Competitive and Sustainable Growth (GROWTH) Programme
SAMARIS
Sustainable and Advanced MAterials for Road InfraStructure
DELIVERABLE D24
ENVIRONMENTAL ANNEXES TO ROAD PRODUCT
STANDARDS
Document number:
SAM-GE-DE24
Version:1 Draft 1
Date: 30.09.05
Name and signature
Drafted: Sabine Boetcher, Klaus Krass
Reviewed: Cliff Nicholls
Verified: Wolfgang Bernrieder
Validated: Pat Maher
Approved by SAMARIS Management Group:
Date
SAMARIS SAM-GE-DE24
TABLE OF CONTENTS
1
INTRODUCTION ........................................................................................................... 1
2
PROCEDURE ................................................................................................................. 2
3
IDENTIFICATION OF RELEVANT ROAD MATERIALS ...................................... 4
3.1
General ............................................................................................................................... 4
3.2
Assessment procedure of selected industrial by-products ............................................. 6
3.3
Assessment procedure of selected recycled materials .................................................. 11
4
IDENTIFICATION OF APPROPRIATE EUROPEAN STANDARDS ................... 13
5
IDENTIFICATION OF HAZARDOUS COMPONENTS AND
APPROPRIATE TEST METHODS ............................................................................ 16
6
DRAFTS OF ANNEXES TO PRODUCT STANDARDS .......................................... 20
6.1
General ............................................................................................................................. 20
6.2
Draft for an environmental annex on aggregates for bituminous mixtures .............. 20
6.3
Draft for an environmental annex on asphalt concrete ............................................... 22
6.4
Draft for an environmental annex on reclaimed asphalt............................................. 22
6.5
Draft of environmental annex on aggregates for unbound and
hydraulically bound materials ....................................................................................... 22
6.6
Draft of environmental annex on unbound mixture specifications ............................ 23
6.7
Handling tar-bound reclaimed road material .............................................................. 23
7
CONCLUSIONS ........................................................................................................... 25
8
REFERENCES .............................................................................................................. 27
APPENDIX A:
TEST FOR TAR ..................................................................................... 29
APPENDIX B:
TEST FOR SULPHUR .......................................................................... 37
APPENDIX C:
ANNEX TO EN 13043 ............................................................................ 41
APPENDIX D:
ANNEX TO EN 13108-1 ........................................................................ 43
APPENDIX E:
ANNEX TO EN 13108-8 ........................................................................ 44
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SAMARIS SAM-GE-DE24
APPENDIX F:
ANNEX TO EN 13242 ............................................................................45
APPENDIX G:
ANNEX TO EN 13285 ............................................................................47
II
SAMARIS SAM-GE-DE24
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SAMARIS SAM-GE-DE24
1 INTRODUCTION
Five years ago, the Forum of European National Highway Research Laboratories (FEHRL)
proposed two projects called MAP (Materials for Asphalt Pavement) and STRIM (Structures
in Maintenance) which were finally merged in a research and development project called
SAMARIS (Sustainable and Advanced MAterial for Road InfraStructure). This project is
part of the Growth programme of the 5th Framework programme and is jointly financed by the
European Commission and the project partners’ national resources. The project period was
fixed from 1st January 2003 to 31st December 2005.
The SAMARIS project is separated in two technical streams. On the one hand, there is the
pavement stream that is subdivided into five Work Packages and, on the other hand, the structure stream that is also structured in different Work Packages.
Work Package 4, entitled “Safety and Environmental Concerns in Material Specifications”, is
a part of the pavement stream and primarily concentrates on addressing safety and environmental aspects in product standards, for example the detection and classification of hazardous
characteristics in road materials. The WP is organised in three tasks. The key objective for
task 4.1 is to produce an overall procedure including appropriate test methods for the identification of hazardous components in road materials regarded as being recyclable. In doing so,
emphasis will be on asphalt. Task 4.2 analyses the need of an investigation of reaction of
pavement materials to fire. Existing tests were checked for their applicability and new test
methods were developed were it was found to be necessary.
This report is the output of task 4.3 and is entitled “Environmental Annexes to Product Standards”. The aim of task 4.3 is to make proposals how environmental sustainability requirements of road materials could be included in the European Product Standards for road materials in form of an annex. Justification is derived from the goal of the European Commission to
incorporate environmental requirements into the second generation of the European Product
Standards for construction materials according to the essential requirement “Hygiene, health
and environment”. This subject was not a part of the mandates for the different construction
materials that have been standardised so far. In relation to these construction materials, the
main focus of task 4.3 is on recyclable (road) materials and industrial by-products which can
be used as aggregates for unbound and bound mixtures. It has to be ascertained whether very
different experience has been gained with the application of these materials in different European Countries. In any case, the requirements for these materials do vary significantly.
In addition to the input from Work Package 4, input has been derived from other Work Packages of this project, particularly Work Package 3 dealing with the assessment of alternative
materials.
After the identifying the relevant road materials to be used for this task, the appropriate European Product Standards are identified. The next step in the proceeding was to find the potential hazardous components and the appropriate test methods. Finally, drafts of annexes to the
Product Standards were developed, duly formatted so as to be suitable for future standardisation.
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2 PROCEDURE
The task proceeding is subdivided into four steps (see Figure 2.1):
Step 1: Identification of relevant road materials
Step 2: Identification of appropriate European Product Standards
Step 3: Identification of hazardous components in road materials and appropriate test methods for their determination
Step 4: Drafts of annexes to Product Standards
Step
No.
Action
Input from
Example
1
Identification of
relevant road materials
WP 3
Industrial by-products,
tar bound materials
2
Identification of
appropriate European
Product Standards
CEN/TC 154
CEN/TC 227
EN 13043
prEN 13108-8
EN 13285
3
Identification of
hazardous components
and appropriate test
method
WP 3
Task 4.1
Literature
Leaching test
Detection of sulphur,
PAH
4
Drafts of annexes to Product Standards
Figure 2.1: Proceeding – Flow chart
In order to make the content of these steps clearer they shall be in detail explained in the following:
Step 1: The identification of the relevant road materials was strongly based on the relevant
input from Work Package 3. Additionally, a literature review was carried out for other potentially useful sources of information for the work. The results of the investigations are those road materials dealing with in the next steps.
Step 2: Step 2 was to identify those European Product Standards where the above mentioned
road materials are covered. These standards are mostly part of the work programmes
of Comité Européen de Normalisation (European Committee for Standardisation,
CEN) Technical Committees TC 154 “Aggregates” and TC 227 “Road materials”.
Step 3: The hazardous components for each road material identified in step 2 were defined
along with an appropriate test method for determination of the relevant component.
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SAMARIS SAM-GE-DE24
A decisive criterion for all of them is the path of danger, e.g. the transport of the hazardous component by air, by soil or by water. For this objective, the work of task 4.1
was incorporated.
Step 4: In this last step, drafts of annexes to some typical standards with environmental requirements were prepared. In doing so, the question as to whether the drafts should
include threshold values for the requirements or whether more rather general advice
should be given is discussed.
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3 IDENTIFICATION OF RELEVANT ROAD MATERIALS
3.1 General
Deliverable N°16 of the SAMARIS project, entitled “Methodology for assessing alternative
materials for road construction” (SAMARIS, 2005) reviewed eight alternative materials.
These materials can be subdivided into industrial by-products and recycled construction
waste.
The industrial by-products selected were:
 crystallised blast furnace slag
 vitrified blast furnace slag
 basic oxygen furnace slag
 electric arc furnace slag
 coal fly ash
 municipal sold incineration bottom ash
These six industrial by-products were selected as the result of an enquiry in the European
countries into which, unfortunately, Germany did not participate. Other residuals from power
plants, such as boiler slag and fly ash from lignite combustion, have an importance in Germany (FGSV, 2003 and 2004; Krass et al., 2004), so that these two industrial by-products were
added to the list. The list of all the selected industrial by-products is given in Table 3.1. The
table also includes the common abbreviations used subsequently in this report.
Table 3.1:
Selected industrial by-products
Industrial by-product
Abbreviation
1
Crystallised (or air-cooled) blast furnace slag
CBF slag
2
Vitrified (or granulated) blast furnace slag
VBF slag
3
Basic oxygen furnace slag
BOF slag
4
Electric arc furnace slag
EAF slag
5
Coal fly ash
CFA
6
Boiler slag
BS
7
Fly ash from lignite combustion
8
Municipal solid waste incinerator bottom ash
FALC
MSWIBA
Concerning recycled construction waste, only crushed concrete was defined in D16
(SAMARIS, 2005) whereas two types are categorised: building demolition crushed concrete
(BDCC) and road crushed concrete (RCC). In practice, it is seldom and often uneconomic for
the load of processing plants to handle the two types of crushed concrete separately. Usually,
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SAMARIS SAM-GE-DE24
all the construction waste is described, as well as processed, in one material group. Justification is given by the fact that crushed concrete from any sources is often polluted by extraneous
components.
However, it is advisable to deal separately with bitumen-bound and tar-bound materials and
the mineral construction waste. Therefore, the recycled material can been distinguished as
listed in Table 3.2.
Table 3.2:
Selected recycled materials
Recycled materials
Abbreviation
1
Crushed mineral construction waste
CMCW
2
Reclaimed asphalt
RA
3
Tar bound reclaimed road material
TB
For better understanding, the selected materials will be described together with the potential
applications of each material in road structure according to D16 (SAMARIS, 2005), see Figure 3.1. The description of the applications is a summary from D16. For detailed information, it is useful to look directly at D16.
