SIST EN 15522-1:2023
(Main)Oil spill identification - Petroleum and petroleum related products - Part 1: Sampling
Oil spill identification - Petroleum and petroleum related products - Part 1: Sampling
This document provides guidance on taking and handling samples related to oil spill identification in legal proceedings. Guidance is given on obtaining samples from both the spill and its potential source.
Preservation of evidence is an essential part of legal procedures and this document presents appropriate oil sampling procedures.
WARNING - The use of this document can 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 users of this document to take appropriate measures to ensure the safety and health of personnel prior to the application of the standard, and to determine the applicability of any other restrictions for this purpose.
IMPORTANT - Most countries have teams with specialists trained in sampling on board of ships. Do not take unnecessary risks, seek assistance from such teams where available.
NOTE For the sake of clarity, the word ‘oil’ is used throughout this document. It can equally refer to crude oil, a petroleum product or mixtures of such.
Identifizierung von Ölverschmutzungen - Rohöl und Mineralölerzeugnisse - Teil 1: Probenahme
Dieses Dokument enthält eine Anleitung für die Probenahme und Handhabung von Proben zur Identifizierung von Ölverschmutzungen für Gerichtsverfahren. Es wird eine Anleitung zur Probenahme sowohl von der Verschmutzung als auch von der potenziellen Quelle gegeben.
Die Beweissicherung ist ein wichtiger Teil von Rechtsverfahren, und in diesem Dokument werden geeignete Verfahren für Ölproben vorgestellt.
WARNUNG - Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen.
Dieses Dokument beansprucht nicht, alle mit seiner Anwendung verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung der Personen, die dieses Dokument anwenden, vor der Anwendung der Norm geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen, und die Anwendbarkeit weiterer diesbezüglicher Beschränkungen festzulegen.
WICHTIG - Die meisten Länder verfügen über Teams mit spezieller Ausbildung für die Probenahme an Bord von Schiffen. Keine unnötigen Risiken eingehen; diese Teams, sofern verfügbar, um Unterstützung bitten.
ANMERKUNG Aus Gründen der Übersichtlichkeit wird in diesem Dokument durchgehend das Wort "Öl" verwendet. Es kann sich gleichermaßen auf Rohöl, ein Mineralölerzeugnis oder Mischungen davon beziehen.
Identification des pollutions pétrolières - Pétrole et produits pétroliers - Partie 1 : Échantillonnage
Le présent document fournit des recommandations de prélèvement et de manipulation des échantillons liés à l'identification d'un déversement pétrolier dans le cadre d'une procédure judiciaire. Ces recommandations ont trait aussi bien à l'échantillonnage du pétrole déversé que de la source potentielle.
La conservation des preuves est un élément essentiel dans le cadre de procédures judiciaires, et les échantillons de pétrole doivent être traités en conséquence (échantillonnage requis par la loi).
AVERTISSEMENT - L’utilisation de ce document peut impliquer des produits, des opérations et du matériel à caractère dangereux.
Le présent document ne prétend pas traiter tous les problèmes de sécurité liés à son utilisation. Il est de la responsabilité des utilisateurs de ce document de prendre les mesures appropriées pour garantir la sécurité et la santé du personnel avant l'application de ce document, et de déterminer l'applicabilité de toute autre restriction à cette fin.
IMPORTANT - La plupart des pays disposent de spécialistes formés au prélèvement d'échantillons à bord des navires. Il est fortement conseillé de ne pas prendre de risques inutiles et de solliciter l'assistance de telles équipes, si elles existent.
NOTE À des fins de clarté, le terme « pétrole » est utilisé tout au long du présent document. Il peut se rapporter au pétrole brut, à un produit pétrolier ou à un mélange des deux.
Prepoznavanje razlitij olj - Nafta in sorodni naftni proizvodi - 1. del: Vzorčenje
Standard EN 15522-1 vsebuje smernice za prevzem in rokovanje z vzorci, ki se jih zbira v sklopu preiskave možnega vira razlitja surove nafte ali naftnega proizvoda v morsko ali vodno okolje. Podane so smernice za odvzem vzorcev tako iz razlitja kot iz potencialnega izvora razlitja.
