EN ISO 13759:1996

SLOVENSKI STANDARD
01-maj-1998
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Petroleum products - Determination of alkyl nitrate in diesel fuels - Spectrometric method
(ISO 13759:1996)
Mineralölerzeugnisse - Bestimmung von Alkylnitrat in Dieselkraftstoff -
Spektrometrisches Verfahren (ISO 13759:1996)
Produits pétroliers - Détermination du nitrate d'alkyle dans les carburants diesels -
Méthode spectrométrique (ISO 13759:1996)
Ta slovenski standard je istoveten z: EN ISO 13759:1996
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

IS0
INTERNATIONAL
STANDARD
First edition
1996-l 2-l 5
Petroleum products - Determination of
alkyl nitrate in diesel fuels - Spectrometric
method
Produits pgtroliers - Determination du nitrate d ’alkyle dans les carberrants
- Mgthode spectrom&rique
diesels
Reference number
OS0 13759: 1996(E)
IS0 13759: 1996(E)
‘\
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
technical committees. Each member body interested in a subject for which
a technical committee has been established has the right to be represented
on that committee. International organizations, governmental and non-
governmental, in liaison with ISO, also take part in the work. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard IS0 13759 was prepared by Technical Committee
ISOmC 28, Petroleum products and lubricants.
Annex A of this International Standard is for information only.
0 IS0 1996
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 l CH-1211 Geneve 20 l Switzerland
Internet
central @ isocs.iso.ch
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Printed in Switzerland
ii
IS0 13759: 1996(E)
INTERNATIONAL STANDARD @ IS0
Petroleum pro Determination of alkyl nitrate in diesel
- Spectrometric method
fuels
The use of this international Standard may involve hazardous materials, operations and
WARNING -
equipment. This standard does not purport to address all of the safety problems 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.
1 Scope
This International Standard specifies a procedure for the determination of alkyl nitrate in diesel fuel in the
concentration range 0,03 % (v/v) to 0,30 % (V/V) (volume fraction 0,03 % to 0,30 %).
A knowledge of the specific alkyl nitrate present in the diesel fuel is required for accurate determinations, as the
calibration of instrumentation is reliant on reference solutions containing the nitrate to be analysed. When the
specific alkyl nitrate is not known, a result comparative to a reference alkyl nitrate (4.2) gives indicative information.
NOTE - The addition of certain alkyi nitrates to diesel fuel enhances the cetane number as measured by the engine test
described in IS0 5165. It has no effect on the cetane index value as described in IS0 4264. See annex A.
The presence of nitrate esters, inorganic nitrate ions and nitrogen oxides will interfere with this determination.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain
registers of currently valid International Standards.
IS0 385-l :I 984, Laboratory glassware - Burettes - Par? I: General requirements.
IS0 835-I :I 981, Laboratory glassware - Graduated pipettes - Part I: General requirements.
IS0 1042: 1983, Laboratory glassware - One-mark volumetric flasks.
IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.

@ YSO
IS0 13759:1996(E)
3 Principle
The alkyl nitrate is hydrolysed in strong sulfuric acid solution and the nitric acid released is reacted with
2,4-dimethylphenol. The nitroxylenol is extracted from the reaction mixture and treated with sodium hydroxide to
form a solution of the yellow salt. The colour intensity is measured spectrometrically at 452 nm, and the
concentration of alkyl nitrate is determined by reference to the calibration curve.
4 Reagents
For the analysis described in this International Standard, use only reagents of recognized analytical grade, and
water complying with the requirements of Grade 3 of IS0 3696.
4.1 Acetic acid (CH&OOH), glacial.
4.2 Alkyll nitrate standard solution.
Pipette 3,0 ml of alkyl nitrate of composition identical to that to be analysed into a 100 ml flask (5.5) and dilute to the
mark with diesel fuel (4.6).
In the absence of knowledge of the specific alkyl nitrate to be analysed, use Z-ethylhexyl nitrate of minimum puaity
97 % to construct the calibration curve.
4.3 Sulfuric acid solution.
Add slowly with stirring, 500 ml of concentrated sulfuric acid, 98 % (m/m) (mass fraction 98 Oh) minimum purity, to
270 ml of cold water.
4.4 Sodium hydroxide solution.
Dissolve 50 g of sodium hydroxide pellets in water, and dilute to 1 000 ml with water.
4.5 2,4=dimethylphenol (xylenol) solution.
Dilute 4 ml of 2,4-dimethylphenol [(CH&C6H30H] with acetic acid (4.1), making up to the mark in a 100 ml flask
. .
(5 5)
. ves (blan k fuel).
46 Diesel fuel or component, clean, stable, containing no additi
similar to that of the sample under test.
NOTE - Where practicable, the composition of the blank fuel should be
4.7 2,2,4=trimethylpentane [CH&(CH&CH2CH(CH3)CHa],
...