1
2
5
3
5
5
4
Figure 3.1: The typical road structure
The different sections of the road structure can be described according to their technical functions as follows:
 Section 1 Surface course
 Section 2 Base layer
 Section 3 Sub-base
 Section 4 Subgrade
 Section 5 Shoulders, landscaping and embankments
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3.2 Assessment procedure of selected industrial by-products
3.2.1 Blast furnace slag
3.2.1.1 General
Blast furnace slag is a by-product of the manufacture of iron by chemical reduction in a blast
furnace. It is formed in a continuous process by the fusion of limestone (and/or dolomite) and
other fluxes with the residues from the carbon source (coke) and non-metallic components of
the iron ore. Blast furnace slag is produced at temperatures around 1500 °C. Depending on
the way of cooling it can be distinguished between crystallised air-cooled blast furnace slag
and glassy granulated (vitrified) blast furnace slag (REACH, 2003).
3.2.1.2 Crystallized Blast Furnace slag (CBF slag)
The essential chemical constituents of CBF slag are listed in Table 3.3.
Table 3.3:
Essential chemical constituents of crystallised blast furnace slag (REACH,
2003)
Constituent
% by mass
Constituent
% by mass
CaO
33 – 42
MnO
0,1 – 1,0
SiO2
33 – 40
K2O
0,3 – 0,9
MgO
7 – 14
Na2O
0,1 – 0,8
Al2O3
9 – 15
Stot.
1,0 – 1.5
Fetot.
0,1 – 0,7
Crystallised blast furnace slag can be used:
 in surface courses, often without covering but, in some countries, with a cover against
erosion (Section 1).
 in all base layers, unbound and bound (Section 2).
 in sub-bases, unbound and bound (Section 3).
 for subgrade (Section 4).
 for shoulders, landscaping and embankment, in some countries with cover (Section 5).
3.2.1.3 Vitrified Blast Furnace slag (VBF slag)
The essential chemical constituents of VBF slag are the same as shown in Table 3.3.
Vitrified blast furnace slag can be used:
 in all base layers, unbound and bound, partly as a fine aggregate or as a binder (Section 2).
 in sub-bases, unbound and bound, in the same function as in section II (Section 3).
 for subgrade (Section 4).
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SAMARIS SAM-GE-DE24
 for shoulders, landscaping and embankment, in some countries with cover (Section 5).
The last use is only a technical possibility but, from the economical point of view, VBF slag is
too valuable for this use (mostly a raw material for cement production).
3.2.2 Basic Oxygen Furnace steel slag (BOF slag)
Basic oxygen furnace slag is produced in a batch process as a by-product of the conversion of
iron to steel. The slag is produced by the addition of fluxes, such as limestone or dolomite,
during blowing oxygen into molten iron. Elements which are unwanted in the steel (like carbon, silicon or phosphate) are either oxidised to gases or are chemically combined into the
slag. The molten slag, which has temperatures around 1600 °C, is air-cooled under controlled
conditions in pits forming crystalline slag.
BOF slag (often called “LD slag”) is a steel slag consists essentially of the chemical constituents listed in Table 3.4.
Table 3.4:
Essential chemical constituents of basic oxygen furnace slag (REACH, 2003)
Constituent
% by mass
Constituent
% by mass
CaO
41 – 53
FeO
17 – 27
CaOfree
2–9
MnO
2–5
SiO2
11 – 18
P2O5
1–3
MgO
1–6
Cr2O3
< 0,5
Al2O3
1–5
Basic oxygen furnace slag can be used on principle dependent on their volume stability for all
sections of a road (Sections 1 to 5).
3.2.3 Electric Arc Furnace slag (EAF slag)
Electric arc furnace slag is produced during a process of melting scrap in an electric induction
furnace at temperatures around 1600 °C. EAF slag resulting from the generation of carbon
steel has properties similar to those of BOF slag.
EAF slag as a steel slag consists essentially of the chemical constituents compiled in Table 3.5.
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SAMARIS SAM-GE-DE24
Table 3.5:
Essential chemical constituents of electric arc furnace slag (REACH, 2003)
Constituent
% by mass
Constituent
% by mass
CaO
22 – 36
FeO
24 – 37
CaOfree
<1
MnO
4–8
SiO2
10 – 18
P2O5
0,5 – 1,0
MgO
3–9
Cr2O3
1–3
Al2O3
4–9
Electric arc furnace slag can be used in the same way as the BOF slag in all sections of a road
(Sections 1 to 5).
3.2.4 Coal Fly Ash (CFA)
Coal fly ash is obtained by electrostatic or mechanical precipitation of dust-like particles from
the flue gases of furnaces fired with coal at 1100 to 1300 °C. Fly ash is a fine powder, which
is mainly composed of spherical glassy particles. Depending upon the type of boiler and the
type of coal: siliceous, silica-calcareous and calcareous fly ashes with pozzolanic and/or latent
hydraulic properties are produced (ECOBA, 2004).
According to the burnt coal fly ash consists essentially of the chemical constituents as compiled in Table 3.6.
Table 3.6:
Essential chemical constituents of coal fly ash (ECOBA, 1997; 1999)
Constituent
% by mass
Constituent
% by mass
SiO2
36 – 60
K2O
0,4 – 6
Al2O3
17,6 – 40
Na2O.
0,1 – 3,5
Fe2O3
2,6 – 17
SO3
0,1 – 2,5
CaO
0,3 – 11,8
TiO2
0,5 – 1,7
MgO
0,5 – 5,4
Coal fly ash can be used:
 in surface courses, usually as a filler, in cement bound courses also as an additive (Section 1).
 in unbound and bond base layers as a filler or as a binder (Section 2).
 in sub-bases in the same kind as in base layers (Section 3).
 for subgrade, as a fine aggregate as well as a binder (Section 4).
 for embankments (Section 5).
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SAMARIS SAM-GE-DE24
3.2.5 Boiler Slag (BS)
Boiler slag is a vitreous grained material deriving from coal combustion in boilers at temperatures of 1500 to 1700 °C, followed by wet ash removal of wet bottom furnaces (ECOBA,
1997; 1999).
The essential chemical constituents of BS, which mainly occurs in Germany, are shown in Table 3.7.
Table 3.7:
Essential chemical constituents of boiler slag (FGSV, 1993)
Constituent
% by mass
Constituent
% by mass
SiO2
40 – 55
K2O
1,5 – 5,5
Al2O3
23 – 35
Na2O
0,1 – 3,5
Fe2O3
4 – 17
SO3
0,1 – 2,0
CaO
1–8
TiO2
0,5 – 1,3
MgO
0,8 – 4,8
Boiler slag as a granulated fine aggregate without any hydraulic properties can be used in all
sections of a road, in unbound layers as well in bound layers (Sections 1 to 5).
3.2.6 Fly Ash from Lignite Combustion (FALC)
Fly ash from lignite combustion occurring in Germany, Spain and some eastern European
countries is obtained by electrostatic or mechanical precipitation of dust-like particles from
the flue gases of furnaces fired with lignite at 1100 to 1300 °C. Fly ash is a fine powder,
which is mainly composed of spherical glassy particles. Depending upon the type of boiler
and the type of lignite siliceous, silica-calcareous and calcareous fly ashes with pozzolanic
and/or latent hydraulic properties are produced (ECOBA, 1999). Depending on the origin of
the burnt lignite, fly ash from lignite combustion consists essentially of chemical constituents
as compiled in Table 3.8.
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Table 3.8:
Essential chemical constituents of fly ash from lignite combustion in some
European countries
Germany
Constituent
two
Greece
Poland
Spain
% by mass
SiO2
20 – 80
21 – 35
20 – 88
49,8 / 53,3
Al2O3
1 –19
10 – 14
0,6 – 9
17,3 / 18,2
Fe2O3
1 – 22
4,5 – 6,5
1,5 – 7
8,7 / 7,9
CaO
2 – 52
30 – 45
3 – 49
24,9 / 20,8
CaOfree
0,1 – 25
 10
n/a
11,4 / 8,6
MgO
0,5 – 11
1,5 – 3
0,5 – 7
1,9 / 1,7
K2O
0–2
0,4 – 0,9
n/a
0,3 / 0,3
Na2O
0,01 – 2
0,5 – 1
n/a
1,7 / 1,6
SO3
1 – 15
4–8
0,4 – 12,5
4,3 / 4,7
TiO2
0,1 – 1
n/a
n/a
n/a
samples only
Fly ash from lignite combustion, a fine material similar to coal fly ash, can normally be used
only for subgrade (Section 4) and embankments (Section 5) due to some problems with the
volume stability.
3.2.7 Municipal Solid Waste Incinerator Bottom Ash (MSWIBA)
Municipal solid waste incinerator bottom ash is defined as "ash particles from incineration
plants of household waste that fall to the bottom of the furnace". Combustion of MSW produces two main streams of residues, i.e. bottom ash and a fly ash. The unprocessed bottom
ash consists of non-burnt materials and inert wastes, e.g. glass, concrete blocks and metals.
Processed MSWI bottom ash, fit to be used as a road construction material, has generally metals separated from the ash and further screened to remove oversized materials.
The range of components in processed MSWIBA, dependent on the burnt waste contents, is
shown in Table 3.9.