Vzorčenje olja je predvsem del pravnih postopkov in ga je treba obravnavati kot vse ostale postopke ohranjanja dokazov (pravno vzorčenje). Če se bo vzorce uporabilo v zvezi s pravnimi postopki, je priporočljivo ta dokument brati skupaj z vsemi drugimi dokumenti, ki jih izdajo regulativni organi v državi ali državah, kjer je do razlitja prišlo.
Pri odvzemu vzorcev so lahko prisotni nevarni materiali, postopki in oprema.
Ta dokument ni namenjen obravnavi vseh varnostnih in zdravstvenih vidikov, ki se navezujejo na podane smernice. Za oblikovanje in vzpostavitev ustreznih varnostnih in zdravstvenih praks ter za določitev uporabnosti regulativnih omejitev pred uporabo je odgovoren uporabnik.
Opomba: Večina držav ima posebej usposobljene skupine za odvzem vzorcev na krovu ladij. Uslužbenci policije ali organov pregona ne prevzemajo nepotrebnih tveganj in po potrebi prosijo za pomoč zadevno skupino.
Zaradi jasnosti se v celotnem dokumentu uporablja beseda »olje«. Beseda se nanaša na surovo nafto, naftni proizvod ali njuno mešanico.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-junij-2023
Nadomešča:
SIST-TP CEN/TR 15522-1:2008
Prepoznavanje razlitij olj - Nafta in sorodni naftni proizvodi - 1. del: Vzorčenje
Oil spill identification - Petroleum and petroleum related products - Part 1: Sampling
Identifizierung von Ölverschmutzungen - Rohöl und Mineralölerzeugnisse - Teil 1:
Probenahme
Identification des pollutions pétrolières - Pétrole et produits pétroliers - Partie 1 :
Échantillonnage
Ta slovenski standard je istoveten z: EN 15522-1:2023
ICS:
13.020.40 Onesnaževanje, nadzor nad Pollution, pollution control
onesnaževanjem in and conservation
ohranjanje
13.060.99 Drugi standardi v zvezi s Other standards related to
kakovostjo vode water quality
75.080 Naftni proizvodi na splošno Petroleum products in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 15522-1
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2023
EUROPÄISCHE NORM
ICS 13.020.40; 75.080 Supersedes CEN/TR 15522-1:2006
English Version
Oil spill identification - Petroleum and petroleum related
products - Part 1: Sampling
Identification des pollutions pétrolières - Pétrole et Identifizierung von Ölverschmutzungen - Rohöl und
produits pétroliers - Partie 1 : Échantillonnage Mineralölerzeugnisse - Teil 1: Probenahme
This European Standard was approved by CEN on 25 December 2022.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye 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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15522-1:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms, definitions and abbreviations . 6
3.1 Terms and definitions . 6
3.2 Abbreviations . 8
4 Principle . 8
5 Sampling in general . 8
5.1 General. 8
5.2 Sampling schedule . 9
5.3 Types of sample . 9
5.4 Sample volume . 10
5.5 Number of samples to be taken . 10
6 Precautions against contamination of samples during collection . 11
6.1 General. 11
6.2 Potential sources of contamination . 11
6.3 Controls . 11
7 Sampling equipment and sample containers and closures . 11
7.1 Introduction . 11
7.2 General instructions and strategies . 12
7.3 Sample containers, closures and packages . 12
7.4 Sample devices . 13
7.4.1 General. 13
7.4.2 For sampling oil layers and oil sheens from water surfaces . 13
7.4.3 For sampling ship’s cargo tanks, bunker tanks and bilges, barges, road tankers, shore tanks
and pipelines . 13
7.4.4 For sampling waterborne oil layers greater than 1 mm thickness . 14
7.4.5 For sampling waterborne very viscous oil layers . 14
7.4.6 Helicopter sampling devices . 15
7.4.7 Less suitable sampling devices . 17
8 Sampling procedures . 18
8.1 Sampling from water surfaces . 18
8.1.1 Sampling oil layers less than 1 mm and sheens . 18
8.1.2 Sampling of viscous oil layers greater than 1 mm thickness . 19
8.1.3 Helicopter sampling . 20
8.2 Sampling beaches, rocky shores, river banks and harbour structures . 20
8.3 Sampling tar balls . 21
8.4 Samples from oiled animals . 21
8.5 Samples from ships, barges or river-craft . 21
8.5.1 General. 21
8.5.2 Sampling cargo, bunker tanks and slop tanks . 22
8.5.3 Sampling from ships, barges or river craft pipelines . 23
8.5.4 Samples from ballast tanks, bilges and void spaces. 23
8.6 Sampling from land tanks and pipelines . 23
8.7 Sampling from road and rail tank wagons . 23
9 Sample documentation and logistics . 23
9.1 Sample information and documentation . 23
9.2 Sealing of samples . 24
9.3 Custody of samples . 25
9.4 Sample holding time . 25
10 Transport and storage of samples . 26
Annex A (informative) Recommended contents of sampling kits . 27
A.1 Oil-spill sampling . 27
A.2 Ships, road and rail tank wagons . 27
Annex B (informative) Examples of forms . 29
B.1 Sample record form . 29
B.2 Sample transport and receipt form . 30
Bibliography . 31
European foreword
This document (EN 15522-1:2023) 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 September 2023, and conflicting national standards shall
be withdrawn at the latest by September 2023.
