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HISTORIC MORTARS: CHARACTERISTICS AND TESTS -

CONCLUDING SUMMARY AND STATE-OF-THE-ART


Caspar J.W.P. Groot1, Peter J.M.Bartos2 and John J. Hughes2

1. Delft University of Technology, Delft, The Netherlands


2. Advanced Concrete and Masonry Centre, University of Paisley, Scotland

1. Introduction

One of the tasks of the RILEM TC 167 “Characterisation of old mortars with respect to
their repair” is to deliver a state-of-the-art report. This state-of-the-art, built from
contributions presented at the International Workshop “Historic Mortars:
Characteristics and Tests”, organised at the University of Paisley (12th-14th May, 1999,
at the mid-point of the committees’ activities) is an important contribution to this aim.
The workshop brought together a representative sample of contemporary world-wide
research and development. Therefore the workshop papers reflect the limits of the
subject area at that time, and this conclusion to the published volume attempts to draw
the various themes in research together into one contribution.

Basic reasons to develop activities regarding the characterisation of old mortars were
formulated in the proposal to create this TC:

“Masonry practice shows that many mistakes are made in choosing mortars for pre-
existing masonry. Recommendations, based on the explanation of the phenomena
which play a role in regard to the compatibility of mortar and brick and aspects like
long-term quality and durability of masonry, are badly needed.

Guidelines dealing with the methodology of choosing, preparing and applying mortars
for restoration and repair are meant to avoid future mistakes in the choosing of a mortar
for specific applications. The economic impact is supposed to be significant; however,
precise estimations are not available”.

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To arrive at better practice in this field of restoration it is essential that the
characterisation of the old materials on which the repair materials are applied are
adequately performed.

In this paper a review is given of the aspects and techniques that are used to characterise
old mortars with a view to repair. Therefore, apart from characterisation much attention
is paid to sampling, damage analysis, compatibility elements, experiences with repair
mortars and specifications.

2. Sampling, damage diagnosis and hypothesis formation

Two major controls operate on sampling practice: the objectives of an investigation and
the analyses (physical, chemical or descriptive) needed to fulfil the objectives (Hughes
& Callebaut). The objectives of a study must be clearly stated before any sampling can
take place. The objectives can be related to conservation and repair related
investigations or more general academic studies, including archaeological
investigations.

Minimum action is required in order to reduce effort and cost and minimise destructive
intervention and damage. The materials, the construction method and stratigraphy of the
building must be understood thoroughly before sampling begins, in order to ensure the
correct materials are sampled and so that sufficient material can be obtained. Spatial
and temporal distribution of materials must be understood to do adequate sampling
(Pursche; Hughes & Callebaut; Blauer Bohm; Leslie; Cardoso; Sass).

The choice of analytical method determines the sampling requirements (Hughes &
Callebaut; Goins; Andersen). The formulation of hypotheses regarding damage
mechanisms (van Hees), or the subject of study directs the choice of analytical method
which in turn has a requirement for a minimum quantity of sample, but also a certain
quality of sample, whether as a coherent lump preserving textural-component
relationships or as a powdered sample.

Visual and other non-destructive evaluations assist in the assessment of ideas about the
variations in the macroscopic characteristics of mortar materials, allowing choices to be
made on the representative nature of sample sets (Cardoso, Válek et al). It is accepted
that for historic structures the opportunities for statistically adequate sampling are
limited due to the culturally precious nature of the materials. Samples should be
representative, but if this is not possible the degree of bias must be understood (Hughes
& Callebaut; Goins, Sass). Sampling should be done by experienced people, who know
what is required to achieve a specific test objective, and he/she should preferably have
experience with the experimental technique and its sampling demands.

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The workshop highlighted the fundamental significance of appropriate sampling in
order to avoid later difficulties.

3. Characterisation of old mortars

3.1 Why and when?


The objective of testing for characterisation may range from the exploration of the
potential and limitations of a testing technique to the determination of essential
properties of an old mortar with a view to the formulation of the composition of an
appropriate repair mortar.

