The clay specimen was tested using an STA 409 PC thermal analyser by NETZSCH (Netzsch Gerätebau GmbH, Wittelsbacherstr. 42, Selb, Germany) coupled with a QMS 403 C Aëolos quadrupole mass spectrometer (Netzsch Gerätebau GmbH, Wittelsbacherstr. 42, Selb, Germany). Simultaneous differential thermal analysis (DTA), thermogravimetric (TG) analysis, differential thermogravimetric (DTG) analysis, and measurement of gases separated from the sample (EGA) were performed. The sample (33.0 mg) was placed in an Al2O3 crucible and heated from 40 °C to 1000 °C at a rate of 10 °C/min with an airflow of 30 mL/min.
Qms 403 c a olos quadrupole mass spectrometer
Manufactured by Netzsch
Sourced in Germany
The Netzsch QMS 403 C Aëolos quadrupole mass spectrometer is a laboratory instrument designed for the analysis of gas samples. The core function of this device is to separate and detect different gas molecules based on their mass-to-charge ratio using a quadrupole mass analyzer.
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4 protocols using qms 403 c a olos quadrupole mass spectrometer
1
Thermal Analysis of Clay Specimen
2
Simultaneous Thermal Analysis of Powdered Samples
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Simultaneous Thermal Analysis (STA) was carried out on samples vacuum-dried and ground to a grain size below 0.010 mm. The tests were carried out using the DTA-TG thermal analysis method together with EGA analysis of the released gases. Measurements were carried out using a STA 449F3 Jupiter thermal analyser (Netzsch, Selb, Germany) coupled to a QMS 403C Aëolos quadrupole mass spectrometer (Netzsch). Measurements were carried out in alumina crucibles (Al2O3), on samples of approximately 75 mg, in a synthetic air atmosphere with a flow rate of 40 mL/min, at a heating rate of 15 °C/min, in the temperature range 30–1000 °C.
3
Thermal Analysis of Solid Samples
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Specimens with the weights of 2.00–10.00 mg (analytical balance A&D GH-202) were tested with a DSC 204 F1 Phoenix® differential scanning calorimeter, TG 209 F1 Iris® thermobalance, and STA 409 PC Luxx® simultaneous thermal analyzer coupled with QMS 403C Aëolos® quadrupole mass spectrometer (NETZSCH, Selb, Germany). Measurements were taken in aluminum (DSC) and alumina (TG, STA-MS) crucibles (lid with a hole) under dry nitrogen flow (20–70 mL·min−1) with a heating rate of 10 °C·min−1. All instruments were previously calibrated for temperatures and enthalpies of phase transitions of pure (99.999%) standard substances in compliance with ASTM Practices E967, E968, E1582, and E2253: cyclohexane, Hg, Ga, benzoic acid, In, Sn, Bi, Pb, Zn, CsCl—for DSC; In, Sn, Bi, Zn, Al, Ag, Au—for TG and STA. Calcium oxalate monohydrate was used for validation of thermobalances. Mean estimated temperature and mass determination errors were 0.3 °C and 0.2%. Experimental data were processed in NETZSCH Proteus® Software according to ASTM E794, E2550 and ISO 11357-1.
4
Thermal Analysis of Cement Pastes
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The cement pastes were tested using the DTA-TG thermal analysis method, coupled with the EGA gas analysis. Measurements were performed with a STA 449F3 Jupiter (Netzsch, Cracov, Poland) device coupled with a QMS 403 C Aëolos quadrupole mass spectrometer (Netzsch, Cracov, Poland). Measurements were carried out in alumina crucibles (Al2O3), on samples weighing approx. 75 mg, in a synthetic air atmosphere with a flow rate of 40 mL/min and a heating rate of 15 °C/min. The measurements were obtained within the temperature range between 30 °C and 1000 °C.
On the basis of the TGA measurements of the mass loss in characteristic temperature ranges, the content of the individual components in the tested samples was estimated.
The content of Ca(OH)2 and CaCO3 in the initial samples after the calculation of their fraction on the basis of the value of the mass loss on the TG curves was determined from the following relationship:
where: X—content of the component in the sample, expressed in % (m/m), ΔMTG—the mass loss based on the TG curve in the temperature range characteristic for a given component, expressed in % (m/m), S— stoichiometric coefficient resulting from the chemical composition of a given component.
The content of Ca(OH)2 was calculated using the value of S = 4.12 and the content of CaCO3 using the value of S = 2.2.
On the basis of the TGA measurements of the mass loss in characteristic temperature ranges, the content of the individual components in the tested samples was estimated.
The content of Ca(OH)2 and CaCO3 in the initial samples after the calculation of their fraction on the basis of the value of the mass loss on the TG curves was determined from the following relationship:
where: X—content of the component in the sample, expressed in % (m/m), ΔMTG—the mass loss based on the TG curve in the temperature range characteristic for a given component, expressed in % (m/m), S— stoichiometric coefficient resulting from the chemical composition of a given component.
The content of Ca(OH)2 was calculated using the value of S = 4.12 and the content of CaCO3 using the value of S = 2.2.
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