Cement and Concrete Composites 135 (2023) 104833

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Cement and Concrete Composites

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A new method to rapidly evaluate the activity of volcanic ash materials

Jianfen Li a, Shujin Li a, **, Lei Peng b, Bing Chen b, *
a
School of Civil and Architectural Engineering Changzhou Institute of Technology, Changzhou, China
b
Shanghai Key Laboratory for Digital Maintenance of Buildings and Infrastructure, Department of Civil Engineering, Shanghai Jiao Tong University, Shanghai, 200240,
China

A R T I C L E I N F O A B S T R A C T

Keywords: A new method of preliminary determination of pozzolanic activity, total dissolved solids (TDS) method, was
Fly ash (FA) proposed and experimental investigation was carried out on fly ash (FA). The electrical conductivity, TDS, pH
Volcanic ash reaction and hydration temperature parameters of FA and calcium hydroxide (CH) suspension were investigated. First-
TDS method
order derivation of TDS was performed, dividing steady-state and unsteady-state dissolution regions. Results
CH
TDS loss rate
suggested that the first-order derivation of TDS can measure the dissolution rate, and was a potential method for
evaluating solubility. The first derivative of TDS indicated that the system gradually changes from the unsteady
state to the steady state stage. The concept of TDS loss rate was proposed mainly to avoid the effect of CH in the
CH-FA–CSH–CAH system, and to highlight the effect of the gelation products generated by the pozzolanic re­
action on TDS. The higher the loss rate of TDS, the stronger its pozzolanic activity.

1. Introduction
There is a certain amount of active components such as activated
silica and activated alumina in the pozzolanic mixture [1]. The so-called
pozzolanic reaction means that these active components react with
calcium hydroxide (CH) to produce hydrated calcium silicate (CSH),
hydrated calcium aluminate (CAH), calcium sulfoaluminate hydrates,
calcium aluminoferrite hydrate and calcium sulfoaluminate ferrite hy­
drate [2,3]. CH can come from lime during the hydration of cement.
Volcanic ash materials mainly include natural ash mixed materials and
artificial volcanic mixed materials. Natural ash mixed materials are
volcanic ash, tuff, zeolite, pumice, diatomite. The artificial volcanic ash
mixed materials include coal gangue, burnt shale, burnt clay, coal slag,
residue after coal combustion, and siliceous slag [4]. Volcanic ash ma­
terials are widely used because of their excellent durability [5–7]. Not
all ash materials are suitable for mixed cement [8,9], which depends on
its pozzolanic activity and the amount and amorphous content of active
silica [10]. A recent study by Contrafatto [9] suggested that some vol­
canic explosive debris to do have enough active silica, which cannot
produce enough pozzolanic reactivity to replace portland cement. One
of the research focuses of pozzolanic materials is the pozzolanic activity
of pozzolanic materials.
The methods of evaluating volcanic ash activity mainly include
direct method and indirect method [11]. The direct method is to
determine residual CH of the reaction system of pozzolanic material and
portland cement hydration product CH solution in each age solution or
in acid-base solution. Direct methods include acid-base dissolution
method, Frattini test method, modified Chapelle test (NFP-18513),
saturated lime method and thermal analysis method [12–15]. The
acid-base dissolution method is to put the volcanic material into a
certain concentration of acid or alkali solution, and the silicon or
aluminum content in the solution is determined after a certain time. The
saturated lime method refers to mixing the pozzolanic material with the
silicate cement slurry or lime solution. Then, the concentration of Ca2+
and OH− remaining in the solution at different ages is determined to
evaluate the pozzolanic activity [16]. The saturated lime method is a
simplified version of the Frattini test. Generally, the lower the Ca2+ and
OH− concentrations, the higher the pozzolanic activity; Thermal anal­
ysis refers to the use of differential thermal analysis (TG-DTA), differ­
ential thermal gravity (TG-DTG), differential scanning calorimetry
(TG-DSC) to measure the cement slurry or lime slurry of pozzolanic
materials in different proportions CH content, and compared with the
control group. Since CH decomposes at 400–550 ◦ C, its content can be
measured by measuring its mass loss by TG-DTG [17]. Indirect methods
mainly include compressive strength test method [18], conductivity
method [19] and hydration heat method [20,21]. Strength index

