Mit der Entwicklung und Einführung ökologischer Bauweise im Neubau sowie neuen Baustoffsystemen in Sandwichbauweise wird es zunehmend erforderlich, neue effektive Befestigungsvarianten zu entwickeln, die eine dauerhafte Fixierung auch unter sicherheitstechnischen Bestimmungen sowie aus Garantie- bzw. haftungsrechtlichen Gründen ermöglichen. Die aus der Praxis bisher bekannten chemischen Befestigungssysteme (Zweikomponentenverbundmörtel, Verbundankerpatronen) weisen hinsichtlich der Applikation unter bautechnischen Bedingungen noch einige Nachteile auf. Dazu gehören vor allem längere Aushärtungszeiten zur Realisierung der abschließenden Verbundfestigkeit, Inhomogenitäten im Verbund, der Einsatz toxischer Verbindungen und eine Limitierung der Applikationsmöglichkeiten in horizontalen und Überkopf-Einsatzbereichen sowie Hohlkammersystemen. Alle zuvor genannten Punkte haben bis jetzt die Nutzung solcher Verbundwerkstoffe als universale Anwendungsmöglichkeit verhindert. Ein neues chemisches Befestigungssystem, welches aus Novolak gehärteten mit Hexamethylentetramin (Hexa) und anorganischen Füllstoff besteht, wurde für Applikationen in Beton entwickelt. Das Bindemittel härtet bei der Temperaturzuführung aus. Die unkatalysierte Befestigungsmasse zeigt bei einer Temperatur zwischen 150-300 °C eine hohe Reaktivität. Die Vorteile dieses Systems sind die unbegrenzte Lagerfähigkeit der vorgemischten härtbaren Masse sowie die Gewährleistung einer homogenen Netzwerkstruktur im gesamten Verbund und sie ist frei von giftigen und flüchtigen Substanzen. Auf den Einsatz toxischer Substanzen wurde verzichtet. In dieser Arbeit wurde die Gesamtkinetik der Reaktion während des Aushärtungsprozesses dieser Polymerkomposite untersucht. Die DSC- (nicht-isothermen, isothermen) und MDSC-Untersuchungen haben sich als ein sicheres Verfahren zur Qualitätskontrolle des Aushärtezustands der Befestigungssysteme herausgestellt. Parallel zur nicht-isothermischen und isothermischen DSC wurden Leitfähigkeitsmessungen durchgeführt, um den Endpunkt der Aushärtungsreaktion zu bestimmen. / The development and introduction of ecological construction methods and the use of sandwich materials make it necessary to develop new fixing systems and technologies. Dealing with the application in concrete and other substrates commercial chemical fixing systems show some disadvantages up to date. Especially the rather long curing time in order to realize the final bond strength, inhomogenities in the composite, the partial use of toxic substances and application limits of such systems in horizontal direction as well as hollow section materials has so far prevented the use of such composites for all-purpose applications. A new chemical fixing system, which consists of hexamethylene tetramine (hexa) cured novolac and inorganic filler, was developed for application in concrete. It is applied by a thermo-curing procedure. The uncatalyzed curable mixture has a high reactivity at temperature between 150-300 °C. Compared with commercial chemical fixing systems, the premixed curable mass has many benefits. First it has a unique storage stability and second, it is free of toxic and volatile substances. Another important aspect is, it is self-foaming. In this study was investigated the overall kinetics of the reaction during the curing process of these polymer composites. An appropriate method for this experiment proved to be the DSC in isothermal and non-isothermal mode and MDSC. This turned out to be a safe quality control technique for these systems. Parallel to the non-isothermal and isothermal DSC conductivity measurements have been performed to determine the end point of the curing reaction.