A number of examples and aims of characterisation were presented at the workshop:

• The identification of the limitations of testing methods, including wet chemical


analysis (Bläuer Böhm; Martinet) and differential thermal analysis (Ellis).
• The problems of the identification of types of pozzolanic materials and natural
hydraulic lime components in old mortars (Van Balen et.al; Charola; Callebaut et
al) and their differentiation.
• The identification of the provenance of natural hydraulic lime (Callebaut et al).
• Diagnosis of the cause(s) of damage focused on a better understanding of damage
mechanisms (van Hees; Blanco-Varela et al; Larsen).

3.2 How?
A number of techniques used for the charcterisation of old mortars were presented and
discussed. The most important ones are listed below with the basic properties which can
be determined by the methods and their limitations:

a) Visual inspection: To observe the number and thickness of coats or applications of


bedding mortar or renders, the presence of cavities, fractures, cracks and macro
porosity within the binder, the presence of hair and other additives and the
abundance and distribution of unmixed binder (lime lumps). Also the lithological
characteristics of aggregate and pozzolanic additives.

b) Acid dissolution and wet chemical analysis: Determination of the binder- non
carbonate aggregate ratio by the acid digestion of the sample using HCL (Van
Balen et al) or HNO3 (Martinet and Quenee). Determination of the chemical
characteristics of the acid soluble fraction of the mortar by various methods
including, AAS, ICP, ion chromatography. Measurement of silica dissolved into
acid solution (soluble silica) for the estimation of hydraulicity of mortar. However,
the presence of pozzolanas in mortars may disrupt the determination of the original
composition by wet chemical analysis, by changing the distribution of soluble silica
due to soluble reaction rim charcteristics around pozzolana grains (van Balen,
Charola). Pozzoloanas will also be reduced in size through acid digestion because

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of reacted rim compositions, resulting in innacurate grain size distribution
determinations (Blauer Bohm). Van Balen et al also demonstrate that the measured
soluble silica varies with temperature and strength of acid used in dissolution, due
to contributions from aggregate and other additives. Carbonate aggregate also
dissolved by acid attack, so cannot be analysed by this method. Pozzolanicity test
by Ca(OH)2 absorption by disagregated mortar is used to estimate the content of
pozzolanic materials. Depends on time of immersion and reactivity of pozzolanic
materials.

c) Optical microscopy: In transmitted polarised light the determination of the


mineralogy of mortar components and textural/spatial interrelationships between
components. Identification is possible of aggregate, binder (including anhydrous
clinker), additives (organic and inorganic) including pozzolans, porosity and
cracking and secondary mineral formation including salts. In reflected light the
identification of hydraulic binders, of anhydrous clinker particles, of mineral
admixtures opaque types. The method is limited by its resolution of approximately
1 micron. Gives a two dimensional cross-sectional view of a 4-5cm2 area, so
issues of representivity become important, especially with large aggregate and
macroscopically variable mortars.

d) X-ray Diffraction (XRD): Mineralogical determination of crystalline phases of the


binder, detection of pozzolan tracer minerals (van Balen et al), detection of belite
and alite (hydraulic lime or portland cement Callebaut et al), detection of
crystallised alteration products e.g. Ettringite (Martinet & Quenee). XRD is limited
by being a bulk material analysis method. It can give no information on the spatial
interrelationships of mortar components, or their structure.

e) Thermal Analysis (DTA and TGA): The identification of characteristic patterns of


temperature change or weight loss of minerals during heating. Ellis identifies the
limitations, where chemical analysis produced results that were not corroborated by
DTA. He also points out the difficulty as a result, of confidently identifying
existing components, with much less information available about past pre-ageing
compositions.

f) SEM with EDX: Characterisation of morphologies and textural interrelationships


of mortar components including carbonates and hydrates (nature, form, structure)
of the binder and the identification of alteration phases. Representivity is a major
requirement for the interpretation of micro-structural features (Goins) observed on
a very small scale. Local qualitative and quantitative elementary composition of
phases under observation, and calculation of stoichiometric mineral formulae for
comparisons.

