This
report
describes
test
procedures and techniques used by the
CEAMaS
partners
to
characterize
sediments and to identify possible reuse in
civil engineering applications.
WP2-A6
DEFINITION OF
CHARACTERIZATION
METHODS
PHYSICAL, GEOTECHNICAL AND
CHEMICAL CHARACTERIZATION OF
MARINE SEDIMENTS REGARDING THEIR
USE FOR CIVIL ENGINEERING
APPLICATIONS
STANDARDS & METHODOLOGIES
CEAMaS WP2.6 REPORT
ECOLE CENTRALE DE LILLE
DELFT UNIVERSITY OF TECHNOLOGY
BRGM
CORK INSTITUTE OF TECHNOLOGY
October 2015
DEFINITION OF CHARACTERIZATION METHODS / October 2015
1
Summary
Introduction ................................................................................................................................ 4
I. Physical characterization ........................................................................................................ 5
I.1. Appearance ....................................................................................................................... 5
I.2. Water content ................................................................................................................... 6
I.3. Solid grain density ............................................................................................................ 7
I.4. Specific surface area ......................................................................................................... 7
I.4.1. Methylene blue sorption ............................................................................................ 7
I.4.2. Brunauer, Emmett and Teller (BET) method ............................................................ 8
I.5. Grain size distribution ...................................................................................................... 9
II. Geotechnical characterization.............................................................................................. 10
II.1. Atterberg limits test....................................................................................................... 10
II.2. Proctor compaction test................................................................................................. 12
II.3. Permeability test............................................................................................................ 13
II.4. California Bearing Ration test ...................................................................................... 14
II.5. Shear box test ................................................................................................................ 14
II.6. Oedometer test .............................................................................................................. 15
II.7. Unsaturated hydraulic conductivity .............................................................................. 16
III. Mineralogical and Chemical characterization .................................................................... 17
III.1. Sulphur......................................................................................................................... 18
III.2. Chloride total ............................................................................................................... 18
III.3. pH ................................................................................................................................ 18
III.4. Leaching ...................................................................................................................... 19
III.5. Determination of Calcium Carbonate content ............................................................. 20
III.6. Organic content............................................................................................................ 20
III.7. Total organic carbon .................................................................................................... 21
III.8. Concentration of trace metals ...................................................................................... 21
III.9. Concentration of organic pollutants ............................................................................ 24
III.10. Bio available fraction of organic pollutants .............................................................. 25
III.11. Mineral composition (XRD) ...................................................................................... 27
III.12. On-site analysis.......................................................................................................... 27
III.12.1. pXRF (portable X-ray fluorescence)................................................................... 28
III.12.2. Multiparametric water quality probe .................................................................. 28
DEFINITION OF CHARACTERIZATION METHODS / October 2015
2
III.12.3. FTIR (portable Fourier Transform mid-InfraRed spectroscopy) ........................ 29
III.12.4. µRaman (portable micro Raman spectroscopy) .................................................. 29
III.13. Mineral fractions composition (grain size chemistry) ............................................... 30
III.13.1. Grain size chemistry in the laboratory ................................................................ 30
III.13.2. Grain size chemistry on site ................................................................................ 31
III.14. TUD specific tests ..................................................................................................... 31
IV. Complementary characterization ....................................................................................... 33
IV.1. TGA ............................................................................................................................. 33
IV.2. Sorption and desorption test ........................................................................................ 34
IV.3. Thermal conductivity test ............................................................................................ 35
IV.4. Zeta Potential ............................................................................................................... 36
IV.5. In situ field equipment ................................................................................................. 38
IV.5.1. Pore pressure sensors ............................................................................................ 38
IV.5.2. Zakbaak ................................................................................................................. 38
IV.5.3 Density by thermal conductivity ............................................................................ 39
References ................................................................................................................................ 40
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Introduction
In the CEAMaS project, the WP2’s objective is to characterize sediments through a set
of techniques and to identify possible reuse in civil engineering applications for these
sediments. These techniques were performed following standards, which vary from one
country to another: any partner used its local ones or European ones.
Sediments were collected in each of the partner countries of the CEAMaS project, split in
equal representative parts and redistributed among the partners for laboratory analysis. Tests
which were performed in laboratories cover a wide range of physical, geotechnical and
chemical tests of which some are commonly performed to evaluate sediments. In fact, Ecole
Centrale de Lille (ECL) and BRGM, both from France, collaborate actively to this
characterization (physical, geotechnical, complementary and chemical tests) according to the
French and European Standards. Cork Institute of Technology (CIT) undertook physical and
geotechnical testing according to the British Standards. And Delft University of Technology
(TUD) achieved physical, geotechnical and chemical tests according to European and Dutch
Standards.
This report aims to describe test procedures and techniques used by the CEAMaS partners
quoted above, with the physical characterization in the first part, the geotechnical
characterization in the second part, complementary tests in the third part and the chemical
characterization in the fourth part (Figure 1).
Figure 1. Marine Sediment Test Categories
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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I. Physical characterization
Physical tests have been achieved by Ecole Centrale de Lille, CIT and TUD in their
respective Civil Engineering laboratories. Those tests (Figure 2) focus on the sediment matter,
giving its general features. They identify general sediment properties including water content,
density, specific surface area and grain size distribution.
Figure 2. Diagram showing the physical characterization techniques
I.1. Appearance
Sediments from four different locations in four different countries were investigated. Table 1
presents the appearance of the different sediments.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Table 1. Appearance of the studied sediments
Origin
Reference
Appearance
France
DS
Clayey aspect, dark grey
colour, smells bad.
Belgium
AS
Clayey aspect, dark brown
colour, smells bad.
LS
Clayey aspect, high organic
matter content, very dark
brown, smells bad.
CS
Silty sandy grain distribution,
presence of shell debris,
brown colour, smells very
bad.
The Netherlands
Ireland
Photo
I.2. Water content
For sediment, water content may be an extremely important index. For example, the
consistency of a fine-grained sediment largely depends on its water content. Ecole Centrale de
Lille determined the water content of sediments by drying samples at 40°C according to the
French Standard NF P 94-050 [1]; but in order to have a wider scope, ECL also dried samples
at 60°C and 105°C. Such a process is compliant with TUD‘s one who dried samples at 105 °C
during 24 hours, in accordance with the European standard NEN 15934:2012 [2]. CIT also
dried the sediment at 105°C in accordance with the British Standard BS 1377-2 [3].