Over the last years, varieties of technologies for biofilm analysis were developed and established. They work on different principles and deliver information about biofilms on different information levels. In this work, chip-calorimetry was applied as an analytical tool that measures heat produced from biofilms. Any change of metabolism in biofilms is reflected by a changed heat flow. The heat, which is the integral of the heat flow vs. time, is quantitatively related to the growth stoichiometry of the biofilm, as described by the Hess’ Law. The heat flow is related to the growth kinetics with the reaction heat as proportionality factor. The results from the calorimetric measurement thus, deliver general information about growth stoichiometry and kinetics. The other interpretation of calorimetric results bases on the assumed proportionality between heat flow and oxygen consumption rate (- 460 kJ/mol ). This ratio is called oxycaloric equivalent. Because in case of aerobic growth the majority of oxygen is consumed in catabolic processes during the electron transport phosphorylation, calorimetry is assumed to provide information about the catabolic side of the metabolism. The newly developed chip-calorimeter applied in this work is much more suitable for biofilm studies compared to conventional microcalorimeters due to the flow-through design of the calorimetric chamber. The measurement of undisturbed growing biofilms and the comparison with conventional biofilm analysis tools (i.e. plate counts, confocal laser scanning microscopy (CLSM), and the determination of intermediates’ concentrations (e.g. ATP)) demonstrate the proper functionality of the calorimetric method and the related cultivation procedure by delivering measurement results in the range of literature values. However, when the biofilms were challenged with antimicrobial agents i.e. antibiotics, bacteriophage, and predatory bacteria, the calorimetric results surprisingly deviated from the reference analyses. By combining the results of the calorimetric and reference analyses, additional information about the antimicrobial effects on biofilms can be acquired. Combination of heat measurement and plate counts, which is one of the most conventional approaches, demonstrated that antimicrobials (especially the bactericidal acting kanamycin) could cause the loss of culturability while the cells were still metabolically active. The measurement of ATP content resulted in values out of the typical range, which indicated that antimicrobial treatments disturbed the cellular ATP regulation and the ATP concentration was no longer linearly correlated to the cell number. ATP measurements are therefore not suitable for antimicrobial susceptibility testing. The comparison of heat profiles with the biovolume determined by quantification of microscopic images shows an elevated cell specific heat production rate after the introduction of some antimicrobials (antibiotics and bacteriophage). In case of antibiotics, this can be explained as a consequence of the bacterial defense mechanisms. Most of the described defense mechanisms against antibiotics need biological energy and therefore drive the electron transport phosphorylation (ETP). In case of biofilm treatments with bacteriophage, the trigger of increasing ETP might be the synthesis of phage proteins, hull material, and genetic information molecules. In aerobic conditions, oxygen is used as terminal electron acceptor. Elevated ETP leads therefore to an increase in oxygen consumption, which correlates to the heat production using oxycaloric equivalent as a factor. These correlations explain the increase of cell specific heat productions as biofilms were challenged by antibiotics and bacteriophage. However, also a decrease of specific heat production was observed (in case of predatory bacteria). Here, the predatory bacteria activity caused various damages in host cells, including the interruption of ETP. With these experiments, chip-calorimetry was demonstrated as a promising complementary tool in biofilm research, which provides deeper insights about metabolic activity and alterations. It benefits from the noninvasive handling and the online, real-time measurement that allow the method to be applied for monitoring purposes. Furthermore, its miniaturized dimension allows easy integration in more complex analytic systems and also reduces experiment costs with minimal media/chemical consumption. This thesis also demonstrates the potential development of chip-calorimetry to be more suitable for routine analyses. The use of superparamagnetic beads as matrix to grow biofilms allows regulated transfer of biofilm samples into and from the measurement chamber. This was an initial step towards automation and higher-throughput analysis. One further outcome of the thesis is based on the highly interesting fact about the elevated heat production rate of the host cells induced by the phage infection observed in the chip- calorimetric experiments. The volume specific detection limit of the chip-calorimeter is lower compared to a commercial microcalorimeter. Thus, the infection effect of phages was additionally measured in microcalorimeter to get better quantitative information about the thermal effect of the infection. The results showed that the immediate heat increase after the addition of phage into the solution of the host cells appeared to be quantitatively related to the infection factor, MOI (Multiplicity of Infection). Unfortunately, microcalorimetric measurements in closed ampoules are often subjected to the oxygen limitation. Thus, this problem of microcalorimetric measurement has been addressed. The combination of experimental results and mathematical modeling showed that the rate of metabolism in the static ampoules is defined by the diffusion rate of oxygen into media. This factor has to be considered while designing biological experiments in closed calorimetric measuring chambers and interpreting the calorimetric results for their biological meaning. Some possible solutions to overcome the oxygen bioavailability problem are e.g. to design the experiments with low biomass, or by using media with elevated density to float the biomass at the interface to air and thus to reduce the diffusion path.