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 supersedes CEN/TR 15522-1:2006.
In comparison with the previous edition CEN/TR 15522-1:2006, the following technical modifications
have been made:
— added another design for a helicopter sampling device as well as some less recommended devices;
— removed ship designs, because this is only relevant for skilled sample takers that should know where
to sample on a ship.
EN 15522 is composed of two parts that describe the following:
— Part 1 on sampling, describing good sampling practice, detailing sampling equipment, sampling
techniques and the handling of oil samples prior to their arrival at the forensic laboratory;
— Part 2 giving the analytical method, which covers the general concepts and laboratory procedures of
oil spill identification, analytical techniques, data processing, data treatment,
interpretation/evaluation and reporting of results.
A list of all parts in the EN 15522 series can be found on the CEN website.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, France, Germany, Greece, Hungary, Iceland, Ireland,
Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the United
Kingdom.
Introduction
This document is composed of two parts that describe the following:
— Part 1 on sampling, describing good sampling practice, detailing sampling equipment, sampling
techniques and the handling of oil samples prior to their arrival at the forensic laboratory;
— Part 2 giving the analytical method, which covers the general concepts and laboratory procedures of
oil spill identification, analytical techniques, data processing, data treatment and interpretation/
evaluation and reporting of results.
This document specifies a forensic method for characterizing and identifying the source of oils spills in
the environment resulting from accidents or intentional discharges. The method may be used in support
of the legal process for prosecuting offenders. This method is based on the experience gained with its
former publications over the years (see [1]).
Where an oil pollution incident has occurred, samples should be collected from both the spill and,
wherever possible, the potential source of the pollutant, e.g. ship, shore side storage tank, pipeline or
vehicle, in order to assist in the identification or confirmation of the source of the spill.
The aim of this document is to give guidance on the current best practice for taking such samples.
Part 1 of EN 15522 is meant to provide general guidelines for legal oil sampling . It does not contain
details relating to all types of spill situation, however, by following these guidelines it should be possible
to collect and provide legally valid samples that can be used in the process of identifying or confirming
the source of the spill.
The issues addressed only cover the mechanics of sample collection. The command and control that may
be put in place during incident response, the authorities who may request sample collection and the
individuals who have the authority to collect samples, will vary from country to country and as a
consequence these issues are not addressed.
Legal sampling (according to Interpol Pollution Crime Forensic Investigation Manual [2]): sampling that has been conducted in
such a way that the results of its analysis can be used in a court of law. Procedures are followed to prove the chain-of-custody of
the samples and to prove that they have not been tampered with.
1 Scope
This document provides guidance on taking and handling samples related to oil spill identification in legal
proceedings. Guidance is given on obtaining samples from both the spill and its potential source.
Preservation of evidence is an essential part of legal procedures and this document presents appropriate
oil sampling procedures.
WARNING — The use of this document can 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 users of this document to take appropriate measures to ensure the safety and health of
personnel prior to the application of the standard, and to determine the applicability of any other
restrictions for this purpose.
