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GUIDELINE FOR DESALINATION OF POROUS SUBSTRATES


TNO BenO
Netherlands Organization for
R.P.J. van Hees Applied Scientific Research
B. Lubelli
S. Naldini

LRMH
V. Vergès-Belmin
A. Bourgès

IUAV
F. Zezza
E. Di Sipio

UASC
A. Heritage
A. Sawdy
2

GUIDELINE FOR DESALINATION OF POROUS SUBSTRATES

This brochure is based on the results obtained by the EU Desalination project 1 and is
focused on the use of desalination poultices. The experience gained showed that any
desalination treatment should be preceded by a thorough investigation of the
masonry to be treated, and even of the building in which is situated. This should
provide the basis on which to make informed decisions regarding treatment. A
practice oriented guideline is proposed, that covers the necessary steps that need to
be taken to achieve an efficient and also in the long term effective treatment.
Target groups of this publication are:
-architects in charge of conservation or restoration projects,
-heritage authorities responsible for the supervision of restoration works,
-conservators,
-owners of monuments.

1
Desalination - Assessment of Desalination Mortars and Poultices for Historic Masonry,
Contract no.: 022714 (2006)
3

Content

1. Introduction
2. State of the art: commonly used poultices and criteria for their selection
3. Desalination principles
4. Preliminary investigations
5. Characterization of poultices
6. Assessment of the efficiency and the effectiveness of the desalination treatment

Annex A. Definitions of used terms


Annex B Possibilities and limitations of some non-invasive and minimally invasive
methods
Annex C Characteristics of certain lithotypes

Literature
4

1. Introduction
Monuments often show severe and extensive decay caused by salts. In addition to
the loss of valuable cultural property, salt damage also results in high maintenance
costs. Types and intensities of damage have to be thoroughly assessed prior to any
intervention. To achieve this goal it is possible to use the Monument Damage
Diagnostic System (MDDS) 2 (fig. 1), which provides a framework for undertaking
investigations using a consistent terminology and methodology.

Fig. 1. State of preservation assessment of the ‘Waag’ building in Amsterdam using MDDS (see also
below).

Salts present in porous materials cause damage through their interaction with
moisture. Consequently, in certain situations the prevention of further moisture
ingress can provide a solution to the problem. However, damage can also occur due
to the hygroscopic uptake of moisture from the air by the salt. Hygroscopic salts can
dissolve and re-crystallize due to changes in air humidity (RH) that cross their
equilibrium relative humidity value. In this case, climate control may provide stable
RH values and thus avoid cycles of crystallization/dissolution. However, the desired
climate for preservation is not always ideal for people, or can be difficult to maintain.
In such situations, direct intervention in the form of desalination treatments may
present a better solution to the problem.

2. State of the art: most commonly used poultices and criteria for their
selection
The use of water based poultices for the extraction of salt is a long established
technique in conservation; however the results obtained are often variable and
unpredictable.
The desalination poultice products available on the market are predominantly either
cellulose powder based or consist of mixtures of cellulose fibers, clay (bentonite,
kaolin, sepiolite, attapulgite) and/or sand and/or light aggregate 3. The ratio of the

2
MDDS, Masonry Damage Diagnostic System - types of damage related to salt crystallization:
efflorescence, crypto florescence, delamination, exfoliation, spalling, scaling, chalking, powdering,
sanding, crumbling, brick-blistering, bursting, loss of bond, blistering, peeling, push-out, rounded edges
of stone blocks. MDDS was originally developed within a EU project and, since then, regularly updated:
Balen K. Van, Mateus J., Binda, L., Baronio, Hees R.P.J. van, Naldini S., Klugt L.van der, Franke L.,
Expert System for the evaluation of the deterioration of ancient brick structures, EU Environment
Program, EV5V-CT92-0108, Research report No. 8, 1999
3
Vergès-Belmin V. and Siedel, H. ‘Desalination of masonries and monumental sculptures by poulticing:
A review’, Restoration of Buildings and Monuments (Bauinstandsetzen und Baudenkmalpflege) 11, 1–
18 (2005)
5

various components, and also the water content of the poultice can vary. The
composition of both commercial products and self-made recipes are generally not
modified to suit the individual properties of the substrates to which they are applied.
A survey on the products existing on the market and their use was carried out in
2006 4 (fig. 2-3). In the countries participating in the inquiry, self made poultices are
preferred. However, it is not possible to draw a general conclusion regarding the
degree of success or failure of desalination treatments, because the situation in the
substrate before and after desalination is not always assessed, and there is no
standard evaluation procedure by which to do this.

Poultice type: regional preferences Poultice materials used


60 [survey Qu. 6]

50
other 3.0%

40
textiles 3.9%

30
low binder mortar 6.5%
modified industrial Paper 16.1%
20 products Clay/sand
mixtures 9.6%

10 industrial products

self made Cellulose pulp 34.8%


Clay minerals 26.1%
0
Missing Great Britain Italy
Germany France other

Figure 2. Poultice types (from the inquiry of 2006)


Figure 3. Used materials for making poultices (from the inquiry of 2006)

