994 resultados para limit of quantitation


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Background: Total immunoglobulin A in saliva (s-IgA) is normally assayed using an enzyme-linked immunosorbent assay. We have investigated methodological issues relating to the use of particle-enhanced nephelometric immunoassay (PENIA)
to measure s-IgA in whole unstimulated saliva and determine its reference range.

Methods: Whole unstimulated resting saliva was collected to determine sample stability (temperature, time, effect of a protease inhibitor), limit of quantitation (LOQ), assay precision and analytical variation. The reference range for 134 healthy adults was determined.

Results: Linearity was excellent (4–10.3 mg L21, P, 0.001; R2 ¼ 0.997) and without significant bias (mean of 20.7%). The lowest intra- and inter-analytical coefficients of variation were 1.8% and 7.5% and LOQ was 1.4 mg L21. The concentration of s-IgA is stable at room temperature for up to 6 h, at 48C for 48 h, at 248C for two weeks and at 2808C for up to 1.3 yr. There is no evidence that a protease inhibitor increases the stability or that repeated freeze–thawing cycles degrade sample quality. The reference ranges for s-IgA concentration, s-IgA secretion, s-IgA:albumin and s-IgA:osmolality were 15.9–414.5 mg L21, 7.2–234.9 mg min21, 0.4–19 and 0.6–8.9, respectively.

Conclusion:
Automated PENIA assay of s-IgA is precise and accurate. High stability of collected saliva samples and the ease and speed of the assay make this an ideal method for use in athletic and military training situations. The convenience of measuring albumin and IgA on the same analytical platform adds to the practicability of the test.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Lipid peroxidation (LPO) has been associated with periodontal disease, and the evaluation of malondialdehyde (MDA) in the gingival crevicular fluid (GCF), an inflammatory exudate from the surrounding tissue of the periodontium, may be useful to clarify the role of LPO in the pathogenesis of periodontal disease. We describe the validation of a method to measure MDA in the GCF using high-performance liquid chromatography. MDA calibration curves were prepared with phosphate-buffered solution spiked with increasing known concentrations of MDA. Healthy and diseased GCF samples were collected from the same patient to avoid interindividual variability. MDA response was linear in the range measured, and excellent agreement was observed between added and detected concentrations of MDA. Samples' intra- and interday coefficients of variation were below 6.3% and 12.4%, respectively. The limit of quantitation (signal/noise = 5) was 0.03 mu M. When the validated method was applied to the GCF, excellent agreement was observed in the MDA quantitation from healthy and diseased sites, and diseased sites presented more MDA than healthy sites (P < 0.05). In this study, a validated method for MDA quantitation in GCF was established with satisfactory sensitivity, precision, and accuracy. (C) 2012 Elsevier Inc. All rights reserved.

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Calciothermic reduction of TiO2 provides a potentially low-cost route to titanium production. Presented in this article is a suitably designed diagram, useful for assessing the degree of reduction of TiO2 and residual oxygen contamination in metal as a function of reduction temperature and other process parameters. The oxygen chemical potential diagram à la Ellingham-Richardson-Jeffes is useful for visualization of the thermodynamics of reduction reactions at high temperatures. Although traditionally the diagram depicts oxygen potentials corresponding to the oxidation of different metals to their corresponding oxides or of lower oxides to higher oxides, oxygen potentials associated with solution phases at constant composition can be readily superimposed. The usefulness of the diagram for an insightful analysis of calciothermic reduction, either direct or through an electrochemical process, is discussed. Identified are possible process variations, modeling and optimization strategies.

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Plastic limit of fine-grained soils is conventionally determined in the laboratory by the soil thread rolling method. Many adverse comments have been recorded in the geotechnical engineering literature on the method about its reproducibility and operator dependency. The presen experimental study, which is based on a well-planned and meticulously executed experimental program, critically evaluates the effect of size of the rolled soil thread on the plastic limit of fine-grained soil and the operator dependency of the results. The results have shown that if the plastic limit tests are performed by a trained operator, then consistent results can be obtained and that the effect of size of the rolled soil thread on plastic limit is negligibly small.

