Total joint arthroplasty surgeries are known to have a high success rate but the longevity of the implants still acts as a limiting factor. Ultrahigh molecular weight polyethylene is the material of choice for the implant bearing surfaces due to its excellent clinical and tribological performance. A common problem associated with the polymer is however the loosening of the implant from its surrounding bone tissue. This phenomenon is caused by a biological reaction to released wear particles. Reducing the release of wear particles will increase the lifespan of implants and can be accomplished by increasing the wear resistance of the material. Crosslinking of the polymer by means of gamma irradiation is a well known approach to achieve an increased wear resistance but eventually leads to oxidation of the polymer. The addition of vitamin E as antioxidant is known to reduce this without significant loss of mechanical properties. A second approach is based on adding reinforcements to the polymer in order to enhance its tribological performance. This work focuses on the thermal and mechanical characterisation of newly developed UHMWPE nano-composites with a focus on the addition of vitamin E and crosslinking by gamma irradiation. Based on previously published results indicating an increased fracture toughness for different composites, Nanodiamonds, multiwalled carbon nanotubes and graphene oxide nanoparticles were dispersed throughout the matrix and consolidated. The thermal characterisation was performed using differential scanning calorimetry, making it possible to identify the different thermal transitions and degree of crystallinity of the polymer. The fracture toughness, an important property in wear due to fatigue, was furthermore characterised by performing three point bending experiments.Finally, by means of a multiaxial pin-on-plate set-up the wear resistance of the materials was analysed.

I följande rapport behandlas ämnet förnyelsebar energi i samband med textila material. I resultatet ges förslag till möjliga tillvägagångssätt för integrering av flexibla solceller i väv- och varptrikå. Alternativ till maskintillverkare och maskintyper redovisas och potentiella användningsområden diskuteras. Även förlag på typ av flexibel solcell presenteras. Teorin vilket rapporten grundar sig på är humanekologisk. Den metod vilken följts är tolkande och har drivit arbetet framåt. Kunskap har hämtats från experter inom områdena textil och solcellsteknik. Arbetsprocessen har varit av teoretisk karaktär vilket uteslutit eventuella laborationer. Slutsatsen visar att dye solar cells (DSC) kan användas med fördel, på grund av dess flexibla egenskap. De maskiner vilka kan tillverka solcellstextil är i standardutförande, dock kan eventuella justeringar på maskinkomponenter vara nödvändiga. Då främst vad gäller nålavstånd, täthet i sked och solv. Engelsk titel: Flexible solar cells in a textile material - Alternatives for integration of renewable energy in weave and warp knittingEngelska nyckelord: Weave, Warp knit, Solar cell textile, Technical textile, Flexible solar cells, DSC / Program: Textil produktutveckling och entreprenörskap

The surface and structural change of human hair fibre have been analysed to determine the oxidation effects for bleached hairs. Three types of bleached hairs (6% H2O2 bleach, 9% H2O2 commercial bleach and commercial persulphate bleach (contains 9% H2O2)) as well as virgin hair were evaluated with the increasing treatment time using Scanning Electron Microscopy (SEM), Reflective Spectrophotometry, Differential Scanning Calorimetry (DSC) and Fourier Transform Infrared (FTIR) Spectroscopy. It is obvious that longer treatment times result in the greater surface and structural damage. However, commercial persulphate bleach causes less surface damage for the cuticle. 6% H202 bleach has overall moderate damage effects on both cuticle and cortex over the treatment time. 9% H2O2 commercial bleach indicates two different damage stages. The first 1.5h bleached hairs show mild oxidation to the surface, whereas the damage becomes heavy after 2h. This phenomenon results in that 9% H2O2 commercial bleach has a more intensive oxidation damage in the cortex than the commercial persulphate bleach. This is in line with DSC investigation which shows that the intermediate filament of 9% H2O2 commercial bleach is heavily damaged after the extensive oxidation time (greater than or equal to2h). Although commercial persulphate bleach contains the stronger oxidising agent, it has a less surface damage than 9% H2O2 commercial bleached hair in FTIR-ATR measurement, and a similar oxidation effect on the matrix as 6% H202 bleached hair in FTIR transmission investigation. In addition, it has been verified by colour measurements that bleached hairs have an overall lighter, yellowish and reddish colour. Consequently, commercial persulphate bleached hair is much lighter and more yellow than 9% H2O2 commercial bleached hair and 6% H202 bleached hair. DSC investigations reveal that the three bleaches have a homogenous oxidation effect on IFs and IFAPs. The deconvolution results using three Gaussian distributions confirm this observation. The stronger bleach results in a homogenous