Evolved Gas Analysis by Infrared Spectroscopy

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Evolved Gas Analysis by Infrared SpectroscopyS. Materazzia; S. Vecchiob

a Department of Chemistry, “Sapienza” Università di Roma, Rome, Italy b Department of ChemicalEngineering (I.C.M.A.), “Sapienza” Università di Roma, Rome, Italy

Accepted uncorrected manuscript posted online: 12 April 2010

Online publication date: 12 April 2010

To cite this Article Materazzi, S. and Vecchio, S.(2010) 'Evolved Gas Analysis by Infrared Spectroscopy', AppliedSpectroscopy Reviews, 45: 4, 241 — 273, doi: 10.1080/05704928.2010.483664, First posted on: 12 April 2010 (iFirst)To link to this Article: DOI: 10.1080/05704928.2010.483664URL: http://dx.doi.org/10.1080/05704928.2010.483664

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Applied Spectroscopy Reviews, 45:241–273, 2010Copyright © Taylor & Francis Group, LLCISSN: 0570-4928 print / 1520-569X onlineDOI: 10.1080/05704928.2010.483664

Evolved Gas Analysis by Infrared Spectroscopy

S. MATERAZZI1 AND S. VECCHIO2

1Department of Chemistry, “Sapienza” Universita di Roma, Rome, Italy2Department of Chemical Engineering (I.C.M.A.), “Sapienza” Universita diRoma, Rome, Italy

Abstract: The analytical applications of the evolved gas analysis (EGA) performed byinfrared spectroscopy, for the period extending from 2005 to 2009, are collected in thisreview. By this technique, the nature of volatile products released by a substance sub-jected to a controlled temperature program are on-line determined, with the possibilityto prove a supposed reaction, either under isothermal or under heating conditions.

Keywords: Evolved Gas Analysis, EGA, TG–FTIR, hyphenated TGA

Introduction

“A technique in which the nature and/or amount of volatile product(s) released by a sub-stance subjected to a controlled temperature program is (are) determined”: this is how theIUPAC Compendium of chemical terminology defines the evolved gas analysis (EGA).

The possibility to on-line detect the nature of the released gases or vapors has becamefundamental to prove a supposed reaction, either under isothermal or heating conditions.

Among the different possibilities, thermoanalytical instruments, such as pyrolyzers,thermobalances, differential thermal analyzers, or calorimeters (but sometimes even simplytemperature-controlled reactors), are the most commonly used tools to heat a sample underinvestigation.

Thermogravimetry, in addition, is very useful for the quantification of each singlegaseous evolution process as the result of an increasing thermal ramp or a defined isother-mal temperature. These techniques have been successfully on-line coupled to performevolved gas analysis. To obtain the infrared (IR) spectra of the gases evolved during theprogrammed analysis, the thermoanalytical instrument is usually coupled with a Fouriertransform infrared (FTIR) spectrometer by means of a heated transfer line; the releasedvapors or gases are so transferred to the heated gas cell of the FTIR instrument, the tem-peratures of the cell and of the transfer line being independently selected.

The history of the EGA-FTIR and EGA-mass spectrometry (MS) hyphenated tech-niques from the first attempts to 2004 has been previously reported (1–6).

In this article, the applications of the evolved gas analysis performed by infrared spec-troscopy for the period extending from 2005 to 2009 are proposed. Many examples arereported from the literature, and often the references are generally obtained from the jour-nals that specialize in thermal analysis. At least 50% of the applications of the evolved gas

Address correspondence to S. Materazzi, Department of Chemistry, “Sapienza” Universita diRoma, p.le A. Moro 5, 00185 Rome, Italy. E-mail: [email protected]

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242 S. Materazzi and S. Vecchio

analysis are devoted to polymers and inorganic compounds, and the review is consequentlyorganized with two separate sections per year. However, the number of publications onhyphenated techniques continues to grow in areas of specialized applications; as a conse-quence, it is not unusual for an article on the topic to appear in an unfamiliar journal or atrade-specific publication.

The problem is that unless the terminology relating to the specifics of the hyphenatedtechnique are present in the published keywords, the articles may be difficult to locate. Asa result, certain important articles may have been overlooked, and the authors apologize forsuch inadvertent omissions.

2005 Applications

Polymers and Inorganics

A typical problem when analyzing the kinetics by dynamic thermogravimetric analysis(TGA) of polymer degradation consists in that different models can fit equally well, orthe model does not fit the TGA data. Although the model is mathematically supported,verification should be done by comparing the results with the FTIR spectra obtained fromthe gases evolved along the experiment. The FTIR analysis of the gases evolved from aTGA experiment could confirm that the logistic mixture model is suitable to analyze adynamic TGA trace (7).

Poly(ethylene terephthalate) was exposed to oxygen and carbon dioxide plasmas fordifferent periods of time. The surface-modified samples were characterized by severaltechniques, included TG-FTIR. The main difference between both types of plasma was thetimescale of degradation, which was much faster when using oxygen plasma. Aggregateglobular features were produced by different treatments due to chain scission and furtherrecombination of evolved products (8).

Thermal behavior of commercial polyvinyl chloride (PVC) cable insulation, bothbefore and after extraction of plasticizers, fillers, and other agents, were tested by TG-FTIRand other ageing methods; the kinetic parameters were used for the lifetime simulation ofthe materials (9). Pyrolysis and fire behavior of high-impact polystyrene (HIPS) containingred phosphorus and melamine polyphosphate were investigated by Braun and Schartel(10), and by TGA/FTIR the evolution of the gases evolved during the catalytic pyrolysisof three commercial ethylene-vinyl acetate copolymers has been studied by Marcilla et al.(11–14). The thermal degradation behavior of bacterial poly (3-hydroxybutyrate) has beenreported by pyrolysis-gas chromatography (GC)-FTIR using a semicontinuous furnace inthe temperature range of 200–600◦C (15). The thermal degradation of polycarbonate inair was studied as a function of mass loss using TGA/FTIR by Jang and Wilkie (16),who showed that oxygen may facilitate branching as well as radical formation via theformation of peroxides. These peroxides undergo further dissociations and combinations,producing aldehydes, ketones, and some branched structures, mainly in the beginning stageof degradation. A study of the thermal decomposition of well-characterized poly(ethyleneoxide) (PEO) under nonoxidative conditions has been conducted by thermogravimetryin both dynamic and isothermal mode also coupled on-line with infrared spectroscopyor mass spectrometry. Analysis of the evolution of low-molecular-weight decompositionproducts by TG/FTIR and TG/MS techniques showed that main decomposition productsare ethyl alcohol, methyl alcohol, alkenes, noncyclic ethers (ethoxymethane, ethoxyetane,and methoxymethane), formaldehyde, acetic aldehyde, ethylene oxide, water, CO, and CO2


Evolved Gas Analysis by Infrared Spectroscopy 243

(17). Zhang et al. (18) studied the thermal stabilities and thermal degradation mechanism ofcarboxy-polycaprolactam prepolymers (PA6), amine-terminated rigid aromatic polyamideprepolymers (PPIA), and their block copolymers (PA6-PPIA-PA6). The results showed thatthe thermal stability of the block copolymers was improved by the block polycondensation,which eliminates the unstable terminal groups, and the strong hydrogen bond interactionbetween the amide linkages.

The thermal properties of poly(aspartic acid), obtained by a new original methodsynthesis in microwave radiation field, were determined by thermogravimetry coupledeither with infrared spectroscopy (TG/FTIR) or with mass spectrometry (TG/MS) (19).

Thermal decomposition processes of TATB and DATE were investigated by using dif-ferential scanning calorimetry (DSC), pressure differential scanning calorimetry (PDSC),TG, TG-FTIR coupled technique, and in situ thermolysis rapid-scan-FTIR coupling tech-nique. Kinetic parameters of thermal decomposition were obtained, and mechanisms ofthermal decomposition were presented. The results showed that there exist some interme-diate products in the initial thermal decomposition process of TATB and DATB, such asbenzofurazan or benzofuroxan compounds (20).

Hyphenated TG-FTIR analysis was among the techniques used for the characterizationof novel mesoporous montmorillonite heterostructure materials (21).

Aluminum nanopowder has a high reactivity with water, which causes its “aging”and consequent reduction in its effectiveness. The thermodesorption of adsorbed gasesand water on nanometer-sized aluminum powders was investigated using on-line coupledthermogravimetry-Fourier transform infrared–mass spectrometry (TG-FTIR-MS) (22). Anew family of mesoporous reactive inorganic solids as obtained as aggregates of nanocrys-talline oxides has proven to be effective destructive sorbents for toxic chemicals: FTIR-evolved gas analysis (EGA) was employed for analysis of surface-bound products (23).

On-line FTIR measurements showed that the products of the thermal decompositionof thiourea and its oxides vary significantly with the reaction temperature (24). CaSO4,the product of sulfur-fixation reaction, decomposes at the temperature higher than 1,200◦Cthat commonly appears in combustion chamber of boiler, which negatively affects thedesulfurization in combustion process. TG-FTIR was exploited to investigate the effectof existence of oxides, carbonates, and oxides/carbonates mixture in the combustion onthermal stability of CaSO4 at high temperature (1,000–1,450◦C) and the results showedthat the addition of oxides and carbonates of some alkaline-earth metals in sulfur-fixationreagent will enhance the decomposition temperature of CaSO4 by more than 50◦C, whichconfirmed the effect of these additives on prohibition of CaSO4 decomposition (25).

