Search results for: within-laboratory reproducibility

Authors: Pavel Damborsky, Martina Zamorova, Jaroslav Katrlik

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Prostate cancer is annually the most common newly diagnosed cancer among men. An extensive number of evidence suggests that traditional serum Prostate-specific antigen (PSA) assay still suffers from a lack of sufficient specificity and sensitivity resulting in vast over-diagnosis and overtreatment. Thus, the early-stage detection of prostate cancer (PCa) plays undisputedly a critical role for successful treatment and improved quality of life. Over the last decade, particular altered glycans have been described that are associated with a range of chronic diseases, including cancer and inflammation. These glycans differences enable a distinction to be made between physiological and pathological state and suggest a valuable biosensing tool for diagnosis and follow-up purposes. Aberrant glycosylation is one of the major characteristics of disease progression. Consequently, the aim of this study was to develop a more reliable tool for early-stage PCa diagnosis employing lectins as glyco-recognition elements. Biosensor and biochip technology putting to use lectin-based glyco-profiling is one of the most promising strategies aimed at providing fast and efficient analysis of glycoproteins. The proof-of-concept experiments based on sandwich assay employing anti-PSA antibody and an aptamer as a capture molecules followed by lectin glycoprofiling were performed. We present a lectin-based biosensing assay for glycoprofiling of serum biomarker PSA using different biosensor and biochip platforms such as label-free surface plasmon resonance (SPR) and microarray with fluorescent label. The results suggest significant differences in interaction of particular lectins with PSA. The antibody-based assay is frequently associated with the sensitivity, reproducibility, and cross-reactivity issues. Aptamers provide remarkable advantages over antibodies due to the nucleic acid origin, stability and no glycosylation. All these data are further step for construction of highly selective, sensitive and reliable sensors for early-stage diagnosis. The experimental set-up also holds promise for the development of comparable assays with other glycosylated disease biomarkers.

Keywords: biomarker, glycosylation, lectin, prostate cancer

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Authors: Jakob Krause

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Past Financial Crisis has shown that contemporary risk management models provide an unjustified sense of security and fail miserably in situations in which they are needed the most. In this paper, we start from the assumption that risk is a notion that changes over time and therefore past data points only have limited explanatory power for the current situation. Our objective is to derive the optimal amount of representative information by optimizing between the two adverse forces of estimator convergence, incentivizing us to use as much data as possible, and the aforementioned non-representativeness doing the opposite. In this endeavor, the cornerstone assumption of having access to identically distributed random variables is weakened and substituted by the assumption that the law of the data generating process changes over time. Hence, in this paper, we give a quantitative theory on how to perform statistical analysis in non-ergodic systems. As an application, we discuss the impact of a paragraph in the last iteration of proposals by the Basel Committee on Banking Regulation. We start from the premise that the severity of assumptions should correspond to the robustness of the system they describe. Hence, in the formal description of physical systems, the level of assumptions can be much higher. It follows that every concept that is carried over from the natural sciences to economics must be checked for its plausibility in the new surroundings. Most of the probability theory has been developed for the analysis of physical systems and is based on the independent and identically distributed (i.i.d.) assumption. In Economics both parts of the i.i.d. assumption are inappropriate. However, only dependence has, so far, been weakened to a sufficient degree. In this paper, an appropriate class of non-stationary processes is used, and their law is tied to a formal object measuring representativeness. Subsequently, that data set is identified that on average minimizes the estimation error stemming from both, insufficient and non-representative, data. Applications are far reaching in a variety of fields. In the paper itself, we apply the results in order to analyze a paragraph in the Basel 3 framework on banking regulation with severe implications on financial stability. Beyond the realm of finance, other potential applications include the reproducibility crisis in the social sciences (but not in the natural sciences) and modeling limited understanding and learning behavior in economics.

Keywords: banking regulation, non-ergodicity, risk management, semimartingale modeling

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Authors: Bharti Jain, Rajeev Jain, Abuzar Kabir, Torki Zughaibi, Shweta Sharma

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Drug-facilitated crimes (DFCs) entail the use of a single drug or a mixture of drugs to render a victim unable. Traditionally, biological samples have been gathered from victims and conducted analysis to establish evidence of drug administration. Nevertheless, the rapid metabolism of various drugs and delays in analysis can impede the identification of such substances. For this, the present article describes a rapid, sustainable, highly efficient and miniaturized protocol for the identification and quantification of three sedative-hypnotic drugs, namely diazepam, chlordiazepoxide and ketamine in alcoholic beverages and complex food samples (cream of biscuit, flavored milk, juice, cake, tea, sweets and chocolate). The methodology involves utilizing fabric phase sorptive extraction (FPSE) to extract diazepam (DZ), chlordiazepoxide (CDP), and ketamine (KET). Subsequently, the extracted samples are subjected to analysis using gas chromatography-mass spectrometry (GC-MS). Several parameters, including the type of membrane, pH, agitation time and speed, ionic strength, sample volume, elution volume and time, and type of elution solvent, were screened and thoroughly optimized. Sol-gel Carbowax 20M (CW-20M) has demonstrated the most effective extraction efficiency for the target analytes among all evaluated membranes. Under optimal conditions, the method displayed linearity within the range of 0.3–10 µg mL–¹ (or µg g–¹), exhibiting a coefficient of determination (R2) ranging from 0.996–0.999. The limits of detection (LODs) and limits of quantification (LOQs) for liquid samples range between 0.020-0.069 µg mL-¹ and 0.066-0.22 µg mL-¹, respectively. Correspondingly, the LODs for solid samples ranged from 0.056-0.090 µg g-¹, while the LOQs ranged from 0.18-0.29 µg g-¹. Notably, the method showcased better precision, with repeatability and reproducibility both below 5% and 10%, respectively. Furthermore, the FPSE-GC-MS method proved effective in determining diazepam (DZ) in forensic food samples connected to drug-facilitated crimes (DFCs). Additionally, the proposed method underwent evaluation for its whiteness using the RGB12 algorithm.

Keywords: drug facilitated crime, fabric phase sorptive extraction, food forensics, white analytical chemistry

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Authors: Zeineb Baatout, Safa Teka, Nejmeddine Jaballah, Nawfel Sakly, Xiaonan Sun, Mustapha Majdoub

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Currently, the economic interests linked to the development of bio-based materials make biomass one of the most interesting areas for science development. We are interested in the β-cyclodextrin (β-CD), one of the popular bio-sourced macromolecule, produced from the starch via enzymatic conversion. It is a cyclic oligosaccharide formed by the association of seven glucose units. It presents a rigid conical and amphiphilic structure with hydrophilic exterior, allowing it to be water-soluble. It has also a hydrophobic interior enabling the formation of inclusion complexes, which support its application for the elaboration of electrochemical and optical sensors. Nevertheless, the solubility of β-CD in water makes its use as sensitive layer limit and difficult due to their instability in aqueous media. To overcome this limitation, we chose to precede by modification of the hydroxyl groups to obtain hydrophobic derivatives which lead to water-stable sensing layers. Hence, a series of benzylated β-CDs were synthesized in basic aqueous media in one pot. This work reports the synthesis of a new family of substituted amphiphilic β-CDs using a green methodology. The obtained β-CDs showed different degree of substitution (DS) between 0.85 and 2.03. These organic macromolecular materials were soluble in common organic volatile solvents, and their structures were investigated by NMR, FT-IR and MALDI-TOF spectroscopies. Thermal analysis showed a correlation between the thermal properties of these derivatives and the benzylation degree. The surface properties of the thin films based on the benzylated β-CDs were characterized by contact angle measurements and atomic force microscopy (AFM). These organic materials were investigated as sensitive layers, deposited on quartz crystal microbalance (QCM) gravimetric transducer, for humidity sensor at room temperature. The results showed that the performances of the prepared sensors are greatly influenced by the benzylation degree of β-CD. The partially modified β-CD (DS=1) shows linear response with best sensitivity, good reproducibility, low hysteresis, fast response time (15s) and recovery time (17s) at higher relative humidity levels (RH) between 11% and 98% in room temperature.

