Characterization of waste - Sampling of waste from extractive industries

This Technical Report gives additional and specific information on sampling for testing of waste from the extractive industry to support the development of appropriate sampling plans. This supplementary guidance to EN 14899 is required because waste from the extractive industry differs considerably from the waste types and sampling scenarios covered in the existing technical reports (CEN/TR 15310-1 to -5) that support the Framework Standard. This guidance document should be used in conjunction with EN 14899 and its supporting technical reports CEN/TR 15310-1 to -5. The approach to sampling described in this document is primarily focused on the requirements to undertake mineralogical and geochemical testing of the waste. Whilst much of the background information provided is also relevant to geotechnical investigations there may be important additional requirements or differences in approach for determining relevant physical parameters. For example, many geotechnical parameters are determined using field tests, which are not discussed in this document. References to alternative source documentation are provided. The guidance provided in this document applies only to above-ground exposure to radio-nuclides present in the undisturbed earth crust and not to the production, processing, handling use, holding, storage, transport, or disposal of radioactive substances that are or have been processed for their radioactive, fissile or fertile properties. This Technical Report provides some discussion of current best practice, but is not exhaustive. To clarify the text, the document provides a number of worked examples in the Annexes.

Charakterisierung von Abfällen - Probenahme von Abfällen aus der mineralgewinnenden Industrie

Caractérisation des déchets - Echantillonnage des déchets issus des industries extractives

Karakterizacija odpadkov - Vzorčenje odpadkov iz industrije bogatenja mineralnih surovin

To tehnično poročilo podaja dodatne in specifične informacije o vzorčenju za preskušanje odpadkov iz industrije bogatenja mineralnih surovin, da se podpre razvoj ustreznih načrtov vzorčenja. Ti dodatni napotki k standardu EN 14899 so potrebni zato, ker se odpadki iz industrije bogatenja mineralnih snovi znatno razlikujejo od vrst odpadkov in primerov vzorčenja, opisanih v obstoječih tehničnih poročilih (CEN/TR 15310-1 do -5), ki podpirajo okvirni standard. Ta dokument z napotki naj bi se uporabljal skupaj s standardom EN 14899 in z njegovimi podpornimi tehničnimi poročili CEN/TR 15310-1 do -5. Pristop k vzorčenju, opisan v tem dokumentu, se osredotoča predvsem na zahteve za izvajanje mineraloških in geokemičnih preskusov odpadkov. Velik del podanih dodatnih informacij velja tudi za geotehnične raziskave, vendar lahko obstajajo pomembne dodatne zahteve ali razlike v pristopu za ugotavljanje ustreznih fizičnih parametrov. Številni geotehnični parametri se na primer določijo s terenskimi preskusi, ki jih ta dokument ne obravnava. Podani so sklici na dokumentacijo iz drugih virov. Smernice iz tega dokumenta se uporabljajo samo za nadtalno izpostavljenost radionuklidom, ki so prisotni v nemoteni zemeljski skorji, ne pa tudi za proizvodnjo, predelavo, ravnanje, uporabo, zadrževanje, shranjevanje, prevoz ali odstranjevanje radioaktivnih snovi, ki se predelujejo ali so se predelovale zaradi svojih radioaktivnih, cepljivih ali oplodnih lastnosti. To tehnično poročilo vsebuje razpravo o sedanjih najboljših praksah, vendar ta razprava ni izčrpna. V dodatkih dokumenta so za pojasnitev besedila navedeni številni delujoči primeri.

General Information

Status
Published
Public Enquiry End Date
29-Feb-2012
Publication Date
26-Dec-2012
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Nov-2012
Due Date
25-Jan-2013
Completion Date
27-Dec-2012

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SLOVENSKI STANDARD
SIST-TP CEN/TR 16365:2013
01-januar-2013
.DUDNWHUL]DFLMDRGSDGNRY9]RUþHQMHRGSDGNRYL]LQGXVWULMHERJDWHQMDPLQHUDOQLK
VXURYLQ
Characterization of waste - Sampling of waste from extractive industries
Charakterisierung von Abfällen - Probenahme von Abfällen aus der mineralgewinnenden
Industrie
Caractérisation des déchets - Echantillonnage des déchets issus des industries
extractives
Ta slovenski standard je istoveten z: CEN/TR 16365:2012
ICS:
13.030.10 Trdni odpadki Solid wastes
SIST-TP CEN/TR 16365:2013 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 16365:2013

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SIST-TP CEN/TR 16365:2013


TECHNICAL REPORT
CEN/TR 16365

RAPPORT TECHNIQUE

TECHNISCHER BERICHT
October 2012
ICS 13.030.10; 73.020
English Version
Characterization of waste - Sampling of waste from extractive
industries
Caractérisation des déchets - Echantillonnage des déchets Charakterisierung von Abfällen - Probenahme von Abfällen
issus des industries extractives aus der mineralgewinnenden Industrie


This Technical Report was approved by CEN on 13 May 2012. It has been drawn up by the Technical Committee CEN/TC 292.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16365:2012: E
worldwide for CEN national Members.