3. Desalination principles
The most suitable desalination technique should be selected each time in relation to
the salt loaded object and the circumstances. For moveable, relatively small objects
that are not sensitive to water, the well established bath method can be very
effective. The object is immersed in a water bath and the water is refreshed, until no
more salts are extracted. The desalination principle upon which the bath method is
based is diffusion.
Some movable objects such as delicate, painted objects comprising water sensitive
materials may not be suitable for immersion in water. In such instances and in the
case of unmovable objects, such as a masonry wall, the desalination may be
performed by the poultice method, which is based on the application of a poultice or
a mortar to the object surface 5.
The treatment itself can be summarized as having two main steps. The first is the
wetting phase: moisture is directly sprayed onto the object or transferred from a wet
poultice/mortar into the object. Salts present in the object dissolve to form a saline
solution. The second phase is that of extraction, whereby the dissolved salt ions
move in the form of an aqueous saline solution from the object into the poultice. The
salt migration can either be generated by the existence of a concentration gradient
between the object and the poultice, in which case the salt ions diffuse through the
solution, or by capillary water flow from the object to the poultice (generally due to
drying) in which the ions are transported within the solution by advection 6. These two
different mechanisms can be broadly translated into two different methods:

4
Survey carried out within the Desalination project (paper presented at the EU Conference in Ljubljana
2008)
5
Other methods like electro-migration are considered less practical for the built cultural heritage. On
electro-migration, see Ottosen L. M. Æ Rörig-Dalgaard I., ‘Desalination of a brick by application of an
electric DC field, Materials and Structures’, 2008
6
Vergès-Belmin et al., 2005
6

1) diffusion controlled wet poulticing methods, whereby the poultice is kept wet
throughout the treatment period (e.g. by the use of a water-proof backing film);
2) drying poultice methods which rely mainly on advective moisture transport, and
where the poultice is allowed to dry by evaporation. 7,8

In short desalination can take place according to different principles, but these are
not always mutually exclusive:
Diffusion: poultices stay wet. Salt ions are transported from the substrate into the
poultice due to differences in ion concentration (fig. 4).
Advection: poultices become dry. Dissolved salts are transported from the substrate
into the poultice by capillary forces during the drying process. The direction of
transport is dependent on the porous structures of the substrate and poultice, such
that saline solution travels from larger pores into finer pores. Consequently, the
substrate must have larger pores than the poultice (fig. 5).
Diffusion is a very slow process, which may take months, whereas advection is a
relatively quick process, which may take a period varying from a few days to a few
weeks depending on the environmental conditions for drying.
The depth to which salts are extracted using a drying poultice is often limited to the
outer few centimeters of the treated surface, and depends on the substrate and
poultice properties and also on the number of poultice applications. In special cases
water can be provided from inside the object to be treated, (e.g. a column) or from
behind (e.g. an isolated wall, a grave stele) and the poultice applied on the drying
side 9.
In current practice, poultices for advection are often applied 2 to 3 times.
By contrast, for the diffusion treatment many more repetitions are usually necessary.

7
Pel, L., Sawdy, A., and Voronina, V., (2009) Physical principles and efficiency of salt extraction by
poulticing, Journal of Cultural Heritage, Volume 11, Issue 1, January 2010, Pages 59-67.
8
Sawdy A., Lubelli B., Voronina V., Funke F., and Pel L., ‘Optimising the extraction of soluble salts from
porous materials by poultices’, Studies in Conservation, Volume 55, Issue 1, 2010, Pages 26-40
9
WTA guideline 3-13-01 /E. ‘Non-destructive desalination of natural stones and other porous building
materials using poultices‘.in Natursteinsanierung nach WTA I bis XII, WTA publications,
Edelsbergstrasse 6, D-80686 München, Germany (2005).
7

start start start

DIFFUSION
end end end Wet poulticing

st
1 Poultice Subsequent End situation
application poultice
applications

start start start

DIFFUSION
Immersion
end end end (or bath method)

Subsequent End situation


Immersion replacement of
bath water

Figure 4. Schematic representation of desalination by diffusion. Salt ions move by diffusion in response
to the presence of a concentration gradient.

start start start

ADVECTION
end end end Drying poulticing

st
1 Poultice Subsequent (Ideal) end
application poultice situation
applications

Figure 5. Schematic representation of desalination by advection. Salt solution moves from the substrate
(large pores) into the poultice (small pores)

Three main risks associated with desalination treatments are related to providing a
high quantity of moisture to a substrate:
-if kept wet, microbiological growth may occur;
-for objects that form part of a larger structure (e.g. a building), moisture may be
inadvertently transferred to other parts of the structure with unexpected
consequences;
8

- the introduction of large amounts of water into an object may weaken its structure
(reducing structural strength), or cause damage to water sensitive materials (e.g. clay
renders, pigments and organic binding media)
- in certain cases salts are present as part of the original materials of the object
(autochthonous salts), or can be formed through the interaction of the original
materials of the object and water (e.g. dolomitic lime when together with gypsum will
give rise to magnesium sulfate salts in the presence of water). In these situations the
introduction of water to the object carries the risk of increasing rather than reducing
the salt load.

When to perform desalination


Desalination of a wall (or large object, non suitable for immersion in water) is
worthwhile in situations where:
• there is no further supply of salts to the object;
• there is no further supply of moisture to the object which would be capable of
transporting salts to the surface;
• the substrate is sufficiently sound to withstand the application and removal of the
poultices;
• the object is not composed of water sensitive materials;
• the object is not composed of materials that will give rise to further salts in the
presence of water (e.g. gypsum and dolomitic lime)

In situations where salts are undergoing dissolution/re-crystallisation cycles in


response to changes in relative humidity, desalination treatments can help to lessen
this activity by reducing the amount of salt in the surface layer of the substrate. In
other words, the rate of damage can be reduced by removing the salts responsible
for the hygroscopic uptake, which are generally located in the first 5-10 mm of the
substrate. However, a durable and effective treatment outcome can only be expected
if there is no new supply of moisture and salt to the object (e.g. from sources such as
capillary rise).

