Evolved Gas Analysis Research Articles

Studying smoldering to flaming transition in polyurethane furnituresubassemblies: Effects of fabrics, flame retardants, and material type

SummaryThe transition from smoldering to flaming was studied on fabric, batting, and foam assemblies via an electric spot ignition source of similar intensity to a cigarette. The materials studied included four different fabrics (cotton, polyester, cotton/polyester blend, flame retardant cotton/polyester blend), two types of batting (cotton, polyester), and three types of polyurethane foam (nonflame retardant, flame retardant by FMVSS 302 testing, flame retardant by BS5852 testing). The results from testing found that materials highly prone to smoldering could propagate smoldering into foams and lead to ignition, whereas materials that tended to melt back from the ignition source did not. Flame retardant fabrics or foam can and do prevent the transition from smoldering to flaming provided sufficient levels of flame retardants are incorporated in the upholstery fabric or foam. The transition from smoldering to flaming of cotton fabric/nonflame retardant foam assembly was also studied using temperature measurements and evolved gas analysis. It was determined that the transition takes place when the oxygen consumption by accelerating smoldering front exceeds the oxygen supply. At this point, the solid fuel gasification becomes driven by thermal decomposition rather than by surface oxidation which leads to high enough concentrations of fuel for flaming combustion to occur.

Evidence for Adsorption of Chlorine Species on Iron (III) (Hydr)oxides in the Sheepbed Mudstone, Gale Crater, Mars

AbstractAncient aquatic environments in Yellowknife Bay, Gale crater, Mars, could create favorable conditions for adsorption of chlorine compounds (perchlorate and chloride) on Fe (III) (hydr)oxides present in the Sheepbed mudstone, such as akaganeite and ferrihydrite. In this work, 5.2 mM ClO4− and 1.7 to 12 mM Cl− were adsorbed onto ferrihydrite and 5.2 mM ClO4− was adsorbed onto akaganeite at ultraacidic (pH 2–2.5), acidic (pH 3.8–4.5), and near‐neutral (pH 6.2–7.7) pH. Samples were characterized by evolved gas analysis and compared to the data collected for the Cumberland sample from the Sheepbed mudstone. Evolved gas analysis showed that ferrihydrite with 0.5–1 wt.% ClO4− adsorbed under ultraacidic and acidic conditions had a well‐resolved O2 peak at 306 °C due to the thermal decomposition of adsorbed ClO4−. All akaganeite samples with 0.5 wt.% adsorbed ClO4− had a weak peak at 312 °C tentatively assigned to decomposing perchlorate. Evolved gas analysis demonstrated that 0.5–2 wt.% Cl− adsorbed on ferrihydrite at ultraacidic and acidic pH was the main contributor to HCl evolved at >470 °C. Comparison with martian observations indicated that the temperature of the O2 peak originating from ClO4− adsorbed on ferrihydrite matched well with the thermal evolution of O2 from the Cumberland. Evolved HCl originating from Cl− adsorbed on ferrihydrite was within the temperature range of the high‐temperature HCl release from Cumberland (~770 °C). These observations suggest that ferrihydrite containing adsorbed ClO4− and Cl− could exist in the mudstone. Experimental results are consistent with adsorption at acidic pH < 4 environments through postdepositional water‐rock interactions of ferrihydrite with acid‐sulfate groundwater containing dissolved chloride and perchlorate.

On the use of TiO2 in Ti(C,N)-WC/Mo2C-(Ta,Nb)C-Co/Ni cermets

In this study, Ti(C,N)-WC/Mo2C-(Ta,Nb)C-Co/Ni cermets with varying [Mo]/([W] + [Mo]) mole ratios and constant [W] + [Mo] content were prepared by using TiO2 and carbon as substitutes for a part of Ti(C,N). In situ carbothermal reaction took place with subsequent liquid phase sintering. The thermal behavior and outgassing behavior were conducted using differential thermal analysis/thermal gravity analysis (DTA-TG) and mass-spectrometric evolving gas analysis (MS-EGA). The microstructure was investigated by scanning electron microscopy (SEM). After being sintered in N2 atmosphere, cermets without TiO2 additions generally showed rimless microstructures with black grains independently distributed from other phases, whereas the cermets with TiO2 addition showed complete core-rim microstructures. The average grain size generally decreased with increasing Mo content, and increased with increasing TiO2 substitution. Moreover, the average grain size increased with decreased N2 pressure from 50 mbar to 10 mbar at any [Mo]/([Mo] + [W]) ratio. The most interesting result was for the Mo-free cermets with 5 mol% TiO2 and 10 mol% TiO2 addition sintered in 50 mbar N2: both the hardness and fracture toughness increased compared with the cermets without TiO2 addition. The HV-KIC behavior of the majority of the cermets was superior to the industrial grades.

Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine

The adsorption of organic micropollutants onto activated carbon is a favourable solution for the treatment of drinking water and wastewater. However, these adsorption processes are not sufficiently understood to allow for the appropriate prediction of removal processes. In this study, thermogravimetric analysis, alongside evolved gas analysis, is proposed for the characterisation of micropollutants adsorbed on activated carbon. Varying amounts of carbamazepine were adsorbed onto three different activated carbons, which were subsequently dried, and their thermal decomposition mechanisms examined. The discovery of 55 different pyrolysis products allowed differentiations to be made between specific adsorption sites and conditions. However, the same adsorption mechanisms were found for all samples, which were enhanced by inorganic constituents and oxygen containing surface groups. Furthermore, increasing the loadings led to the evolution of more hydrated decomposition products, whilst parts of the carbamazepine molecules were also integrated into the carbon structure. It was also found that the chemical composition, especially the degree of dehydration of the activated carbon, plays an important role in the adsorption of carbamazepine. Hence, it is thought that the adsorption sites may have a higher adsorption energy for specific adsorbates, when the activated carbon can then potentially increase its degree of graphitisation.

Quantitative Analysis of Red Phosphorus in Polypropylene by Evolved Gas Analysis Mass Spectrometry.

Quantitative analysis of red phosphorus in polypropylene was studied using a temperature programmable pyrolyzer in combination with a mass spectrometer. Evolved gas analysis (EGA) profiles were obtained by continuous measurements of evolved gases from a sample while heating the sample at a constant heating rate. During heating of the sample, red phosphorus sublimates into P4 molecules, which have characteristic ions (m/z 31, 62, 93 and 124). Red phosphorus in polypropylene was determined from the m/z 62 ion peak area of the EGA profile with good reproducibility. The determined value was close to the value of original formulation and to the one determined by pyrolysis-GC/MS.

Plastics in Heritage Science: Analytical Pyrolysis Techniques Applied to Objects of Design.

The first synthetic polymers were introduced as constituents of everyday life, design objects, and artworks at the end of the 19th century. Since then, the history of design has been strictly connected with the 20th century evolution of plastic materials. Objects of design from the 20th century are today a precious part of the cultural heritage. They raise specific conservation issues due to the degradation processes affecting synthetic polymer-based plastics. Museums and collections dealing with the conservation of design objects and modern materials need to base their conservation strategies on compositional data that reveal the formulations of historical plastics and their decay processes. Specific and specifically optimized analytical tools are thus needed. We employed flash analytical pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC/MS) and evolved gas analysis coupled with mass spectrometry (EGA-MS) to characterize “historic polymeric materials” (HIPOMS) and heritage plastics at the molecular level with high chemical detail. This approach complements non-invasive spectroscopic diagnosis whenever it fails to obtain significant or complete information on the nature and the state of preservation of the materials under study. We determined the composition of several 20th century design objects (1954–1994) from the Triennale Design Museum of Milan (Triennale Milano - Museo del Design Italiano), which for different morphological, chemical, or physical reasons were unsuitable for characterization by non-invasive spectroscopy. EGA-MS proved capable for the study of the different fractions constituting heterogeneous micro-samples and for gaining an insight into their degradation processes from the contextual interpretation of thermal and mass-spectrometric data.

PET Fibers Modified with Cloisite Nanoclay.

The alternative method of reducing the flammability of polyethylene terephthalate (PET) fibers, analogous to dyeing of PET fibers with dispersed dyes in a high-temperature bath, was proposed. A commercial organophilic montmorillonite Cloisite®15A (C15A) was applied as a flame retardant. The aim of the presented work was to evaluate the effectiveness of the introduced modifier and the improvement of the flame-retardant properties of PET fibers by limiting oxygen index (LOI) and thermogravimetric analysis (TGA) measurements. Evolved gas analysis (EGA) by spectrometric method (FTIR) during coupled thermogravimetric analysis (TGA) was applied in order to confirm no increase in the toxicity of volatile degradation products released from burning modified fibers. The nanocomposite nature of modified fibers was confirmed based on the structural parameters of the fibers determined using wide-angle X-ray scattering (WAXS) and small angle X-ray scattering (SAXS) X-ray diffraction methods.