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The heats of combustion of mono-, di-, tri- and tetramethylammonium perchlorates have been determined by bomb calorimetry. The data have been used to explain why the thermal behavior of ammonium perchlorate (AP) is considerably modified in presence of these compounds as shown by differential thermal analysis. Above a particular concentration of methylammonium perchlorate (MAP), AP ignites in a single step around 290°C. The minimum concentration of a MAP (mono-, di-, tri- or tetra-) needed to cause ignition of AP in a single step depends on intramolecular “elemental stoichiometric coefficient” of the mixtures that has the same value regardless of the MAP. Furthermore, the calorimetric values of these mixtures are the same. The heat evolved on ignition of such a composition appears to determine the lower concentration limit of combustion of its mixture with AP.

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The maximum height of a siphon is generally assumed to be dependent on barometric pressure—about 10 m at sea level. This limit arises because the pressure in a siphon above the upper reservoir level is below the ambient pressure, and when the height of a siphon approaches 10 m, the pressure at the crown of the siphon falls below the vapour pressure of water causing water to boil breaking the column. After breaking, the columns on either side are supported by differential pressure between ambient and the low-pressure region at the top of the siphon. Here we report an experiment of a siphon operating at sea level at a height of 15 m, well above 10 m. Prior degassing of the water prevented cavitation. This experiment provides conclusive evidence that siphons operate through gravity and molecular cohesion.

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This paper elucidates the relative importance of soil structure and various compositional factors in influencing the liquid limit of natural kaolinitic soils. Earlier studies dealt with purified systems and anticipated that the liquid limit of the soils would increase with percentage clay size fraction and surface area, and that soils with a greater degree of paricle flocculation would possess a higher liquid limit than soils with a more parallel particle arrangement. The results revealed that the inter-particle attraction and repulsion forces have a prominent role in determining the liquid limit of kaolinitic soils. These forces determine the particle arrangement (clay fabric) which in turn regulates the liquid limit values. The influence of clay fabric was ascertained from the relationships of liquid limit with shrinkage limit and sediment volume (in water) values. It was anticipated that kaolinitic soils with a greater degree of particle flocculatin and a higher liquid limit would shrink less and occupy a higher sedimentation volume. As expected an increase in liquid limit was accompanied by an increase in shrinkage limit and sediment volume in water.

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A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method was developed to determine olanzapine (OLZ) in human urine. After solid-phase extraction with SPE cartridge, the urine sample was analysed on a C-18 column (Symmetry 3.5 mu m, 50 x 4.6 mm i.d) interfaced with a triple quadrupole tandem mass spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of ammonium acetate (pH 7.8)-acetonitrile (10:90, v/v). The method was linear over a concentration range of 1-100 ngml(-1). The lower limit of quantitation was 1 ngml(-1). The intra-day and inter-day relative standard deviation across three validation runs over the entire concentration range was < 11.5 %. The accuracy determined at three concentrations (8.0, 50.0 and 85.0 ngml(-1) OLZ) was within +/- 1.21 % in terms of relative errors.

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Nonextremal solution with warped resolved-deformed conifold background is important to study the infrared limit of large N thermal QCD. Earlier works in this direction have not taken into account all the backreactions on the geometry, namely from the branes, fluxes, and black-hole carefully. In the present work we make some progress in this direction by solving explicitly the supergravity equations of motions in the presence of the backreaction from the black hole. The backreactions from the branes and the fluxes on the other hand and to the order that we study, are comparatively suppressed. Our analysis reveal, among other things, how the resolution parameter would depend on the horizon radius and how the renormalization group flows of the coupling constants should be understood in these scenarios, including their effects on the background three-form fluxes. We also study the effect of switching on a chemical potential in the background and, in a particularly simplified scenario, compute the actual value of the chemical potential for our case.