* Corresponding author.
** Corresponding author.
E-mail addresses: lisj@czu.cn (S. Li), hntchen@sjtu.edu.cn (B. Chen).

https://doi.org/10.1016/j.cemconcomp.2022.104833
Received 1 September 2022; Received in revised form 22 September 2022; Accepted 25 October 2022
Available online 31 October 2022
0958-9465/© 2022 Elsevier Ltd. All rights reserved.
J. Li et al.
method (ASTM C311 [22], ASTM C 989 [23] and ASTMC 1240 [24]),
that is, a certain amount of volcanic ash material is used to estimate the
volcanic ash activity index based on the ratio of the compressive
strength of the 28-day experimental group and the control group [11].
Generally, the larger the ratio, the higher the activity. The hydration
heat reaction method is to evaluate the activity of volcanic ash by
measuring the constant temperature hydration heat of the lime-volcanic
ash material-water system. The greater the hydration reaction heat at
the same age, the higher the activity. Although the existing volcanic ash
evaluation methods are relatively comprehensive, some methods have a
long test cycle (intensity index method) [22], insufficient temperature
sensitivity (hydration heat method) [25], and high cost (lime absorption
method and thermal analysis method) [26], long experimental steps
[27]. Therefore, it is still necessary to develop new volcanic ash response
evaluation methods, enrich volcanic ash determination methods, and
solve practical needs.
Efforts has been made for evaluating the activity of volcanic ash
materials. Tashiro et al. [28] proposed a method for evaluating volcanic
ash reaction by preparing a slurry composed of fine ceramsite, FA, silica
fume, kaolin, acid clay, zeolite, and quartz activated with silicate. Under
accelerated curing conditions (60 ◦ C, 72 h), the resistance and con­
sumption of silicate were measured. The results showed that except
kaolin, the resistance of active pozzolans increased significantly, but the
resistance of non-active material quartz did not increase significantly.
Except for FA, the resistance was directly proportional to the con­
sumption of portland stone. Combining resistance measurement with
Portland stone consumption can be used for rapid evaluation of pozzo­
lanic activity. There are also techniques that can quickly assess the
pozzolanic activity of specific materials in a short time. Sharma et al.
[29] studied the chemical and physical parameters of 25 FA samples and
found that the content of soluble silicon is relatively low and has the
characteristics of low pozzolanic ash. Based on the soluble silica content
and fineness of FA, an empirical formula for quickly estimating the
reactivity of FA with lime was established. Raask and Bhaskar [30]
determined the pozzolanic activity of FA by measuring the dissolution
rate of silica in FA in 0.1 M hydrofluoric acid. The extraction rate of
silicon follows the law of logarithm, and the extraction rate constant was
adopted as pozzolanic activity indicator. Luxán et al. [31] proposed a
method for evaluating the activity of pozzolans. This method was based
on the measurement of the compensated conductivity of the saturated
CH solution of the added material over time. However, this method was
only applicable to natural products, such as milky white rock, diato­
maceous earth, tuff, etc., and was not ideal for determining the pozzo­
lanic activity of FA [19]. Subsequently, Sugita et al. [32] used the
Luxán’s method to evaluate the pozzolanic activity of rice husk ash
(RHA). They found that there was a significant difference between the
amorphous silicon content in the RHA sample and the conductivity
change of the RHA/saturated lime suspension and showed a good cor­
relation. As we all know, the reaction of lime (or cement) pozzolans has
not been well understood, and has become a research topic for many
researchers.
Recently, total dissolved solids (TDS) has been widely used in water
quality testing and other fields due to its simple measurement method,
low cost, fast and reliable [33,34]. TDS is measured in mg/L which in­
dicates how many milligrams of dissolved solids are dissolved in 1 L of
water. The higher the value of TDS, the more dissolved. Generally, the