Table 3.9:
10
Range of components in processed municipal solid waste incinerator bottom
ash (FGSV, 2005)
Components
% by mass
ash, incl. parts of slag
30 – 80
glass / ceramics
10 – 50
metals
0–5
miscellaneous
0 – 25
unburnt particles
< 0,5
SAMARIS SAM-GE-DE24
The MSWIBA can be used:
 in unbound and cement bound sub-bases (Section 3).
 for subgrade (Section 4).
 for shoulders, landscaping and embankment, normally with cover against erosion (Section 5).
3.3 Assessment procedure of selected recycled materials
3.3.1 Crushed Mineral Construction Waste (CMCW)
Crushed mineral construction waste is defined as mineral material resulting from rebuilding or
demolition of building elements such as walls, floors and foundation and of roads. It will be
processed according to the new purpose.
As an example of the requirements in Germany, some objective examples are shown in Table 3.10.
Table 3.10: Objective requirements for components in crushed mineral construction
waste (FGSV, 2004)
Component
Reclaimed asphalt
Clinker, brick, ceramics
Sand-lime brick, mortar
Mineral lightweight material as pumice- or gas concrete
Foreign matters as wood, rubber, plastics
% by mass
 30
 30
5
1
 0,2
Crushed mineral construction waste can be used:
 in base layers, normally unbound, but also in cement-bound and, in some countries, bitumen-bound as well (Section 2).
 in unbound sub-bases (Section 3).
 for subgrade (Section 4).
 for shoulders, landscaping and embankments (Section 5).
3.3.2 Reclaimed Asphalt (RA)
According to EN 13108-8, reclaimed asphalt is “asphalt, not containing tar, reclaimed by milling of asphalt road layers, by crushing of plates torn up from asphalt pavements or lumps from
asphalt plates and asphalt from surplus production”.
Reclaimed asphalt can dependent on its origin be used:
 in bitumen bound surface courses, together with unused bitumen and aggregates (Section 1).
 in base layers, bitumen bound as in surface courses and with a limited quantity in unbound layers (Section 2).
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SAMARIS SAM-GE-DE24
 in sub-bases, unbound with limited quantities (Section 3).
 for subgrade and landscaping as well as embankment (Sections 4 and 5).
However, the last application is rather a down cycling and, therefore, should be avoided.
3.3.3 Tar Bound reclaimed road material (TB)
Tar bound reclaimed road material is material containing tar, and possibly bitumen as well,
that is reclaimed by milling of bound road layers, by crushing of plates torn up from bound
pavements or lumps from bound plates.
Tar bound reclaimed road material can only be used in cold mixed base layers and sub-bases
with bitumen and/or cement as the binder (Sections 2 and 3). This application needs further
examination for environmental reasons.
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SAMARIS SAM-GE-DE24
4 IDENTIFICATION OF APPROPRIATE EUROPEAN
STANDARDS
Concerning the technical specifications for construction products, distinction has to be made
between:
 mandated European product standards,
 mandated European Technical Approval of a product, and
 “voluntary” product standards.
A mandated European product standard is a standard fulfilling the Construction Products Directive (CPD) (EEC, 1988). The final outcome of standardisation work is a harmonised
standard (hEN) for a construction product. A construction product is presumed to be fit for its
intended use if it bears the CE marking which attests the conformity of the construction product to technical specifications of the relevant hEN.
A European Technical Approval (ETA) for a construction product has the same status as the
hEN, the only difference being in the procedure of preparing the specification.
In contrary to that, a “voluntary” product standard is a European standard for a construction
product without a mandate, but produced in accordance with the rules of the European Committee for Standardisation (CEN).
Even if the main focus of this report is on the series of relevant hENs recently produced or in
preparation, the “voluntary” standards cannot be excluded because it is, for example, possible
to produce unbound mixtures (having no CE marking) using CE marked aggregates as well by
non-CE marked aggregates. In both cases, the environmental requirements have to be fulfilled.
The following tables list the most important European standards for road materials. These
standards are produced by different Technical Committees of CEN. These committees are:
 CEN/TC 336 “Bituminous binders”
 CEN/TC 154 “Aggregates”
 CEN/TC 227 “Road materials”
Table 4.1 is a compilation of the product standards needed for the production of hot mix asphalt. All the mentioned standards are harmonised standards or en route to become hENs.
The European standards for the production of hydraulically bound materials and unbound materials are listed in Table 4.2. In this area of road materials, there are also some “voluntary”
European standards.
In the “comment” column, some standards are marked with a “D”, which stands for there being a draft of an environmental annex in Chapter 6. These standards were selected because
they are typical mandated or non-mandated product standards.
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Table 4.1:
Identification of appropriate European Product Standards for binder, aggregates and their bituminous mixtures
Number of
Standard
Title
Comment
EN 12591
Bitumen and bituminous binders – Specification for paving grade bitumens
hEN 14023
Bitumen and bituminous binders – Framework specification for polymer modified bitumens
hEN 13043
Aggregates for bituminous mixtures and surface treatments for roads, airfields and other trafficked areas
D
hEN 13108-1
Bituminous mixtures – Material specifications – Part 1:
Asphalt concrete
D
hEN 13108-2
Bituminous mixtures – Material specifications – Part 2:
Asphalt concrete for very thin layers
hEN 13108-3
Bituminous mixtures – Material specifications – Part 3:
Soft asphalt
hEN 13108-4
Bituminous mixtures – Material specifications – Part 4:
Hot rolled asphalt
hEN 13108-5
Bituminous mixtures – Material specifications – Part 5:
Stone mastic asphalt
hEN 13108-6
Bituminous mixtures – Material specifications – Part 6:
Mastic asphalt
hEN 13108-7
Bituminous mixtures – Material specifications – Part 7:
Porous asphalt (PA)
hEN 13108-8
Bituminous mixtures – Material specifications – Part 8:
Reclaimed asphalt
14
D
SAMARIS SAM-GE-DE24
Table 4.2:
Identification of appropriate European Product Standards for aggregates
and hydraulically bound and unbound mixtures
Number of
Standard
Title
Comment
hEN 12620
Aggregates for concrete
hEN 13877-1
Concrete pavements – Part 1: Materials
hEN 13242
Aggregates for unbound and hydraulically bound materials
for use in civil engineering work and road construction
D
EN 13285
Unbound mixtures – Specifications
D
EN 14227-1
Hydraulically bound mixtures – Specifications – Part 1:
Cement bound granular mixtures
EN 14227-2
Hydraulically bound mixtures – Specifications – Part 2:
Slag bound mixtures
EN 14227-3
Hydraulically bound mixtures – Specifications – Part 3:
Fly ash bound mixtures
EN 14227-4
Hydraulically bound mixtures – Specifications – Part 4:
Fly ash for hydraulically bound mixtures
EN 14227-5
Hydraulically bound mixtures – Specifications – Part 5:
Hydraulic road binder bound mixtures
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5 IDENTIFICATION OF HAZARDOUS COMPONENTS AND
APPROPRIATE TEST METHODS
Recycling of previously laid road materials and the use of industrial by-products is a logical
consequence of the fact that natural resources are decreasing because of rather dissipative consumption in the past. For a long time, responsible bodies for construction requirements were
very sceptic about the application of such materials and the reuse of asphalt pavements. This
scepticism is a result of the inexperience with the materials and the emerging questions about
durability and environmental impact. Danger was not only seen for workers during the processing but also for the soil and water in consequence of leaching of hazardous components
from the materials. Deliverable N° 23 of the SAMARIS project, entitled “Procedures for
identifying hazardous component materials for asphalt” (SAMARIS, 2005) points out that experience already exists with the incorporation of the industrial by-products in asphalt which
are mentioned in Chapter 3 (EAPA, 2004). However, as well as the statement in Deliverable
N° 23, some countries, particularly Germany, have long-standing experience in the use of byproducts in both unbound and hydraulically bound layers. Therefore, it makes sense to determine their hazardous components in order to define requirements in environmental annexes
for aggregates and for bituminous mixtures standards as well as for unbound and hydraulically
bound mixtures standards in order to enhance the reliability in their application.
According to Deliverable N° 16 and to the experience in Germany, leaching of the materials
potentially leads to a hazard for the soil or the water. The hazardous characteristics of the
chosen materials are listed in Table 5.1 based on Deliverable N° 16 and “Technische
Lieferbedingungen für Gesteinskörnungen im Straßenbau (FGSV, 2004)”. These hazardous
characteristics are mostly chemical properties which refer, in each case, to a certain concentration in an eluate.
In Table 5.1, a bracketed cross means that this characteristic is not mentioned in Deliverable
N° 16 but recommended in Germany.
Deliverable N° 16 identifies Boron, Selenium, Molybdenum, Antimony and Barium as hazardous characteristics. These elements are a new subject of discussion for industrial-byproducts and recycling materials. Therefore, they have not been taken into consideration in
the remainder of the work. Nevertheless, they should be kept in mind for further analyses in
the future.
Similarly, the hazardous characteristics of recycled materials are listed in Table 5.2.
The tables do not include threshold values because they are also dependant on the test method
used, which was not the same in all the European Countries for a long time, as well as the requirements.
16
SAMARIS SAM-GE-DE24
Table 5.1:
Decisive hazardous characteristics for industrial by-products
Hazardous
characteristic
pH-value
El. conductivity
CBF
slag
VBF
slag
BOF
slag
EAF
slag
CFA
BS
FALC
MSWIBA †
X
X
X
X
X
(X)
(X)
X
(X)
(X)
(X)
(X)
(X)
(X)
(X)
(X)
(X)
(X)
X
(X)
(X)
X
Chloride
(X)
Sulphate
(X)
Cyanide (e. p.)