The water content is calculated as the ratio of the mass of water to the mass of solid grains in
a sample, as presented in Equation (1). It is denoted by ω and expressed in percentage.
(%) 
Mh  Md
Md
(1)
Where:
DEFINITION OF CHARACTERIZATION METHODS / October 2015
6
: Mass of the humid sample
: Mass of the dried sample.
I.3. Solid grain density
The solid grain density presents the weight of the solid sediment particles per unit volume of
the solid phase, regardless of voids between the grains. Ecole Centrale de Lille and CIT
determined it using a Helium pycnometer, presented in Figure 3.
Figure 3. Pycnometer AccuPyc 1330
I.4. Specific surface area
The specific surface area is an important property for the characterization of clayey materials.
It is used to understand the behavior of sediments in the phenomena of shrinkage and
swelling, and cations exchange capacity. The specific surface area can be determined through
the following two sorption techniques: methylene blue sorption and Brunauer, Emmett and
Teller (BET) method [4].
I.4.1. Methylene blue sorption
This method determines the total area of ions exchange between the clay fraction and
methylene blue molecules. It essentially comprises the outer surface which is between the
clay particles and the corresponding inner surface in the interlayer space. The test measures
the amount of methylene blue that can be adsorbed by the sediment suspended in water. Ecole
Centrale de Lille recognized the maximum sorption when on a filter paper appeared a light
blue aureole around the spot made by the solution (Figure 4). With the French Standard NF P
94-068 [5], VBS (a coefficient linked to methylene blue concentration) is determined and
DEFINITION OF CHARACTERIZATION METHODS / October 2015
7
allows to deduce the specific surface area. The specific surface area (Ss) can be calculated
from the following equation of Santamarina and al [6].
(2)
Where:
: Specific surface, in m2/g
: Value obtained through the spot method.
: Blue content of the titration solution (= 10 g / ml).
: Avogadro's number (6.02 x 1023 atoms / mol).
:
Area covered by a methylene blue molecule (130 Ų).
Figure 4. Methylene blue test
I.4.2. Brunauer, Emmett and Teller (BET) method
This method determines the volume of dinitrogen (N2) adsorbed by the low temperature
sample. The principle of the test is based on the sorption isotherm theory of multilayer gas
which has been developed by Brunauer, Emmett and Teller (BET) in 1983. This technique
permits to measure only the external surface area, as the gas used can not penetrate into the
layers of the clay. The equipment used in the test performed by Ecole Centrale de Lille is
Micromeritics ASAP 2010 (Figure 5).
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 5. BET ASAP 2000
I.5. Grain size distribution
Particle size analysis shows the percentage distribution of solid particles according to their
size. CIT performed particle size analysis by undertaking wet sieving and the hydrometer test.
First the material was washed through a 63 µm sieve. The material larger than 63 µm was
dried (105 °C) and sieved through a range of sieve sizes (75 mm to 63 µm). The material less
than 63 µm was washed into a container and left to settle. Once settled the water was
siphoned off and the material was oven dried at 105 °C. The sediment less than 63 µm was
used in the hydrometer test to identify the grain size distribution of the sediment less than 63
µm. The tests were undertaken in accordance with BS 1377-2 [3].
On the other hand, the Mastersizer 2000 (Figure 6), used by ECL and TUD, determines the
size of particles by measuring the intensity of light scattered as a laser beam passes through a
dispersed particulate sample in a liquid. The light scattered by the particles at various angles
is measured by a multi-element detector and numerical values relating to the scattering pattern
are then recorded for an analysis, using an appropriate optical model and mathematical
procedure to yield the proportion of total volume to a discrete number of size classes forming
a volumetric particle size distribution.
Figure 6. The laser particle sizer Malverne Mastersizer 2000
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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II. Geotechnical characterization
Geotechnical tests have been performed by Ecole Centrale de Lille, CIT and TUD in
their Civil Engineering laboratories (Figure 7). They allow us to know which behaviour the
sediments would have if related to civil engineering applications (roads, railways, canals,
bridges and viaducts, tunnels, dams, wells and boreholes, quarries, buildings ...). They are as
follows: Atterberg limits test, determination of calcium carbonate content, Proctor compaction
test, permeability test, California Bearing Ratio test, shear box test, odometer test, and organic
content.
Figure 7. Diagram showing the geotechnical characterization techniques
II.1. Atterberg limits test
The consistency of the sediment varies considerably with its water content. By gradually
decreasing the water content of a sample of saturated sediment, it cycles through several
states:
• The liquid state;
• The plastic state, with the malleable sample;
• The solid state.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
10
The transition from one state to another is at levels that are the plastic limit (from the solid to
plastic state) and the liquid limit (from the plastic state to the liquid state).
ECL determined these limits according to the French standard NF P 94-051 [7]:
 The liquid limit (LL) by Casagrande method (Figure 8) is determined by
extending on a cup a layer of material in which a groove is drawn through a Vshaped instrument and by printing to the cup similar shocks until the groove is
closed over 1 cm. The process ought to be repeated with different water
contents for a number of shocks between 15 and 35. The liquid limit is the
water content of the sample with a number of shocks equal to 25. Because it is
difficult to obtain a test with exactly 25 shocks, the procedure is performed
multiple times with a range of water contents and the results are interpolated.
 The plastic limit (PL) is the water content, at which a sediment can no longer
be deformed by rolling into 3.0 mm diameter rolls without crumbling (Figure
9). To make the rolls, we take a humid bull of the sample, then we roll it on a
smooth plate with hand or with another plate. If the 3mm diameter is not
reached with crumbles simultaneously, the sample must be moisturized (when
crumbles appear first) or dried in an oven (when diameter is reached without
crumbles) and homogenized. The operation is repeated until the diameter is
reached and crumbles appear simultaneously.
Figure 8. Liquid limit determination using
Casagrande apparatus
Figure 9. Plastic limit determination by
rolling
CIT determined these limits according to the British Standard BS 1377-2 [3]:
 CIT used the cone penetrometer test to determine the Liquid Limit. In the test,
a sediment sample is placed in a 55 mm diameter, 40 mm deep metal cup. A
stainless steel cone weighing 80 g (including the shaft) and having a 30° angle
is positioned so that its tip just touches the sample. The cone is released for 5
seconds so that it may penetrate the soil. The liquid limit is defined as the
water content of the soil which allows the cone to penetrate exactly 20 mm
DEFINITION OF CHARACTERIZATION METHODS / October 2015
11
during that period of time. Because it is difficult to obtain a test with exactly 20
mm penetration, the procedure is performed multiple times with a range of
water contents and the results are interpolated.
