Lubricants - Determination of aerobic biological degradation of fully formulated lubricants in an aqueous solution - Test method based on CO2-production

This document specifies a procedure for determining the degree of aerobic degradation of fully formulated lubricants. The organic material in a fully formulated lubricant is exposed in a synthetic aqueous medium under laboratory conditions to an inoculum from activated sludge.
Biodegradation resulting in mineralisation of the organic material can be determined by measuring released CO2 in a total organic carbon (TOC-) analyser. In contrast to existing test methods measuring released CO2 this method uses a precise preparation procedure for non-water soluble organic material.
The above mentioned method applies to fully formulated lubricants which
a)   are water-soluble, non-water soluble or emulsifiable, and
b)   are not toxic and not inhibitory to the test microorganisms at the test concentration.
The presence of inhibitory effects is determined as specified in this document.
This test method is focused on fresh water as test medium. Tests in sea water are currently not included in this method, but may be introduced later.

Schmieröle - Bestimmung des aeroben biologischen Abbaus von fertig formulierten Schmierstoffen in wässriger Lösung - Prüfverfahren mittels CO2-Produktion

Dieses Dokument legt ein Prüfverfahren für die Bestimmung des Grades des aeroben Bioabbaus fertig formulierter Schmierstoffe fest. Das organische Material in einem fertig formulierten Schmierstoff wird in einem künstlichen wässrigen Medium einem Inokulum aus Belebtschlamm ausgesetzt.
Der Bioabbau, der zur Mineralisierung des organischen Materials führt, kann durch Messung des frei-gesetzten CO2 in einem TOC-Analysator (en: total organic carbon) bestimmt werden. Im Gegensatz zu vorhandenen Prüfverfahren, die freigesetztes CO2 messen, nutzt dieses Verfahren eine präzise Probenvorbereitung für nicht-wasserlösliches organisches Material.
Das zuvor genannte Verfahren gilt für fertig formulierte Schmierstoffe, die:
a) wasserlöslich, nicht-wasserlöslich oder emulgierbar sind und
b) nicht toxisch und nicht hemmend gegenüber den Prüfmikroorganismen bei der Prüfkonzentration sind.
Das Vorhandensein von hemmenden Wirkungen wird nach diesem Dokument bestimmt.
Dieses Prüfverfahren ist auf Frischwasser als Prüfmedium fokussiert. Prüfungen in Meerwasser sind derzeit in diesem Verfahren nicht erfasst, können jedoch zu einem späteren Zeitpunkt eingeführt werden.

Lubrifiants - Détermination de la biodégradabilité aérobie, en solution aqueuse, de lubrifiants complètement formulés - Méthode basée sur le dégagement de CO2

Le présent document définit une procédure pour la détermination du degré de dégradation aérobie de lubrifiants complètement formulés. La matière organique contenue dans un lubrifiant complètement formulé est placée en milieu aqueux synthétique dans des conditions de laboratoire et exposée à un inoculum de boues activées.
La dégradation biologique entraînant une minéralisation de la matière organique peut être déterminée en mesurant le dégagement de CO2 dans un analyseur de carbone organique total (COT). Contrairement aux méthodes d’essai existantes mesurant le dégagement de CO2, cette méthode s’appuie sur une procédure préparatoire précise pour une matière organique non soluble dans l’eau.
La méthode susmentionnée s’applique aux lubrifiants complètement formulés qui :
a)   sont solubles dans l’eau, non solubles dans l’eau ou émulsifiables ; et
b)   ne sont pas toxiques et n’ont aucun effet d’inhibition sur les microorganismes d’essai à la concentration d’essai.
La présence d’effets inhibiteurs est déterminée dans les conditions spécifiées par le présent document.
Cette méthode d’essai utilise de l’eau douce comme milieu d’essai. Les essais en eau de mer ne sont pas inclus actuellement dans cette méthode, mais peuvent être introduits à une date ultérieure.

Maziva - Določevanje aerobne biološke razgradnje polno formuliranih maziv v vodni raztopini - Preskusna metoda, ki temelji na proizvodnji CO2

Ta standard določa postopek za določanje stopnje aerobne razgradnje polno formuliranih maziv. Organski material v polno formuliranem mazivu je v sintetičnem vodnem mediju pod laboratorijskimi pogoji izpostavljen inokulumu iz aktivnega blata. Biološko razgradnjo, ki povzroča mineralizacijo organskega materiala, je mogoče določiti z merjenjem sproščenega CO2 v analizatorju skupnega organskega ogljika (TOC). Zgoraj navedena metoda velja za polno formulirana maziva, ki a) so topna v vodi, niso topna v vodi ali emulzivna; b) niso strupena in niso zaviralna za preskusne mikroorganizme pri preskusni koncentraciji. Določiti je mogoče prisotnost zaviralnih učinkov.