X
DOC
Boron *
X
X
X
X
X
Aluminium
Vanadium
X
X
X
X
X
X
Chromium VI
X
(X)
X
Nickel
(X)
X
Copper
(X)
X
Zinc
(X)
X
(X)
(X)
Chromium tot.
X
X
Arsenic
X
Selenium *
X
X
Molybdenum *
X
Cadmium
X
X
X
(X)
(X)
X
Lead
†
additionally TOC as hazardous characteristic
*
see explanations above
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X
X
Antimony *
Barium *
X
X
17
SAMARIS SAM-GE-DE24
Table 5.2:
Decisive hazardous characteristics for recycled materials
Kind of
determination
Leaching test
Hazardous
characteristic
CMCW
pH - value
X
El. conductivity
X
Chloride
X
Sulphate
X
Chromium VI
X
Phenol index
EOX
Content by mass
†
*
RA
TB
X
(X)
(X)
X
X
(X)
Hydrocarbons
X
PAH (EPA) *
X
Sulphur †
X
PCDD †
X
PCB †
X
only if susceptible
Environmental Protection Agency of USA
Practical experiments of in situ measurements with lysimeters on roads in comparison to laboratory leaching tests have shown that it is impossible to describe the leaching behaviour of
industrial by-products or recycled material by just one laboratory leaching test (Knauber,
1991; Mesters, 1993). Obviously, there is an influence:
 by the kind of application of the materials (e. g. unbound or bound),
 by the position of the layer in which these materials are used within the road (i.e. application in a surface layer or under a dense layer) and
 by the hydro-geological situation within the road construction which is also influenced
by ground water level (Radenberg, 1995).
On the strength of past experience, it is sufficient to test an industrial by-product or a recycled
material by leaching, e.g. in a shaking test or in a tank test. With such a test, it is possible in
principle to characterise the leaching behaviour of a by-product or a recycled material.
Since 2002, EN 1744-3 “Tests for chemical properties of aggregates – Part 3: Preparation of
eluates by leaching of aggregates” has been available. This standardised test method is a tank
test that is suitable for these investigations.
Furthermore, Deliverable N° 23 identifies the contents by mass of tar, sulphur (see Table 5.2)
and airborne particles as potential hazards for reclaimed asphalt (RA). The airborne particles
come within the limits of job safety and are, for this reason, not part of the work of Task 4.3,
which concentrates on product standards for road materials and their potential impact on soil
and water.
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SAMARIS SAM-GE-DE24
Tar, especially coal tar and other tar distillates, was used as a binder in the past in many European countries because its hazard was not then so well known. Amongst other things, the
danger can come from the polycyclic aromatic hydrocarbons (PAHs) which can, on the one
hand, potentially be leached out of the pavement after the construction if contact to water is
existent. One the other hand, fumes can be inhaled by the workers during the heating, for example, in asphalt mixing plants or during work with the hot asphalt on the construction site.
Even skin-contact can be harmful. Benzo(a)pyrene (BaP) is one of the best known PAHs that
is noted for being carcinogenic. Therefore, tar bound materials still present a problem when
treating some reclaimed asphalt (RA).
Different types of test methods exist for detecting tar. They are described in detail, with their
assets and drawbacks, in Deliverable N°23 (SAMARIS, 2005). The most reliable procedure is
to detect the PAH content of a road material. As result, a test for PAH is recommended in deliverable N°23 which is described in Appendix A.
In bituminous binders, sulphur is naturally present in different contents depending on the
origin of the applied crude oil. If it is solid, sulphur is not a hazardous component with regard
to leaching because of its insolubility in water. However, danger can emerge during its use in
asphalt or bitumen if the temperature at which the binder or the asphalt is heated exceeds
about 160 °C (SAMARIS, 2005). In that case, reaction of sulphur in bitumen and the release
of the highly poisonous hydrogen sulphide (H2S) are possible. An after-effect of inhalation of
this gas includes a palsy of the lungs. Moreover, if bituminous binders with a high content of
sulphur are overheated, sulphur dioxide gas (SO2) may be generated which can, in conjunction
with water vapour, cause acid rain. Breathed in, it can produce alterations in pulmonary defences. Based on Deliverable N°23 (SAMARIS, 2005), a test for the determination of sulphur
is given in Appendix B.
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SAMARIS SAM-GE-DE24
6 DRAFTS OF ANNEXES TO PRODUCT STANDARDS
6.1 General
Starting from the considerations discussed above, this chapter proposes drafts for environmental annexes to product standards. As examples for typical product standards, environmental
annexes for hEN 13043, hEN 13108-1, hEN 13108-8, hEN 13242 and EN 13285 have been
drafted.
In addition to these environmental annexes, a separate section deals with possible handling of
tar bound reclaimed road material (TB).
6.2 Draft for an environmental annex on aggregates for bituminous
mixtures
In response to the note in Annex ZA of EN 13043, “Aggregates for bituminous mixtures and
surface dressings for roads and other trafficked areas”, that states “In addition to any specific
clauses relating to dangerous substances contained in this standard there may be other requirements applicable to the products falling within this scope”, the following environmental
annex is proposed:
For natural aggregates, the environmental compatibility is given by default. There is no need
for further testing. The same can be assumed for boiler slag (BS).
For recycled aggregates and industrially produced aggregates, the hazardous characteristics
have to be determined in accordance with Table 6.1 and Table 6.2.
The leaching test shall be carried out in accordance with EN 1744-3. The PAH content shall
be determined in accordance with Appendix A.
Provisions valid at the place of use can be used to assess the suitability of recycled or industrially produced aggregates.
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SAMARIS SAM-GE-DE24
Table 6.1:
Hazardous characteristics to determine for crushed mineral construction
waste (CMCW)
Kind of determination
Leaching test
Content by mass
†
‡
*
(X)
Hazardous characteristic
CMCW
pH − value
(X)
El. conductivity
(X)
Chloride
X
Sulphate
X
Chromium VI
X
EOX
X
Hydrocarbons †
X
PAH (EPA) *
X
PCDD ‡
X
PCB ‡
X
only hydrocarbons not originated from bitumen
only if susceptible
Environmental Protection Agency of USA
values to determine for information only
Table 6.2:
Hazardous characteristics for industrially produced aggregates to determine
within a leaching test
Hazardous characteristic
pH − value
El. conductivity
Sulphate
Vanadium
Chromium tot.
Arsenic
Cadmium
CBF slag
VBF slag
BOF slag
EAF slag
CFA
(X)
(X)
X
(X)
(X)
X
(X)
(X)
(X)
(X)
X
X
X
X
(X)
(X)
X
X
X
X
X
(X) = values to determine for information only
The format of this annex is shown in Appendix C.
Concerning this product standard, it would be reasonable to amend the present annex ZA with
relevant information concerning hazardous characteristics as mentioned above.
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6.3 Draft for an environmental annex on asphalt concrete
In response to Note 1 in Annex ZA in prEN 13108-1, “Bituminous mixtures – Material specification – Part 1: Asphalt concrete”, which is similar to the text of Annex ZA of hEN 13043 given above, the following environmental annex is proposed:
If industrially produced aggregates or recycled aggregates are to be used for the production
of asphalt concrete, these aggregates shall fulfil the environmental specifications according to
the environmental annex of EN 13043.
If reclaimed asphalt is to be used for the production of asphalt concrete, the reclaimed asphalt
shall fulfil the environmental specifications according to the environmental annex of
EN 13108-8.
The format of this annex is shown in Appendix D.
Concerning this product standard, it would be reasonable to amend the present annex ZA with
the relevant information concerning hazardous characteristics as mentioned above.
6.4 Draft for an environmental annex on reclaimed asphalt
According to the definition of reclaimed asphalt in hEN 13108-8, “Bituminous mixtures – Material specification – Part 8: Reclaimed asphalt”, the presence of tar in reclaimed asphalt is not
permitted. However, clause 4.2.1 of hEN 13108-8 requires the type of binder to be documented and declared. Therefore, the following environmental annex is proposed:
For proving the binder consists solely of bitumen in reclaimed asphalt, information about the
construction of the road (i.e. files or documentation of the construction time, or former results
of quality control) can be applied.
In case of doubt, the PAH (EPA) content shall be determined in accordance with Appendix A
and the phenol index after a leaching test shall be determined in accordance with EN 1744-3.
If a content of 30 mg PAH/kg of reclaimed asphalt and a phenol index of 0,1 mg/l are not exceeded, it can be assumed that the reclaimed asphalt does not contain tar.
In case of doubt, the content of sulphur shall be determined and declared according to Appendix B.
The format of this annex is shown in Appendix E.
Concerning this product standard, it would be reasonable to amend the present annex ZA by
relevant information concerning hazardous characteristics as mentioned above.
6.5 Draft of environmental annex on aggregates for unbound and
hydraulically bound materials
In response to the note in Annex ZA of hEN 13242, “Aggregates for unbound and hydraulic
bound materials for use in civil engineering work and road construction”, that states “In addi-
22
SAMARIS SAM-GE-DE24
tion to any specific clauses relating to dangerous substances contained in this standard there
may be other requirements applicable to the products falling within this scope” , the following
environmental annex is proposed:
For natural aggregates, the environmental compatibility is given by default. There is no need
for further testing. The same can be assumed for boiler slag (BS).
For recycled aggregates and industrially produced aggregates, the hazardous characteristics
have to be determined in accordance with Table 6.1 and Table 6.2.