Keywords: β-cyclodextrin, green synthesis, humidity sensor, quartz crystal microbalance

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Authors: Ariadne C. Catto, Luis F. da Silva, Khalifa Aguir, Valmor Roberto Mastelaro

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Zinc oxide (ZnO) pure or doped are one of the most promising metal oxide semiconductors for gas sensing applications due to the well-known high surface-to-volume area and surface conductivity. It was shown that ZnO is an excellent gas-sensing material for different gases such as CO, O2, NO2 and ethanol. In this context, pure and doped ZnO exhibiting different morphologies and a high surface/volume ratio can be a good option regarding the limitations of the current commercial sensors. Different studies showed that the sensitivity of metal-doped ZnO (e.g. Co, Fe, Mn,) enhanced its gas sensing properties. Motivated by these considerations, the aim of this study consisted on the investigation of the role of Co ions on structural, morphological and the gas sensing properties of nanostructured ZnO samples. ZnO and Zn1-xCoxO (0 < x < 5 wt%) thin films were obtained via the polymeric precursor method. The sensitivity, selectivity, response time and long-term stability gas sensing properties were investigated when the sample was exposed to a different concentration range of ozone (O3) at different working temperatures. The gas sensing property was probed by electrical resistance measurements. The long and short-range order structure around Zn and Co atoms were investigated by X-ray diffraction and X-ray absorption spectroscopy. X-ray photoelectron spectroscopy measurement was performed in order to identify the elements present on the film surface as well as to determine the sample composition. Microstructural characteristics of the films were analyzed by a field-emission scanning electron microscope (FE-SEM). Zn1-xCoxO XRD patterns were indexed to the wurtzite ZnO structure and any second phase was observed even at a higher cobalt content. Co-K edge XANES spectra revealed the predominance of Co2+ ions. XPS characterization revealed that Co-doped ZnO samples possessed a higher percentage of oxygen vacancies than the ZnO samples, which also contributed to their excellent gas sensing performance. Gas sensor measurements pointed out that ZnO and Co-doped ZnO samples exhibit a good gas sensing performance concerning the reproducibility and a fast response time (around 10 s). Furthermore, the Co addition contributed to reduce the working temperature for ozone detection and improve the selective sensing properties.

Keywords: cobalt-doped ZnO, nanostructured, ozone gas sensor, polymeric precursor method

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Authors: Alexander E. Hramov, Vadim V. Grubov, Alexey A. Koronovskii, Maria K. Kurovskaуa, Anastasija E. Runnova

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The perception of visual signals in the brain was among the first issues discussed in terms of multistability which has been introduced to provide mechanisms for information processing in biological neural systems. In this work the influence of the cognitive noise on the visual perception of multistable pictures has been investigated. The study includes an experiment with the bistable Necker cube illusion and the theoretical background explaining the obtained experimental results. In our experiments Necker cubes with different wireframe contrast were demonstrated repeatedly to different people and the probability of the choice of one of the cubes projection was calculated for each picture. The Necker cube was placed at the middle of a computer screen as black lines on a white background. The contrast of the three middle lines centered in the left middle corner was used as one of the control parameter. Between two successive demonstrations of Necker cubes another picture was shown to distract attention and to make a perception of next Necker cube more independent from the previous one. Eleven subjects, male and female, of the ages 20 through 45 were studied. The choice of the Necker cube projection was detected with the Electroencephalograph-recorder Encephalan-EEGR-19/26, Medicom MTD. To treat the experimental results we carried out theoretical consideration using the simplest double-well potential model with the presence of noise that led to the Fokker-Planck equation for the probability density of the stochastic process. At the first time an analytical solution for the probability of the selection of one of the Necker cube projection for different values of wireframe contrast have been obtained. Furthermore, having used the results of the experimental measurements with the help of the method of least squares we have calculated the value of the parameter corresponding to the cognitive noise of the person being studied. The range of cognitive noise parameter values for studied subjects turned to be [0.08; 0.55]. It should be noted, that experimental results have a good reproducibility, the same person being studied repeatedly another day produces very similar data with very close levels of cognitive noise. We found an excellent agreement between analytically deduced probability and the results obtained in the experiment. A good qualitative agreement between theoretical and experimental results indicates that even such a simple model allows simulating brain cognitive dynamics and estimating important cognitive characteristic of the brain, such as brain noise.

Keywords: bistability, brain, noise, perception, stochastic processes

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Authors: Kamal Kaushik, Dandpani Epili, Ajay G. V., Ashutosh, S. Pradhaan

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Introduction: Radiation therapy has come a long way over a period of decades, from 2-dimensional radiotherapy to intensity-modulated radiation therapy (IMRT) or VMAT. For advanced radiation therapy, we need better patient position reproducibility to deliver precise and quality treatment, which raises the need for better image guidance technologies for precise patient positioning. This study presents a two tattoo simulation with roll correction technique which is comparable to other advanced patient positioning techniques. Objective: This is a site-specific study is aimed to perform a comparison between various treatment positioning techniques used for the treatment of patients of Ca- Breast undergoing radiotherapy. In this study, we are comparing 5 different positioning methods used for the treatment of ca-breast, namely i) Vacloc with 3 tattoos, ii) Breast board with three tattoos, iii) Thermoplastic cast with three fiducials, iv) Breast board with a thermoplastic mask with 3 tattoo, v) Breast board with 2 tattoos – A roll correction method. Methods and material: All in one (AIO) solution immobilization was used in all patient positioning techniques for immobilization. The process of two tattoo simulations includes positioning of the patient with the help of a thoracic-abdomen wedge, armrest & knee rest. After proper patient positioning, we mark two tattoos on the treatment side of the patient. After positioning, place fiducials as per the clinical borders markers (1) sternum notch (lower border of clavicle head) (2) 2 cm below from contralateral breast (3) midline between 1 & 2 markers (4) mid axillary on the same axis of 3 markers (Marker 3 & 4 should be on the same axis). During plan implementation, a roll depth correction is applied as per the anterior and lateral positioning tattoos, followed by the shifts required for the Isocentre position. The shifts are then verified by SSD on the patient surface followed by radiographic verification using Cone Beam Computed Tomography (CBCT). Results: When all the five positioning techniques were compared all together, the produced shifts in Vertical, Longitudinal and lateral directions are as follows. The observations clearly suggest that the Longitudinal average shifts in two tattoo roll correction techniques are less than every other patient positioning technique. Vertical and lateral Shifts are also comparable to other modern positioning techniques. Concluded: The two tattoo simulation with roll correction technique provides us better patient setup with a technique that can be implemented easily in most of the radiotherapy centers across the developing nations where 3D verification techniques are not available along with delivery units as the shifts observed are quite minimal and are comparable to those with Vacloc and modern amenities.

Keywords: Ca. breast, breast board, roll correction technique, CBCT

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Authors: Bilel Chalghaf, Mathieu Varin

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Forest characterization in Quebec, Canada, is usually assessed based on photo-interpretation at the stand level. For species identification, this often results in a lack of precision. Very high spatial resolution imagery, such as DigitalGlobe, and Light Detection and Ranging (LiDAR), have the potential to overcome the limitations of aerial imagery. To date, few studies have used that data to map a large number of species at the tree level using machine learning techniques. The main objective of this study is to map 11 individual high tree species ( > 17m) at the tree level using an object-based approach in the broadleaf forest of Kenauk Nature, Quebec. For the individual tree crown segmentation, three canopy-height models (CHMs) from LiDAR data were assessed: 1) the original, 2) a filtered, and 3) a corrected model. The corrected CHM gave the best accuracy and was then coupled with imagery to refine tree species crown identification. When compared with photo-interpretation, 90% of the objects represented a single species. For modeling, 313 variables were derived from 16-band WorldView-3 imagery and LiDAR data, using radiance, reflectance, pixel, and object-based calculation techniques. Variable selection procedures were employed to reduce their number from 313 to 16, using only 11 bands to aid reproducibility. For classification, a global approach using all 11 species was compared to a semi-hierarchical hybrid classification approach at two levels: (1) tree type (broadleaf/conifer) and (2) individual broadleaf (five) and conifer (six) species. Five different model techniques were used: (1) support vector machine (SVM), (2) classification and regression tree (CART), (3) random forest (RF), (4) k-nearest neighbors (k-NN), and (5) linear discriminant analysis (LDA). Each model was tuned separately for all approaches and levels. For the global approach, the best model was the SVM using eight variables (overall accuracy (OA): 80%, Kappa: 0.77). With the semi-hierarchical hybrid approach, at the tree type level, the best model was the k-NN using six variables (OA: 100% and Kappa: 1.00). At the level of identifying broadleaf and conifer species, the best model was the SVM, with OA of 80% and 97% and Kappa values of 0.74 and 0.97, respectively, using seven variables for both models. This paper demonstrates that a hybrid classification approach gives better results and that using 16-band WorldView-3 with LiDAR data leads to more precise predictions for tree segmentation and classification, especially when the number of tree species is large.