General Information

Status
Published
Publication Date
19-Feb-2019
Withdrawal Date
30-Aug-2019
Current Stage
9020 - Submission to 2 Year Review Enquiry - Review Enquiry
Start Date
15-Apr-2024
Completion Date
15-Apr-2024

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SLOVENSKI STANDARD
01-april-2019
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Lubricants - Determination of aerobic biological degradation of fully formulated lubricants
in an aqueous solution - Test method based on CO2-production
Flüssige Mineralölerzeugnisse - Bestimmnung des aerobe biologischen Abbaus von
vollständig formulierten Schmierstoffen in wässriger Lösung - Prüfverfahren mittels CO2-
Produktion
Bio-lubrifiants - Détermination de la biodégradabilité aérobie, en solution aqueuse, de
lubrifiants complètement formulés - Méthode basée sur le dégagement de CO2
Ta slovenski standard je istoveten z: EN 17181:2019
ICS:
75.100 Maziva Lubricants, industrial oils and
related products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17181
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2019
EUROPÄISCHE NORM
ICS 75.100
English Version
Lubricants - Determination of aerobic biological
degradation of fully formulated lubricants in an aqueous
solution - Test method based on CO2-production
Bio-lubrifiants - Détermination de la biodégradabilité Schmierstoffe - Bestimmung der aeroben biologischen
aérobie, en solution aqueuse, de lubrifiants Abbaubarkeit ausformulierter Schmiermittel in
complètement formulés - Méthode basée sur le wässrigem Medium - Testmethode basierend auf CO2-
dégagement de CO2 Bestimmung
This European Standard was approved by CEN on 14 December 2018.

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 CEN-CENELEC Management Centre 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 CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17181:2019 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 8
5 Test environment . 8
6 Reagents . 8
7 Apparatus . 9
8 Procedure. 10
8.1 Preparation of mineral medium . 10
8.2 Preparation of the test volumes . 10
8.2.1 Test sample . 10
8.2.2 Reference compound . 11
8.2.3 Inhibition control . 11
8.2.4 Elimination control . 11
8.3 Preparation of the inoculum . 11
8.3.1 General . 11
8.3.2 Inoculum from an activated sludge plant . 11
8.3.3 Pre-conditioning . 11
8.3.4 Pre-exposure . 11
8.4 Test . 12
Table 1 — Overview on the desired final test matrix . 12
9 Calculation and reporting of results . 13
9.1 Theoretical amount of CO released from test sample . 13
9.2 Percentage biodegradation . 13
9.3 Expression of results . 14
10 Validity and precision . 14
10.1 Validity . 14
10.2 Precision . 15
10.2.1 General . 15
10.2.2 Repeatability . 15
10.2.3 Reproducibility . 15
11 Test report . 15
Annex A (informative) Comparison table of most common mineralisation methods . 17
Annex B (informative) Sample insertion . 22
Annex C (informative) Specification of reference compound High Oleic Reference Oil
(HORO) . 24
Annex D (informative) Example of degradation curves . 25
Figure D.1 — Example of degradation curve . 25
Bibliography . 26

European foreword
This document (EN 17181:2019) has been prepared by Technical Committee CEN/TC 19 “Gaseous and
liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, 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 August 2019, and conflicting national standards shall
be withdrawn at the latest by August 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Introduction
Existing test methods for determination of aerobic biodegradation of organic substances in an aqueous
medium (e.g. numerous ISO and OECD test methods) are widely used. Moreover, all actually existing
ecolabels, international and national regulations and recommendations are working with them.
Testing of organic substances requires a broad scope of preparation tools to maintain comparable
results for all different materials appearing liquid, solid, water-soluble, non-water-soluble or
emulsifiable.
In consequence of this, results may differ regarding the choice of test method, preparation procedure or
inoculum thus leading to low levels of reproducibility and repeatability.
Fully formulated lubricants (oils or greases or emulsions) are complex mixtures of mostly organic
compounds that are mainly water insoluble. Based on ISO 9439 (resp. OECD 301B) this test method has
been aligned by modifying sample preparation and test procedure for such complex mixtures in order
to achieve improved significance of test results. The test method described in this document, however,
was not assessed for greases. The precision statement therefore only applies for lubricating oils.
Finally, from customer’s point of view a biodegradation test method for the final product of improved
significance will result in better market transparency, enhanced reputation of “bio-lubricants” and
confidence of the customer in this product group.
1 Scope
This document specifies a procedure for determining the degree of aerobic degradation of fully
formulated lubricants. The organic material in a fully formulated lubricant is exposed in a synthetic
aqueous medium under laboratory conditions to an inoculum from activated sludge.
Biodegradation resulting in mineralisation of the organic material can be determined by measuring
released CO in a total organic carbon (TOC) analyser. In contrast to existing test methods measuring
released CO this method uses a precise preparation procedure for non-water soluble organic material.
The above mentioned method applies to fully formulated lubricants which
a) are water-soluble, non-water soluble or emulsifiable, and
b) are not toxic and not inhibitory to the test microorganisms at the test concentration.
The presence of inhibitory effects is determined as specified in this document.
This test method is focused on fresh water as test medium. Tests in sea water are currently not included
in this method, but may be introduced later.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
ISO 9439, Water quality — Evaluation of ultimate aerobic biodegradability of organic compounds in
aqueous medium — Carbon dioxide evolution test
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1
organic material
total amount of all organic compounds a fully formulated lubricant consists of
3.2
aerobic biodegradation
consumption of organic
...

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