Braun et al. (26) reported the thermostabilization of lignin fibers used as precursorsfor carbon fibers in air. Spectroscopic analyses revealed the oxidation of susceptible groupswithin the lignin macromolecule to ketones, phenols, and possibly carboxylic acids inthe early stage of the reaction; the later stage involving the loss of CO2 and water andthe formation of anhydrides and possibly esters. The understanding of the mechanism ofactivated carbon prepared from cellulose residues from the acid hydrolysis of Discoreazingiberensis C.H. Wright was useful to investigate systematically, with the help of TG-FTIR, the pyrolysis of the carbonization with ZnCl2 on different conditions (27) and thenumerical modeling of straw combustion in a fixed bed was proposed by Zhou et al. (28).

Evolved gas Fourier transform infrared spectroscopy was often applied to the analysisof complexes. An aqueous solution-gel route was developed for the preparation of the fer-roelectric material strontium bismuth niobate, and TG-FTIR analysis was important to haveinformation on the behavior of the precursor during thermal treatment for the deposition ofthin films (29, 30). Levchenko and coworkers (31) completed the characterizaton of in situ



direct synthesized silver alkanethiolates, AgS(CH2)nCH3, with various long chain-lengthsubstituents (n = 9, 11, 15, and 17). TG-FTIR studies identified the nature of the decompo-sition products from the low- and high-temperature decompositions of calcium magnesiumacetate, assessed as an agent for the reduction of NOx, SO2, and HCl, at the pilot scale, in adown-fired combustor (32). The investigation of europium(III) sulphate hydrate and samar-ium(III) sulphate hydrate was performed by thermal analysis and simultaneous infraredEGA-FTIR spectroscopy to determine the dehydration and decomposition steps and tocalculate the water content (33). The thermal behavior of 1,2,4-triazole and 1,2,4-triazinederivatives was described by Sikorska-Iwan and Modzelewska-Banachiewicz (34). Vec-chio et al. studied the kinetic and the decomposition mechanism of zirconium and titaniumphosphates intercalated with 1,10-phenanthroline (35) and palladium(II) 1-allylimidazolecomplexes (36). The gaseous products of the decomposition of hexaaminecobalt(III) ox-alate tetrahydrate were qualitatively and quantitatively analyzed by MS and FTIR to confirmthe gaseous products of HACOT decomposition under studied atmospheres (37).

Jang and Wilkie applied FTIR evolved gas analysis to clays (38), policarbonate de-composition (16, 39), and polystyrene (40).

Insulations and insulation binders used in standard home insulations and stove insula-tions were analyzed by TG-FTIR and the comparison of the off-gassing differences betweenvarious binder systems has proven to be very useful in development of binder systems (41).

Teng et al. (42), using a TG-FTIR coupled method, obtained direct evidence of thedecomposition process of lithium hexafluorophosphate. Their study showed that LiPF6 isstable under normal temperature when the content of water is very low.

Veiderma and coworkers (43) published a review of the results on single and coupledsubstitutions of F for OH and of CO3 and SO4 for PO4 in synthetic and natural apatites, theirinfluence on apatite structure and properties, studied by peak fitting FTIR, X-ray diffrac-tion (XRD), TG/differential thermal analysis (DTA) and TG/EGA methods. Tansuaaduand coworkers (44) studied the thermal reactions in natural fluorapatite or fluorcarbonateapatite and ammonium sulfate mixtures with mole ratio 1:4 at calcination up to 500◦C bysimultaneous thermogravimetry and FTIR analysis of the evolved gases, showing that thecomposition of natural apatite has little impact on the release of NH3.

Slager and Prozonic (45) reported the calibration of the IR signals from TGA effluentgas using decomposition of solids and evaporation of liquids. The IR signal separates theTGA weight losses for quantitation and allows a successful deconvolution of the TGA datawhere several compounds are evolving from the TGA at the same time. It is unnecessaryto heat the transfer lines and IR cell as long as the effluent has some volatility at ambienttemperature.

Gallignani and coworkers (46) published a critical review about on-line gaseous phasesgeneration with FTIR spectrometry detection. Different experimental approaches for thedetermination of ethanol and carbonates in different samples and for the simultaneousdetermination of benzene, toluene, and methyl tert-butyl ether in gasoline and butyl acetate,toluene, and methyl ethyl ketone in commercial paint solvents has been compared to EGA.The results are in good agreement.

Other Applications

A computational fluid dynamics (CFD) modeling study has been undertaken to examine thecofiring of pulverized coal and biomass with particular regard to the burnout of the largerdiameter biomass particles. Computations were based on a research combustion facilitythat replicates an industrial coal-fired power station (47). The effect of coal oxidation in



air at 140◦C on the technological properties of cokes obtained at laboratory scale from twomedium volatile bituminous coals has been studied by Cimadevilla et al. (48). TG-FTIRdata for tar evolution from 35 coals of different elemental compositions revealed a generallyconsistent behavior for coals from different parts of the world, showing increasing activationenergies with increasing coal rank. The same correlation was also true for methane, althoughthe slope of the activation energy versus carbon content curve was rather flat, at least upto about 90% carbon content (49). The thermal degradation of refuse-derived fuels wasreported by several authors and was shown to take place through several main mass lossstages; the analyses of evolved gas allowed discrimination of the contributions of thedifferent fractions (paper, low density polyethylene (LDPE), wood, rubber, etc.) to theglobal decomposition (50, 51). The pyrolysis behavior of two types of biomass (pine andwheat) and a Polish lignite (Turow) in the presence of minerals and ion-exchanged calciumusing a variety of laboratory-scale methods including pyrolysis-gas chromatography–massspectrometry (py-GC-MS) and thermogravimetric analysis coupled to a FTIR spectrometerwas studied by Stojanowska and Jones (52). Thermochemical treatment of waste effluentsoriginating from the olive oil food industry was investigated by Taralas and Kontominas(53) and from palm oil by Yan et al. (54).

The FTIR spectra of the gaseous products during thermal degradation of films based onxanthan/wheat starch and xanthan/maize starch showed for the xanthan a broad absorptionin the 2,750–3,300 cm−1 region, probably indicating decomposition of a-d-mannopyranosylgroups, present in xanthan side chains. For pure starches, absorptions related to alcoholO-H stretching, CO stretching of CO2, CO, and carbonyl compounds were observed.For xanthan/starch mixtures (50/50) the same compounds as those for the pure polymerdegradation were evolved (55). The pyrolysis characteristics of wheat straw with steamexplosion and solid fermentation treatment were investigated by the thermogravimetrycoupled with Fourier infrared spectroscopy to analyze the evolved gases and to characterizethe four stages (56).

Thirteen saccharide tobacco ingredients have been pyrolyzed using TGA under 10%oxygen in nitrogen to simulate the burning conditions of a smoldering cigarette. Someproducts were generated in several distinct temperature regions, indicating that more thanone mechanism of pyrolysis was operating in a given saccharide. The work has indicated thatformaldehyde is generated from the pyrolysis of most of the saccharides in 10% oxygen innitrogen (57). Four kinds of reconstituted tobacco sheets were heated in a thermogravimetricanalyzer in different atmospheres: the profiles of the evolving products were recorded bythe thermogravimetric analyzer coupled to a TG-FTIR spectrometer (58).

The thermal behavior under nonisothermal conditions of some low-acidity carboxyliccationites with acrylic-divinylbenzene (DVB) matrix was investigated in air and nitrogenatmosphere up to 600◦C. Thermal analysis (TG/DTG) combined with MS and FTIR wasused to characterize the resins decomposition steps and the degradation products (59).

Production of electronic boards containing brominated flame retardants is constantlyincreasing, posing important problems with disposal of products containing these materials.Barontini et al. (60) investigated the thermal degradation behavior of electronic boardsmanufactured using tetrabromobisphenol A and diglycidyl ether of bisphenol A epoxyresins. In order to solve the problem of secondary pollution during crushing of discardedprinted circuit boards (PCB), pyrolysis behavior and corresponding pyrolysis products ofdiscarded PCB were mensurated using TG-FTIR analysis system. The mechanisms oftransport and generation of irritant gas formed during crushing of PCB were analyzed (61).

Thermal analysis, coupled with FTIR spectroscopy, was proposed by Materazzi andcoworkers to determine the quality of foods like pasta (62).



The FTIR spectra of gas products evolved during the thermal degradation of filmsformed by soy protein isolate–sodium dodecyl sulfate complex indicated the formation ofCO2, CO, NH3, and other unsaturated compounds, suggesting that the reaction mechanismincluded at the same time the scission of the C N, C(O) NH, C(O) NH2, NH2, andC(O) OH bonds of the protein (63).