The leaching test shall be carried out in accordance with EN 1744-3. The PAH content shall
be determined in accordance with Appendix A.
Provisions valid at the place of use can be used to assess the suitability of recycled or industrially produced aggregates.
The format of this annex is shown in Appendix F.
Concerning this product standard, it would be reasonable to amend the present annex ZA with
the relevant information concerning hazardous characteristics as mentioned above.
6.6 Draft of environmental annex on unbound mixture
specifications
In response to Annex D of EN 13285, “Unbound mixtures – Specifications” that states “It is
the producer’s responsibility to ensure that if any dangerous substances are identified, their
contents do not exceed the limits in force according to the provisions valid in the place of use
of unbound mixture”, the following environmental annex is proposed:
If CE marked industrially produced aggregates or CE marked recycled aggregates should be
used for the production of unbound mixtures, these aggregates have to fulfil the environmental
specifications according to the environmental annex of EN 13242.
If industrially produced aggregates or recycled aggregates without CE marking should be
used for the production of unbound mixtures, these aggregates have to fulfil the environmental
specifications analogously.
The format of this annex is shown in Appendix G.
6.7 Handling tar-bound reclaimed road material
Tar was formerly used as a binder in road constructions. However, that binder has not been
widely used for many years and, in some countries, it is forbidden because of its dangerous
components. Nevertheless, during the re-construction of roads, tar-bound layers are often
found in the road. In that case, the best option is to leave that material in the road, whenever
possible. The alternative is that the tar-bound material has to be deposited at high cost or has
to be re-used as a road material (tar-bound reclaimed road material – TB).
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SAMARIS SAM-GE-DE24
The content of PAH can used to differentiate between TB and RA. As described in Section 6.4, a content of more than 30 mg/kg of RA means that the material is a tar-bound material, at least with tar-containing binder.
Due to the fact that, at higher temperature of about more than 90 C, the PAH emissions are
dangerous for the staff of a hot mixture plant as well as those on the construction site, the TB
should be used in cold mixtures and not re-used in hot mixtures.
In recent years, the cold mixture technique has developed in this area, particularly in some
countries with the in-situ variant (Verbundprojekt, 2004). The usual binders for such cold
mixtures are bitumen emulsion, cement or a combination of both these binders. Initially, the
technique with foamed bitumen was successfully developed (Jenkins, 2000).
Unfortunately, there is no product standard giving specifications for TB. Furthermore,
EN 14260, “Derivatives from coal pyrolysis – Coal tar and pitch based binders and related
products: road tars – Characteristics and test methods”, contains only a common description
of tar binder without any applications.
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SAMARIS SAM-GE-DE24
7 CONCLUSIONS
The goal of Task 4.3 was to draft environmental annexes to the relevant European product
standards for road materials.
From the start of the Construction Product Directive (CPD), one of the essential requirements
has been “Hygiene, health and environment”. This requirement was introduced for the first
generation of European product standards. However, it is the intention of the European
Commission (EC) to implement this essential requirement in the second generation of European standards. The requisite preparations have been made by the EC (Mandate M/366; CEN
2005).
Input from Deliverable N 16 concerning the relevant materials and their hazardous components was considered and supplemented. The materials that have been identified in this deliverable are:
 crystallised blast furnace slag
 vitrified blast furnace slag
 basic oxygen furnace slag
 electric arc furnace slag
 coal fly ash
 boiler slag
 fly ash from lignite combustion
 municipal sold incineration bottom ash
 crushed mineral construction waste
 reclaimed asphalt
 tar bound reclaimed road material.
Test methods proposed in Deliverable N°23 were assumed and imbedded in drafts for environmental annexes for the following product standards for road materials:
 hEN 13043,
 hEN 13108-1,
 hEN 13108-8,
 hEN 13242,
 EN 13285.
The handling with tar-bound reclaimed road material is covered separately. It can be stated
that the re-use of that material is possible but only in cold mixtures in order to avoid air pollution by dangerous components, such as PAH.
The drafts in the Appendices C to F should be a help for people involved in standardisation,
particularly those on CEN Technical Committees TC154, “Aggregates”, and TC227, “Road
materials”.
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SAMARIS SAM-GE-DE24
The Appendices include proposals for the formulation and, if appropriate, tables with definitive hazardous characteristics. With regard to reclaimed asphalt, threshold values are defined
for the content of PAH and the phenol index.
Beyond the recommendations given, there is also a need for standardisation, as supporting
documents, the methods for analysis (e.g. PAH and sulphur in reclaimed asphalt). Proposals
for these methods are given in Deliverable N° 23 (Appendices A and B).
The hope remains that such environmental annexes will expand into the next generation of
road product standards in order to enforce the safety when dealing with industrial by-products
and recycled materials.
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SAMARIS SAM-GE-DE24
8 REFERENCES
Comité Européen de Normalisation (2002). Aggregates for bituminous mixtures and surface treatments for roads, airfields and other trafficked areas. EN 13043: 2002.
Comité Européen de Normalisation (2002). Bituminous mixtures – Material specifications
– Part 8: Reclaimed asphalt. EN 13108-8: 2002.
Comité Européen de Normalisation (2005). Mandate M/366: Development of horizontal
standardized assessment methods for harmonized approaches relating to dangerous substances under the Construction Products Directive.
Comité Européen de Normalisation (2002). Tests for chemical properties of aggregates –
Part 3: Preparation of eluates by leaching of aggregates. EN 1744-3: 2002.
Comité Européen de Normalisation (2003). Derivatives from coal pyrolysis – Coal tar and
pitch based binders and related products: road tars – Characteristics and test methods. EN
14260: 2003.
European Asphalt Pavement Association (2004). Industry statement on the recycling of asphalt mixes and use of waste of asphalt pavements.
European Coal Combustion Products Association eV (2004). Information Bulletin 3, Minerals from Coal – The Green Label.
European Coal Combustion Products Association eV (1997, 1999). Technical Bulletins 1
and 2.
European Economic Community (1988). The Construction Products Directive, Council Directive 89/106/EEC.
FGSV (1993). Merkblatt über die Verwendung von Schmelzkammergranulat im Straßenbau,
Köln (in German).
FGSV (2003). Hinweise zur Verwendung von Braunkohlenflugasche aus Kraftwerken mit
Kohlenstaubfeuerung im Erdbau, Köln (in German).
FGSV (2004). Technische Lieferbedingungen für Gesteinskörnungen im Straßenbau, Köln
(in German).
Jenkins, K J (2000). Mix design considerations for cold and half-warm bituminous mixes
with emphasis on foamed bitumen, University of Stellenbosch.
Knauber, M (1991). Entwicklung eines Verfahrens zur praxisnahen Beurteilung der Umweltverträglichkeit von industriellen Nebenprodukten im Straßenbau (Feldversuche), Bochum
(in German).
Krass et al. (2004). Anfall, Aufbereitung und Verwertung von Recycling-Baustoffen
und industriellen Nebenprodukten im Wirtschaftsjahr 2001, Straße + Autobahn, Bonn (Journal, in German).
Mesters, K (1993). Abschätzung der Mobilisierbarkeit von leichtlöslichen Salzen aus Müllverbrennungsasche am Beispiel eines Lärmschutzwalles, Bochum (in German).
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Radenberg, M (1995). Bewertung der wasserwirtschaftlichen Gefährdung durch pechhaltige
Recycling-Baustoffe im Straßenbau anhand einer numerischen Simulation, Bochum (in German).
REACH (2003). http://www.umweltbundesamt.de/reach/reach.htm
SAMARIS (2005). Critical analysis of documents from Europe and United States with special reference to assessment of alternative materials. Deliverable N° 9.
SAMARIS (2005). Existing specific national regulations applied to material recycling. Deliverable N° 4.
SAMARIS (2005). Literature review of recycling of by-products in road construction in Europe. Deliverable N° 5.
SAMARIS (2005). Methodology for assessing alternative materials for road construction.
Deliverable N° 16.
SAMARIS (2005). Procedures for identifying hazardous component materials for asphalt.
Deliverable N° 23.
Verbundprojekt des Bundesministeriums für Bildung und Forschung (2004). Prozessund Verfahrenstechnik für die umweltschonende Straßensanierung durch Kaltrecycling mit
Schaumbitumen, APS – RUB – SAT – WIRTGEN.
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SAMARIS SAM-GE-DE24
Appendix A: Test for Tar
A1
Scope
This Appendix describes a procedure for the quantitative determination of polycyclic aromatic
hydrocarbons (PAHs) in a binder recovered from recycled asphalt that is suspected of containing tar. This procedure involves two steps: a pre-separation of bitumen samples through application, extraction onto the thin layer chromatography (TLC) plate to the scanning of the fluorescent spots and a quantification of individual PAHs by high pressure liquid chromatography
(HPLC).
A2
Normative references
This method incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text, and the publications
are listed hereafter. For dated references, subsequent amendments to or revisions of any of
these publications apply to this method only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including
amendments).
EN 12594, Bitumen and bituminous binders – Preparation of test samples.
EN 12697-3, Bituminous mixtures – Test methods for hot mix asphalt – Part 3: Bitumen recovery: Rotary evaporator.
EN 12697-4, Bituminous mixtures – Test methods for hot mix asphalt – Part 4: Bitumen recovery: Fractionating column.
NF X 43-329, Stationary source emissions – Sampling and measurement of polycyclic aromatic hydrocarbons and tars at emission.
NIOSH, Method 5506, Issue 3, Polynuclear aromatic hydrocarbons by HPLC.
