Effects of experimental conditions on the determination of the effective carbon number

2003 ◽  
Vol 57 (9-10) ◽  
pp. 639-644 ◽  
Author(s):  
M. Kállai ◽  
V. Máté ◽  
J. Balla
Keyword(s):  
Carbon Number ◽  
Experimental Conditions

Antithrombin-mediated Inhibition of Factor Vlla-Tissue Factor Complex by the Synthetic Pentasaccharide Representing the Heparin Binding Site to Antithrombin

1996 ◽  
Vol 76 (01) ◽  
pp. 005-008 ◽  
Author(s):  
Jean Claude Lormeau ◽  
Jean Pascal Herault ◽  
Jean Marc Herbert
Keyword(s):  
Binding Site ◽  
Tissue Factor ◽  
Residual Activity ◽  
Coagulation Factors ◽  
Heparin Binding ◽  
Experimental Conditions ◽  
First Order ◽  
Heparin Binding Site ◽  
Coagulant Activity

SummaryWe examined the effect of the synthetic pentasaccharide representing the minimal binding site of heparin to antithrombin on the antithrombin-mediated inactivation of factor Vila bound to tissue factor. This effect was compared to the effect of unfractionated heparin. Using purified recombinant human coagulation factors and either a clotting or an amidolytic assay for the determination of the residual activity of factor Vila, we showed that the pentasaccharide was an efficient antithrombin-dependent inhibitor of the coagulant activity of tissue factor-factor Vila complex. In our experimental conditions, assuming a mean MW of 14,000 for heparin, the molar pseudo-first order rate constants for ATIII-mediated FVIIa inhibition by ATIII-binding heparin and by the synthetic pentasaccharide were found to be similar with respective values of 104,000 ± 10,500 min-1 and 112,000 ± 12,000 min-1 (mean ± s.e.m., n = 3)

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

scholarly journals Software-guided microscale flow calorimeter for efficient acquisition of thermokinetic data

2021 ◽  
Author(s):  
Timothy Aljoscha Frede ◽  
Marlene Dietz ◽  
Norbert Kockmann
Keyword(s):  
Design Of Experiments ◽  
Process Development ◽  
Reaction Conditions ◽  
Experimental Conditions ◽  
Flow Calorimeter ◽  
Microscale Flow ◽  
Increased Sensitivity ◽  
Important Time ◽  
Optimal Reaction

AbstractFast chemical process development is inevitably linked to an optimized determination of thermokinetic data of chemical reactions. A miniaturized flow calorimeter enables increased sensitivity when examining small amounts of reactants in a short time compared to traditional batch equipment. Therefore, a methodology to determine optimal reaction conditions for calorimetric measurement experiments was developed and is presented in this contribution. Within the methodology, short-cut calculations are supplemented by computational fluid dynamics (CFD) simulations for a better representation of the hydrodynamics within the microreactor. This approach leads to the effective design of experiments. Unfavourable experimental conditions for kinetics experiments are determined in advance and therefore, need not to be considered during design of experiments. The methodology is tested for an instantaneous acid-base reaction. Good agreement of simulations was obtained with experimental data. Thus, the prediction of the hydrodynamics is enabled and the first steps towards a digital twin of the calorimeter are performed. The flow rates proposed by the methodology are tested for the determination of reaction enthalpy and showed that reasonable experimental settings resulted. Graphical abstract A methodology is suggested to evaluate optimal reaction conditions for efficientacquisition of kinetic data. The experimental design space is limited by thestepwise determination of important time scales based on specified input data.

scholarly journals Apparent Young’s Modulus of the Adhesive in Numerical Modeling of Adhesive Joints

Materials ◽  
2021 ◽  
Vol 14 (2) ◽  
pp. 328
Author(s):  
Kamil Anasiewicz ◽  
Józef Kuczmaszewski
Keyword(s):  
Numerical Model ◽  
Young’S Modulus ◽  
Adhesive Joint ◽  
Young's Modulus ◽  
Precise Determination ◽  
Adhesive Joints ◽  
Experimental Conditions ◽  
Element Simulation ◽  
Joint Material

This article is an evaluation of the phenomena occurring in adhesive joints during curing and their consequences. Considering changes in the values of Young’s modulus distributed along the joint thickness, and potential changes in adhesive strength in the cured state, the use of a numerical model may make it possible to improve finite element simulation effects and bring their results closer to experimental data. The results of a tensile test of a double overlap adhesive joint sample, performed using an extensometer, are presented. This test allowed for the precise determination of the shear modulus G of the cured adhesive under experimental conditions. Then, on the basis of the research carried out so far, a numerical model was built, taking the differences observed in the properties of the joint material into account. The stress distribution in a three-zone adhesive joint was analyzed in comparison to the standard numerical model in which the adhesive in the joint was treated as isotropic. It is proposed that a joint model with three-zones, differing in the Young’s modulus values, is more accurate for mapping the experimental results.

