ASTM D4046-91(2000)e1

Standard Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry

SCOPE
1.1 This test method describes 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 preferred units are acceptable SI units.  
1.4 This standard does not purport to address all of the safety problems, 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 Note 1.

General Information

• Status: Historical
• Publication Date: 09-Apr-2000
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaced By: ASTM D4046-91(2005) - Standard Test Method for Alkyl Nitrate in Diesel Fuels by Spectrophotometry
• Effective Date: 01-May-2005
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 10-Apr-2000
• Referred By: ASTM D189-06(2019) - Standard Test Method for Conradson Carbon Residue of Petroleum Products
• Effective Date: 10-Apr-2000
• Referred By: ASTM D524-15(2019) - Standard Test Method for Ramsbottom Carbon Residue of Petroleum Products
• Effective Date: 10-Apr-2000
• Referred By: ASTM D4530-15(2020) - Standard Test Method for Determination of Carbon Residue (Micro Method)
• Effective Date: 10-Apr-2000

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
e1
Designation:D4046–91(Reapproved 2000)
Standard Test Method for
Alkyl Nitrate in Diesel Fuels by Spectrophotometry
This standard is issued under the fixed designation D 4046; 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.
e NOTE—Warning notes were placed in the text in April 2000.
1. Scope 5. Interferences
1.1 This test method describes a procedure for the determi- 5.1 Other nitrate esters, inorganic nitrate ions, and nitrogen
nation of 0.03 to 0.30 volume % of alkyl nitrate in diesel fuels. oxides will interfere.
1.2 This test method can be used for the determination of
6. Apparatus
any alkyl nitrate in diesel fuel provided that standards used for
calibration contain the same alkyl nitrate ester as the test 6.1 Absorption Cells, matched, having a 1.000 6 0.002-cm
path length.
specimens to be analyzed.
1.3 The preferred units are acceptable SI units. 6.2 Separatory Funnel, Squibb-type glass stoppered with
TFE-fluorocarbon stopcock, 125-mL capacity.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 6.3 Shaking Machine, automatic, capable of multiple
samples and 250 oscillations/min.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 6.4 Spectrophotometer, capable of measuring absorption in
the region of 452 6 5 nm.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 7. 6.5 Volumetric Flask, 10- and 100-mL capacity.
6.6 Measuring Pipet, 1-mL, 3-mL, 4-mL, and 10-mL.
2. Referenced Documents
6.7 Buret, 10-mL capacity.
2.1 ASTM Standards:
2 7. Reagents
D 1193 Specification for Reagent Water
7.1 Purity of Reagents—Reagent grade chemicals shall be
3. Summary of Test Method
used in all tests. Unless otherwise indicated, it is intended that
3.1 The determination is based on the simultaneous hy- all reagents conform to the specifications of the committee on
drolysis of the ester in 65 % sulfuric acid solution and nitration Analytical Reagents of theAmerican Chemical Society, where
of m-xylenol by the nitric acid liberated. The nitroxylenol is such specifications are available. Other grades may be used,
extracted from the reaction mixture and reacted with sodium provided it is first ascertained that the reagent is of sufficiently
hydroxide to form the yellow salt. The color is measured high purity to permit its use without lessening the accuracy of
spectrophotometrically at 452 nm, and the concentration of the determination.
alkyl nitrate is determined by reference to the slope of the 7.2 Purity of Water—Unless otherwise indicated, references
calibration curve. to water shall be understood to mean reagent water conforming
to Type II of Specification D 1193.
4. Significance and Use
7.3 Acetic Acid, reagent grade.
4.1 Thistestmethodcanbeusedtodeterminetheamountof 7.4 Alkyl Nitrate.
alkyl nitrate that has been added to diesel fuel to improve
7.5 Alkyl Nitrate, Standard Solution—Pipet 3.0 mL of the
Cetane Number. The test method is applicable as a basis for alkyl nitrate to be determined into a 100-mL volumetric flask
judging compliance with specifications covering any alkyl
and dilute to volume with diesel fuel.
nitrate.
1 3
This test method is under the jurisdiction of ASTM Committee D02 on Reagent Chemicals, American Chemical Society Specifications, American
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Chemical Society, Washington, DC. For suggestions on the testing of reagents not
D02.03 on Elemental Analysis. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved March 15, 1991. Published July 1991. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 4046 – 81. Last previous edition D 4046 – 87. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D4046–91 (2000)
7.6 Diesel Fuel, additive-free (Warning—Flammable.).
where:
7.7 Isooctane (2,2,4-trimethylpentane). (Warning—
A = sum of the volume percent alkyl nitrate standards and
Flammable.).
B = sum of corrected absorbances.
7.8 Isopropyl Alcohol, reagent grade. (Warning—
9. Procedure
Flammable.).
7.9 m-Xylenol Solutions—Dilute 4 mL of m-xylenol (2,4-
9.1 Pipet 1.0 mL of test specimen into a 10-mL volumetric
dimethylphenol) to 100 mL in acetic acid.
flask and dilute to volume with isopropyl alcohol.
7.10 Sodium Hydroxide Solution—Dissolve 50 g of sodium
9.2 Pipet1.0mLofthesampletestspecimenpreparedin9.1
hydroxide (NaOH) pellets in 1000 mL of distilled water.
into a 125-mLseparatory funnel.To another funnel add 1.0 mL
7.11 Sulfuric Acid—Add slowly with stirring, 500 mL of
of blank isopropyl alcohol.
nitrate-free sulfuric acid (H SO ) (rel dens
...