EN 14832:2005

SLOVENSKI STANDARD
01-september-2005
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Petroleum and related products - Determination of the oxidation stability and corrosivity
of fire-resistant phosphate ester fluids
Mineralölerzeugnisse und verwandte Produkte - Bestimmung der
Oxidationsbeständigkeit und der Einwirkung auf Metallwerkstoffe von
schwerentflammbaren Flüssigkeiten auf der Basis von Phosphorsäureestern
Pétrole et produits connexes - Détermination de la stabilité a l'oxydation et de la
corrosivité des fluides difficilement inflammables a base d'esters phosphates
Ta slovenski standard je istoveten z: EN 14832:2005
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN 14832
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2005
ICS 75.080
English version
Petroleum and related products - Determination of the oxidation
stability and corrosivity of fire-resistant phosphate ester fluids
Pétrole et produits connexes - Détermination de la stabilité Mineralölerzeugnisse und verwandte Produkte -
à l'oxydation et de la corrosivité des fluides difficilement Bestimmung der Oxidationsbeständigkeit und der
inflammables à base d'esters phosphates Einwirkung auf Metallwerkstoffe von schwerentflammbaren
Flüssigkeiten auf der Basis von Phosphorsäureestern
This European Standard was approved by CEN on 25 May 2005.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14832:2005: E
worldwide for CEN national Members.

Contents
Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions.4
4 Principle.5
5 Reagents and materials.5
6 Apparatus .6
7 Samples and sampling .9
8 Preparation of glassware.9
9 Preparation of metal test pieces .9
10 Procedure .10
11 Calculation.10
12 Expression of results.11
13 Precision.11
14 Test report .12
Bibliography.13

Foreword
This European Standard (EN 14832:2005) has been prepared by Technical Committee CEN/TC 19 “Petroleum
products, lubricants and related products”, the secretariat of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an identical text or
by endorsement, at the latest by December 2005, and conflicting national standards shall be withdrawn at the latest
by December 2005.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark,
Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