Keywords: tree species, object-based, classification, multispectral, machine learning, WorldView-3, LiDAR

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Authors: Henry Memczak, Marc Hovestaedt, Bernhard Ay, Sandra Saenger, Thorsten Wolff, Frank F. Bier

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The influenza viruses cause flu epidemics every year and serious pandemics in larger time intervals. The only cost-effective protection against influenza is vaccination. Due to rapid mutation continuously new subtypes appear, what requires annual reimmunization. For a correct vaccination recommendation, the circulating influenza strains had to be detected promptly and exactly and characterized due to their antigenic properties. During the flu season 2016/17, a wrong vaccination recommendation has been given because of the great time interval between identification of the relevant influenza vaccine strains and outbreak of the flu epidemic during the following winter. Due to such recurring incidents of vaccine mismatches, there is a great need to speed up the process chain from identifying the right vaccine strains to their administration. The monitoring of subtypes as part of this process chain is carried out by national reference laboratories within the WHO Global Influenza Surveillance and Response System (GISRS). To this end, thousands of viruses from patient samples (e.g., throat smears) are isolated and analyzed each year. Currently, this analysis involves complex and time-intensive (several weeks) animal experiments to produce specific hyperimmune sera in ferrets, which are necessary for the determination of the antigen profiles of circulating virus strains. These tests also bear difficulties in standardization and reproducibility, which restricts the significance of the results. To replace this test a peptide-based assay for influenza virus subtyping from corresponding virus samples was developed. The differentiation of the viruses takes place by a set of specifically designed peptidic recognition molecules which interact differently with the different influenza virus subtypes. The differentiation of influenza subtypes is performed by pattern recognition guided by machine learning algorithms, without any animal experiments. Synthetic peptides are immobilized in multiplex format on various platforms (e.g., 96-well microtiter plate, microarray). Afterwards, the viruses are incubated and analyzed comparing different signaling mechanisms and a variety of assay conditions. Differentiation of a range of influenza subtypes, including H1N1, H3N2, H5N1, as well as fine differentiation of single strains within these subtypes is possible using the peptide-based subtyping platform. Thereby, the platform could be capable of replacing the current antigenic characterization of influenza strains using ferret hyperimmune sera.

Keywords: antigenic characterization, influenza-binding peptides, influenza subtyping, influenza surveillance

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Authors: Phenias Nsabimana, Jérôme W. Some, Hilda Vasanthakaalam, Stefaan De Henauw, Souheila Abbeddou

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Tools for the dietary assessment in adults are limited in low- and middle-income settings. The objective of this study was to develop and validate a semi-quantitative food frequency questionnaire (FFQ) against the multiple pass-24 h recall tool for use in urban and rural Rwanda. A total of 212 adults (154 females and 58 males), 18-49 aged, including 105 urban and 107 rural residents, from the four regions of Rwanda, were recruited in the present study. A multiple-pass 24- H recall technique was used to collect dietary data in both urban and rural areas in four different rounds, on different days (one weekday and one weekend day), separated by a period of three months, from November 2020 to October 2021. The details of all the foods and beverages consumed over the 24h period of the day prior to the interview day were collected during face-to-face interviews. A list of foods, beverages, and commonly consumed recipes was developed by the study researchers and ten research assistants from the different regions of Rwanda. Non-standard recipes were collected when the information was available. A single semi-quantitative FFQ was also developed in the same group discussion prior to the beginning of the data collection. The FFQ was collected at the beginning and the end of the data collection period. Data were collected digitally. The amount of energy and macro-nutrients contributed by each food, recipe, and beverage will be computed based on nutrient composition reported in food composition tables and weight consumed. Median energy and nutrient contents of different food intakes from FFQ and 24-hour recalls and median differences (24-hour recall –FFQ) will be calculated. Kappa, Spearman, Wilcoxon, and Bland-Altman plot statistics will be conducted to evaluate the correlation between estimated nutrient and energy intake found by the two methods. Differences will be tested for their significance and all analyses will be done with STATA 11. Data collection was completed in November 2021. Data cleaning is ongoing and the data analysis is expected to be completed by July 2022. A developed and validated semi-quantitative FFQ will be available for use in dietary assessment. The developed FFQ will help researchers to collect reliable data that will support policy makers to plan for proper dietary change intervention in Rwanda.

Keywords: food frequency questionnaire, reproducibility, 24-H recall questionnaire, validation

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Authors: Martin Cai, Khadijah B. Hashim, Leng Leo, Edmund F. Tian

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Analysis of traditional Chinese medicinal (TCM) supplements has always been a laborious task, particularly in the case of multi‐ingredient formulations. Traditionally, herbal extracts are analysed using one or few markers compounds. In the recent years, however, pharmaceutical companies are introducing health supplements of TCM active ingredients to cater to the needs of consumers in the fast-paced society in this age. As such, new problems arise in the aspects of composition identification as well as quality analysis. In most cases of products or supplements formulated with multiple TCM herbs, the chemical composition, and nature of each raw material differs greatly from the others in the formulation. This results in a requirement for individual analytical processes in order to identify the marker compounds in the various botanicals. Thin-layer Chromatography (TLC) is a simple, cost effective, yet well-regarded method for the analysis of natural products, both as a Pharmacopeia-approved method for identification and authentication of herbs, and a great analytical tool for the discovery of chemical compositions in herbal extracts. Recent technical advances introduced High-Performance TLC (HPTLC) where, with the help of automated equipment and improvements on the chromatographic materials, both the quality and reproducibility are greatly improved, allowing for highly standardised analysis with greater details. Here we report an industrial consultancy project with ONI Global Pte Ltd for the analysis of LAC Liver Protector, a TCM formulation aimed at improving liver health. The aim of this study was to identify 4 key components of the supplement using HPTLC, following protocols derived from Chinese Pharmacopeia standards. By comparing the TLC profiles of the supplement to the extracts of the herbs reported in the label, this project proposes a simple and cost-effective analysis of the presence of the 4 marker compounds in the multi‐ingredient formulation by using 4 different HPTLC methods. With the increasing trend of small and medium-sized enterprises (SMEs) bringing natural products and health supplements into the market, it is crucial that the qualities of both raw materials and end products be well-assured for the protection of consumers. With the technology of HPTLC, science can be incorporated to help SMEs with their quality control, thereby ensuring product quality.

Keywords: traditional Chinese medicine supplement, high performance thin layer chromatography, active ingredients, product quality

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Authors: Alice Robba, Renaud Bouchet, Celine Barchasz, Jean-Francois Colin, Erik Elkaim, Kristina Kvashnina, Gavin Vaughan, Matjaz Kavcic, Fannie Alloin

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With their high theoretical energy density (~2600 Wh.kg-1), lithium/sulfur (Li/S) batteries are highly promising, but these systems are still poorly understood due to the complex mechanisms/equilibria involved. Replacing S8 by Li2S as the active material allows the use of safer negative electrodes, like silicon, instead of lithium metal. S8 and Li2S have different conductivity and solubility properties, resulting in a profoundly changed activation process during the first cycle. Particularly, during the first charge a high polarization and a lack of reproducibility between tests are observed. Differences observed between raw Li2S material (micron-sized) and that electrochemically produced in a battery (nano-sized) may indicate that the electrochemical process depends on the particle size. Then the major focus of the presented work is to deepen the understanding of the Li2S material charge mechanism, and more precisely to characterize the effect of the initial Li2S particle size both on the mechanism and the electrode preparation process. To do so, Li2S nanoparticles were synthetized according to two ways: a liquid path synthesis and a dissolution in ethanol, allowing Li2S nanoparticles/carbon composites to be made. Preliminary chemical and electrochemical tests show that starting with Li2S nanoparticles could effectively suppress the high initial polarization but also influence the electrode slurry preparation. Indeed, it has been shown that classical formulation process - a slurry composed of Polyvinylidone Fluoride polymer dissolved in N-methyle-2-pyrrolidone - cannot be used with Li2S nanoparticles. This reveals a complete different Li2S material behavior regarding polymers and organic solvents when going at the nanometric scale. Then the coupling between two operando characterizations such as X-Ray Diffraction (XRD) and X-Ray Absorption and Emission Spectroscopy (XAS/XES) have been carried out in order to interpret the poorly understood first charge. This study discloses that initial particle size of the active material has a great impact on the working mechanism and particularly on the different equilibria involved during the first charge of the Li2S based Li-ion batteries. These results explain the electrochemical differences and particularly the polarization differences observed during the first charge between micrometric and nanometric Li2S-based electrodes. Finally, this work could lead to a better active material design and so to more efficient Li2S-based batteries.