IMPORTANT — Most countries have teams with specialists trained in sampling on board of ships. Do not
take unnecessary risks, seek assistance from such teams where available.
NOTE For the sake of clarity, the word ‘oil’ is used throughout this document. It can equally refer to crude oil,
a petroleum product or mixtures of such.
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.
EN 15522-2:2023, Oil spill identification — Petroleum and petroleum products — Part 2: Analytical method
and interpretation of results
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
3 Terms, definitions and abbreviations
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 https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1 Terms and definitions
3.1.1
chain of custody
practice of ensuring security of the sample so that no one has an opportunity to tamper with or otherwise
alter the sample or the results
Note 1 to entry: It includes chronological documentation that records the sequence of sample handling including
sampling, sealing, storage, transfer, analysis and disposal to ensure that only documented sample handlers have
direct access to the samples.
3.1.2
sample heterogeneity
non-representative or non-homogenous character of samples caused for example by variable degrees of
mixing within a tank or oil slick
3.1.3
contamination
changes in oil composition which take place during/after the spillage in either sample by addition of non-
petroleum compounds from biogenic (e.g. fat from feathers) or anthropogenic sources (e.g. compounds
from plastics)
Note 1 to entry: Mixing and contamination are used to differentiate between the addition of petroleum products
(mixing) and non-petroleum products (contamination).
3.1.4
weathering
changes in oil composition which can occur after the spillage due to environmental processes, including
evaporation, dissolution, emulsification, oxidation, biological decomposition, wax redistribution
Note 1 to entry: In situ burning will result in additional changes to oil composition.
3.1.5
bilge water
mixture including water and oil collected in the bilge of a ship as a result of leakage, drainage, etc.
3.1.6
slop
mixture of water and oil residues from cargo tanks in oil tankers that may contain oil/water emulsions,
wax, sediments and other tank residues
3.1.7
sludge
deposits, generally from the purification of fuel and lubrication oils, consisting of mixtures including oil,
wax, sand and water
3.1.8
tank washings
tank washing water containing cargo tank residues including oil, wax, sediment and other foreign matter
EXAMPLE Tank cleaning chemicals.
3.1.9
background samples
samples representing the background that can be expected in source or spill samples
Note 1 to entry: E.g. sample from the surface water close to but not contaminated by the spill, sample from the deck
just next to a contaminated part of the deck of which a sample has been taken.
Note 2 to entry: Background samples from water should, where possible, be taken in the same manner as the spill
samples (e.g. via ETFE net).
Note 3 to entry: Background (according to Interpol Pollution Crime Forensic Investigation Manual [2]: Background
(Control) sample: a sample of soil, water, air or other medium that is not believed to be impacted by the deleterious
environmental discharge and is believed to represent a “clean sample”.
3.1.10
petroleum
crude oil (pure or mixed) and all its products resulting from its distillation or processing in units of
mixtures and refining
EXAMPLES Fuels, gas oils, kerosene, gasoline, residues, solvents, etc.
3.2 Abbreviations
For the purposes of this document, the following abbreviations apply.
PE Polyethylene
ETFE Ethylene-tetrafluorethylene
PTFE Polytetrafluorethylene
PA 6.6 Polyamide 6.6
4 Principle
Samples form an important aspect of any investigation and care should be taken to ensure that they are
as representative of both the spill and the potential source as possible.
When investigating a spill, samples are usually taken from:
— the water surface (sea, river, canal or lake);
— shoreline or banks (sand, shingle, rocks and oiled animals and vegetation);
— marine or river ship’s cargo tanks, fuel tanks, waste oil tanks, slop tanks, ballast tanks, bilges, or other
(oiled) areas (e.g. deck, hull);
— land tanks and pipelines;
— road and rail vehicles.
For each type of spill, specific instructions and materials are required or advised.
All spills and potential sources are to be sampled. Sampling takes place as soon as possible and before
any cleaning operation commences.
Samples are handled as legal evidence and are kept in a chain of custody until identification and possible
legal procedure has been completed.
5 Sampling in general
5.1 General
Whenever possible sampling should occur immediately after the spill and prior to any cleaning
operations. If this is not possible avoid areas where chemical treatments have been used.