Bakgrunden till detta examensarbete var att Qumex Materialteknik vid ett flertal tillfällen konstaterat att material av typen SS 0725 har uppvisat bristfälliga härdresultat. Materialet, som är relativt nytt på marknaden, är ett gjutjärn av typen segjärn och utmärker sig gentemot andra segjärn på grund av sitt höga innehåll av kisel. Då segjärn enligt den nu gällande EN-standarden klassificeras efter sina mekaniska egenskaper uppstår ett problem gällande SS 0725. Materialet uppfyller de krav som är ställda för EN-GJS-500-7 och hamnar därmed under samma materialbeteckning som ett segjärn med betydligt lägre kiselhalt. Att två material med olika kemisk sammansättning hamnar under samma beteckning kan innebära problem. Syftet med denna rapport är att fastslå vilken påverkan den höga kiselhalten har på materialet vid värmebehandling av typen släckhärdning med efterföljande anlöpning. I försöken ingick fyra material. Det som skiljde materialen åt var halterna av koppar och kisel. De härdades vid tre olika temperaturer och under tre olika tider för att sedan släckas i olja. Målet med släckhärdningen var att materialen skulle få en helt martensitisk struktur vilket då klassades som ett bra härdresultat. Resultatet utvärderades sedan genom optisk mikroskopi och hårdhetsmätningar. En undersökning av materialens fasomvandlingstemperaturer genomfördes med hjälp av Differential Scanning Calorimetry. Resultatet visar att kiselhalten har stor påverkan på den temperatur som krävs för att erhålla ett bra härdresultat. För material med låg kiselhalt uppnåddes fullständig martensitbildning efter släckhärdning från 840°C. För material med hög kiselhalt uppnåddes liknande strukturella och hårdhetsmässiga resultat först vid en så hög temperatur som 900°C och behandlingstider längre än 1 h. Den relativa skillnad som uppmättes i fasomvandlingstemperatur med hjälp av Differential Scanning Calorimetry mellan högkiselmaterial och lågkiselmaterial var 45°C. Detta resultat kombinerat med analyserna av härdprocesserna visar att det krävs kraftigt ökad temperatur vid värmebehandling av högkiselmaterialet SS 0725. / The background to this thesis was that Qumex Materialteknik at several occasions had received material of type SS 0725 that had shown deficient heat treatment results. The material, which is relatively new, is a cast iron of type ductile iron and differ against other ductile irons because of its high silicon content. According to EN standard ductile irons are classified by their mechanical properties. A problem then occurs with the new material SS 0725 because of this. The material fulfils the requirements for EN-GJS-500-7 and is therefore in the same classification as a ductile iron with much lower silicon content. Two materials having major differences in chemical composition ending up in the same classification can be problematic. The purpose of this report is to determine impact of high silicon content in ductile iron when heat treated and quench hardened. The experiment included four materials, and the major difference between the materials were their content of copper and silicon. The heat treatment process was performed at three different temperatures and three different treatment times. Afterwards the samples were quenched in oil. The ambition of the quench hardening was to obtain a material structure of 100% martensite. By optical microscopy and hardness measurements the results then were evaluated. An investigation of the phase transformation temperature in the materials was made by using Differential Scanning Calorimetry. The results show that the amount of silicon content has great influence on the temperature for receiving good hardening results. To achieve 100% martensite after quench hardening in materials with low silicon content the temperature needs to be over 840°C. For material with high level of silicon content the temperature for achieving 100% martensite needs to be 900°C and the treatment time should be over 1 h. The relative difference in phase transformation temperature was measured using Differential Scanning Calorimetry. The results of the measurements between the materials with high silicon content and materials with low silicon content was 45°C. This result combined with the analysis of the heat treatment process shows that a major increase of the temperature is needed to heat treat SS 0725.