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g) Physical testing: Moisture and gas transport behaviour (water, vapour and gas
permeability by Banfill and Forster; Válek et al) and freeze thaw testing, for
damage diagnosis mechanism (Van Hees). In situ gas permeability measurement
(Válek et al) is promising, but several potential limitations were identified,
especially concerning the effects of moisture content.

h) Mechanical testing: Compressive strength, E-modulus, flexural strength, bond


strength. Mechanical testing on samples from historic mortars is often not feasible,
as the samples are too small.

It emerged from the workshop that the most effective way to characterise a mortar is to
use a combination of techniques, as each technique only provides a partial
characterisation. Different combinations of techniques are used depending on the aim of
the characterisation. It is also clear that the professional background and experience of
the researcher plays a role in the choice of applied techniques.

The TC-167COM has worked on the formulation of a number of flow charts to assist in
mineralogical, chemical, and physical characterisation (Middendorf). These, as well as
the schemes of Van Balen et al and Callebaut et al, can be applied as an aid to analysis-
not as proscriptive schemes. These charts give a comprehensive idea of the possibilities
for characterisation in the different fields as described above, and also put useful
constraints upon the sample requirements and sample preparation needed. They clarify
the potential pathways for analysis, allowing analysts to chose that appropriate for their
purposes, without precluding the later use of other pathways. The conservative use of
sample should be encouraged, if the range of potential analysis is understood, reducing
the need for later resampling on-site. One of the tasks of the TC-COM will be to
provide recommendations on the use of these flow charts as a function of the objective
of the investigation. This will amongst others be done through the analysis of specific
damage cases, to aid in the formulation of an actualistic model of mortar analysis

3.3 Characterisation with a view to repair


The relevance of detailed knowledge regarding the characterisation of old mortars was
debated in several contributions. According to Leslie et al (Scottish Lime Centre Trust)
one of the most important factors in the analysis of old mortars is an understanding of
the surrounding building structure and conditions. The same applies to the existing
function of the mortar. An interesting example in this respect is are the differences in
function of ‘sealing’ mortars in dry stone build (no mechanical function Maxwell) and
thick joint masonry (Byzantine, Baronio, Binda with a significant mechanical function).

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Leslie of Scottish Lime Centre Trust observed that the need for data that are relevant to
the requirements of building conservation are: the hydraulicity of the binder, the
relative weights of binder and aggregate and the aggregate grading in order to identify
the necessary components to produce a compatible mortar. This information can (cost
and time extensive) be obtained through simple examination by eye and binocular
microscope, of the sample coupled with acid dissolution and aggregate separation.

More emphasis on porosity and strength characterisation was advocated by Charola &
Henriques. It would be appear that the identification of actual hydraulic components
may not be necessary for either the characterisation of the mortar or the development of
a successful formulation for its replacement. Determination of porosity characteristics
related to strength may serve as a more important guideline for matching repair mortars
to existing ones in historic structures, than much emphasis on the detailed knowledge of
hydraulic components. The work of Válek et al on the in-situ gas permeability of
masonry may relate a porosity related property indirectly to strength and hydraulic
properties. This approach underlines the importance of the characterisation of moisture
condition and behaviour within masonry.

However, again it appears that a combination of methods is perhaps more appropriate


for characterisation.

3.4 Mathematical simulation and modelling


The Workshop showed the need for development of predictive theoretical models,
which would simulate/predict, the behaviour of mortars used for different purposes and
subject to different environmental conditions. Such models would either predict
behaviour and properties of a mortar of a given composition, and prepared/applied in a
specific manner or indicate basic properties, and consequently compositions for such
mortars from specific performance requirements.

At present, there is still a long way to go before reliable, truly predictive models, even
of a partial, not universal, scope become available. However, the Workshop confirmed
that advanced numerical methods are already being applied in the domain of historic
mortars and their repair. There were three presentations that considered in detail
physical properties relevant to historic mortars, two of which were largely theoretical
and the last experimental.

