Analysis of cement slurries by inductively coupled plasma optical emission spectrometry with axial viewing

The feasibility of Portland cement analysis by introduction of slurries in an inductively coupled plasma optical emission spectrometer (ICP-OES) with axial viewing has been evaluated. After a fast manual grinding of the cement samples, owing to the pulverized state of this material, 0.1% m/v slurries were prepared in 1% v/v HCl. The calibration was performed adopting two strategies: one based on slurries prepared from different masses (50, 75, 100 and 125 mg) of a Portland cement standard reference material (NIST SRM 1881), and the other one based on aqueous reference solutions. A complete analysis of cement for major (Al, Ca, Fe, Mg and Si), minor and trace elements (Mn, P, S, Sr and Ti) was accomplished. Both strategies led to accurate results for commercial Portland cement samples, except for Si and Ti. for which the calibration with aqueous reference solutions resulted in low values. Applying a paired t-test it was shown that most results were in agreement at a 95% confidence level with a conventional fusion decomposition procedure. The ICP-OES with axial viewing and end-on gas configuration for removal of the recombination plasma zone was effective for cement slurry analysis without any undesirable particle deposition in the pre-optics interface and without severe spectral interferences. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Completeness of beta-phase decomposition reaction in Cu-Al-Ag alloys

The completeness of beta-phase decomposition reaction in the Cu-11wt%Al-xwt%Ag alloys (x = 0, 1, 2, and 3) was studied using differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and optical microscopy (OM). The results indicated that beta-phase transformations are highly dependent on cooling rate and on the presence of Ag. on slow cooling, the silver presence prevents the beta- and beta(1)-phase decomposition; thus, inducing the martensitic phase formation. After rapid cooling, a new thermal event is observed and the reverse martensitic transformation is shifted to lower temperatures.

Thermal analysis applied in the crystallization study of SrSnO3

SrSnO3 was synthesized by the polymeric precursor method with elimination of carbon in oxygen atmosphere at 250 A degrees C for 24 h. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After calcination at 500, 600 and 700 A degrees C for 2 h, samples were evaluated by X-ray diffraction (XRD), infrared spectroscopy (IR) and Rietveld refinement of the XRD patterns for samples calcined at 900, 1,000 and 1,100 A degrees C. During thermal treatment of the powder precursor ester combustion was followed by carbonate decomposition and perovskite crystallization. No phase transition was observed as usually presented in literature for SrSnO3 that had only a rearrangement of SnO6 polyhedra.

Sewage sludge coke estimation using thermal analysis

The imposition of more stringent legislation by CETESB in the State of So Paulo (Brazil) governing the disposal and utilization of sewage sludge, coupled with the growth in its generation has prompted a drive for alternative uses of sewage sludge. One option that is especially promising, due to its potential to valorize sludge, is its conversion into carbonaceous adsorbents or coke for industrial effluents treatment. Thus, a methodology is presented to estimate the coke produced from the sludge of a sewage treatment station using thermal analysis. The used sewage sludge, which comes from aerobic treatment, was collected in the wastewater treatment station of Barueri, one of the largest of the So Paulo metropolitan area. The sludge samples were collected, dried, ground, and milled until they passed an ABNT 200 sieve. The inert ambient used during its thermal treatment produces inorganic matter and coke as residual materials. Coke formation occurs in the 200-500 A degrees C range and, between 500 and 900 A degrees C, its thermal decomposition occurs. The highest formation of coke occurs at 500 A degrees C.

Studies on double selenates. I. Thermal decomposition of lanthanum and alkali metal double selenates

Thermogravimetry, differential thermal analysis and other methods of analysis have been used to study the decomposition of hydrated lanthanum and alkali metal double selenates up to 1300°C. The results showed slight variations in the initial temperature of the various intermediate decomposition stages of the double selenates, as compared with the initial temperature of the corresponding decomposition of the simple selenates. The results also permitted the suggestion of mechanisms of thermal decomposition of these compounds. © 1980.

Thermal decomposition of hydrated selenites of trivalent lanthanides and yttrium

Hydrated lanthanide(III) and yttrium(III) selenites were prepared. Simultaneous thermogravimetric and differential thermal analysis, classical differential thermal analysis, X-ray diffraction and other methods of analysis have been used in the characterisation as well as in the study of the thermal decomposition of these compounds. The results led to the composition and thermal stability and also to interpretations concerning the thermal decomposition mechanisms. © 1990.

