840 resultados para SAMPLE DILUTION
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Microwave digestions of mercury in Standards Reference Material (SRM) coal samples with nitric acid and hydrogen peroxide in quartz vessels were compared with Teflon® vessel digestion by using flow injection cold vapor atomic absorption spectrometry. Teflon® vessels gave poor reproducibiUty and tended to deliver high values, while the digestion results from quartz vessel show good agreement with certificate values and better standard deviations. Trace level elements (Ag, Ba, Cd, Cr, Co, Cu, Fe, Mg, Mn, Mo, Pb, Sn, Ti, V and Zn) in used oil and residual oil samples were determined by inductively coupled plasma-optical emission spectrometry. Different microwave digestion programs were developed for each sample and most of the results are in good agreement with certified values. The disagreement with values for Ag was due to the precipitation of Ag in sample; while Sn, V and Zn values had good recoveries from the spike test, which suggests that these certified values might need to be reconsidered. Gold, silver, copper, cadmium, cobalt, nickel and zinc were determined by continuous hydride generation inductively coupled plasma-optical emission spectrometry. The performance of two sample introduction systems: MSIS™ and gas-liquid separator were compared. Under the respective optimum conditions, MSIS^"^ showed better sensitivity and lower detection limits for Ag, Cd, Cu, Co and similar values for Au, Ni and Zn to those for the gas-liquid separator.
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The nature of this research is to investigate paleoseismic deformation of glacial soft sediments from three sampling sites throughout the Scottish Highlands; Arrat's Mills, Meikleour and Glen Roy. The paleoseismic evidence investigated in this research will provide a basis for applying criteria to soft sediment deformation structures, and the trigger mechanisms that create these structures. Micromorphology is the tool used in this to investigate paleoseismic deformation structures in thin section. Thin section analysis, (micromorphology) of glacial sediments from the three sampling sites is used to determine microscale evidence of past earthquakes that can be correlated to modem-day events and possibly lead to a better understanding of the impact of earthquakes throughout a range of sediment types. The significance of the three sampling locations is their proximity to two major active fault zones that cross Scotland. The fault zones are the Highland Boundary Fault and the Great Glen Fault, these two major faults that parallel each other and divide the country in half Sims (1975) used a set of seven criteria that identified soft sediment deformation structures created by a magnitude six earthquake in Cahfomia. Using criteria set forth by Sims (1975), the paleoseismic evidence can be correlated to the magnitude of the deformation structures found in the glacial sediments. This research determined that the microstructures at Arrat's Mill, Meikleour and Glen Roy are consistent with a seismically induced origin. It has also been demonstrated that, even without the presence of macrostructures, the use of micromorphology techniques in detecting such activity within sediments is of immense value.
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The effects of sample solvent composition and the injection volume, on the chromatographic peak profiles of two carbamate derivatives, methyl 2-benzimidazolecarbamate (MBC) and 3-butyl-2,4-dioxo[1,2-a]-s-triazinobenzimidazole (STB), were studied using reverse phase high performance liquid chromatograph. The study examined the effects of acetonitrile percentage in the sample solvent from 5 to 50%, effects of methanol percentage from 5 to 50%, effects of pH increase from 4.42 to 9.10, and effect of increasing buffer concentration from ° to 0.12M. The effects were studied at constant and increasing injection mass and at four injection volumes of 10, 50, 100 and 200 uL. The study demonstrated that the amount and the type of the organic solvents, the pH, and the buffer strength of the sample solution can have a pronounced effect on the peak heights, peak widths, and retention times of compounds analysed. MBC, which is capable of intramolecular hydrogen bonding and has no tendency to ionize, showed a predictable increase .in band broadening and a decrease in retention times at higher eluting strengths of the sample solvent. STB, which has a tendency to ionize or to strongly interact with the sample solvent, was influenced in various ways by the changes in ths sample solvent composition. The sample solvent effects became more pronounced as the injection volume increased and as the percentage of organic solvent in the sample solution became greater. The peak height increases for STB at increasing buffer concentrations became much more pronounced at higher analyte concentrations. It was shown that the widely accepted procedure of dissolving samples in the mobile phase does not yield the most efficient chromatograms. For that reason samples should be dissolved in the solutions with higher aqueous content than that of the mobile phase whenever possible. The results strongly recommend that all the samples and standards, regardless whether the standards are external or internal, be analysed at a constant sample composition and a constant injection volume.