Depraetere presented a numerical consideration of moisture transfer mechanisms; a


physical property important for the practical compatibility of mortars in combination
with bricks in masonry. Four conditions for contact between mortars and bricks are
defined and the effects of each set of conditions studied theoretically. Importantly
perhaps, Depraetere notes that the porus structure of mortar cured in cube moulds will
vary from that formed in practical contact in actual masonry joints, implying that the

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study of seperately prepared materials is perhaps inadequate for a thourough
characterisation. He concludes that methods for the study of the moisture properties of
the interfacial zone in mortar joints have yet to be developed.

Drdácký et al present a numerical model of the mechanical behaviour of mortars


reinforced with animal hair (specifically goat’s hair). This was compared with
experimental deformations of plain and hair reinforced mortars. For extensional stresses
hair reinforcement has a large effect, but is negligible for compressive deformation.

In a direct experimental approach Vermeltfoort et al studied the mechanical behaviour


of two combinations of repointed brick masonry under thermal fluctuations using
Electronic Specle Pattern Interferometry (ESPI). They concluded that hard repointing
applied to soft bedding mortar shows high mechanical incompatibility. Soft pointing
mortars did not affect the distribution of strain in the samples, due to a low Youngs
modulus in comparison with the other materials.

4. Compatibility

The analysis of damage cases of relatively recent repairs has resulted in an increased
awareness of the importance of the compatibility between the new repair material and
the old substrate.

Compatibility requirements of repair mortars should be related to:


• properties/characteristics of the in-situ, old material (physical, mineralogical,
chemical).
• the environmental influencing factors (frost, salts,…).
• the function of the mortar material.
• the state of conservation (degradation as a result of an operating damage process).

A definition of compatibility is given by van Hees as:


“The new mortar should be as durable as possible, without (directly or indirectly)
causing damage to the original material.”

5. Development and testing of repair mortars and consolidants

In order to determine whether the compositional and physical properties of a repair


mortar are compatible with the surrounding material and the environmental conditions,
and to assess the properties of fresh mortars (e.g. workability characteristics), tests
related to key properties may be performed. Many of the characterisation techniques are
the same as used for the description of historic mortars (e.g. XRD, SEM):

• Chemical: mineralogy, carbonation, salt attack, pozzolanic reactions, setting time


(Bromblet, Toumbakari et al, Allen et al, Van Balen et al)

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• Physical: porosity, water permeability, vapour permeability, shrinkage, freeze-thaw
and other accelerated ageing tests. (Bromblet, Válek et al, Banfill and Forster,
Waldum, Toumbakari et al)
• Application technique: plasticity, consistency, water retention. (Thomson)
• Mechanical: bond, compressive and E-modulus, surface hardness. (Bromblet,
Binda et al, Toumbakari et al, McPolin).
• Advanced analysis and chemical/ physical characterisation. XRD, ESEM (Allen et
al).

For the use of repair mortars (derived from traditional formulations or modern ready-
made composition) the application technique is has a large influence on the
performance. Workmanship is very important.

5.1 Binders
There is general agreement that the use of highly hydraulic cement based mortars for
restoration and renovation has caused extensive damage to cultural heritage (eg.
Michoinova). This is because the properties of these type of mortars can be highly
incompatible with the ancient materials and structures on which they are applied. As a
result of the awareness of this problem the use of traditional materials for repair is
promoted by many workers in the field of restoration. This accounts for the renewed
interest regarding the application of lime and pozzolanic material in repair mortars.

However, despite a long tradition in their use, it is still difficult to develop a good lime
mortar. Important reasons are that the traditional know-how and experience has almost
been lost and that the new limes significantly differ from the old ones (Fischer). In
addition, traditional methods of application are being recorded in an effort to better
understand the results of technical characterisation of historic mortars, and to better
specify and apply their replacements during conservation work (Lui).

5.1.1 Non- hydraulic Lime


Specific problems regarding the application of lime mortars are:
-insufficient bond with the substrate occurring under unfavourable application
conditions (e.g. too cold or too warm).
-slow hardening and carbonation.
-low porosity.
-vulnerability to frost, salt and water damage.
Therefore, improvement of the properties of lime mortars is often needed. However, the
approach to improve lime mortar properties may differ.