structural damage on both para- and ortho-cortex with increasing bleaching time. Commercial persulphate bleach and 9% H2O2 commercial bleach have a progressive damage effect on the ortho- and para- cortex than 6% H202 bleach. Kinetics analysis is conducted for the virgin and bleached hairs by using various heating rates according to ASTM-E698. The activation energies of 260 kJ/mol for the virgin hair and 295 kJ/mol for the commercial persulphate bleached hair (2h) are determined from the slope of the regression line of peak temperature, TD (as 1/TD) and heating rate, β (as lnβ) on the basis of the Arrhenius-equation. The predominant structural damage for various heating rates only occurs in the IF. It is shown that a linear increase in DeltaHD occurs for lower heating rates, while it is constant for higher heating rates. This can be ascribed to the hypothesis that a lower heating rate favours a crystal transformation change (alpha-β transformation), while a higher rate favours a crystalline-amorphous transformation. SEM examines the morphological changes of hair samples after DSC. The cortex has been dissolved at the lower heating rate. The commercial persulphate bleached hairs (2h) show an overall shrunk cuticle surface and fewer and smaller hydrolysed protein granules, due to the previous damage of the alpha-helix in the cortical cell.

o comportamento, frente ao envelhecimento físico, do sistema diglicidil éter do bisfenol-A (DGEBA) curado com diaminodifenilmetano (DOM) foi estudado em função da estrutura química, induzida pela cura, e do tempo de envelhecimento. Sistemas estequiométricos foram submetidos a Calorimetria Diferencial de Varredura (DSC) e Análise Térmica Dinâmico-Mecânica (DMTA). A cura isotérmica da resina epóxi foi realizada em uma etapa a 115°C e 135°C, por 20, 30, 45, 60 e 90 mino As amostras foram envelhecidas a 100°C por períodos de 4 até 72h. A extensão do envelhecimento físico foi associado com a área do pico endotérmico que aparece na região da transição vítrea, de acordo com os termogramas de DSC. Foi observado que a entalpia de relaxação aumenta gradualmente com o tempo de envelhecimento. Por DMT A, observou-se variações na magnitude do fator de perda (tan õ), no pico máximo, em função do grau de cura e do tempo de envelhecimento. O módulo dinâmico de armazenamento a 100°C (E'1CX)) deslocou-se para valores maiores assim como a Tg, medida através do pico a da curva log E", com o aumento do tempo de envelhecimento. A velocidade de envelhecimento e as energias de ativação da transição α foram obtidas a partir de parâmetros dinâmico-mecânicos e após associados com as diferentes histórias de cura e envelhecimento do material. De modo geral, a velocidade de envelhecimento (Ra) decresce com o aumento do grau de reticulação para sistemas curados a 115°C e passa por um mínimo para as amostras curadas a 135°C. As energias de ativação mostram uma tendência crescente com o tempo de envelhecimento. Concluiu-se que a técnica de DMTA é muito sensível às mudanças estruturais devido à cura e ao envelhecimento físico realizados nos sistemas investigados. Os resultados dinâmico-mecânicos obtidos para as misturas curadas segundo diferentes histórias térmicas salientam a importância da seleção adequada das condições de cura para que se possam obter as melhores propriedades destes materiais. / Physical aging behavior of diglycidyl ether of bisphenol-A (DGEBA) cured with diaminodiphenylmethane (DDM) have been investigated as a function of chemical structure, induced by cure, and aging time. Stoichiometric systems have been submitted to Differencial Scanning Calorimetry (DSC) and Dynamic Mechanical Thermal Analysis (DMTA) measurements. The isothermal curing of the epoxy resin was carried out in one step at 115°C and at 135°C for 20, 30, 45, 60 and 90 mino Samples were aged at 100°C for periods of time from 4 to a maximum of 72 h. The extent of physical aging has been measured by the area of the endothermic peak which appears within the glass transition region according to DSC thermograms. The enthalpy relaxation was found to increase gradually with aging time. Variations on magnitude of the loss factor (tan õ), on the maximum peak, have been observed as a function of degree of cure and aging time. The dynamic storage modulus at 100°C ( E' 100) changed with increasing physical aging to higher values as well as the glass transition temperature (Tg) as measured by the a peak on log E" curves. Aging rates and α transition activation energies were obtained through DMT A parameters analysis and then associated with different curing and aging histories of the material. Generally, the aging rate (Ra) decreases with increasing crosslinking degree for the systems cured at 115°C and passes through a minimum for those cured at 135°C. The activation energies demonstrate a tendecy to increase with aging time. It was concluded that the DMTA technique is very sensitive to structural changes in the investigated epoxy systems due to curing and physical aging . The DMTA results obtained from mixtures cured with different thermal histories underline the importance of adequate selection of curing conditions in order to obtain the optimum properties for these materiais.

