definition of characterisation methods

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

DEFINITION OF CHARACTERIZATION METHODS / October 2015 1

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


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


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


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


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.


Table 1. Appearance of the studied sediments

Origin Reference Appearance Photo

France DS Clayey aspect, dark grey

colour, smells bad.

Belgium AS Clayey aspect, dark brown

colour, smells bad.

The Netherlands LS

Clayey aspect, high organic

matter content, very dark

brown, smells bad.

Ireland CS

Silty sandy grain distribution,

presence of shell debris,

brown colour, smells very

bad.

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.

(%) h d

d

M M

M

(1)

Where:


: 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


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 Å²).

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).


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


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.


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 V-

shaped 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


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.

http://en.wikipedia.org/wiki/Moisture_content

http://en.wikipedia.org/wiki/Soil

http://en.wikipedia.org/wiki/Density


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.


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


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


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.


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.

http://ec.europa.eu/environment/water/water-framework/priority_substances.htm


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.


III.4. Leaching

Within the BRGM laboratory, leaching studies were done following the standard NF EN

12457-2:2002 [22]. Experimental conditions are:

o liquid to solid ratio of 10 l/kg dry matter

o leachant = water

o 1 time shaking 24 hr

o particles < 4 mm

o leachate filtered through a 0.45µm filter

o dry matter content ratio, 105 °C

o 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


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:


(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.


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.


- 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).


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).


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


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


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.


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


III.12.3. FTIR (portable Fourier Transform mid-InfraRed spectroscopy)

Volatile or semi-volatile organic contaminants can be monitored on-site using well-

established 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


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 Size Distribution (%)

Mesh µm Mass Mass

100 149 0.8 0.8

150 105 2.1 2.9

200 74 6 8.9

270 53 8.8 17.7

325 44 9.6 27.3

400 37 5.9 33.2

590 30 12.7 45.9

810 20 22.1 68

1190 15 12.3 80.3

1680 10 19.7 100

Figure 29. Sediment classification according to size (source: USGS), sieves and an

example of size distribution


0

10

20

30

40

50

60

70

80

90

149 105 74 53 44 37 30 20 15 10

Fe % conc

SiO2 % conc

Mass %

Size Size Conc % Conc %

Mesh µm Fe % conc SiO2 % conc

100 149 8.44 45.2

150 105 12 76.8

200 74 22.2 62.2

270 53 41.4 52.6

325 44 28.25 53.5

400 37 24 59.6

590 30 25.18 57.9

810 20 24.41 59

1190 15 36.97 41

1680 10 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.


Table 4. Maximum emission of chloride and sulphate

Parameter Shaped, L/s 10 leaching

(emission after 64days in

mg/m2)

Non shaped

(mg/kg d.s.)

IBC-building

material

(mg/kg d.s.)

Cl- 110.000 616 8.800

SO42- 165.000 1.730 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.


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.


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)


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).


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)


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:


ζ = 4 π μ U / 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.


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


References

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drying method, AFNOR, 1995.

[2] NEN EN 15934-2012. Sludge, Treated biowaste, soil and waste - Calculation of dry

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[3] BS 1377-2: Methods of Test for Soils for Civil Engineering Purposes- Part 2:

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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).

http://www.ceamas.eu/

definition of characterisation methods

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