 The plastic limit (PL) is determined by following the same process than ECL
one.
Those limits help to calculate the plasticity index (PI). It is the value obtained by subtracting
the plastic limit from the liquid limit, as presented in Equation (3). This index is important as
it quantifies the range in water content over which the sediment is in plastic state.
(3)
The consistency of a sediment sample is expressed by the liquidity index (LI). The liquidity
index is calculated, as presented in Equation (4), by scaling the natural moisture content to the
liquid limit and plastic limit.
(4)
II.2. Proctor compaction test
The Proctor compaction test determines the optimal water content at which a
given sediment type will become most dense and achieve its maximum dry density. It consists
of compacting sediment at known water content into a cylindrical mould with a hammer at a
given height. The bulk of its characteristics (mass of the hammer, height at which the mass
fall, magnitude of compactive effort, mould size, number of blows and their distribution…) is
resumed in a standard, which in case of ECL is the French Standard NF P94-093 [9] and in
case of TUD is the European Standard NEN-EN 13286-2 [10].
For a better repeatability, ECL used the Controlab automatic proctor device (Figure 10); for a
given standard, it achieves automatically all its specifications. The sediment is usually
compacted into the mold to a certain amount of equal layers, each receiving a number of
blows from a standard weighted hammer at a specified height. This process is then repeated
for various water contents. And the dry densities are determined for each. It is just necessary
to measure the mass of the sample after its drying in a stove and to calculate the volume of the
mould, seen that the sample filled it. The graphical relationship of the dry density to water
content is then plotted to establish the compaction curve. The maximum dry density is finally
obtained from the peak point of the compaction curve and its corresponding water content,
also known as the optimal water content.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 10. Automatic proctor device
II.3. Permeability test
This method, regarding the French Standard NF X 30-442 [11], is used to characterize the
permeability coefficient of the materials used for the containment of waste or contaminated
sediment. It is also used in the fields of civil engineering and hydrogeology in general. ECL
benefited from the expertise of BRGM thanks to M. Boris CHEVRIER, geotechnical engineer
at the BRGM project team specialized in waste containment, characterization and
implementation of fine materials.
The test is performed on a representative sample of the material, placed in a rigid cylindrical
ring. The lower and upper bases are equipped with drainage discs. For a set of loads and for a
stabilized compaction (end of the primary consolidation), the liquid flow is established by
application of variable hydraulic load between the two sides of the specimen (Figure 11). The
determination of the permeability coefficient is done according to the standard quoted above.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 11. Permeater
II.4. California Bearing Ration test
The California Bearing Ratio test is undertaken to determine a relationship between force and
penetration when a cylindrical plunger of standard cross sectional area penetrates the soil at a
given rate. The test was undertaken in accordance with BS1377-4 by CIT [12]. Once the
California Bearing Ratio is determined the ultimate bearing capacity of the soil can be
calculated using the Equation (6).
(5)
Where:
CBR: California Bearing Capacity
qu: Ultimate bearing capacity
II.5. Shear box test
The shear box test is undertaken to calculate the direct shear strength of the sediment. A
square prism of soil is laterally restrained and sheared along a horizontal plane while subject
to a pressure applied. Material was first prepared by drying (105 °C) and sieved through a
3mm sieve. The material passing the sieve was used for the shear box test. By applying
DEFINITION OF CHARACTERIZATION METHODS / October 2015
14
normal pressures of 9.4 kg, 14.4 kg and 19.4 kg the relationship between measured shear
stress at failure and normal applied stress was obtained. The cohesion and friction angle of the
soil was calculated by graphing the results. The test was undertaken in accordance with BS
1377-7 [13].
II.6. Oedometer test
The oedometer test consists in determining the compressibility characteristics of sediment that
estimates compaction of sediment mass. The test is performed on a sample placed in a rigid
cylindrical enclosure (oedometer cell). A device applies to this chamber a vertical axial force,
the specimen being drained top to down and kept saturated during testing. The load is applied
by maintained constant levels successively increasing and decreasing according to a defined
program, specified in our case by the French Standard XP P 94-090-1 [14]. The height
variations of the sample are measured during the test in function of the duration of the load
application. This test has been carried out both manually and automatically, with the GDSlab
oedometer cell, as shown in Figure 12.
By loading and unloading a sample in the oedometer cell, a compressibility curve (which
represents the void index using the effective pressure) is obtained and allows the calculation
of the swelling index Cs. And for a given load, by plotting the height variations in function of
the time, we can express the compression index Cv.
Figure 12. Automatic oedometer and manual oedometer
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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II.7. Unsaturated hydraulic conductivity
The Hydroprop measures the soil moisture characteristic curve in the unsaturated zone and
determines the unsaturated hydraulic conductivity of soil samples, as shown in Figure 13.
Figure 13. Hydroprop
The hydroprop can be used to test the drying and rewetting behaviour of the soil, including
the behaviour of sediment exposed to air and rewetted. This is a typical scenario when
sediment is used on land, in which ripening and dewatering change the structure and hence
moisture behaviour of the sediment.
Figure 14. Hydroprop result, example of change in irreversible drainage of water
(1st drying phase) and different drying behaviour during 2nd drying step.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III. Mineralogical and Chemical characterization
The classification of sediments can also be based on their chemical composition. The
potential use and the allowed disposal methods are linked to these chemical properties with
regard to the presence of different types of pollutants. The focus within the national standards
of most EU member states lies on the concentration of heavy metals and organic pollutants
(mainly PAH’s and PCB’s), although the list of potential environmental threatening
substances is long. The EU Water Framework Directive (WFD) defines 33 priority substances
(http://ec.europa.eu/environment/water/water-framework/priority_substances.htm), with the
option to define waterbody specific substances. Recently, emerging substances like
Tributyltin (TBT), pharmaceuticals (pharma pollutants) and micro plastics, are investigated
and guidelines for monitoring and impact assessment are being implemented (like the OSPAR
criteria for TBT, reference number 2004-15).
The TU Delft and Deltares focused on the currently used list of pollutants for the WFD, with
additional parameters like chloride and sulphide content when required for testing the
suitability for reuse of sediments as building material (currently only allowed within Flanders
and The Netherlands). BRGM performed on-site characterization and chemical
characterization in its analytical laboratory, in order to determine the organic and inorganic
substances content. And CIT achieved the chemical characterization via the National
Laboratory Service in the United Kingdom, insisting on the heavy metal contaminants
(Arsenic, Cadmium, Chromium, Copper, Lead, Mercury, Nickel, Zinc) and organic
contaminants (PCB’s, PAH16, Hexachlorcyclohexane, Hexachlorbenzene, TBT & DBT,
Total Extractable Hydrocarbon, DDT/DDE/DDD, Drins sum).