1 Scope
This European Standard specifies a method for assessing the oxidation stability of phosphate ester hydraulic
fluids. These products fall into category HFDR of EN ISO 6743-4 [2] and into categories TSD, TGD and TCD
of ISO 6743-5 [3]. The amount of acid developed during the test and the mass changes of the metal
specimens are used to assess the level of oxidation stability.
The precision of the test method applies to changes in acid number up to 3,0 mg KOH/g and changes in mass
of up to 3 mg per test piece. The change of acidity is determined using one of the test methods ISO 6618,
ISO 6619, or ISO 7537. Results from two different test methods are not necessarily compatible and direct
comparison needs caution.
NOTE This test method may also be applied to other non-aqueous fire-resistant fluids, such as those falling into
category HFDU of EN ISO 6743-4 [2].
WARNING — The use of this European Standard may involve hazardous materials, operations and
equipment. This document does not purport to address all of the safety problems associated with its
use. It is the responsibility of the user of this document to establish appropriate safety and health
practices and determine the applicability of regulatory limitations prior to use.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
EN 10277-2, Bright steel products — Technical delivery conditions — Part 2: Steels for general engineering
purposes
EN ISO 2160, Petroleum products — Corrosiveness to copper — Copper strip test (ISO 2160:1998)
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170:2004)
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
ISO 6618, Petroleum products and lubricants — Determination of acid or base number — Colour-indicator
titration method
ISO 6619, Petroleum products and lubricants — Neutralization number — Potentiometric titration method
ISO 7537, Petroleum products — Determination of acid number — Semi-micro colour-indicator titration
method
3 Terms and definitions
For the purposes of this European Standard, the following terms and definitions apply.
3.1
oxidation stability
sum of the changes in acid number of the fire-resistant fluid and of water in the absorption vessel when
subjected to the accelerated oxidizing conditions specified in this document
3.2
corrosivity
change in mass of specified metal test pieces subjected to the accelerated oxidizing conditions specified in
this document
4 Principle
A test portion of fluid, of known acid number, is placed in a test vessel, which contains cleaned and weighed
copper and steel test pieces. The fluid and test pieces are then subjected to a temperature of 120 °C under an
oxygen flow rate of 1 l/h for 164 h. The exhausted gaseous acidic products of the oxidation are absorbed in
water, and the acid number of this phase is determined. The acid number of the test portion and the mass of
the test pieces are determined at the end of the test period, and the results are calculated as the sum of the
changes in acid number, and/or the change in mass of the individual test pieces.
5 Reagents and materials
Unless otherwise specified, reagents shall be of recognized analytical grade.
5.1 Water, conforming to the requirements of grade 3 of EN ISO 3696.
5.2 Oxygen, Minimum purity 99,4 %.
5.3 Phenolphthalein, 1 g/l ethanolic solution.
5.4 Potassium hydroxide, 0,1 mol/l ethanolic solution.
5.5 Wash solvent, use either 2,2,4-trimethylpentane or petroleum spirit with a boiling range of 60 °C to
80 °C for the metal test pieces.
5.6 Acetone.
CAUTION — Acetone is a flammable liquid and should be handled with appropriate care.
5.7 Strong oxidizing cleaning solution.
The reference oxidizing cleaning solution, on which precision was based, is chromsulfuric acid (see the
warning statement below), but alternative non-chromium containing solutions, such as ammonium persulfate
in concentrated sulfuric acid (8 g/l) have also been found to give satisfactory cleanliness. Other non-alkaline
laboratory cleaning agents that are demonstrated to give equivalent cleanliness to chromsulfuric acid, may be
used for routine analysis.
CAUTION — Chromsulfuric acid is a health hazard. It is toxic, a recognized carcinogen as it contains
Cr-VI compounds, highly corrosive and potentially hazardous in contact with organic materials. When
using chromsulfuric acid cleaning solution, eye protection and protective clothing are essential. Never
pipette the cleaning solution by mouth. After use, do not pour cleaning solution down the drain, but
neutralize it with great care owing to the concentrated sulfuric acid present, and dispose of it in
accordance with standard procedures for toxic waste (chromium is highly dangerous to the
environment).
Non-chromium containing, strong oxidizing acid cleaning solutions are also highly corrosive and
potentially hazardous in contact with organic materials, but do not contain chromium which has
special disposal problems.
5.8 Abrasives, silicon carbide paper or cloth of 65 µm (grade 240) and of 30 µm (grade 600) grit size.
-4
5.9 Drying agent, molecular sieve with a pore size of 4 x 10 µm or other equivalent means for drying the
oxygen (5.2).
6 Apparatus
6.1 Heating block or heating bath
Consisting of an aluminium block (see Figure 1) or an oil bath (see Figure 2), capable of maintaining a
temperature in the test portion of 120 °C ± 0,5 °C. It shall be fitted with an outer cover of non-asbestos thermal
insulating material such that the surface temperature does not exceed 60 °C. The design of the bath and test
vessel supports shall ensure that the test vessel is heated over a length of 150 mm.
In the case of an aluminium heating block, there shall not be a gap between the test vessel and the thermal
insulation. In the case of an oil bath, the test vessel shall be immersed to a depth of 137 mm, and the distance
from the bottom of the test vessel to the underside of the bath cover shall be 150 mm ± 2 mm. The gap
between test vessel and bath cover shall be sealed by means of an O-ring.

Key
1 Aluminium block 3 Test vessel
2 Thermal insulation 4 O-ring
Figure 1 — Heating block
Key
1 Oil 4 O-ring
2 Bath cover 5 Test vessel support
3 Test vessel 6 Bottom heating bath
Figure 2 — Oil bath
6.2 Test vessels
Constructed of borosilicate glass, of length 210 mm ± 2 mm, outer diameter 28 mm ± 0,5 mm, wall thickness
2 mm ± 0,2 mm, and fitted with a female tapered ground-glass joint of either 24/29 or 24/39 size. A second
test vessel is used as the absorption vessel.
6.3 Inserts
Constructed of borosilicate glass, with a male tapered ground-glass joint to fit into the test vessel and
absorption vessel. They are equivalent to a wash-bottle insert, carrying a glass inlet tube of outside diameter
5 mm ± 0,4 mm and a wall thickness of 0,8 mm ± 0,1 mm, with the bottom tip bevelled at 30°. The distance
between the tip of the inlet tube and the bottom of the test vessel shall be 2,5 mm ± 0,5 mm when fitted. The
inserts shall be fitted with a joint connector of suitable gas-tight design, such that two inserts fitted together
give a horizontal distance of 100 mm to 200 mm between the test vessel and absorption vessel. Other joint
connectors or connections like PTFE tubing may be used if they fulfil the requirements of this clause. The
general arrangement is illustrated in Figure 3.
Key
1 Oxygen inlet 4 Female tapered ground glass joint
2 Joint connector 5 Test vessel
3 Insert 6 Absorption vessel
Figure 3 — General arrangement of apparatus
6.4 Flowmeter, capable of measuring a flow rate of 1 l/h to the nearest 0,1 l/h.
NOT
...