Investigation with using thermal analysis of gas evolution and sintering of nanopowders of zirconia prepared by sol-gel method

Thermal and XRD analyses were used to study partially stabilized zirconia powders produced by sol-gel method in order to investigate gas evolution in annealing in air and densification behavior of these powders in compaction and subsequent sintering. It was found that the powders of the initial gel contain a large amount of gas adsorbates. The amount of adsorbates decreases as the annealing temperature grows. At annealing temperature of 700 ºC, adsorbates are completely removed from the powders and the latter obtain a crystalline structure with a predominant tetragonal phase. Gas adsorbates affect densification of powder compacts during sintering and facilitate the production of ceramics with a porosity of not more than 5 %. It is shown that the production of low porosity ceramics is complicated even though powders subjected to annealing may contain nano-sized impurities or be free of these. Low-melting additives are proposed to be used for ceramics production.

Real time monitoring of slow pyrolysis of polyethylene terephthalate (PET) by different mass spectrometric techniques

In the context of waste upgrading of polyethylene terephthalate (PET) by pyrolysis, this study presents three on-line mass spectrometric techniques with soft ionization for monitoring the emitted decomposition products and their thermal dependent evolution profiles. Pyrolysis experiments were performed using a thermogravimetric analyzer (TGA) under nitrogen atmosphere with a heating rate of 5 °C/min from 30 °C to 600 °C. Single-photon ionization (SPI at 118 nm/10.5 eV) and resonance enhanced multiple photon ionization (REMPI at 266 nm) were used with time-of-flight mass spectrometry (TOF-MS) for evolved gas analysis (TGA-SPI/REMPI-TOFMS). Additionally, the chemical signature of the pyrolysis products was investigated by atmospheric pressure chemical ionization (APCI) ultra high resolution Fourier Transform ion cyclotron resonance mass spectrometry (FT-ICR MS) which enables assignment of molecular sum formulas (TGA-APCI FT-ICR MS). Despite the soft ionization by SPI, the fragmentation of some compounds with the loss of the [O-CH = CH2] fragment is observed. The major compounds were acetaldehyde (m/z 44), benzoic acid (m/z 122) and a fragment of m/z 149. Using REMPI, aromatic species were selectively detected. Several series of pyrolysis products were observed in different temperature intervals, showing the presence of polycyclic aromatic hydrocarbons (PAHs), especially at high temperatures. FT-ICR MS data showed, that the CHO4 class was the most abundant compound class with a relative abundance of 45.5%. The major compounds detected with this technique corresponded to m/z 193.0495 (C10H9O4+) and 149.0233 (C8H5O3+). Based on detailed chemical information, bulk reaction pathways are proposed, showing the formation of both cyclic monomer/dimer and linear structures.

Study on Thermal Decomposition Behavior, Gaseous Products, and Kinetic Analysis of Bis-(Dimethylglyoximato) Nickel(II) Complex Using TG-DSC-FTIR-MS Technique

The fiber-like bis-(dimethylglyoximato) nickel(II) complex, Ni(DMG)2 was successfully synthesized. The obtained samples were characterized by SEM-EDS, FT-IR, XRD, and XPS. The TG-DSC-FTIR-MS coupling technique was used to characterize the thermal decomposition behavior and evolved gas analysis of Ni(DMG)2. The non-isothermal decomposition reaction kinetic parameters were obtained by both combined kinetic analysis and isoconversional Vyazovkin methods. It was found that Ni(DMG)2 begins to decompose at around 280 °C, and a sharp exothermic peak is observed in the DSC curve at about 308.2 °C at a heating rate of 10 °C·min−1. The main gaseous products are H2O, NH3, N2O, CO, and HCN, and the content of H2O is significantly higher than that of the others. The activation energy obtained by the combined kinetic analysis method is 170.61 ± 0.65 kJ·mol−1. The decomposition process can be described by the random nucleation and growth of the nuclei model. However, it was challenging to attempt to evaluate the reaction mechanism precisely by one ideal kinetic model.

In situ characterization of foam morphology during melting of simulated waste glass using x-ray computed tomography

During batch-to-glass conversion, a glass-forming melt connects, creating a foam layer between the batch and the glass melt. Due to its transience and opacity, investigation of this foam layer presents a formidable challenge. In this work, we use in situ x-ray computed tomography to characterize the foam morphology that evolves during batch-to-glass conversion of a simulated nuclear waste glass. Rapid 1-min scans with 38 μm voxels were performed to capture the foam structure during heating. Geometric volume, total porosity, and bubble size distribution are reported. Using evolved gas analysis and combining the temperature-dependent melt viscosity with x-ray data, we describe the evolution of foam structure during the foam growth and subsequent collapse.

