of
7. Reagents
alkyl nitrate is determined by reference to the slope of the
7.1 Purity of Reagents—Reagent grade chemicals shall be
calibration curve.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the committee on
4. Significance and Use
Analytical Reagents of theAmerican Chemical Society, where
4.1 In diesel fuel, the presence of alkyl nitrates such as amyl
3
such specifications are available. Other grades may be used,
nitrate, hexyl nitrate, or octyl nitrate causes a higher residue
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
1
This test method is under the jurisdiction of ASTM Committee D02 on
the determination.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved
3
in 1981. Last previous edition approved in 2011 as D4046 – 11. DOI: 10.1520/ Reagent Chemicals, American Chemical Society Specifications, American
D4046-14. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
*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
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D4046 − 14
7.2 Purity of Water—Unless otherwise indicated, references least 10 min or when phases separate cleanly (see Note 2).
...
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: D4046 − 11 D4046 − 14
Standard Test Method for
1
Alkyl Nitrate in Diesel Fuels by Spectrophotometry
This standard is issued under the fixed designation D4046; 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*
1.1 This test method covers a procedure for the determination of 0.03 to 0.30 volume % of alkyl nitrate in diesel fuels.
1.2 This test method can be used for the determination of any alkyl nitrate in diesel fuel provided that standards used for
calibration contain the same alkyl nitrate ester as the test specimens to be analyzed.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 Section 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3. Summary of Test Method
3.1 The determination is based on the simultaneous hydrolysis of the ester in 65 % sulfuric acid solution and nitration of
m-xylenol by the nitric acid liberated. The nitroxylenol is extracted from the reaction mixture and reacted with sodium hydroxide
to form the yellow salt. The color is measured spectrophotometrically at 452 nm, and the concentration of alkyl nitrate is
determined by reference to the slope of the calibration curve.
4. Significance and Use
4.1 In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate causes a higher residue value
than observed in untreated fuel, which can lead to erroneous conclusions as to the coke forming propensity of the fuel. The
presence of such alkyl nitrate in the fuel can be determined using this test method. This test method can be used to determine the
amount of alkyl nitrate that has been added to diesel fuel to improve Cetane Number. The test method is applicable as a basis for
judging compliance with specifications covering any alkyl nitrate.
5. Interferences
5.1 Other nitrate esters, inorganic nitrate ions, and nitrogen oxides will interfere.
6. Apparatus
6.1 Absorption Cells, matched, having a 1.000 6 0.002-cm path length.
6.2 Separatory Funnel, Squibb-type glass stoppered with TFE-fluorocarbon stopcock, 125-mL capacity.
6.3 Shaking Machine, automatic, capable of multiple samples and 250 oscillations/min.
6.4 Spectrophotometer, capable of measuring absorption in the region of 452 6 5 nm.
6.5 Volumetric Flask, 10- and 100-mL capacity.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 1, 2011June 1, 2014. Published July 2011July 2014. Originally approved in 1981. Last previous edition approved in 20052011 as
D4046–91(2005).D4046 – 11. DOI: 10.1520/D4046-11.10.1520/D4046-14.
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 ----------------------
D4046 − 14
6.6 Measuring Pipet, 1-mL, 3-mL, 4-mL, and 10-mL.
6.7 Buret, 10-mL capacity.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, where such
3
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type II of Specification
...
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