Amsterdam Method Series AMS 1057-1, Determination of polycyclic aromatic compounds in
condensed bitumen fumes – High performance liquid chromatography method with UVfluorescence and UV-adsorption detection.
A3
Terms and definitions
The following terms and definitions apply:
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A3.1
polycyclic aromatic hydrocarbons (PAHs)
chemicals consisting of a number of benzene rings that are grouped together, some of which
with three to seven (usually four to six) are known to cause, or are suspected of causing, cancer in humans
Note: The samples are analysed for 16 polycyclic aromatic hydrocarbons that are listed as priority
pollutants by the Environmental Protection Agency (EPA)
A3.2
chromatographic processes
separation techniques involving mass-transfer between stationary and mobile phases
A3.3
thin layer chromatography (TLC)
a sophisticated method of separating mixtures of two or more compounds in which separation
is accomplished by the distribution of the mixture between two phases (stationary and moving) on the principle that different compounds will have different solubilities and adsorptions
to the two phases between which they are to be partitioned
Note: TLC is a solid-liquid technique in which the two phases are a solid (stationary phase) and a
liquid (moving phase). The solids most commonly used in chromatography are silica gel (SiO2 x
H2O) and alumina (Al2O3 x H2O). Both of these adsorbents are polar, but alumina is more so. Silica
is also acidic whilst alumina is available in neutral, basic or acidic forms. TLC is a sensitive, fast,
simple and inexpensive analytical technique. It is a micro technique in that as little as 10-9 g of material can be detected, although the sample size is from 1 to 100x10-6 g. TLC involves spotting the
sample to be analysed near one end of a sheet of glass or plastic that is coated with a thin layer of an
adsorbent. The sheet, which can be the size of a microscope slide, is placed on end in a covered jar
containing a shallow layer of solvent. Differential partitioning occurs between the components of the
mixture dissolved in the solvent and the stationary adsorbent phase as the solvent rises by capillary
action up through the adsorbent. The more strongly a given component of a mixture is adsorbed onto
the stationary phase, the less time it will spend in the mobile phase and the more slowly it will migrate
up the plate.
A3.4
high performance liquid chromatography (HPLC)
a mode of chromatography that utilises a liquid mobile phase to separate the components of a
mixture
Note: HPLC is the most widely used analytical technique. The components (or analytes) are first dissolved in a solvent and then forced to flow through a chromatographic column under a high pressure.
In the column, the mixture is resolved into its components. The amount of resolution is important,
and is dependent upon the extent of interaction between the solute components and the stationary
phase. The stationary phase is defined as the immobile packing material in the column. The interaction of the solute with mobile and stationary phases can be manipulated through different choices of
both solvents and stationary phases. As a result, HPLC acquires a high degree of versatility not found
in other chromatographic systems and it has the ability to easily separate a wide variety of chemical
mixtures.
30
SAMARIS SAM-GE-DE24
A3.5
ultraviolet/visible detector (UV/Vis)
a chemical compound that interacts with an electromagnetic field
Note 1: Any chemical compound could interact with the electromagnetic field. A beam of the electromagnetic radiation passing through the detector flow-cell will experience some change in its intensity due to this interaction. Measurement of this change is the basis of most optical HPLC detectors.
Radiation absorbance depends on the radiation wavelength and the functional groups of the chemical
compound. An electromagnetic field, depending on its energy (frequency), can interact with electrons
causing their excitation and transfer onto a higher energy level, or it can excite molecular bonds causing their vibration or rotation of the functional group. The intensity of the beam which corresponds to
the possible transitions will decrease while it is passing through the flow-cell. According to the Lambert-Bear law, absorbance of the radiation is proportional to the compound concentration in the cell
and the length of the cell.
Note 2: UV and visible region of the electromagnetic radiation corresponds to the excitation of the
relatively low energy electrons such as pi-electrons, or non-paired electrons of some functional
groups. For example, any compounds which have a benzene ring will show absorbance at 205-225
and 245-265 nm. The latter range corresponds to the excitation of conjugated p-electrons of the benzene ring.
Note 3: The majority of organic compounds can be analysed by UV/VIS detectors. Almost 70 % of
published HPLC analyses are performed with UV/VIS detectors. This fact, plus the relative ease of
its operation, makes the UV detector the most useful and the most widely used liquid chromatography
detector.
A3.6
fluorescence detector
compounds having specific functional groups that are excited by shorter wavelength energy
and emit higher wavelength radiation which is usually measured at right angles to the excitation
Note 1: Fluorescence detectors are probably the most sensitive of the existing modern HPLC detectors. It is possible to detect even a presence of a single analyte molecule in the flow cell. Typically,
fluorescence sensitivity is 10 to 1000 times higher than that of the UV detector for strong UV absorbing materials. Fluorescence detectors are very specific and selective among the others optical detectors, which is normally used as an advantage in the measurement of specific fluorescent species in
samples.
Note 2: About 15 % of all compounds have a natural fluorescence. The presence of conjugated pielectrons especially in the aromatic components gives the most intense fluorescent activity. Also, aliphatic and alicyclic compounds with carbonyl groups and compounds with highly conjugated double
bonds fluoresce, but usually to a lesser degree. Most un-substituted aromatic hydrocarbons fluoresce
with quantum yield increasing with the number of rings, their degree of condensation and their structural rigidity.
Note 3: Fluorescence intensity depends on both the excitation and emission wavelength, allowing selectively detect some components while suppressing the emission of others. The detection of any
component significantly depends on the chosen wavelength and if one component could be detected at
280 ex and 340 em, another could be missed. Most of the modern detectors allow fast switch of the
excitation and emission wavelength, which offer the possibility to detect all the components in the
mixture. For example, in the very important poly-nuclear aromatic chromatogram, the excitation and
emission wavelengths were 280 and 340 nm, respectively, for the first 6 components, and then
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changed to the respective values of 305 and 430 nm; the latter values represent the best compromise
to allow sensitive detection of compounds.
A4
Principle
A weighed sample of suspected tar-containing binder is diluted with dichloromethane and
spots of this binder solution are applied along a horizontal line on a TLC plate. Then the TLCplate with the spots is placed vertically in the chromatography-chamber filled with a layer of
approximately 10 mm of the carrying liquid (70 % n-hexane / 30 % toluene). This liquid will
be vertically adsorbed by the silica gel coating due to its capillary attraction and pass the
spots. The difference in solubility of the binder components will precipitate in various distances from the spots. After dying, the spots can be determined under UV-light with a wavelength of 366 nm (PAH is traceable by the fluorescence of precipitated soluble binder components). After that, the band of silica gel where the spots of PAH are identified is scraped, removed, dissolved in a solvent mixture (equal proportions of dichloromethane and methylic alcohol) and kept in the dark for 2 h. This solution of extracted PAH is then analysed by HPLC
to determine the individual PAH content.
A5
Apparatus
A5.1
Thin layer chromatography kit
including a 200 x 200 mm² glass development tank and lid and TLC preparative plates of
250 m particle and 60 Angstrom pore.
A5.2
Liquid chromatograph
provided with ternary solvent delivery system, variable volume injector, heated column compartment and on-line degasser of solvent.
A5.3
Programmable fluorescence detector
provided with multi-channel output, timed event programmability and low dispersion flowcell.
A5.4
Ultra-violet photo-diode array detector
provided with constant optical band-pass.
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SAMARIS SAM-GE-DE24
A6
Procedure
A6.1
Preparation of bituminous binders
A6.1.1
Recover the suspected tar-containing binder from the reclaimed asphalt pavement in accordance to EN 12697-3 or EN 12697-4 or procedures derived from these norms. Prepare samples
of the recovered bitumen in accordance with EN 12594.
A6.1.2
Place the recovered binder in a solution of dichloromethane with a concentration of 25 g/L.
A6.2
Pre-separation of samples by thin layer chromatography (TLC)
A6.2.1
On a preparative TLC-plate (200 x 200 mm²), coated with a thin layer of silica gel, apply 1 mL
of the binder solution along a horizontal line from 20 mm of the lower plate side. Near this
line, also apply a pilot spot of standard PAHs solution (10 l). Then place the TLC plate under
a hood for 15 min in order to dry off the solvent.
CAUTION: Some of the PAHs in the calibration mixture present a serious risk if incorrectly
handled. Avoid all skin contact by the best possible means.
A6.2.2
Saturate the chromatography-chamber with vapour from the carrying liquid (70 % n-hexane;
30 % toluene) for 1 h in order to decrease the absorption time. Place the TLC-plate with the
two kinds of spots (pilot and sample) vertically in the chromatography-chamber filled with a
layer of approximately 10 mm of the carrying liquid. This liquid will be vertically adsorbed by
the silica gel coating due to its capillary attraction and pass the spots. The difference in solubility of the binder components will precipitate in various distances from the spots. When
100 % of the height of the plate is reached by the carrying liquid (normally in 45 min), dry the
TLC-plate under the hood without ventilation for 30 min to 45 min.
A6.2.3
Determine the spots under UV-light with a wavelength of 366 nm by comparing the migration
distance of the sample and the spot with that of the standard PAHs solution. Scrape, re-move
and dissolve in 12 mL of solvent mixture (equal proportions of dichloromethane and methylic
alcohol) the band of silica gel where the spots of sample PAH were identified and keep them
in the dark for 2 h (to permit the transfer of PAHs from the silica gel to the solvent mixture
and to avoid the PAHs damage by the light).