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This study investigated, retrospectively, whether recidivism in a sample of court-ordered'graduates of an alcohol education and awareness program could be predicted. This alcohol education program was based on adult education principles and was philosophically akin to the thoughts of Drs. Jack Mezirow, Stephen Brookfield, and Patricia Cranton. Data on the sample of 214 Halton IDEA (Impaired Driver Education and Awareness) graduates were entered into a spread sheet. Descriptive statistics were generated. Each of the 214 program graduates had taken several tests during the course of the IDEA program. These tests measured knowledge, attitude about impaired driving, and degree of alcohol involvement. Test scores were analyzed to determine whether those IDEA graduates who recidivated differed in any measurable way from those who had no further criminal convictions after a period of at least three years. Their criminal records were obtained from the Canadian Police Information Centre (CPIC). Those program graduates who reoffended were compared to the vast majority who did not reoffend. Results of the study indicated that there was no way to determine who would recidivate from the data that were collected. Further studies could use a qualitative model. Follow-up interviews could be used to determine what impact, if any, attendance at the IDEA program had on the life of the graduates.
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This study sought to compare the results of the Motivation Assessment Scale (MAS; Durand & Crimmins, 1988), Questions About Behavior Function Scale (QABF; Matson & Vollmer, 1996) and Functional Analysis Screening Tool (FAST; Iwata & Deleon, 1996), when completed by parent informants in a sample of children and youth with autism spectrum disorders (ASD) who display challenging behaviour. Results indicated that there was low agreement between the functional hypotheses derived from each of three measures. In addition, correlations between functionally analogous scales were substantially lower than expected, while correlations between non-analogous subscales were stronger than anticipated. As indicated by this study, clinicians choosing to use FBA questionnaires to assess behavioural function, may not obtain accurate functional hypotheses, potentially resulting in ineffective intervention plans. The current study underscores the caution that must be taken when asking parents to complete these questionnaires to determine the function(s) of challenging behaviour for children/youth with ASD.
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The present research focused on the pathways through which the symptoms of posttraumatic stress disorder (PTSD) may negatively impact intimacy. Previous research has confirmed a link between self-reported PTSD symptoms and intimacy; however, a thorough examination of mediating paths, partner effects, and secondary traumatization has not yet been realized. With a sample of 297 heterosexual couples, intraindividual and dyadic models were developed to explain the relationships between PTSD symptoms and intimacy in the context of interdependence theory, attachment theory, and models of selfpreservation (e.g., fight-or-flight). The current study replicated the findings of others and has supported a process in which affective (alexithymia, negative affect, positive affect) and communication (demand-withdraw behaviour, self-concealment, and constructive communication) pathways mediate the intraindividual and dyadic relationships between PTSD symptoms and intimacy. Moreover, it also found that the PTSD symptoms of each partner were significantly related; however, this was only the case for those dyads in which the partners had disclosed most everything about their traumatic experiences. As such, secondary traumatization was supported. Finally, although the overall pattern of results suggest a total negative effect of PTSD symptoms on intimacy, a sex difference was evident such that the direct effect of the woman's PTSD symptoms were positively associated with both her and her partner's intimacy. I t is possible that the Tend-andBefriend model of threat response, wherein women are said to foster social bonds in the face of distress, may account for this sex difference. Overall, however, it is clear that PTSD symptoms were negatively associated with relationship quality and attention to this impact in the development of diagnostic criteria and treatment protocols is necessary.
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Payment for the Cogswell, Sample and Howard accounts, Feb. 29, 1884.
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Payment for the Cogswell, Howard and Sample accounts, Aug. 29, 1884.