conductivity value can be used to understand the salt in the solution. The
higher the conductivity, the higher the salinity and the higher the TDS.
This provides a theoretical basis and feasibility basis for the successful
application of TDS in volcanic ash detection. To date, to the best of the
author’s knowledge, no volcanic ash material has been evaluated by TDS
for volcanic ash activity.
This work aims to propose a new method for rapid evaluation of
volcanic ash activity, TDS loss rate method. This method has rapid
detection, clear physical meaning, low cost, high sensitivity, strong
discrimination ability, and has great application potential. It will
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Cement and Concrete Composites 135 (2023) 104833
provide a more scientific method for detecting pozzolanic activity, and
can be successfully used to detect pozzolanic activity of FA.
2. Materials and methods
2.1. Materials
The test material was China Class I FA, and its chemical composition
was determined by X-ray fluorescence spectrometer (XRF) as shown in
Table 1. CH is analytical pure and the technical conditions comply with
Q/CYDZ221-2007 with chemical purity ≥95.0%, hydrochloric acid
insoluble matter ≤0.05% and ammonium hydroxide precipitate
≤0.25%.
2.2. Testing methods
The FA and CH were dried in a drying oven at a temperature of 60 ◦ C
for 24 h 0.2000g CH and 0.2500g FA were weighed quantitatively. CH
was poured into a 100 ml beaker, then 0.2500g of FA was added, and the
liquid-solid ratio was 0.45/100. The computer heating platform pre-
heats the deionized water in the beaker to 36.5 ◦ C. The TDS detector,
pH digital display and temperature monitoring sensor were inserted into
the beaker and the corresponding TDS content, pH value and tempera­
ture were recorded. The detailed test items are displayed in Fig. 1.
3. Results and discussion
3.1. Determination TDS of FA and CH solution
Fig. 2 shows the TDS and conductivity of FA/CH suspension with
time. It can be found from Fig. 2a that TDS generally shows an upward
trend. After about 14400s, TDS was 2.15 g/L. The growth rate of TDS
was faster in the first 1000s, and the growth gradually declined after
1000s. Fig. 2b is obtained by the first derivation of Fig. 2a. It can be
found that the TDS growth rate changed from unsteady to steady state at
about 5000s, which was caused by the rapid dissolution of the FA/CA
system at the initial stage, and then gradually dissolved after 5000s.
Fig. 2c presents that the change in conductivity is wave-like and grad­
ually undulating, and finally the conductivity gradually reaches about
5.0 μm/cm. By the first derivation of Fig. 2c, the derivative of conduc­
tivity is obtained as showed in Fig. 2d. It can be found that the unsteady
state phase was about 6400s, and then entered the steady state phase.
The occurrence of unsteady state may be caused by the physical changes
in the dissolution process of the FA/CH suspension system. From the
molecular point of view, the position of atomic molecules or ions in the
solid state was basically fixed, and even if there was vibration, the
amplitude was not large. Therefore, the solid state had a certain order
and the degree of confusion was relatively small. But after dissolving it
became hydrated ions, then according to the random movement of
molecular and ions, the degree of disorder increased. Finally, the degree
of confusion and entropy increased.
3.2. Determination TDS and pH of FA
TDS, pH and temperature change curves of FA are presented in Fig. 3.
Fig. 3a showed the change of FA TDS with time. The TDS increased
rapidly in the initial stage, and finally maintained balance. Fig. 3b was
the result of the first derivation of Fig. 3a. It can be found that when the
time lasted about 8400s, the dissolution rate of TDS changed from
relatively rapid to equilibrium, that is, the dissolution system has been
Table 1
Chemical composition of FA oxides detected by XRF(%).
SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SO3
39.38 27.50 4.81 17.84 1.82 1.01 1.81 3.74
J. Li et al. Cement and Concrete Composites 135 (2023) 104833

Fig. 1. Experimental test project (a) schematic diagram (b) test platform (c) samples.