Talawar and coworkers (64) reviewed the process technology for the manufactureof dinitrogen pentoxide and its utility for the synthesis of most powerful explosives oftoday and studied the thermolysis of diaminoglyoxime and its evaluation as a ballisticmodifier in double-base propellant formulations. The hyphenated TG-FTIR data also re-vealed the evolution of gases containing species such as CN, NH, OH and oxides ofnitrogen during thermal decomposition (65). Turcotte and coworkers (66) investigated thethermal properties of the energetic material 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaaza-tetracyclo-(5.5.0.05,9.03,11)-dodecane (HNIW), also known as CL-20, by simultaneousTG-DTA-FTIR-MS.

2006 Applications


Organic solvents cyclohexane, dichloromethane, hexane, and tetrahydrofuran were tested toseparate the dioctylphthalate (DOP) as plasticizer from the PVC-based materials; the releaseof DOP, HCl, and CO2 was observed by simultaneous TG-FTIR (67). The thermal degrada-tion of polymethacrylates containing carboxylic groups, namely, poly(methacryloyloxybutanoic acid) (PMBA), poly(methacryloyloxy hexanoic acid) (PMHA), and poly(p-methacryloyloxy benzoic acid) (PMBeA), was investigated; the analysis by FTIR of thevolatile products from the studied polymers was shown to differ notably from those ob-tained for polymethacrylic acid (68). Thermal degradation behaviors of polyoxymethylenein nitrogen have been systematically studied by Duan and coworkers (69). Two primarydegradation mechanisms were definitely determined by the production of formaldehydeand carbon monoxide collected from successive on-line FTIR spectra. The TG/FTIR tech-nique has been employed to study the evolution of the gases evolved during the thermal andcatalytic decomposition of low-density (LDPE) and high-density polyethylene (HDPE).This technique allows obtaining the infrared spectra of the gases evolved in situ, as theyare generated. The evolution of the gases obtained during the progressive deactivation ofthe catalysts employed (HZSM5 and HUSY) has also been studied (70, 71).

The thermal dehydroxylation of a goethite-carbonate solid solution was studied withcombined FTIR-temperature programmed desorption (TPD) experiments. The TPD datarevealed dehydroxylation peaks involving the intrinsic dehydroxylation of goethite and alow-temperature peak which was shown to be associated to the release of nonstoichiometricwater from the goethite bulk and surface (72).

Rapid-scan FTIR spectroscopy and time-of-flight (ToF) mass spectrometry were uti-lized to study thermal decomposition of three imidazolium-based ionic liquids, with 1-ethyl-3-methyl-imidazolium (emim) as the cation and nitrate, cloride, and bromide as theanions. The thermal decomposition involved heating rates of 2000 K/s and temperatures to435◦C in an ambient inert gas at 1 atm. Using sub-milligram quantities of each compound,examinations of the evolution of gas-phase species revealed that the most probable sites forproton transfer and subsequent secondary reactions were primarily the methyl group andsecondarily the ethyl group (73).



Cutting of single-walled carbon nanotubes (SWNT) has been achieved by extensiveozonolysis at room temperature. Monitoring of the evolved gases for both pristine andpurified SWNT indicated that CO2 was produced during the ozonolysis process with adependence on both system pressure and temperature. During heating, FTIR analysis ofgases released also indicated that carbon oxygen groups on the sidewalls of SWNT arereleased as CO2 (74).

Poly (vinyl alcohol) (PVA) and l-lactic acid (LA) were compounded and characterizedwith several techniques, included EGA by FTIR, to get biodegradable polymeric film withuseful mechanical, thermal, and bacteriostatic properties for possible medical or packagingapplications (75).

The reaction kinetics of the oxidation and gasification of four types of model and realdiesel soot have been characterized for a wide range of conditions relevant for moderndiesel engine exhaust and continuously regenerating particle trapping or filter systems. Thereactivity of the investigated diesel soot and model substances was positively correlatedwith their oxygen mass fraction and negatively correlated with their carbon mass fraction(76).

The employment of used tires as a new source of raw materials for different applicationscan be a partial solution to the great environmental problems generated by these productsconcerning their disposal at waste depots. High-resolution thermogravimetric analysis (Hi-Res TGA) was used to quantify the elastomer composition of SBR/NR in tire formulations.FTIR-EGA was also employed for composition quantification of used tires and the resultswere compared to those obtained by Hi-Res TGA (77).

The decomposition temperature, thermal behavior, kinetic parameters, and evolvedgas pattern of a dimeric copper complex with N,N-dimethylaminoethanol, a precursor forchemical vapor deposition, was described by Mazhar et al. (78). Synthesis and characteri-zation of metal polycarboxylates constructed from lanthanides (79) or transition metal ions(80) were reported by Rz

↪aczyska and coworkers. Thermal decomposition of a compound

consisting of a tetrachloroferrate(III) anion and a quinolinium cation, of general formula(QH)(FeCl4), has been studied by Wyrzykowski et al. using TG-FTIR, TG-MS, DTA, andDTG techniques (81). DSC, TG and TG-FT-IR, and XRPD have been used to examinethe effects of supposedly inert atmospheres of argon and nitrogen on the mechanism ofthe thermal decomposition of copper(II) oxalate (82). The thermal decomposition of di-ethyldithiocarbamato tellurium (IV) was investigated by simultaneous TG/DTG/DSC-FTIRmethod in nitrogen atmosphere by Wang et al. (83).

The thermal degradation process of ethoxylated bisphenol A (BPA) and oxyalkyle-nated 2,6-toluylenediamine-based polyurethane (PU) foams blown with pentane and flameretarded by novel NaH2PO4 and NaHSO4 intumescent system (5:3, w/w) was studied byTG-MS and TG-FTIR (84, 85). Sawicka published the results of TG-FTIR, DSC, andquantum-chemical studies on the thermal decomposition of quaternary ethyl-ammonium(86) and methyl-ammonium halides (87). The thermolysis of benzenediazonium tetrafluo-roborate was studied by thermogravimetry in dynamic mode. The speed of the thermolysiswas estimated gravimetrically and by infrared spectroscopy, considering the change ofthe intensity of the absorption band at 1,498 cm−1, which corresponds to fluorobenzene(88).

Two enantiomeric forms of xylose were characterized by thermal analysis and theirevolved gases were analyzed with combined TG-FTIR technique (89). The thermal behaviorof l-leucine under inert conditions was investigated by Li and coworkers (90). The resultsof a kinetic study showed that the decrease in mass of l-leucine was due to subliming ratherthan decomposing. And this was proved by the FTIR spectrum analysis and the directly



observed subliming phenomenon. The results of TG-FTIR experiments showed that therewas only one stage of decomposition process that happened after the subliming of leucine.

The influence of several experimental parameters that may affect the quantification ofFTIR signals have been studied using a combined TA-FTIR-MS system. Parameters studiedincluded sample mass (1–400 mg), carrier gas flow rate (25–200 mL min−1), resolution ofthe FTIR spectrometer (1–32 cm−1), and location of injection of the calibrating gas. MSanalysis, which was not significantly affected by the experimental conditions, was usedas a reference for assessing the accuracy of quantification by FTIR. The quantificationof the spectroscopic signals was verified by the decomposition (NaHCO3) or dehydration(CuSO4–5H2O) of compounds with well-known stoichiometry (91, 92).

Other Applications

The use of biomass fuels, representing a renewable energy source, reduces the consumptionof fossil fuels and limits the emissions of SOx, NOx, and heavy metals. The devolatilizationof biomass fuels (of different origin, properties, and composition) and biomass componentswas studied coupling TG analysis with infrared spectroscopy by Biagini and coworkers(93). The pyrolysis of palm oil wastes was conducted using TG-FTIR by Yang et al.(94) Cashew nut shells were studied by Tsamba et al. (95) because they are importantbiomass wastes abundant in most of the tropical countries. As biomass feedstock, theyare important energy sources that can play an important role as fuel for energy generationthrough the ordinary thermochemical processes (95). Chicken litter disposal is a majoreconomic and pollution concern. Poor waste management practices lead to air and wa-ter pollution. To produce a useful renewable resource for energy, optimal conditions forcombustion were studied by TG-MS and TG-FTIR (96, 97). In order to study the effectof minerals on biomass pyrolysis, experiments on pyrolysis of corn straw with differentpretreatment methods were performed by using a TGA coupled with an FTIR spectrometry(98).

Focusing on the Argonne premium coals, which cover a wide range in rank betweenlignite (Ro = 0.25) and low-volatile bituminous (Ro = 1.68), TG-FTIR provided complexpyrolysis profiles of oxygen-containing gases, which yield information on the sources of thedifferent peaks observed in coal as a function of rank from a chemical-structure standpoint(99, 100). Coupled TG-FTIR technique was used for identification of gaseous compoundsevolved at thermal treatment of six coal samples from different deposits (Bulgaria, Russia,Ukraine) (101). Thermal analysis and combustion characteristics of mixture of oil shale andoil shale semi-coke were investigated on a TG-FTIR analyzer, with regard to comparing theprocess of the mixture with those of the individual components (102, 103). TG-FTIR andflow reactor experiments were performed to study soot oxidation on MnOx-CeO2 mixedoxide catalysts in model diesel exhaust gas (104, 105).

A new oxygen carrier CaSO4 used in chemical-looping combustion was developed.The reaction kinetics of system which consisted of CaSO4 and CH4 were studied usingTG-FTIR (106).

Armenta et al. developed a new vapor-phase manifold coupled with FTIR spectroscopyto determine the ethanol amount in mouthwash (107).