4. Preliminary investigations
Before performing a desalination treatment, some preliminary investigations are
essential, concerning the object 10; the observed damage; the properties of the
damaged materials; the type and quantity of salts present; the distribution of liquid
moisture; and the environmental conditions.
The historical and cultural value of the object should be evaluated and its state of
conservation assessed.
Maintenance and monitoring of the state of conservation of the object after treatment
should also be undertaken.

The evaluation of the historical and cultural value of the object should take into
account:
• the original aspect of the object
• the significance (e.g. art historical) of the object as evidence of a certain style,
taste, or building method
• the aesthetic/historic/cultural role of the object within its context (e.g. urban).
• all original construction and restoration (substitution of materials, additions of
parts) phases and their historical and technical relevance
• the function(s)/use of the object

10
Object may be a building or part of it, a statue, a fresco etc.
9

The technical investigations start with a visual inspection. The assessment of the
state of conservation of the object includes a condition mapping: e.g. the lithotypes,
mortars and painting layers, the damage types and intensities are reported on maps
realized on the basis of pictures shots or designs at appropriate scale. At this stage,
a good knowledge of the historical background of the parts to be mapped is very
important.

Once the first assessment is completed, additional investigations, including a survey


of the liquid moisture sources, the environmental conditions, and sampling for
analysis, can be performed. In the specific case of poultice desalination, the following
information should be collected or determined from samples:

• Substrate: composition, pore-size distribution, and total porosity (an indication


can be obtained by measuring capillary absorption and penetration coefficients)
• Moisture: quantity and distribution within the object, pathways of supply to the
object
• Salts: type, quantity and distribution within the object

Pre wetting
Information regarding the sensitivity of the object to water, the type of salt, its
crystallization pattern and distribution in the wall is important to decide on whether,
and if so, how and to what extent to pre-wet.

Wetting can be performed in different ways (e.g. wet poultice application, free water
absorption…). Regardless of the method used, it is important to determine the
required amount of water per square meter, because this will contribute to determine
the depth of wetting. The speed of the water absorption can be estimated on the
basis of the capillary suction properties of the substrate.

Furthermore, it is possible that, due to the differences in solubility, certain salts are
preferably removed from a mixture of salts. What is left would then have a different
equilibrium RH, which has consequences on the role played by the environment on
dissolution crystallization cycles of the salts, and thus on the damage development 11.

Problems related to the use of a poultice


When the object surface is very fragile or damaged, the application and removal of a
desalination poultice may result in physical damage to the object. In such cases it is
necessary to protect the substrate with an intervention layer such as Japanese tissue
prior to application of the poultice. This can help to reduce the degree of mechanical
disturbance to the object during the application of the poultice and facilitates its
removal, as well as reducing the amount of residue poultice material left behind on
the surface after treatment.
A significant problem associated with the use of poultices is that of clearance, i.e.
residues of poultice material are left behind on the object surface after treatment
which can be optically disfiguring and difficult to remove. For example, in the case of
poultices containing kaolin, this will typically leave white stains behind after removal.
Any consolidation treatment of the salt laden substrate should be performed with
utmost care and after extensive trials: for example, in the presence of salts,

11
Sawdy, A., Heritage, A., and Pel, L., ‘A review of salt transport in porous media, assessment methods
and salt reduction treatments’, in Salt Weathering on Buildings and Stone Sculptures, Proceedings from
the International Conference 22-24 October 2008, National Museum Copenhagen, Denmark, eds. L.M.
Ottosen, I. Rörig-Dalgaard, P.K. Larsen, I. Brajer, P. Bøllingstoft, M. Marciniak and M. Svane, Technical
University of Denmark, Lyngby (2008) 1-28.
10

consolidation with an ethyl-silicate may result in an incomplete reaction, causing


water-repellency of the substrate and difficulties in using desalination poultices.

Classification of substrates
For desalination purposes, substrates can be classified according to their main pore
sizes:
Very fine (< 0.1 µm ), fine (< 0.1-1 µm), medium (1-10µm) and coarse (>10µm).

If the values are <0.1µm, the only desalination method available in practice is that of
diffusion controlled wet poulticing. This is because generally poultice materials do
not comprise a large amount of pores smaller than 0.1 µm, that would be able to
extract salts from such substrates by advection. Moreover, the rate of capillary
transport in pores < 0.1µm is very much reduced, and would therefore require much
longer poulticing times.

The range of pore sizes present in different materials can vary substantially. While
hand moulded brick generally falls into the medium pore size class, natural stone
may belong to any of the classes (see table in annex).
When two materials, such as brick and mortar, are combined within masonry, the
poultice should be adapted to the material possessing the smaller pores. Water
provided during treatment migrates from the coarse porous material to the fine
porous one. In most cases, the mortar has finer pores than the brick and so the
extracting poultice generally needs to have even smaller pores than the mortar.