The figure 15 shows the diagrams summarizing the chemical tests performed in the CEAMaS
project.
In the BRGM laboratory, samples preparation before analysis was done by drying at 40 °C
and then grinding to 250 µm (planetary ring mill) according to NF ISO 11464:2006 [18].
On the other hand, the Dutch normalization of sediment and soils requires that the organic
matter and lutum content (particle fraction < 2 μm) are known. The concentration of metals
and organic pollutants expressed in mg (or μg) per kg dry weight are also required. Therefore
the samples have also been dried for the tests related to TUD laboratory.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 15. Diagram showing chemical characterization techniques
III.1. Sulphur
The sulphur content was determined by dry combustion according to NF ISO 15178:2001
[19]. The sample is heated to a temperature of 800°C in a stream of oxygen-containing gas.
The SO2 arising from the combustion is measured by infrared spectrometry.
III.2. Chloride total
The chloride was extracted using an alkaline fusion. Powdered sample was mixed with
sodium carbonate and was fused in a furnace. The chloride was quantified by potentiometric
method according to Rodier J (1996) [20].
III.3. pH
pH was analysed according to NF ISO 10390:2005 [21]. pH is determined using a glass
electrode in a 1:5 (volume fraction) suspension of sediment in water. The pH of the
suspension is measured using a pH-meter Inolab 7310P.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III.4. Leaching
Within the BRGM laboratory, leaching studies were done following the standard NF EN
12457-2:2002 [22]. Experimental conditions are:
o
o
o
o
o
o
o
liquid to solid ratio of 10 l/kg dry matter
leachant = water
1 time shaking 24 hr
particles < 4 mm
leachate filtered through a 0.45µm filter
dry matter content ratio, 105 °C
Test sample mass corresponding to 0.090 kg ± 0.005 kg of dry mass
In the TUD laboratory, the leaching test is part of the test conducted for reuse of materials
under the Dutch Soil directive (Besluit bodemkwaliteit, regeling bodemkwaliteit). It followed
the Dutch protocol NEN 7373:2004 [23]. In this test protocol the soil/sediment is leached with
a 10 to 1 liquid to solid ratio (L/S 10), taking subsamples of the leaching water to calculate the
total emission (Figure 16).
The leaching column test takes 64 days, with 8 subsamples at given liquid to solid ratios and
prescribed time intervals. To assure that the columns can meet the requirement with regard to
the flux needed in 64 days, the material is first tested on the permeability by forcing the water
flow with a peristaltic pump. If the column pressure builds up to > 2 bar or if the seals are
leaking, the sediment is deluded with 50 % glass beads of 2 mm in diameter. The reduced
sediment mass is then taken into account for the leaching test. The water entering the column
is demineralised water, acidified with Nitric acid to a pH of 4 and a conductivity of
< 1 μS/cm. The pH and conductivity in the eluate water are also measured.
Conservation of the samples and detection of the metals in the leaching water was carried out
by the method described in IV.6 (LA-ICP-MS)).
Figure 16. Leaching columns for NEN 7373:2004 test
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III.5. Determination of Calcium Carbonate content
Calcimeter Bernard method (Figure 17) is used in this work according to the standard NF P
94-048 [8] to determine the percentage of calcium carbonate (CaCO3).
The determination of CaCO3 (%) is based on the volumetric analysis of the carbon dioxide
CO2, which is liberated during the application of hydrochloric acid solution HCl in sediment’s
carbonates and is described with the following reaction:
(CaCO3 + MgCO3 etc.) + 2 HCl → (CaCl2 + MgCl2 etc.) + H2O + CO2 ↑
The presence of calcium carbonate (CaCO3) is established by adding some drops of HCl to
the sediment. The degree of effervescence of carbon dioxide gas is indicative for the amount
of calcium carbonate present.
Figure 17. Bernard Calcimeter
III.6. Organic content
The test is to determine the loss of mass of a sample previously dried, after calcination in an
oven at a temperature of 450 °C. We had to place the crucible in the furnace and raise the
temperature gradually. Each tested sample is maintained for at least 3 hours in the oven at a
temperature between 450 °C and 500 °C. This test was performed by ECL according to the
French standard XP P 94-047 [15].
The organic content is calculated from weighing the crucible and its contents before and after
calcination. The organic content is the arithmetic mean of n samples for analysis and is
expressed as a percentage rounded to the whole number:
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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(6)
Where:
: Content of calcinalted organic matter.
: Mass of the crucible and its content before calcination.
: Mass of the crucible and its content after calcination.
: Mass of the crucible.
: Number of trials.
III.7. Total organic carbon
In the BRGM laboratory, total organic carbon (TOC) was determined according to NF ISO
10694:1995 [24]. Organic Carbon is analysed on a specific C and S analyser, the EMIA 820V
from Horiba company after a pretreatment of the sample with HCl acidification to eliminate
mineral carbon from the sample.
In the TUD laboratory, the organic matter content was measured according to the European
NEN-EN protocol 15935:2012 [25]. This standard requires a number of pretreatment steps.
First, the sample has to be sieved so that only particles > 2 mm are screened out. For
sediments, the pretreatment and sample homogenization are done in accordance with the
Dutch protocol NEN 5719:1999 [26]. The sample is dried for 24 hours at 105 °C, in
accordance with European protocol NEN 15934:2012 [27], to determine the dry weight. A
weighed test portion is burned up in a furnace to constant mass at (550 ± 25) °C. The
difference in mass before and after the ignition process is used to calculate the loss on
ignition.
III.8. Concentration of trace metals
Within the BRGM laboratory, trace metals and metalloids (As, Cr, Ni, Zn, Cd, Cu, Pb) are
analysed after a total sample digestion with a sodium peroxide sinter and an analysis by -ICP-AES (Horiba - Jobin Yvon spectrometer model JY 166) according to standard NF EN ISO
11885:2009 [28]. Hg is analysed on a specific mercury analyser (AMA 254 from Altec) by
amalgam concentration followed by absorption detection. Table 2 presented ICP/AES
analysis lower (LD) and upper analytical limits on samples dehydrated at 450°C – Precision is
relative 10 to 15 % in mid-range.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Table 2. ICP/AES analysis lower (LD) and upper analytical limits on samples
When better detection limits are required, samples can be analysed using ICP/MS:
Table 3. ICP/MS analysis lower analytical limits.