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SIST-TP CEN/TR 16365:2013
CEN/TR 16365:2012 (E)
Contents
Foreword .3
Introduction .4
1 Scope .6
2 Key elements of a sampling plan .6
2.1 General .6
2.2 Identify involved parties (EN 14899:2005, 4.2.1) .6
2.3 Identify general objectives (EN 14899:2005, 4.2.2) .8
2.4 Collect background information and undertake field inspection (EN 14899:2005, 4.2.5) .8
2.4.1 General .8
2.4.2 Existing information .8
2.4.3 Field inspection .9
2.4.4 Analogous sites . 10
2.5 Determine specific objectives and corresponding level of testing (EN 14899, 4.2.3) . 10
2.5.1 Introduction . 10
2.5.2 Determine the level of testing . 11
2.5.3 Determine the required number and size of samples . 13
2.6 Identify constituents to be tested (EN 14899:2005, 4.2.4) . 14
2.7 Identify health and safety precautions (EN 14899:2005, 4.2.6) . 14
2.8 Select sampling approach (EN 14899:2005, 4.2.7, and CEN/TR 15310-1:2006, Clause 4) . 15
2.8.1 General . 15
2.8.2 Determine the practical instructions . 23
2.9 Identify the most appropriate sampling technique (EN 14899:2005, 4.2.8, and
CEN/TR 15310-2) . 29
3 Sample handling in the field . 33
3.1 General . 33
3.2 Sub-sampling . 34
3.3 Sample preparation and storage (CEN/TR 15310-4). 35
3.3.1 General . 35
3.3.2 Packaging . 35
3.3.3 Preparation and storage . 36
3.4 Transport the sample to the laboratory (EN 14899:2005, 5.2, and CEN/TR 15310-4) . 37
4 Documentation (long and short form of sampling plan) . 37
4.1 Document the sampling plan and produce instructions for the sampler (EN 14899:2005,
Clause 6) . 37
4.2 Produce a field sampling record (EN 14899) . 37
5 Sampling (EN 14899:2005, 5.1) . 38
6 Sampling uncertainty and other issues . 39
Annex A (informative) Example sampling plans for waste characterization for exploration,
operation and closure stages of extractive industries . 40
A.1 General . 40
A.2 Example detailed sampling plan for exploration stage . 40
A.3 Example short form sampling plan for exploration/ permitting stage . 47
A.4 Operation stage – Simple system – Aggregate quarry . 49
Annex B (informative) Example sampling record . 53
Bibliography . 54

2

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SIST-TP CEN/TR 16365:2013
CEN/TR 16365:2012 (E)
Foreword
This document (CEN/TR 16365:2012) has been prepared by Technical Committee CEN/TC 292
“Characterization of waste”, the secretariat of which is held by NEN.
The preparation of this document by CEN is based on a mandate by the European Commission (Mandate
M/395), which assigned the development of standards on the characterization of waste from extractive
industries.
This Technical Report is intended to supplement the existing series of five Technical Reports dealing with
sampling techniques and procedures for waste, and provides specific information for sampling of waste from
the extractive industry. It follows the principles laid down in EN 14899, Characterization of waste  Sampling
of waste materials  Framework for the preparation and application of a Sampling Plan. Further information
on the relationship between the production of a sampling plan and the overall testing programme objectives
can be found in CEN/TR 15310-5.
 CEN/TR 15310-1, Characterization of waste — Sampling of waste materials — Part 1: Guidance on
selection and application of criteria for sampling under various conditions;
 CEN/TR 15310-2, Characterization of waste — Sampling of waste materials — Part 2: Guidance on
sampling techniques;
 CEN/TR 15310-3, Characterization of waste — Sampling of waste materials — Part 3: Guidance on
procedures for sub-sampling in the field;
 CEN/TR 15310-4, Characterization of waste — Sampling of waste materials — Part 4: Guidance on
procedures for sample packaging, storage, preservation, transport and delivery;
 CEN/TR 15310-5, Characterization of waste — Sampling of waste materials — Part 5: Guidance on the
process of defining the sampling plan.
This Technical Report focuses mainly on sampling for geochemical rather than geotechnical requirements.
Sampling for geotechnical requirements is only addressed to a limited extent and references are made to
existing documentation. The Technical Report elaborates on a range of potential approaches and tools of
specific relevance to the sampling and testing of wastes from the extractive industry. This approach enables
the project manager to tailor his sampling plan to a specific testing scenario and continues the ‘shop shelf’
approach to sampling plan development for waste testing outlined in CEN/TR 15310-1 to -5. This approach
allows flexibility in the selection of the sampling approach, sampling point, method of sampling and equipment
used. It provides the necessary background information pertaining to the factors that influence the choice of
these detailed components of the sampling exercise, and information on the necessary statistical choices that
can then be applied to determine the most appropriate testing programme for any given sampling scenario.
This Technical Report also makes references to the overall guidance document for characterization of waste
from extractive industries (CEN/TR 16376) which gives guidance and recommendations on the application of
methods for the characterization of waste from extractive industries.
3