Baker and coworkers used a thermogravimetric system connected to a Fourier trans-form infrared spectrometer to examine aspects of the pyrolytic generation of formaldehydefrom sugars and tobacco samples in order to provide pyrolytic information to explain someof the diverse observations and mechanistic factors involved in the generation of formalde-hyde during cigarette smoking (108). Moreover, Baker reviewed the studies assessing the



influence of tobacco ingredients on the chemistry and toxicity of cigarette mainstreamsmoke (109).

The influence of polycaprolatone-triol (PCL-T) on the thermal degradation propertiesof soy protein isolate (SPI)-based films was studied by Schmidt and Soldi. The FTIRspectra of gas products evolved during the thermal degradation indicated the formation ofOH, CO2, NH3, and other saturated compounds, suggesting that the reaction mechanisminvolved simultaneous scission of the C(O) O polyester bonds and C N, C(O) NH,C(O) NH2, and NH2 bonds of the protein (110).

The influence of the heating rate and of the presence of oxygen on the decompositionpathways and on the decomposition product yields obtained from the thermal degradationof waste electronic boards containing brominated flame retardants was investigated byTG-FTIR techniques (111). The characteristics of HBr forming and scavenging duringthe pyrolysis of waste printed circuit boards were investigated using the TG-FTIR and aquartz-pipe pyrolysis system (112).

A systematic and comparative evaluation of the pyrolysis of halogen-free flame-retarded epoxy resins containing phosphine oxide, phosphinate, phosphonate, and phos-phate and the fire behavior of their carbon fiber composites was presented by Braun etal. (113). Decomposition pathways are proposed based on thermogravimetry also coupledwith evolved gas analysis (TG-FTIR), kinetics, and analysis of the residue. Similar studieswere also reported by Romzo et al. (114).

The aging characteristics of pyrotechnic compositions are influenced not only bytemperature but by surrounding effects as humidity and vibrations. The thermal stabilityof the pyrotechnic system magnesium-sodium nitrate was investigated by using massspectrometry and Fourier transform infrared spectroscopy to analyze the evolved gases.Only above 170◦C were evolving gases detected, whereas during the first step no gases weredetectable. The detected gas mainly consisted of CO2, CO, and N2O, with smaller amountsof NO2, NO, and possibly HCN (115). Experiments using simultaneous TG-DTA coupledwith FTIR and MS were performed on BTAw (bis-(1(2)H-tetrazol-5yl)-amine monohy-drate, recently considered for use as a low-smoke pyrotechnic fuel) in both helium and dryand CO2-free air atmospheres, and evolved gas analysis was used to determine the gaseousdecomposition products (116). Diaminofurazan (DAF), used as a precursor in the synthesisof many high-performance insensitive high explosives, was characterized by thermalstudies and evaluated as a ballistic modifier in double-base propellant formulations (117).

There is a need of fine 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) for various highexplosive formulations to achieve desired mechanical strength, ease in processing, and,finally, to provide better performance of the end product. The characteristic properties offine TATB thus obtained have been confirmed by FTIR, DSC, and TG-FTIR (118).

Pyrolysis and combustion of wood under different oxygen concentrations were studiedby using TG-FTIR analysis. Effects of oxygen concentration on TGA of wood and evolvedgas analysis were thoroughly analyzed, and as a consequence the process of pyrolysisand combustion of wood was divided into four steps (119). Fei and coworkers (120, 121)published their TG-FTIR studies that have been used to determine the total acidity andcarboxylic acid contents for a range of lignites. Based on the investigation of the polysac-charide structure of cellulose by using Fourier transform spectrum analysis, the pyrolysisbehavior of cellulose was studied at a heating rate of 20 K/min by TG analysis coupled withFTIR. Experimental results showed that the decomposition of cellulose mainly occurredat the temperature range of 550–670 K (122). The pyrolysis behavior of white pine wasstudied at different heating rates by TG analysis coupled with FTIR. Experimental resultsshowed that the pyrolysis of wood can be considered as the pyrolysis of the combination



of three main components; that is cellulose, hemicellulose, and lignin. The product mainlyconsisted of acids, alcohols, aldehydes, ketones, esters, water, and small-molecule gases(123). Wood ceramics (WCS) are new porous carbon materials that have been shown topossess many excellent properties. In order to investigate the chemical mechanism, pyroly-sis of medium density fiberboard (MDF) was analyzed by thermogravimetry coupled withFourier transform infrared spectroscopy (124).

2007 Applications


Chuang (125) investigated the thermal degradation of diacetylene-containing polyurethane.The three stages of degradation of copolymers involved four and five steps of degradation,respectively, as revealed by TG-FTIR, which identified the main decomposition products:CO2, tetrahydrofuran, and ether-containing olefin. Datta and Rohn (126) investigated ther-mal transitions and stability of polyurethane intermediates and polyurethanes. Thermal de-composition of obtained glycolysates and polyurethanes was followed by thermogravimetrycoupled with Fourier transform infrared spectroscopy. Main products of thermal decom-position were identified. The aging of a filled and cross-linked ethylene propylene dieneelastomer was studied by Tomer et al. (127). The thermal stability of EPDM was assessedby TGA and evolved volatile gases were identified using FTIR coupled spectroscopy.

Soudais and coworkers proposed a coupled DTA-TGA-FT-IR investigation of thepyrolytic decomposition of EVA, PVC, and cellulose (128).

The combined TG-FTIR technique was employed to study of decomposition pathwayof new lanthanide complexes with 1,2,4-benzenetricarboxylic acid (129). Thermoanalyt-ical studies of titanium(IV) acetylacetonate xerogels were reported with emphasis on therole of evolved gas analysis (EGA by FTIR and MS) (130). The temperature-programmeddesorption (TPD) of electrostatically hydrogen- and metal-bonded oxalate complexes at thegoethite surface was investigated with concerted FTIR measurements (TPD-FTIR) to 660 Kand mass spectrometer analyses of the evolved gases to 900 K. These reactions took placewith the concomitant dehydroxylation reaction of goethite to hematite and decarbonation ofbulk-occluded carbonate. The measurements revealed three important stages of desorption(131). Lead zirconate titanate nanopowders (PZT) were prepared by modified sol-gel pro-cess in ethylene glycol system with zirconium nitrate as the zirconium source. The researchshowed that it was critical to add lead acetate after the reaction of zirconium nitrate and tetra-butyl titanate in ethylene glycol system for preparing PZT of exact titanium content. Thereaction mechanisms of the sol synthesis, preparation of xerogel, and agglutinating processwere characterized using FTIR, nuclear magnetic resonance (NMR) imaging, TG-FTIR,and GC-MS (132). The thermal decomposition mechanism of ammonium phosphomolyb-date hydrate in air and inert gas atmospheres was determined and the intermediate andfinal products formed during the thermal decomposition were characterized by Ilhan etal. (133). Imidazole rings of histidine residues often form part of the metal-binding sitein metalloproteins, so ligands with the 2-imidazolyl units are good models for mimickingbiological metal-binding sites because the histidine imidazole ring is often attached viathe 2-position to the side chain when the imidazole is coordinated to a metal. Thermo-analytical studies on biomimetic molecules were reported by Materazzi and coworkers(134).

Madarasz and coworkers (135) studied the evolved gas analyses (TG/DTA-MS and TG-FTIR) on dehydration and pyrolysis of magnesium nitrate hexahydrate in air and nitrogen.



Malecka et al. (136) proposed a TG/DTA/MS/IR study on decomposition of cadmiummalonate hydrates in inert and oxidative atmosphere.

Thermogravimetry coupled with infrared evolved gas analysis and pyrolysis gaschromatography–mass spectrometry demonstrated that multiwall carbon nanotube pres-ence slightly delays thermal volatilization (15–20◦C) without modification of the thermaldegradation mechanism (137).

An on-line-coupled TG-FTIR EGA instrument has been used to identify and monitorthe evolution of gaseous products during the thermal decomposition of phenylalanine,glycine, and tyrosine in flowing N2 atmosphere up to 800◦C. The results indicated that thethermolysis processes of these compounds are similar (138, 139).

The thermal decomposition of two energetic ionic liquids, formed by pairing the4-amino-1,2,4-triazolium cation with chloride and nitrate anions, was studied by confinedrapid thermolysis. Rapid-scan FTIR spectroscopy and time-of-flight mass spectrometrywere utilized in conjunction to identify the products of decomposition. Decomposition wasachieved under heating rates of 2000 K/s and temperatures up to 340◦C (140).

A typical problem when analyzing the kinetics by dynamic TGA of polymer degra-dation consists in that different models can fit equally well, or the model does not fit theTGA data. It has been suggested that this is due to the presence of overlapping processes.High-resolution TGA helps to clarify the problem in some cases, but in many other casesthe problem remains unsolved. The FTIR analysis of the gases evolved from a TGA experi-ment confirmed that the logistic mixture model is suitable to analyze a dynamic TGA trace.It was also found that the logistic mixture model is suitable to separate single componentsfrom FTIR spectra (141).

