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1. Introduction - Firenze University Press

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2.2. Synthetic standards<br />

To test the accuracy of the three methods, ten synthetic standards (STD1-10) representative of the<br />

mineralogical composition of APCr were formulated. Analytical grade reagents; calcium carbonate<br />

(CaCO3), portlandite (Ca(OH)2), lime (CaO), anhydrite (CaSO4), gypsum (CaSO4.2H2O), bassanite<br />

(CaSO4.0.5H2O), halite (NaCl), sylvite (KCl) and quartz (SiO2) were combined according to Table<br />

<strong>1.</strong> The produced synthetic standards were stored in a desiccated environment to avoid possible<br />

alteration due to atmospheric humidity.<br />

STD1 to STD4 were formulated with a high percentage of reactive calcium phases (portlandite and<br />

lime) and a low content of calcium carbonate, simulating the composition of an untreated APCr.<br />

Other standards (STD7, STD9 and STD10) were formulated without reactive calcium species and<br />

with higher percentage of calcium carbonate, simulating the composition of a carbonated APCr.<br />

The influence of the other phases including gypsum and anhydrite were also investigated.<br />

Table <strong>1.</strong> Percentage mineralogical composition of synthetic standards<br />

Standard<br />

ID<br />

CaCO3 Ca(OH)2 CaO CaSO4<br />

CaSO4<br />

.2H2O<br />

CaSO4<br />

.0.5H2O NaCl KCl SiO2<br />

(Calcite) (Portlandite) (Lime) (Anhydrite) Gypsum Bassanite Halite Sylvite Quartz<br />

STD1 0.2 - 20.8 6.5 14.1 14.9 22.3 6.1 15.1<br />

STD2 14.1 2<strong>1.</strong>9 10.4 18.8 - - 20.0 9.9 5.0<br />

STD3 20.7 37.2 - - 10.0 - 15.9 5.6 10.6<br />

STD4 20.6 24.4 - 6.5 - 6.2 3<strong>1.</strong>8 10.5 -<br />

STD5 24.7 5.0 - - - 9.5 14.6 17.1 29.3<br />

STD6 40.0 6.9 9.9 5.4 3.9 17.1 4.9 9.2 2.7<br />

STD7 36.1 - - 4.5 - 14.8 26.9 17.8 -<br />

STD8 50.9 4.3 5.1 4.0 15.9 19.8 - - -<br />

STD9 5<strong>1.</strong>3 - - 8.2 5.3 10.1 14.9 10.2 -<br />

STD10 55.6 - - 19.9 - - 14.6 - 9.9<br />

The synthetic standards were tested using the three methods to assess their carbon dioxide content<br />

[CO2 (%)]. All tests were conducted in triplicate for each material. The carbon dioxide uptake<br />

[CO2,uptake (%)] can be calculated as difference between carbon dioxide content of treated sample<br />

[CO2,treated (%)] minus the carbon dioxide content of untreated sample [CO2,untreated (%)] according to<br />

eq. (1).<br />

CO CO (%) CO (%)<br />

(1)<br />

2, uptake(%)<br />

2,<br />

treated<br />

2,<br />

untreateted<br />

A validation process was carried out. Carbon dioxide content [CO2(%)] in synthetic standards was<br />

measured and compared with the expected values. The accuracy and precision of the methods was<br />

evaluated. Equation (2) was used to assess the relative error of mean ( REm) [19]:<br />

RE m<br />

Z T<br />

(2)<br />

T<br />

where Z is the analytical result and T is the calculated true value. Precision was assessed by<br />

sample standard error of the mean ( SEm) (3), where is the standard deviation according to (4), n<br />

is the number of measurements and xi are the observed value for the sample and xm is the mean<br />

value of these measurements:<br />

SE m<br />

<br />

(3)<br />

n<br />

207

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