Tetraammineplatinum(II) and Tetraamminepalladium(II) Chromates as Precursors of Metal Oxide Catalysts.

[M(NH3 )4 ]A (M=Pt, Pd; A=CrO4 , Cr2 O7 ) and [Pt(NH3 )4 (NO2 )(Cr2 O7 )]NO3 complex salts were synthesized and characterized by a number of physicochemical methods of analysis (IR, single-crystal and powder XRD, and simultaneous thermogravimetry and differential scanning calorimetry with evolved gas analysis mass spectrometry). Thermolysis of the salts obtained in a hydrogen atmosphere proceeds with the partial reduction of chromium to a metallic state and the formation of Mx Cr1-x (M=Pt, Pd) metal solid solution with a chromium content of up to 22 at % and chromium(III) oxide. The thermal decomposition of salts in an inert and oxidizing atmosphere passes through the formation stage of the MCrO2 phase with the delafossite structure followed by its subsequent decomposition into chromium(III) oxide and noble metal. Nanosized Pt-Cr2 O3 and Pd-Cr2 O3 composites obtained by the thermolysis of precursor salts in air at 500 °C and being held at this temperature for 1 h showed a high catalytic activity in the CO total oxidation (TOX) and preferential oxidation in the excess of hydrogen (PROX) processes compared with that of monometallic Pt and Pd powders.

Flame-retardant polyurethane elastomer based on aluminum salt of monomethylphosphinate

The flame retardancy of polyurethane (PU) elastomer based on aluminum monomethylphosphinate (MeP-Al) was investigated. Thermal analysis, evolved gas analysis (TG-FTIR), flammability tests (LOI, UL 94), heat release rate (HRR) (microcombustion calorimeter), and chemical analysis of residues (SEM–EDX and FTIR) were used to investigate the flame-retardant performance and mechanism of the PU/MeP-Al. Results show that adding MeP-Al endows PU desired flame retardancy and anti-dripping property. The sample containing 20 mass% of MeP-Al passes the UL 94 V0 rating with LOI value of 29.6% and no dripping during combustion. Moreover, the heat release during combustion and the amount of organic volatile from PU decomposition are significantly reduced. The good flame retardancy, anti-dripping property, dramatically a reduction in release of heat and organic compounds are attributed to the efficient action of the MeP-Al in both the gas and condensed phase. In the gas phase, the MeP-Al decomposes into monomethylphosphinic acid to inhibit flame and reduces the heat release. In the condensed phase, MeP-Al turns into the tough aluminum pyrophosphonate and promotes PU to form stable carbonaceous char by interacting with PU.

Thermal Analysis, Compressibility, and Decomposition of Synthetic Bastnäsite-(La) to Lanthanum Oxyfluoride

Understanding basic material properties of rare earth element (REE) bearing minerals such as their phase stability and equations of state can assist in understanding how economically viable deposits might form. Bastnäsite is the most commonly mined REE bearing mineral. We synthesized the lanthanum-fluoride end member, bastnäsite-(La) (LaCO3F), and investigated its thermal behavior and decomposition products from 298 K to 1173 K under ambient pressure conditions through thermogravimetric analysis, differential scanning calorimetry, evolved gas analysis, and high temperature powder X-ray diffraction. We also investigated the compressibility of bastnäsite-(La) via single crystal X-ray diffraction in diamond anvil cells at an ambient temperature up to 11.3 GPa and from 4.9 GPa to 7.7 GPa up to 673 K. At ambient pressure, bastnäsite-(La) was stable up to 598 K in air, where it decomposed into CO2 and tetragonal γ-LaOF. Above 948 K, cubic α-LaOF is stable. High temperature X-ray diffraction data were used to fit the Fei thermal equation of state and the thermal expansion coefficient α298 for all three materials. Bastnäsite-(La) was fit from 298 K to 723 K with V0 = 439.82 Å3, α298 = 4.32 × 10−5 K−1, a0 = −1.68 × 10−5 K−1, a1 = 8.34 × 10−8 K−1, and a2 = 3.126 K−1. Tetragonal γ-LaOF was fit from 723 K to 948 K with V0 = 96.51 Å3, α298 = 2.95×10−4 K−1, a0 = −2.41×10−5 K−1, a1 = 2.42×10−7 K−1, and a2 = 41.147 K−1. Cubic α-LaOF was fit from 973 K to 1123 K with V0 = 190.71 Å3, α298 = −1.12×10−5 K−1, a0 = 2.36×10−4 K−1, a1 = −1.73 × 10−7 K−1, and a2 = −17.362 K−1. An ambient temperature third order Birch–Murnaghan equation of state was fit with V0 = 439.82 Å3, K0 = 105 GPa, and K’ = 5.58.