Other methods are available at BRGM laboratories:
- XRF (X-ray fluorescence) on fused discs and/or on pressed pellets. This method is more
precise and complete than ICP/AES for major elements and is also useful for refractory trace
elements, XRF is the emission of characteristic "secondary" (or fluorescent) X-rays from a
material that has been excited by bombarding with high-energy X-rays. The phenomenon is
used for elemental analysis of solids, powders or liquids. It does not depend on the efficiency
of digestion or extraction prior to analysis.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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- AAS (Atomic absorption, by flame: FAAS, graphite furnace: GFAAS, or cold vapor:
CVAAS) for samples exceeding the upper limits for ICP.
Figure 18. X-Ray Fluorescence (XRF) Spectrometer
Within the TUD laboratory, the first step after sample homogenization is the digestion of the
solid matrix with nitric acid and hydrochloric acid (aqua regia) for the determination of the
selected elements. It followed the Dutch protocol NEN-EN 13346:2000 [29] for this step.
This standard was approved by the EU. This standard specifies methods for the extraction,
with aqua regia, of trace elements and phosphorus from sludges and sludge products. The
resulting solution is suitable for the determination of As, Cd, Cr, Cu, Hg, Ni, Pb, Se, Zn and P
using spectrometric techniques. The EU-approved NEN-EN-ISO 17294-2:2004 [30] was
followed for the application of the inductively coupled plasma mass spectrometry (ICP-MS).
Due to the marine conditions, the samples had to be diluted 10 times to keep the matrix
interference within the systems tolerance levels.
Detection was by Laser ablation ICP-MS. This technique is used for the in situ analysis of
trace elements in solid samples. It can determine many elements in the periodic table to high
degrees of accuracy and precision. The technique measures trace elements at a lower
concentration range (1 ppb - 100 ppm).
Solid particles are physically ablated due to the interaction of a high power laser beam (> 1 x
1010 Wcm-2) with the surface of the sample. The particles are carried in a stream of inert gas
(helium or argon) into an argon plasma where they are ionized prior to measurement in a mass
spectrometer. Isotopes are measured to determine elemental concentrations. The TUD
laboratory is equipped with a ThermoFischer Scientific Element 2 magnetic sector ICP-MS
and a Geolas (MicroLas, Goettingen, Germany) 193 nm excimer laser ablation system (Figure
19).
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 19. LA-ICP-MS setup
III.9. Concentration of organic pollutants
Within the BRGM laboratory, the 16 PAH molecules of the US/EPA list are considered,
according to French practice, as representative of the group. These molecules were extracted
using a hot extraction with pressurized fluid according to the French standard XP X 33
012:2000 [31]. PAH 16 were analysed by HPLC-UV-DAD according to NF EN ISO
17993:2004 [32]. The analyses were focused also on the seven PCB indicators (PCBi)—i.e.
PCB Aroclor 28, 52, 101, 118, 138, 153 and 180. For PCB analysis, solids were extracted
according to the French Standard XP X33-012:2000 [33] using hot extraction with
pressurized fluid. PCBs were quantified according to the NF EN ISO 6468:1997 [34] standard
using gas chromatography.
On the other hand, the detection of the organic pollutants has been outsourced to
Eurofins/Analytica in Barneveld, The Netherlands. Eurofins/Analytica is an accredited
laboratory, using ISO/NEN standards for sample storage, sample homogenization, solid phase
extraction and the detection of individual organic components.
For the detection of PAH’s the European ISO 13859:2014 [35] is used, describing the
determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and
high performance liquid chromatography (HPLC). For PCB’s the Dutch standard NEN
6980:2008+C1:2010+C2:2011 [36] describes the protocol to measure organochlorine
insecticides, chlorobenzenes and polychlorine biphenyls (PCB’s) by using gas
chromatography (Figure 20).
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 20. GC-MS setup
III.10. Bio available fraction of organic pollutants
TUD used passive samplers with 5 different solid to sampler ratios to determine the bio
available fraction of PAH’s and PCB’s in the sediment.
A passive sampler is defined as an additional phase to which a pollutant can adsorb in
equilibrium with other phases like water, sediment and organisms. This is represented in
Figure 21.
Figure 21. Partitioning of organic pollutants between different phases.
The added extra phase, the passive sampler, is represented by the yellow sheets
The concentration adsorbed to the passive sampler can be used to calculate the concentration
in water if the partition coefficient is known. Since a homogeneous and artificial passive
DEFINITION OF CHARACTERIZATION METHODS / October 2015
25
sampler (a silicone rubber) was used, the partitioning and sorption kinetics are known, as
shown in Figure 22.
Figure 22. Silicone rubber, depleting the water phase by adsorbing the pollutant
If sediments are added in different solid to passive sampler ratio’s to this equilibrium can also
be calculated with regard to the solid phase (Figure 23). The difference with a total sediment
concentration for organic pollutants (see IV.7) is that only the pollutants that can exchange
with the water phase (and therefor the passive sampler) are removed from the sediment. The
unavailable pollutants stay within the sediment, but they also pose no threat to organisms
since they are not released from the sediment (therefore no biological uptake takes place). For
this reason TUD calls the use of passive samplers the detection of the bioavailable organic
pollutant fraction.
Figure 23. Relation between concentration stripped from the sediment (going into the
passive sampler) at different sediment to sampler ratios, calculating the inaccessible sediment
concentration
DEFINITION OF CHARACTERIZATION METHODS / October 2015
26
The sediment samples were mixed in 5 sediment to passive sampler material ratios, with
water added to a fixed volume. For each sediment the dry weight was determined by drying a
subsample at 105 °C for 24 hours. The samples were put on a rolling table for 6 weeks, after
which the passive sampling material was removed. The passive samplers were pre-spiked
with deuterium labelled equivalent PAH’s and PCB’s, to determine if ad/desorption
equilibrium was reached. The PAH’s and PCB’s were stripped from the passive sampler by
Soxhled extraction with dichloromethane, assisted by microwave (MAE) heating, followed by
a clean-up step (purified sand column). For the detection of PAH’s the European ISO
13859:2014 [35] is used, describing the determination of polycyclic aromatic hydrocarbons
(PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC).
