ASTM D1839-91(2000)e1

Standard Test Method for Amyl Nitrate in Diesel Fuels

SCOPE
1.1 This test method covers the determination of 0.1 to 0.5 volume percent amyl nitrate in diesel fuels.  
1.2 The preferred units are acceptable metric units.  
1.3 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. > 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: 09-Apr-2000
• 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

• Replaced By: ASTM D1839-91(2005) - Standard Test Method for Amyl Nitrate in Diesel Fuels
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1839–91(Reapproved 2000)
Standard Test Method for
Amyl Nitrate in Diesel Fuels
This standard is issued under the fixed designation D 1839; 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—Editorial corrections were made throughout in April 2000.
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 percent amyl nitrate in diesel fuels.
5. Interferences
1.2 The preferred units are acceptable metric units.
5.1 Nitrateesters,inorganicnitrateions,andnitrogenoxides
1.3 This standard does not purport to address all of the
will interfere to give high results.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Apparatus
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.
light path.
NOTE 1—This test method has been used for the determination of hexyl
6.2 Distillate Collector, borosilicate glass with standard
nitrate in diesel fuels, but has not been cooperatively tested for such
taper joints and sealed-in funnel (Fig. 1).
samples. For the determination of hexyl nitrate, use standards containing
6.3 Electric Heating Mantle, to fit a 300-mL round-bottom
nitrate esters of primary hexanol. Use a density of 0.97 in calculating
flask, and having a variable transformer.
results.
6.4 Lunge-type Pipet, 2-mL capacity.
2. Referenced Documents
NOTE 2—A 2.5-mL hypodermic syringe, with scabbard, can be used
2.1 ASTM Standards:
instead of the Lunge pipet.
D 1193 Specification for Reagent Water
6.5 Reflux Condenser (Allihn-type), borosilicate glass, 300
D 4057 Practice for Manual Sampling of Petroleum and
mm long, with standard-taper joints.
Petroleum Products
6.6 Round-Bottom Flask, of borosilicate glass and having a
300-mL capacity.
3. Summary of Test Method
6.7 Separatory Funnel, Squibb-type, 125-mL capacity.
3.1 This test method is based on the simultaneous hydroly-
6.8 Shaking Machine, automatic, capable of 250
sis of the ester in 62.5 % sulfuric acid and nitration of
oscillations/min.
m-xylenol by the nitric acid liberated. The nitroxylenol is
6.9 Spectrophotometer, capable of measuring absorption in
distilled from the reaction mixture and reacted with sodium
the region of 452 nm.
hydroxide to form the yellow sodium salt. Residual diesel fuel
is removed by ether extraction. The color is measured spectro-
7. Reagents
photometrically at 452 nm, and the concentration of amyl
7.1 Purity of Reagents—Reagent grade chemicals shall be
nitrate is determined by reference to a standard curve.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
4. Significance and Use
tee onAnalytical Reagents of theAmerican Chemical Society,
4.1 Thistestmethodcanbeusedtodeterminetheamountof
where such specifications are available. Other grades may be
amyl nitrate that has been added to diesel fuels to improve
used, provided it is first ascertained that the reagent is of
1 4
This method is under the jurisdiction of ASTM Committee D02 on Petroleum Obtainable from Corning Glass Co., Corning, NY, Catalog No. 3320.
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on Reagent Chemicals, American Chemical Society Specifications, American
Elemental Analysis. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved March 15, 1991. Published July 1991. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1839 – 61 T. Last previous edition D 1839 – 87. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 05.02. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D1839–91 (2000)
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 exceeding 2 mL (Note 4), and not
containing more than 1.0 mg of amyl nitrate.Add 2 mL of the
m-xylenol solution and shake thoroughly.Add 50 mLof H SO
4. Shake for 30 min on the automatic shaking machine.
Transfer the con
...