It is important to take samples from both the spill and the source even when it appears certain where the
spill originated.
Sampling procedures, which are connected to liability investigations, shall be performed in a manner that
preserves the samples' value as evidence.
ETFE is most well-known by the DuPont brand name Tefzel® and is an example of a suitable commercially
available product. An example is a Tefzel® net manufactured by SEFAR – Internet: www.sefar.com (Sefar Fluortex
Product ref. 09-150/36 or 9-250/39). This information is given for the convenience of users of this document and
does not constitute an endorsement by CEN of this product.
Sampling procedures and other suggestions in connection with sampling are briefly described in this
clause. The information given is designed to assist the sample collector in obtaining samples, which may
be used for identifying oil spills.
If samples are to be used in connection with legal proceedings, this document should be read in
conjunction with any documents issued by the regulatory authorities in the country or countries where
the spill has occurred.
These suggestions do not contain details relating to all types of spill situations, but should merely be
regarded as general guidelines. However, by following these guidelines it should be possible to collect
and provide legally valid samples that can help to determine the source responsible for the spill.
It is recommended that photographs are taken of the site being sampled to support the investigation.
5.2 Sampling schedule
It is essential that all possible sources of a spill are sampled in order to determine its origin. It is also
important that the samples are collected as soon as possible after the spill.
IMPORTANT — Unbiased spill samples shall always be taken before any cleaning operation takes place.
If a source sample is not obtained shortly after the spillage, it may be impossible to obtain a relevant
sample at a later date. This can render the analyses of the spill samples useless with respect to the
determination of the source responsible for the spill.
If any part of the spill differs in any respect from other parts, extra samples shall be taken to check if more
than one spill has occurred in the area.
If the spill response operation continues for more than one day, samples should be taken every day to
make it possible to determine the degree of weathering of the oil, as well as possible contamination by
other oils.
Nevertheless, this frequency can be adapted according to the situation and to the response time and
clean-up of the site, but at least one sampling per week for long periods is recommended, or at least to
make sure to have enough samples for legal processing.
If an oil sample is suspected to be contaminated with material already in the water, on the deck or on the
hull etc., also take samples including the ‘contaminant’. E.g. waters in harbours and estuaries may contain
traces of various petroleum products and when spills in such waters are sampled it is therefore important
to provide the laboratory with background samples of the water.
5.3 Types of sample
The following types of oil or oily mixture can occur at spill sites and shall then be sampled:
— oil, oily water, heavily emulsified oil, tar balls or lumps on the water surface;
— mixtures of oil and sorbents or other materials which are soaked with oil;
— mixtures of oil and foreign materials on beaches;
— surfaces, rocks, quays, plants, sand, sediments and soil contaminated with oil;
— oiled animals on the water surface or on beaches.
Background (according to Interpol Pollution Crime Forensic Investigation Manual [2]: Background (Control) sample: a sample
of soil, water, air or other medium that is not believed to be impacted by the deleterious environmental discharge and is believed
to represent a “clean sample”.
The following types of oil or oily mixture can occur at suspected sources and shall then be sampled:
— pure oil in ships, offshore constructions or land facilities;
— oily water in bilges and slop tanks on board ships;
— oily sludge in sludge tanks on board ships.
When relevant, the following types of additional samples should be sampled:
— background samples from the engine, deck, hull, water, beach, etc. when possible.
Oil wiped with an ETFE net (see 3.2) from a deck may contain contaminants from the deck. Therefore, an
additional sample should be taken by wiping a “clean” part of the deck next to the spill location with a
clean ETFE net.
NOTE 1 Where ETFE is written this can apply equally to PTFE.
— counter samples.
Laws can be different in European countries, but in general the potential offender has the right of defence
and can ask for a second set of samples to be analysed in a laboratory of choice (see 9.3).
NOTE 2 Witnessing can be agreed, as an alternative for counter samples. Witnessing is common between
commercial laboratories on request of insurance companies. There are, for example, many commercial laboratories
specialized in the analysis of physical properties of petroleum or petroleum products, but not in oil spill
identification. An analyst of such a laboratory can be asked to witness the unsealing, sample preparation, sample
analysis and sample evaluation of an oil case. When results been obtained according to the appropriate protocols,
the witness can indicate this, including remarks, on the final oil case report.
