ASTM D1839-14
(Test Method)Standard Test Method for Amyl Nitrate in Diesel Fuels
Standard Test Method for Amyl Nitrate in Diesel Fuels
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 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 and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Buy Standard
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Standard Test Method for
1
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* 4. Significance and Use
1.1 This test method covers the determination of 0.1 to 0.5 4.1 Indieselfuel,thepresenceofalkylnitratessuchasamyl
nitrate, hexyl nitrate, or octyl nitrate causes a higher residue
volume % amyl nitrate in diesel fuels.
value than observed in untreated fuel, which can lead to
NOTE 1—This test method has been used for the determination of hexyl
erroneous conclusions as to the coke forming propensity of the
nitrate in diesel fuels, but has not been cooperatively tested for such
fuel. The presence of such alkyl nitrate in the fuel can be
samples. For the determination of hexyl nitrate, use standards containing
determined using this test method. This test method can be
nitrate esters of primary hexanol. Use a density of 0.97 in calculating
results.
used to determine the amount of amyl nitrate that has been
added to diesel fuels to improve cetane number. This test
1.2 The values stated in SI units are to be regarded as
method is applicable as a basis for judging compliance with
standard. No other units of measurement are included in this
specifications covering amyl nitrate.
standard.
1.3 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
5.1 Nitrateesters,inorganicnitrateions,andnitrogenoxides
responsibility of the user of this standard to establish appro-
will interfere to give high results.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Apparatus
6.1 Absorption Cells, matched, having a 1.000- 6 0.002-cm
2. Referenced Documents
light path.
2
2.1 ASTM Standards:
3
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.
3. Summary of Test Method
6.4 Lunge-type Pipet, 2-mL capacity.
3.1 This test method is based on the simultaneous hydroly-
NOTE 2—A 2.5-mL hypodermic syringe, with scabbard, can be used
sis of the ester in 62.5 % sulfuric acid and nitration of instead of the Lunge pipet.
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.
hydroxide to form the yellow sodium salt. Residual diesel fuel
6.6 Round-Bottom Flask, of borosilicate glass and having a
is removed by ether extraction. The color is measured spectro-
300-mL capacity.
photometrically at 452 nm, and the concentration of amyl
nitrate is determined by reference to a standard curve. 6.7 Separatory Funnel, Squibb-type, 125-mL capacity.
6.8 Shaking Machine, automatic, capable of 250
oscillations/min.
1
This test method is under the jurisdiction of ASTM Committee D02 on
6.9 Spectrophotometer, capable of measuring absorption in
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
the region of 452 nm.
Subcommittee D02.03 on Elemental Analysis.
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved
in 1961. Last previous edition approved in 2011 as D1839 – 11. DOI: 10.1520/
3
D1839-14. The sole source of supply of the apparatus known to the committee at this time
2
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
1
the ASTM website. of the responsible technical committee, which you may attend.
*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 ----------------------
D1839 − 14
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 be
...
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: D1839 − 11 D1839 − 14
Standard Test Method for
1
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*
1.1 This test method covers the determination of 0.1 to 0.5 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
3. Summary of Test Method
3.1 This test method is based on the simultaneous hydrolysis of the ester in 62.5 % sulfuric acid and nitration of m-xylenol by
the nitric acid liberated. The nitroxylenol is distilled from the reaction mixture and reacted with sodium hydroxide to form the
yellow sodium salt. Residual diesel fuel is removed by ether extraction. The color is measured spectrophotometrically at 452 nm,
and the concentration of amyl nitrate is determined by reference to a standard curve.
4. 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.
5. Interferences
5.1 Nitrate esters, inorganic nitrate ions, and nitrogen oxides will interfere to give high results.
6. Apparatus
6.1 Absorption Cells, matched, having a 1.000- 6 0.002-cm light path.
3
6.2 Distillate Collector, borosilicate glass with standard taper joints and sealed-in funnel (Fig. 1).
6.3 Electric Heating Mantle, to fit a 300-mL round-bottom flask, and having a variable transformer.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 1, 2011June 1, 2014. Published July 2011July 2014. Originally approved in 1961. Last previous edition approved in 20052011 as
D1839–91(2005).D1839 – 11. DOI: 10.1520/D1839-11.10.1520/D1839-14.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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.
3
The sole source of supply of the apparatus known to the committee at this time is obtainable from Corning Glass Co., Corning, NY, Catalog No. 3320. If you are aware
of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
1
technical committee, which you may attend.
*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 ----------------------
D1839 − 14
FIG. 1 Distillation Apparatus
6.4 Lunge-type Pipet, 2-mL capacity.
NOTE 2—A 2.5-mL hypodermic syringe, with scabbard, can be used instead of the Lunge pipet.
6.5 Reflux Condenser (Allihn-type), borosilicate glass, 300 mm 300 mm long, with standard-taper joints.
6.6 Round-Bottom Flask, of borosilicate glass and
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.