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Introduction
The guidance outlined in this Technical Report is focused on the key elements to be considered in the
development of a sampling plan for extractive waste. This report should be used in conjunction with EN 14899
and its supporting technical reports and is intended to supplement the information contained in these
documents with specific and essential information relevant to the sampling of waste from the extractive
industry. Where appropriate this report also makes reference to the overall guidance document for
characterization of waste from extractive industries (CEN/TR 16376) which gives guidance and
1)
recommendations on the application of methods for the characterization of waste from extractive industries .
1) Specific features of extractive waste
The extractive industry includes, metal mines, rock quarries, salt mines, coal mines, sand and gravel,
limestone and onshore oil and gas operations. When mineralogical material is extracted it is exposed to
changes in physico-chemical conditions, which may result in chemical and physical instability of previously
stable geological material.
The life cycle of extractive industries starts with the early phase of exploration through operation to closure
and after care. In the context of sampling three phases have been defined in this document:
 exploration (including design and permitting);
 operation (extraction and processing, including transport and deposition of waste); and
 closure (including existing waste deposits).
From a sampling perspective different sampling scenarios may be more relevant than the operational phases.
For example sampling from diamond drill cores may take place both during exploration and operation,
sampling at existing waste rock dumps and tailings facilities may take place both during operation and at
closed sites. Both operational phases and sampling scenarios are used as parallel concepts in this document.
One significant feature that makes characterization of extractive waste different from waste characterization in
general is the fact that sampling and characterization ideally take place before the waste is produced, i.e.
based on drill cores (or drill mud) from exploration drilling. Characterization during exploration is critical since
subsequent waste management plans are developed on the basis of this information. However, the availability
of material for sampling and characterization at the exploration stage is commonly limited which means that
follow-up checks to ensure that the initial data and interpretation are correct will often be needed during
operation. If pilot scale tests, extraction and/or processing, are carried out this will have the added benefit of
producing a larger number of potential samples for sampling and testing as well as giving the opportunity to
sample process waste, i.e. tailings. While the majority of waste is commonly produced during the operation
phase of a mine, waste characterization needs to be considered for all phases of the mine life.
The operational phase of a mine or quarry encompasses all the activities from mineral deposit development to
detailed planning for closure. There are two main waste streams from the production process that need to be
characterised, i.e. waste material generated as part of the extraction that will not go through mineral
processing and the waste produced during processing. The waste produced prior to mineral processing will
primarily be waste rock separated at the excavation front. In a hard rock mine, sampling may be done before
blasting from drill cores, or after blasting. After mineral processing the waste will primarily be tailings (i.e. tail
end of the process), and samples may be collected from pipelines, discharge trenches or conveyer belts.
Extractive waste may contain chemicals added as part of the production process. Normally, if not recovered
for construction purposes, all extractive waste is deposited on site.

1) As defined in Directive 2006/21/EC.
4

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This guidance is also applicable for sampling from closed sites in case sampling and testing of waste is
required. Sampling at closed sites, including abandoned historic mine-sites, may in some cases require
specific approaches e.g. due to accessibility and limited background information.
NOTE Given the great variety of waste types, sampling situations and objectives, this Technical Report cannot
provide definitive instructions that cover all scenarios. Instead, it discusses the basic considerations to be followed, and
provides guidance on selection of sampling approaches that might be relevant to the three principle phases of a mine:
1) Exploration, 2) Operation and 3) Closure. Sampling of existing waste deposits at mines that are still in operation would
be very similar to Scenario 3) Closure.
2) Document structure
The structure of this sampling guideline is based on the concepts and procedural steps outlined in Figure 2 of
EN 14899:2005 and subsequent subclauses, with some additions to address specific features of the extractive
industry.
Clause 2 key elements of a sampling plan, is the core of this guidance document. This clause is divided into
ten sub-sections that describe the steps of developing sampling plans, from defining the involved parties to
describing the sampling techniques. It lists possible objectives for the different stages of the extractive waste
characterization, background information that may be available, explains generic levels of testing and
describes sampling approaches and techniques.
5

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SIST-TP CEN/TR 16365:2013
CEN/TR 16365:2012 (E)
1 Scope
This Technical Report gives additional and specific information on sampling for testing of waste from the
extractive industry to support the development of appropriate sampling plans. This supplementary guidance to
EN 14899 is required because waste from the extractive industry differs considerably from the waste types
and sampling scenarios covered in the existing technical reports (CEN/TR 15310-1 to -5) that support the
Framework Standard. This guidance document should be used in conjunction with EN 14899 and its
supporting technical reports CEN/TR 15310-1 to -5.
The approach to sampling described in this document is primarily focused on the requirements to undertake
mineralogical and geochemical testing of the waste. Whilst much of the background information provided is
also relevant to geotechnical investigations there may be important additional requirements or differences in
approach for determining relevant physical parameters. For example, many geotechnical parameters are
determined using field tests, which are not discussed in this document. References to alternative source
documentation are provided.
The guidance provided in this document applies only to above-ground exposure to radio-nuclides present in
the undisturbed earth crust and not to the production, processing, handling use, holding, storage, transport, or
disposal of radioactive substances that are or have been processed for their radioactive, fissile or fertile
properties.
This Technical Report provides some discussion of current best practice, but is not exhaustive. To clarify the
text, the document provides a number of worked examples in the Annexes.
2 Key elements of a sampling plan
2.1 General
The sampling plan identifies the appropriate and practical activities required to achieve the set objectives of
the characterization testing programme. The purpose of a sampling exercise shall be clearly understood by
the sampler. The development of a sampling plan helps to ensure that the objectives of any waste testing
programme are consistently met and is crucial for cost effective and appropriate sampling. The sampling plan
provides traceability which can be used to validate the data produced. This is especially important where new
datasets will be generated over time.
The framework standard EN 14899 identifies a process flow chart that defines the essential elements of a
sampling plan and how those elements are linked. The basic steps identified in this flow chart have been
followed in this supplementary guidance, with some minor changes (see Figure 1) to account for specific
circumstances of the extractive industry. The flow chart indicates a step by step process to sampling plan
development, although in reality they may be considered out of order. Some elements of the sampling plan
may be prepared in parallel and iterations may be necessary. Additional information is provided in the
following sections that are specific to the extractive industry.
It is important to recognise that characterization may often be an iterative process. The sampling plan may
initially be developed for screening purposes and may then form the basis of a characterization study. The
characterization study may require testing of samples previously collected but not subjected to testing or form
the basis for collection of more samples required for more comprehensive testing all specified in the sampling
(Figure 1).
Characterization of waste from a quarry may be relatively simple in comparison to wastes from metal
extraction. However, generating a sampling plan using the outline approach advocated in this guidance
document is still recommended. Development of a comprehensive sampling plan will facilitate discussions
with stakeholders, and it may help the operator to identify issues that may require consideration.
2.2 Identify involved parties (EN 14899:2005, 4.2.1)
It is recommended that sampling plans for a given site and phase of operation are, where possible, discussed
with involved parties prior to any sampling taking place. It is important to identify and include parties with an
6