Made available in DSpace on 2014-06-11T19:31:04Z (GMT). No. of bitstreams: 0 Previous issue date: 2009-03-06Bitstream added on 2014-06-13T19:01:17Z : No. of bitstreams: 1 idalgojunior_e_dr_bauru.pdf: 2079411 bytes, checksum: df3a2a8007dd150c42361dca5a38338a (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / No presente estudo, quatro vidros 20 'Li IND. 2' O-80Te 'O IND. 2' foram preparados com composição nominal idêntica mas com diferentes histórias térmicas. As técnicas de difração de raios-X, espectroscopia no infravermelho, espectroscopia Raman e calorimetria diferencial de varredura foram usadas para compreender os efeitos da história térmica sobre as propriedades térmicas e estruturais dos vidros estudados. Observou-se que as propriedades investigadas dependem fortemente da história térmica dos vidros. Os resultados de difração de raios-X revelaram a presença de três fases cristalinas distintas у-Te 'O IND. 2', α-Te 'O IND. 2, у-Te 'O IND. 2', α-Te 'O IND. 2 e α- 'Li IND. 2'Te 'O IND. 2''O IND. 5' nos vidros estudados com a seguinte sequência de cristalização у-Te 'O IND. 2' 'seta' α-Te 'O IND. 2 'seta' у-Te 'O IND. 2', α-Te 'O IND. 2 'seta' α- 'Li IND. 2'Te 'O IND. 2''O IND. 5. A fase у-Te 'O IND. 2' é metaestável enquanto as fases cristalinas у-Te 'O IND. 2' e α- 'Li IND. 2'Te 'O IND. 2''O IND. 5' persistem até os estágios finais da cristalização. A estrutura das bandas no espectro infravermelho é similar àquelas observadas em vidros Te O IND. 2'. Para vidros selecionados, as energias de ativação associadas as fases cristalinas foram calculadas considerando que os picos de cristalização das curvas de DSC possam ser representados por três funções lorentzianas reportados em diferentes tamanhos de partículas. Os resultados de DSC sugerem ainda que tratamentos térmicos a longos tempos, em torno de 'T IND. g', imediatamente após o quenching são favoráveis para a produçao de regiões ordenadas nos vidros sem necessariamente aumentar o número de núcleos na matriz vítrea. / In the present study, four 20 'Li IND. 2' O-80Te 'O IND. 2', glasses were prepared with identical nominal composition but with different histories. X-Ray Diffraction, Infrared Sprectroscopy, Raman Spectroscopy and Differential Scanning Calorimetry techniques were used to understand the effects of the thermal histories on the thermal and structural properties of the studied glasses. It was observed that investigated properties depend strongly on the thermal histories of the glasses. X-ray Diffraction results reveal the presence of three distinct у-Te 'O IND. 2', α-Te 'O IND. 2 and α- 'Li IND. 2'Te 'O IND. 2''O IND. 5' crystalline phases in the studied glasses with the following crystallization у-Te 'O IND. 2' 'seta' α-Te 'O IND. 2 'seta' у-Te 'O IND. 2', α-Te 'O IND. 2 'seta' α- 'Li IND. 2'Te 'O IND. 2''O IND. 5 sequence. The у-Te 'O IND. 2' is a mestastable phase while α- 'Li IND. 2'Te 'O IND. 2''O IND. 5' crystalline phases persist up to the final stages of the in situ bulk crystallization. The infrared band structure of the studied glasses is similar to the one observed in glassy Te 'O IND. 2'. For selected glasses, activation energies were evaluated from lorentzian three-peak deconvolution of the DSC crystallization peak recorded at different particle sizes. DSC results suggested that heat annealing immediately after quenching at temperatures around 'T IND. g' and longer times are favorable to produce local ordered regions in the glass without necessarily the nuclei number in the glass matrix.