Other Applications

A K-Al2O3 catalyst was prepared using the wet impregnation method with K2CO3 asa precursor salt. During the activation process, a clear interaction between potassiumcarbonate-derived species and the support took place resulting in the formation of Kaluminate-like species, as observed by EGA-MS and FTIR (142). The pyrolysis of polymersand copolymers in the presence of zeolites as catalysts was proposed by Marcilla et al.(143–145).

EGA by TGA/FTIR was used to study the thermal decomposition products evolvedduring the degradation of several commercially available organo-clays. It was found thatthe decomposition pattern of the organoclays was different for each sample (146). Amethodology has been developed for EGA in clay raw materials and ceramic compositionsused in ceramic tile manufacture using several coupled thermal analysis techniques(TG-DSC-quadrupole–mass spectrometry (QMS)-FTIR). The different types of gases(CO2, CO, NOx, F, SOx) evolving from these raw materials during a thermal cycle upto a peak temperature of 1,200◦C were characterized. The thermal analysis technique(TG-DSC-QMS-FTIR) is a suitable technique for analyzing evolved gases with lowuncertainties for carbon compounds quantification. Furthermore, the methodology allowsthe mineralogical origin identification of the elements present in the evolved gases (147).TG integrated with FTIR was used to investigate the activities and selectivities of HUSY,REY, and HZSM-5 zeolites and, furthermore, the heavy oil cracking catalyst MLC anddistillate oil cracking catalyst CIP used in China’s refining industry (148).

Identification and monitoring of gaseous species released during thermal decomposi-tion of pure thiourea in argon, helium, and air atmosphere have been carried out by bothon-line coupled TG-FTIR and simultaneous TG/DTA-MS apparatuses (149).



Combustion characteristics of pulverized coal in O2/N2 or O2/CO2 mixtures werestudied by TG-FTIR. The influence of particle size and atmosphere on combustion charac-teristics of pulverized coal was analyzed. Experimental results showed that finer pulverizedcoal has better burning characteristics than the coarser one, and the FTIR three-dimensionalspectra also indicated that the combustion products in O2/CO2 mixtures are significant dif-ferent from those in O2/N2 mixtures (150). Desulfurization efficiency as well as mineralcomposition and microstructure of desulfurization residues were investigated when cofir-ing high-sulfur coal and Ca-Al based additives in a high-temperature electric resistancefurnace, and the decomposition of CaSO4 and products composition of pure mineral sys-tem CaO-Al2O3-CaSO4 were studied by means of TG-FTIR-XRD (151). FTIR coupledwith TGA, which can provide in situ data in real time, was applied by Song et al. (152) toilluminate the SO2 evolution in the product gases during CaS oxidation. A thermoanalyticaltechnique combined with FTIR equipment was used for comparative estimation of thermalbehavior of samples with simultaneous identification of gaseous compounds formed andemitted at thermooxidation of solid fossil fuels (oil shale, semi-coke, coal) from differentdeposits (Estonia, Israel, Jordan, Morocco, Bulgaria, Russia). Notable differences in thecomposition of gaseous compounds evolved as well as differences in the absorbance ofindividual species in FTIR spectra depending on the origin of fuel and on the heating rateused were determined (153).

The fire retardancy mechanisms of aluminum diethylphosphinate in combination withmelamine polyphosphate and zinc borate were analyzed in glass-fiber-reinforced polyamide6,6. The influence of phosphorus compounds on the polyamide decomposition pathwayswas characterized using thermal analysis coupled with evolved gas analysis (TG-FTIR)(154). The effect of phosphorus and nitrogen on flame-retardant cellulose was studied byGaan and Sun (155). Differential scanning calorimetry coupled with Fourier transform in-frared spectroscopy was applied to identify the gas products evolved during the combustionreactions of polymers containing various flame retardants. Results are compared with orwithout flame retardant (156).

Thermal analysis combined with composition analysis has been used to identifyevolved gas when burning solid waste and to demonstrate the advanced incineration tech-nology, which is adapted to process the selected solid waste. TG coupled with FTIRspectroscopy and mass spectrometry (TG-FTIR-MS) offers structural identification ofcompounds evolved during combustion processes (157). Cheng et al. identified evolvedgases when burning household waste (158, 159). Thermogravimetric behavior of simulatedmedical waste was studied in the atmosphere of nitrogen and air at different heating rates.Experimental results show that the main thermogravimetric stages of simulated medicalwaste in the atmosphere of nitrogen and air have the similar products (160). Experimentaltests and results obtained for the study of tire waste pyrolysis, conducted by means ofthermogravimetric analysis of the material and the simultaneous determination, throughFourier transform infrared and mass spectrometry of the decomposition products were re-ported by Galvagno et al. (161). Hall and Williams (162) analyzed the products from thepyrolysis of plastics recovered from the commercial-scale recycling of waste electrical andelectronic equipment.

Accurate determination of gas concentration emitted during thermal degradation (py-rolysis) of biomass in forest fires has been demonstrated to be one of the key points in recentresearch on physical-based fire spread models. However, it has not been really well solvedby classical invasive sensors and procedures. De Castro et al. (163) applied a methodol-ogy to use open-path Fourier transform–based infrared (OP-FTIR) spectrometry as a re-mote sensing technique that permits in situ, nonintrusive, and simultaneous measurements.Main gaseous by-products have been measured and quantified in terms of path-integrated



concentrations. Different emission ratios have been determined for the species under study.These results can help to simplify the modeling of pyrolysis processes inside the physical-based models for fire spread. Based on the investigation of the polysaccharide structure ofcellulose by using Fourier transform spectrum analysis, the pyrolysis behavior of cellulosewas studied by Wang and coworkers (164) and Yang et al. (165). Cofiring of secondarybiomass fuels with coal in coal-fired pulverized fuel boilers is facing increased applicationin large-scale power production. To expand the fundamental knowledge on the thermo-chemical behavior of biomass and waste fuels especially regarding the release of the fuelbound nitrogen, the characterization of chicken litter (CL), biomass mix (BM), and meat andbone meal (MBM) and an high viscosity (HV) coal blend was performed using TG-FTIRanalysis (166). Short rotation willow coppice (SRC) and a synthetic biomass, a mixture ofthe basic biomass components (cellulose, hemicellulose, and lignin), were investigated forthe influence of potassium on their pyrolysis behaviors (167). Cashew nut shells are onetype of the most abundant biomass tropical wastes that can be used for energy generation.The pyrolysis product yields obtained by TG-FTIR analysis were compared with the avail-able data in the literature for wood, and it was found that cashew nut shells have tars andvolatiles at levels equivalent to those of wood pellets (168). Thermal analysis and combus-tion characteristics of mixtures of oil shale and its semi-coke were investigated by meansof an on-line TG-FTIR interconnection analyzer, with the aim of comparing the behaviorof the mixture with that of its components (169). Pressurized pyrolysis characteristics andkinetics of biomass (wheat straw) were investigated using an advanced TG-FTIR under thecatalytic and non catalytic conditions. As FTIR has shown, the elevated pressure and usedcatalysts can decrease apparent activation energy and can increase the CO and CH4 yield(170). Kinetic research on the pyrolysis of lignin was carried out by Yao et al. (171). Thecatalytic effects of five metal chlorides, including CaCl2, KCl, NiCl2, CoCl2, and ZnCl2, onthe pyrolysis of lignite were investigated by Zou et al. (172). The results showed that CaCl2and ZnCl2 inhibited the conversion of organic matters into light species during pyrolysisof lignite samples, whereas KCl, NiCl2, and CoCl2 promoted the conversion.

TGA combined with infrared analysis of the EGA has been used to study the thermaldegradation behavior of epoxy resin in both air and nitrogen. The mass loss as a function oftemperature has been correlated with the evolution of carbon monoxide (CO) and carbondioxide (CO2), and oxygen consumption as measured using an oxygen analyzer (173).Toldy and coworkers (174) proposed the study of the flame-retardant mechanism of anewly synthesized phosphorus-containing reactive amine, which can be used both as cross-linking agent in epoxy resins and as a flame retardant. The mode of action and degradationpathway were investigated by in situ analysis of the gases evolved during the degradationby thermogravimetric measurements coupled on-line with infrared (TG-EGA-FTIR) andmass spectroscopy (TG/DTA-EGA-MS).

Using TG-MS and TG-FTIR, Matuschek et al. (175) studied the composition of severalsamples of ambient aerosol particles including different types of laboratory-generatedparticles (pigment black, diffusion flame soot, spark-generated carbon) and two ambientaerosol samples (diesel soot and particulates collected in a road tunnel).