Keywords: Li-ion/Sulfur batteries, Li2S nanoparticles effect, Operando characterizations, working mechanism

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Authors: Kyung Jin Kim, Jiwon Kwak, Jae-Hoon Lee, Soo Suk Lee

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MicroRNAs (miRNA) are a class of endogenous, single-stranded, small, and non-protein coding RNA molecules typically 20-25 nucleotides long. They are thought to regulate the expression of other genes in a broad range by binding to 3’- untranslated regions (3’-UTRs) of specific mRNAs. The detection of miRNAs is very important for understanding of the function of these molecules and in the diagnosis of variety of human diseases. However, detection of miRNAs is very challenging because of their short length and high sequence similarities within miRNA families. So, a simple-to-use, low-cost, and highly sensitive method for the detection of miRNAs is desirable. In this study, we demonstrate a novel bi-directional extension (BDE) assay. In the first step, a specific linear RT primer is hybridized to 6-10 base pairs from the 3’-end of a target miRNA molecule and then reverse transcribed to generate a cDNA strand. After reverse transcription, the cDNA was hybridized to the 3’-end which is BDE sequence; it played role as the PCR template. The PCR template was amplified in an SYBR green-based quantitative real-time PCR. To prove the concept, we used human brain total RNA. It could be detected quantitatively in the range of seven orders of magnitude with excellent linearity and reproducibility. To evaluate the performance of BDE assay, we contrasted sensitivity and specificity of the BDE assay against a commercially available poly (A) tailing method using miRNAs for let-7e extracted from A549 human epithelial lung cancer cells. The BDE assay displayed good performance compared with a poly (A) tailing method in terms of specificity and sensitivity; the CT values differed by 2.5 and the melting curve showed a sharper than poly (A) tailing methods. We have demonstrated an innovative, cost-effective BDE assay that allows improved sensitivity and specificity in detection of miRNAs. Dynamic range of the SYBR green-based RT-qPCR for miR-145 could be represented quantitatively over a range of 7 orders of magnitude from 0.1 pg to 1.0 μg of human brain total RNA. Finally, the BDE assay for detection of miRNA species such as let-7e shows good performance compared with a poly (A) tailing method in terms of specificity and sensitivity. Thus BDE proves a simple, low cost, and highly sensitive assay for various miRNAs and should provide significant contributions in research on miRNA biology and application of disease diagnostics with miRNAs as targets.

Keywords: bi-directional extension (BDE), microRNA (miRNA), poly (A) tailing assay, reverse transcription, RT-qPCR

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Authors: Shengnan Chen, Shuhua Wang

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Successful production of hydrocarbon from unconventional tight oil reserves has changed the energy landscape in North America. The oil contained within these reservoirs typically will not flow to the wellbore at economic rates without assistance from advanced horizontal well and multi-stage hydraulic fracturing. Efficient and economic development of these reserves is a priority of society, government, and industry, especially under the current low oil prices. Meanwhile, society needs technological and process innovations to enhance oil recovery while concurrently reducing environmental impacts. Recently, big data analysis and artificial intelligence become very popular, developing data-driven insights for better designs and decisions in various engineering disciplines. However, the application of data mining in petroleum engineering is still in its infancy. The objective of this research aims to apply intelligent data analysis and data-driven models to exploit unconventional oil reserves both efficiently and economically. More specifically, a comprehensive database including the reservoir geological data, reservoir geophysical data, well completion data and production data for thousands of wells is firstly established to discover the valuable insights and knowledge related to tight oil reserves development. Several data analysis methods are introduced to analysis such a huge dataset. For example, K-means clustering is used to partition all observations into clusters; principle component analysis is applied to emphasize the variation and bring out strong patterns in the dataset, making the big data easy to explore and visualize; exploratory factor analysis (EFA) is used to identify the complex interrelationships between well completion data and well production data. Different data mining techniques, such as artificial neural network, fuzzy logic, and machine learning technique are then summarized, and appropriate ones are selected to analyze the database based on the prediction accuracy, model robustness, and reproducibility. Advanced knowledge and patterned are finally recognized and integrated into a modified self-adaptive differential evolution optimization workflow to enhance the oil recovery and maximize the net present value (NPV) of the unconventional oil resources. This research will advance the knowledge in the development of unconventional oil reserves and bridge the gap between the big data and performance optimizations in these formations. The newly developed data-driven optimization workflow is a powerful approach to guide field operation, which leads to better designs, higher oil recovery and economic return of future wells in the unconventional oil reserves.

Keywords: big data, artificial intelligence, enhance oil recovery, unconventional oil reserves

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Authors: Veronique Jubera, Ka-Young Kim, U-Chan Chung, Amelie Veillere, Jean-Marc Heintz

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Emitting materials and all solid state lasers are widely used in the field of optical applications and materials science as a source of excitement, instrumental measurements, medical applications, metal shaping etc. Recently promising optical efficiencies were recorded on ceramics which result from a cheaper and faster ways to obtain crystallized materials. The choice and optimization of the sintering process is the key point to fabricate transparent ceramics. It includes a high control on the preparation of the powder with the choice of an adequate synthesis, a pre-heat-treatment, the reproducibility of the sintering cycle, the polishing and post-annealing of the ceramic. The densification is the main factor needed to reach a satisfying transparency, and many technologies are now available. The symmetry of the unit cell plays a crucial role in the diffusion rate of the material. Therefore, the cubic symmetry compounds having an isotropic refractive index is preferred. The cubic Y3NbO7 matrix is an interesting host which can accept a high concentration of rare earth doping element and it has been demonstrated that SPS is an efficient way to sinter this material. The optimization of diffusion losses requires a microstructure of fine ceramics, generally less than one hundred nanometers. In this case, grain growth is not an obstacle to transparency. The ceramics properties are then isotropic thereby to free-shaping step by orienting the ceramics as this is the case for the compounds of lower symmetry. After optimization of the synthesis route, several SPS parameters as heating rate, holding, dwell time and pressure were adjusted in order to increase the densification of the Eu3+ doped Y3NbO7 pellets. The luminescence data coupled with X-Ray diffraction analysis and electronic diffraction microscopy highlight the existence of several distorted environments of the doping element in the studied defective fluorite-type host lattice. Indeed, the fast and high crystallization rate obtained to put in evidence a lack of miscibility in the phase diagram, being the final composition of the pellet driven by the ratio between niobium and yttrium elements. By following the luminescence properties, we demonstrate a direct impact on the SPS process on this material.

Keywords: emission, niobate of rare earth, Spark plasma sintering, lack of miscibility

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Authors: Christelle E. Chua, Alicia L. Ho

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The development of a panel of differential gene expression signatures has been of interest in the field of biomarker discovery for radiation exposure. In the absence of the availability of exposed human subjects, lymphocyte cell lines have often been used as a surrogate to human whole blood, when performing ex vivo irradiation studies. The extent of variation between different lymphocyte cell lines is currently unclear, especially with regard to the expression of extracellular miRNA. This study compares the expression profile of extracellular miRNA isolated from different lymphocyte cell lines. It also compares the profile of miRNA obtained when different exosome isolation kits are used. Lymphocyte cell lines were created using lymphocytes isolated from healthy adult males of similar racial descent (Chinese American and Chinese Singaporean) and immortalised with Epstein-Barr virus. The cell lines were cultured in exosome-free cell culture media for 72h and the cell culture supernatant was removed for exosome isolation. Two exosome isolation kits were used. Total exosome isolation reagent (TEIR, ThermoFisher) is a polyethylene glycol (PEG)-based exosome precipitation kit, while ExoSpin (ES, Cell Guidance Systems) is a PEG-based exosome precipitation kit that includes an additional size exclusion chromatography step. miRNA from the isolated exosomes were isolated using miRNEASY minikit (Qiagen) and analysed using nCounter miRNA assay (Nanostring). Principal component analysis (PCA) results suggested that the overall extracellular miRNA expression profile differed between the lymphocyte cell line originating from the Chinese American donor and the cell line originating from the Chinese Singaporean donor. As the gender, age and racial origins of both donors are similar, this may suggest that there are other genetic or epigenetic differences that account for the variation in extracellular miRNA gene expression in lymphocyte cell lines. However, statistical analysis showed that only 3 miRNA genes had a fold difference > 2 at p < 0.05, suggesting that the differences may not be of that great a significance as to impact overall conclusions drawn from different cell lines. Subsequent analysis using cell lines from other donors will give further insight into the reproducibility of results when difference cell lines are used. PCA results also suggested that the method of exosome isolation impacted the expression profile. 107 miRNA had a fold difference > 2 at p < 0.05. This suggests that the inclusion of an additional size exclusion chromatography step altered the subset of the extracellular vesicles that were isolated. In conclusion, these results suggest that extracellular miRNA can be isolated and analysed from exosomes derived from lymphocyte cell lines. However, care must be taken in the choice of cell line and method of exosome isolation used.