To illustrate this point, the pore size distribution of three substrates and one mortar is
displayed in figures 6 to 7. The three substrates shown, Migné limestone, fired clay
brick and Bentheim sandstone belong respectively to the “fine “ “medium” and
“coarse “ pore size groups (fig. 6). The mortar, a lime based mortar, belongs to the
“fine”, “medium” and “coarse” pore size groups (fig. 7). If this mortar needs to be
desalinated, the pores belonging to the ‘fine’ category determine the choice of the
poultice.

Migne limestone Fired-clay brick Bentheimer sandstone


35 8.0
Incremental intrusion volume(vol/vol)
cumulative intrusion volume (vol/vol)

30 7.0
6.0
25
5.0
20
4.0
15
3.0
10
2.0
5 1.0
0 0.0
0.001 0.01 0.1 1 10 100 1000
pore diameter (micrometer)

Figure 6. Example of 3 different pore size distributions (MIP measurements): Migné limestone: Ø = 0.3
µm; Fired clay brick: Ø = 5 µm; Bentheim sandstone: Ø = 30 µm (classes, respectively: “fine”, “medium”,
“coarse”.
11

30 1,4

Cumm. intr. volume 25 1,2

Incr. int. volume


(vol/vol%) 1

(vol/vol%)
20
0,8
15
0,6
10
0,4
5 0,2
0 0
0,001 0,01 0,1 1 10 100 1000
Pore diameter (µm)

Figure 7. Pore size distribution of a lime mortar; classes “fine “(0.1 -1 µm), “medium” (1 - 10 µm) and
coarse (>10 µm).

In the following sections, details of a modular system of poultices will be given, which
has been constructed to fit the different substrates pore size classes.

5. Characterization of poultices
Poultices need to be characterized on the basis of their pore size distribution. In
addition to this, the poultice workability and adhesion to the substrate are also very
important criteria.

Pore size distribution of the poultice


The pore-size distribution of the poultice material can change during drying, and so
ideally the poultice should be characterized in both its wet and dry states. This can
ideally be achieved through a combination of different measurement techniques, for
example Nuclear Magnetic Resonance (NMR) for the study of poultices in the wet
state and Mercury Intrusion Porosimetry (MIP) for the study of poultices 12 in the dry
state.
However, NMR is a technique which requires very specialized equipment and
expertise and is therefore generally only available at high level research institutions,
whereas MIP is the most commonly used technique for the determination of pore size
distribution of materials and is widely available.
In addition, imaging techniques such as a combination of Polarized Fluorescent
Microscopy (PFM) on thin sections of dry poultices and (Environmental) Scanning
Electron Microscopy ((E)SEM) can also be useful to gain a better understanding of
the size and shape of the pores.

An example of SEM microphotograph is given in fig. 8. The poultice on the left is


composed of cellulose and comprises a network of fibers, with “inter fibers spaces” of
ca. 10-20 µm. The poultice on the right is a mixture of clay (kaolin), with very fine
grains (pores of ca. 0.3 µm), and 0.5-1 mm sand, leading to coarse pores ca. 50 –
150 µm wide.

12
Lubelli B., Hees van R.P.J., ‘Desalination of masonry structures: fine tuning of pore size
distribution of poultices to substrate properties’, Journal of Cultural Heritage, available on line
http://dx.doi.org\10.1016\j.culher.2009.03.005
12

Figure 8. Microstructure of two poultices as observed with ESEM.

Consistency, workability and adhesion of the poultice


A poultice must be easy to prepare and have a good working consistency, such that
it can be easily applied to a vertical surface and spread out to the desired thickness
(fig. 9).

When drying, the poultice should not shrink too much in order to avoid any
detachment and thus capillary interruption between the substrate and the poultice.
Usually conservators determine such properties empirically on a trial and error basis.

Figure 9. Applying a poultice with good workability and adhesion is relatively easy

However, these properties can be determined using existing tests for


characterising the workability, consistency, adhesion and drying shrinkage of fresh
plaster or rendering mortars. Since mortars have many characteristics in common
with poultices, it is possible to apply standardized methods. For example flow and
cone penetration tests (EN459-2: 2001 13 and EN 413-2: 1994 14), set up originally for

13 EN 459-2:2001, ‘Chaux de construction, méthodes d’essai’ in Ciments et Chaux, recueil Normes


Bâtiments et travaux publics, AFNOR pp. 455-493 (2001)
14 413-2:1994, Ciments à maçonner, méthodes d’essais‘ in Ciments et Chaux, recueil Normes
Bâtiments et travaux publics, AFNOR, pp. 435-448 (1994)
13

mortars and cement pastes 15, can be used for characterizing the workability and
consistency of poultices, respectively. Tests on commonly used poultice recipes have
been undertaken to determine the optimum flow and cone penetration values for a
poultice with appropriate workability properties (Table 1)

Table 1. Domains of flow and penetration for the best workability of the most common kinds of poultices

Flow % Penetration mm
Cellulose based 3 -10 1-2
Mineral based 6 - 33 0.5 - 4
Cellulose/ mineral mixtures 8 - 25 2-4

As to date there is no available standardized adhesion test; a new test method was
devised within the frame of the Desalination project. It is performed using a flow
table, to which a porous substrate (20 % porosity, w-value of 10.3 kg/m2/h0.5, size
5x5x10 cm) is fixed in a vertical orientation. The fresh poultice is applied to the
substrate and a maximum of 15 shocks are delivered via the table. The adhesion,
expressed in %, corresponds to the proportion of shocks the poultice has resisted
before it becomes detached. For example, if the poultice is still attached to the
substrate after 15 shocks, the maximum adhesion qualification is reached, i.e. 100
%, while a poultice that is detached after 7 shocks will be qualified as having 50 %
adhesion. This test can be adapted to various categories of substrates.