2008 Applications


Chuang et al. (176) reported the thermal degradation of poly(siloxane-urethane) copoly-mers. The two stages of degradation have been found to comprise eight degradationsteps and two interchange reactions, as revealed by TG-FTIR analysis. Experimental



results indicated that polyimides derived from ODPA and several alicyclic-containingdiamines show fairly high thermal stability and no weight loss before a temperatureof 400◦C in nitrogen. The TG-IR results represented that the major evolved productsfrom the nonoxidative thermal degradation were detected to be hydrocarbons, CO, CO2,H2O, and aromatic compounds (177). TG-FTIR and fluorescence studies by Chen andhis coworkers (178) showed that the coordinated Eu2O3 nanoparticles with average sizeof less than 20 nm are surrounded by a three-dimensional network and are properlyincorporated into the polymethyl methacrylate (PMMA) and polystyrene (PS) matrix,the hybrid films can emit intense red light under ultraviolet radiation, and their emissionfluorescence spectra display the same characteristic emission peaks of Eu3+ ions (178).The thermal decomposition of polyurethanes obtained from glycolysates (produced viaglycolysis of waste polyurethane foam) was followed by TG coupled with FTIR spec-troscopy (179). The effect of lanthanum oxide on thermooxidative degradation behaviorof LLDPE was studied by thermogravimetry, oxidation induction time measurements,rheological, and TG-FTIR analyses. The TG-FTIR results showed that the products ofthermooxidative degradation of LLDPE in the initial stage did not change in the presenceof lanthanum oxide; however, the chain scission reaction at high temperature could behindered (180). The pyrolysis of PVC was qualitatively analyzed by TG-FTIR, and HClremoval efficiency of Ca-based additives was semi-quantitatively studied by means ofTG-FTIR. Additionally, the thermodynamic equilibrium modeling was also carried outto understand the formation of HCl from PVC and from mixtures of PVC with differentadditives. Experimental results showed that the pyrolysis of PVC took place in twosteps accompanied by the release of HCl and hydrocarbon, respectively. Almost all Cltransformed to HCl, and hardly any other kinds of Cl compounds were detected. Theaddition of Ca-based additives extended the second weight loss step of PVC, but they didnot affect the release time when the maximum HCl concentration appeared. The maximumHCl concentration decreased according to the increase of additive amount; that is, the HClremoval efficiency increased as the Ca/Cl molar ratio increased (181). The thermal behaviorof Cd2+ and Co2+ phenyl-vinyl-phosphonates was studied using two different experimentalstrategies: the coupled TG-EGA (FTIR) technique by decomposition in nitrogen and airand the kinetic analysis of TG data obtained in dynamic air atmosphere at four heating rates(182).

Latex collected from natural rubber trees forming membranes can be used as bioma-terials in several fields being the degradation temperature a key parameter. TG coupled toFTIR is a useful technique to investigate the thermal degradation of both latex and castfilms (membranes), which were obtained from Hevea brasiliensis (RRIM 600 clone) andused without stabilization (183).

Flame-retarded thermoplastic polymer compounds were prepared containing recycledrubber tires, low-density polyethylene, ethylene vinyl acetate copolymer, and an intumes-cent additive system consisting of waste polyurethane foam and ammonium polyphosphate.The environmental impact was estimated by determining the gas components of CO2 andCO evolving from the compounds during the burning process using a gas analyzer systemconstructed by coupling an FTIR unit to a mass loss calorimeter. The new material formsa thermoplastic rubber of excellent processability, making it suitable for application in theconstruction industry (184). Possible flame-retardant mechanisms were also revealed byPawlowski and Schartel by applying TG-FTIR hyphenated analysis (185).

Thermal analysis of three azomonoether dyes, exhibiting liquid-crystalline properties,was performed in dynamic air atmosphere by Rotaru and coworkers (186) because thethermal stability studies and the evaluation of the kinetic parameters of each physical or



chemical transformations are essential for a full characterization, before attempting accuratethin films’ depositions of such materials used in nonlinear optical applications.

Pyrolysis and combustion are both promising treatments for oil sludge. These processeswere studied by TG-FTIR by Song et al. (187–189), and the results indicated that boththermal processes were composed of five phases: drying and gas desorption, light oilreactions, heavy oil reactions, semi-coke reactions, and mineral reactions. Due to theexistence of O2, the mass loss during combustion was higher than during pyrolysis andthe light oil reaction phase was more significantly influenced. The characteristics and gasproduct properties of pyrolyzing sewage sludge were determined by Shao et al. (190),aiming to utilize efficiently the waste for energy recovery. The gas products released underdifferent pyrolysis conditions were analyzed on-line using FTIR spectroscopy and theresults showed that the gas composition was highly dependent on temperature, and thereleasing of the gas species was consistent with the weight loss of sludge in pyrolysis.

The crystal structure and the thermoanalytical study of a manganese(II) complex with1-allylimidazole was reported by Materazzi and Vecchio (191). Evolved gas analysis al-lowed proving the oxidative decomposition pattern of the examined complex (191). Thethermal decomposition of zinc and strontium acetate hemihydrate has been studied byTG-DTA/DSC and TG coupled with FTIR under nonisothermal conditions in nitrogen gasfrom ambient temperature to 600◦C (192, 193). Thermal decomposition of ammoniumparatungstate tetrahydrate under nonreducing conditions was reported by Fait and cowork-ers (194). Thermal decomposition of compounds consisting of tetrahalogenocuprate(II)anions and a tetraethylammonium cation (195) and bis(tetraethylammonium) tetrachloro-ferrate(II) has been studied using TG-FTIR, TG-MS, and DTA techniques (196).

A Pb(Zr,Ti)O3 precursor gel made from a sol prepared using 1,1,1,-tris(hydroxymethyl)ethane, lead acetate, and zirconium and titanium propoxides, stabilizedwith acetylacetone, was analyzed using TGA-FTIR analysis by Chowdhury et al. (197).To better understand the influence of two different manganese ores on structure, mineralcomposition, and reductibility of sinter produced from them, the coupled TG-FTIR tech-nique was used to simultaneously measure mass losses and evolved gas composition (198).The thermal stability and the structure of a new co-crystal of theophylline formed with ph-thalic acid was characterized by a complete TG/DTA-EGA-MS and TG-EGA-FTIR study(199). The thermal behavior of nicotinic acid under inert conditions was investigated byTG, FTIR, and TG/DSC-FTIR. The results of TG/DSC-FTIR and FTIR indicated that thethermal behavior of nicotinic acid can be divided into four stages: a solid–solid phase tran-sition (176–198◦C), the process of sublimation (198–232◦C), melting (232–263◦C), andevaporation (263–325◦C) when the experiment was performed at the heating rate of 20 Kmin−1 (200).

The partial oxidation of methanol for the production of hydrogen was investigatedin both a fixed-bed microreactor and in a thermogravimetric analyzer (TG-FTIR) from180 to 250◦C using a commercial Cu/ZnO/Al2O3 catalyst (201). The decomposition ofan amorphous precursor for S-doped titania (TiO2) nanopowders, prepared by controlledsol-gel hydrolysis-condensation of titanium(IV) tetraisopropoxide and thiourea in aqueousisopropanol, has been studied up to 800◦C in flowing air by simultaneous thermogravimet-ric and differential thermal analysis coupled on-line with quadrupole mass spectrometer(TG/DTA-MS) and FTIR spectrometric gas cell (TG-FTIR) for analysis of gases and theirevolution dynamics (by EGA) in order to explore and model thermal annealing processesof fabrication techniques leading to S:TiO2 photocatalysts with photocatalytic activitiesunder visible light (202). Zhang et al. (203) tested the Pt/CeO2 catalysts with differentcalcination temperatures to evaluate their effect on hydrogen iodide (HI) decomposition in



the sulfur-iodine cycle at various temperatures. CO oxidation and decomposition behaviorsover nanosized 3% Au/Fe2O3 catalyst and over the Fe2O3 support were studied in situvia thermogravimetry coupled to on-line FTIR spectroscopy (TG-FTIR), which was usedto obtain temperature-programmed reduction (TPR) curves and evolved gas analysis. Thecatalyst was prepared by a sonication-assisted Au colloid based method and had an Auparticle size in the range of 2–5 nm. Carburization studies of H2 prereduced samples werealso made in CO gas (204).

Ammonium nitrate (AN) is one of the main nitrogen fertilizers used in fertilizationprograms. However, AN has some serious disadvantages—being well soluble in water,hardly 50% of the N-species contained are assimilated by plants. The second disadvantageof AN is associated with its explosive properties. Kaljuvee et al. (205) clarified the influenceof different lime-containing substances—mainly Estonian limestone and dolomite—asinternal additives on thermal behavior of AN.

Ross and DeVore (206), using EGA-FTIR, investigated the desorption of nitric acidfrom boehmite and from gibbsite (206).

Armenta et al. (207) presented a critical review of on-line vapor-phase generationcombined with Fourier transform infrared spectrometry for detection. They discussed dif-ferent experimental approaches developed for generating the vapor phase based on differentprinciples (e.g., thermal volatilization, acid-base, redox reaction, and covalent hydride gen-eration). By using examples of applications, they demonstrated the analytical potential ofon-line vapor-phase generation in vibrational spectrometry in order to improve the selec-tivity and the sensitivity of the measurement step and to make environmentally friendlyprocedures available for problem solving in the analytical laboratory (207).

Thermal analysis is a useful tool for investigating the properties of polymer/claynanocomposites and mechanisms of improvement of thermal properties. In their review,Leszczynska and Pielichowski (208) presented examples of applications of DSC, modulatedtemperature differential scanning calorimetry (MT-DSC), dynamic mechanical thermalanalysis (DMA), thermal mechanical analysis (TMA), TG, and thermoanalytical methods;that is, TG coupled with Fourier transformation infrared spectroscopy (TG-FTIR) and massspectroscopy (TG-MS) in characterization of nanocomposite materials.