Keywords: biomarker, extracellular miRNA, isolation methods, lymphocyte cell line

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Authors: Kim Norgaard Helmersen, Jan Silberberger

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Questions of style and reproducibility in relation to architectural design are not only continuously debated; the very concepts can seem quite provocative to architects, who like to think of architectural design as depending on intuition, ideas, and individual personalities. This standpoint - dominant in architectural discourse - is challenged in the present paper presenting early findings from a comparative STS-inspired research study of architectural design teaching and research at different architecture schools in varying national contexts. In philosophy of science framework, the paper reflects empirical observations of design teaching at the Royal Academy of Fine Arts in Copenhagen and presents a tentative theoretical framework for the on-going research project. The framework suggests that architecture – as a field of knowledge production – is mainly dominated by three epistemological positions, which will be presented and discussed. Besides serving as a loosely structured framework for future data analysis, the proposed framework brings forth the argument that architecture can be roughly divided into different schools of thought, like the traditional science disciplines. Without reducing the complexity of the discipline, describing its main intellectual positions should prove fruitful for the future development of architecture as a theoretical discipline, moving an architectural critique beyond discussions of taste preferences. Unlike traditional science disciplines, there is a lack of a community-wide, shared pool of codified references in architecture, with architects instead referencing art projects, buildings, and famous architects, when positioning their standpoints. While these inscriptions work as an architectural reference system, to be compared to codified theories in academic writing of traditional research, they are not used systematically in the same way. As a result, architectural critique is often reduced to discussions of taste and subjectivity rather than epistemological positioning. Architects are often criticized as judges of taste and accused that their rationality is rooted in cultural-relative aesthetical concepts of taste closely linked to questions of style, but arguably their supposedly subjective reasoning, in fact, forms part of larger systems of thought. Putting architectural ‘styles’ under a loop, and tracing their philosophical roots, can potentially open up a black box in architectural theory. Besides ascertaining and recognizing the existence of specific ‘styles’ and thereby schools of thought in current architectural discourse, the study could potentially also point at some mutations of the conventional – something actually ‘new’ – of potentially high value for architectural design education.

Keywords: architectural theory, design research, science and technology studies (STS), sociology of architecture

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Authors: Norazlan Mohmad Misnan, Maizatul Hasyima Omar, Mohd Isa Wasiman

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Papaya (Carica papaya L., Caricaceae) is a tree which mainly cultivated for its fruits in many tropical regions including Australia, Brazil, China, Hawaii, and Malaysia. Beside of fruits, its leaves, seeds, and latex have also been traditionally used for treating diseases, which also reported to possess anti-cancer and anti- malaria properties. Its leaves have been reported to consist of various chemical compounds such as alkaloids, flavonoids and phenolics. Clitorin and manghaslin are among major flavonoids presence. Thus, the aim of this study is to quantify the purity of these isolated compounds (clitorin and manghsalin) by using quantitative Nuclear Magnetic Resonance (qNMR) analysis. Only fresh C. papaya leaves were used for juice extraction procedure and subsequently was freeze-dried to obtain a dark green powdered form of the extract prior to Centrifugal Partition Chromatography (CPC) separation. The CPC experiments were performed using a two-phase solvent system comprising ethyl acetate/butanol/water (1:4:5, v/v/v/v) solvent. The upper organic phase was used as the stationary phase, and the lower aqueous phase was employed as the mobile phase. Ten fractions were obtained after an hour runtime analysis. Fraction 6 and fraction 8 has been identified as clitorin (m/z 739.21 [M-H]-) and manghaslin (m/z 755.21 [M-H]-), respectively, based on LCMS data and full analysis of NMR (1H NMR, 13C NMR, HMBC, and HSQC). The 1H-qNMR measurements were carried out using a 400 MHz NMR spectrometer (JEOL ECS 400MHz, Japan) and deuterated methanol was used as a solvent. Quantification was performed using the AQARI method (Accurate Quantitative NMR) with deuterated 1,4-Bis(trimethylsilyl)benzene (BTMSB) as an internal reference substances. This AQARI protocol includes not only NMR measurement but also sample preparation that provide highest precision and accuracy than other qNMR methods. The 90° pulse length and the T1 relaxation times for compounds and BTMSB were determined prior to the quantification to give the best signal-to-noise ratio. Regions containing the two downfield signals from aromatic part (6.00–6.89 ppm), and the singlet signal, (18H) arising from BTMSB (0.63-1.05ppm) were selected for integration. The purity of clitorin and manghaslin were calculated to be 52.22% and 43.36%, respectively. Further purification is needed in order to increase its purity. This finding has demonstrated the use of qNMR for quality control and standardization of various plant extracts and which can be applied for NMR fingerprinting of other plant-based products with good reproducibility and in the case where commercial standards is not readily available.

Keywords: Carica papaya, clitorin, manghaslin, quantitative Nuclear Magnetic Resonance, Centrifugal Partition Chromatography

Procedia PDF Downloads 496

Authors: Lenon M. Pereira, Helen J. Khoury, Marcos E. A. Andrade, Dean L. Cutajar, Vinicius S. M. Barros, Anatoly B. Rozenfeld

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With the increase of beam widths and the advent of multiple-slice and helical scanners, concerns related to the current dose measurement protocols and instrumentation in computed tomography (CT) have arisen. The current methodology of dose evaluation, which is based on the measurement of the integral of a single slice dose profile using a 100 mm long cylinder ionization chamber (Ca,100 and CPPMA, 100), has been shown to be inadequate for wide beams as it does not collect enough of the scatter-tails to make an accurate measurement. In addition, a long ionization chamber does not offer a good representation of the dose profile when tube current modulation is used. An alternative approach has been suggested by translating smaller detectors through the beam plane and assessing the accumulated dose trough the integral of the dose profile, which can be done for any arbitrary length in phantoms or in the air. For this purpose, a MOSFET dosimeter of small dosimetric volume was used. One of its recently designed versions is known as the MOSkin, which is developed by the Centre for Medical Radiation Physics at the University of Wollongong, and measures the radiation dose at a water equivalent depth of 0.07 mm, allowing the evaluation of skin dose when placed at the surface, or internal point doses when placed within a phantom. Thus, the aim of this research was to characterize the response of the MOSkin dosimeter for X-ray CT beams and to evaluate its application for the accumulated dose assessment. Initially, tests using an industrial x-ray unit were carried out at the Laboratory of Ionization Radiation Metrology (LMRI) of Federal University of Pernambuco, in order to investigate the sensitivity, energy dependence, angular dependence, and reproducibility of the dose response for the device for the standard radiation qualities RQT 8, RQT 9 and RQT 10. Finally, the MOSkin was used for the accumulated dose evaluation of scans using a Philips Brilliance 6 CT unit, with comparisons made between the CPPMA,100 value assessed with a pencil ionization chamber (PTW Freiburg TW 30009). Both dosimeters were placed in the center of a PMMA head phantom (diameter of 16 cm) and exposed in the axial mode with collimation of 9 mm, 250 mAs and 120 kV. The results have shown that the MOSkin response was linear with doses in the CT range and reproducible (98.52%). The sensitivity for a single MOSkin in mV/cGy was as follows: 9.208, 7.691 and 6.723 for the RQT 8, RQT 9 and RQT 10 beams qualities respectively. The energy dependence varied up to a factor of ±1.19 among those energies and angular dependence was not greater than 7.78% within the angle range from 0 to 90 degrees. The accumulated dose and the CPMMA, 100 value were 3,97 and 3,79 cGy respectively, which were statistically equivalent within the 95% confidence level. The MOSkin was shown to be a good alternative for CT dose profile measurements and more than adequate to provide accumulated dose assessments for CT procedures.