Preparation and thermal decomposition of solid state compounds of 4-methoxybenzylidenepyruvate and trivalent lanthanides and yttrium

Solid state compounds were prepared of Ln-4-MeO-BP, where Ln is a trivalent lanthanide (except promethium) or yttrium, and 4-MeO-BP is 4-methoxybenzylidenepyruvate. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential scanning calorimetry (DSC) and other methods of analysis have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1993.

Thermal decomposition of the hydrated basic carbonates of lanthanides and yttrium in CO2 atmosphere

The hydrated basis carbonates of lanthanides and yttrium were prepared by precipitation from homogeneous solution via the hydrolysis of urea, without the addition of an auxiliary anion. Thermogravimetry, derivative thermogravimetry (TG-DTG), and differential thermal analysis (DTA) have been used in the study of these compounds in CO2 atmosphere. The results lead to the composition and thermal stability of the studied compounds, and also to a comparative study with reported results in air atmosphere. © 1993.

Thermal decomposition and stability in a series of tetrafluorborate copper(I) complexes

Tetrafluorborate copper(I) complexes containing acetonitrile, triphenylphosphine, 1,10-phenanthroline, 2,2′-bipyridine and 2-quinolinethiol have been prepared in order to study their thermal stabilities as a function of the ligands present. The characterization of the above compounds was carried out by elemental analysis and IR spectroscopy. Their thermal behaviour has been investigated and the final products were identified by X-ray powder diagrams. © 1995.

Influence of polymerization on the synthesis of SrTiO3: Part I. Characteristics of the polymeric precursors and their thermal decomposition

The influence of polymerization on the thermal decomposition of polymeric precursors and phase formation was investigated during synthesis of SrTiO3. The precipitation of polymeric precursor in acetone produced a more thermal stable precursor with lower weight loss during decomposition. This more stable precursor retarded the formation of the SrTiO3 phase. From thermal analysis, XRD and FT-IR the presence of an intermediate phase during decomposition of the precursors was observed. This is a mixed (Sr,Ti) carbonate phase with the proposed composition of Sr2Ti2O5.CO3. © 1995.

Thermal decomposition of some diuretic agents

Thermogravimetry-derivative thermogravimetry and differential scanning calorimetry were used to study the thermal behaviour of furosemide, hydrochlorothiazide, spironolactone, and amiloride hydrochloride. The results revealed the extents of their thermal stability and also permitted interpretations concerning their thermal decompositions. © 1996 Akadémiai Kiadó.

Thermal decomposition of some analgesic agents

Thermogravimetry, derivative thermogravimetry (TG, DTG) and differential scanning calorimetry (DSC), were used to study the thermal behaviour of mefenamic acid, ibuprofen, acetaminophen, sodium diclofenac, phenylbutazone, dipyrone and salicylamide. The results led to thermal stability data and also to the interpretation concerning the thermal decomposition. © 1996 Akadémial Kiadó.

Thermal decomposition of the magnesium, zinc, lead and niobium chelates derived from 8-quinolinol

Solid M-Ox compounds, where M represents Mg(II), Zn(II), Pb(II) and NbO(III), and Ox is 8-quinolinol, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), nuclear magnetic resonance (NMR) and infrared absorption spectra (IR) have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1997 Akadémiai Kiadó.

Synthesis, characterization and thermal decomposition of [Pd2 (C2-dmba) (μ-SO4) (μ-SO4) SO22]

The bridged sulphate complex [Pd2 (C2,dmba) (μ-SO4) (SO2)2] has been obtained by reacting a saturated solution of SO2 in methanol and the cyclometallated compound [Pd(C2,N-dmba)(μ-N3)]2; (dmba = N,N-dimethylbenzylamine), at room temperature for 24 h. Reaction product was characterized by elemental analysis, NMR comprising 13C{1H} and 1H nuclei and I.R. spectrum's measurements. Thermal behavior has been investigated and residual products identified by X-ray powder diffraction.

A thermal analysis study of some transition-metal dithizonates

Solid dithizonates of Fe(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II), have been prepared. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and elemental analysis have been used to characterize and study the thermal stability and thermal decomposition of these compounds.