ASTM D1839-11
(Test Method)Standard Test Method for Amyl Nitrate in Diesel Fuels
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.
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.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D1839 − 11
StandardTest 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 Thistestmethodcanbeusedtodeterminetheamountof
amyl nitrate that has been added to diesel fuels to improve
volume % amyl nitrate in diesel fuels.
cetane number. This test method is applicable as a basis for
NOTE 1—This test method has been used for the determination of hexyl
judging compliance with specifications covering amyl nitrate.
nitrate in diesel fuels, but has not been cooperatively tested for such
samples. For the determination of hexyl nitrate, use standards containing
5. Interferences
nitrate esters of primary hexanol. Use a density of 0.97 in calculating
results.
5.1 Nitrateesters,inorganicnitrateions,andnitrogenoxides
will interfere to give high results.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
6. Apparatus
standard.
6.1 Absorption Cells, matched, having a 1.000- 6 0.002-cm
1.3 This standard does not purport to address all of the
light path.
safety concerns, if any, associated with its use. It is the
3
responsibility of the user of this standard to establish appro- 6.2 Distillate Collector, borosilicate glass with standard
priate safety and health practices and determine the applica- taper joints and sealed-in funnel (Fig. 1).
bility of regulatory limitations prior to use.
6.3 Electric Heating Mantle, to fit a 300-mL round-bottom
flask, and having a variable transformer.
2. Referenced Documents
6.4 Lunge-type Pipet, 2-mL capacity.
2
2.1 ASTM Standards:
NOTE 2—A 2.5-mL hypodermic syringe, with scabbard, can be used
D1193 Specification for Reagent Water
instead of the Lunge pipet.
D4057 Practice for Manual Sampling of Petroleum and
6.5 Reflux Condenser (Allihn-type), borosilicate glass, 300
Petroleum Products
mm long, with standard-taper joints.
3. Summary of Test Method 6.6 Round-Bottom Flask, of borosilicate glass and having a
300-mL capacity.
3.1 This test method is based on the simultaneous hydroly-
6.7 Separatory Funnel, Squibb-type, 125-mL capacity.
sis of the ester in 62.5 % sulfuric acid and nitration of
m-xylenol by the nitric acid liberated. The nitroxylenol is
6.8 Shaking Machine, automatic, capable of 250
distilled from the reaction mixture and reacted with sodium
oscillations/min.
hydroxide to form the yellow sodium salt. Residual diesel fuel
6.9 Spectrophotometer, capable of measuring absorption in
is removed by ether extraction. The color is measured spectro-
the region of 452 nm.
photometrically at 452 nm, and the concentration of amyl
nitrate is determined by reference to a standard curve.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
1
This test method is under the jurisdiction of ASTM Committee D02 on
all reagents shall conform to the specifications of the Commit-
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
tee onAnalytical Reagents of theAmerican Chemical Society,
D02.03 on Elemental Analysis.
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved
in 1961. Last previous edition approved in 2005 as D1839–91(2005). DOI:
3
10.1520/D1839-11. 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
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D1839 − 11
7.8 m-Xylenol Solution—Dilute 4 mL of m-xylenol (2,4-
5
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 Prepareaserie
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D1839–91(Reapproved 2005) Designation: D1839 – 11
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.
1.2The values stated in SI units are to be regarded as the standard.
1.3This 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.
NOTE1—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—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 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
´1
Current edition approved May 1, 2005. Published May 2005. Originally approved in 1961. Last previous edition approved in 2000 as D1839–91(2000) . DOI:
10.1520/D1839-91R05.
Current edition approved June 1, 2011. Published July 2011. Originally approved in 1961. Last previous edition approved in 2005 as D1839–91(2005). DOI:
10.1520/D1839-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
*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 – 11
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.
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 long, with standard-taper joints.
6.6 Round-Bottom Flask, of borosilicate glass an
...
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