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Payment for the Cogswell, Howard and Sample accounts, Feb. 27, 1885.
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The effects of magnetic dilution and applied pressure on frustrated spinels GeNi2O4, GeCo2O4, and NiAl2O4 are reported. Dilution was achieved by substitution of Mg2+ in place of magnetically active Co2+ and Ni2+ ions. Large values of the percolation thresholds were found in GeNi(2-x)MgxO4. Specifically, pc1 = 0.74 and pc2 = 0.65 in the sub-networks associated with the triangular and kagome planes, respectively. This anomalous behaviour may be explained by the kagome and triangular planes behaving as coupled networks, also know as a network of networks. In simulations of coupled lattices that form a network of networks, similar anomalous percolation threshold values have been found. In addition, at dilution levels above x=0.30, there is a T^2 dependency in the magnetic heat capacity which may indicate two dimensional spin glass behaviour. Applied pressures in the range of 0 GPa to 1.2 GPa yield a slight decrease in ordering temperature for both the kagome and triangular planes. In GeCo(2-x)MgxO4, the long range magnetic order is more robust with a percolation threshold of pc=0.448. Similar to diluted nickel germanate, at low temperatures, a T^2 magnetic heat capacity contribution is present which indicates a shift from a 3D ordered state to a 2D spin glass state in the presence of increased dilution. Dynamic magnetic susceptibility data indicate a change from canonical spin glass to a cluster glass behaviour. In addition, there is a non-linear increase in ordering temperature with applied pressure in the range P = 0 to 1.0 GPa. A spin glass ground state was observed in Ni(1-x)MgxAl2O4 for (x=0 to 0.375). Analysis of dynamic magnetic susceptibility data yield a characteristic time of tau* = 1.0x10^(-13) s, which is indicative of canonical spin glass behaviour. This is further corroborated by the linear behaviour of the magnetic specific heat contribution. However, the increasing frequency dependence of the freezing temperature suggests a trend towards spin cluster glass formation.
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In the context of multivariate linear regression (MLR) models, it is well known that commonly employed asymptotic test criteria are seriously biased towards overrejection. In this paper, we propose a general method for constructing exact tests of possibly nonlinear hypotheses on the coefficients of MLR systems. For the case of uniform linear hypotheses, we present exact distributional invariance results concerning several standard test criteria. These include Wilks' likelihood ratio (LR) criterion as well as trace and maximum root criteria. The normality assumption is not necessary for most of the results to hold. Implications for inference are two-fold. First, invariance to nuisance parameters entails that the technique of Monte Carlo tests can be applied on all these statistics to obtain exact tests of uniform linear hypotheses. Second, the invariance property of the latter statistic is exploited to derive general nuisance-parameter-free bounds on the distribution of the LR statistic for arbitrary hypotheses. Even though it may be difficult to compute these bounds analytically, they can easily be simulated, hence yielding exact bounds Monte Carlo tests. Illustrative simulation experiments show that the bounds are sufficiently tight to provide conclusive results with a high probability. Our findings illustrate the value of the bounds as a tool to be used in conjunction with more traditional simulation-based test methods (e.g., the parametric bootstrap) which may be applied when the bounds are not conclusive.
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In this paper, we develop finite-sample inference procedures for stationary and nonstationary autoregressive (AR) models. The method is based on special properties of Markov processes and a split-sample technique. The results on Markovian processes (intercalary independence and truncation) only require the existence of conditional densities. They are proved for possibly nonstationary and/or non-Gaussian multivariate Markov processes. In the context of a linear regression model with AR(1) errors, we show how these results can be used to simplify the distributional properties of the model by conditioning a subset of the data on the remaining observations. This transformation leads to a new model which has the form of a two-sided autoregression to which standard classical linear regression inference techniques can be applied. We show how to derive tests and confidence sets for the mean and/or autoregressive parameters of the model. We also develop a test on the order of an autoregression. We show that a combination of subsample-based inferences can improve the performance of the procedure. An application to U.S. domestic investment data illustrates the method.