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SAMARIS SAM-GE-DE24
A6.3
Quantitative determination of PAH levels by HPLC
A6.3.1
Take 1,5 mL of the solution floating on the surface and filter it through a 0,45 m syringe filter. After that, directly inject 5 l of the solution into the HPLC.
Note: The procedure is considered the best way to eliminate the silica in order to leave only the PAHs
in solution.
A6.3.2
Set up the HPLC with the following parameters:
 Waters PAH column (250 mm length x 4,6 mm internal diameter, C18 stationary phase and
5 m of particle size).
 Column temperature of 30 °C.
 Flow rate of 1,5 mL/min.
 Mobile phase gradient (water – distilled, deionised, degassed – and acetonitrile – HPLC
grade, degassed):
o 0 min
50 % acetonitrile / 50 % water.
o 5 min
50 % acetonitrile / 50 % water.
o 20 min
100 % acetonitrile.
o 28 min
100 % acetonitrile.
o 32 min
50 % acetonitrile / 50 % water.
o 46 min
50 % acetonitrile / 50 % water.
 Detectors type:
o UV detector at 254 nm.
o Fluorescence detector results with an optimisation of excitation/emission wavelengths
for each PAH as given in Table A.1.
 Analysis time of 46 min.
 Calibration undertaken weekly by external standard (16 PAHs test mixture – EPA 610 Polynuclear Aromatic Hydrocarbons, Supelco, N° 4S8743 or equivalent, provided with a certificate of analysis).
 An injected volume of 5 l.
A6.3.3
Allow the chromatograph and detectors to stabilise for 1 h prior to analysis, according to the
operating conditions in A6.3.2.
A6.3.4
Inject 5 L of the calibration mixture with different known concentrations and draw calibration curves for each detector and each PAH.
A6.3.5
Inject 5 L of the sample solutions.
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SAMARIS SAM-GE-DE24
Table A.1: Fluorescence detector results
Analyte
Excitation wavelength Emission wavelength
(nm)
(nm)
Naphthalene
224
330
Acenaphthylene
224
330
Acenaphthene
270
323
Fluorene
270
323
Phenanthrene
260
380
Anthracene
260
380
Fluoranthene
270
400
Pyrene
270
400
Benzo(a)anthracene
270
385
Chrysene
270
385
Benzo(b)fluoranthene
280
410
Benzo(k)fluoranthene
280
410
Benzo(a)pyrene
280
410
Dibenzo(a,h)anthracene
270
466
Benzo(g,h,i)perylene
270
466
Indeno(l 2,3-c,d)pyrene
270
466
A6.3.6
Calibrate and quantitate the unknown samples by measuring peak heights for each elute and
calculate the corresponding amount in the sample (necessity of applying dilution factor in calculations to take account of the different steps of sample pre-separation).
A6.3.7
Repeat steps A6.1 to A6.3.6 twice.
A6.3.8
Calculate the PAHs content as the average of the two (or three) individual values.
A6.4
Expression of results
A6.4.1
Express the content of each PAH detected in HPLC in percent or in concentration.
A6.4.2
Express the results by applying the PAH-16 list as defined by the Environmental Protection
Agency (EPA) in the USA (EPA 610 Polynuclear Aromatic Hydrocarbons).
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SAMARIS SAM-GE-DE24
A7
Test report
The PAHs levels determination report shall contain at least the following information:
a) A reference to this test method.
b) The type and identification of the sample under this procedure.
c) The HPLC test conditions, including column type, temperature, injection volume, mobile
phase and detectors type.
d) Any deviation, by agreement or otherwise, from the procedure specified.
e) The date of the procedure.
A8
Precision
This proposal for a test procedure is under development and no precision is currently available. It will have to be determined in an inter-laboratory test.
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SAMARIS SAM-GE-DE24
Appendix B: Test for Sulphur
B1
Scope
This Appendix describes a procedure for the quantitative determination of the total sulphur in
bituminous binders recovered from recycled asphalt (RA). This procedure involves emulsifying bitumen in water before the analysis by Inductively Coupled Plasma – Atomic Emission
Spectrometry.
B2
Normative references
This method incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text, and the publications
are listed hereafter. For dated references, subsequent amendments to or revisions of any of
these publications apply to this method only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including
amendments).
EN 12594, Bitumen and bituminous binders – Preparation of test samples.
EN 12697-3, Bituminous mixtures – Test methods for hot mix asphalt – Part 3: Bitumen recovery: Rotary evaporator.
EN 12697-4, Bituminous mixtures – Test methods for hot mix asphalt – Part 4: Bitumen recovery: Fractionating column.
B3
Terms and definitions
The following terms and definitions apply:
B3.1
inductively coupled plasma – atomic emission spectrometry (ICP-AES)
technique for elemental analysis in which a plasma source is used to dissociate the sample into
its constituent atoms or ions, exciting them to a higher energy level
Note 1: ICP-AES is one of the most common techniques for elemental analysis. Its high specificity,
multi-element capability and good detection limits result in the use of the technique in a large variety
of applications. All kinds of dissolved samples can be analysed, varying from solutions containing
high salt concentrations to diluted acids.
Note 2: A plasma source is used to dissociate the sample into its constituent atoms or ions, exciting
them to a higher energy level. They return to their ground state by emitting photons of a characteristic
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SAMARIS SAM-GE-DE24
wavelength depending on the element present. This light is recorded by an optical spectrometer.
When calibrated against standards, the technique provides a quantitative analysis of the original sample.
B4
Principle
In the ICP-AES, a plasma source is used to make specific elements emit light, after which a
spectrometer separates this light in the characteristic wavelengths. A solid sample is normally
first dissolved and mixed with water but, in the case of a bituminous binder, it is emulsified in
water, made of two phases: xylene and distilled water with a non-ionic surfactant (Triton X® 100). The stabilised bitumen emulsion is then transformed into an aerosol by a socalled nebuliser. The bigger droplets are separated from the smallest in a specially spraychamber. The smallest droplets (1-10 m) are transferred by an argon flow into the heart of the
ICP-AES, the argon plasma. The bigger droplets (>90 %) are pumped to waste.
Note 1: The bitumen/water emulsion avoids the use of aromatic solvent in ICP-AES, which can result
in specific analysis conditions and special pump tubing that are not easy problems for a typical laboratory to overcome. Moreover, the ICP-AES is robust enough to allow direct analysis of liquids.
In the plasma, a lot of energy is transferred to the nebulised sample that is decomposed, atomised and ionised, promoting the excitation of atoms and ions electrons to higher energy levels.
When these excited atoms and ions return to their ground state or to lower excitation states
they will emit electromagnetic radiation in the ultra-violet/visible range of the spectrum. Each
excited element emits specific wavelengths, i.e. has a typical emission spectrum. The intensity
of the radiation is proportional to the element concentration.
Note 2: Commercially available standards can be used to calibrate the ICP-AES, which makes it possible to perform highly quantitative analysis.
B5
Apparatus
B5.1
Inductively coupled plasma – atomic emission spectrometer (ICP-AES)
provided with different parameters and specifications given in Table B.1.
Table B.1: Parameters specified for ICP-AES
Parameter
Mounting
Focal length
Specification
Czerny-Turner
Parameter
Grating number of grooves
st
Specification
2400 g/mm
0,64 m
1 order resolution
0,025 nm
Thermoregulation
Yes
2nd order resolution
0,012 nm
Nitrogen purge
Yes
Order
2nd order
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SAMARIS SAM-GE-DE24
B6
Procedure
B6.1
Sample preparation
B6.1.1
Recover the suspected sulphur-containing binder from the reclaimed asphalt pavement in accordance to EN 12697-3 or EN 12697-4 or procedures derived from these norms. Prepare
samples of the recovered bitumen in accordance with EN 12594.
B6.1.2
Weigh 1,5 g of recovered binder into a 100 mL beaker and dissolve in 5 mL of xylene. Accelerate the dissolution by using an ultrasonic bath. After complete dissolution, add 2 mL of Triton X® 100 in drops with continuous magnetic agitation. In the same manner, add 25 mL of
distilled water. Place the emulsion into a 100 mL flask, rinse the beaker several times with distilled water and fill the flask with water to 100 mL.
Note: The emulsion is fully prepared when no adherence occurs on the beaker walls.
B6.1.3
Repeat step B6.1.1 twice.
B6.1.4
Prepare three control samples in the same manner as step B6.1.1 except using sulphur instead
of the binder recovered from RA.
Note: The emulsion particle sizes are about 10 m and it is recommended not to analyse the emulsion
after 5 days.
B6.2
Operating conditions for ICP-AES
Operate the ICP-AES using the conditions given in Table B.2 for both the test and control
samples.
Table B.2: Operating conditions for ICP-AES
Parameters
Conditions
Parameters
RF Generator power
1200 W
Sample uptake
Plasma gas flow rate
18 L/min
Type of nebuliser
Auxiliary gas flow rate
0,6 L/min
Type of spray chamber
Sheath gas flow rate
0,4 L/min
Argon humidifier
Nebuliser flow rate
1,4 bars
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Injector tube diameter
Conditions
1,2 mL/min
Concentric (TR-50-C3)
Scott
No
3,0 mm
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SAMARIS SAM-GE-DE24
B6.3
Wavelength selection and analytical conditions (ICP-AES)
Use the line with the highest sensitivity for analysis of sulphur. The slits are 30 x 50 m, the
analysis mode is Gaussian and the integration time is 0,6 s.
Note: The highest sensitivity can be used because there should be no problems with interferences.