Factors affecting in vitro and in vivo antioxidant effects. Experimental conditions and nature of oxidants determine antioxidant efficacy

2021 ◽  
pp. 1-9
Author(s):  
Etsuo Niki
Keyword(s):  
Biological Molecules ◽  
Experimental Conditions ◽  
Factors Affecting ◽  
Beneficial Effects ◽  
Multiple Oxidants ◽  
Antioxidant Effects

Reactive oxygen and nitrogen species have been implicated in the onset and progression of various diseases and the role of antioxidants in the maintenance of health and prevention of diseases has received much attention. The action and effect of antioxidants have been studied extensively under different reaction conditions in multiple media. The antioxidant effects are determined by many factors. This review aims to discuss several important issues that should be considered for determination of experimental conditions and interpretation of experimental results in order to understand the beneficial effects and limit of antioxidants against detrimental oxidation of biological molecules. Emphasis was laid on cell culture experiments and effects of diversity of multiple oxidants on antioxidant efficacy.

scholarly journals Application of Bar Adsorptive Microextraction for the Determination of Levels of Tricyclic Antidepressants in Urine Samples

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  
Keyword(s):  
Tricyclic Antidepressants ◽  
Matrix Effects ◽  
Activated Carbons ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Experimental Conditions ◽  
Analytical Methodology ◽  
Low Efficiency

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.

scholarly journals Validation of a Method Based on Triglycerides for the Detection of Low Percentages of Hazelnut Oil in Olive Oil by Column Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1346-1353 ◽  
Author(s):  
Diego L García-González ◽  
María Viera-Macías ◽  
Ramón Aparicio-Ruiz ◽  
Maria T Morales ◽  
Ramón Aparicio
Keyword(s):  
Liquid Chromatography ◽  
Olive Oil ◽  
Carbon Number ◽  
Hazelnut Oil ◽  
Equivalent Carbon Number ◽  
Experimental Conditions ◽  
Mathematical Algorithm ◽  
Relative Standard ◽  
Triglyceride Content ◽  
The Difference

Abstract The difference between theoretical and empirical triglyceride content is a powerful tool to detect the presence of any vegetable oil in olive oil. The current drawback of the method is the separation between equivalent carbon number ECN42 compounds, which affects the reliability of the method and, hence, its cutoff limit. The determination of the triglyceride profile by liquid chromatography using propionitrile as the mobile phase has recently been proposed to improve their quantification, together with a mathematical algorithm whose binary response determines the presence or absence of hazelnut oil. Twenty-one laboratories from 9 countries participated in an interlaboratory study to evaluate the performance characteristics of the whole analytical method. Participants analyzed 12 samples in duplicate, split into 3 intercomparison studies. Statistically significant differences due to the experimental conditions were found in some laboratories, which were detected as outliers by use of Cochran's and Grubbs' tests. The relative standard deviations (RSD) for repeatability and reproducibility were determined following the AOAC Guidelines for Collaborative Studies. The analytical properties of the method were determined by means of the sensitivity (0.86), selectivity (0.94), and reliability (72) for a cutoff limit of 8 (probability 94).

scholarly journals Reaktive E=C(p–p)π Systeme, XXXIV Addition von Alkoholen oder primären Aminen an Phosphaalkene F3CP=C(F)OR. Neue Trifluormethylphosphane und -phosphaalkene/Reactive E = C( p – p ) π-Systems, XXXIV Addition of Alcohols or Primary Amines to Phosphaalkenes F3CP= C(F)OR . Novel Trifluoromethylphosphanes and Phosphaalkenes

1993 ◽  
Vol 48 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Joseph Grobe ◽  
Duc Le Van ◽  
Gudrun Lange
Keyword(s):  
High Resolution Mass Spectrometry ◽  
Molar Ratio ◽  
Primary Amines ◽  
The Novel ◽  
Experimental Conditions ◽  
Pull System ◽  
Fragment Ions ◽  
New Compounds ◽  
C Nmr

The course of the reactions o f fluorophosphaalkenes F3CP = C (F)OR [R = Me (1), Et (2)] with methanol or ethanol strongly depends on the experimental conditions. Thus at 70 °C a mixture of the 2-phosphapropionic acid ester F3CP (H )CO2R [R = Me (3), Et (4)] and trifluoromethylphosphane H2PCF3 is formed [molar ratio: 3 or 4 /H2 CF3 ≈1/1]. If the precursors F3CP (H )CO2R [R = Me (3), Et) are used as starting materials, the reaction with ROH under the same conditions affords 3 and 4, respectively, (90 to 95% yield) with only traces of H2PCF 3. In the presence o f iPr2NH these precursors react with R′OH to give the novel trifluoromethylphosphaalkenes F3CP = C (OR )OR [R /R′: Me/Me (6); E t/E t (7); Me/Et (8)]. With Et2NH , 3 undergoes an addition/elimination process yielding the interesting push/pull system Et2N(F)C = P-CO2Me (5). 1 and 2 react with primary amines R′NH2 (R′= tBu, Me) with stereoselective formation of the fairly labile phosphaalkenes F3CP = C(OR)NHR′ [R /R′: Me/tBu (9), Et/tBu(10), Me/Me (11)] with trans-positions for CF3 and NHR′.The new compounds 3 -11 were characterized by spectroscopic investigations (1H , 19F, 31P, 13C NMR ; IR, MS) and determination of M+ or typical fragment ions [M+ -OR ] by high resolution mass spectrometry.