5.4 Sample volume
In general, samples should be taken from the thickest oil accumulations. Whenever possible each sample
should contain between 10 ml and 100 ml of oil. Should that be impossible, even extremely small amounts
of oil can be considered for laboratory analysis.
IMPORTANT — While analyses can be undertaken on very small samples they may be overly affected by
weathering and hence less representative. Taking sufficient sample material is therefore strongly
recommended.
It may be difficult to acquire visible traces of oil in the sample when collecting from very thin oil films on
the water surface. The use of ETFE nets is strongly recommended for sampling such oil films because the
oil sticks to the net and can therefore be collected from a larger area.
If ETFE nets are not available water samples shall be collected. Even when only small amounts of oil are
visible in a sample, or there is oil odour, sufficient material may be present for the laboratory to analyse.
5.5 Number of samples to be taken
The collection of several samples from the spill area is strongly recommended. A minimum of two
samples should be collected, even in small spills. The distance between the sampling positions should aid
documenting the total range and distribution of the spill.
Be aware that the composition of the oil may have varied during the spillage, or that more than one source
caused the spill.
It may be sufficient to take only one source sample from any single sampling point on-board a ship or
offshore/land-based installation. If required for administrative reasons (e.g. counter samples), more than
one sample may be taken from each sampling point.
However, if there is any suspicion of sample inhomogeneity indicated by different texture/colours, e.g.
on the water surface, on rocks and beaches, in bilges and sludge tanks, at least two, if necessary more,
samples should be taken to cover the variance in composition of the samples.
Samples should also be collected from background environments (engine, deck, hull, water, beach, etc.)
whenever relevant, in order to determine whether the spilled oil has been contaminated by an earlier
spill or other organic material.
6 Precautions against contamination of samples during collection
6.1 General
It is critical to take precautions to prevent contaminating the samples during collection. Disposable nitrile
gloves should be worn. Sampling equipment will ideally be disposable due to challenges of thoroughly
cleaning oiled equipment in the field. If equipment has to be reused, great care needs to be taken to ensure
that it is thoroughly cleaned and stored appropriately prior to further use.
6.2 Potential sources of contamination
Avoiding contamination of the samples during sampling is essential. All the following possible sources of
contamination should be considered and the appropriate control applied if necessary. These are:
— residue of earlier samples remaining on sampling containers, funnels, scoops, spatulas and other
equipment;
— material from the site during sampling;
— residual water in or on ropes, chains or extension handles;
— dust or dirty water on the container closure;
— hands and gloves;
— transport and general handling.
6.3 Controls
Contamination can be minimized by taking the following appropriate action:
— check that the equipment is clean;
— ensure that samples are taken without the sampling location having been otherwise
disturbed/altered beforehand;
— store containers and closures in a clean environment;
— avoid touching the material to be sampled with fingers, hands or gloves.
If contamination is suspected this should be reported and if possible, a fresh sample should be collected.
7 Sampling equipment and sample containers and closures
7.1 Introduction
It should be noted that some of the equipment specified may only be available from specialist sources. It
is recommended that sampling kits should be prepared and readily available.
A description of the contents of suitable sampling kits is given in Annex A, [3] and [4].
It might be useful to contact the laboratory to which you normally send your samples and ask for
assistance and advice.
7.2 General instructions and strategies
Samples shall be taken and placed in containers that will ensure their safety and integrity during
transport to the laboratory and storage prior to analysis. All sampling devices, containers and closures
should be designed and constructed to maintain the initial characteristics of the material being sampled.
Their cleanliness should be confirmed before use.
7.3 Sample containers, closures and packages
Sampling containers should be made from inert materials (e.g. glass, PTFE, PA). They need openings of a
sufficient size to accommodate the material being sampled and should be fitted with inert lined (e.g.
PTFE) lids.
Metal closures, corks and rubber bungs should not be used as these may either react with, or contaminate,
the material being sampled.
The capacity of the container will be dependent on the material being sampled and will usually be 100 ml
to 500 ml. Larger wide mouth air-tight containers may be necessary to sample tar-balls (see 8.3).