Keywords: computed tomography dosimetry, MOSFET, MOSkin, semiconductor dosimetry

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Authors: Marine Regnier, Pascal Bost, Matthieu Horgnies

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Some of the problems to be solved for the concrete industry are linked to the use of low-reactivity cement, the hardening of concrete under cold-weather and the manufacture of pre-casted concrete without costly heating step. The development of these applications needs to accelerate the hydration kinetics, in order to decrease the setting time and to obtain significant compressive strengths as soon as possible. The mechanisms enhancing the hydration kinetics of alite or Portland cement (e.g. the creation of nucleation sites) were already studied in literature (e.g. by using distinct additions such as titanium dioxide nanoparticles, calcium carbonate fillers, water-soluble polymers, C-S-H, etc.). However, the goal of this study was to establish a clear ranking of the efficiency of several types of additions by using a robust and reproducible methodology based on isothermal calorimetry (performed at 20°C). The cement was a CEM I 52.5N PM-ES (Blaine fineness of 455 m²/kg). To ensure the reproducibility of the experiments and avoid any decrease of the reactivity before use, the cement was stored in waterproof and sealed bags to avoid any contact with moisture and carbon dioxide. The experiments were performed on Portland cement pastes by using a water-to-cement ratio of 0.45, and incorporating different compounds (industrially available or laboratory-synthesized) that were selected according to their main composition and their specific surface area (SSA, calculated using the Brunauer-Emmett-Teller (BET) model and nitrogen adsorption isotherms performed at 77K). The intrinsic effects of (i) dry powders (e.g. fumed silica, activated charcoal, nano-precipitates of calcium carbonate, afwillite germs, nanoparticles of iron and iron oxides , etc.), and (ii) aqueous solutions (e.g. containing calcium chloride, hydrated Portland cement or Master X-SEED 100, etc.) were investigated. The influence of the amount of addition, calculated relatively to the dry extract of each addition compared to cement (and by conserving the same water-to-cement ratio) was also studied. The results demonstrated that the X-SEED®, the hydrated calcium nitrate, the calcium chloride (and, at a minor level, a solution of hydrated Portland cement) were able to accelerate the hydration kinetics of Portland cement, even at low concentration (e.g. 1%wt. of dry extract compared to cement). By using higher rates of additions, the fumed silica, the precipitated calcium carbonate and the titanium dioxide can also accelerate the hydration. In the case of the nano-precipitates of calcium carbonate, a correlation was established between the SSA and the accelerating effect. On the contrary, the nanoparticles of iron or iron oxides, the activated charcoal and the dried crystallised hydrates did not show any accelerating effect. Future experiments will be scheduled to establish the ranking of these additions, in terms of accelerating effect, by using low-reactivity cements and other water to cement ratios.

Keywords: acceleration, hydration kinetics, isothermal calorimetry, Portland cement

Procedia PDF Downloads 256

Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

Procedia PDF Downloads 148

Authors: Irina Veselova, Maria Makedonskaya, Olga Eremina, Alexandr Sidorov, Eugene Goodilin, Tatyana Shekhovtsova

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Such catecholamines as dopamine, norepinephrine, and epinephrine are the principal neurotransmitters in the sympathetic nervous system. Catecholamines and their metabolites are considered to be important markers of socially significant diseases such as atherosclerosis, diabetes, coronary heart disease, carcinogenesis, Alzheimer's and Parkinson's diseases. Currently, neurotransmitters can be studied via electrochemical and chromatographic techniques that allow their characterizing and quantification, although these techniques can only provide crude spatial information. Besides, the difficulty of catecholamine determination in biological materials is associated with their low normal concentrations (~ 1 nM) in biomaterials, which may become even one more order lower because of some disorders. In addition, in blood they are rapidly oxidized by monoaminooxidases from thrombocytes and, for this reason, the determination of neurotransmitter metabolism indicators in an organism should be very rapid (15—30 min), especially in critical states. Unfortunately, modern instrumental analysis does not offer a complex solution of this problem: despite its high sensitivity and selectivity, HPLC-MS cannot provide sufficiently rapid analysis, while enzymatic biosensors and immunoassays for the determination of the considered analytes lack sufficient sensitivity and reproducibility. Fluorescent and SERS-sensors remain a compelling technology for approaching the general problem of selective neurotransmitter detection. In recent years, a number of catecholamine sensors have been reported including RNA aptamers, fluorescent ribonucleopeptide (RNP) complexes, and boronic acid based synthetic receptors and the sensor operated in a turn-off mode. In this work we present the fluorescent and SERS turn-on sensor systems based on the bio- or chemorecognizing nanostructured films {chitosan/collagen-Tb/Eu/Cu-nanoparticles-indicator reagents} that provide the selective recognition, visualization, and sensing of the above mentioned catecholamines on the level of nanomolar concentrations in biomaterials (cell cultures, tissue etc.). We have (1) developed optically transparent porous films and gels of chitosan/collagen; (2) ensured functionalization of the surface by molecules-'recognizers' (by impregnation and immobilization of components of the indicator systems: biorecognizing and auxiliary reagents); (3) performed computer simulation for theoretical prediction and interpretation of some properties of the developed materials and obtained analytical signals in biomaterials. We are grateful for the financial support of this research from Russian Foundation for Basic Research (grants no. 15-03-05064 a, and 15-29-01330 ofi_m).

Keywords: biomaterials, fluorescent and SERS-recognition, neurotransmitters, solid-phase turn-on sensor system

Procedia PDF Downloads 406

Authors: Alberto Sanchidrián, José A. Parra, Jesús Alonso, Julián Pecharromán, Antonia Pacios, Consuelo Huerta

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Glass is a commonly used material in building; there is not a unique design solution as plates with a different number of layers and interlayers may be used. In most façades, a security glazing have to be used according to its performance in the impact pendulum. The European Standard EN 12600 establishes an impact test procedure for classification under the point of view of the human security, of flat plates with different thickness, using a pendulum of two tires and 50 kg mass that impacts against the plate from different heights. However, this test does not replicate the actual dimensions and border conditions used in building configurations and so the real stress distribution is not determined with this test. The influence of different boundary conditions, as the ones employed in construction sites, is not well taking into account when testing the behaviour of safety glazing and there is not a detailed procedure and criteria to determinate the glass resistance against human impact. To reproduce the actual boundary conditions on site, when needed, the pendulum test is arranged to be used "in situ", with no account for load control, stiffness, and without a standard procedure. Fracture stress of small and large glass plates fit a Weibull distribution with quite a big dispersion so conservative values are adopted for admissible fracture stress under static loads. In fact, test performed for human impact gives a fracture strength two or three times higher, and many times without a total fracture of the glass plate. Newest standards, as for example DIN 18008-4, states for an admissible fracture stress 2.5 times higher than the ones used for static and wing loads. Now two working areas are open: a) to define a standard for the ‘in situ’ test; b) to prepare a laboratory procedure that allows testing with more real stress distribution. To work on both research lines a laboratory that allows to test medium size specimens with different border conditions, has been developed. A special steel frame allows reproducing the stiffness of the glass support substructure, including a rigid condition used as reference. The dynamic behaviour of the glass plate and its support substructure have been characterized with finite elements models updated with modal tests results. In addition, a new portable impact machine is being used to get enough force and direction control during the impact test. Impact based on 100 J is used. To avoid problems with broken glass plates, the test have been done using an aluminium plate of 1000 mm x 700 mm size and 10 mm thickness supported on four sides; three different substructure stiffness conditions are used. A detailed control of the dynamic stiffness and the behaviour of the plate is done with modal tests. Repeatability of the test and reproducibility of results prove that procedure to control both, stiffness of the plate and the impact level, is necessary.

Keywords: glass plates, human impact test, modal test, plate boundary conditions

Procedia PDF Downloads 307

Authors: Ayten Ekin Meşe, Selahattin Şentürk, Melike Duvanoğlu

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Petroleum refineries are a highly complex process industry with continuous production and high operating costs. Physical separation of crude oil starts with the crude oil distillation unit, continues with various conversion and purification units, and passes through many stages until obtaining the final product. To meet the desired product specification, process parameters are strictly followed. To be able to ensure the quality of distillates, routine analyses are performed in quality control laboratories based on appropriate international standards such as American Society for Testing and Materials (ASTM) standard methods and European Standard (EN) methods. The cut point of distillates in the crude distillation unit is very crucial for the efficiency of the upcoming processes. In order to maximize the process efficiency, the determination of the quality of distillates should be as fast as possible, reliable, and cost-effective. In this sense, an alternative study was carried out on the crude oil distillation unit that serves the entire refinery process. In this work, studies were conducted with three different crude oil distillates which are Light Straight Run Naphtha (LSRN), Heavy Straight Run Naphtha (HSRN), and Kerosene. These products are named after separation by the number of carbons it contains. LSRN consists of five to six carbon-containing hydrocarbons, HSRN consist of six to ten, and kerosene consists of sixteen to twenty-two carbon-containing hydrocarbons. Physical properties of three different crude distillation unit products (LSRN, HSRN, and Kerosene) were determined using Near-Infrared Spectroscopy with multivariate calibration. The absorbance spectra of the petroleum samples were obtained in the range from 10000 cm⁻¹ to 4000 cm⁻¹, employing a quartz transmittance flow through cell with a 2 mm light path and a resolution of 2 cm⁻¹. A total of 400 samples were collected for each petroleum sample for almost four years. Several different crude oil grades were processed during sample collection times. Extended Multiplicative Signal Correction (EMSC) and Savitzky-Golay (SG) preprocessing techniques were applied to FT-NIR spectra of samples to eliminate baseline shifts and suppress unwanted variation. Two different multivariate calibration approaches (Partial Least Squares Regression, PLS and Genetic Inverse Least Squares, GILS) and an ensemble model were applied to preprocessed FT-NIR spectra. Predictive performance of each multivariate calibration technique and preprocessing techniques were compared, and the best models were chosen according to the reproducibility of ASTM reference methods. This work demonstrates the developed models can be used for routine analysis instead of conventional analytical methods with over 90% accuracy.