Fig. 2. The change of TDS and conductivity of FA/CH suspension with time (a) TDS; (b) TDS derivative; (c) conductivity; (d) conductivity derivative.

transformed from the unsteady state to the steady state stage. Overall,
the TDS dissolution value of FA was low. Even when the dissolution time
was about 3420s, the TDS value still did not exceed 3.0. Fig. 3c
demonstrated that its temperature increased first, and then fluctuated at
37 ◦ C. The pH value in Fig. 3d increased rapidly to 10.3 in the short term
from 0s to 1748s and stabilized at 10.4 in the long term.
3.3. TDS and pH of CH
The solubility of CH decreases with increasing temperature. The
reason for this phenomenon is that CH has two hydrates Ca(OH)2⋅2H2O
and Ca(OH)2⋅12H2O. The solubility of these two hydrates is large, and
the solubility of anhydrous CH is very small. As the temperature in­
creases, these crystalline hydrates gradually become anhydrous CH,
which cause the solubility of CH decreases with increasing temperature.
At 20 ◦ C, 30 ◦ C, 40 ◦ C, and 50 ◦ C, the solubility of CH in 100 g of water is
0.165 g, 0.153 g, 0.141 g, and 0.138 g, respectively. Therefore, in order
to accelerate the reaction of the solution system and make the CH
supersaturated, the mass of CH in the suspension is determined to be
0.2g in this method. CH is a white FA-like solid, slightly soluble in water.
It can be found that after adding water, there were two layers, the upper
aqueous solution was called clear lime water, and the lower suspension
was called lime milk or lime slurry.
Fig. 4 exhibits the evolution of TDS, TDS derivation, temperature and
pH of CH. Fig. 4a showed that TDS shows a tendency to increase rapidly
and then slowly. Implementing the first derivative of Fig. 4a can obtain
the TDS change rate in Fig. 4b. It can be found that around 3660s, CH
changes from the non-steady-state phase to the steady-state phase.
Fig. 4c showed that the hydration temperature gradually increased,
indicating that CH dissolves in water and releases heat. Compared with
the TDS of FA, the TDS value of CH was larger, indicating its greater
solubility. Fig. 4d showed that its pH rose rapidly in the short time of the
first 500s, the pH value reached 10.9, and then slowly increased,
reaching 11.1 at 2000s. Finally, the pH value reached 11.3 and main­
tained this value for a longer period of time.
Most solids absorbed heat when they were dissolved in water.

3
J. Li et al. Cement and Concrete Composites 135 (2023) 104833

Fig. 3. TDS, pH and temperature change curves of FA (a) TDS; (b) TDS derivative; (c) pH change; (d) temperature change.

Fig. 4. TDS, temperature and pH evolution of CH (a) TDS; (b) TDS derivation; (c) temperature evolution; (d) pH value evolution.

According to the principle of equilibrium movement, the temperature
rose and the equilibrium was conducive to moving in the direction of
endotherm. However, a few substances were exothermic when dis­
solved, such as CH. This indicated that the solubility of CH decreased
with increasing temperature. When a substance was dissolved in water,
two processes usually occur: one was the diffusion of solute molecules or
ions. This process absorbed heat and was a physical process; the other
was the interaction of solute molecules or ions with water molecules to
form hydrated molecules or ions. This process was an exothermic
chemical process. Obviously, the exotherm of CH was attributed to the
thermal effect of its dissolution process, which was induced by the dif­
ference in the relative amounts of ion diffusion endotherm and ion
hydration exotherm. It can be found that the heat of hydration of CH
ions was greater than the endotherm of the ion diffusion process.
3.4. TDS evaluation method of CH-FA–CSH–CAH suspension system
CH FA will undergo volcanic ash reaction at a certain time, and the
potential active silica and aluminum oxide will dissolve and generate
hydrated calcium silicate (CSH) and hydrated calcium aluminate (CAH).
In order to evaluate the overall volcanic ash response of the calcium
hydroxide-fly ash-hydrated calcium silicate-hydrated calcium aluminate
(CH-FA–CSH–CAH) system, the increase rate of TDS of the system was
adopted for characterization and measurement. The increase rate of TDS