During sampling, care shall be taken not to switch lids between sampling containers to prevent cross-
contamination. For this purpose, it is advisable to mark not only the container with the individual sample
ID code, but also the lid.
Plastic sample bags and containers should be avoided for oil forensic sampling, because components from
the plastic material may migrate into the oil and interfere with the analysis.
NOTE Plastics in general interact with oil samples. Tested exceptions are products made from Nylon® (poly
amide(PA)), Teflon® (polytetrafluoroethylene (PTFE)) and Tefzel® (ethylene-tetrafluoroethylene (ETFE)) .
Non-PA Polyamide, PTFE or ETFE plastic containers or bags may be used as a last resort. However, doing
so may call into question the sample validity when used as evidence in court proceedings.
Depending on the means of transportation and storage, secondary packaging and additional cooling of
the sample containers may be required. Plastic bags or boxes in which the sample container can be sealed
should be of sufficient strength and size to accommodate the sample(s) and retain its sealed condition
during transportation.
Samples have to be sealed (directly or in the secondary packaging). Sealing of samples is a key procedure
for legal sampling.
Plastic or cardboard boxes that can be sealed may be used for transporting the samples (be aware
cardboard may soak through if using cooling pads/cool packs etc.). If the samples are to be transported
by air, the packages should conform to all the necessary regulatory requirements and be International
Aviation Transport Association (IATA) approved.
The containers shall be clearly, unambiguously and uniquely labelled and sealed so that they cannot be
opened without breaking the seal.
Nylon®, Teflon® and Tefzel® are examples of suitable products available commercially. This information is given for the
convenience of users of this document and does not constitute an endorsement by CEN of this product.
7.4 Sample devices
7.4.1 General
In all situations, when possible, ETFE nets should be used. ETFE does not contaminate the samples and
can readily be extracted in the laboratory with a solvent, without contaminating the extract. To ensure
that all ETFE nets used for oil spill forensics are free of contamination and any traces of oil, they should
be checked as part of quality assurance at the laboratory. Alternatively, the laboratory may provide pre-
checked ETFE nets.
Both ETFE and oil are non-polar and hydrophobic and are attracted to each other. Therefore, oil can be
collected from the water surface by sweeping an ETFE net through the (thin) oil layer. The net can also
be used to wipe oil from objects, e.g. engines, deck, hull, rocks, feathers.
NOTE ETFE nets do not float on water so they will sink slowly.
7.4.2 For sampling oil layers and oil sheens from water surfaces
For sampling, use an ETFE net approximately 200 mm by 300 mm or 150 mm by 200 mm, fixed to a rod
and line by means of a disposable stainless steel clip (see Figure 1).
The impact of weathering between the moment of spillage and sampling cannot be undone. Therefore, to
ensure the analytical outcome even in cases of weathered spills, take several samples from sheens on
water with ETFE nets, collecting as much oil as possible. Do not add water to the glass bottle in which the
net is stored. Water contains bacteria that will reduce compounds in the sample.
If it appears that no oil has been collected by the net, a second sample by ETFE net can be taken to secure
the results.
Figure 1 — ETFE net fixed to a rod and line with a disposable stainless steel clip
7.4.3 For sampling ship’s cargo tanks, bunker tanks and bilges, barges, road tankers, shore tanks
and pipelines
Use sampling equipment, containers and closures as specified in EN ISO 3170 (see also [3] and [4]).
For sampling bunker tanks from the deck using sounding pipes, use a thick-walled brass tube less than
25 mm in diameter containing a 10 ml glass tube. The brass tube is fitted with a ring to enable attachment
to a measuring tape. The brass tube should be constructed with an asymmetric end that ensures that it
ETFE is most well-known by the DuPont brand name Tefzel® and is an example of a suitable commercially available product.
An example is a Tefzel® net manufactured by SEFAR – Internet: www.sefar.com (Sefar Fluortex Product ref. 09-150/36 or 9-
250/39). This information is given for the convenience of users of this document and does not constitute an endorsement by
CEN of this product.
lies horizontally when touching the tank bottom and should be of sufficient weight to allow it to sink into
viscous oils (see Figure 2).