Eine kalorimetrische Kristallisationsuntersuchung unter dynamischer Abkühlung ist bisher noch nicht erfolgt, auch weil die klassischen DSC-Messsysteme hierfür thermisch zu träge sind und die Einschwingzeiten zu lang sind. Durch die Weiterentwicklung der Prüftechnik, insbesondere auf dem Gebiet der Hochgeschwindigkeitskalorimetrie, erscheint es jedoch erstmals möglich, das dynamische Abkühlverhalten prozessnah nachbilden zu können und die Auswirkung auf die Kristallisation zu untersuchen. Im Rahmen dieser Arbeit wurde daher versucht die dynamische Abkühlung einer Kunststoffschmelze aus PBT kalorimetrisch in Abhängigkeit der Werkzeugtemperatur und der Bauteilgeometrie nachzubilden, jeweils bei Betrachtung verschiedener Bauteiltiefen. Hierfür wurden numerisch nichtlineare Kühlratenverläufe bestimmt, die im Anschluss durch Segmentierung linearisiert und somit in ein FSC-Programm überführt werden konnten. Anhand der resultierenden Wärmestromverläufe konnte gezeigt werden, dass eine Interpretation der kalorimetrischen Erfassung unter dynamischer Abkühlung möglich ist und der Verlauf der Kristallisation in verschiedenen Bauteiltiefen in Abhängigkeit der weiteren Randbedingungen nachvollzogen werden kann. / A calorimetric investigation of the crystallization of thermoplastics under dynamic cooling has not performed yet, also because the classical DSC measuring systems are thermally too slow for this purpose and the corresponding settling times are too long. However, as a result of the further development of testing technology, especially in the field of high-speed calorimetry, it seems possible to simulate the dynamic cooling behavior of real processing and to investigate its effects on crystallization. In this work the dynamic cooling of a polymer melt was simulated calorimetrically depending on the tool temperature and the part geometry, in each case considering the different cooling behavior of different part depths. Therefore, numerically nonlinear cooling rate profiles were determined, which could then be linearized by segmentation and thus converted into a calorimetric program. On the basis of the resulting heat flow characteristics it could be shown that an interpretation of the calorimetric detection under dynamic cooling is possible and the course of the crystallization in different part depths can be reconstructed in dependence on the further boundary conditions.

<p>Virtually all biologically relevant functions and processes are mediated by non-covalent, molecular recognition events, demonstrating astonishingly diverse affinities and specificities. Despite extensive research, the origin of affinity and specificity in aqueous solution - specifically the relationship between ligand binding thermodynamics and structure - remains remarkably obscure and is further complicated in the context of multivalent interactions. Multivalency describes the combinatorial interaction of multiple discrete epitopes across multiple binding surfaces where the association is considered as the sum of contributions from each epitope and the consequences of multivalent ligand assembly. Gaining the insight necessary to predictably influence biological processes with novel therapeutics begins with an understanding of the molecular basis of solution-phase interactions, and the thermodynamic parameters that follow from those interactions. Here we continue our efforts to understand the basis of aqueous affinity and the nature of multivalent additivity.</p><p>Multivalent additivity is the foundation of fragment-based drug discovery, where small, low affinity ligands are covalently assembled into a single high affinity inhibitor. Such systems are ideally suited for investigating the thermodynamic consequences of multivalent ligand assembly. In the first part of this work, we report the design and synthesis of a fragment-based ligand series for the Grb2-SH2 protein and thermodynamic evaluation of the low affinity ligand fragments compared to the intact, high affinity inhibitor by single and double displacement isothermal titration calorimetry (ITC). Interestingly, our investigations reveal positively cooperative multivalent additivity - a binding free energy of the full ligand greater than the sum of its constituent fragments - that is largely enthalpic in origin. These results contradict the most common theory of multivalent affinity enhancement arising from a "savings" in translational and rotational entropy. The Grb2-SH2 system reported here is the third distinct molecular system in which we have observed enthalpically driven multivalent enhancement of affinity.