Unusual role of labile phenolics in imparting flame resistance to polyamide

In the quest for development of halogen-free FR additive and better understanding of the structure-flammability relationship, here we report the synthesis and characterization of a series of phenolic and benzylic succinamides, with and without aliphatic hydroxyl groups. These compounds allow for detailed investigation of the influence of these functional groups on thermal stability and FR properties in their native form and as coatings on Nylon 66 fabric. The thermal stability, char formation, heat release characteristics and thermal decomposition pathway of synthesized succinamides were studied by thermogravimetric analysis (TGA), microscale combustion calorimetry (MCC) and TGA-FTIR (Fourier Transform Infrared Spectroscopy). Phenolic succinamide, 2,3 dihydroxy-N1,N4-bis(4-hydroxybenzyl)succinamide (C1) and N1,N4-bis(4-hydroxybenzyl)succinamide (C3), exhibits about 20% char yield with low heat release characteristics while benzylic succinamides, N1,N4-dibenzyl-2,3-dihydroxysuccinamide (C2) and N1,N4-dibenzylsuccinamide (C4), exhibit poor char yield and high heat release characteristics. Thermal decomposition followed by evolved gas analysis of all these succinamides indicate that the decomposition pathway is very much dependent on the presence of phenolic moieties. Heat release characteristic and flammability of Nylon 66 coated with succinamides (10% by weight) clearly indicate that the coating of C1 and C3 impart flame resistance to Nylon 66. These studies clearly reveal that phenolic derivatives are essential for improving the thermal stability, flame resistance and lowering the heat release characteristics of Nylon 66 through char formation.

TG-FTIR for kinetic evaluation and evolved gas analysis of cellulose with different structures

In this study, the effect of structural characteristics of cellulose on its pyrolysis behavior was investigated. The structure of crystalline cellulose was altered by ball milling (BM) pretreatment, resulting in decreases in crystallinity and degree of polymerization. The initial pyrolysis temperature of BM-cellulose decreased, as well as the temperature at which maximum weight loss rate was achieved. Moreover, BM-cellulose was observed to produce more solid residue. The pyrolysis process was fitted by n-order reaction model. The global activation energy of Un-treated cellulose (228.3–270.6 kJ/mol) was higher than that of BM-cellulose (166.8–187.0 kJ/mol). TG-FTIR experiment showed that BM-cellulose yielded more CO2 and H2O than Un-treated cellulose. This research provided a comprehensive analysis of the effects of structural characteristics of cellulose on the pyrolysis behavior of cellulose.

Thermal behavior of naproxen and ketoprofen nonsteroidal anti-inflammatory drugs

Nonsteroidal anti-inflammatory drugs naproxen (NAP) ((+)-(S)-2-(6-methoxynaphthalen-2-yl) propionic acid) and ketoprofen (KET) (RS)-(2-(3-benzoylphenyl)-propionic acid) were investigated by thermoanalytical techniques (TG/DTG/DTA, DSC and hot-stage microscopy) and evolved gas analysis (TG-FTIR) for evaluating their thermal behavior. In air, TG curve of NAP presented one mass loss step followed by the burning of carbonaceous material, with final residue of 1.5%, while in nitrogen, a single mass loss step was observed. After melting, if the sample is submitted to an isotherm it evaporates. According to DSC curve, NAP melts at 153.5 °C (∆Hfus = 31.6 kJ mol−1; ∆Sfus = 73.5 J K−1 mol−1) and recrystallizes in the cooling step. These events were confirmed by hot-stage microscopy. TG-FTIR studies revealed that NAP decomposes by releasing 2-methoxynaphthalene and propionic acid. Ketoprofen TG curves in both atmospheres presented a single mass loss. When the sample was kept under isotherm, after melting, it evaporated. From DSC data, the melting at 93.3 °C (∆Hfus=28.4 kJ mol−1, ∆Sfus = 76.9 J K−1 mol−1) was observed, without crystallization or cooling.