Key
x 10 ml glass tube
y thick-walled heavy brass tube
Figure 2 — Thick-walled brass tube
7.4.4 For sampling waterborne oil layers greater than 1 mm thickness
Use a disposable polyethylene (PE) cornet suspended from a metal ring (in aluminium, 25 cm – 30 cm in
diameter) fixed to an aluminium pole, having a 10 mm to 15 mm hole in its base to allow the liquid to
drain in a controlled manner (see Figure 3).
Key
A PE cornet D pole
B metal ring E hole
C holder
Figure 3 — PE cornet
7.4.5 For sampling waterborne very viscous oil layers
Use a clean metal (preferably aluminium, copper or stainless steel) pipe or rod, and swipe it through the
oil layer in order to get a representative layer of oil on the rod. Wipe the oil from the rod with an ETFE
net and store it in a glass/PTFE container or a Nylon® bag. Instead of a massive rod, a pipe can be used
when the end is closed to prevent that the inside is or becomes contaminated.
When the oil does not stick to the rod, use the following alternatives:
— the PE cornet, see Figure 3,
— a clean plastic bucket (single-use), or
— an aluminium foil container (single-use).
The bucket may be used to sweep up the oil water mixture and then the viscous oil can be sampled from
the bucket by ETFE net or spatula.
The aluminium foil container may be punctured before use and be used to drain the water away after
sampling the oil water mixture, retaining the viscous oil, which then can be collected by ETFE net or
spatula or even be transported in the aluminium container (wrapped in further packaging).
7.4.6 Helicopter sampling devices
Several sampling devices are used internationally. Some examples are shown below.
Figure 4 shows a helicopter-sampling device, which makes use of a PE fastener, holding two PE bottles as
floating bodies and a glass bottle for sampling.
Key
1 polyethylene-block with 3 threads 3 glass-bottle (open)
2 polyethylene-bottles (closed) 4 opening
5 metal wire for the line
Figure 4 — Helicopter sampling device
Due to the buoyancy of the three empty bottles, the sampling device initially floats horizontally on the
water’s surface, so that both the water and the surface layer film of oil can flow into the sampling bottle
(3 in Figure 4). While filling, this bottle sinks down and directs the opening upwards, so that water can
no longer flow into or out of the bottle.
Alternatively, the glass bottle (3 in Figure 4) in the sampling device can be substituted with a PTFE tube,
screwed onto the PE block. A folded ETFE net (Figure 5 C, approximately 10 cm × 25 cm) is placed inside
the PTFE tube secured by metal clips. See Figure 5 A and B for the modified sampling device.
Following sampling the PTFE tube, complete with the ETFE net, is removed from the PE-block, sealed in
a plastic bag and sent chilled to the laboratory for analysis. As the ETFE net remains within the PTFE tube
it avoids contamination via contact with the plastic bag.
Key
A & B modified sampling device
C folded EFTE net
Figure 5 — Modified helicopter sampling device
Another design of a helicopter-sampling device uses a floating aluminium body to which an ETFE net is
attached (see photos Figure 6). This sampler is very slim and can be transported to the sampling site pre-
assembled in a pre-cleaned container. After sampling, the oiled ETFE net is detached from the sampler’s
body and transferred into a clean wide-neck glass bottle with a PTFE lined lid. The oiled aluminium body
is returned to the container to avoid cross-contamination.
Figure 6 — Pre-assembled helicopter-sampling device beside (left) and packed in transport
container (right)
7.4.7 Less suitable sampling devices
Some time-honoured sample strategies can be used, when no other equipment is available, but they have
considerable drawbacks:
Wooden material (spatula; clothes-peg):
— soaks up oil;
— is not cleanable;
— might lead to cross contamination.
Taking watery oil samples by skimming a bottle over the water surface:
— not much oil in the bottle, but a lot of water;
— possible secondary weathering in the bottle during holding time;
— more effort for the laboratory;
— a lot of oil on the outside of the bottle, which has to be cleaned (which rarely works completely);
— resulting in a lot of oily waste and probably NOT in a clean bottle;
— labels get oily or don’t attach to the glass properly;
— risk of cross-contamination during handling/transport;
— risk
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