Orientador: José Paschoal Batistuti / Banca: Maria Helena Martini / Banca: Valdir Augusto Neves / Banca: José Alfredo Gomes Arêas / Banca: João Bosco Faria / Resumo: A partir da farinha da semente de goiaba (Psidium guajava), cuja composição centesimal é de aproximadamente 6,17 l 0,04% de umidade, 8,43 l 0,12% de proteína e alto teor de fibras, 60,88 l 0,9%, obteve-se isolado protéico (IP) através da precipitação isoelétrica (pI 4,5), cuja fração majoritária pertence à classe das glutelinas. As condições para o preparo do IP foram definidas a partir da curva de solubilidade em água x pH e temperatura de 25 l 3 ºC. Tais condições permitiram obter isolados protéicos com rendimento de extração de 45,2 l 0,5% (pH10,0) e 66,2 l 0,5% (pH11,5) e elevado conteúdo protéico 96,4 l 0,5% e 93,5 l 0,4% respectivamente. A capacidade de absorção de água e óleo foram baixas, apresentando 1,05 l 0,07 e 2,3 l 0,01 mL/g proteína respectivamente para IP 10,0 e 1,65 l 0,07 e 1,70 l 0,07 mL/g pr oteína respectivamente para IP 11,5. A maior capacidade de emulsificação, foi observado para o IP 11,5, 140 l 8 g óleo/g prot., comparado com o IP 10,0, 37 l 2 g óleo/g prot. A formação de gel foi observada em pH neutro e ausência de sal, apresentando as concentrações de 8% para IP 10,0 e 10% para IP 11,5. A cromatografia revelou a presença de dois picos para ambos isolados com sete frações de proteínas de diferentes pesos moleculares. As curvas TG-DTG / DSC revelaram maior quantidade de água para o IP 10,0 e elevada temperatura de estabilidade térmica 200 oC para ambos isolados. / Abstract: From the guava seed flour (Psidium guajava), whose centesimal composition belongs to about 6,17 ??0,04% of moisture, 8,43 ??0,12% of protein and high content of fibers, 60,88 ??0,9%, the protein isolate (PI) was obtained through the isoelectric precipitation (Ip 4,5) whose majority belongs to glutelins class proteins. The conditions for the preparation of the PI was defined from the solubility curve in water x pH and temperature of 25 ??3ºC. Such conditions allowed to obtain protein isolated with extraction yield of 45,2 ??0,5% (pH10,0) and 66,2 ??0,5% (pH11,5) and high protein content of 96,4 ??0,5% and 93,5 ??0,4% respectively. The absorption capacity for water and oil were low, showing 1,05 l 0,07 and 2,3 l 0,01 mL/g protein, respectively, for PI 10,0 and 1,65 l 0,07 and 1,70 l 0,07 mL/g protein, respectively, for PI 11,5. The most emulsification capacity was observed for PI 11,5 (140 l 8 g oil/g prot.), compared to PI 10,0 (37 l 2 g oil/g prot.). The gel formation was observed in neutral pH and salt absence, showing the concentrations of 8% to PI 10,0 and 10% to PI 11,5. The chromatography shows the presence of two peaks for both protein isolated with seven fractions of proteins with different molecular weights. The curves of TG-DTG / DSC revealed high water quantity for PI 10,0 and high temperature for thermal stability 200 °C for both isolates. / Mestre

Submitted by Jean Medeiros (jeanletras@uepb.edu.br) on 2016-04-13T13:00:25Z No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) / Approved for entry into archive by Secta BC (secta.csu.bc@uepb.edu.br) on 2016-06-13T20:27:28Z (GMT) No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) / Made available in DSpace on 2016-06-13T20:28:54Z (GMT). No. of bitstreams: 1 PDF - Rayanne Sales de Araújo Batista.pdf: 2799391 bytes, checksum: bfd7e21254a6a5383f8798d74f80923d (MD5) Previous issue date: 2015-03-19 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Retinoic acid (RA), widely used in dermatological and cosmetic products, has low stability in the presence of air and light, with sensitivity to heat and oxidation, so it is particularly important to implement the quality control of its finished products