4
J. Li et al.
can be determined by the following formula:
C0 − CF(aq) (t)
CCA− FA− CSH− CAH (t) = × 100% (1)
C0
Where CCA− FA− CSH− CAH (t) is the percentage of TDS growth rate for a
given suspension and a given time t, C0 is the initial TDS value of the CH-
FA–CSH–CAH solution system, CF(aq) is the absolute TDS of the CH-
FA–CSH–CAH suspension in a given time. It was not difficult to find that
CCA− FA− CSH− CAH (t) will also be affected by temperature and the ratio of
FA/CH liquid to solid.
3.5. Relative increase rate of TDS with time (CH-FA–CSH–CAH
suspension system)
According to the CH-FA–CSH–CAH suspension system formula pro­
posed above, the TDS growth rate calculation method of the CH-
FA–CSH–CAH system can be determined accordingly.
Fig. 5 presents a schematic diagram of calculating the TDS increase
rate of the CH-FA–CSH–CAH suspension system. Curve a represented the
curve of the TDS of the FA/CH suspension system with time, and curve b
represented the change of the TDS of the FA suspension with time. Curve
c was the value obtained by subtracting curve b from curve a. Curve c
reflected the change curve of TDS of CH-FA–CSH–CAH system with
time. According to the initial value of curve c, its TDS change rate can be
calculated.
Fig. 6 exhibits the TDS change rate of the CH-FA–CSH–CAH sus­
pension system. It can be found from Fig. 6a that the overall TDS growth
rate of the TDS system was gradually increasing. Fig. 6b presented the
first derivative of Fig. 6a, the TDS change rate of the reaction system. It
was not difficult to find that when the reaction continues to about 5000s,
the system gradually changed from the unsteady state to the steady state
stage. Fig. 6c represented an enlargement of the initial stage of Fig. 6a.
In the initial stage, TDS fluctuated greatly, showing the characteristics of
increasing first and then decreasing and then increasing. This may be
ascribed to the dissolution of pozzolanic material FA and CH, resulting
in system instability. Therefore, the detection time of volcanic ash re­
action should not be carried out prematurely, otherwise the detection
accuracy may be affected. It has been reported in the literature that the
conductivity was used for rapid evaluation in the range of 1000s [19]
and1200s [31]. Based on the observation and analysis of the first de­
rivative of the evolution of TDS with time, we believed that the detection
of volcanic ash activity in such a short period of time may result in
inaccurate data.
Fig. 5. A diagram of the calculation method of the TDS growth rate of the CH-
FA–CSH–CAH suspension system.
5
Cement and Concrete Composites 135 (2023) 104833
However, this indicator used to reflect the overall TDS change rate of
the system only can reflect the change of the initial TDS value in the CH-
FA–CSH–CAH suspension system. Therefore, the calculated CH-
FA–CSH–CAH can only roughly reflect the incremental change of TDS
from a qualitative perspective. Because of the presence of CH, the TDS
growth rate was also affected by the dissolution and ionization of CH
itself. Therefore, merely investigating CH-FA–CSH–CAH was not enough
to determine the effect of volcanic ash reaction products on TDS.
Because we did not know whether it was the change of TDS caused by
CH or the change of TDS caused by pozzolanic reaction. To this end, we
put forward the concept of TDS loss rate.
3.6. TDS loss rate
The concept of TDS loss rate was proposed mainly to remove the
effect of CH in the CH-FA–CSH–CAH system, and to highlight the effect
of the gelation products generated by the pozzolanic reaction on TDS.
This made it unnecessary to consider the amount of reactants too much
to interfere with the experiment when evaluating volcanic ash activity.
The expression was proposed as follows:
CCHFA (t) =
CCA (t) − CCA− FA− CSH− CAH (t)
× 100% (2)
CCA (t)
Where CCHFA (t) is the percentage of TDS loss for a given suspension and a
given time t, CCA (t) is the TDS of the CH solution before adding FA,
CCA− FA− CSH− CAH (t) is the absolute loss of conductivity of the FA/CH
suspension in a given time.
Fig. 7 shows the calculation method of TDS loss rate. Curve a pre­
sented the change of the TDS of the FA/CA suspension with time. Curve
