ASTM D4046-11
(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
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 the 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 − 11
StandardTest 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* Cetane Number. The test method is applicable as a basis for
judging compliance with specifications covering any alkyl
1.1 This test method covers a procedure for the determina-
nitrate.
tion 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
5. Interferences
any alkyl nitrate in diesel fuel provided that standards used for
5.1 Other nitrate esters, inorganic nitrate ions, and nitrogen
calibration contain the same alkyl nitrate ester as the test
oxides will interfere.
specimens to be analyzed.
1.3 The values stated in SI units are to be regarded as
6. Apparatus
standard. No other units of measurement are included in this
6.1 Absorption Cells, matched, having a 1.000 6 0.002-cm
standard.
path length.
1.4 This standard does not purport to address all of the
6.2 Separatory Funnel, Squibb-type glass stoppered with
safety concerns, if any, associated with its use. It is the
TFE-fluorocarbon stopcock, 125-mL capacity.
responsibility of the user of this standard to establish appro-
6.3 Shaking Machine, automatic, capable of multiple
priate safety and health practices and determine the applica-
samples and 250 oscillations/min.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 7.
6.4 Spectrophotometer, capable of measuring absorption in
the region of 452 6 5 nm.
2. Referenced Documents
6.5 Volumetric Flask, 10- and 100-mL capacity.
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water 6.6 Measuring Pipet, 1-mL, 3-mL, 4-mL, and 10-mL.
6.7 Buret, 10-mL capacity.
3. Summary of Test Method
3.1 The determination is based on the simultaneous hydro-
7. Reagents
lysis of the ester in 65 % sulfuric acid solution and nitration of
7.1 Purity of Reagents—Reagent grade chemicals shall be
m-xylenol by the nitric acid liberated. The nitroxylenol is
used in all tests. Unless otherwise indicated, it is intended that
extracted from the reaction mixture and reacted with sodium
all reagents conform to the specifications of the committee on
hydroxide to form the yellow salt. The color is measured
Analytical Reagents of theAmerican Chemical Society, where
spectrophotometrically at 452 nm, and the concentration of
3
such specifications are available. Other grades may be used,
alkyl nitrate is determined by reference to the slope of the
provided it is first ascertained that the reagent is of sufficiently
calibration curve.
high purity to permit its use without lessening the accuracy of
4. Significance and Use the determination.
4.1 Thistestmethodcanbeusedtodeterminetheamountof 7.2 Purity of Water—Unless otherwise indicated, references
alkyl nitrate that has been added to diesel fuel to improve to water shall be understood to mean reagent water conforming
to Type II of Specification D1193.
1
This test method is under the jurisdiction of ASTM Committee D02 on
7.3 Acetic Acid, reagent grade.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved
3
in 1981. Last previous edition approved in 2005 as D4046–91(2005). DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D4046-11. 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
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D4046 − 11
NOTE 2—If no color forms, check the pH. When the solution is not
7.4 Alkyl Nitrate.
alkaline, add an additional 10.0 mL of NaOH solution and correct
7.5 Alkyl Nitrate, Standard Solution—Pipet 3.0 mL of the
calculations for the increased solution volume.
alkyl nitrate to be determined into a 1
...
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:D4046–91(Reapproved 2005) Designation:D4046–11
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.
1.3The values stated in SI units are to be regarded as the standard.
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 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.
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
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
´1
Current edition approved May 1, 2005. Published May 2005. Originally approved in 1981. Last previous edition approved in 2000 as D4046–91(2000) . DOI:
10.1520/D4046-91R05.
Current edition approved June 1, 2011. Published July 2011. Originally approved in 1981. Last previous edition approved in 2005 as D4046–91(2005). DOI:
10.1520/D4046-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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 ----------------------
D4046–11
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 D1193.
7.3 Acetic Acid, reagent grade.
7.4 Alkyl Nitrate.
7.5 Alkyl Nitrate, Standard Solution—Pipet 3.0 mL of the alkyl nitrate to be determined into a
...
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