ASTM D1839-14(2019)
(Test Method)Standard Test Method for Amyl Nitrate in Diesel Fuels (Withdrawn 2019)
Standard Test Method for Amyl Nitrate in Diesel Fuels (Withdrawn 2019)
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 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 % by volume amyl nitrate in diesel fuels.
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.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
WITHDRAWN RATIONALE
This test method covers the determination of 0.1 % to 0.5 % by volume amyl nitrate in diesel fuels.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in November 2019 because it is not being used in the industry. This standard was used for the determination of cetane improvers in diesel. Most of the concerns with the use of cetane improvers and diesel fuel storage stability are from the time when higher sulfur diesel fuels were used. Cetane improvers have also been shown to affect the thermal stability of the fuels. Current cetane improvers do not include this chemical any longer. Hence, there is no need for this standard.
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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 − 14 (Reapproved 2019)
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 hydroxide to form the yellow sodium salt. Residual diesel fuel
is removed by ether extraction. The color is measured spectro-
1.1 This test method covers the determination of 0.1 % to
photometrically at 452 nm, and the concentration of amyl
0.5 % by volume amyl nitrate in diesel fuels.
nitrate is determined by reference to a standard curve.
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
4. Significance and Use
samples. For the determination of hexyl nitrate, use standards containing
4.1 Indieselfuel,thepresenceofalkylnitratessuchasamyl
nitrate esters of primary hexanol. Use a density of 0.97 in calculating
results.
nitrate, hexyl nitrate, or octyl nitrate causes a higher residue
value than observed in untreated fuel, which can lead to
1.2 The values stated in SI units are to be regarded as
erroneous conclusions as to the coke forming propensity of the
standard. No other units of measurement are included in this
fuel. The presence of such alkyl nitrate in the fuel can be
standard.
determined using this test method. This test method can be
1.3 This standard does not purport to address all of the
used to determine the amount of amyl nitrate that has been
safety concerns, if any, associated with its use. It is the
added to diesel fuels to improve cetane number. This test
responsibility of the user of this standard to establish appro-
method is applicable as a basis for judging compliance with
priate safety, health, and environmental practices and deter-
specifications covering amyl nitrate.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5. Interferences
dance with internationally recognized principles on standard-
5.1 Nitrateesters,inorganicnitrateions,andnitrogenoxides
ization established in the Decision on Principles for the
will interfere to give high results.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
6. Apparatus
Barriers to Trade (TBT) Committee.
6.1 Absorption Cells, matched, having a 1.000 cm 6
2. Referenced Documents 0.002 cm light path.
2 3
2.1 ASTM Standards: 6.2 Distillate Collector, borosilicate glass with standard
D1193 Specification for Reagent Water taper joints and sealed-in funnel (Fig. 1).
D4057 Practice for Manual Sampling of Petroleum and
6.3 Electric Heating Mantle, to fit a 300 mL round-bottom
Petroleum Products
flask, and having a variable transformer.
6.4 Lunge-type Pipet, 2 mL capacity.
3. Summary of Test Method
3.1 This test method is based on the simultaneous hydroly-
NOTE 2—A 2.5 mL hypodermic syringe, with scabbard, can be used
instead of the Lunge pipet.
sis of the ester in 62.5 % sulfuric acid and nitration of
m-xylenol by the nitric acid liberated. The nitroxylenol is
6.5 Reflux Condenser (Allihn-type), borosilicate glass,
distilled from the reaction mixture and reacted with sodium
300 mm long, with standard-taper joints.
6.6 Round-Bottom Flask, of borosilicate glass and having a
This test method is under the jurisdiction of ASTM Committee D02 on 300 mL capacity.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
6.7 Separatory Funnel, Squibb-type, 125 mL capacity.
Subcommittee D02.03 on Elemental Analysis.
Current edition approved April 15, 2019. Published May 2019. Originally
approved in 1961. Last previous edition approved in 20141 as D1839 – 14. DOI:
10.1520/D1839-14R19. The sole source of supply of the apparatus known to the committee at this time
For referenced ASTM standards, visit the ASTM website, www.astm.org, or is obtainable from Corning Glass Co., Corning, NY, Catalog No. 3320. If you are
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM aware of alternative suppliers, please provide this information to ASTM Interna-
Standards volume information, refer to the standard’s Document Summary page on tional Headquarters.Your comments will receive careful consideration at a meeting
the ASTM website. of the responsible technical committee, which you may attend.
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D1839 − 14 (2019)
7.6 Sodium Hydroxide Solution (20 g⁄L)—Dissolve 20 g of
sodium hydroxide (NaOH) pellets in water and dilute to 1 L.
7.7 Sulfuric Acid (5+3) —Slowly add, with stirring,
500 mL of nitrate-free concentrated sulfuric acid (H SO , rel
2 4
dens 1.84) to 300 mLof water.The m-xylenol solution must be
added before the H SO , otherwise low or negative results will
2 4
be obtained. Cool before use.
7.8 m-Xylenol Solution—Dilute 4 mL of m-xylenol (2,4-
dimethylphenol ) to 100 mL with acetone. Prepare fresh each
day.
8. Sampling
8.1 Samples shall be taken in accordance with the appropri-
ate instructions in Practice D4057.
9. Preparation of Calibration Curve
9.1 Prepareaseriesofstandardsamplescontainingaknown
amount of amyl nitrate in diesel fuel, covering the range of
0.2 mg to 2.0 mg of amyl nitrate per gram (Note 3). Weigh
0.5 gportionsofthesestandards,tothenearest0.1 mg,intothe
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-
FIG. 1 Distillation Apparatus
bration curve by plotting absorbance values as the ordinate and
corresponding milligrams of amyl nitrate per 50 mL as the
abscissa.
6.8 Shaking Machine, automatic, capable of 250
oscillations/min.
NOTE 3—Experience with the method indicates that different base
stocks of diesel fuels do not cause variations in the results. If low results
6.9 Spectrophotometer, capable of measuring absorption in
are obtained for a particular fuel, prepare standards using the fuel in
the region of 452 nm.
question to check the reaction and recoveries.
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