Drying shrinkage of the poultice


If a poultice shrinks too much while it dries, it might detach from the substrate. The
quantification of drying shrinkage can be easily achieved by adopting a method used
in soil science. The wet poultice is applied to a cylindrical glass petri dish, and is
dried at constant temperature and air flow. Shrinkage expressed in % of the wet
poultice, according to the following equation:

Shrinkage (%) = 100 * (wet diameter - dry diameter)


wet diameter

The ideal situation is no drying shrinkage at all. Table 2 shows the drying shrinkage
of three different poultice recipes.

Table 2. Drying shrinkage of three poultice recipes. W c = water content (weight of water divided by
weight of dry poultice).

Ratio dry powder in vol. Wc Drying shrinkage (%)

Cellulose BW40:BC1000 1:1 4.5 9


Kaolin/sand 0,8:1 0.2 1
Cellulose/Kaolin/sand 1:0.8:1 0.4 5

While cellulose powder and bentonite both exhibit a high degree of shrinkage, kaolin
shows a very limited degree of shrinkage. The shrinkage of a poultice may be further
reduced by the use of aggregates.
A general rule for an acceptable drying shrinkage value cannot be given, because
this also depends on the degree of adhesion; desalination can proceed even in a
cracked poultice, as long as adhesion (i.e. contact between poultice and substrate)
exists.

15
Bourgès A. and Vergès-Belmin V. ‘A New methodology to determine rheologic behavior and
mechanical properties of desalination poultices‘. Torun : Wydawnictwo Naukowe, cop. 2008 In : 11th
International congress on deterioration and conservation of stone, 15-20 sept. 2008, Torun, Poland :
proceedings / ed. by Jadwiga W. Lukaszewicz, Piotr Niemcewicz, vol. 1, 581-588 (2008)
14

Desalination poultices and substrates – modular system


If it is planned to desalinate the substrate by advection-based methods, the poultice
should have pores smaller than those of the substrate (fig. 10). For example,
cellulose, a very commonly used material (fig. 3), possesses mainly large pores (10-
15 µm) ( 16), which are therefore unsuitable, for extracting salt from brick by advection
( 17). Nevertheless, the poultice pores should not be too small, because the speed of
water transport decreases significantly with pore size. Consequently, if the poultice
pores are too small, desalination can become extremely slow. Furthermore, the
poultice should have a high total porosity to enhance the extraction process and to
increase its capacity to store the extracted salts.

Step 2: transfer of water Step 1: transfer of water into the


from substrate to substrate from big pores of the
poultice during drying poultice

Figure 10. Working principle of the poultice, whereby:


- the poultice possesses small and large pores
- the large pores provide water (for pre-wetting), while the small pores extract salts during
drying
Water can alternatively be applied by spraying.

The pore-size distribution of a poultice can be controlled by varying the:


• composition (clay, sand and other components like cellulose)
• type of clay
• ratio between components
• grain size distribution of the aggregate
The proportion and nature of the components determine the water quantity adapted
to obtain a proper workability. The water content Wc (weight of water/weight of dry
poultice) influences the total porosity of the poultice.

A higher clay content generally results in a larger quantity of small pores, whereas
the larger the sand grain size, the larger the pores are.

Modular system
A modular system of poultices was developed on the basis of the classification of
substrates according to their pore size distribution (fig. 11).
The modular system comprises 4 different classes of poultices, related to the pore
size distribution of the substrate. Three of the poultice classes are intended for
desalination according to the advection principle, and one of the classes is intended
for diffusion based desalination. While this last poultice class can be used for all
substrate pore size classes; it is however most appropriate for the smallest pore
sizes (< 0.1 µm), which can not be desalinated using advective poultices (table 3).

16
Lubelli B., Hees van R.P.J., 2009
17
Vergès-Belmin V , Sawdy Heritage A., Bourgès A. and Doehne E. ‘Desalination with cellulose
poultices: myths and realities’. In preparation
15

Table 3. Modular system of poultices : Each poultice category is suitable to desalinate certain
categories of substrate pore sizes. A = appropriate extraction poultice; P = possible extraction poultice

Poultice Substrate
micro pores small pores meso pores macro pores
< 0.1 µm 0.1 – 1 µm 1-10 µm 10-100 µm
Advection 1. A P P
2. A P
3. A
Diffusion 4. A P P P

Migne limestone Fired-clay brick Bentheim sandstone


35 8.0

Incremental intrusion volume(vol/vol)


cumulative intrusion volume (vol/vol)

30 7.0
4
6.0
25
5.0
20
4.0
15
3.0
10
2.0
1 2 3
5 1.0
0 0.0
0.001 0.01 0.1 1 10 100 1000
pore diameter (micrometer)
Figure 11. Modular system of poultices: the arrows indicate the pore size the poultice should have for
each class of pore size of the substrate (see table A).