performing tests indicators of stability. Therefore, the objective was to develop an analytical method to evaluate the thermal stability of an RA cream formulation through the correlation of analytical techniques, high performance liquid chromatography with ultraviolet detection efficiency (HPLC-UV), differential scanning calorimetry (DSC) and vibrational absorption spectroscopy in the infrared Fourier transform spectroscopy (FTIR). Previously been established chromatographic conditions for development of the analytical method using HPLC-UV system, which was subjected to analytical tests specified in RE ANVISA Nº 899/2003 for validation. For evaluation of the thermal stability the cream samples were subjected to thermal stress in an oven at temperatures of 60, 70 and 80 °C and subsequently analyzed by HPLC-UV over the period of 0, 24, 48 and 72 h. DSC analyzes and FTIR spectra were carried out from the binary mixture (BM) of the RA and excipients of the cream formulation to investigate possible physical and/or chemical interactions. According to the data obtained it was possible to develop an analytical method by validated HPLC-UV, and based thereon, for analyzing and quantifying the RA content cream formulation, it has been found that from 70 ° C caused a decrease in the content of RA, and 0-order kinetics; and 80 ° C, followed a kinetic order 2 by setting up a reaction of bimolecular type. The analytical techniques DSC and FTIR showed the absence of chemical and physical interaction in most MB among the components of the formulation, except only for the carrier sodium metabisulfite. Thus, we can infer that it has a well-defined thermal behavior and compatibility of its components. / O ácido retinoico (AR), largamente utilizado em produtos dermatológicos e cosméticos, apresenta baixa estabilidade na presença de ar e luz, com sensibilidade ao calor e à oxidação, assim, é particularmente importante implementar o controle de qualidade de seus produtos acabados realizando ensaios indicadores de estabilidade. Logo, objetivou-se desenvolver um método analítico para avaliar a estabilidade térmica de uma formulação creme de AR através da correlação de técnicas analíticas, cromatografia líquida de alta eficiência com detecção ultravioleta (CLAE-UV), calorimetria exploratória diferencial (DSC) e espectroscopia vibracional de absorção na região do infravermelho com transformada de Fourier (FTIR). Previamente foram estabelecidas as condições cromatográficas para desenvolvimento do método analítico utilizando um sistema de CLAE-UV, o qual foi submetido aos testes analíticos especificados na RE ANVISA nº 899/2003 para validação do mesmo. Para avaliação da estabilidade térmica, as amostras do creme foram submetidas a estresse térmico em estufa nas temperaturas de 60, 70 e 80 º C, e posteriormente analisadas por CLAE-UV no período de 0, 24, 48 e 72 h. As análises de DSC e dos espectros de FTIR foram realizadas a partir das misturas binárias (MB) do AR e excipientes da formulação creme a fim de investigar possíveis interações físicas e/ou químicas. De acordo com os dados obtidos foi possível desenvolver um método analítico por CLAE-UV validado, e com base no mesmo, para análise e quantificação do teor de AR em formulação creme, constatou-se que a partir de 70 ° C ocorreu redução no teor de AR, e cinética de ordem 0; a 80 ° C, obedeceu uma cinética de ordem 2, configurando uma reação do tipo bimolecular. As técnicas analíticas DSC e FTIR mostraram a ausência de interação física e química na maioria das MB entre os componentes da formulação, com exceção apenas para o excipiente metabissulfito de sódio. Desta forma, podemos inferir que a mesma apresenta um comportamento térmico bem definido e compatibilidade entre seus componentes.