For PCB’s the Dutch standard NEN 6980:2008+C1:2010+C2:2011 [36] describes the
protocol to measure organochlorine insecticides, chlorobenzenes and polychlorine biphenyls
(PCB’s) by using gas chromatography. The results were compared with the total
concentrations in sediment for PAH’s and PCB’s (see IV.7) to derive the sediment bio
available concentration.
III.11. Mineral composition (XRD)
X-ray diffraction is a versatile, non-destructive technique that can be used to investigate the
structure of materials (Figure 24). X-ray diffraction patterns can be used to determine the
crystal structure and crystalline compounds present in a sample. In sediments, XRD may be
used besides chemical analysis to identify the nature of constitutive minerals (quartz,
carbonates, clays, oxides, sulphides, phosphates...).
Figure 24. X-Ray Diffraction (XRD) Spectrometer
III.12. On-site analysis
Field analysis methods were developed initially for the needs of waterways sediments
management (GeDSeT InterReg project, 2013) and more generally for contaminated sites
diagnostics and investigations.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III.12.1. pXRF (portable X-ray fluorescence)
This technique is similar to laboratory XRF (§ IV.6) but uses a handheld instrument, able to
provide multielement analyses in a few minutes. This can be used for site reconnaissance and
preliminary characterisation, for sample homogeneity verification before sending to the
laboratory, for dredging operations monitoring and decision-making help for sediment loads,
for treatment operations monitoring, and for sediment suitability checks at the reuse point.
Figure 25. pXRF spectrometer on site at Dunkirk
The useful range of elements by pXRF comprises Pb, As, Zn, Cu, Fe, Mn, Cr, Ti, Ca, K, Zr,
Sr, Rb, and may comprise Mo, U, Th, Se, W, Ni, Co, V, S, Ba, Sb, Sn, Cd, Ag, Nb depending
upon concentrations. Lower and upper analytical limits vary according to element and
sediment matrix, but typical LDs are in the 5 ppm – 50 ppm range for trace elements and 250
– 500 ppm for light or major elements on usual sediment compositions.
III.12.2. Multiparametric water quality probe
This device incorporates in a single probe various sensors (temperature, conductivity, pH,
Eh/ORP, dissolved oxygen, turbidity, pressure/depth and chloride) with recording capabilities.
It may therefore record water quality along an X-Y path, along depth (underwater or in a well)
or along time at a fixed location (events monitoring). This is useful for site characterisation
prior to dredging (baseline) and for dredging monitoring (especially turbidity, in relation with
suspended particle impacts).
Figure 26. Multiparametric probe on site
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III.12.3. FTIR (portable Fourier Transform mid-InfraRed spectroscopy)
Volatile or semi-volatile organic contaminants can be monitored on-site using wellestablished techniques of gas chromatography (GC/FID). Less volatile or persistent
contaminants cannot be analysed on site and must be analysed in the laboratory (§ IV.7)
unless a highly sophisticated mass spectrometry instrument is available (GC/MS, for instance
HapSite). Based on the outcome of the GeDSeT project results (2013), FTIR was found to be
promising for PAH and other heavy hydrocarbons detection. Tests were carried in the
laboratory during CEAMaS.
Figure 27. FTIR spectrometer on site in a vehicle
III.12.4. µRaman (portable micro Raman spectroscopy)
The recent availability of field portable Raman spectrometers allows the collection of similar
spectra without the water or darkness restrictions. Its main limitation is the lack of experience
and feedback. The instrument best suited for the CEAMaS testing (TSI Ez-785) was first
examined in July 2015 in prototype form, and was made available in the last weeks of the
project. It is therefore not yet possible to make any recommendation about the use of µRaman
for sediment management, apart for investigating further this promising technology.
Figure 28. µRaman spectrometers in the lab
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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III.13. Mineral fractions composition (grain size chemistry)
This method consists in weighing and analysing separately the grain size fractions of a
sample, in order to better understand its engineering properties and the behaviour of pollutants
(i.e. preferential concentration in the finer grain fraction). This allows the evaluation of the
relevance of grain size separation at the industrial scale prior to reuse and/or disposal.
Applications:
-
determination of grain size cut-off to optimise major element composition for reuse
properties (ex: silica)
-
determination of grain size cut-off to reduce pollutant contents below a given value
-
reduction of the volume to be managed as hazardous waste
-
separation of fractions that may be disposed at sea or reused with inert status
III.13.1. Grain size chemistry in the laboratory
Grain size separation of a sediment sample is performed usually by dry or wet sieving, or by
other lab techniques, followed by the weighing of each fraction. The number and size (mesh)
of cut-off fractions depends upon the application.
Size
Mesh
Size
µm
100
150
200
270
325
400
590
810
1190
1680
Mass
149
105
74
53
44
37
30
20
15
10
0.8
2.1
6
8.8
9.6
5.9
12.7
22.1
12.3
19.7
Distribution (%)
Mass
0.8
2.9
8.9
17.7
27.3
33.2
45.9
68
80.3
100
Figure 29. Sediment classification according to size (source: USGS), sieves and an
example of size distribution
DEFINITION OF CHARACTERIZATION METHODS / October 2015
30
90
80
Size
Mesh
70
60
50
Fe % conc
40
SiO2 % conc
30
Mass %
20
10
0
149 105
74
53
44
37
30
20
15
10
Size
µm
100
150
200
270
325
400
590
810
1190
1680
149
105
74
53
44
37
30
20
15
10
Conc %
Conc %
Fe % conc SiO2 % conc
8.44
45.2
12
76.8
22.2
62.2
41.4
52.6
28.25
53.5
24
59.6
25.18
57.9
24.41
59
36.97
41
56.92
12.6
Figure 30. Sediment composition according to size (Fe, Si). Example of distribution
Figure 31. Distribution of mass in grain size fractions, and repartition
III.13.2. Grain size chemistry on site
The above method is both lengthy and expensive, as it is labour-intensive, and it requires
several lab analyses for each sample.
Taking profit of the field analysis techniques (§ IV.10), BRGM tested the feasibility of
performing an orientation grain size analysis based on the results of a simple wet sieving
separation, followed by pXRF measurements on wet and dried samples.
This method does not provide the level of reliability of lab-based grain size analysis, but it
provides useful information on pollutant distribution, and cut-off sizes, within less than a day,
at a fraction of the lab cost.
III.14. TUD specific tests
For the reuse of sediment as a building material there are rules with regard to the chloride and
sulfate content of the material.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Table 4. Maximum emission of chloride and sulphate
Parameter
ClSO42-
Shaped, L/s 10 leaching
(emission after 64days in
mg/m2)
110.000
165.000
Non shaped
(mg/kg d.s.)