6. Assessment of the efficiency and the effectiveness of the desalination


Efficiency and effectiveness have to be considered separately 18: the efficiency
relates to the expected immediate performance of the poultice, while the
effectiveness relates to its long term performance. As a result, effectiveness is
dependent on an extensive range of parameters, and should be estimated taking into
account all possible sources of damage which can (re)appear (e.g. rising damp, new
sources of salt…).

Efficiency of the treatment


The assessment of the treatment efficiency is based on the comparison of the
quantity of salt present in the substrate after treatment with the quantity of salt
originally present.
This assessment is usually done by means of minimally invasive techniques, based
on drilling of powder from the substrate. In the Desalination Project non invasive
techniques have been used and compared with the traditional ones.

Non invasive techniques


The innovative methodology based on non invasive techniques developed within the
project is a useful tool to characterize the substrate, to assess the salt damage and
to control the effect of the desalination treatment.

18
See Annex A
16

This methodology can be applied on different porous building materials (brick and
hard stone) affected by weathering processes.
The procedure comprises the diagnostic phase (pre treatment), and the control
phase (post treatment), see annex B, table 3. The procedure is based on a
combination of digital image processing, colour measurements, ultrasonic pulses,
infrared thermographic analysis and resistivity measurements. These techniques are
employed, before treatment, to characterize the support and, after treatment, to
assess the effectiveness of the applied treatment.
Digital image analysis (ICAW technique) detects the textural properties of the
substrates and the moist spots (fig.12a). Colour measurements (CIElab system)
allow to measure the effect of desalination as a change in colour. Ultrasonic pulses
determine the state of conservation of the substrate. IR thermography registers the
changes of masonry temperature due to the extraction of the salts (fig.12b). The
resistivity measurements are employed to determine sub surface variations linked to
the presence of moisture and salt and to monitor the long term effect of the
treatments; an increase of resistivity values after desalination indicates a positive
effect of desalination; decrease in the resistivity over time indicates a renewed salt
and moisture accumulation (fig.12c).
The research methodology described showed to be a useful tool in the evaluation of
the treatment and the characterization of substrates.

Fig. 12 Diagnosis and control phase of the research methodology: a) digital image analysis; b) IR
thermography (before and after application); c) monitoring of resistivity at different depths over time.

Minimally invasive techniques


Minimally invasive techniques are usually based on drilling of powder from the
substrate.
The powder drilled after each desalination treatment should contain less salt than
before the treatment: the salt amount can either be gravimetrically assessed (after
first dissolving the salts), or by means of Ion Chromatography (IC). Hygroscopic
Moisture Content (HMC) measurements are also suitable if the substrate does not
contain hygroscopic components such as clay minerals. N.B. The quantification of
salts or the measurement of electric conductivity on poultices can be used to asses
the optimum number of poultice applications, but gives only a very rough estimation
of the desalination efficiency.
The salt amount before and after desalination treatment should be measured at least
up to the depth reached by the water provided during desalination (depth of wetting).
17

An indication of the depth of wetting can be obtained when the water amount in the
poultice and the absorption properties of the substrate are known 19.

Sampling for the determination of the salt amount should be performed at different
depths (for example 0-1, 1-2, 2-3, 3-4, 4-5 cm etc.).
The efficiency (% of extracted salts with respect to the initial amount) can be
calculated for each sampling depth

Efficiency (0-x cm) = 100 * (salt before 0-X cm - salt after 0-X cm)
salt before 0-X cm

The salt amount can be expressed in different ways depending on the analysis
method used to quantify the salt amount (e.g. if IC is used the total ion content can
be used).

In order to check if any redistribution of the salt in depth occurred, the salt content at
different depths before and after treatment should be taken into account (fig. 13).

0.25

0.2
Chlorides (%)

0.15
before
after
0.1

0.05

0
1 2 3 4 5 6 7 8 9 10
Depth (cm)

Figure 13. Chloride distribution before and after a desalination treatment: the salt content at the surface
has decreased, but salts have accumulated in depth

A provisional qualification/classification of the efficiency of desalination poultices to be further


related to desalination depth is given in table 4.

Table 4. Classification of treatment efficiency

Quality Efficiency

very high 90-100


high 75-90
medium 50-75
low 25-50
very low 0-25
dangerous, salt enrichment <0

Several standards already exist, that attempt to specify target threshold values for
salt (or rather ion) quantities present in a substrate. While these standards are
intended to provide practical guidance, nevertheless their implementation can be
problematic. Some standards are very rigorous, and hard to achieve in practice.

19
Bourgès A., (2009). Practical advice regarding working properties and consistency. Proceedings of
the Desalination Colloquium, Cologne, 28-29 September 2009
18

Moreover, most of the standards give threshold values for single anions (Cl-, SO4--,
while it is known that the risk of salt damage depends on the salt type, since some
salts cause more damage than others (e.g. the amount of SO4 which can be
considered acceptable will change depending on whether sodium sulfate or calcium
sulfate salts are present). Moreover, the threshold values specified are given as
weight percentages, which may equate to a different degree of salt load (and hence
damage potential) depending on the porosity of the material. Values given by these
standards should therefore always be considered solely as an indication, and should
be checked in relation to the specific situation.
In table 5 threshold values as defined by WTA and by LRMH are given.