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A wide range of tests for heteroskedasticity have been proposed in the econometric and statistics literature. Although a few exact homoskedasticity tests are available, the commonly employed procedures are quite generally based on asymptotic approximations which may not provide good size control in finite samples. There has been a number of recent studies that seek to improve the reliability of common heteroskedasticity tests using Edgeworth, Bartlett, jackknife and bootstrap methods. Yet the latter remain approximate. In this paper, we describe a solution to the problem of controlling the size of homoskedasticity tests in linear regression contexts. We study procedures based on the standard test statistics [e.g., the Goldfeld-Quandt, Glejser, Bartlett, Cochran, Hartley, Breusch-Pagan-Godfrey, White and Szroeter criteria] as well as tests for autoregressive conditional heteroskedasticity (ARCH-type models). We also suggest several extensions of the existing procedures (sup-type of combined test statistics) to allow for unknown breakpoints in the error variance. We exploit the technique of Monte Carlo tests to obtain provably exact p-values, for both the standard and the new tests suggested. We show that the MC test procedure conveniently solves the intractable null distribution problem, in particular those raised by the sup-type and combined test statistics as well as (when relevant) unidentified nuisance parameter problems under the null hypothesis. The method proposed works in exactly the same way with both Gaussian and non-Gaussian disturbance distributions [such as heavy-tailed or stable distributions]. The performance of the procedures is examined by simulation. The Monte Carlo experiments conducted focus on : (1) ARCH, GARCH, and ARCH-in-mean alternatives; (2) the case where the variance increases monotonically with : (i) one exogenous variable, and (ii) the mean of the dependent variable; (3) grouped heteroskedasticity; (4) breaks in variance at unknown points. We find that the proposed tests achieve perfect size control and have good power.
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In this paper, we study several tests for the equality of two unknown distributions. Two are based on empirical distribution functions, three others on nonparametric probability density estimates, and the last ones on differences between sample moments. We suggest controlling the size of such tests (under nonparametric assumptions) by using permutational versions of the tests jointly with the method of Monte Carlo tests properly adjusted to deal with discrete distributions. We also propose a combined test procedure, whose level is again perfectly controlled through the Monte Carlo test technique and has better power properties than the individual tests that are combined. Finally, in a simulation experiment, we show that the technique suggested provides perfect control of test size and that the new tests proposed can yield sizeable power improvements.
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Ce Texte Presente Plusieurs Resultats Exacts Sur les Seconds Moments des Autocorrelations Echantillonnales, Pour des Series Gaussiennes Ou Non-Gaussiennes. Nous Donnons D'abord des Formules Generales Pour la Moyenne, la Variance et les Covariances des Autocorrelations Echantillonnales, Dans le Cas Ou les Variables de la Serie Sont Interchangeables. Nous Deduisons de Celles-Ci des Bornes Pour les Variances et les Covariances des Autocorrelations Echantillonnales. Ces Bornes Sont Utilisees Pour Obtenir des Limites Exactes Sur les Points Critiques Lorsqu'on Teste le Caractere Aleatoire D'une Serie Chronologique, Sans Qu'aucune Hypothese Soit Necessaire Sur la Forme de la Distribution Sous-Jacente. Nous Donnons des Formules Exactes et Explicites Pour les Variances et Covariances des Autocorrelations Dans le Cas Ou la Serie Est un Bruit Blanc Gaussien. Nous Montrons Que Ces Resultats Sont Aussi Valides Lorsque la Distribution de la Serie Est Spheriquement Symetrique. Nous Presentons les Resultats D'une Simulation Qui Indiquent Clairement Qu'on Approxime Beaucoup Mieux la Distribution des Autocorrelations Echantillonnales En Normalisant Celles-Ci Avec la Moyenne et la Variance Exactes et En Utilisant la Loi N(0,1) Asymptotique, Plutot Qu'en Employant les Seconds Moments Approximatifs Couramment En Usage. Nous Etudions Aussi les Variances et Covariances Exactes D'autocorrelations Basees Sur les Rangs des Observations.