</p><p>Previous research by our group into similar multivalent affinity enhancements in protein-carbohydrate systems - the so-called "cluster glycoside effect" - revealed that evaluation of multivalent interactions in the solution-phase is not straightforward due to the accessibility of two disparate binding motifs: intramolecular, chelate-type binding and intermolecular, aggregative binding. Although a number of powerful techniques for evaluation of solution-phase multivalent interactions have been reported, these bulk techniques are often unable to differentiate between binding modes, obscuring thermodynamic interpretation. In the second part of this work, we report a competitive equilibrium approach to Molecular Recognition Force Microscopy (MRFM) for evaluation of ligand binding at the single-molecule level with potential to preclude aggregative associations. We have optimized surface functionalization strategies and MRFM experimental protocols to evaluate the binding constant of surface- and tip-immobilized single stranded DNA epitopes. Surprisingly, the monovalent affinity of an immobilized species is in remarkable agreement with the solution-phase affinity, suggesting the competitive equilibrium MRFM approach presents a unique opportunity to investigate the nature of multivalent additivity at the single molecule level.</p> / Dissertation

Organic emissions with focus on terpenes, from biomass drying and storage were investigated by Solid Phase Microextraction (SPME) and GC-FID and GC-MS. The remaining terpenes in the biomass (Spruce and pine wood chips) after drying were dependant on the drying temperature and drying medium used. The drying medium used was steam or hot air; the drying temperatures used were 140degreeC, 170degreeC and 200degreeC. Steam drying at 170degreeC left more of the terpenes remaining in the wood chips, not emitting them into the drying medium. The terpenes emitted from storage of forest residues and bark and wood chips increased up to three-four or four-five months of storage, and then dropped down to approximately the same low level as the first month. The leachate taken from the forest residue pile contained 27µg PAH per liter. The SPME response for a monoterpene (a-terpene) at different temperatures, amounts and humidities was quantified. The highest concentration calibrated was 250 ppm and the lowest 9.4 ppm. There is a better linear agreement at higher temperatures (70degreeC and 100degreeC) than lower temperatures (below 40degreeC). Organic emissions from biofuel combustion were measured at three medium sized (~ 1MW) biomass fired moving grate boilers fired with different fuels: dry wood fuel, forest residues and pellets. The PAH emissions varied by almost three orders of magnitude between the three boilers tested, 2.8-2500 microgram/m3. It was difficult to identify any general parameters correlating to the PAH emissions. The variation in PAH emission is most probably a result of boiler design and tuning of the combustion conditions. When comparing the contribution to self-heating from different wood materials by means of isothermal calorimetry with different metals added and stored at different temperatures, the differences were quite large. Some of the samples released as much as 600mW/kg, whereas others did not contribute at all to the self-heating. The storage temperature, at which the samples released the most heat, was 50C. There was a peak in heat release for most of the samples after 10-30 days. Stepwise increase in temperature did not favour the heat release in the sample Dry Mix; the heat released was even lower than when it was directly put in the different storage temperatures. When metal is added, there is an increase in heat release, the reference sample without metal released 200mW/kg compared to 600mW when copper was added.