On the Negative Excess Isotherms for Methane Adsorption at High Pressure: Modeling and Experiment

SPE Journal ◽  
2019 ◽  
Vol 24 (06) ◽  
pp. 2504-2525 ◽  
Author(s):  
Jing Li ◽  
Keliu Wu ◽  
Zhangxin Chen ◽  
Kun Wang ◽  
Jia Luo ◽  
...  
Keyword(s):  
High Pressure ◽  
Mass Balance ◽  
High Pressures ◽  
Pore Wall ◽  
Void Volume ◽  
Excess Adsorption ◽  
Experimental Conditions ◽  
Accessible Volume ◽  
Adsorbed Phase

Summary An excess adsorption amount obtained in experiments is always determined by mass balance with a void volume measured by helium (He) –expansion tests. However, He, with a small kinetic diameter, can penetrate into narrow pores in porous media that are inaccessible to adsorbate gases [e.g., methane (CH4)]. Thus, the actual accessible volume for a specific adsorbate is always overestimated by an He–based void volume; such overestimation directly leads to errors in the determination of excess isotherms in the laboratory, such as “negative isotherms” for gas adsorption at high pressures, which further affects an accurate description of total gas in place (GIP) for shale–gas reservoirs. In this work, the mass balance for determining the adsorbed amount is rewritten, and two particular concepts, an “apparent excess adsorption” and an “actual excess adsorption,” are considered. Apparent adsorption is directly determined by an He–based volume, corresponding to the traditional treatment in experimental conditions, whereas actual adsorption is determined by an adsorbate–accessible volume, where pore–wall potential is always nonpositive (i.e., an attractive molecule/pore–wall interaction). Results show the following: The apparent excess isotherm determined by the He–based volume gradually becomes negative at high pressures, but the actual one determined by the adsorbate–accessible volume always remains positive.The negative adsorption phenomenon in the apparent excess isotherm is a result of the overestimation in the adsorbate–accessible volume, and a larger overestimation leads to an earlier appearance of this negative adsorption.The positive amount in the actual excess isotherm indicates that the adsorbed phase is always denser than the bulk gas because of the molecule/pore–wall attraction aiding the compression of the adsorbed molecules. Practically, an overestimation in pore volume (PV) is only 3.74% for our studied sample, but it leads to an underestimation reaching up to 22.1% in the actual excess amount at geologic conditions (i.e., approximately 47 MPa and approximately 384 K). Such an overestimation in PV also underestimates the proportions of the adsorbed–gas amount to the free–gas amount and to the total GIP. Therefore, our present work underlines the importance of a void volume in the determination of adsorption isotherms; moreover, we establish a path for a more–accurate evaluation of gas storage in geologic shale reservoirs with high pressure.

Determination of the Isoflavone Genistein in Soybeans by High-Performance Liquid Chromatography Following Cloud Point Extraction

2012 ◽  
Vol 95 (3) ◽  
pp. 845-849 ◽  
Author(s):  
Mohammad Mirzaei ◽  
Atieh Karimi Naeini ◽  
Mansoureh Behzadi
Keyword(s):  
Cloud Point ◽  
High Performance ◽  
Cloud Point Extraction ◽  
Uv Detector ◽  
Experimental Conditions ◽  
Solid Ratio ◽  
Assisted Extraction ◽  
Ultrasonic Assisted ◽  
Replicate Measurements

Abstract A simple and sensitive method has been developed for preconcentration and determination of genistein in soybeans. This method is based on cloud point extraction (CPE) of genistein from soybeans using ethylene glycol monoalkyl ether (Genapol X-080) as a nonionic surfactant. The concentration of extracted genistein was determined by HPLC with a UV detector. Optimum experimental conditions were established. With 5% Genapol X-080 (v/v), a liquid/solid ratio of 25:1 mL/g, and ultrasonic-assisted extraction at 40°C for 45 min, the extraction percentage of genistein reached its highest value. The preconcentration factor for genistein was about 16.5. The RSD for seven replicate measurements and the LOD were ±4.45% and 15.0 ng/mL, respectively. CPE is simple, inexpensive, and suitable for extraction of genistein from soybean. It uses environmentally friendly surfactants and offers a convenient alternative to more conventional extraction systems.

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