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Recent research into formulations of traditional mortars gave more knowledge about
and insight into the use traditional additives (Fischer). Problems stemming from
different properties between traditional lime and modern lime production are sometimes
solved using traditional lime production techniques.

The potential of pure lime mortars was demonstrated in a test programme (Waldum)
performed under severe climatic conditions (with significant salt and frost attack). The
results showed relative positive durability performance. It turned out that some pure
lime mortars could compete in weatherability with a factory-made restoration mortar
containing a combination of air lime and hydraulic lime.

Bromblet studied the formulation of stone repair and rendering mortars composed of
non-hydraulic hydrate with the addition of stone dust. He found that the addition of
stone dust affects the porosity and capillarity of otherwise identical mortars. The best
mortars had low strength, low soluble salt content and were easily removed from their
substrate for further repair.

Strottman also introduced a novel non-hydraulic lime product with small particle size
that permits rapid carbonation. This was developed to produce a useful injection repair
mortar, with low water content and composition compatible with historic masonry.

Hansen et al examined the effects of ageing on the portlandite crystal evolution in non-
hydraulic lime putty, and the subsequent effects on consistency, water retention and
plasticity. XRD analysis of crystal morphology correlated well with performance test
results, as the relative abundance of hexagonal plate-like crystals increased. However,
the performance of different sources did not entirely correlate with the age of putty,
indicating that the particular source of lime is an important factor in the determination
of quality.

5.1.2 Lime +pozzolanic materials and hydraulic limes


The application of pozzolanic materials in lime mortars, to improve the durability
performance may be considered as a continuation of traditional practice.

From tests performed in the Smeaton project (Teutonico) it was concluded that (i) brick
dust of bricks fired lower than 900 oC, in lower size particle range (<75µm) can act as
reactive pozzolans assisting initial set and increasing durability, while (ii) larger
particles (>300µm), due to porosity, improve resistance to frost and salt crystallisation.
In the continuation of their comparative study of hydraulic mortars (Teutonico et al) it
was concluded that:
- as regards hydraulic lime:sand mortars a relationship between hydraulicity and water
vapour permeability might be suggested. This suggestion is confirmed by Banfill and
Forster.

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- the addition of significant proportions of lime putty to hydraulic lime:sand mortars has
a marked effect on several characteristics of the mortars including vapour permeability,
compressive strength and performance in salt crystallisation.

Hughes also demonstrated in a testing program the positive effects of using brick dust.
He evaluated the practical ‘benefit’ as a function of the firing temperature (of the bricks
from which the dust was made) and the fineness of the grains. The effect of coarse high
temperature dust is minimal for practical curing conditions, though they may influence
vapour permeability as a result of increase of porosity. Fine low temperature dust plus
adequate water supply may be beneficial.

Investigations on the environmental effects of SO2 (Blanco-Varela et al) showed that


pozzolans containing iron may be sensitive to SO2 attack (as iron is a strong catalyst of
the sulphation reaction).

Toumbakari et al describe the development of the design of multi-blend grouts for the
consolidation of historic masonry structures. The grouts tested contain lime, natural
pozzolans, and in some mixes, low quantities of OPC and silica fume. It was concluded
that it was possible to successfully combine these material and satisfy the requirements
for injections grouts (including low bleeding, low shrinkage, good bonding, setting in
dry and wet environments, penetration of sufficiently small voids).

Michoinova also presented a study of consolidation mortars, where the properties were
altered through the addition of polymers. Simple tests were applied to measure
penetration, tensile strength, setting and rheology

5.1.3 Cement
More and more ready-made mortars are as well becoming available for restoration.
These mortars, often called restoration mortars, generally contain cements. Mortar
design is focussed on performance characteristics such as setting time, mechanical
properties (compressive strength, E-modulus, flexural strength, bond strength), moisture
transport behaviour (water ,vapour and gas permeability) and durability (ageing tests).