Thesis (PhD)--Stellenbosch University, 2013. / ENGLISH ABSTRACT: The first part of this study describes the synthesis of new porous materials from basic building blocks. Five structurally related ligands namely: N,N'-bis(3-pyridylmethyl)-naphthalene diimide (L1), N,N'-bis(4-pyridylmethyl)-naphthalene diimide (L2), N,N'-bis(4-pyridylmethyl)- pyromellitic diimide (L3), N,N'-bis(3-pyridylmethyl)-pyromellitic diimide (L4) and 2-(pyridin-4- ylmethyl)-benzene tricarboxylic anhydride (L5) were synthesised. Ligands L1 and L2 were reacted with metal nitrates and carboxylates as co-ligands in a systematic manner with a view to obtaining potentially porous 3–D coordination polymers. Ten structurally diverse coordination polymers were obtained and they were characterised by single-crystal X-ray diffraction, powder X-ray diffraction and thermogravimetric analysis. Four of these compounds absorb moderate amounts of CO2 and, in addition, show sorption selectivity towards CO2 over N2. The reaction of L3 and L4 with transition metal halides yielded two 1–D chains, while the reaction of L5 with transition metal nitrates yielded seven coordination polymers of which four are 2–D and three are 1–D. Of the 2–D structures three are isostructural. The second part of this work describes a variable pressure study of a flexible metal-organic framework [Zn2(BDC)2(BPY)] (BPY = 4,4 -bipyridine and BDC = 1,4-benzene dicarboxylic acid). [Zn2(BDC)2(BPY)] is one of the few examples of a flexible metal-organic framework that undergoes phase transformations in response to gas pressure. The high pressure sorption recorded for this metal-organic framework displays two inflection steps in the pressure range 0 to 30 bar, possibly indicating two phase transformations. The gas-loaded structures for each phase transformation were determined by means of single-crystal X-ray diffraction. High-pressure differential scanning calorimetry was also carried out on the system in order to determine accurate gate-opening pressures, as well as the energies involved with each phase transformation. The results correlate with those obtained from single-crystal X-ray diffraction and high-pressure sorption. The final section reports the mechanochemical synthesis of two Werner complexes [NiCl2(4- PhPy)4] (1), [CoCl2(4-PhPy)4] (2) and their corresponding solid solution [Ni0.5Co0.5Cl2(4-PhPy)4] (3) (PhPy = phenyl pyridine). The solid solution could only be formed by mechanochemical synthesis and not by conventional solution crystallisation methods. The solid solution exhibits sorption properties that differ from those of the pure compounds. / AFRIKAANSE OPSOMMING: Die eerste deel van hierdie studie beskryf die sintese van nuwe poreuse stowwe uit basiese boublokke. Vyf struktureel verwante ligande naamlik: N,N'-bis(3-piridielmetiel)-naftaleen diimied (L1), N,N'-bis(4-piridielmetiel)-naftaleen diimied (L2), N,N'-bis(4-piridielmetiel)- piromellitien diimied (L3), N,N'-bis(3-piridielmetiel)-piromellitien diimied (L4) en 2-(piridiel-4- ielmetiel)benseen trianhidried (L5) is gesintetiseer. Ligande L1 en L2 is gereageer met metaal nitrate en karboksielsure as mede-ligande in 'n sistematiese wyse met 'n oog op die verkryging van potensieel poreuse 3–D koördinasie polimere. Tien struktureel diverse koördinasie polimere is verkry en hulle is gekarakteriseer deur enkel-kristal X-straal-diffraksie, poeier X-straal diffraksie en termo-analise (thermal analysis). Vier van hierdie verbindings het matige hoeveelhede CO2 geabsorbeer en, bykomend, wys sorpsie selektiwiteit van CO2 oor N2. Die reaksie van L3 en L4 met oorgangsmetaalhaliede het twee 1–D kettings gevorm, terwyl die reaksie van L5 met oorgangsmetaal nitrate sewe koördinasie polimere opgelewer het, waarvan vier 2–D en drie 1–D polimere is. Van die 2–D polimere het drie vergelykbare strukture. Die tweede deel van hierdie werk beskryf 'n veranderlike druk studie van 'n buigsame metaalorganiese raamwerk [Zn2(BDC)2(BPY)] (BPY = 4,4-bipiridien en BDC = 1,4-benseen dikarboksielsuur). [Zn2(BDC)2(BPY)] is een van die min voorbeelde van 'n buigsame metaalorganiese raamwerk wat fase transformasies (phase transformations) ondergaan in respons op ‘n verandering in gas druk. Die hoë-druk sorpsie aangeteken vir hierdie metaal-organiese raamwerk vertoon twee infleksie stappe in die gebestudeerde druk gebied (0 tot 30 bar), wat moontlik op twee fase transformasies dui. Die gas-gelaaide strukture vir elke fase transformasie is bepaal deur middel van enkel-kristal X-straal-diffraksie. Hoë-druk differensiële skandeer kalorimetrie (differential scanning calorimetry) is ook uitgevoer op die stelsel ten einde dié akkurate hekopenings druk, sowel as die energie betrokke by elke fase transformasie te bepaal. Die resultate stem ooreen met dié verkry vanaf enkel-kristal X-straal diffraksie en hoë-druk sorpsie. Die finale afdeling bespreek die meganochemiese sintese van twee Werner komplekse [NiCl2(4-PhPy)4] (1) en [COCl2(4-PhPy)4] (2) en hul ooreenstemmende vaste oplossing (solid solution) [Ni0.5Co0.5Cl2(4-PhPy)4] (3). Die vaste oplossing kan slegs gevorm word deur meganochemiese sintese en nie deur konvensionele oplossing kristallisasie metodes. Die vaste oplossing vertoon sorpsie eienskappe wat verskil van dié van die suiwer verbindings.