Keywords: crude distillation unit, multivariate calibration, near infrared spectroscopy, data preprocessing, refinery

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Authors: B. B. S. Pereira, M. O. Souza, L. P. Zanetti, L. C. S. Oliveira, J. R. P. Moreno, M. P. Souza, V. R. Colturato, C. M. Machado

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Background: The introduction of prophylactic or preemptive therapies has effectively decreased the CMV mortality rates after hematopoietic stem cell transplantation (HSCT). CMV antigenemia (pp65) or quantitative PCR are methods currently approved for CMV surveillance in pre-emptive strategies. Commercial assays are preferred as cut-off levels defined by in-house assays may vary among different protocols and in general show low reproducibility. Moreover, comparison of published data among different centers is only possible if international standards of quantification are included in the assays. Recently, the World Health Organization (WHO) established the first international standard for CMV detection. The real time PCR COBAS Ampliprep/ CobasTaqMan (CAP/CTM) (Roche®) was developed using the WHO standard for CMV quantification. However, the cut-off for the introduction of antiviral has not been determined yet. Methods: We conducted a retrospective study to determine: 1) the sensitivity and specificity of the new CMV CAP/CTM test in comparison with pp65 antigenemia to detect episodes of CMV infection/reactivation, and 2) the cut-off of viral load for introduction of ganciclovir (GCV). Pp65 antigenemia was performed and the corresponding plasma samples were stored at -20°C for further CMV detection by CAP/CTM. Comparison of tests was performed by kappa index. The appearance of positive antigenemia was considered the state variable to determine the cut-off of CMV viral load by ROC curve. Statistical analysis was performed using SPSS software version 19 (SPSS, Chicago, IL, USA.). Results: Thirty-eight patients were included and followed from August 2014 through May 2015. The antigenemia test detected 53 episodes of CMV infection in 34 patients (89.5%), while CAP/CTM detected 37 episodes in 33 patients (86.8%). AG and PCR results were compared in 431 samples and Kappa index was 30.9%. The median time for first AG detection was 42 (28-140) days, while CAP/CTM detected at a median of 7 days earlier (34 days, ranging from 7 to 110 days). The optimum cut-off value of CMV DNA was 34.25 IU/mL to detect positive antigenemia with 88.2% of sensibility, 100% of specificity and AUC of 0.91. This cut-off value is below the limit of detection and quantification of the equipment which is 56 IU/mL. According to CMV recurrence definition, 16 episodes of CMV recurrence were detected by antigenemia (47.1%) and 4 (12.1%) by CAP/CTM. The duration of viremia as detected by antigenemia was shorter (60.5% of the episodes lasted ≤ 7 days) in comparison to CAP/CTM (57.9% of the episodes lasting 15 days or more). This data suggests that the use of antigenemia to define the duration of GCV therapy might prompt early interruption of antiviral, which may favor CMV reactivation. The CAP/CTM PCR could possibly provide a safer information concerning the duration of GCV therapy. As prolonged treatment may increase the risk of toxicity, this hypothesis should be confirmed in prospective trials. Conclusions: Even though CAP/CTM by ROCHE showed great qualitative correlation with the antigenemia technique, the fully automated CAP/CTM did not demonstrate increased sensitivity. The cut-off value below the limit of detection and quantification may result in delayed introduction of pre-emptive therapy.

Keywords: antigenemia, CMV COBAS/TAQMAN, cytomegalovirus, antiviral cut-off

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Authors: Olga Yu Kurapova, Alexander V. Shorokhov, Vladimir G. Konakov

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Nowadays, due to their exceptional anion conductivity at high temperatures cubic zirconia solid solutions, stabilized by rare-earth and alkaline-earth metal oxides, are widely used as a solid electrolyte (SE) materials in different electrochemical devices such as gas sensors, oxygen pumps, solid oxide fuel cells (SOFC), etc. Nowadays the intensive studies are carried out in a field of novel fully stabilized zirconia based SE development. The use of precursor powders for SE manufacturing allows predetermining the microstructure, electrical and sensor characteristics of zirconia based ceramics used as SE. Thus the goal of the present work was the investigation of the effect of precursor powder size on the electrical and sensor characteristics of fully stabilized zirconia-based solid electrolytes with compositions of 0,08Y2O3∙0,92ZrO2 (YSZ), 0,06Ce2O3∙ 0,06Y2O3∙0,88ZrO2 and 0,09Ce2O3∙0,06Y2O3-0,85ZrO2. The synthesis of precursors powders with different mean particle size was performed by sol-gel synthesis in the form of reversed co-precipitation from aqueous solutions. The cakes were washed until the neutral pH and pan-dried at 110 °С. Also, YSZ ceramics was obtained by conventional solid state synthesis including milling into a planetary mill. Then the powder was cold pressed into the pellets with a diameter of 7.2 and ~4 mm thickness at P ~16 kg/cm2 and then hydrostatically pressed. The pellets were annealed at 1600 °С for 2 hours. The phase composition of as-synthesized SE was investigated by X-Ray photoelectron spectroscopy ESCA (spectrometer ESCA-5400, PHI) X-ray diffraction analysis - XRD (Shimadzu XRD-6000). Following galvanic cell О2 (РО2(1)), Pt | SE | Pt, (РО2(2) = 0.21 atm) was used for SE sensor properties investigation. The value of РО2(1) was set by mixing of O2 and N2 in the defined proportions with the accuracy of  5%. The temperature was measured by Pt/Pt-10% Rh thermocouple, The cell electromotive force (EMF) measurement was carried out with ± 0.1 mV accuracy. During the operation at the constant temperature, reproducibility was better than 5 mV. Asymmetric potential measured for all SE appeared to be negligible. It was shown that the resistivity of YSZ ceramics decreases in about two times upon the mean agglomerates decrease from 200-250 to 40 nm. It is likely due to the both surface and bulk resistivity decrease in grains. So the overall decrease of grain size in ceramic SE results in the significant decrease of the total ceramics resistivity allowing sensor operation at lower temperatures. For the SE manufactured the estimation of oxygen ion transfer number tion was carried out in the range 600-800 °С. YSZ ceramics manufactured from powders with the mean particle size 40-140 nm, shows the highest values i.e. 0.97-0.98. SE manufactured from precursors with the mean particle size 40-140 nm shows higher sensor characteristic i.e. temperature and oxygen concentration EMF dependencies, EMF (ENernst - Ereal), tion, response time, then ceramics, manufactured by conventional solid state synthesis.

Keywords: oxygen sensors, precursor powders, sol-gel synthesis, stabilized zirconia ceramics

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Authors: C. A. Barros, Ana P. Barroso

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Any industrial company needs to determine the amount of variation that exists within its measurement process and guarantee the reliability of their data, studying the performance of their measurement system, in terms of linearity, bias, repeatability and reproducibility and stability. This issue is critical for automotive industry suppliers, who are required to be certified by the 16949:2016 standard (replaces the ISO/TS 16949) of International Automotive Task Force, defining the requirements of a quality management system for companies in the automotive industry. Measurement System Analysis (MSA) is one of the mandatory tools. Frequently, the measurement system in companies is not connected to the equipment and do not incorporate the methods proposed by the Automotive Industry Action Group (AIAG). To address these constraints, an R&D project is in progress, whose objective is to develop a web and cloud-based MSA tool. This MSA tool incorporates Industry 4.0 concepts, such as, Internet of Things (IoT) protocols to assure the connection with the measuring equipment, cloud computing, artificial intelligence, statistical tools, and advanced mathematical algorithms. This paper presents the preliminary findings of the project. The web and cloud-based MSA tool is innovative because it implements all statistical tests proposed in the MSA-4 reference manual from AIAG as well as other emerging methods and techniques. As it is integrated with the measuring devices, it reduces the manual input of data and therefore the errors. The tool ensures traceability of all performed tests and can be used in quality laboratories and in the production lines. Besides, it monitors MSAs over time, allowing both the analysis of deviations from the variation of the measurements performed and the management of measurement equipment and calibrations. To develop the MSA tool a ten-step approach was implemented. Firstly, it was performed a benchmarking analysis of the current competitors and commercial solutions linked to MSA, concerning Industry 4.0 paradigm. Next, an analysis of the size of the target market for the MSA tool was done. Afterwards, data flow and traceability requirements were analysed in order to implement an IoT data network that interconnects with the equipment, preferably via wireless. The MSA web solution was designed under UI/UX principles and an API in python language was developed to perform the algorithms and the statistical analysis. Continuous validation of the tool by companies is being performed to assure real time management of the ‘big data’. The main results of this R&D project are: MSA Tool, web and cloud-based; Python API; New Algorithms to the market; and Style Guide of UI/UX of the tool. The MSA tool proposed adds value to the state of the art as it ensures an effective response to the new challenges of measurement systems, which are increasingly critical in production processes. Although the automotive industry has triggered the development of this innovative MSA tool, other industries would also benefit from it. Currently, companies from molds and plastics, chemical and food industry are already validating it.