Comparing the performance of ready-made renders containing portland cement and


traditional lime-based renders, Marie-Victoire, concluded that it is feasible to design a
ready-made render with comparable properties to traditional renders.

In severe climates, especially where frost damage may be expected, cements in


combination with limes, are used in heritage masonry. Maurenbrecher reports on the
durability testing of pointing mortars based on 1:2:8 (portland cement: lime: damp
sand) mixes. Much emphasis of the program is on the freeze-thaw resistance of weaker

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more deformable, breathable mortars. It was concluded that premix mortars (containing
light weight aggregated) performed better than common cement mortars; it was also
observed that with volume batching, lime putty can contain a much larger quantity of
lime than the same volume of dry hydrated lime.

The Smeaton Project test results suggest that small quantities of cement to lime:sand
mortars (less than 1:3:12) are likely to have a detrimental effect on strength and
durability.

5.2 Traditional and modern mortars.


Basically the approaches of “traditional” and “modern” repair mortar designers
markedly differ:
- the first trying to find solutions starting from traditional materials to subsequently
fulfil compatibility requirements,
- and the latter starting from compatible materials requirements to develop a
formulation of a replacement mortar (to be achieved if necessary using modern
materials).
Mutual understanding of the pro’s and con’s of both approaches may promote the
development of better repair mortars.

6. Specifications

6.1 Composition
From the repair requirements mentioned above, it can be concluded that there is no one
universal solution with regard to the composition of a repair mortar. Between the early
80’s and end 90’s specifications for repair mortars developed from global
recommendations to more quantified performance specifications. This can be illustrated
through the following examples:

S.Peroni recommended in 1981 for the application of restoration mortar the following:

• easy workability
• rapid and reliable setting in both dry and wet environment
• slow shrinkage during setting
• mechanical and thermal characteristics, and porosity similar to those of the
components (natural stones, bricks etc.) of the masonry
• soluble salt as low as possible

More specific research on compatibility requirements resulted in 1997 (Sasse en


Snetlage) in a series of requirements in which propertes of the repair mortar are related
to substrate properties in a quantitative way:

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Repair mortar requirements (1997):
----------------------------------------------------------------------------------------------
Property Symbol Requirement compared
to substrate.
---------------------------------------------------------------------------------------------
Dynamic E-modulus E 20-100 % (60)
Compressive strength σd 20-100 % (60)
Thermal expansion coefficient αth 50-150 % (100)
Water absorption coefficient W 50-100 %
Damp diffusion resistance µ 50-100 %
Bond strength σh 0.5-0.8
----------------------------------------------------------------------------------------------

It may be expected that more detailed research on the application of repair mortars
under specific conditions will result in an extension of this type of quantitative
recommendations. However, there will remain a need for global composition
recommendations as in many cases the financial means for testing are limited or
lacking.

7. References

The papers referred to in this review paper are all contained, unless otherwise indicated
below, within this RILEM published volume titled:

“Historic Mortars: Characteristics and tests”, Bartos P.J.M., Groot C.J.W.P and Hughes
J.J. (Editors), Proceedings of the International RILEM workshop, Advanced Concrete
and Masonry Centre, University of Paisley, Scotland, May 12-15th 1999.

Additional references in the text:

Peroni S., Tersigni C., Torraca G., Cerea S., Forti M., Guidobaldi F., Rossi-Doria P.,
De Rege A. Picchi D., Pietrafitta F.J., Benedetti G. and Nesbitt R. C., ‘Lime based
mortars for the repair of ancient masonry and possible substitutes’, in ‘Mortars,
Cements and Grouts used in the Conservation of Historic Buildings’ Proceedings of the
Symposium, Rome, 1981 (ICCROM, Rome 1981) 297-310.

Sasse H.R. and Snethlage R. ‘Methods for the Evolution of stone conservation
treatments.’ in Saving our architectural heritage : the conservation of historic stone
structures. Edited by N.S. Baer and R. Snethlage, John Wiley & Sons Ltd., (1997), P.
223-243.

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