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SIST-TP CEN/TR 16365:2013
CEN/TR 16365:2012 (E)
interest at an early phase in the testing programme. This may include e.g. people from different parts of the
organisation of the operator, consultants, regulators and local stakeholders. This approach may avoid or
minimise confusion at a later date and facilitate acceptance from involved parties. Well-communicated
sampling plans may provide confidence that the results generated from the sampling and testing programme
will be valid.

The numbers in the chart refer to the clauses within this document.
Figure 1 — Flowchart of sampling plan modified from Figure 2, EN 14899:2005
7

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SIST-TP CEN/TR 16365:2013
CEN/TR 16365:2012 (E)
2.3 Identify general objectives (EN 14899:2005, 4.2.2)
The overarching objectives of a testing programme define the type and quality of information required from
sampling and analysis. During the various phases in the life of a mine there may be more than one objective
and therefore a need for more than one sampling plan. Whilst the overall objective can be identified prior to
any background data collection and on-site investigation the technical objectives can usually only be set once
this information has been gathered.
Example overarching objectives may be to contribute data to:
 design a waste facility;
 development of a waste management plan;
 design/evaluation of closure options;
 design/evaluation of management options for abandoned sites.
The overall guidance document (CEN/TR 16376) includes a discussion on when and why characterization
may be needed and the context within which characterization data may need to be applied. However, it does
not cover information on how to apply these characterization results, e.g. for dam design or closure planning.
For guidance on how to use characterization results correctly for predictive modelling or design purposes
references are made to other sources of information.
2.4 Collect background information and undertake field inspection (EN 14899:2005, 4.2.5)
2.4.1 General
It is essential to obtain pertinent background information to develop good sampling plans for future, existing,
closed and abandoned facilities. The background information allows the development of clear and precise
instructions for sampling. Background information can be divided into three categories: existing information
including site background information; field inspection information; and analogous geology. These three
categories are discussed in the following clauses.
2.4.2 Existing information
Obtaining background information on a proposed extractive operation and collating this information to feed
into the development of a testing program and sampling plan is essential when defining appropriate detailed
objectives for sampling and testing. Careful inclusion of valid prior information can greatly reduce the cost per
unit of error and dramatically reduce the size of the samples required. Relevant existing information may
include data from previous exploration work as well as investigations carried out for other land uses or local
data on background concentrations of key constituents in soils surface waters.
The use of existing information would typically be complemented by a field visit. It is important to emphasise
that although existing data may be very useful, its relevance should be evaluated prior to using the data in any
decision making process. If data is available from previous sampling programmes, the evaluation of suitability
would include looking at the:
1) type of sampling undertaken;
2) consistency of test data and analytical procedures used;
3) objectives of previous sampling and testing.
If a site moves from exploration to operation a new sampling plan will need to be developed and the waste
characterization data used for design and permitting will then become the background information for the
operation stage.
8

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CEN/TR 16365:2012 (E)
The overall guidance document (CEN/TR 16376:2012, Clause 5) gives further recommendations on site
background information that may be useful.
2.4.3 Field inspection
A field inspection provides valuable information on local conditions, e.g. any access restrictions that may
impact upon the planned sampling approach e.g. appropriate selection of sampling points. The information
that may be gathered by a field inspection will be very different for an exploration site compared to an on-
going operation or a closed waste facility. Examples of information that should be collected include:
a) Exploration
1) topography, accessibility;
2) geology;
3) mineralogy/iron phases in drilling material, overburden and exposed bedrock;
4) relevant environmental factors.
b) Operation
1) accessibility;
2) geology;
3) mineralogy/iron phases;
4) additives;
5) grain size variation;
6) erosion features and slumping;
7) excavation and transport methods;
8) material type (tailings, waste rocks);
9) potential hazards;
10) relevant environmental factors.
c) Closure and closed sites
1) accessibility;
2) geology;
3) mineralogy/iron mineral phases;
4) seepage/seepage colour and possible field measurements of seepage;
5) water/air erosion features at disposal facilities;
6) grain size variation;
7) slumping;
9