Table 5. Threshold values of the anion concentration for different harmful salts (from WTA guideline 3-
20
13-01/E) and from LRMH

WTA LRMH
(% by weight) (% by weight)
Chlorides 0.1 0.1
Nitrates 0.15 0.5
Sulfates 0.25 ≈ 5 (for gypsum)
0.1 (for other sulfates)

Depth of salt removal


An efficient desalination should result in a reduction of the salt concentration as deep
as possible (e.g. up to 2 cm, or more).
A model of the assumed possible salt distribution before and after desalination is
given in fig. 14.

Figure 14. Model of possible salt distribution before and after desalination treatment

An efficient desalination is considered as being achieved if the area under the curve
total salt content = f(depth), is lower after desalination than before desalination. This
supposes that sampling is performed deeper than the depth reached by water during
poulticing, in order to get an appropriate knowledge of the salt distribution before and
after treatment.
An example of a successful desalination trial is given by the test panels of salt loaded
masonry ‘master proofs’ of the Masons’ Tower in the ‘Waag’ (Amsterdam, the
Netherlands) (fig. 15-16).

20
Ministère de la Culture et de la communication, sous direction des monuments historiques,
mission étude et travaux ed. 2003. Ouvrages en pierre de taille: fascicule technique, cahier
des clauses techniques particulières, mode de métré, bordereau de prix unitaire. 219p.
19

Figure 15. Desalination poultice trials at The ‘Waag’ in Amsterdam (left), the Masons’ tower (middle),
and poultices applied on test panels inside the tower (right).

Extraction efficiency at different depths


100 average of 2 bricks
80

60
Efficiency [%]

40

20

0
6-7 cm
3-4 cm
4-5 cm
5-6 cm
0-1 cm
1-2 cm
2-3 cm

6-7 cm
4-5 cm
5-6 cm
0-1 cm
1-2 cm
2-3 cm
3-4 cm

5-6 cm
6-7 cm
2-3 cm
3-4 cm
4-5 cm
0-1 cm
1-2 cm
5-6 cm
6-7 cm
3-4 cm
4-5 cm
0-1 cm
1-2 cm
2-3 cm

-20
cell/bentonite/sand bentonite/sand cell/kaolin/sand kaolin/sand
-40

Figure 16 Efficiency of desalination treatment in the Masons’ tower (‘Waag’, Amsterdam):


Salt extraction (up to 90%) in depth (up to 7 cm) has been obtained by 2 applications of the selected
poultices. The salt content was evaluated measuring the HMC at 97% RH.

Effectiveness of the treatment


The assessment of the effectiveness of a treatment includes:
• efficiency of the performed treatment
• long term effect of desalination.

This implies that long term monitoring is necessary after a desalination treatment.
20

Annex A
Definitions of used terms
The following terms are used within the EU Desalination project and in this
publication according to the given definitions.

Desalination
Desalination means the extraction of soluble salts from a given object/substrate 21.

Aim of desalination
The aim of desalination is to extract salt from a substrate up to a certain depth,
depending on the circumstances.

Advection
Dissolved salts are transported within a moving fluid.

Diffusion
Salt molecules are transported from a region of higher concentration to one of lower
concentration by random molecular motion.

Desalination poultice
A desalination poultice is a soft mass made of different non water soluble elements
(generally a mixture of e.g. clay, cellulose, sand) mixed with water. The word
"poultice" comes from the Latin puls, pultes, meaning ‘porridge’.

Efficiency
The efficiency of a treatment is related to the percentage of salt extracted.

Effectiveness
The effectiveness of desalination is the long term effect of the treatment.

21
‘Die signifikante Reduzierung des Gehaltes an bauschädlichen Salzen in porösen
Baustoffen..’, cf. WTA Zerztörungsfreies Entsalzen von Naturstein und anderen porösen
Baustoffen mittels Kompressen, Merkblatt E-3-13-01/D, Dez. 2002, p.2.
21

Annex B
Possibilities and limitations of some non-invasive and minimally invasive
methods

Table 1 Summary of the techniques available for measurement of the moisture


content in porous materials

Method Principle Advantages Limits


Gravimetric Moisture weight The samples can be also Little destructive
method used for salt assessment
Calcium Increase of pressure due It can be performed on Little destructive.
carbide method to acetylene formation in site. The samples can not be re-used.
the presence of moisture The method is less precise than the
gravimetric method.
Capacitance Variation of the dielectric Non-destructive Calibration is necessary for each
moisture constant of a material in material
methods presence of water Low moisture contents can not be
measured
Deviations are caused by the presence
of salts
Difficulties of using it on rough surfaces
Resistance Decrease of the electric Non-destructive Influence of the surface pressure
moisture resistance of a material Suitable for measuring applied to the pins
meters in presence of water moisture content in wood Not suitable for not homogeneous
materials
Not suitable for not homogenous
distributed moisture
Deviations in presence of salts
Neutron probe Deceleration effect of Measurements can be Low radioactivity
(*) hydrogen atoms on repeated at the same Variation of the analysis volume:
neutrons point - masonry drier = analysis volume
greater
- masonry wetter = analysis volume
smaller
Additional hydrogen in gypsum,
cement, can cause deviations

Georadar (*) The waves make the Non destructive Deviation in salt-rich masonry
water dipoles swing; this Metallic components can cause large
has a deceleration deviations. Calibration necessary.
effect.
Microwave Absorption of shortwave Non destructive Limited depth of penetration
method energy in a material Metallic components can cause
(10Ghz) resulting from the extreme deviations
electric dipole relaxation Difficulties with not homogeneous
of water molecules materials
Thermography It records the surface Non destructive It does not give information on the
(*) temperature. moisture content in depth.
It is influenced by evaporation cooling,
presence of surface treatment,
absence of homogeneity in the
structure.

