ASTM D1839-91(2005)

Standard Test Method for Amyl Nitrate in Diesel Fuels

SIGNIFICANCE AND USE
This test method can be used to determine the amount of amyl nitrate that has been added to diesel fuels to improve cetane number. This test method is applicable as a basis for judging compliance with specifications covering amyl nitrate.
SCOPE
1.1 This test method covers the determination of 0.1 to 0.5 volume % amyl nitrate in diesel fuels.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 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.
Note 1—This test method has been used for the determination of hexyl nitrate in diesel fuels, but has not been cooperatively tested for such samples. For the determination of hexyl nitrate, use standards containing nitrate esters of primary hexanol. Use a density of 0.97 in calculating results.

General Information

• Status: Historical
• Publication Date: 30-Apr-2005
• ICS: 71.040.40 - Chemical analysis
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.03 - Elemental Analysis

Relations

• Replaces: ASTM D1839-91(2000)e1 - Standard Test Method for Amyl Nitrate in Diesel Fuels
• Effective Date: 01-May-2005
• Replaced By: ASTM D1839-11 - Standard Test Method for Amyl Nitrate in Diesel Fuels
• Effective Date: 01-Jun-2011
• Referred By: ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
• Effective Date: 01-May-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D1839–91(Reapproved 2005)
Standard Test Method for
Amyl Nitrate in Diesel Fuels
This standard is issued under the fixed designation D1839; 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. This test method is applicable as a basis for
judging compliance with specifications covering amyl nitrate.
1.1 This test method covers the determination of 0.1 to 0.5
volume % amyl nitrate in diesel fuels.
5. Interferences
1.2 The values stated in SI units are to be regarded as the
5.1 Nitrateesters,inorganicnitrateions,andnitrogenoxides
standard.
will interfere to give high results.
1.3 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-
6.1 Absorption Cells, matched, having a 1.000- 6 0.002-cm
priate safety and health practices and determine the applica-
light path.
bility of regulatory limitations prior to use.
6.2 Distillate Collector, borosilicate glass with standard
NOTE 1—This test method has been used for the determination of hexyl
taper joints and sealed-in funnel (Fig. 1).
nitrate in diesel fuels, but has not been cooperatively tested for such
6.3 Electric Heating Mantle, to fit a 300-mL round-bottom
samples. For the determination of hexyl nitrate, use standards containing
flask, and having a variable transformer.
nitrate esters of primary hexanol. Use a density of 0.97 in calculating
6.4 Lunge-type Pipet, 2-mL capacity.
results.
NOTE 2—A 2.5-mL hypodermic syringe, with scabbard, can be used
2. Referenced Documents
instead of the Lunge pipet.
2.1 ASTM Standards:
6.5 Reflux Condenser (Allihn-type), borosilicate glass, 300
D1193 Specification for Reagent Water
mm long, with standard-taper joints.
D4057 Practice for Manual Sampling of Petroleum and
6.6 Round-Bottom Flask, of borosilicate glass and having a
Petroleum Products
300-mL capacity.
6.7 Separatory Funnel, Squibb-type, 125-mL capacity.
3. Summary of Test Method
6.8 Shaking Machine, automatic, capable of 250
3.1 This test method is based on the simultaneous hydroly-
oscillations/min.
sis of the ester in 62.5 % sulfuric acid and nitration of
6.9 Spectrophotometer, capable of measuring absorption in
m-xylenol by the nitric acid liberated. The nitroxylenol is
the region of 452 nm.
distilled from the reaction mixture and reacted with sodium
hydroxide to form the yellow sodium salt. Residual diesel fuel
7. Reagents
is removed by ether extraction. The color is measured spectro-
7.1 Purity of Reagents—Reagent grade chemicals shall be
photometrically at 452 nm, and the concentration of amyl
used in all tests. Unless otherwise indicated, it is intended that
nitrate is determined by reference to a standard curve.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
4. Significance and Use
where such specifications are available. Other grades may be
4.1 Thistestmethodcanbeusedtodeterminetheamountof
used, provided it is first ascertained that the reagent is of
amyl nitrate that has been added to diesel fuels to improve
The sole source of supply of the apparatus known to the committee at this time
This method is under the jurisdiction of ASTM Committee D02 on Petroleum is obtainable from Corning Glass Co., Corning, NY, Catalog No. 3320. If you are
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on aware of alternative suppliers, please provide this information to ASTM Interna-
Elemental Analysis. tional Headquarters.Your comments will receive careful consideration at a meeting
Current edition approved May 1, 2005. Published May 2005. Originally of the responsible technical committee , which you may attend.
´1 4
approved in 1961. Last previous edition approved in 2000 as D1839 – 91 (2000) . Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D1839-91R05. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
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 [e-mail]. 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.
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D1839–91 (2005)
9. Preparation of Calibration Curve
9.1 Prepareaseriesofstandardsamplescontainingaknown
amount of amyl nitrate in diesel fuel, covering the range of 0.2
to 2.0 mg of amyl nitrate per gram (Note 3). Weigh 0.5-g
portions of these standards, to the nearest 0.1 mg, into the
Squibb-type separatory funnels and treat as described in
Section 10. Calculate the milligrams of amyl nitrate in each
standardbymultiplyingtheweightofthestandardtakenbythe
corresponding concentration of amyl nitrate. Construct a cali-
bration curve by plotting absorbance values as the ordinate and
corresponding milligrams of amyl nitrate per 50 mL as the
abscissa.
NOTE 3—Experience with the method indicates that different base
stocks of diesel fuels do not cause variations in the results. If low results
are obtained for a particular fuel, prepare standards using the fuel in
question to check the reaction and recoveries.
10. Procedure
10.1 Weigh into a separatory funnel a sample of diesel fuel
to the nearest 0.1 mg, not exceed
...