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In this study, the influence of tool rotation speed and feed rate on the forming limit of friction stir welded Al 6061-T651 sheets has been investigated. The forming limit curve was evaluated by limit dome height test performed on all the friction stir welded sheets. The welding trials were conducted at a tool rotation speed of 1300 and 1400 r/min and feed rate of 90 and 100 mm/min. A third trial of welding was performed at a rotational speed of 1500 r/min and feed rate 120 mm/min. It is found that with increase in the tool rotation speed, from 1300 to 1400 r/min, for a constant feed rate, the forming limit of friction stir welded blank has improved and with increase in feed rate, from 90 to 100 mm/min, for a constant tool rotation speed, it has decreased. The forming limit of friction stir welded sheets is better than unwelded sheets. The thickness gradient after forming is severe in the cases of friction stir welded blanks made at higher feed rate and lower rotation speed. The strain hardening exponent of weld (n) increases with increase in tool rotation speed and it decreases with increase in feed rate. It has been demonstrated that the change in the forming limit of friction stir welded sheets with respect to welding parameters is due to the thickness distribution severity and strain hardening exponent of the weld region during forming. There is not much variation in the dome height among the friction stir welded sheets tested. When compared with unwelded sheets, dome height of friction stir welded sheets is higher in near-plane-strain condition, but it is lesser in stretching strain paths.

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While Fiber Bragg Grating (FBG) sensors have been extensively used for temperature and strain sensing, clad etched FBGs (EFBGs) have only recently been explored for refractive index sensing. Prior literature in EFBG based refractive index sensing predominantly deals with bulk refractometry only, where the Bragg wavelength shift of the sensor as a function of the bulk refractive index of the sample can be analytically modeled, unlike the situation for adsorption of molecular thin films on the sensor surface. We used a finite element model to calculate the Bragg wavelength change as a function of thickness and refractive index of the adsorbing molecular layer and compared the model with the real-time, in-situ measurement of electrostatic layer-by-layer (LbL) assembly of weak polyelectrolytes on the silica surface of EFBGs. We then used this model to calculate the layer thickness of LbL films and found them to be in agreement with literature. Further, we used this model to arrive at a realistic estimate of the limit of detection of EFBG sensors based on nominal measurement noise levels in current FBG interrogation systems and found that sufficiently thinned EFBGs can provide a competitive platform for real-time measurement of molecular interactions while simultaneously leveraging the high multiplexing capabilities of fiber optics.

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Is the Chandrasekhar mass limit for white dwarfs (WDs) set in stone? Not anymore, recent observations of over-luminous, peculiar type Ia supernovae can be explained if significantly super-Chandrasekhar WDs exist as their progenitors, thus barring them to be used as cosmic distance indicators. However, there is no estimate of a mass limit for these super-Chandrasekhar WD candidates yet. Can they be arbitrarily large? In fact, the answer is no! We arrive at this revelation by exploiting the flux freezing theorem in observed, accreting, magnetized WDs, which brings in Landau quantization of the underlying electron degenerate gas. This essay presents the calculations which pave the way for the ultimate (significantly super-Chandrasekhar) mass limit of WDs, heralding a paradigm shift 80 years after Chandrasekhar's discovery.

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The present article describes a working or combined calibration curve in laser-induced breakdown spectroscopic analysis, which is the cumulative result of the calibration curves obtained from neutral and singly ionized atomic emission spectral lines. This working calibration curve reduces the effect of change in matrix between different zone soils and certified soil samples because it includes both the species' (neutral and singly ionized) concentration of the element of interest. The limit of detection using a working calibration curve is found better as compared to its constituent calibration curves (i.e., individual calibration curves). The quantitative results obtained using the working calibration curve is in better agreement with the result of inductively coupled plasma-atomic emission spectroscopy as compared to the result obtained using its constituent calibration curves.