abstract: In medical imaging, a wide variety of methods are used to interrogate structural and physiological differences between soft tissues. One of the most ubiquitous methods in clinical practice is Magnetic Resonance Imaging (MRI), which has the advantage of limited invasiveness, soft tissue discrimination, and adequate volumetric resolution. A myriad of advanced MRI methods exists to investigate the microstructural, physiologic and metabolic characteristics of tissue. For example, Dynamic Contrast Enhanced (DCE) and Dynamic Susceptibility Contrast (DSC) MRI non-invasively interrogates the dynamic passage of an exogenously administered MRI contrast agent through tissue to quantify local tracer kinetic properties like blood flow, vascular permeability and tissue compartmental volume fractions. Recently, an improved understanding of the biophysical basis of DSC-MRI signals in brain tumors revealed a new approach to derive multiple quantitative biomarkers that identify intrinsic sub-voxel cellular and vascular microstructure that can be used differentiate tumor sub-types. One of these characteristic biomarkers called Transverse Relaxivity at Tracer Equilibrium (TRATE), utilizes a combination of DCE and DSC techniques to compute a steady-state metric which is particularly sensitive to cell size, density, and packing properties. This work seeks to investigate the sensitivity and potential utility of TRATE in a range of disease states including Glioblastomas, Amyotrophic Lateral Sclerosis (ALS), and Duchenne’s Muscular Dystrophy (DMD). The MRC measures of TRATE showed the most promise in mouse models of ALS where TRATE values decreased with disease progression, a finding that correlated with reductions in myofiber size and area, as quantified by immunohistochemistry. In the animal models of cancer and DMD, TRATE results were more inconclusive, due to marked heterogeneity across animals and treatment state. Overall, TRATE seems to be a promising new biomarker but still needs further methodological refinement due to its sensitivity to contrast to noise and further characterization owing to its non-specificity with respect to multiple cellular features (e.g. size, density, heterogeneity) that complicate interpretation. / Dissertation/Thesis / Masters Thesis Biomedical Engineering 2018

L’utilisation d’adhésifs polyépoxy et plus particulièrement de pâte de calage dans l’aéronautique est chose très courante. L’augmentation des cadences de production des aéronefs poussent les fournisseurs à adapter les temps technologiques de ces produits (temps d’application et de complète polymérisation) : ainsi, la cinétique de réticulation des adhésifs de demain devra être lente à température ambiante et pouvant être accélérée à tout moment. Pour cela, la piste envisagée pour ces tra-vaux est la polymérisation sous rayonnement infrarouge. La cinétique de ré-action a été évaluée par analyse thermique (DSC) ou par analyse spectrosco-pique (MIR ou PIR). Les résultats obtenus ont mis en évidence un effet thermique et non thermique du rayonnement infrarouge. Grâce à plusieurs expérimentations, les résultats montrent que le rayonnement infrarouge interagit avec les groupe-ments époxydes dont l’énergie d’activation de la réaction avec les amines primaires diminue. Par ailleurs, l’utilisation d’un plan d’expérience a permis de montrer que l’adhérence et les propriétés mécaniques de ces adhésifs augmentaient suite à l’utilisation du rayonnement infrarouge.

In this study, we have investigated the relationship between the process-microstructure to predict and modify the material's properties. Understanding these relationships allows the identification and correction of processing deficiencies when the desired properties are not achieved, depending on the microstructure. Hence, the co-relation between process-microstructure-properties helped reduce the number of experiments, materials & tool costs and saved much time. In the case of high entropy alloys, friction stir welding (FSW) causes improved strength due to the formation of fine grain structure and phase transformation from f.c.c to h.c.p. The phase transformation is temperature sensitive and is studied with the help of differential scanning calorimetry (DSC) to calculate the enthalpy experimentally to obtain ΔGγ→ε. The second process discussed is heat treatment causing precipitation evolution. Fundamental investigations aided in understanding the influence of strengthening precipitates on mechanical properties due to the aging kinetics – solid solution and variable artificial aging temperature and time. Finally, in the third case, the effect of FSW parameters causes the thermal profile to be generated, which significantly influences the final microstructure and weld properties. Therefore, a computational model using COMSOL Multiphysics and TC-Prisma is developed to generate the thermal profile for different weld parameters to understand its effect on the microstructure, which would eventually affect and predict the final properties of the weld. The model's validation is done via DSC, TEM, and mechanical testing.