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8) potential hazards;
9) relevant environmental factors.
Signs of water and air erosion, especially on tailings, can indicate, to some degree, the extent to which the
waste material has been transported from its original position. The following information can be used to
identify the area to be sampled.
 erosion features;
 aeolian transport of tailings from original deposit;
 stability of existing tailings and waste rocks.
Mapping the deposit mineralogy and the presence of iron phases (for sulfide containing mineralisation) is an
essential part of evaluating the risks associated with current and future waste from the site. The mineralogy
rather than the bulk chemistry provides a first indication of potential drainage quality, acid generating minerals,
and neutralizing minerals. If the rocks have been exposed to air and water variations (where groundwater is
being lowered due to pumping) over short or long periods, secondary minerals may give an indication of how
the waste will behave when it is subsequently exposed to air and water.
The type of processing and use of additives, and type of waste being generated will give an indication of the
type of analyses that may be necessary and define health and safety precautions during sampling and
handling of the samples. If first evaluation indicates that there is a potential for acid/neutral rock drainage
(A/NRD) or leaching from tailings, it may be necessary to obtain samples from a pilot processing plant.
The presence of seepage, colour and field measurements of the seepage, aid in defining, for example, the
level of testing and type of analysis. These observations and field measurements give an indication of the
oxidation reactions and leaching taking place within the waste material. For example:
 Drainage pH and total dissolved solids may indicate if there is already A/NRD or alkaline drainage from
existing waste dumps or from the mineralization of in situ outcrops.
 Colour of drainage water or waste rock may provide an indication of A/NRD or alkaline drainage and the
rock’s neutralizing potential and reactivity. The colours yellow, orange, red, brown are commonly linked
with different iron phases precipitated as a result of acid drainage.
2.4.4 Analogous sites
During evaluation of background information it may be possible to identify where the mineral deposit has
analogous sites with information. Information from the analogous sites may be used to identify key issues and
help focus the sampling plan on relevant as
...

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 16365:2012
01-februar-2012
.DUDNWHUL]DFLMDRGSDGNRY9]RUþHQMHRGSDGNRYL]LQGXVWULMHERJDWHQMDPLQHUDOQLK
VXURYLQNLYVHEXMHMRVXOILG
Characterization of waste - Sampling of waste from extractive industries
Charakterisierung von Abfällen - Ergänzung zur CEN/TR 15310-Reihe um einschlägige
Beispiele aus der mineralgewinnenden Industrie
Caractérisation des déchets - Echantillonnage des déchets issus des industries
extractives
Ta slovenski standard je istoveten z: FprCEN/TR 16365
ICS:
13.030.10 Trdni odpadki Solid wastes
kSIST-TP FprCEN/TR 16365:2012 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
kSIST-TP FprCEN/TR 16365:2012

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kSIST-TP FprCEN/TR 16365:2012


TECHNICAL REPORT
FINAL DRAFT
FprCEN/TR 16365
RAPPORT TECHNIQUE

TECHNISCHER BERICHT

January 2012
ICS 13.030.10; 73.020
English Version
Characterization of waste - Sampling of waste from extractive
industries
Caractérisation des déchets - Echantillonnage des déchets Charakterisierung von Abfällen - Probenahme von Abfällen
issus des industries extractives aus der mineralgewinnenden Industrie


This draft Technical Report is submitted to CEN members for Technical Committee Approval. It has been drawn up by the Technical
Committee CEN/TC 292.

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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.

Warning : This document is not a Technical Report. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a Technical Report.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TR 16365:2012: E
worldwide for CEN national Members.

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kSIST-TP FprCEN/TR 16365:2012
FprCEN/TR 16365:2012 (E)
Contents
Foreword .3
Introduction .4
1 Scope .6
2 Key elements of a sampling plan .6
2.1 General .6
2.2 Identify involved parties (EN 14899:2005, 4.2.1) .6
2.3 Identify general objectives (EN 14899:2005, 4.2.2) .8
2.4 Collect background information and undertake field inspection (EN 14899:2005, 4.2.5) .8
2.4.1 General .8
2.4.2 Existing information .8
2.4.3 Field inspection .9
2.4.4 Analogous sites . 10
2.5 Determine specific objectives . 11
2.6 Determine generic level of testing (EN 14899:2005, 4.2.3) . 11
2.7 Identify constituents to be tested (EN 14899:2005, 4.2.4) . 13
2.8 Identify health and safety precautions (EN 14899:2005, 4.2.6) . 13
2.9 Select sampling approach (EN 14899:2005, 4.2.7, and CEN/TR 15310-1:2006, Clause 4) . 14
2.9.1 General . 14
2.9.2 Identify the technical goals . 15
2.9.3 Determine the practical instructions . 23
2.10 Identify the most appropriate sampling technique (EN 14899:2005, 4.2.8, and
CEN/TR 15310-2) . 29
3 Sample handling in the field . 33
3.1 General . 33
3.2 Sub-sampling . 34
3.3 Sample preparation and storage (CEN/TR 15310-4). 35
3.3.1 General . 35
3.3.2 Packaging . 35
3.3.3 Preparation and storage . 36
3.4 Transport the sample to the laboratory (EN 14899:2005, 5.2, and CEN/TR 15310-4) . 37
4 Documentation (long and short form of sampling plan) . 37
5 Sampling (EN 14899:2005, 5.1) . 38
6 Sampling uncertainty and other issues . 38
Annex A (informative) Example sampling plans for waste characterisation for exploration,
operation and closure stages of extractive industries . 40
A.1 General . 40
A.2 Example detailed sampling plan for exploration stage . 40
A.3 Example short form sampling plan for exploration/ permitting stage . 47
A.4 Production stage – Simple system – Aggregate quarry . 49
Annex B (informative) Example sampling record . 53
Bibliography . 54