616
1.730
IBC-building
material
(mg/kg d.s.)
8.800
20.000
There are exceptions for reuse of these concentrations limits when the natural conditions are
brackish to marine (>5.000 mg/l Cl-). Knowing the chloride and sulphate concentration is
however crucial for the area of application of marine sediments. Hence the cation composition
is detected by ICP-MS (see III.8, same method as metals) and the anion composition by ion
chromatography (IC). The IC analyses was carried on the eluate water from the leaching tests
(see IV.4) by Deltares with a Thermo Scientific Dionex ICS Capillary HPIC system.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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IV. Complementary characterization
Marine sediments are not very common in the civil engineering application. In order to have a
wider and a more accurate scope of its features, Ecole Centrale de Lille and Delft University
of Technology achieved some further tests (Figure 32).
Figure 32. Diagram showing the complementary characterization techniques
IV.1. TGA
ThermoGravimetric Analysis (TGA) measures the variation of the mass of a sample subjected
to a temperature regime. It is carried out using the apparatus Labsys, which is composed of a
structure incorporating a scale module TG, an oven and a software driving the different
modules. The sample was weighed and after it has been placed on the sensor (TG cane), as
shown in Figure 33.
The temperature measurement is performed by the thermocouple associated with the TG rod.
The temperature cycle adapted to study the behaviour of our samples is a set of ramps and
isotherms.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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creuset
Figure 33. Thermographic analyzer LABSYS TG
IV.2. Sorption and desorption test
The purpose of this test is to measure the ability of the material to absorb and restore water
vapor that surrounds it. ECL performed the test according to the French standard NF EN ISO
12571 [16], using the method of the climatic chamber. ECL used the climate chamber
GINTRONIC Gravitest 6400 (Figure 34). It helped to determine the sorption and desorption
isotherm curves.
Sorption curve
The specimen is dried to a constant mass. While being maintained at a constant
temperature, the specimen is placed successively in a series of test environments, the relative
humidity increases stepwise, with the value of 30%, 50%, 75% and 95%. The moisture
content is determined when equilibrium is reached with the atmosphere. The balance with the
environment is obtained by weighing the sample until a constant mass. Knowledge of the
moisture content for each relative humidity is used to draw the sorption curve.
Desorption curve
The starting point of a desorption curve corresponds to a relative humidity of at least
95%. This value can be the last point of the sorption curve or be achieved by sorption from a
previously dried specimen. While being maintained at a constant temperature, the specimen is
placed successively in a series of test environments, the relative humidity decreases stepwise.
The moisture content is determined when atmosphere equilibrium is reached. The balance
with the environment is obtained by weighing the sample until a constant mass.
Knowledge of the moisture content for each relative humidity is used to draw the sorption /
desorption isotherms. The moisture content, u, is calculated as follows for each specimen:
(7)
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Where:
: Mass of the sample before the drying
: Mass of the sample after the drying
Figure 34. The Gintronic Gravitest 6400
IV.3. Thermal conductivity test
The test consists in the determination of the thermal conductivity of a given sediment with the
flow meter Lasercomp Fox 600 (Figure 35). This test was performed according to the French
standard NF EN 12664 [17]. Once the door of the test chamber is opened, the sample can be
introduced between the two plates. The top plate is stationary while the bottom plate can
move both up and down. Each time a sample is introduced into the test chamber, the bottom
plate moves until there is contact with the top plate. Moreover a transducer thin layer of high
output energy flux is attached to the surface of each plate with an active area of 254mm x
254mm in their centres with a thermocouple for accurate readings of the surface temperature.
But seen the low sediments quantity available, we added a short and removable thermocouple
which allows us to use a cylindrical dried and compacted sample with 20 mm of height and 50
mm of diameter. Each plate also includes an integrated circuit to the heating / cooling system
that can make the temperature vary on the sample surface between -15 °C and 85 °C.
The sample must have flat upper and lower surfaces, must be rigid having contact with the
plates and thermocouples. We therefore compacted sediments in a Proctor mould at the
optimum water content, collected a part of that compacted sample using a cylindrical ring
oedometer and dried it in the oven.
The apparatus is provided with a software interface that retrieves data and proceeds to the
calculation of the thermal conductivity (knowing the temperature, the thickness and the heat
flow through its sensors).
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 35. Flow meter Lasercomp Fox 600
IV.4. Zeta Potential
Clay particles are negatively charged, meaning that they attract positive charged particles. In
the simplest charge model, the Helmholtz model (Figure 36), the positive charged particles
form the inner Helmholtz plane. The surface charge potential is linearly dissipated from the
surface to the conditions satisfying the charge.
Figure 36. Helmholtz model for charge distribution
The Helmholtz model is too static with regard to the charge distribution. A more
commonly used model is the Gouy-Chapman Double Layer theory. This theory is based on a
diffuse double layer, in which the change in concentration of the counter ions near a charged
surface follows the Boltzman distribution:
n = no exp(-zeY/kT)
(8)
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Where:
no = bulk concentration
z = charge on the ion
e = charge on a proton
k = Boltzmann constant
Improvement on the Goup-Chapman is theory is made by the Stern modification of the
diffuse double layer. His theory states that ions do have finite size, so cannot approach the
surface closer than a few nm. The double layer is formed in order to neutralize the charged
surface and, in turn, causes an electrokinetic potential between the surface and any point in
the mass of the suspending liquid, as shown in Figure 37. This voltage difference is on the
order of millivolts and is referred to as the surface potential. The magnitude of the surface
potential is related to the surface charge and the thickness of the double layer.
Figure 37. Stern diffuse double layer model
By measurement of the charge at the diffuse double layer boundary (the zeta potential) as
function of ionic strength and composition of the bulk solution, the diffuse double layer
behaviour can be studied. This has been demonstrated by the zeta-potential measurements.
Knowledge of the double layer composition is important, since a large double layer (low zeta
potential (< -20mV) = low ionic strength, monovalent cations) tends to repulse clay particles.
While a small double layer (high zeta potential (> -20mV) = high ionic strength, bivalent
cations) can lead to flocculation (by Van der Waals binding between clay particles).