B7
Expression of results
Measure the sulphur contents of both the test and control samples after the three different
emulsion preparations, with the concentration given as the mean value of 5 measurements.
Note: The content of sulphur analysed by ICP-AES is given in concentration (mg/kg or ppm).
B8
Test report
The sulphur determination report shall contain at least the following information:
a) A reference to this Test Method.
b) The type and identification of the sample under this procedure.
c) The sample preparation conditions, including the surfactant type and weight of the bitumen
taken for the emulsion.
d) the analytical conditions of ICP-AES measurements.
e) Any deviation, by agreement or otherwise, from the procedure specified.
f) The date of the procedure.
B9
Precision
This proposal for a test procedure is under development and no precision is currently available. It will have to be determined in an inter-laboratory test.
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SAMARIS SAM-GE-DE24
Appendix C: Annex to EN 13043
Environmental Annex
to EN 13043 “Aggregates for bituminous mixtures and surface treatments for roads, airfields and other trafficked areas”
(normative)
With reference to the essential requirement “Hygiene, health and environment” of the “Construction Product Directive” (CPD), aggregates have to comply with the following specifications.
For natural aggregates, the environmental compatibility is given by default. There is no need
for further testing. The same can be assumed for boiler slag (BS).
For recycled aggregates and industrially produced aggregates, the hazardous characteristics
have to be determined in accordance with Table C.1 and Table C.2.
Table C.1: Hazardous characteristics to determine for crushed mineral construction
waste (CMCW)
Kind of determination
Leaching test
Content by mass
†
‡
*
(X)
Hazardous characteristic
CMCW
pH − value
(X)
El. conductivity
(X)
Chloride
X
Sulphate
X
Chromium VI
X
EOX
X
Hydrocarbons †
X
PAH (EPA) *
X
PCDD ‡
X
PCB ‡
X
only hydrocarbons not originating from bitumen
only if susceptible
Environmental Protection Agency of USA
values to determine only for information
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SAMARIS SAM-GE-DE24
Table C.2: Hazardous characteristics for industrially produced aggregates to determine within a leaching test
Hazardous characteristic
pH − value
El. conductivity
Sulphate
Vanadium
Chromium tot.
CBF slag
VBF slag
BOF slag
EAF slag
CFA
(X)
(X)
X
(X)
(X)
X
(X)
(X)
(X)
(X)
X
X
X
X
(X)
(X)
X
X
X
X
X
Arsenic
Cadmium
(X) = values to determine only for information
The leaching test shall be carried out in accordance with EN 1744-3. The PAH content shall
be determined in accordance with (Appendix A).
Provisions valid at the place of use can be used to assess the suitability of recycled or industrially produced aggregates.
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SAMARIS SAM-GE-DE24
Appendix D: Annex to EN 13108-1
Environmental Annex
to EN 13108-1 “Bituminous mixtures – Material specifications –
Part 1: Asphalt concrete”
(normative)
With reference to the essential requirement “Hygiene, health and environment” of the “Construction Product Directive” (CPD), aggregates have to comply with the following specifications.
If natural aggregates are to be used for the production of asphalt concrete, the environmental
compatibility is given by default. There is no need for further testing. The same can be assumed for boiler slag (BS).
If industrially produced aggregates or recycled aggregates are to be used for the production of
asphalt concrete, these aggregates shall fulfil the environmental specifications according to the
environmental annex of EN 13043.
If reclaimed asphalt is to be used for the production of asphalt concrete, the reclaimed asphalt
shall fulfil the environmental specifications according to the environmental annex of
EN 13108-8.
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Appendix E: Annex to EN 13108-8
Environmental Annex
to EN 13108-8 “Bituminous mixtures – Material specifications –
Part 8: Reclaimed asphalt”
(normative)
With reference to the essential requirement “Hygiene, health and environment” of the “Construction Product Directive” (CPD), aggregates have to comply with the following specifications.
For proving the binder consists solely of bitumen in reclaimed asphalt, information about the
construction of the road (i.e. files or documentation of the construction time, or former results
of quality control) can be applied.
In case of doubt, the PAH (EPA) content shall be determined in accordance with (Appendix A)
and the phenol index after a leaching test shall be determined in accordance with EN 1744-3.
If a content of 30 mg PAH/kg of reclaimed asphalt and a phenol index of 0,1 mg/l are not exceeded, it can be assumed that the reclaimed asphalt does not contain tar.
In case of doubt, the content of sulphur shall be determined and declared according to (Appendix B).
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Appendix F: Annex to EN 13242
Environmental Annex
to EN 13242 “Aggregates for unbound and hydraulically bound materials for use in civil
engineering work and road construction”
(normative)
With reference to the essential requirement “Hygiene, health and environment” of the “Construction Product Directive” (CPD), aggregates have to comply with the following specifications.
For natural aggregates, the environmental compatibility is given by default. There is no need
for further testing. The same can be assumed for boiler slag (BS).
For recycled aggregates and industrially produced aggregates, the hazardous characteristics
have to be determined in accordance with Table F.1 and Table F.2.
Table F.1:
Hazardous characteristics to determine for crushed mineral construction
waste (CMCW)
Kind of determination
Leaching test
Content by mass
†
‡
*
(X)
Hazardous characteristic
CMCW
pH − value
(X)
El. conductivity
(X)
Chloride
X
Sulphate
X
Chromium VI
X
EOX
X
Hydrocarbons †
X
PAH (EPA) *
X
PCDD ‡
X
PCB ‡
X
only hydrocarbons not originating from bitumen
only if susceptible
Environmental Protection Agency of USA
values to determine only for information
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Table F.2:
Hazardous characteristics for industrially produced aggregates to determine within a leaching test
Hazardous characteristic
pH − value
El. conductivity
Sulphate
Vanadium
Chromium tot.
Arsenic
Cadmium
CBF slag
VBF slag
BOF slag
EAF slag
CFA
(X)
(X)
X
(X)
(X)
X
(X)
(X)
(X)
(X)
X
X
X
X
(X)
(X)
X
X
X
X
X
(X) = values to determine only for information
The leaching test shall be carried out in accordance with EN 1744-3. The PAH content shall
be determined in accordance with (Appendix A).
Provisions valid at the place of use can be used to assess the suitability of recycled or industrially produced aggregates.
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SAMARIS SAM-GE-DE24
Appendix G: Annex to EN 13285
Environmental Annex
to EN 13285 “Unbound mixtures - Specifications”
(normative)
With reference to the Annex D the dangerous substances in the aggregates of the unbound
mixture have to be identified as follows:
If natural aggregates are to be used for the production of unbound mixtures, the environmental
compatibility is given by default. There is no need for further testing. The same can be assumed for boiler slag (BS).
If CE marked industrially produced aggregates or CE marked recycled aggregates should be
used for the production of unbound mixtures, these aggregates have to fulfil the environmental specifications according to the environmental annex of EN 13242.
If industrially produced aggregates or recycled aggregates without CE marking should be used
for the production of unbound mixtures, these aggregates have to fulfil the environmental
specifications analogously.
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SAMARIS SAM-GE-DE24
Figures
Figure 2.1: Proceeding – Flow chart ........................................................................................... 2
Figure 3.1: The typical road structure ......................................................................................... 5
Tables
Table 3. 1: Selected industrial by-products ................................................................................4
Table 3.2: Selected recycled materials ...................................................................................... 5
Table 3.3: Essential chemical constituents of crystallised blast furnace
slag (REACH, 2003) ................................................................................................ 6
Table 3.4: Essential chemical constituents of basic oxygen furnace slag
(REACH, 2003) .......................................................................................................7
Table 3.5: Essential chemical constituents of electric arc furnace slag
(REACH, 2003) .......................................................................................................8
Table 3.6: Essential chemical constituents of coal fly ash (ECOBA,
1997; 1999) ..............................................................................................................8
Table 3.7: Essential chemical constituents of boiler slag (FGSV, 1993) ..................................9
Table 3.8: Essential chemical constituents of fly ash from lignite
combustion in some European countries................................................................ 10
Table 3.9: Range of components in processed municipal solid waste
incinerator bottom ash (FGSV, 2005) ....................................................................10
Table 3.10: Objective requirements for components in crushed mineral
construction waste (FGSV, 2004)........................................................................... 11
Table 4.1: Identification of appropriate European Product Standards for
binder, aggregates and their bituminous mixtures..................................................14
Table 4.2: Identification of appropriate European Product Standards for
aggregates and hydraulically bound and unbound mixtures ..................................15
Table 5.1: Decisive hazardous characteristics for industrial by-products ............................... 17
Table 5.2: Decisive hazardous characteristics for recycled materials .....................................18
Table 6.1: Hazardous characteristics to determine for crushed mineral
construction waste (CMCW) .................................................................................21
Table 6.2: Hazardous characteristics for industrially produced
aggregates to determine within a leaching test ....................................................... 21
Table A.1: Fluorescence detector results .................................................................................35
Table B.1: Parameters specified for ICP-AES .........................................................................38
Table B.2: Operating conditions for ICP-AES ........................................................................39
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SAMARIS SAM-GE-DE24
Table C.1: Hazardous characteristics to determine for crushed mineral
construction waste (CMCW) ................................................................................. 41
Table C.2: Hazardous characteristics for industrially produced aggregates to determine within a leaching test ............................................................... 42
Table F.1: Hazardous characteristics to determine for crushed mineral
construction waste (CMCW) ................................................................................. 45
Table F.2: Hazardous characteristics for industrially produced aggregates to determine within a leaching test ............................................................... 43
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