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Foreword
This document (FprCEN/TR 16365:2012) has been prepared by Technical Committee CEN/TC 292
“Characterization of waste”, the secretariat of which is held by NEN.
This document is currently submitted to the Technical Committee Approval.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
This Technical Report is intended to supplement the existing series of five Technical Reports dealing with
sampling techniques and procedures for waste, and provides specific information for sampling of waste from
the extractive industry. It follows the principles laid down in EN 14899, Characterization of waste  Sampling
of waste materials  Framework for the preparation and application of a Sampling Plan. Further information
on the relationship between the production of a sampling plan and the overall testing programme objectives
can be found in CEN/TR 15310-5.
 CEN/TR 15310-1, Characterization of waste — Sampling of waste materials — Part 1: Guidance on
selection and application of criteria for sampling under various conditions;
 CEN/TR 15310-2, Characterization of waste — Sampling of waste materials — Part 2: Guidance on
sampling techniques;
 CEN/TR 15310-3, Characterization of waste — Sampling of waste materials — Part 3: Guidance on
procedures for sub-sampling in the field;
 CEN/TR 15310-4, Characterization of waste — Sampling of waste materials — Part 4: Guidance on
procedures for sample packaging, storage, preservation, transport and delivery;
 CEN/TR 15310-5, Characterization of waste — Sampling of waste materials — Part 5: Guidance on the
process of defining the sampling plan.
This Report focuses mainly on sampling for geochemical rather than geotechnical requirements. Sampling for
geotechnical requirements is only addressed to a limited extent and references are made to existing
documentation. The Technical Report elaborates on a range of potential approaches and tools of specific
relevance to the sampling and testing of wastes from the extractive industry. This approach enables the
project manager to tailor his sampling plan to a specific testing scenario and continues the ‘shop shelf’
approach to sampling plan development for waste testing outlined in CEN/TR 15310-1 to -5. This approach
allows flexibility in the selection of the sampling approach, sampling point, method of sampling and equipment
used. It provides the necessary background information pertaining to the factors that influence the choice of
these detailed components of the sampling exercise, and information on the necessary statistical choices that
can then be applied to determine the most appropriate testing programme for any given sampling scenario.
This Technical Report also makes references to the overall guidance document for characterization of waste
from extractive industries (FprCEN/TR 16376) which gives guidance and recommendations on the application
of methods for the characterization of waste from extractive industries.
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Introduction
The guidance outlined in this Technical Report is focused on the key elements to be considered in the
development of a sampling plan for extractive waste. This report should be used in conjunction with EN 14899
and its supporting technical reports and is intended to supplement the information contained in these
documents with specific and essential information relevant to the sampling of waste from the extractive
industry. Where appropriate this report also makes reference to the overall guidance document for
characterisation of waste from extractive industries (FprCEN/TR 16376) which gives guidance and
1)
recommendations on the application of methods for the characterization of waste from extractive industries .
1) Specific features of extractive waste
The extractive industry includes, metal mines, rock quarries, salt mines, coal mines, sand and gravel,
limestone and onshore oil and gas operations. When mineralogical material is extracted it is exposed to
changes in physico-chemical conditions, which may result in chemical and physical instability of previously
stable geological material.
The life cycle of extractive industries starts with the early phase of exploration through operation to closure
and after care. In the context of sampling three phases have been defined in this document:
 Exploration (incl. design and permitting);
 Operation (extraction and processing, including transport and deposition of waste); and
 Closure (including existing waste deposits).
From a sampling perspective different sampling scenarios may be more relevant than the operational phases.
For example sampling from diamond drill cores may take place both during exploration and operation,
sampling at existing waste rock dumps and tailings facilities may take place both during operation and at
closed sites. Both operational phases and sampling scenarios are used as parallel concepts in this document.
One significant feature that makes characterization of extractive waste different from waste characterization in
general is the fact that sampling and characterization ideally take place before the waste is produced, i.e.
based on drill cores (or drill mud) from exploration drilling. Characterization during exploration is critical since
subsequent waste management plans are developed on the basis of this information. However, the availability
of material for sampling and characterization at the exploration stage is commonly limited which means that
follow-up checks to ensure that the initial data and interpretation are correct will often be needed during
operation. If pilot scale tests, extraction and/or processing, are carried out this will have the added benefit of
producing a larger number of potential samples for sampling and testing as well as giving the opportunity to
sample process waste, i.e. tailings. While the majority of waste is commonly produced during the operation
phase of a mine, waste characterisation needs to be considered for all phases of the mine life.
The operational phase of a mine or quarry encompasses all the activities from mineral deposit development to
detailed planning for closure. There are two main waste streams from the production process that need to be
characterised, i.e. waste material generated as part of the extraction that will not go through mineral
processing and the waste produced during processing. The waste produced prior to mineral processing will
primarily be waste rock separated at the excavation front. In a hard rock mine, sampling may be done before
blasting from drill cores, or after blasting. After mineral processing the waste will primarily be tailings (i.e. tail
end of the process), and samples may be collected from pipelines, discharge trenches or conveyer belts.
Extractive waste may contain chemicals added as part of the production process. Normally, if not recovered
for construction purposes, all extractive waste is deposited on site.