Other Applications

The flame-retardant mechanisms of aluminum diethylphosphinate (AlPi) and its combina-tion with melamine cyanurate (MC) in glass-fiber-reinforced poly(butylene terephthalate)(PBT/GF) were analyzed using thermoanalytical techniques also coupled for evolved gasanalysis (TGA-FTIR) (209). The flame retardance of aromatic thermotropic liquid co-polyester (TLCP) on polyethyleneterephtalate (PET) was investigated. Evolved gas anal-ysis by IR measurements indicated that TLCP would decompose to produce phosphorus-containing small molecular compounds in the pyrolysis process (210, 211). Flame-retardantproperties of polyethylene (PE)/graphite intercalation compounds (GIC) intercalated withphosphorous compounds were evaluated by limiting oxygen index by Han et al. (212).Toldy and coworkers (213) proposed the study of the flame-retardant mechanism of anewly synthesized phosphorus-containing reactive amine, which can be used both as cross-linking agent in epoxy resins and as a flame retardant. The mode of action and degradationpathway were investigated by in situ analysis of the gases evolved during the degradationby thermogravimetric measurements coupled on-line with infrared (TG-EGA-FTIR) andmass spectroscopy (TG/DTA-EGA-MS).

Tu et al. (214) investigated the pyrolysis properties of animal manures using athermogravimetric analyzer coupled with the Fourier transform infrared spectroscopy.



Experimental results showed that an animal manure pyrolysis process can be divided intothree stages: dehydration, pyrolysis, and carbonization. These stages may produce differedfeatures on end residuum, weight loss rate, and peak features.

FTIR spectrometry was employed to detect the gas evolved from bituminous coalduring the combustion process by Duan et al. (215).

The catalytic effect of three kinds of potassium salts on cellulose pyrolysis kineticsand products was studied on a thermogravimetric analyzer coupled with a Fourier trans-form infrared spectroscopy. Experimental results showed that potassium salts catalyzedthe dehydration and depolymerization reactions in the initial pyrolysis stage, enhanced therelease of oxygenated gases, intensively catalyzed the formation of char, and restrainedthe production of volatiles (216–218). The addition of calcium carbonate caused a de-crease in S-containing compounds that evolved from the pulp mill lime sludge combustion.The temperature range for decomposition by pyrolysis is higher than for decompositionby combustion. FTIR spectra of the gases evolved showed considerable amounts of Ca,in addition to HNCO and CH4 absorptions. NH3 gas was not detected, and sulfur- andnitrogen-containing gases only developed in insignificant amounts (219). Switchgrass is ahigh-yielding perennial grass that has been designated as a potential energy crop, and onemethod of converting switchgrass to energy is by thermochemical conversion to syngas.The pyrolysis process was found to comprise four stages: moisture evaporation, hemi-cellulose decomposition, cellulose decomposition, and lignin degradation. FTIR analysisshowed that the following gases were given off during the pyrolysis of switchgrass: car-bon dioxide, carbon monoxide, acetic acid, ethanol, and methane (220). The gas productsemitted from rice husk were detected on-line with FTIR by Fu et al. (221). The main gasproducts were H2O, CO, CH4, and some organic carbohydrate mixtures. The pyrolysisbehavior of three typical agricultural residues including rice husk, rice straw, and wheatstraw was studied at different heating rates (15, 40, and 100◦C/min) in a dynamic nitrogenflow of 80 mL/min by TG analysis coupled with FTIR. The various gaseous productsreleased during biomass pyrolysis were examined (222, 223). The release behavior ofnitrogen-containing gases such as NH3, HCN, NO, and HNCO during wheat straw py-rolysis was also examined in argon atmosphere to reveal the distribution and selectivityof nitrogen compounds from biomass volatile matters. The results showed that experi-mental conditions have a great effect on the distribution of fuel-nitrogen during pyrolysis(224).

The thermal decomposition of a kind of brominated epoxy resin (BER) printed circuitboard was investigated by using TG-FTIR and Py-GC/MS and the mechanism of the thermaldecomposition of the resin was discussed by Li and coworkers (225).

Pyrolysis of certain medical waste materials and their mixtures was studied usingthermogravimetry coupled with Fourier transform infrared spectroscopy. From TG andDTG curves, the materials had little effect for each other in the medical waste pyrolysis.From FTIR curves, evolved volatile products from mixture were almost the sum of volatileproducts evolved from each material that composed the mixture, and there was no distinctreaction between each material (226, 227).

2009 Applications


Shen and Gu (228) performed experiments to investigate the mechanism of the cellulosepyrolysis and the formation of the main products. The evolution of the gaseous productswas examined by the 3-D FTIR spectrogram.



The thermal performance of polymers (aromatic polyesters) prepared from isoph-thaloyl chloride with diphenolic acid and its esters was studied by thermal analysis and thedecomposition mechanisms were investigated by hyphenated TG-FTIR analysis. The anal-yses of the decomposition process and products indicated that the pendent carboxyl groupsare responsible for its low thermal stability. Accordingly, a decomposition mechanism forthe first stage was proposed (229).

A cyclohexane solution of PS (polystyrene) and an ethyl acetate solution of PMMAwere used as flowing liquid; the ZnO/polymer hybrid colloids were successively producedby focused pulsed laser ablation of ZnO target in interface of solid and flowing liquid. Thehybrid films were characterized by fluorescence spectrum, thermogravimetry with FTIR(TG/FTIR), and X-ray photoelectron spectrum (230).

The thermal decomposition processes of polypropylene (PP) formulations containingintumescent flame-retardant (IFR) additives as well as the individual components in thecomposites have been studied by Zhang et al. (231), who showed that the initial releasegases such as NH3 or H2O helps to swell the melted PP polymer and to improve the flameretardance of IFR-PP composite (231). In the same view, Wang and coworkers (232) studiedmelamine phosphate (MP) and the mixture of MP and pentaerythritol (PER) and biodegrad-able PVA/glycerol-plasticized thermoplastic starch (TPS) and its intumescent flame-retardant composites with microencapsulated ammonium polyphosphate (MCAPP) (233).

The flame retardance of poly(butylene terephthalate) containing aluminum dieth-lyphosphinate and/or nanometric metal oxides such as TiO2 or Al2O3 was investigated.AlPi acts mainly in the gas phase through the release of diethylphosphic acid, which pro-vides flame inhibition. Part of AlPi remains in the solid phase, reacting with the PBT tophosphinate-terephthalate salts that decompose to aluminum phosphate at higher tempera-tures. The metal oxides interact with the PBT decomposition and promote the formation ofadditional stable carbonaceous char in the condensed phase (234). Huang and Wang (235)published a TGA-FTIR study on the effect of CaCO3 on the thermal degradation of EBAcopolymer.

The thermal degradation behavior of hydrogenated nitrile-butadiene rubber (HNBR)/clay nanocomposite and HNBR/clay/carbon nanotubes nanocomposites was reported byChen et al. (236).

Poly(lactic acid) (PLA)-grafted TiO2 particles were prepared by in situ melt polycon-densation of lactic acid onto the surface of TiO2 nanoparticles. The resulting products werecharacterized by FTIR, XPS, TG-FTIR, XRD analysis, and electron microscopy observa-tion to have a better understanding of bonding between the graft polymer and nanopar-ticles (237). Indium- and gallium-doped ZnO nanoparticles were prepared by Cimitanand coworkers (238). A comprehensive study of the preparation process, including a thor-ough investigation by TG-FTIR and TG-MS of the thermal-purification procedure, waspresented.

The thermal oxidation/degradation behaviors and the flame-retardant mechanism ofepoxy resin (EP) and EP/silsesquioxane composites were studied by Wu and coworkers(239). Nitrogen polyhedral oligomeric silsesquioxane (NPOSS) can retard the movementand scission of polymeric chains of EP and form a stable charred layer in the condensedphase to prevent the underlying materials from further combustion (239).

Simultaneous thermogravimetric and differential thermal analysis coupled on-line withquadrupole mass spectrometer (TG/DTA-MS) and FTIR spectrometric gas cell (TG-FTIR)have been applied for analysis of released gases (EGA) and their evolution dynamics inorder to explore and simulate thermal annealing processes of fabrication techniques of theaimed S:TiO2 photocatalysts with photocatalytic activities under visible light (240, 241).



Decomposition of crystalline and amorphous titanium(IV)oxo-acetylacetonate chemi-cals have been studied in situ up to 800◦C in flowing air by simultaneous thermogravimet-ric and differential thermal analysis coupled on-line with quadrupole mass spectrometer(TG/DTA-MS) and FTIR spectrometric gas cell (TG-FTIR) for the analysis of evolvedgases (EGA) in order to get more information about pyrolytic processes taking place atelevated temperatures during smooth TiO2 layer processing (242).

Ti and urea, mixed according to the molar ratios of 2:1, 3:1, and 4:1, were milled underthe same condition, and the products decomposed from the as-synthesized powders werecharacterized by DSC and TG-FTIR. The results showed that the reaction progress is adiffusion reaction and that ammonia gas (NH3) and cyanic acid (HNCO), the decomposedproducts of urea, react with the refined Ti to form TiN. The grain refinement of Ti has asignificant effect on the efficiency of reactive ball milling (243, 244). Doca et al. (245)published a TG, EGA, and kinetic study by nonisothermal decomposition of a polyanilinewith different dispersion degree.