The electrophoretic mobility of the suspensions was measured using a ZetaNano device from
Malvern (Zetasizer Nano Z). This mobility is measured using a patented laser interferometric
technique called M3-PALS (Phase analysis Light Scattering). The Zeta Potential values were
related to the mobility using the Smoluchwski formula (Hunter 1981,1989). It is known that
the Smoluchwski formula is valid when Debye length, 1/k, is much smaller than the particle
radius (kL>>1) for particles of any shape. The Smoluchoswski´s equation gives a direct
relation between the potential and the electrophoretic mobility:
DEFINITION OF CHARACTERIZATION METHODS / October 2015
37
ζ=4πμU/ε
(9)
Where :
U is electrophoretic mobility at actual temperature,
ε is viscosity of suspending liquid, μ is dielectric constant, and
ζ is the zeta potential (Zeta Sizer Nano Serie System 3.0 Operating Instructions).
The zeta potential measurements were carried out as a function of pH, type and concentration
of electrolyte, and concentration of solid in solution. The average of 10 measurements was
taken to represent the measured potential. The applied voltage during the measurements was
50V with the ZetaNano. The series of measurements in which we varied the salt concentration
are always made from high to low concentration of salt.
IV.5. In situ field equipment
In the field experiments, TUD has used a number of additional measurements.
IV.5.1. Pore pressure sensors
The pore pressure sensors measuring atmospheric pressure above water level and hydrostatic
pressure below water, as shown in figure 38.
Figure 38. Pressure sensors with increasing depth, results first 10 days
IV.5.2. Zakbaak
The zakbaak is a steel plate on a stick (Figure 39). The position of the zakbaak is measured by
DGPS (or manually, compared to a fixed reference point). The zakbaak is placed at different
positions during filling of a site with sediment.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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Figure 39. Zakbaak
IV.5.3 Density by thermal conductivity
The capacity to conduct heat is a function of the sediment density. By heating the sediment
and follow the heat dissipation with an optical wire, the consolidation of sediments when
applied as land fill material can be followed in both depth and time.
We applied 60 watt of heat on a 2m long glowing cable during 10 minutes, heating the
sediment surrounding the optical cable with + 30 °C, as shown in Figure 40.
Figure 40. Thermal conductivity to determine changes in density, field setup
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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References
[1] NF P 94-050: Soils: Investigation and testing - Determination of moisture content. Oven
drying method, AFNOR, 1995.
[2] NEN EN 15934-2012. Sludge, Treated biowaste, soil and waste - Calculation of dry
matter fraction after determination of dry residue or water content.
[3] BS 1377-2: Methods of Test for Soils for Civil Engineering Purposes- Part 2:
Classification Tests”, British Standards Institution, London 1990.
[4] Brunauer S., Emmet P.H., Teller E. Adsorption of gases in multimolecular layers.
Contribution from the Bureau of Chemistry and Soils and George Washington University;
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[5] NF P 94-068. Soils: Investigation and testing-Measuring of the methylene blue adsorption
capacity of a rocky soil-Determination of the methylene blue of a soil by means of the stain
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[6] Santamarina, J.C, Klein, Y.H, Prencke, E. Specific Surface: Determination and Relevance.
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limit test using Casagrande apparatus- Plastic limit test on rolled thread, AFNOR, 1993.
[8] NF P 94-048. Soils: Investigation and testing-Determination of the carbonate contentCalcimeter method, AFNOR, 1996.
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test on quasi satured fine grained soil with loading in increments, AFNOR, 1997.
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[15] XP P 94-047. Soils: Investigation and testing-Determination of the organic matter
content-Ignition method, AFNOR, 1998.
[16] NF EN ISO 12571. Hygrothermal performance of building materials and products Determination of hygroscopic sorption properties, AFNOR, 2000.
[17] NF EN 12664. Thermal performance of building materials and products -Determination
of thermal resistance by means of guarded hot plate and heat flow meter methods - Dry and
moist products of medium and low thermal resistance, AFNOR, 2001.
[18] NF ISO 11464. Soil Quality - Pretreatment of Samples for physico-chemical analysis,
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[19] NF-ISO-15178:2001. Soil quality - Determination of total sulfur by dry combustion
[20] Rodier J (1996). The analysis of water, 8 édition, Dunod, Paris.
[21] NF ISO 10390:2005. Soil quality — Determination of pH.
[22] NF EN 12457-2: Characterization of waste - Leaching - Leaching for compliance testing
of granular waste materials and sludges - Part 2: Test single tarpaulin with a liquid-solid ratio
of 10 l / kg and a granularity of less than 4 mm (without or with reduction granularity), 2002.
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components from granular materials with a column test - Solid earthy and stony materials,
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combustion (elementary analysis), 1995.
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Fraction after Determination of Dry Residue or Water Content, 2012.
[28] NF EN ISO 11885. Water quality - Determination of selected elements by optical
emission spectroscopy with inductively coupled plasma frequency (ICP-OES), 2009.
[29] NEN-EN 13346. Characterisation of Sludges - Determination of Trace Elements and
Phosphorus - Aqua Regia Extraction Methods, 2000.
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DEFINITION OF CHARACTERIZATION METHODS / October 2015
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[32] NF EN ISO 17993. Water quality - Determination of 15 polycyclic aromatic
hydrocarbons (PAH) in water by HPLC with fluorescence detection after liquid-liquid
extraction, 2004.
[33] XP X33-012. Characterisation of Sludges - Determination of Polynuclear Aromatic
Hydrocarbons (PAH) and Polychlorinated Biphenyls (PCB), 2000.
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polychlorinated biphenyls and chlorobenzenes - Method using gas chromatography after
liquid-liquid extraction, 1997.
[35] ISO 13859. Soil quality -- Determination of polycyclic aromatic hydrocarbons (PAH) by
gas chromatography (GC) and high performance liquid chromatography (HPLC), 2014.
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content of organochlorine insecticides, chlorobenzenes and polychlorine biphenyls by using
gas chromatography
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distribution in soil and sediment by sieve and pipet.
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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CEAMaS brings together eight partners from Belgium, France, Ireland and the Netherlands in
order encourage knowledge and consensus to raise new solutions of reuse of marine
sediments applicable to all of Europe. The project aims to promote the beneficial re-use of
marine sediments in civil engineering applications, in a sustainable, economical and socially
acceptable manner. The partnership expertise covers civil engineering, geosciences, coastal
and maritime engineering, dredging and sediment management, geography, sustainable
construction
www.ceamas.eu
CEAMaS is an INTERREG IVB project. INTERREG IVB provides funding for
interregional cooperation across Europe. It is implemented under the European
Community’s territorial co-operation objective and financed through the
European Regional Development Fund (ERDF).
DEFINITION OF CHARACTERIZATION METHODS / October 2015
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