1) As defined in Directive 2006/21/EC.
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This guidance is also applicable for sampling from closed sites in case sampling and testing of waste is
required. Sampling at closed sites, including abandoned historic mine-sites, may in some cases require
specific approaches e.g. due to accessibility and limited background information.
NOTE Given the great variety of waste types, sampling situations and objectives, this Technical Report cannot
provide definitive instructions that cover all scenarios. Instead, it discusses the basic considerations to be followed, and
provides guidance on selection of sampling approaches that might be relevant to the three principle phases of a mine: 1)
Exploration, 2) Operation and 3) Closure. Sampling of existing waste deposits at mines that are still in operation would be
very similar to Scenario 3) Closure.
2) Document structure
The structure of this sampling guideline is based on the concepts and procedural steps outlined in Figure 2 of
EN 14899:2005 and subsequent subclauses, with some additions to address specific features of the extractive
industry.
Clause 3, key elements of a sampling plan, is the core of this guidance document. This clause is divided into
nine sub-sections that describe the steps of developing sampling plans, from defining the involved parties to
describing the sampling techniques. It lists possible objectives for the different stages of the extractive waste
characterisation, background information that may be available, explains generic levels of testing and
describes sampling approaches and techniques.
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1 Scope
This Technical Report gives additional and specific information on sampling for testing of waste from the
extractive industry to support the development of appropriate sampling plans. This supplementary guidance to
EN 14899 is required because waste from the extractive industry differs considerably from the waste types
and sampling scenarios covered in the existing technical reports that support the Framework Standard. This
guidance document should be used in conjunction with EN 14899 and its supporting technical reports
CEN/TR 15310-1 to -5.
The approach to sampling described in this document is primarily focused on the requirements to undertake
mineralogical and geochemical testing. Whilst much of the background information provided is also relevant to
geotechnical investigations there may be important additional requirements or differences in approach for
determining relevant physical parameters. For example, many geotechnical parameters are determined using
field tests, which are not discussed in this document. References to alternative source documentation are
provided.
The guidance provided in this document applies only to above-ground exposure to radio-nuclides present in
the undisturbed earth crust and not to the production, processing, handling use, holding, storage, transport, or
disposal of radioactive substances that are or have been processed for their radioactive, fissile or fertile
properties.
This Technical Report provides some discussion of current best practice, but is not exhaustive. To clarify the
text, the document provides a number of worked examples in the Annexes.
2 Key elements of a sampling plan
2.1 General
The sampling plan identifies the appropriate and practical activities required to achieve the set objectives of
the characterisation testing programme. The purpose of a sampling exercise shall be clearly understood by
the sampler. The development of a sampling plan helps to ensure that the objectives of any waste testing
programme are consistently met and is crucial for cost effective and appropriate sampling. The sampling plan
provides traceability which can be used to validate the data produced. This is especially important where new
datasets will be generated over time.
The framework standard EN 14899 identifies a process flow chart that defines the essential elements of a
sampling plan and how those elements are linked. The basic steps identified in this flow chart have been
followed in this supplementary guidance, with some minor changes (see Figure 1) to account for specific
circumstances of the extractive industry. The flow chart indicates a step by step process to sampling plan
development, although in reality they may be considered out of order. Some elements of the sampling plan
may be prepared in parallel and iterations may be necessary. Additional information is provided in the
following sections that are specific to the extractive industry.
It is important to recognise that characterisation may often be an iterative process. The sampling plan may
initially be developed for screening purposes and may then form the basis of a characterisation study. The
characterisation study may require testing of samples previously collected but not subjected to testing or form
the basis for collection of more samples required for more comprehensive testing all specified in the sampling
(Figure 1).
Characterisation of waste from a quarry may be relatively simple in comparison to wastes from metal
extraction. However, generating a sampling plan using the outline approach advocated in this guidance
document is still recommended. Development of a comprehensive sampling plan will facilitate discussions
with stakeholders, and it may help the operator to identify issues that may require consideration.
2.2 Identify involved parties (EN 14899:2005, 4.2.1)
It is recommended that sampling plans for a given site and phase of operation are, where possible, discussed
with involved parties prior to any sampling taking place. It is important to identify and include parties with an
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interest at an early phase in the testing programme. This may include e.g. people from different parts of the
organisation of the operator, consultants, regulators and local stakeholders. This approach may avoid or
minimise confusion at a later date and facilitate acceptance from involved parties. Well-communicated
sampling plans may provide confidence that the results generated from the sampling and testing programme
will be valid.