Portable NMR The magnetic moments Non destructive Until now only applied in laboratory.
(*) of the nuclei (e.g Metallic compounds causes deviations.
(Nuclear hygrogen) are Limited depth of material investigated.
Magnetic manipulated by suitably
Resonance) chosen radio frequency
fields, resulting in a so
called spin-echo signal.
The amplitude of this
signal is proportional to
the number of nuclei
excited by the radio
frequency field.

(*)The methods should be used by trained personnel


22

Table 2 Summary of the techniques available for measurement of the salt content
and type in walls

Method Principle Advantages Limits


Hygroscopic Increase of weight The samples can be re- Little destructive
moisture due to hygroscopic used.. Only indicative
measurements adsorption Indication of:
- Presence
- Quantity
- Type
Salt test strips Chemical reaction Can be performed on site Only indicative
leading to change of
colour
Ion Bond of ions on Precise ion identification Identification of ions, but not of type of
chromatography oppositely charged and quantification salt
(*) material
XRD (X-Ray Scattered intensity Salt identification, also of Only indicative quantification of salt.
Diffraction) (*) of an X-ray beam different hydrated forms Detection limit (3-5% salt content)
hitting a sample as
a function of
incident and
scattered angle,
polarization, and
wavelength or
energy
(E)SEM- EDX (E)SEM: Identification of: Only indicative quantification (provided
(Enviromental) beam electrons hit - Location of salt a flat surface is analyzed)
Scanning Electron the specimen - Crystallization pattern
Microscope surface and - Ion type (by mapping
equipped with produce signals that also salt type)
Energy-Dispersive are collected with - Different hydrated
X-ray appropriate forms
spectroscopy (*) detectors.

EDX: investigation
through interactions
between
electromagnetic
radiation and
matter, analyzing x-
rays emitted by the
matter being hit with
charged particles.
Other chemical
analyses (*)

(*) Methods to be used by trained personnel


23

Table 3 Summary of the NDT techniques foreseen in the Desalination project NDT
methodology
Method Principle Advantages Limits
ICAW Digital image analyses It detects the textural It does not give information on the
technique (*) properties of the moisture content in depth: quantitative
substrates, the moist information can not be directly acquired
spots and the
modifications of the
surface morphology

Color CIElab system It controls the perceptive The measurements can be influenced
measurement of the treatment and the by variation of relative humidity and
(*) quantitative assessment temperature.
of any discoloration Data collected over one year gives an
caused by the exhaustive knowledge of the seasonal
desalination process effects on chromatic coordinates
variation

IR Record of the surface The changes of masonry It does not give information on the
thermography temperature values. temperature linked to the moisture content in depth.
(*) extraction of salts are It is influenced by evaporation cooling,
registered presence of surface treatment,
absence of homogeneity in the
structure.

Ultrasonic Acoustic waves The mechanical Depth of penetration is influenced by


pulses transmission properties of the substrate characteristics
(*) substrate are detected

Resistivity Decrease of the electric It is possible to register It is influenced by substrate


measurement properties (resistivity) of the real resistivity values characteristics.
(geoelectrical a material in presence of of the substrate and the Calibration with laboratory tests is
method) water and salts depth of desalination necessary
(*) treatment. Quantitative information can not be
The measurements can directly acquired
be easily repeated

(*)The methods should be used by trained personnel

Schematic overview of Non Invasive Technique research methodology


24

Annex C
Characteristics of some lithotypes

Substrate Country Type Porosity W value B value Mean pore


of origin % Kg/(m²,h0,5) cm/ h0,5 radius (µm)
Serena I Sandstone 3,0 0,32 0,4 0,02
Balegem B Silic, 10,9 0,4 0,7 0,1
limestone
Massangis F Limestone 15,1 2,2 1,7 0,4
Courville F Limestone 19,9 3,9 1,6 0,11
Ferruginous B Sandstone 24,8 5,2 2,5 15
sandstone
Savonnières F Limestone 38,4 5,5 1,9 4
Euville F Limestone 16 5,9 5,5 45
Lavoux F Limestone 25,0 10,4 5 0,3
Migné F Limestone 30,5 10,6 6,5 0,6
Calcium silicate NL Brick 28,9 13,2 4,42 9,9
brick
Soft Mud brick I Brick 41,8 19,7 - 1,01
Fired clay brick NL Brick 32,4 20 11,7 10
St Maximim F Limestone 37,7 29,3 9,8 15
Tuffeau F Silic, 45,5 30,8 7,7 3,90
limestone
Bentheim G Sandstone 27 38,2 26,5 20-50
After 22
Country of origin: I = Italy; F = France; B = Belgium; N = Netherlands; G = Germany

22
A. Miquel, V. Vergès-Belmin & P. Bromblet : Methodology of the research in the laboratory : selection
and characterisation of substrates . In : Salt compatibility of surface treatments (SCOST) : Final report
of the European contract ENV4-CT98-0710 / ed. by Eddy De Witte [Brussels : Kik-Irpa], 2001, 314 p.
25

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WTA Zerztörungsfreies Entsalzen von Naturstein und anderen porösen Baustoffen


mittels Kompressen, Merkblatt E-3-13-01/D, Dez. 2002

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