Nemliher and coworkers (246) studied the characteristics of bioaragonite of shells ofrecent T. decussatus. IR analysis of the evolved gases revealed the emission of water andCO2. The peculiarity of bioaragonite was explained by substitution of H2O and sulphateion into the lattice.

The CeO2 and Ni/CeO2 catalysts with different calcination temperatures were testedfor hydrogen production in sulfur-iodine (SI or IS) cycle. It was evident that there was achange in particle size and morphology as the calcination temperature increased from 300to 900◦C (247, 248).

Thermal decomposition of a mixed valence copper complex has been studied upto 1,000◦C in flowing air by simultaneous thermogravimetric and differential thermalanalysis coupled on-line with quadrupole mass spectrometer (TG/DTA-MS) and FTIRspectrometric gas cell (TG-FTIR) in comparison. The release of some of the includedammonia to 170◦C, then simultaneously ammonia (NH3) and sulfur dioxide (SO2) from175 to 225◦C were detected, and the evolution of SO2 from thiosulfate ligands continuedin several overlapping stages until 410◦C and it is escorted by explicit exothermic heateffects at around 237, 260, 358, and 410◦C (249). A detailed study on identification andthermal decomposition of the Pd(NH3)2(NO2)2 and trans-Pt(NH3)2(NO2)2 was reportedby Madarasz et al. (250). The unified evolved gas analyses reported evolution of N2,H2O, NH3, N2O, NO, and NO2 gases as gaseous product components in the exothermicdecomposition of both trans- starting from ca. 230 and 220◦C, in sealed crucibles with apinhole on the top (250). Stycze and coworkers (251) reported the thermal decomposition ofcompounds consisting of tetrahalogenomanganese(II) anions, (MnBrnCl4-n)2− (n = 0–4),and a tetrabutylammonium cation. The initiation of decomposition of several energetic ionicliquids (EILs) was studied by confined rapid thermolysis. Rapid-scan FTIR spectroscopyand time-of-flight mass spectrometry were utilized to identify the products evolved fromsub-milligram quantities subjected to heating rates of about 2000 K/s (252). Ayszczek (253)proposed the thermal investigation and infrared evolved gas analysis of light lanthanide(III)complexes with pyridine-3,5-dicarboxylic acid.

Other Applications

Hexaglycidyl cyclotriphosphazene (HGCP), a reactive flame retardant, was synthesizedand characterized by El Gouri and coworkers (254). The gases evolved in an air flow werestudied by means of TG-FTIR to test the improvement of the thermal stability at elevatedtemperature with higher char yields.



Molecular distillation was used to separate bio-oil into a light fraction, a middlefraction, and a heavy fraction. The pyrolysis characteristics of the bio-oil fractions weredetermined by TG-FTIR, and the weight loss of components was in agreement with thechemical composition (255). Orange peel degradation was studied by Zapata et al. (256)The volatiles compounds and the gas products were mainly CO2, CO, CH4, together witha mixture of acids, aldehydes, or ketones. The results could explain the nonautocatalyticcharacter of the reactions during the decomposition process.

Comparative data about the products of pyrolysis of biomasses that are potentiallyavailable at economic bases for the production of biofuels are important, and agriculturalresidues such as coconut shell, sugarcane bagasse, corn stalks, and peanut shell were chosento be investigated. TG-FTIR indicated tendencies in the rate of the formation of importantspecies during the pyrolysis process of the four biomasses studied. The interpretation ofthe spectra allowed the proposition of characteristic absorbance ratios and the comparisonof these values allowed inferences about the relative abundances of components formed inthe pyrolysis of the biomasses (257). Giuntoli and coworkers characterized two differentsecondary fuels: dry distiller’s grains with solubles (DDGS) and chicken manure. Thesematerials have high content of nitrogen and ashes, which limits their usage in thermalapplications due to potential excessive NOx emissions and problems of slagging, fouling,corrosion, and loss of fluidization. The fuels tested here were received from industrialpartners. In order to reduce the ash content, the fuels were pretreated using a water-leaching pretreatment. Pyrolysis of these fuels has been monitored through a TG-FTIRsetup. Quantification of the following volatile species was possible: CO, CO2, CH4, HCN,NH3, HNCO, H2O (258).

Cotton stalk, a representative agricultural biomass in China, mixed with municipalsolid waste (MSW) with high ash content and low calorific value, was analyzed. Pyrolysischaracteristics and pollutant emission performance from MSW and stalk blends at differentmass proportions were studied (259).

Switchgrass is a high-yielding perennial grass that has been designated as a potentialenergy crop (thermochemical conversion to syngas). It is required that the rate of thermal de-composition of switchgrass and the rate of production of components of the syngas be quan-tified. FTIR analysis showed that the following gases were given off during the pyrolysisof switchgrass: carbon dioxide, carbon monoxide, acetic acid, ethanol, and methane (260).

O2/CO2 coal combustion technology is considered as one of the most promising tech-nologies for CO2 sequestration due to its economical advantages and technical feasibility.It is significant to study the sulfur transfer behavior of coal in O2/CO2 atmosphere fororganizing combustion properly and controlling SO2 emission effectively. To clarify theeffect of atmosphere on the sulfur transfer behavior, a TG-FTIR system was employed tostudy the formation behaviour of sulfur-containing gas species from coal pyrolysis in CO2

atmosphere compared with that in N2 atmosphere (261–264). The application of the TG-FTIR analysis to coal pyrolysis demonstrated that adding H2 into the pyrolysis atmosphereincreases the contents of phenolic and carboxylic compounds in the produced pyrolysis oil,and it promotes as well the cracking of aliphatic hydrocarbons during pyrolysis. AddingCH4 causes more aliphatic hydrocarbons, single aromatic ring chemicals, and phenoliccompounds in the pyrolysis oil (265).

The gaseous products evolving from pyrolysis of pesticide residue were investigated byLi et al. (266). The results showed that SO2 is the main gaseous product in the temperaturerange 300–600◦C, accompanied by a small amount of other gases such as CO2 and H2O,and CO emitted at high temperature during pyrolysis (266).



Commercial light-cured dental composites were compared under cured and uncuredconditions. Dental composite evaluation suggested a high thermal stability and inorganiccontent in an RES D sample (267).

Three native asphalt samples (from a Roman quarry in central Italy, from a Romanship sunk south of France, from the eye of a Thracian bronze head) were characterizedby several techniques included TG-FTIR analysis to support archaeological investigationsreconstructing their thermal history and composition (268).

Marcilla et al. (269) proposed a singular characterization of microalgal species (Nan-nochloropsis sp.) through TGA/FTIR analysis (269).

Pyrolysis behavior and pyrolysis products (liquid products with a high boiling point)of scrap printed circuit boards were investigated using a TG-FTIR analysis system. Themain component of liquid products was aromatic compounds with substituted functionalgroup (270).

Solid waste from dyestuff production, classified as “hazardous waste,” was studied byJiang et al. (271) in an inert atmosphere using thermogravimetric analysis coupled withFourier transform infrared spectroscopy. A total weight loss of 35.1 wt% was observed,and the temperature trend of evolving gaseous products, such as CO2, CO, H2O, HCN,and SO2, was investigated. Girods et al. (272) proposed a comparison of gasification andpyrolysis of thermal pretreated wood board waste.

The complex reactions of typical medical waste materials pyrolysis and the evolutionof different volatile species has been monitored by TG-FTIR and predicted by a distributedactivation energy model (DAEM) (273).

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https://www.researchgate.net/publication/239395528_Mass_Spectrometry_Coupled_to_Thermogravimetry_TG-MS_for_Evolved_Gas_Characterization_A_Review?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

https://www.researchgate.net/publication/253235372_Effect_of_Red_Phosphorus_and_Melamine_Polyphosphate_on_the_Fire_Behavior_of_HIPS?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

https://www.researchgate.net/publication/253235372_Effect_of_Red_Phosphorus_and_Melamine_Polyphosphate_on_the_Fire_Behavior_of_HIPS?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

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https://www.researchgate.net/publication/244358118_TGAFTIR_study_of_the_evolution_of_the_gases_evolved_in_the_catalytic_pyrolysis_of_ethylene-vinyl_acetate_copolymers_Comparison_among_different_catalysts?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==



https://www.researchgate.net/publication/239395526_Thermogravimetry_-_Infrared_Spectroscopy_TG-FTIR_Coupled_Analysis?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

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https://www.researchgate.net/publication/223426725_Pielichowski_K_Fiejtuch_K_Non-oxidative_thermal_degradation_of_polyethylene_oxide_kinetic_and_thermoanalytical_study_J_Anal_Appl_Pyrolysis_73_131-138?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

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https://www.researchgate.net/publication/226424538_Multi-instrumental_analysis_of_asphalts_of_archaeological_interest?el=1_x_8&enrichId=rgreq-44388c4ebc05ba6811f9f802fe5e8ac0-XXX&enrichSource=Y292ZXJQYWdlOzI0NTMyODg2MDtBUzoxNTI0NTkwNDk3MDU0NzJAMTQxMzM2MDQ3ODMxMw==

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