b described the change of the suspension TDS of FA with time. Curve c
was determined by subtracting curve b from curve a. Curve d minus
curve b was the net loss of TDS. Further calculation, the ratio of the
subtraction value (net loss) between curve d and curve d to curve d was
the TDS loss rate of volcanic ash reaction. The TDS loss rate can be used
to evaluate the pozzolanic activity of pozzolanic materials. The fore­
going research had clarified that during the earlier period of volcanic
ash reaction, it basically appeared in an unsteady state, and the data
fluctuated greatly, which was not conducive to accurately reflect the loss
rate of TDS. Therefore, it was more appropriate to select the data at
about 2000s to calculate TDS loss. In this FA case, the intersection of
curves c and d was selected as the starting point for the calculation of
TDS loss rate.
Fig. 8 presents evolution of TDS loss rate over time. It can be found
that about 2000s, the TDS loss rate of volcanic ash appeared.
Obviously, the loss rate of TDS presented a characteristic of rapid
increase and then gradually stable. It was worth noting that the volcanic
ash reaction had a certain delay. The reaction system first underwent a
self-dissolution process, and then gradually started the reaction. The
reaction increased rapidly and then gradually stabilized. The higher the
loss rate of TDS, the stronger its pozzolanic activity. On the contrary, it
shows that the lower the volcanic ash activity. It is true that the volcanic
ash reaction will also be affected by temperature and the concentration
and type of volcanic ash reactants. Subsequent studies will conduct
quantitative research on temperature, initial reactant concentration and
volcanic ash material types.
4. Conclusion
(1) The overall TDS of FA and CH suspension showed a gradual
increasing trend with time. In the reaction lasting 5000s, the first
derivative of TDS reflected that TDS was still in an unsteady state,
and after 5000s TDS showed a steady state characteristic. The
electrical conductivity of FA and CH showed a wavy spiral up­
ward trend, and the non-steady state time was longer, lasting
about 6400 s to enter the steady state stage.
J. Li et al.
Fig. 6. TDS change rate of CH-FA–CSH–CAH suspension system (a) TDS increase rate; (b) first derivative; (c) enlargement of graph (a).
Fig. 7. TDS loss rate calculation method.
(2) The TDS of FA presented a trend of rapid growth and then slowed
growth with the reaction time. When balanced, the TDS value
was smaller. The TDS non-steady-state phase of FA was converted
into a steady-state phase with a duration of about 8400s, indi­
cating that the dissolution rate of FA was slow. The first-order
derivation of TDS can measure the dissolution rate of reactants,
which was a potential method for evaluating solubility.
(3) The TDS growth of CH exhibited the characteristics of rapid in­
crease with time and then increase slowly. The derivative of TDS
indicated that CH entered the steady-state phase from unsteady
state at about 3660s. CH dissolved in water and released heat.
Compared with the TDS of FA, the TDS value of CH was larger,
indicating its greater solubility.
(4) The calculated CH-FA–CSH–CAH can only roughly reflect the
incremental change of TDS from a qualitative perspective. The
mere investigation of the TDS growth rate of the CH-
6
Cement and Concrete Composites 135 (2023) 104833
Fig. 8. Evolution of TDS loss rate over time.
FA–CSH–CAH suspension system was not enough to determine
the effect of volcanic ash reaction products on TDS.
(5) The concept of TDS loss rate was proposed, mainly to remove the
effect of CH in the CH-FA–CSH–CAH system, which highlighted
the effect of the gelation products generated by the pozzolanic
reaction on TDS. The higher the loss rate of TDS, the stronger its
pozzolanic activity. On the contrary, it indicated that the lower
the volcanic ash activity.
(6) TDS loss rate can become a new potential method for evaluating
volcanic ash activity, which will provide useful exploration for
the rapid evaluation of the activity of volcanic ash materials.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
J. Li et al. Cement and Concrete Composites 135 (2023) 104833

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