The numbers in the chart refer to the clauses within this document.
Figure 1 — Flowchart of sampling plan modified from Figure 2, EN 14899:2005
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2.3 Identify general objectives (EN 14899:2005, 4.2.2)
The overarching objectives of a testing programme define the type and quality of information required from
sampling and analysis. During the various phases in the life of a mine there may be more than one objective
and therefore a need for more than one sampling plan. Each objective should be translated into specific
technical objectives or goals in the sampling plan which are sufficiently detailed to define all aspects of the
required sampling programme. Whilst the overall objective can be identified prior to any background data
collection and on-site investigation the technical objectives can usually only be set once this information has
been gathered.
Example overarching objectives may be to contribute data to:
 design a waste facility;
 development of a waste management plan;
 design/evaluation of closure options;
 design/evaluation of management options for abandoned sites.
The overall guidance document (FprCEN/TR 16376) includes a discussion on when and why characterisation
may be needed and the context within which characterisation data may need to be applied. However, it does
not cover information on how to apply these characterisation results, e.g. for dam design or closure planning.
For guidance on how to use characterisation results correctly for predictive modelling or design purposes
references are made to other sources of information.
2.4 Collect background information and undertake field inspection (EN 14899:2005, 4.2.5)
2.4.1 General
It is essential to obtain pertinent background information to develop good sampling plans for future, existing,
closed and abandoned facilities. The background information allows the development of clear and precise
instructions for sampling. Background information can be divided into three categories: existing information
including site background information; field inspection information; and analogous geology. These three
categories are discussed in the following clauses.
2.4.2 Existing information
Obtaining background information on a proposed extractive operation and collating this information to feed
into the development of a testing program and sampling plan is essential when defining appropriate detailed
objectives for sampling and testing. Careful inclusion of valid prior information can greatly reduce the cost per
unit of error and dramatically reduce the size of the samples required. Relevant existing information may
include data from previous exploration work as well as investigations carried out for other land uses or local
data on background concentrations of key constituents in soils and surface waters.
The use of existing information would typically be complemented by a field visit. It is important to emphasise
that although existing data may be very useful, its relevance should be evaluated prior to using the data in any
decision making process. If data is available from previous sampling programmes, the evaluation of suitability
would include looking at the:
1) type of sampling undertaken;
2) consistency of test data and analytical procedures used;
3) objectives of previous sampling and testing.
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If a site moves from exploration to operation a new sampling plan will need to be developed and the waste
characterisation data used for design and permitting will then become the background information for the
operation stage.
The overall guidance document (FprCEN/TR 16376:2012, Clause 5) gives further recommendations on site
background information that may be useful.
2.4.3 Field inspection
A field inspection provides valuable information on local conditions, e.g. any access restrictions that may
impact upon the planned sampling approach e.g. appropriate selection of sampling points. The information
that may be gathered by a field inspection will be very different for an exploration site compared to an on-
going operation or a closed waste facility. Examples of information that should be collected include:
a) Exploration
1) Topography, accessibility;
2) Geology;
3) Mineralogy/iron phases in drilling material, overburden and exposed bedrock;
4) Relevant environmental factors.
b) Operation
1) Accessibility;
2) Geology;
3) Mineralogy/iron phases;
4) Additives;
5) Grain size variation;
6) Erosion features and slumping;
7) Excavation and transport methods;
8) Material type (tailings, waste rocks);
9) Potential hazards;
10) Relevant environmental factors.
c) Closure and closed sites
1) Accessibility;
2) Geology;
3) Mineralogy/iron mineral phases;
4) Seepage/seepage colour and possible field measurements of seepage;
5) Water/air erosion features at disposal facilities;
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6) Grain size variation;
7) Slumping;
8) Potential hazards;
9) Relevant environmental factors.
The evaluation of the sample size and number of samples that should be collected is primarily dictated by the
heterogeneity of the waste (e.g. variations in mineralogical composition and content of hazardous
components), grain size variation during production, excavation and transport methods, material type (tailings,
waste rocks) and associated environmental impacts. Statistical requirements (e.g. precision, accuracy,
uncertainty) and available resources (i.e. cost) will also influence the number and size of samples required for
a test program.
Signs of water and air erosion, especially on tailings, can indicate, to some degree, the extent to which the
waste material has been transported from its original position. The following information can be used to
identify the area to be sampled.
 Erosion features;
 Aeolian transport of tailings from original deposit;
 Stability of existing tailings and waste rocks.
Mapping the deposit mineralogy and the presence of iron phases (for sulfide containing mineralisation) is an
essential part of evaluating the risks associated with current and future waste from the site. The mineralogy
rather than the bulk chemistry provides a first indication of potential drainage quality, acid generating minerals,
and neutralizing minerals. If the rocks have been exposed to air and water variations (where groundwater is
being lowered due to pumping) over short or long periods, secondary minerals may give an indication of how
the waste will behave when it is subsequently exposed to air and water.
The type of processing and use of additives, and type of waste being generated will give an indication of the
type of analyses that may be necessary and define health and safety precautions during sampling and
handling of the samples. If first evaluation indicates that there is a potential for acid/neutral rock drainage
(A/NRD) or leaching from tailings, it may be necessary to obtain samples from a pilot processing plant.
The presence of seepage, colour and field measurements of the seepage, aid in defining, for example, the
level of testing and type of analysis. These observations and field measurements give an indication of the
oxidation reactions and leaching taking place within the waste material. For example:
 Drainage pH and total dissolved solids
...

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