High‐Temperature HCl Evolutions From Mixtures of Perchlorates and Chlorides With Water‐Bearing Phases: Implications for the SAM Instrument in Gale Crater, Mars

AbstractEvolved hydrogen chloride (HCl) detected by the Sample Analysis at Mars (SAM) instrument's evolved gas analysis (EGA) mode on board the Mars Science Laboratory Curiosity rover has been attributed to oxychlorines (i.e., perchlorates and chlorates) or chlorides in Gale crater samples. Previous laboratory EGA studies of oxychlorines have been unable to reproduce the high‐temperature (>600 °C) HCl evolutions observed in most Gale crater samples. The objective of this work was to reproduce these high‐temperature HCl releases from laboratory mixtures of perchlorates and chlorides with phases that evolve water upon heating. Magnesium and sodium perchlorate and chloride were mixed with saponite, nontronite, and a basaltic glass and analyzed in a laboratory thermal evolved gas analyzer configured to operate similarly to the SAM instrument. Na perchlorate and chloride evolved HCl only when mixed with all three water‐producing phases. Mg perchlorate and chloride evolved a mid ‐temperature HCl release (~450–550 °C) and evolved an additional high‐temperature HCl release (~810–820 °C) when mixed with saponite. This work demonstrated that chlorides, either originally present or from perchlorate decomposition, evolved high‐temperature HCl when reacting with water from water‐producing phases. The HCl release temperature was dependent on the mixture's mineralogy and chemical composition. HCl releases detected by SAM were consistent with oxychlorines and/or chlorides in the presence of water‐producing phases. Additionally, this work provided constraints on the presence of oxychlorines or chlorides and their cation types, which has implications for past aqueous and diagenetic processes, the potential for past life, and detection of organics by EGA.

Elucidation of the decomposition reactions of low-fluorine YBa2Cu3O7-x precursors during film pyrolysis

Chemical solution deposition methods such as low-fluorine metal organic decomposition, are nowadays widely employed in the production of YBa2Cu3O7-x superconducting films. The investigation of the chemical reactions that convert the organic precursors into the pyrolysis product is essential for the optimization of the pyrolysis step, and, ultimately, for the comprehension of the growth process. In this work, a detailed analysis of the single-salt precursors, of the ternary precursor solution and its thermal decomposition was carried out through infrared spectroscopy (FITR), thermogravimetric analysis (TGA), evolved gas analysis (EGA), X-Ray diffraction (XRD), coupled with quench experiments, and X-Ray photoelectron spectroscopy (XPS). The combination of these techniques led to the identification of the precursors and the proposal of a reaction path for pyrolysis. More in detail, a copper/ammonia coordination compound was identified and it is the first to decompose at low temperatures via a mixed path of hydrolysis and oxidation to produce copper oxide. The decomposition of the other two precursors is superimposed at higher temperatures and it yields a mixture of BaF2, YF3 and Ba1-xYxF2+x.

Comparative study of the thermal behavior of Sr\u2013Cu\u2013O gels obtained by sol\u2013gel and microwave-assisted sol\u2013gel method

In the literature data, several papers reported the synthesis by various chemical or physical methods of the SrCu2O2 (SCO) having possible applications in thermoelectric or completely electronic devices such as solar cells, liquid crystal displays and touch screen. A great challenge is represented by the formation of the pure SrCu2O2 (SCO), due to the high labiality of the Cu valence, depending on temperature. In the present paper, the thermal behavior of Sr–Cu–O gels obtained by sol–gel (SG) or microwave (MW)-assisted SG methods was studied in order to establish the appropriate thermal conditions for pure nanostructured SrCu2O2 preparation. As reagents, copper and strontium acetylacetonate in alcoholic media were used. The starting solutions were homogenized either by stirring for 2 h at room temperature or were exposed to MW for 5 min at 300 W and a frequency of 2.45 GHz. Both solutions were left to gel at room temperature. The obtained gels were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, as well as by thermal analysis combined with evolved gas analysis (TG/DTA-MS) measurements in air, inert and reducing atmospheres. For both type of samples, a stepwise thermal decomposition of the gels was noticed in a large temperature range. In the case of samples obtained by microwave-assisted SG method, a higher number of thermal effects were registered assigned to a higher number of molecular species formed in the sample. The residues obtained by non-isothermal treatment up to 900 °C, of both type of samples, were investigated by X-ray diffraction. The results demonstrate the influence of the MW on the SG synthesis and on the thermal properties of the resulted gels. Based on the obtained results, the required thermal treatment of the gels in order to obtain convenient precursors powders for obtaining pure SrCu2O2 could be proposed.