Studies on strongly correlated electron systems over decades have allowed physicists to discover unusual properties such as spin density waves, ferromagnetic and antiferromagnetic states with unusual ordering of spins and orbitals, and Mott insulating states, to name a few. In this thesis, the focus will be on the specific heat property of these materials exhibiting novel electronic ground states in the presence and absence of a field. The purpose of these measurements is to characterize the phase transitions into these states and the low energy excitations in these states. From measurements at the phase transitions, one can learn about the amount of order involved [i.e. entropy: ΔS = ∫Δc p/T dT], while measurements at low temperatures illuminate the excitation spectrum. In order to study the thermodynamic properties of the materials at their phase transitions, a high sensitive technique, ac-calorimetry was used. The ac-calorimeter, workhorse of our low dimensional materials lab, is based on modulating the power that heats the sample and measuring the temperature oscillations of the sample around its mean value. The in-house ac-calorimetry set up in our lab has the capability to produce a quasi-continuous readout of heat capacity as a function of temperature. A variety of single crystals were investigated using this technique and a few among them are discussed in my thesis. Since many of the crystals that are studied by our group are magnetically active, it becomes useful for us to also study them in the presence of a moderate to high magnetic field. This motivated me to design, develop, and build a heat capacity probe that would enable us to study the crystals in the presence of non-zero magnetic fields and at low temperatures. The probe helped us not only to revisit some of the studied materials and to draw firm conclusions on the previous results but also is vital in exploring the untouched territory of novel materials at high magnetic fields (~ 14 T).

LHCb est l'une des quatre grandes expériences installées sur l'anneau du LHC. Le détecteur a pour but la mesure précise de la violation de CP et de canaux rares de désintégration dans le secteur des mésons B. Le calorimètre de l'expérience est un ensemble de quatre sous-systèmes : le détecteur de pied de gerbe, le ''preshower'' et les calorimètres électromagnétique (ECAL) et hadronique (HCAL). Il est essentiel pour la reconstruction des événements, pour le déclenchement de l'expérience et pour l'identification des électrons et des photons. Après une revue du détecteur LHCb, l'électronique des calorimètres est décrite dans la première partie de ce mémoire. Dans un premier temps l'électronique de lecture des voies des photomultiplicateurs des ECAL et HCAL est présentée en mettant l'accent sur ses performances, puis la carte de contrôle de l'ensemble du système calorimétrique de l'expérience est détaillée. Les chapitres trois et quatre concernent les programmes de test de cette électronique, les choix technologiques permettant de la rendre suffisamment tolérante aux radiations et les mesures quantifiant cette tolérance. La seconde partie de ce mémoire porte d'abord sur l'identification des photons avec les calorimètres de LHCb. La méthode est présentée avec ses performances. Enfin, l'étalonnage absolu en énergie des PRS et ECAL, basée sur les données enregistrées avec le détecteur en 2010, est décrite dans le dernier chapitre de cette même seconde partie.

No description available.