Keywords: automotive Industry, industry 4.0, Internet of Things, IATF 16949:2016, measurement system analysis

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Authors: Mitali Saha, Soma Das

Abstract:

The fabrication of nanoscale materials for use in chemical sensing, biosensing and biological analyses has proven a promising avenue in the last few years. Cholesterol has aroused considerable interest in recent years on account of its being an important parameter in clinical diagnosis. There is a strong positive correlation between high serum cholesterol level and arteriosclerosis, hypertension, and myocardial infarction. Enzyme-based electrochemical biosensors have shown high selectivity and excellent sensitivity, but the enzyme is easily denatured during its immobilization procedure and its activity is also affected by temperature, pH, and toxic chemicals. Besides, the reproducibility of enzyme-based sensors is not very good which further restrict the application of cholesterol biosensor. It has been demonstrated that carbon nanotubes could promote electron transfer with various redox active proteins, ranging from cytochrome c to glucose oxidase with a deeply embedded redox center. In continuation of our earlier work on the synthesis and applications of carbon and metal based nanoparticles, we have reported here the synthesis of carbon nanotubes (CCNT) by burning coconut oil under insufficient flow of air using an oil lamp. The soot was collected from the top portion of the flame, where the temperature was around 6500C which was purified, functionalized and then characterized by SEM, p-XRD and Raman spectroscopy. The SEM micrographs showed the formation of tubular structure of CCNT having diameter below 100 nm. The XRD pattern indicated the presence of two predominant peaks at 25.20 and 43.80, which corresponded to (002) and (100) planes of CCNT respectively. The Raman spectrum (514 nm excitation) showed the presence of 1600 cm-1 (G-band) related to the vibration of sp2-bonded carbon and at 1350 cm-1 (D-band) responsible for the vibrations of sp3-bonded carbon. A nonenzymatic cholesterol biosensor was then fabricated on an insulating Teflon material containing three silver wires at the surface, covered by CCNT, obtained from coconut oil. Here, CCNTs worked as working as well as counter electrodes whereas reference electrode and electric contacts were made of silver. The dimensions of the electrode was 3.5 cm×1.0 cm×0.5 cm (length× width × height) and it is ideal for working with 50 µL volume like the standard screen printed electrodes. The voltammetric behavior of cholesterol at CCNT electrode was investigated by cyclic voltammeter and differential pulse voltammeter using 0.001 M H2SO4 as electrolyte. The influence of the experimental parameters on the peak currents of cholesterol like pH, accumulation time, and scan rates were optimized. Under optimum conditions, the peak current was found to be linear in the cholesterol concentration range from 1 µM to 50 µM with a sensitivity of ~15.31 μAμM−1cm−2 with lower detection limit of 0.017 µM and response time of about 6s. The long-term storage stability of the sensor was tested for 30 days and the current response was found to be ~85% of its initial response after 30 days.

Keywords: coconut oil, CCNT, cholesterol, biosensor

Procedia PDF Downloads 282

Authors: Stephanie P. Nigro

Abstract:

The Exhale Breath Hold (EBH) technique presents a promising approach to enhance the precision and efficacy of External Beam Radiation Therapy (EBRT) for abdominal tumours, which include liver, pancreas, kidney, and adrenal glands. These tumours are challenging to treat due to their proximity to organs at risk (OARs) and the significant motion induced by respiration and physiological variations, such as stomach filling. Respiratory motion can cause up to 40mm of displacement in abdominal organs, complicating accurate targeting. While current practices like limiting fasting help reduce motion related to digestive processes, they do not address respiratory motion. 4DCT scans are used to assess this motion, but they require extensive workflow time and expose patients to higher doses of radiation. The EBH technique, which involves holding the breath in an exhale with no air in the lungs, stabilizes internal organ motion, thereby reducing respiratory-induced motion. The primary benefit of EBH is the reduction in treatment volume sizes, specifically the Internal Target Volume (ITV) and Planning Target Volume (PTV), as demonstrated by smaller ITVs when gated in EBH. This reduction also improves the quality of 3D Cone Beam CT (CBCT) images by minimizing respiratory artifacts, facilitating soft tissue matching akin to stereotactic treatments. Patients suitable for EBH must meet criteria including the ability to hold their breath for at least 15 seconds and maintain a consistent breathing pattern. For those who do not qualify, the traditional 4DCT protocol will be used. The implementation involves an EBH planning scan and additional short EBH scans to ensure reproducibility and assist in contouring and volume expansions, with a Free Breathing (FB) scan used for setup purposes. Treatment planning on EBH scans leads to smaller PTVs, though intrafractional and interfractional breath hold variations must be accounted for in margins. The treatment decision process includes performing CBCT in EBH intervals, with careful matching and adjustment based on soft tissue and fiducial markers. Initial studies at two sites will evaluate the necessity of multiple CBCTs, assessing shifts and the benefits of initial versus mid-treatment CBCT. Considerations for successful implementation include thorough patient coaching, staff training, and verification of breath holds, despite potential disadvantages such as longer treatment times and patient exhaustion. Overall, the EBH technique offers significant improvements in the accuracy and quality of abdominal EBRT, paving the way for more effective and safer treatments for patients.

Keywords: abdominal cancers, exhale breath hold, radiation therapy, respiratory motion

Procedia PDF Downloads 26

Authors: M. Shiva Prasad, S. R. Atchuta, T. Vijayaraghavan, S. Sakthivel

Abstract:

The world is in need of efficient energy conversion technologies which are affordable, accessible, and sustainable with eco-friendly nature. Solar energy is one of the cornerstones for the world’s economic growth because of its abundancy with zero carbon pollution. Among the various solar energy conversion technologies, solar thermal technology has attracted a substantial renewed interest due to its diversity and compatibility in various applications. Solar thermal systems employ concentrators, tracking systems and heat engines for electricity generation which lead to high cost and complexity in comparison with photovoltaics; however, it is compatible with distinct thermal energy storage capability and dispatchable electricity which creates a tremendous attraction. Apart from that, employing cost-effective solar selective receiver tube in a concentrating solar thermal (CST) system improves the energy conversion efficiency and directly reduces the cost of technology. In addition, the development of solar receiver tubes by low cost methods which can offer high optical properties and corrosion resistance in an open-air atmosphere would be beneficial for low and medium temperature applications. In this regard, our work opens up an approach which has the potential to achieve cost-effective energy conversion. We have developed a highly selective tandem absorber coating through a facile wet chemical route by a combination of chemical oxidation, sol-gel, and nanoparticle coating methods. The developed tandem absorber coating has gradient refractive index nature on stainless steel (SS 304) and exhibited high optical properties (α ≤ 0.95 & ε ≤ 0.14). The first absorber layer (Cr-Mn-Fe oxides) developed by controlled oxidation of SS 304 in a chemical bath reactor. A second composite layer of ZrO₂-SiO₂ has been applied on the chemically oxidized substrate by So-gel dip coating method to serve as optical enhancing and corrosion resistant layer. Finally, an antireflective layer (MgF₂) has been deposited on the second layer, to achieve > 95% of absorption. The developed tandem layer exhibited good thermal stability up to 250 °C in open air atmospheric condition and superior corrosion resistance (withstands for > 200h in salt spray test (ASTM B117)). After the successful development of a coating with targeted properties at a laboratory scale, a prototype of the 1 m tube has been demonstrated with excellent uniformity and reproducibility. Moreover, it has been validated under standard laboratory test condition as well as in field condition with a comparison of the commercial receiver tube. The presented strategy can be widely adapted to develop highly selective coatings for a variety of CST applications ranging from hot water, solar desalination, and industrial process heat and power generation. The high-performance, cost-effective medium temperature receiver tube technology has attracted many industries, and recently the technology has been transferred to Indian industry.

Keywords: concentrated solar thermal system, solar selective coating, tandem absorber, ultralow refractive index

Procedia PDF Downloads 89